xgt7000v manual

X-RAY ANALYTICAL MICROSCOPEXGT-7000V

Instruction ManualCODE:GZ0000090619

July, 2007 © 2007 HORIBA, Ltd.

PrefaceThis manual describes the operation of the X-RAY ANALYTICAL MICROSCOPE, XGT-7000V. Be sure to read this manual before using the product to ensure proper and safe operation ofthe instrument. Also safely store the manual so it is readily available whenever necessary.

Product specifications and appearance, as well as the contents of this manual are subject tochange without notice.

Warranty and ResponsibilityHORIBA warrants that the Product shall be free from defects in material and workmanshipand agrees to repair or replace free of charge, at HORIBA’s option, any malfunctioned ordamaged Product attributable to HORIBA’s responsibility for a period of one (1) year from thedelivery unless otherwise agreed with a written agreement. In any one of the following cases,none of the warranties set forth herein shall be extended；

Any malfunction or damage attributable to improper operationAny malfunction attributable to repair or modification by any person not authorized byHORIBA Any malfunction or damage attributable to the use in an environment not specified in thismanualAny malfunction or damage attributable to violation of the instructions in this manual oroperations in the manner not specified in this manualAny malfunction or damage attributable to any cause or causes beyond the reasonablecontrol of HORIBA such as natural disastersAny deterioration in appearance attributable to corrosion, rust, and so onReplacement of consumables

HORIBA SHALL NOT BE LIABLE FOR ANY DAMAGES RESULTING FROM ANYMALFUNCTIONS OF THE PRODUCT, ANY ERASURE OF DATA, OR ANY OTHER USESOF THE PRODUCT.

TrademarksGenerally, company names and brand names are either registered trademarks or trademarksof the respective companies.

Conformable DirectiveThis equipment conforms to the following directives and standards:

Installation EnvironmentThis product is designed for the following environment.

Installation Categories IIPollution degree 2

Information on Disposal of Electrical and Electronic Equipment

FCC RulesAny changes or modifications not expressly approved by the party responsible for complianceshall void the user's authority to operate the equipment.

WARNINGThis equipment has been tested and found to comply with the limits for a Class A digitaldevice, pursuant to part 15 of the FCC Rules. These limits are designed to providedreasonable protection against harmful interference when the equipment is operated in acommercial environment. This equipment generates, uses, and can radiate radio frequencyenergy and, if not installed and used in accordance with the instruction manual, may causeharmful interference to radio communications. Operation of this equipment in a residential area is likely to cause harmful interference inwhich case the user will be required to correct the interference at his own expense.

Directives: the EMC Directive 89/336/EEC, in accordance with Article 10(1) of the Directivethe Low Voltage Directive 2006/95/EC

Standards: [the EMC Directive]EN61326: 1997/A3: 2003 Class B, Minimum requirements[the Low Voltage Directive] EN61010-1: 2001

The crossed out wheeled bin symbol shown on the product oraccompanying documents indicates separate collection for waste electricaland electronic equipment (WEEE) under the WEEE Directive 2002/96/EC inthe European Union.This product should not be disposed of as unsorted household waste.

Your correct disposal of WEEE will contribute to reducing wasteful consumption of naturalresources and protecting human health and the environment from potential negative effectscaused by hazardous substances in products.

Contact your supplier for information on applicable disposal methods.

For your safetyWarning messages are described in the following manner. Read the messages and follow theinstructions carefully.

Meaning of warning messages

Symbols

This indicates an imminently hazardous situation which, if not avoided, will result in death or serious injury. This signal word is to be limited to the most extreme situations.

This indicates a potentially hazardous situation which, if not avoided, could result in death or serious injury.

This indicates a potentially hazardous situation which, if not avoided, may result in minor or moderate injury. It may also be used to alert against unsafe practices.Without safety alert indication of hazardous situation which, if not avoided, could result in property damage.

Description of what should be done, or what should be followed

Description of what should never be done, or what is prohibited

Safety PrecautionsThis section provides precautions to enable you to use the product safely and correctly and toprevent injury and damage. The terms of DANGER, WARNING, and CAUTION indicate thedegree of imminency and hazardous situation. Read the precautions carefully as it containsimportant safety messages.

DANGER

High voltageDo not touch inside with power ON.

Electrical hazardous voltage can cause shock or death.Do not disconnect HV connector while power is ON. Wait one minute after poert is turned OFF.

WARNING

Electric ShockTo prevent electric shock, ground this unit.However, never ground it using a hazardous medium such as gas pipe.

Extremely Low Temperature (-196°C)Do not touch low-temperature parts.When replenishing liquid nitrogen (-196°C), make sure to wear safety glasses and thermal insulated leather gloves, and handle the liquid nitrogen carefully to keep it away from the skin and clothing.If liquid nitrogen is spilled or splashed on the skin or clothing, it may cause serious damage to the skin and subcutaneous tissue.

Oxygen DeficiencyMake sure to ventilate the room to avoid the risk of suffocation.Nitrogen gas (N2) can create oxygen deficient atmosphere.

CAUTION

If the X-ray indicator remains lit even when the sample chamber cover is open (to insert a sample or for any other reason), discontinue use of the XGT-7000V immediately, to prevent possible damage to hands or fingers inside the chamber.

Be careful not to spill out the liquid nitrogen when refilling.If liquid nitrogen spills on the detector cable or peripheral devices, it may cause breakage.

When opening/closing the door, move down the Z axis from the measurement position referring to the height adjustment camera. Opening/closing the door without the Z axis moved down may damage the sample.

Since the accurate stage is mounted to the door, open/close the door slowly. If not so, the door may be broken or the stage may be damaged.

Be sure not to pinch your hand at opening/closing the door. Otherwise it can cause injury.

In replenishing liquid nitrogen, the funnel and beaker are cooled to a very low temperature. Hold the upper part of the funnel and the grip of the beaker.Do not apply any force on the frozen funnel and beaker. They can be broken easily. If the funnel or beaker is cracked, replace it with new one.If liquid nitrogen overflows from the inlet, do not force the lid onto the inlet, and just wait for liquid nitrogen to evaporate naturally.

Put nothing on the fan filter. If not so, the XGT-7000V may be damaged.

Points of concernUse of the equipment in a manner not specified by the manufacturer may impair the protectionprovided by the equipment. And it may also reduce equipment performance.The product employs precision driving parts (XYZ stage) and a high-voltage power source forX-ray. Therefore, exercise the following precautions:

Use the product in an environment free from corrosive gas.Avoid using the product in a location close to equipment using strong electric power (suchas an electric furnace), or near a radio or sound wave source.Do not give a shock or large vibrations to the product. To move the product to anotherlocation, contact our service or sales office.Avoid turning ON the power again immediately after turning it OFF.Since Windows XP is used, the specified procedure must be taken to shut off the power.Read this instruction manual carefully, and follow the relevant instructions.Do not use the cord set (power cable) for other products than this system.Be sure to observe the cautionary matters written in this manual for handling this system.

Disposal of the productWhen disposing of the product, follow the related laws and/or regulations of your country fordisposal of the product.

Description in this manualNote

This interprets the necessary points for correct operation and notifies the important points forhandling the unit.

ReferenceThis indicates the part of where to refer the information.

TipThis indicates reference information.

