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5350 NE Dawson Creek Drive Hillsboro, Oregon 97124-5793

Tools for Nanotech™

Platinum Deposition Technical Note

PN 4035 272 21851-D

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Principal ContributorsClive Chandler

Michael Megorden

Technical Publications TeamJudy Lane Green

Susan “Dash” Gilpin

email: [email protected]

Copyright © 2007 by FEI Company

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C O N F I D E N T I A L — F E I L i m i t e d R i g h t s D a t a

Contents

Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1Gas Injection System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1Platinum Deposition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

Fast Scanning and Layer Growth . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2Beam Current and Pattern Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

Determining Resistance for Pt Deposition . . . . . . . . . . . . . . . . . . . . . . . 3Standard Formula . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3Applying the Formula . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4Working with a Required Resistance . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

Electron Beam Deposition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5Electron Beam Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6Stage Tilt . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7Suggested Procedure (with xP Software) . . . . . . . . . . . . . . . . . . . . . . . . 8

Operating Conditions for Ion Beam Deposition . . . . . . . . . . . . . . . . . 10Material Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10Smarter Material Files, Sidewinder Columns . . . . . . . . . . . . . . . . . . . 10Beam Current . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13Coatings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13Device Edit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

GIS Maintenance Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14Safety Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

GIS Refill Procedures. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

Removing the GIS. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16Required Equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16Handling the GIS Injector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16Turning off the Compressed Air Source . . . . . . . . . . . . . . . . . . . . . . . 16Removing the Injector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

Removing the Chemical Crucible . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21Preparing for Crucible Removal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21Removing the Needle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22Removing the Empty Crucible . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22Unpacking the New Crucible . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

Replacing the Chemical Crucible . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25Installing the Crucible . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

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C O N F I D E N T I A L — F E I L i m i t e d R i g h t s D a t a

Reinstalling the Gas Injector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27GIS Installation Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27Reconnecting the Compressed Air Source . . . . . . . . . . . . . . . . . . . . . . 28Pumping Down the GIS Injector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

Aligning and Adjusting the Needle . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30Coarse Alignment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31Fine Alignment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

Adjusting the GIS Speed. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

Resetting the GIS Lifetime Counter . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

Setting the Crucible Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35Crucible Default Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35Setting the Omega Controller Setpoint . . . . . . . . . . . . . . . . . . . . . . . . . 35Changing the Newport Controller Setpoint . . . . . . . . . . . . . . . . . . . . 36

GIS Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

Platinum (Methylcyclopentadienyl [Trimethyl] Platinum) MSDS . 39

Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

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FEI Limited Rights Data C O N F I D E N T I A L

Platinum Deposition

OverviewGas Injection SystemThe Gas Injection System (GIS) beam chemistry installed on your FEI® system is used in conjunction with the selected beam for milling, depositing, or etching a drawn or associated pattern into the sample surface. See your system user’s guide for additional information.

Platinum DepositionIon beam deposition is a delicate balance between decomposing adsorbed gas to produce a conductive layer and sputtering material from the sample surface. Too much sputtering can change deposition to etching.

Many parameters affect deposition results. The deposition rate, which determines results, is a combination of the local gas flux and:

Beam currentScan area (pattern size)Scan speed (dwell time per pixel and beam overlap)

In turn, local gas flux on the sample is determined for a particular deposition material by:

Needle position relative to the sample (both separation and offset from the center line)Needle diameter Crucible temperature

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Platinum Deposition Fast Scanning and Layer Growth

FEI Limited Rights DataC O N F I D E N T I A L

Fast Scanning and Layer GrowthIn ion beam deposition, fast scanning produces fast layer growth over a wide range of ion beam currents and scan areas.

As the beam scans a pattern, it steps from point to point. With fast scanning, the dwell time at any particular point is short. At each point, the ion beam converts any gas on the surface to a deposited product, then sputters material away until it moves to the next point. The longer the ion beam remains at the point, the less net deposition there is. The net deposition rate is the deposition rate minus the sputtering rate. See Deposition Efficiency for Platinum below.

Figure 1 Deposition Efficiency for Platinum

A B C

Rateµm/min(thickness/time)

High-efficiency deposition per ion. Ion dose on each pass does not decompose all gas.

Slow layer growth rate & long deposition time.

Most efficient growth rate. Each beam scan uses up nearly all gas.

All gas is used up by only part of ion dose at each point. Remaining ions then sputter surface.