Contents

1 BEFORE USING THE XGT-7000V . . . . . . . . . . . . . . . . . . . . . 11.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

1.2 System configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.2.1 Appearance of the XGT-7000V . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

1.3 Name and explanation of analysis unit . . . . . . . . . . . . . . . . . . . . . 31.3.1 Analysis unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31.3.2 Right side of analysis unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41.3.3 Indicator of analysis unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51.3.4 Operation panel of analysis unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71.3.5 XGT controller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

1.4 Installation conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

1.5 Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101.5.1 Modification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101.5.2 Power cable . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101.5.3 Grounding . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101.5.4 Physical shock (impact) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101.5.5 User of XGT-7000V software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101.5.6 Power setting on PC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101.5.7 Installing other applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101.5.8 Handling of liquid and powder samples . . . . . . . . . . . . . . . . . . . . . . . 101.5.9 Handling liquid nitrogen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 111.5.10 Connecting detector cables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 111.5.11 Vacuum pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

1.6 Filling dewar with liquid nitrogen . . . . . . . . . . . . . . . . . . . . . . . . . . 12

2 BASIC OPERATIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132.1 Starting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

2.2 How to shut-down . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

2.3 Opening/closing sample chamber door . . . . . . . . . . . . . . . . . . . . 15

3 SAMPLE SETUP AND VACUUMING . . . . . . . . . . . . . . . . . . . 163.1 Mounting sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

3.1.1 Samples with a thickness of less than 15 mm . . . . . . . . . . . . . . . . . . 163.1.2 Samples with a thickness of 15 mm to 33 mm . . . . . . . . . . . . . . . . . 183.1.3 Samples with a thickness of 34 mm to 53 mm . . . . . . . . . . . . . . . . . 203.1.4 Samples with a thickness of 54 mm to 72 mm . . . . . . . . . . . . . . . . . 223.1.5 Samples with a thickness of 73 mm to 93 mm . . . . . . . . . . . . . . . . . 243.1.6 Samples with low-contrast transmission X-ray . . . . . . . . . . . . . . . . . 263.1.7 Transmitted X-ray Filter Insertion . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

3.2 Evacuating the analysis probe and sample chamber . . . . . . . . . . 28

3.3 Adjustment of Optical Image Window . . . . . . . . . . . . . . . . . . . . . . 29

3.3.1 Setting of X-ray applied position . . . . . . . . . . . . . . . . . . . . . . . . . . . . 293.3.2 Compensate stage moving distance . . . . . . . . . . . . . . . . . . . . . . . . . 313.3.3 Whole image position calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . 313.3.4 Adjustment of height standard line . . . . . . . . . . . . . . . . . . . . . . . . . . 31

4 MAINTENANCE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 324.1 Replenishing liquid nitrogen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

4.2 Checking vacuum condition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 364.2.1 Checking vacuum condition of the analysis probe . . . . . . . . . . . . . . 364.2.2 Checking vacuum condition of the sample chamber . . . . . . . . . . . . 36

4.3 Checking X-ray generator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

4.4 Checking vacuum condition of sample chamber . . . . . . . . . . . . . 37

4.5 Applying grease to the XY stage . . . . . . . . . . . . . . . . . . . . . . . . . 38

4.6 Replacing the X-ray indicator (X-RAYS ON) lamp . . . . . . . . . . . . 39

4.7 Cleaning the fan filters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

4.8 Analysis probe window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 414.8.1 Installation procedure for analysis probe window . . . . . . . . . . . . . . . 414.8.2 How to remove the analysis probe window . . . . . . . . . . . . . . . . . . . 43

5 TROUBLESHOOTING . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 445.1 Alarm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44

5.2 Power supply troubles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

5.3 Operation troubles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46

5.4 Other troubles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

6 APPENDIX . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 486.1 Measurement Principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

6.2 Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 516.2.1 Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 516.2.2 Data processor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 526.2.3 Ambient conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 536.2.4 Power source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 536.2.5 Mass . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 536.2.6 Dimensions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53

6.3 Wiring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

7 ACCESSORIES. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56

1 BEFORE USING THE XGT-7000V

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1.1 OverviewThe XGT-7000V X-Ray Analytical Microscope has been designed to simultaneously measureand analyze the transmitted X-ray image, fluorescent X-ray image, and X-ray spectrum of asample. The XGT-7000V allows you to analyze the elements contained in a sample(qualitative analysis) and the content of a certain element (quantitative analysis). It is alsocapable of analyzing the inner structure of a sample using transmitted X-rays as well asanalyzing the distribution of elements using the mapping function. By using the X-ray GuideTube (XGT), the X-ray can be narrowed down without reducing the intensity, enabling amicroanalysis in a shorter time.

Instead of using a conventional detector that must be cooled with liquid nitrogen to preventlithium from spreading, the XGT-7000V uses a high-purity silicon detector called XEROPHY®.Since liquid nitrogen needs to be filled only when a measurement is performed, there issubstantial labor savings in both handling and maintenance.

The software installed in the XGT-7000V is compatible with Microsoft Windows, so thatanybody can operate it.

A handy clipboard enables spectrums, analysis results, images and other data to betransferred to other Microsoft Windows-compatible applications.


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1.2 System configuration

1.2.1 Appearance of the XGT-7000VXGT-7000V consists of the following units.

Fig. 1 View of the XGT-7000VNames and explanation of analysis unit

Analysis unit: radiates X-rays to the sample and then detects the emitted fluorescentX-rays with its semiconductor type detector.

Personal computer: control the measurement operations and display, save, or access thecollected data.

Data processor: processes the measured signals sent from the detector.XGT controller: is a control device for manually moving the sample stage in the X-Ydi-

rection. A power switch and emergency stop switch for the XGT arealso incorporated.

Printer: prints out a hard copy of the data.Vacuum pump: produces vacuum for surrounding section of detector and sample

chamber.

Analysis unit

Dataprocessor

Display

Personalcomputer

Printer

XGT controller

Vacuum pump


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1.3 Name and explanation of analysis unit

1.3.1 Analysis unit.

Fig. 2 Analysis unit

1 Indicator lamp Indicates the state of XGT-7000V.“ 1.3.3 Indicator of analysis unit ” (page 5).

2 Operation panel of analysis unit

It is equipped with a timer, dimming control, and vacuum leak switch. For more information, refer to “ 1.3.4 Operation panel of analysis unit ” (page 7).

3 Handle for chamber open/close

While pulling down the sample chamber door unlock levers, pull the both handles toward you. The sample chamber door will open. The door will start moving down after pulling it fully to the front. To close the door, lift the door to the point where it can move horizontally, and then slide the door toward the back until it is locked.

4 Sample chamber door unlock levers

Pulling down these levers at the both sides unlocks the sample chamber door.


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1.3.2 Right side of analysis unit

Fig. 3 Right side of analysis unit

5 XYZ stage This is a unit to move the sample into 3 axis directions.

6 Sample holder This is a holder to set samples. It is necessary to change the holder height depending on the sample height.

ReferenceRefer to “ 3.1 Mounting sample ” (page 16).

7 Whole image observation camera

The whole image observation camera is a CCD camera to display the whole image of the sample in optical image window.

8 Detailed image observation camera

The detailed image observation camera is a CCD camera to display the magnified image of the sample in optical image window.

9 Sample height adjustment camera

The sample height adjustment camera is a camera to adjust sample height.

10 Vacuum piping interface For vacuuming, connect the part to vacuum pump with metal flexible tube.


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1.3.3 Indicator of analysis unit

Fig. 4 Indicator of analysis unit

11 Liquid nitrogen (LN) check lamp

A lamp to indicate the remained volume of liquid nitrogen and the detector state. Green lamp lit: liquid nitrogen left Red lamp lit: No liquid nitrogen left, detector is not returned to room temperature Orange lamp lit: No liquid nitrogen left, detector is at room temperature

12 X-ray circuitry reset button　（ERR)

This is the lamp to be lit when an error has occurred.It illuminates when the equipment cannot be vacuumed within a set time or no X-rays are generated.When the lamp is lit, troubleshoot it referring to “ 5 TROUBLESHOOTING ” (page 44).

13 X-ray indicator (X-RAYS ON)

The X-ray indicator lights up when X-rays are being radiated. This indicator is linked to the open-close switch for the sample chamber cover and to the start/stop of the measurement. When this indicator dies, X-ray is not generated any longer. As long as the indicator is normal, pressing the switch will make the indicator lit. If pressing the switch does not make the indicator lit, replace the indicator because it is out of operation.

NoteWhen there is no liquid nitrogen left, replenish it by referring to “ 4.1 Replenishing liquid nitrogen ”(page 33).

CAUTION

If the X-ray indicator remains lit even when the sample chamber cover is open (to insert a sample or for any other reason), discontinue use of the XGT-7000V immediately, to prevent possible damage to hands or fingers inside the chamber.

NoteDo not press the switch when the X-ray indicator light is on. The X-ray stops generating andmeasurement stops.


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Table 1 Status of the vacuum indicator

14Vacuum pump switch/Vacuum indicator for chamber(VAC C)

A switch to turn ON/OFF the vacuum pump to evacuate the chamber. The color changes depending on the status of the equipment. Refer to Table 1 for details.

15Vacuum pump switch/Vacuum indicator for analysis probe(VAC P)

A switch to turn ON/OFF the vacuum pump to evacuate the surround-ings of XGT and Si detector. The color changes depending on the status of the equipment. Refer to Table 1 for details.

NoteGenerally, the lamp turns to green (vacuum status) with approx. 2 minutes.If the vacuum pump switch/vacuum indicator (VAC) for chamber does not turn to green even after 3minutes have passed since the vacuum pump was turned ON, the pump is automatically turned OFFalso. In those situations, refer to “ 5 TROUBLESHOOTING ” (page 44).

NoteGenerally, the lamp turns to green (vacuum status) with approx. 10 seconds.s

Switch Color of indicator Status

VAC C

Green Under vacuum pressure

Red

Under normal pressureThe pump does not start operating even if you press the button. This status is caused by the following:

The lid of the sample chamber is open.The analysis probe window has been installed.The vacuum leak switch is set to AIR.

Orange

Under normal pressureThe vacuum pump starts operating by pressing the button. It will turn green when the equipment has reached a vacuum.

VAC P

Green Under vacuum pressure

Red

Under normal pressureThe pump does not start operating even if you press the button. This status is caused by the following:

No analysis probe window has been installed.The vacuum leak switch is set to AIR.

Orange

Under normal pressureThe vacuum pump starts operating by pressing the button. It will turn green when the equipment has reached a vacuum.


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1.3.4 Operation panel of analysis unit

Fig. 5 Operation panel of analysis unit

16 Hour meter The hour meter lets you to see the operating hours of the X-ray gener-ator.

17 Vacuum leak switch

The vacuum leak switch is the switch with a lock which returns the pressure around the XGT and the Si detector to air pressure. If this switch is turned upwards, the pressure returns to air pressure with the solenoid valve open.Pull down the edge of the toggle before switching the switch.

NoteBe sure to turn OFF the vacuum pump before operation. Check that this switch is turned downwardsbefore turning ON the vacuum pump.

18 Whole image illumination volume

The whole image illumination volume is a control volume to adjust brightness of the entire images.

19 Detailed image illumination volume

The detailed image illumination volume is a control volume to adjust brightness of the minute images.

20 Transmit illumination volumeThe transmit illumination volume is a control volume to adjust brightness in observing the detailed images by transmitted illumination.

21 Sample chamber illumination volume

The sample chamber illumination volume allows you to control the brightness in the sample chamber.


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1.3.5 XGT controller

1 Emergency stop switch

This switch is used to pause the operation of the equipment when it is malfunctioning. Pressing this button causes power shutdown and emergency stop of the analysis unit. To restart it, turn OFF the power switch, return the button to the original state by rotating the red flange, and then turn ON the power switch. And reboot the PC.

2 Power switch (key switch)This is the key switch for turning ON the equipment power.Turning it to the back turns ON the power while turning it to the front turns OFF the power.

3 Z-axis stage operation switch

This is the switch for moving the sample stage up and down. With the switch at the top of the lever pressed down, the stage goes up by tilting the lever toward the back and goes down by tilting the lever toward the front.The more the lever is tilted, the faster the stage moves. If the switch at the top of the lever is released, the stage stops moving regardless of the angle of the lever.

NoteMove the stage while checking with eyes. Do not move up the stage once the detailed image isfocused, as that position is the upper limit of the movement. Otherwise, the sample and/orequipment may be damaged.

4 XY axes stage operation switch

This switch is used for manually moving the sample stage right and left (X-axis) as well as front and back (Y-axis). The more the lever is tilted, the faster the stage moves.

NoteIf the key is lost, you can no longer start up the equipment. Take maximum care for it.Please contact us when you lost it. We will reissue it.


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1.4 Installation conditionsTo enable the proper use of the XGT-7000V, pay attention to the following installationconditions.

TemperatureOperating temperature: 5°C to 40°CTemperature to guarantee performance: 10°C to 35°C

HumidityMaximum relative humidity 80% for temperatures up to 31°C from 5°C decreasing linearlyto 50％ relative humidity at 40°C.

PowerVoltage: Single phase,100 V, 120 V, 220 V, 240 V AC ±10%Frequency: 50 Hz/60 Hz ±1.0%Power consumption: Below 1.5 kVA (60 Hz), Below 1.8 kVA (50 Hz) (Including vacuum pump, but excluding PC, LCD, and printer)

Installation space2.4 m × 1.3 m or wider(Leave approximately one additional meter of space around the periphery of the XGT-7000Vto allow for maintenance work.)

NoteThe effects of ambient temperature may alter image position. Minimize fluctuation of ambienttemperature to within 3°C when measuring minute areas.When the equipment is continuously used at temperatures of 35°C or higher, lower the tube currentand tube voltage so that the temperature of the X-ray tube will not rise too high. When the equipment is used at temperatures of 10°C or lower, it takes more time to evacuate theequipment. If the evacuation has failed to finish by the set time with the ERR lamp illuminated, pressthe ERR lamp to cancel the error and reactivate the vacuum pump.

NoteIf using in a different power supply voltage from the time of shipment, contact the nearestHORIBA sales representatives.Prepare 1 set of AC 3 P plug. Refer to “ Fig. 15 Wiring (XGT-7000V) ” (page 55).To prevent electric shock, ground the XGT-7000V.

NoteThe total mass of this unit is about 260 kg. Install the XGT-7000V in a horizontal and solidlocation.Vibration may cause a jumbled image. Install the XGT-7000V in a vibration-free location.


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1.5 Precautions

1.5.1 ModificationDo not disassemble or modify the internal workings of the XGT-7000V.

1.5.2 Power cableDo not use the power code that comes with the product for other instruments.

1.5.3 Grounding

To prevent electric shock and to ensure proper performance of the XGT-7000V, be sure thesystem is grounded.

1.5.4 Physical shock (impact)Ensure that the analyzer receives no external shock.Do not allow the analyzer to experience strong shock from external sources. The inner surfaceof the liquid nitrogen filler port is especially delicate, so use special care when filling the dewarwith liquid nitrogen.The personal computer has a built-in hard disk. Hard disks are sensitive to shock, so usesufficient care around this unit.

1.5.5 User of XGT-7000V softwareThis software should be used by the user authorized as “Administrator.”

1.5.6 Power setting on PCSet the power supply setting to "System standby: No" in the control panel. Otherwise, it maycause the XGT-7000V to malfunction.

1.5.7 Installing other applicationsThe operation of the XGT-7000V cannot be guaranteed if software applications other than theXGT-7000V application are installed. If the XGT-7000V does not operate well with anothersoftware application, discontinue the use of that application.

1.5.8 Handling of liquid and powder samplesDO NOT vacuum the sample chamber when a liquid or powder sample is measured.Otherwise, it may spray the sample in the chamber, causing the breakdown of the equipment.When measuring such samples, be sure to install an analysis probe window.

WARNING

Electric ShockTo prevent electric shock, ground this unit.However, never ground it using a hazardous medium such as gas pipe.


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1.5.9 Handling liquid nitrogen

1.5.10 Connecting detector cablesThere are proper procedures for connecting and disconnecting the detector cables from theanalyzer and from the detector. If these procedures are not followed correctly, the detectormay be damaged. Refer to “ Fig. 15 Wiring (XGT-7000V) ” (page 55).

1.5.11 Vacuum pumpDo not keep running the pump with air open as it may cause the malfunction.

WARNING

Extremely Low Temperature (-196°C)Do not touch low-temperature parts.When replenishing liquid nitrogen (-196°C), make sure to wear safety glasses and thermal insulated leather gloves, and handle the liquid nitrogen carefully to keep it away from the skin and clothing.If liquid nitrogen is spilled or splashed on the skin or clothing, it may cause serious damage to the skin and subcutaneous tissue.