Lower beam current;larger patterns

2–6 pA/µm2

medium patternsHigher beam current;smaller patterns

Deposition stops and milling begins

Current Density (pA/µm2)

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Platinum Deposition Determining Resistance for Pt Deposition


Beam Current and Pattern AreaThe deposition rate also depends on the scan area and scan speed (dwell time and overlap—not imaging scan rate), so be careful when setting up a series of experiments to measure deposition rate as a function of beam current and pattern area.

At low beam current with large pattern areas, deposition efficiency (deposited atoms per incident ion) is high, but thickness growth rate of the deposited layer (measured in µm/min) is low. See area A in Figure 1.

At intermediate values, maximum growth rate occurs (see area B in Figure 1), but the exact conditions vary with current and other scan parameters. It is recommended that beam current into the pattern area be in the range of 2–6 pA/µm2, which results in about 1 µm thickness in 60 seconds. See area B in Figure 1.

With high ion beam current and small pattern areas, the deposition efficiency falls until net milling, rather than deposition, occurs. See area C in Figure 1.

Determining Resistance for Pt DepositionUse the formula below to determine the size of the platinum strip that best meets the needed resistance.

Standard FormulaStandard thickness (height) is 1 µm for each platinum track. You can vary the track height; however, height variations affect resistivity (ρ), which is based on 10–20 ohms per square for 1 µm thick.

Figure 2 Finding Resistance for Platinum

NO

TE The formula presented

here applies to platinum deposited with the ion beam.

W

H

1 µm

7 µm

1 µm

L R = L W

x p

where, R = resistancep = 10–20Ω x µm

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Platinum Deposition Determining Resistance for Pt Deposition


Applying the FormulaIn Figure 2, the black lines represent 1 µm measurements (or squares) of the track. Using the formula with these known dimensions results in the following:

R = 7 µm/1 µm2 . 10−20 Ω . µm

R = 70–140 Ω

Working with a Required ResistanceWhen you want to achieve a desired resistance with deposition between two vias, use the following formula:

where:

R = resistance

ρ = 10−20 Ω ⋅ µm

W LRH--------- ρ×=

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Platinum Deposition Electron Beam Deposition


Electron Beam DepositionThe electron beam can be used to deposit a thin protective coating of carbon-rich platinum that grows relatively slowly and conforms to high-aspect ratio structures as it is deposited. Electron beam deposition of platinum is useful for samples that are sensitive to the ion beam or where excellent step coverage is needed over high-aspect ratio structures, such as photoresist exposure matrices.

Electron beam-deposited platinum is carbon-rich due to incomplete fractionation of the metal-organic precursor gas (compared to ion beam-deposited platinum, which has a lower ratio of carbon to platinum). The higher carbon content can improve differential contrast for TEM sample preparation. It also increases the resistivity, however, which may be a disadvantage in circuit edit applications.

NO

TE

If your machine is running automated processes for metrology or DA, do not make any changes to your tool or process without clearance from your FEI product manager.

High-aspect-ratio Si structures coated with electron beam-deposited platinum prior to cross-sectioning and imaging.

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Electron Beam ParametersThe deposition rate of electron beam-deposited platinum varies with the energy and current of the electron beam (and the secondary-emission efficiency of the material being coated). In general, a rate of 0.1 µm/minute is achievable for the ~10 µm2 usually coated for TEM samples. In this case, one minute is usually more than sufficient to protect the surface from subsequent ion beam deposition at 30 kV, because the penetration of the 30 kV ion beam into the electron beam platinum is < 0.05 µm.

For a total deposition thickness of > 0.1 µm, it may be efficient to deposit in two stages—first with the electron beam, then with the ion beam.

In setting electron beam parameters, choose conditions that maximize the number of secondary electrons at the surface—i.e., low energy and high current. A beam energy of < 5 kV and a spot size > 3 is generally appropriate. Optimize gun tilt to maximize current. Use SHR mode; in UHR mode, beam distortion from the presence of the GIS needle may compromise results.

The following general conditions are recommended for electron beam deposition. However, you can vary system parameters to optimize deposition for your material/process or to protect electron beam-sensitive substrates.

Table 1 Electron Beam Parameters for Platinum Deposition (1 of 2)

Parameter RangeRecommended Value Notes

Beam energy 2–5 kV 2 kV The deposition rate generally increases as kV is lowered, as long as the current does not decrease appreciably. Within the 2–5 kV range, it may be convenient to use higher beam currents for process considerations. For example, FEI automated metrology processes have used 5 kV (with spot 5, 30 µm electron beam aperture, and SRH mode).

Spot size 4–5 5 The purpose is to maximize current, which increases with spot size. Spot 5 is a good compromise between maximizing current and keeping a reasonable physical spot size.

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Stage TiltYou can set the stage tilt to 0° or 52° when depositing platinum with the electron beam. If you are only depositing a flat pad, working at 52° may be more efficient on a DualBeam™ system; you can then easily follow electron beam deposition with ion beam deposition because the sample will already be normal to the ion beam.

If you want to evenly cover small features of high aspect ratio, you may achieve better results with the sample at 0°, which is normal to the electron beam.

If you use 0° stage tilt, exercise caution to avoid needle-sample collision. The GIS needle may hit the sample at eucentric height, since it is typically not aligned for operation at 0°. This risk is system-dependent, however, and may not occur on your tool. If you have not tried deposition at 0° before, lower the sample ~500 µm below eucentric height before inserting the needle, then slowly raise the sample to eucentric height. While raising the stage, watch for sudden contrast change, slight movement of the needle, or stage current fluctuation, all of which indicate contact between the sample and the needle.

Note that pattern placement is not aligned to the electron beam, so qualify the offset with your unique machine conditions or coat a larger area to make sure the area of interest is covered.

Aperture 30–50 µm N/A A larger aperture (e.g., 50 µm) yields more current and therefore faster deposition and is recommended with lower kV beam currents. However, if process considerations make it more convenient to use the same conditions as imaging, a slightly higher kV (e.g., 5 kV) with a 30 µm aperture is a good compromise.

Table 1 Electron Beam Parameters for Platinum Deposition (2 of 2)

Parameter RangeRecommended Value Notes

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Suggested Procedure (with xP Software)1. Find eucentric height near the area of interest with the

electron beam, per normal DualBeam procedure.

2. Choose appropriate electron beam parameters—e.g. 2 kV, spot 5, 50 µm aperture, SRH mode, as suggested above.

3. Choose the stage tilt desired for electron beam deposition. If you are depositing at 0° instead of 52°, use caution and lower the sample before inserting the needle, as described above.

4. Insert the GIS needle. Verify that the feature of interest is still in the field of view and is not blocked by the needle.

5. Select Serial as the Pattern Order on the xP Work page.

6. With the electron beam chosen as the primary beam, draw the pattern for deposition (normally a solid box pattern).

7. Draw an additional pattern where the electron beam can stop when deposition is finished. This additional box is suggested because the electron beam does not have a high-speed mechanical blanker, and the subsecond pause while the software recognizes the end of deposition and blanks the beam can leave a small spire of platinum. Make this additional box small and place it where it won’t interfere with subsequent work. Choose a deposition time of < 1 second. This box must be the last pattern in the series.

8. For versions of xP prior to xP 3.0, select an ion beam current of 1 or 10 pA. Even though you are not using the ion beam, the beam diameter associated with the selected aperture affects the spacing of points in the pattern.

9. Select pt_low.mtr as the material file (or another file with 0% overlap).

If the time does not update in either of the last two steps (indicating the pattern has not updated), make sure you are in Serial patterning mode.

10. Select Use: E-BEAM in the Patterning group of the Work page.

11. Manually type the pattern time (usually 60 or 120 seconds). The material file selection will change to “None,” but the parameters set by pt_low.mtr do not change.

NO

TE

Avoid 1E frame grabs during electron beam deposition; these will leave a small spire at a random location. Use continuous scans instead.

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12. Begin patterning. If the START/STOP PATTERN toolbar button is grayed out, make sure the electron beam is chosen as the primary beam.

The pattern will not appear on the real-time monitor, which displays only the position and approximate intensity of the ion beam. The sound of the platinum GIS valve opening signals the beginning of deposition.

It can be difficult to view the deposition with the electron beam normal to the sample (the pattern can appear as a shadow), but if you tilt the stage (after retracting the GIS needle), the deposition is easier to see.

13. After deposition, retract the GIS. If you are going to do ion beam deposition next, remember to select Use: I-BEAM on the Work page and select an appropriate material file.

Note that GIS needles are normally aligned to maximize ion beam deposition, so the gas flux may not be optimum for electron beam deposition. It may be possible to increase the deposition rate with modified GIS alignment, as long as ion beam deposition is not adversely affected.