CAUTION



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1.6 Filling dewar with liquid nitrogenTo check the remained volume of the liquid nitrogen, “ Liquid nitrogen (LN) check lamp ”(page 5) of the analysis unit explanation.Liquid nitrogen can cause frostbite and suffocation. Use with sufficient care when handlingliquid nitrogen. Be sure to read “ 1.5.8 Handling of liquid and powder samples ” (page 10),before filling the dewar with liquid nitrogen.

When no liquid nitrogen is left, the liquid nitrogen (LN) check lamp changes from green lampto red lamp. When the detector becomes at room temperature, the orange lamp lights.

When the orange lamp is lit, turn off the power of the whole system and replenish the liquidnitrogen. Wait for more than an hour and then turn on the power of the whole system.If the elapsed time is within an hour after the red lamp is lit, turn off the power of the wholesystem and replenish the liquid nitrogen. The system will be ready to use after waiting forapproximately 30 minutes.If the elapsed time is more than an hour after the red lamp is lit, wait until the orange lamplights and then replenish the liquid nitrogen.It takes about 10 hours to change from red light to orange light (the time differs by ambienttemperature). If the analyzer is used in high frequency, we recommend to replenish the liquidnitrogen on every third day of operation before the liquid nitrogen runs out.The capacity of the dewar is 3 L. The consumption of the liquid nitrogen is 1 L per daymaximum.At continuous measurements, replenish the liquid nitrogen at least every three days isrecommended.

The Xerophy detector has a built-in protection circuit that prevents damage to the detectoreven if the power of the unit is turned ON with no liquid nitrogen in the detector.

ReferenceIf no liquid nitrogen is remained, replenish by referring to “ 4.1 Replenishing liquid nitrogen ” (page33).

NoteEven if the elapsed time is more than an hour after the red lamp is lighted, the liquid nitrogen can bereplenished and be used before the lamp changes to orange. However, ice may form inside the dewar tank (the amount of ice depends on the water content ofliquid nitrogen and the ambient humidity).When ice forms inside the Dewar tank, the detector element cannot be cooled. An electrical noisewill be generated because the small parts of ice move inside the dewar tank. This may cause atemporary decline in the performance of energy resolution.As to the above, we recommend to resupply liquid nitrogen after the lamp turns to orange. If the decline of performance happens in energy resolution, return the Dewar tank to roomtemperature and remove all water content from inside the tank. Then replenish with liquid nitrogenagain.

2 BASIC OPERATIONS

13

2 BASIC OPERATIONS

2.1 StartingBefore turning the power ON, check the following points:

Is the detector filled with liquid nitrogen?Fill the detector with liquid nitrogen at least one hour before starting the analysis. Thedetector does not function without liquid nitrogen.

Is the consumption of liquid nitrogen increasing?If the detector malfunctions and the amount of internal vacuum deteriorates, theconsumption of liquid nitrogen will increase. (e.g., Although the dewar was full theprevious day, it became empty the following day.) When this occurs, stop using XGT-7000V and contact the nearest HORIBA sales representatives.

The ambient temperature must no exceed the guaranteed operating temperature.

Operation procedure1. Turn ON the key switch for the XGT controller.

Power is ON for analyzing unit, data processing unit, vacuum pump, and printer.2. Turn ON the power switch located on the personal computer.

Windows starts up.3. Click the program start up menu and select “Horiba” and “XGT-7000V”.

XGT-7000V starts up.

4. Select “Spectrum” or “Mapping “ button on Navigator and click “Sam-ple”

button.5. Click “Origin Search” button.

“Origin Search” dialog box appears.

6. Click on the “OK” button.The origin search is performed.

7. Measure the provided copper plate and perform the warm-up operation.Set the provided copper plate to the XGT-7000V and perform the measurement with themeasurement conditions of X-ray tube vol. ”50 kV”, Current “1 mA”, Process time “1”, and10 µmXGT for approx. 1000 seconds.

ReferenceFor how to operate the software, refer to the help documentation that comes with the software.

2 BASIC OPERATIONS

14

2.2 How to shut-downExiting XGT-7000V programTerminate the XGT program by performing the following steps, returning to the Windowsscreen:

1. Click on the button in the upper right corner of the title bar in the Spectrumwindow.

2. Quit Windows after shutdown of the program.

Turning OFF XGT-7000V power switch1. Turn OFF the key switch.

NoteTurning OFF the power when still accessing a floppy or hard disk may damage the disk.

2 BASIC OPERATIONS

15

2.3 Opening/closing sample chamber doorThe locking mechanism is provided for the sample chamber door of XGT-7000V taking thesafety into consideration.To open the door, therefore, it is necessary to pull down the sample chamber door unlocklever.

When opening the sample chamber door:1. While pulling down the sample chamber door unlock levers, pull the sample

chamber door toward you.2. After pulling the sample chamber door to the front, push it downward.

When closing the sample chamber door:1. Hold the handles with both hands, lift the sample chamber door to the point where

it can move horizontally, and then push it toward the back.2. Push it until you hear a click sound.

NoteBoth the right and left lock levers must be unlocked.Be careful not to pinch the hand when you lower it.

1. Pull down the unlock lever toward you. 2. Pull toward you.

3. Push down.

4. Lift it horizontally and push it until you hear a click sound.

3 SAMPLE SETUP AND VACUUMING

16


3.1 Mounting sampleThe XGT-7000V is capable of measuring samples with a thickness of up to 100 mm using the20-mm-thick sample holders.

NoteTo measure a sample with an uneven surface, focus the highest portion of the surface and never liftthe probe any more. Otherwise, the analysis probe may come into contact with the sample.

3.1.1 Samples with a thickness of less than 15 mmUse sample mounting tray P and four sample holders.Operation procedure1. Affix the sample onto sample mounting tray P using tapes such as carbon tape and

dual-sided adhesive tape. Be sure the surface of sample is as horizontal as possible.

2. Mount sample mounting tray P onto a sample holder and secure it with the fourscrews.

3. Mount the sample holder that contains the sample mounting tray onto the otherthree holders that have been piled up.

4. Click the [Move to sample exchange position] in the Sample window of the XGT-7000V software. The XYZ stage will move toward you.

5. Open the sample chamber door of the analysis unit. 6. Pull down the Z stage operation switch and lower the XYZ stage to the bottom.


17

7. Mount the sample holders on the XYZ stage and secure it with the knurl screws atthe front and the right side.

8. Close the sample chamber door.9. Click the [Height regulation camera] button in the Sample window of the XGT-7000V

software. The view is switched to that of the height regulation camera and the sample is shown onthe screen.

10. Adjust the height of the stage using the stage Z axis precision feed switch so thatthe highest point of the sample comes under the standard line for height.

11. Click the [Whole Image] in the Sample window of the XGT-7000V software. Confirm that the whole image of the sample is displayed on the screen.

Top of XY stage

Sample holder

Screws


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3.1.2 Samples with a thickness of 15 mm to 33 mmUse sample mounting tray P and three sample holders.Operation procedure1. Affix the sample onto sample mounting tray P using tapes such as carbon tape and



3. Mount the sample holder that contains the sample mounting tray onto the other twoholders that have been piled up.


5. Open the sample chamber door of the analysis unit. 6. Pull down the Z stage operation switch and lower the XYZ stage to the bottom. 7. Mount the sample holders on the XYZ stage and secure it with the knurl screws at

the front and the right side. 8. Close the sample chamber door.9. Click the [Height regulation camera] button in the Sample window of the XGT-7000V





19

Top of XY stage

Sample holder

Screws


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3.1.3 Samples with a thickness of 34 mm to 53 mmUse sample mounting tray P and two sample holders.Operation procedure1. Affix the sample onto sample mounting tray P using tapes such as carbon tape and



3. Mount the sample holder that contains the sample mounting tray onto the otherholder.


5. Open the sample chamber door of the analysis unit.6. Pull down the Z stage operation switch and lower the XYZ stage to the bottom. 7. Mount the sample holders on the XYZ stage and secure it with the knurl screws at






21

Top of XY stage

Sample holder

Screws


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3.1.4 Samples with a thickness of 54 mm to 72 mmUse sample mounting tray P and one sample holder.Operation procedure1. Affix the sample onto sample mounting tray P using tapes such as carbon tape and




4. Open the sample chamber door of the analysis unit. 5. Pull down the Z stage operation switch and lower the XYZ stage to the bottom.6. Mount the sample holders on the XYZ stage and secure it with the knurl screws at






23

Top of XY stage

Sample holder

Screws


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3.1.5 Samples with a thickness of 73 mm to 93 mmUse sample mounting tray P and one sample holder.Operation procedure1. Mount sample mounting tray P onto a sample holder and secure it with the four

screws.


3. Open the sample chamber door of the analysis unit.4. Pull down the Z stage operation switch and lower the XYZ stage to the bottom. 5. Secure the sample holder with the knurl screws at the front and the right side with

the sample mounting tray placed at the bottom. 6. Mount the sample. 7. Close the sample chamber door.8. Click the [Height regulation camera] button in the Sample window of the XGT-7000V





25

Top of XY stage

Sample holder

Screws


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3.1.6 Samples with low-contrast transmission X-rayWhen you analyze a very thin sample or one susceptible to the influence from acrylic samplemounting tray in terms of X-ray absorption, use sample mounting tray L. How to affix the sample1. Affix the X-ray transmission film on the center hole (50 mm square) of sample

mounting tray L using tapes.

2. Affix the sample onto the center of the X-ray transmission film using tapes such ascarbon tape and two-sided adhesive tape.

Sample holderUse different sample holders for samples with different thicknesses as shown below.

NoteSample holders need to be changed according to the thickness of the sample due to the limitation ofthe stage stroke in Z-axis.


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3.1.7 Transmitted X-ray Filter InsertionWhen a transmitted X-ray image is reversed, insert a transmitted X-ray filter.

NoteNormally, remove the transmitted X-ray filter when using.When the reversed image does not improve even by transmitted X-ray filter insertion, decreasethe current value to obtain a good image. Refer to the help documentation for how to adjust thecurrent value.

Operating procedure1. Open the chamber door.2. Push the changeover knob shown in Fig. X toward the stage side.3. When removing the transmitted X-ray filter, pull the changeover knob in the

opposite direction of the stage.

Fig. 6 Changing the transmitted X-ray filter (Figure showing the XGT with the filter inserted)

Changeover knob

Transmitted X-ray filter

When taking it off

When inserting it


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3.2 Evacuating the analysis probe and sample chamberEvacuating the analysis probe and sample chamber produces a vacuum around the sample,making light elements (11Na to 13Al) detectable. Operation procedure1. Check that either one of the vacuum pump switch/vacuum indicator (VAC) for

analysis probe or chamber is lit in orange. The vacuum indicator for the analysis probe is lit in orange when the vacuum holding filmis used, while the vacuum indicator for the chamber is lit when no vacuum holding film isused.

2. Press the vacuum pump switch lit in orange. The vacuum pump will turn ON and start vacuuming. The vacuum pump turns OFF if youpress the switch once again.

Once the analysis probe is vacuumed, it will not return to the atmospheric pressure unless thevacuum leak switch is used. To return it to the atmospheric pressure in cases where theanalysis probe window is removed or X-ray transmission film is replaced, pull the top of thevacuum leak switch toggle upward and then push down the switch upward.

NoteDO NOT vacuum the sample chamber when a liquid or powder sample is measured. Otherwise, it mayspray the sample in the chamber, causing the breakdown of the equipment. When measuring suchsamples, be sure to install an analysis probe window.

NoteNo indicator will illuminate in orange when the vacuum leak switch is set to the AIR side or thesample chamber door is not fully closed. When both the indicators are lit in red, check both thevacuum leak switch and the sample chamber door.

NoteIf the vacuum pump switch/vacuum indicator (VAC) for analysis probe does not turn to greeneven after 30 seconds have passed since the vacuum pump was turned ON, the pump isautomatically turned OFF. If the vacuum pump switch/vacuum indicator (VAC) for chamber doesnot turn to green even after 3 minutes have passed since the vacuum pump was turned ON, thepump is automatically turned OFF also. In those situations, refer to “ 5 TROUBLESHOOTING ”(page 44).


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3.3 Adjustment of Optical Image Window

3.3.1 Setting of X-ray applied positionThis is the setting which the actual X-ray applied position corresponds to the crossing point ofthe cross maker to show the applied position. Perform the setting when there is a gapbetween the crossing point of the cross maker and X-ray applied position.For the detailed explanation on the operating procedure, refer to the help documentation.

Operation procedureFor 10 µm XGT: 1. Set the sample for calibration of X-ray applied position and adjust the focus.2. Move the stage so that the center of the hole to adjust XGT which diameter is 10 µm

corresponds to the cross point of cross marker indicating the X-ray appliedposition.

Fig. 7 Magnified image of calibration sample

Adjustment for XGT with diameter of 10 µm

Adjustment for XGT with diameter of 100 µm

45 µm ± 5 µm dia. hole Slit with 105 µm + 5 µm width (horizontal/vertical)

( part is W: formation membrane part of tungsten)


30

3. Map the calibration sample for irradiation position using the following conditions.

4. Move the X-ray applied position to the center point of the calibration sample forirradiation position based on the acquired image.

5. Adjust the X-ray applied position in accordance with the settings of [Option] - [Set-ting of Video Windows].

For φ100 µm XGT:1. Perform the same procedure with φ10 µm XGT. Set the sample for calibration of X-

ray applied position. Move the stage so that the center of the hole to adjust XGTwhich diameter is φ100 µm corresponds to the cross point of cross markerindicating the X-ray applied position.

2. Perform the operation by following the same procedure of φ10 µm XGT.

XGT diameter: 10 µmX-ray tube voltage: 50 kVX-ray tube current: 1 mARepeatability: 1Live time: 200 secondsPixels: 256 pixels × 256 pixelsWidth: 0.512 mm

XGT diameter: 100 µmX-ray tube voltage: 15 kVX-ray tube current: 1 mARepeatability: 1Live time: 200 secondsPixels: 256 pixels × 256 pixelsWidth: 0.512 mm


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3.3.2 Compensate stage moving distanceThe followings are the explanation of how to calibrate the actual stage moving distance inaccordance with the distance on the optical microscope image.For the explanation on the operating procedure, refer to the help documentation.

3.3.3 Whole image position calibrationThis compensates the image position moving by clicking the [Whole image] button.For the explanation on the operating procedure, refer to the help documentation.

NoteBefore executing this function, set the whole image calibration sample, switch to the detailed imageand focus the camera.

3.3.4 Adjustment of height standard lineThe following is the adjustment procedure of height standard line displayed in adjusting theheight.For the explanation on the operating procedure, refer to the help documentation.

4 MAINTENANCE

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4 MAINTENANCEIn order to use the unit in good accuracy, periodical maintenance is needed.

Check item Maintenance period Note

Replenishing liquid nitrogen Daily page 33

Checking vacuum condition Daily page 36

Checking X-ray generator Monthly page 37

Checking vacuum pump oil level Every 3 months page 37

Cleaning the fan filters Every 6 months page 40

Replacing vacuum pump oil Every year page 37

Applying grease to the XY stage Once a year (recommended) page 38

Replacing the X-ray indicator (X-RAYS ON) lamp When the lamp burns out page 39

Replacing the analysis probe window When the film breaks page 41

4 MAINTENANCE

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4.1 Replenishing liquid nitrogen

For the replenish of liquid nitrogen, be sure to check the color of the liquid nitrogen (LN) checklamp. “ Liquid nitrogen (LN) check lamp ” (page 5).

Operation procedure1. Remove the stopper cap of the liquid nitrogen holding vessel on the top surface of

the rear of the analysis unit.