Use a straight needle for electron beam deposition, not a “stovepipe,” or coaxial needle.

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Platinum Deposition Operating Conditions for Ion Beam Deposition


Operating Conditions for Ion Beam DepositionMaterial FilesThe following operating conditions apply to ion beam deposition of platinum. For further information on electron beam deposition, see “Electron Beam Parameters” on page 6.

Several material files are available for use with platinum deposition, depending on the application.

Smarter Material Files, Sidewinder ColumnsSystems with sidewinder ion columns should be using FEI xP software version 3.0 or better and have the Smarter Material Files installed. These files include dwell time, overlap (OL), and minimum loop time and allow the GIS to function according to specifications.

Custom files will need to be reformatted to the new Smarter Material File format.

Table 2 Material Files Available with Platinum

File Name ApplicationOverlap

(%)Dwell (µs)1

1. Material files express dwell time in dwell units. One dwell unit equals 0.1 microseconds.

Deposition Rate (µm3/nC)

pt_mag.mtr Standard Pt deposition for circuit edit applications where resistivity is important. Used for acceptance test.

–50 0.2 0.5

pt_low.mtr Pt deposition with low current (< 1 nA)

0 0.2 0.5

pt_high_mag.mtr Used for fast deposition over large areas with a high beam current (≥ 1 nA)

–150 0.2 0.5

pt_tem.mtr Used with AutoTEM™ Wizard

–200 0.2 0.5

pt_via.mtr Used to fill vias with Pt 0 0.2 1

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To reformat custom files:

1. Open one of the existing smarter material files and save a copy as your new custom file by using File > Save as.

2. Open the new custom smarter material file and fill in your old material file parameters, taking note of the following changes:

OL is now split into OL_FS and OL_SS. See Figure 3, “Pixel Spacing Using OL_FS and OL_SS,” on page 11. Copy your old Overlap value into both places.

OL_FS stands for Overlap_Fast Scan, which is the pixel spacing for the pixels making up the long lines the beam will scan in a raster pattern.

OL_SS stands for Overlap_Slow Scan, which is the spacing between the lines when the raster scan changes direction.

Leave Beam_Tuning: YES turned on for all deposition files. Material selectivity will also be enhanced by leaving this feature turned on.Copy your dwell time in to the dwell value spot.Set the Min_looptime_mSec: x to Min_looptime_mSec: 1.Recalculate the Sputter Rate (Sr) value for the new material file. The units for sputter rate are µm3/nC. The calculation requires that the amount of material removed or added is calculated in µm3 and this is divided by the beam current used (expressed in nA) multiplied by the pattern time in seconds.

Figure 3 Pixel Spacing Using OL_FS and OL_SS

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Beam CurrentChoosing the proper beam current and material file for your platinum deposition depends on the area to be deposited. Use the following procedure to determine the proper beam current.

1. Find the area of deposition. For example, if the strap is to be 1 µm wide by 20 µm long, the area is 20 µm2.

2. Calculate the suggested beam current based on this formula:

where 20 µm2 is the calculated area in the example given

In the first part, calculate for both 2 and 6 pA/µm2 to give you the correct range. In this example, the results are 40 and 120 pA.

3. Select the beam current that is between your highest and lowest calculation.

With 40 pA and 120 pA calculation results, select an ion beam current of 100 pA.

2pAµm2----------- 20µm2× 40pA=

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Platinum Deposition Applications


ApplicationsThis section describes the coating and filling applications for ion beam deposition.

CoatingsCoating large areas with platinum is best accomplished at a high current density. This is contrary to the deposition parameters that are used for the platinum and insulator deposition because these materials would be sputtered away by the high current density. Figure 1, “Deposition Efficiency for Platinum,” on page 2 shows the dependency of the deposition rate and the current density of the patterns. The current density shown is 10 times greater than for the similar figure for platinum, but the net result is still a deposition of platinum.

Device EditThe requirements for device edit differ greatly from those for coating large areas. For this application, the best results are obtained using a conventional needle instead of the coaxial needle because the conventional needle provides the best gas flow to obtain a low-resistivity metal film. This is critical for device edit applications and also allows a deposit with the least amount of overspray of the material, minimizing cleanup after deposition.

To minimize the possibility of electrostatic discharge damaging the circuit, use the lowest possible beam current while still maintaining a reasonable deposition time. A current density of 10 pA/µm2 is reasonable for depositing platinum for device edit.