WARNING

Extremely Low Temperature (-196 )Do not touch low-temperature parts.When replenishing liquid nitrogen (-196 ), make sure to wear safety glasses and thermal insulated leather gloves, and handle the liquid nitrogen carefully to keep it away from the skin and clothing.If liquid nitrogen is spilled or splashed on the skin or clothing, it may cause serious damage to the skin and subcutaneous tissue.


CAUTION


4 MAINTENANCE

34

2. Insert the special funnel exclusive for replenishing liquid nitrogen into the openingwith the overflow hose draped on the left side of analysis unit.

3. Press gently the rubber part of the funnel so that it may block the opening fully.

4. Place the beaker under the end of the overflow hose to catch any excess liquidnitrogen.The beaker is intended only to prevent the overflow from spattering on the floor.Do not use it to replenish liquid nitrogen.

4 MAINTENANCE

35

5. Supply liquid nitrogen.Use an insulated container to carry liquid nitrogen and supply it until it reaches the upperlevel marked on the funnel.

6. Stop pouring in liquid nitrogen when it has started coming out of the overflow hoseand into the beaker. Do not remove the funnel until all liquid nitrogen has drainedout of it.

CAUTION

In replenishing liquid nitrogen, the funnel and beaker are cooled to a very low temperature. Hold the upper part of the funnel and the grip of the beaker.Do not apply any force on the frozen funnel and beaker. They can be broken easily. If the funnel or beaker is cracked, replace it with new one.If liquid nitrogen overflows from the inlet, do not force the lid onto the inlet, and just wait for liquid nitrogen to evaporate naturally.

4 MAINTENANCE

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4.2 Checking vacuum condition

4.2.1 Checking vacuum condition of the analysis probe

Meaning of lamp color:Green lamp lit: vacuum conditionRed lamp lit: not ready for vacuumingOrange lamp lit: ready for vacuuming

The vacuuming for the analysis probe cannot be done without the X-ray window mounted.Before vacuuming, check that the X-ray window is mounted and the lamp turns in orange.

Before measuring a sample, check that the analysis probe is evacuated (vacuuming) byturning ON the vacuum switch for analysis probe. When the XGT-7000V is in normal status,the lamp color will change to green (Vacuum status) with approx. 10 seconds.

If the probe is not evacuated, or the VAC lamp continues lighting red, perform the operationsof “ 4.6 Replacing the X-ray indicator (X-RAYS ON) lamp ” (page 39) and “ 4.4 Checkingvacuum condition of sample chamber ” (page 37).

4.2.2 Checking vacuum condition of the sample chamber

Meaning of lamp color:Green lamp lit: vacuum condition Red lamp lit: not ready for vacuumingOrange lamp lit: ready for vacuuming

The vacuuming for the sample chamber cannot be done with the X-ray window mounted.Before vacuuming, check that the X-ray window is removed and the lamp turns in orange.(Vacuuming the sample chamber simultaneously evacuates inside the analysis probe.)

Before measuring a sample, check that the sample chamber is evacuated (vacuuming) byturning ON the vacuum switch for analysis probe. When the XGT-7000V is in normal status,the lamp color will change to green (Vacuum status) with approx. 2 minutes.

NoteX-ray transmission film is resin, and it is damaged from an X-ray.Replace the film regularly, once a week for continuous operation.

4 MAINTENANCE

37

If the chamber is not evacuated, perform the operations described in “ 4.4 Checking vacuumcondition of sample chamber ” (page 37) .

4.3 Checking X-ray generatorCheck the time shown by the hour meter located on the front of the analysis unit (refer to “Hour meter ” (page 7)). The lifetime of the X-ray generator depends on the conditions. Prepare for the replacement ofthe X-ray generator when the elapsed operating time is either (shorter) one of approximately2000 hours or 1 year. And contact the nearest HORIBA sales representatives beforeperforming the replacement.

4.4 Checking vacuum condition of sample chamberIf the vacuum pump oil level is too low, the degree of vacuum cannot increase. If the vacuumpump oil level is too high, oil may be expelled from the exhaust tube. Check the oil level inorder to maintain an appropriate degree of vacuum.

Fig. 8 Checking vacuum pump oil

There is an oil level gauge on the front of the vacuum pump.Check to make sure that the oil level can be seen inside the red circle.When the oil level is below the red circle, remove the oil mist trap and supply pump oil.Before checking the oil level, make sure the pump is stopped and the pump suction mouth isin atmospheric pressure.

NoteThe vacuum pump oil is an expendable item. Replace the oil every 1 year.For how to replace it, refer to the instruction manual for the vacuum pump.

4 MAINTENANCE

38

4.5 Applying grease to the XY stageThe XY Stage needs regular greasing. (Recommended interval: Once a year)

NoteWhen applying grease to the XY stage, contact us.

4 MAINTENANCE

39

4.6 Replacing the X-ray indicator (X-RAYS ON) lampWhen the X-RAYS ON lamp (see page 4) is blown-out, replace it using the lamp replacementkit (P/N: 9038002700). The life of the lamp is approximately 10,000 hours.

1. Hold the concave portion of the lamp lens and pull it to remove the lens.

2. Insert the attached standard lamp set (screwdriver) into the square-hole portion ontop of the lamp holder and pull the lamp holder to remove it.Pull the lamp downward from the holder to remove it.

3. Pull out the lamp from the lamp holder.

4. Insert a new lamp into the holder and mount the lamp holder to the main body.When mounting the lamp holder, align the direction of metal bracket in the main body withthat of square-hole portion of the lamp holder, press the root of the lamp holder (aroundthe lamp) downward using the screwdriver, and lock the square-hole portion to the lug ofthe metal bracket.

5. Push the lens of the lamp into the main body.When mounting the lens, push it in while aligning the concaved portion of lens rear sidewith the position of lug of the main body.

NoteBe sure to turn off the power switch on the front before replacing the lamp.

4 MAINTENANCE

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4.7 Cleaning the fan filtersDetach the filters from the top and back of the XGT to clean them by removing the dirt using avacuum cleaner every six months or so. Wash them with water once a year or so. (After thewash, be sure to dry them before reinstalling them.)

NoteThe cleaning intervals for the filters depend on the service conditions. The guidelines above assumethat the degree of dirt is similar to the one for office furniture.

Filter on top

Filter at rear

4 MAINTENANCE

41

4.8 Analysis probe windowThe analysis probe window is used for measurements in which only the analysis probe isvacuumed.When analyzing a sample in the air, install the analysis probe window, and then vacuum onlythe analysis probe for analysis. When analyzing a sample in a vacuum, remove the analysisprobe window, and then vacuum the entire sample chamber for analysis.

4.8.1 Installation procedure for analysis probe windowOperating procedure1. Place the X-ray transmission film on the X-ray transmission film holder, and screw

the locking rings with O-rings to assemble the analysis probe window.Use this procedure also when replacing the X-ray transmission film.

Fig. 9 Assembling the analysis probe window

NoteUse an X-ray transmission film (diameter: 64 mm - part No. 9068001000). No cell window(diameter: 80 mm; part No. 9038000200) is applicable. The X-ray transmission film holder has 6 screw holes, two times the number of screws used tofasten the X-ray transmission film securing ring. This allows the X-ray transmission filmsecuring ring to be alternatively fastened in the completely opposite orientation. Whichever 3screw holes may be used to fasten the ring.

4 MAINTENANCE

42

2. Insert the analysis probe window into the analysis probe with the window orientedto fit the installation jaws of the probe.

Fig. 10 Analysis probe window

3. Turn the analysis probe window approximately 45 degrees until it hits the end.

4. After turning the vacuum leak switch to the VAC side, turn ON the vacuum pump,and then check that the vacuum indicator is lit in green.

Analysis probewindow installationjaw

Top in the sample chamber

X-ray transmissionfilm holder

NoteIf the vacuum indicator is not illuminated in green, remove the X-ray transmission film holder andreassemble it. If the O-ring is found to have any flaw, replace it with the spare O-ring.If the above action does not solve the problem, contact the nearest HORIBA sales representative.