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Platinum Deposition GIS Maintenance Overview


GIS Maintenance OverviewGIS customer maintenance procedures can include any or all of the following procedures:

Crucible refill or exchangeNeedle replacementNeedle alignmentChecking and adjusting the needle insert/retract speedResetting the GIS lifetime (Supervisor login required)Setting crucible temperatures

Only personnel who have received FEI Customer Maintenance Training should perform maintenance procedures on the GIS units. Unauthorized personnel performing these procedures may void the warranty. For information on customer training, call FEI Customer Service at 1-503-726-2800 or 1-866-MYFEICO (693-3426).

Safety PrecautionsGas injection systems contain potentially corrosive byproducts. Spilled crucible materials can be hazardous. Read the Material Safety Data Sheets for the appropriate chemical.

Wear chemically resistant gloves and eye protection at all times during the crucible exchange.

Leave the needle pointing down at all times to avoid spilling crucible materials.

Do not attempt any GIS maintenance procedures without chemical safety training. Know in advance how to respond to a chemical spill. Handle all chemicals in accordance with local, state, and federal regulations.

WA

RN

ING

!

Always use an exhausted enclosure (such as a laboratory fume hood) when refilling or exchanging a GIS chemical crucible. Perform these procedures with the sash in the lowered position.

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Platinum Deposition GIS Refill Procedures


GIS Refill ProceduresIf you find that your deposition or etching rates are poor, the change in pressure after the GIS valve is opened is small, or you are nearing the lifetime allotted for the chemistry, it is time to refill the GIS.

The average lifetime observed for platinum is 120 hours.

The refill procedure for the platinum GIS consists of the following steps:

“Removing the GIS” on page 16“Removing the Chemical Crucible” on page 21“Replacing the Chemical Crucible” on page 25“Reinstalling the Gas Injector” on page 27“Aligning and Adjusting the Needle” on page 30“Adjusting the GIS Speed” on page 34“Resetting the GIS Lifetime Counter” on page 35“Setting the Crucible Temperature” on page 35

NO

TE

Refill procedures vary by gas chemistry. Consult the technical note for your specific gas chemistry before attempting to refill or replace the GIS.

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Platinum Deposition Removing the GIS


Removing the GISFor 8XX and 12XX DualBeam™ systems, contact an FEI-trained service engineer for servicing the GIS. For all other systems, follow the steps below.

Required EquipmentGIS workstand, PN 17002Laboratory fume hoodPowder-free, chemically resistant gloves—e.g., latex or nitrileDisposable wipesChemically resistant apronEye protection3/32" hex Allen ball driver5/32" hex Allen ball driverAdditional site-specific personal protective equipment (PPE)Fine needle-nose tweezersMask (optional)

Handling the GIS InjectorAlways hold the GIS injector with the needle pointed down. Do not invert the GIS injector.

Do not drop the GIS unit. Dropping the GIS unit may cause a chemical spill and damage the unit.

Turning off the Compressed Air SourceBefore removing the GIS injector, you must turn off the compressed air source to the system or detach the quick-disconnect fitting at the GIS bank. If the quick-disconnect fitting is not available, proceed to step 3.

1. Turn off the heat to the GIS crucible. Wait until the heat status light is blue, indicating the GIS unit is cool.

2. Vent the system.

3. Locate the compressed air source to the system. This is usually a valve located on the wall behind the instrument, controlling house pressure or a similar facility.

4. Note the setting for the pressure regulator (60–80 psi).

CA

UT

ION

Only personnel who have received FEI Customer Maintenance Training should perform maintenance procedures on the GIS units. Unauthorized personnel performing these procedures may void the warranty. For information on customer training, call FEI Customer Service at 1-503-726-2800.

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5. Close the main valve or pressure regulator to stop the flow of high pressure air to the system. An error message “Compressed air low pressure” may display on the system monitor. Ignore it for now.

Removing the Injector1. Wearing your chemical safety gear (gloves, goggles, apron),

remove each of the three air lines from the GIS injector at the quick-release connectors. (Push the plastic collar into the body of the connector, then pull out the air line.) See Figure 4.

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2. Unplug the control cable from the GIS injector by turning the screws on the cable counterclockwise, then pulling the cable connector off the GIS injector connector.