4 MAINTENANCE

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4.8.2 How to remove the analysis probe windowOperating procedure1. Turn OFF the vacuum pump, turn the vacuum leak switch to the AIR side, and then

turn OFF the XGT after one minute or so.2. Hold the analysis probe window, and turn it approximately 45 degrees until it hits

the end.

3. Pull the analysis probe window downward to remove it.

4. Flip over the probe window, loosen the screws (3 pieces) on the film securing ring,and then remove the ring.

5. Remove the X-ray transmission film and clean the holder.It is not necessary to apply grease to the O-ring.

6. Turn the vacuum leak switch to the VAC side.

NoteThe XGT cannot be vacuumed with the vacuum leak switch set to the AIR side.Be sure to return the switch to the VAC side after removing the window.

5 TROUBLESHOOTING

44

5 TROUBLESHOOTING

5.1 Alarm

Alarm Countermeasures

The ERR alarm is lit.

When the equipment has failed to reach a vacuum by the set time with the ERR lamp lit, troubleshoot it referring to “Vacuum is not achieved.” in “ 5.4 Other trou-bles ” (page 47).When the ERR lamp is lit due to a problem not related to the vacuum condition, press the X-ray ON lamp (X-RAYS ON) switch. If the X-ray indicator lamp does not light, the lamp is out. Replace the lamp.

If you can perform the measurement normally, there is no problem.Press the reset button and wait for one minute. If the alarm lights up again soon, there may be a mechanical problem. Contact the nearest HORIBA sales representatives.

The hardware error of "Detector not cooled"occurs when measurement starts.

This alarm is output if the detector is not cooled enough when the power is turned ON.The cooling condition of the detector can be checked by the liquid nitrogen (LN) check lamp of the analysis unit. If the lamp is green, the detector is cooled enough. If the lamp is red or orange, the detector is not yet cooled.To avoid this alarm, turn on the power after the detector is cooled enough.If the lamp is red or orange when the power is turned ON, replenish liquid nitrogen carefully by following the procedures in " 1.5 Filling Dewar with Liquid Nitrogen " on page 9. When the lamp turns green, turn OFF the power of the analyzer and wait for 10 seconds. Then turn ON the power.

Reference“ 4.6 Replacing the X-ray indicator (X-RAYS ON) lamp ” (page 39)

5 TROUBLESHOOTING

45

5.2 Power supply troubles

Symptom Inspection part Inspection details Action

No power

Power supply cable

Confirm that respective cables for the XGT-7000V analysis unit, personal computer, data processor, LCD, printer, and vacuum pump are correctly connected.

Connect the cables correctly.。

Confirm that power is supplied. Supply power.

Power supply switch

Confirm that respective switches for the data processor, personal computer, LCD, printer, and vacuum pump are turned ON.

Turn ON the power supply switches.

Emergency stop switch

Be sure to check that the emergency stop switch is not left depressed.

When the emergency stop switch is left depressed, turn OFF the power using the key switch, release the emergency stop state by turning the button, and then turn ON the key switch again.

Be sure to check that the key switch has been turned ON again after releasing the emergency stop state.

No power is supplied just by releasing the emergency stop state. You must turn OFF and ON the key switch after that.

When no abnormality is found in the above inspection parts, the fuse may be blown out. Contact the nearest HORIBA representatives.

Vacuum pump does not operate

Data processor power supply

Confirm that the power supply cable of the data processor is correctly connected.

Connect the power supply cable correctly.

Confirm that power is supplied. Supply power.

Confirm that the breaker of the data processor is ON.

Turn the breaker ON.If the breaker is thrown soon again, stop the use and contact the nearest HORIBA representatives.

Power switch on main body of pump

Confirm that power supply of the main body of the pump is turned ON. Turn ON the power supply switch.

5 TROUBLESHOOTING

46

5.3 Operation troubles

Symptom Action

The detailed image cross cursor does not match up with the sample measurement position.

Set the X-ray applied position.

An unidentifiable peak appears in the vicinity of 18.9 keV and 21.5 keV in the spectrum.

This is not an error. It is a Compton diffusion peak caused by the Rh-K rays of the X-ray tube target.

A peak appears in the area of 1 keV or below in the spectrum.

This is the effect of external noise or vibration. Remove the source of noise or vibration or relocate the analyzer.

Auto current cannot be adjusted. X-ray intensity is too low. Adjust the current manually.

5 TROUBLESHOOTING

47

5.4 Other troubles

Symptom Inspection part Inspection details Action

Measurement result is different from expected.

Measurement pointConfirm that the measurement point meets the X-ray irradiation point correctly.

Adjust the X-ray irradiation to the measurement point using the optical image window.

Vacuum is not achieved.

Piping in the vacuum system

Confirm that the vacuum hose connection is correct. Connect the piping correctly.

Vacuum pump oil Confirm that there is enough oil. Replace or resupply the oil annually.

X-ray transmitting film Confirm that the X-ray transmitting film is not broken.

If the X-ray transmitting film is broken or any of the problems mentioned above is not found, replace the film (See “ 4.6 Replacing the X-ray indicator (X-RAYS ON) lamp ” (page 39)).

O-ring for the sample chamber door

Check that the O-ring for damage and amount of grease applied.

When the O-ring is damaged, replace it. When the amount of grease is insufficient, apply grease to it.

Ambient temperatureCheck that the ambient temperature is within the guaranteed operating temperature range.

When the ambient temperature is below the guaranteed operating temperature range, the performance of the vacuum pump becomes low, resulting in failure to reach a vacuum within the set time. In such a case, press the ERR button to reset the error, and vacuum the equipment again.

No X-ray is generated. X-Ray ON lamp

Press the X-RAY ON lamp with the sample chamber closed, and then confirm that the lamp lights.

If the lamp does not light up, replace it.

Mapping is interrupted. SYNC cable Check the cable connection. Reconnect the cable.

The software is inoperative. Emergency stop switch Confirm that the emergency stop

switch is not pressed.

Turn OFF the power switch and rotate the red flange of the emergency stop switch to return it to the original state.Then turn ON the power switch. And reboot the PC.

6 APPENDIX

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6 APPENDIX

6.1 Measurement PrinciplesThe XGT-7000V is designed as follows:(a) The X-rays generated in the X-ray tube are converged into a very thin X-ray beam with theX-ray guide tube (XGT).(b) This beam is irradiated to the sample while its surface is being scanned.(c) The X-ray transmitted image of the sample and the distribution images of its elements arethen obtained.The X-ray transmitted image is obtained from the fluorescent X-rays which have transmittedthe sample, using the Si semiconductor detector. The measurement data and the positioninformation obtained when the sample was scanned are used to form an image with the dataprocessor and then display it on the LCD.

Fig. 11 Block diagram of the XGT-7000V

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What Is the X-ray?The X-ray belongs to one of the electromagnetic waves such as visible radiation, but its wavelength is very short. (approximately 10-8 to 10-11 m.)Like other electromagnetic waves, the X-ray has the characteristics of both "waves" and"particles." Therefore, it is expressed using its energy (E) for those of energy particles. Thefollowing equation holds between l and E:E = 124/l (E:keV, l:nm)This means that as the wavelength is shorter, the energy is larger.

What Is the X-ray Fluorescence?When X-rays are irradiated to atoms, the electrons on the orbit of the internal shell areexpelled to the outside and then the orbit becomes vacant. Now the electrons on the orbit ofthe external shell fall on the vacant orbit and the X-rays equivalent to the energy differencebetween both orbits are generated. This is called X-ray fluorescence (see Fig. 12).Since the energy difference between the orbits has a value specific to the atom, the generatedX-rays are called the characteristic X-rays or specific X-rays. On the other hand, the irradiatedX-rays are called the primary X-rays or excitation X-rays.

Fig. 12 Generation of X-rays fluorescence

Generation of X-raysFor the source of the primary X-rays to generate the X-ray fluorescence, an X-ray tube orradioactive isotopes (R1) are generally used. The XGT-7000V uses an X-ray tube.The X-ray tube is a certain type of vacuum tube, consisting of a tungsten filament, a target,and a beryllium window (see Fig. 13).

Fig. 13 Structure of X-ray tube

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When the tube current flows through the filament with voltage applied between the filamentand the target, thermions are generated, accelerated, and then hit against the target. Now X-rays are generated and irradiated through the beryllium window.The characteristics of the generated X-rays greatly vary depending on the substance of thetarget, the applied tube voltage and current. The XGT-7000V uses rhodium (Rh) for the target.

Converging the X-raysThe X-ray guide tube (XGT) has a hollow glass tube, in which all the fluorescent X-rays arereflected on the inner surface. This tube thus ensures that the X-rays are sent withoutsacrificing their intensity. A high-bright micro X-ray beam is irradiated to the sample by cuttingthe exit end of the XGT small, so that even a very small area can be analyzed.

Si DetectorThe characteristic X-rays generated from the sample are detected by the Si detector. Thedetector, which is configured as shown in Fig. 14, outputs current pulses to the outside withthe energy of the incoming X-rays. The current pulses proportional to the energy of the X-raysare converted to voltage by the preamplifier, amplified by the proportional amplifier, and thenenter the multichannel wave height analyzer (MCA). The pulses are classified by the heightand the classified pulses are counted.

Pulse height:Corresponds to the energy of X-raysPulse count:Corresponds to the intensity of X-rays with that energy

Fig. 14 Si detector

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6.2 Specifications

6.2.1 Analyzer

X-ray microbeam generator

DetectorSi detector

Nal detector

Sample stageSample size and mass

Scanning range

Two-dimension resolution 100 µm (100 µm dia. XGT, FWHM when WD=1 mm) and10 µm (10 µm dia. XGT, FWHM when WD= 1 mm)

X-ray generator

X-ray tube (target: Rh)Tube voltage: 15 kV, 30 kV, or 50 kV (changeable)Tube current: 0.002 mA to 1.0 mA (changeable)X-ray tube life guarantee time: 2000 hours or 1 year (shorter one)

Detector High-purity silicon detector, XEROPHY®Detectable elements Na (Z=11) to U (Z=92)Effective area 38.5 mm2

Energy resolution 150 eV or less (Mn, in Processing Time P6)P/B ratio (1 keV) 10000 : 1 or moreCooling method Liquid nitrogenDetection window Be window

X-ray light-sensitive element Na (Tl) crystalSignal amplifier Photomultiplier tubeDetection window Be window

340 mm (W) × 250 mm (D) × 80 mm (H) or 100 mm (W) × 100 mm (D) × 100 mm (H)Max. mass 1 kg or less

Min.: 256 µm × 256 µm to Max.: 100 mm × 100 mmMin. feeding pitch: 2 µm

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Optical microscopeCCD camera

Moving the stage from the whole image/ detailed image to the specified position using amouse cursor is possible.The detailed image is pictured in the same axis as the X-axis.Adjusting the sample height by looking into the CCD camera image is possible.

6.2.2 Data processor

Display

Computer

Qualitative analysis (spectrum measurement)

Quantitative analysis

Whole image Magnifying scale: approx. 2 times (on 17 inches LCD)Indication area: approx. 130 mm × 100 mm

Detailed image Magnifying scale: approx. 100 times (on 17 inches LCD)Indication area: approx. 2 mm × 1.6 mm

Sample height Magnifying scale: approx. 2 times (on 17 inches LCD)Indication area: approx. 130 mm × 100 mm

Size 17-inch LCD

CPU Pentium Ⅳ (3.0 GHz) or upperMemory 1 GB or moreHard disk 40 GB or moreOS Windows®XP

Energy range 40 keV (10 eV/channel)Vertical axis scale Possible to switch between linear scale or Log scaleKLM marker Characteristic X-ray peakPeak label Element symbols are displayed on spectrum.Automatic qualitative analysis Peak search and element identification

Matching The hard disk is searched for a spectrum with a composition similar to that of the sample.

Multi-point AnalysisSpecify multiple measurement points on the mapping image of which was measured by using the whole image, or detailed image, and automatically performs subsequent measurement.

Saving and call-up of spectrum data Spectrum data is saved on and called up from the hard disk.

FPM Quantitative Analysis Standard less, 1-point calibration

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Mapping analysis

Color printer

6.2.3 Ambient conditions

6.2.4 Power source

6.2.5 Mass

6.2.6 Dimensions

Can specify the mapping position by optical image (whole image/ detailed image)Can move the stage to the specified position by using the image cursor on each image

Mapping range 100 mm × 100 mm stage256 µm × 256 µm to 100 mm × 100 mm

Image display Scale marker, image cursor, contrast adjustmentImage processing Pseudo-color, RGB, image line analysisImage saving and calling up Save or call up each mapping image to a disc.Smart Map Add/delete the element after mapping.

Included as standard item

TemperatureOperating temperature 5 to 40

Performance guarantee temperature 10 to 35

HumidityTemperature range between 5°C and 31°C Max. relative humidity 80%

Temperature range between 31°C and 40°C Linearly decreases until relative humidity reaches 50%

Voltage 100 V, 120 V, 220 V, or 240 V AC ±10%Frequency 50 Hz /60 Hz ±1.0%

Power consumption Below 1.5 kVA (60 Hz), Below 1.8 kVA (50 Hz)(Including vacuum pump, but excluding PC, LCD, and printer)

Plug Two independent 3-pin sockets (with grounding)A set of main unit + vacuum pump and PC with accessories

Grounding Grounding resistance of 100Ω or less (equivalent to Class 3 grounding)

Analyzer unit Approx. 200 kgData processor Approx. 30 kgXGT controller Approx. 1.5 kgVacuum pump Approx. 30 kg

Main unit 700 (W) × 900 (D) × 800 (H) mmData processor 240 (W) × 560 (D) × 510 (H) mm

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6.3 WiringThe cable wirings between units are connected as shown in the wiring diagram “ Fig. 15Wiring (XGT-7000V) ” (page 55).For installation and removal of the wirings and pipings, contact the nearest HORIBA salesrepresentatives.

Wiring between data processor and SI detector

Wiring procedure is as follows. For removing the wiring, take the reverse procedure.1. Grounding2. Connecting the PSI connector

Be sure to screw the PSI connector tightly.3. Connecting the HV connector

The HV connector is a BNC-type connector. Be sure to lock it by turning its plug to theright when wiring.

The detector cable and the Si detector connector (PSI, HV) are connected inside the analyzer.Normally you do not need to remove the wirings. In times of removal, take the reverseprocedure of the above procedure (3. to 1.).

NoteMake sure to turn OFF the power switch before wiring.Connect the detector cable to the connector (PSI, HV) of the rear panel for XGT-7000V dataprocessor and to the connector (PSI, HV) of the detector. Be sure to ground them.

NoteIf a high voltage is applied when the PSI connector is unconnected, this will cause breakage of thedetector. Do not mistake the order of connection.

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Fig. 15 Wiring (XGT-7000V)

7 ACCESSORIES

56

7 ACCESSORIESProduct No. Name Specifications Application Appearance Min. Qty.

9068000400 Sample mounting tray P

For use with 100 mm sample stage Used for normal samples 1 pc.

9068000800 Sample mounting tray L

For use with 100 mm sample stage

Used for thick samples or samples with low transmitted image contrast

1 pc.

9068001000X-rays transmission film

Exclusive film 64 mm dia.100 sheets per box

Analysis probe window 1 box

F0020861200 Silicone grease SH11150 g tube For application on seals 1 tube

9068000900 Pump oilOil for vacuum pump 500 mL per bottle

Used to replenish vacuum pump oil 1 bottle

9068001700 PC support Clear resin X-rays transmission film support 1 pc.

9038002700 Lamp replacement set

Lamp: 4 pcs. Replacement tool: 1 pc.

X-RAYS ON lamp 1 set

2 Miyanohigashi, Kisshoin Minami-ku, Kyoto 601-8510 Japanhttp://www.horiba.com

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