Figure 4 GIS Adjustment Features

Air line

Thumbscrew

Lockingring

Control cable(to GIS controller)

Valve-open air line (green)

Locking screw(inside)

Knurled valve adjustment knob

Insert speed thumbscrew

Insert air line (red)

Retract air line (black)

Retract speed thumbscrew

Locking setscrew on GIS collar

Flange clamps (2)

GIS flange

Alignment setscrews (4)(present only on early models)

Adjusting setscrews (4)

Clamp screws (4)


Red Viton O-ring

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3. Two flange clamps secure the GIS injector to the chamber. Remove the two clamp screws securing each clamp to the chamber. Carefully pull out the GIS injector from the chamber, taking care not to bump other components.

Clamp screws

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4. Set the GIS injector needle-end down onto the GIS workstand and transport it to the chemical hood. See Figure 5.

Figure 5 GIS Injector and Workstand

CA

UT

ION

Leave the needle pointing down at all times. Do not touch the portion of the GIS injector that extends into the chamber without wearing gloves.

GIS injector mounts in center of workstand

Spare slot to store removed crucible or rubber plug

Workstand

Black shipping seal (from refill kit) to cover crucible while out of shipping container and waiting for installation (remove before installing crucible)

Spare slot for replacement crucible storage (ready for installation)

Rubber plug

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Platinum Deposition Removing the Chemical Crucible


5. If the GIS will not be reinstalled within 30 minutes:

Install the port cover over the GIS flange in the chamberReconnect the quick-disconnect fittings or turn on the compressed airClick PUMP on the Startup page to evacuate the chamber.

Removing the Chemical CrucibleRemove the chemical crucible whenever you refill or replace a crucible.

Preparing for Crucible RemovalPrepare for crucible removal by venting the crucible and removing the GIS needle.

1. Loosen the locking screw in the knurled valve adjustment knob (located on top of the GIS injector). See Figure 6.

2. Tighten the knurled knob on top of the GIS injector (by turning it clockwise) until the valve plunger is lifted off the O-ring seat. While turning the knob, resistance indicates that the valve is opening (against a spring tension). Continue until you feel even more resistance (tight) to indicate the valve is fully open.

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Removing the Needle1. Twist the needle counterclockwise to remove it from the end

of the crucible.

2. Set the needle aside in a clean place for later reinstallation on the new crucible.

Removing the Empty Crucible1. Slightly loosen the four 2-56 socket head capscrews securing

the crucible to the GIS injector.

2. Remove three of the four capscrews.

3. Grasp the crucible and remove the remaining screw to release the crucible from the unit; remove the crucible.

4. Place the crucible in one of the two holes in the top plate of the workstand (see Figure 5, “GIS Injector and Workstand,” on page 20).

Figure 6 GIS Injector Installation Diagram

To Open the valve:Loosen the locking screw. Turn the knurled knob clockwise until you feel resistance, then one turn more.

To Close the valve:Turn the knurled knob counterclockwise until you feel no resistance, then turn clockwise until you barely feel resistance. Tighten the locking screw.

Locking screw (3/32”);use Allen wrench.

Insert position adjustment collar(setscrew not shown)

Crucible

Needle

Crucible-mounting screws


Upper flange screwsMounting flange

WA

RN

ING

!

Do not tip the crucible; any material remaining in the crucible will spill.

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5. Remove and discard the mounting flange O-ring from the top of the old crucible, in compliance with local, state and federal regulations. (See Figure 7, “GIS Crucible—Side View,” on page 24.)

6. Change gloves in order to reduce the risk of contamination. Dispose of the old gloves in compliance with local, state, and federal regulations.

Unpacking the New Crucible1. New chemical crucibles and O-rings are packaged in a class-

100 tri-layer foil bag. Remove this foil bag from the shipping container and place it in a ventilated fume hood.

If the shipping container also contains an aperture and needle, remove them from the container and place them in the fume hood.

2. Carefully cut open the foil bag to avoid damaging the O-ring. Remove the crucible and O-ring.

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3. After installing the new crucible on the GIS, transfer the black shipping seal (Figure 7) from the new crucible to the old crucible.

4. If the new crucible does not come with a needle and aperture, transfer the needle and aperture from the old crucible to the new one.

5. Place the new crucible with the cap side up in a side hole of the GIS workstand.

6. Dispose of empty crucible, residual chemicals, and related parts in compliance with local, state and federal regulations.

You are now ready to install the crucible on the gas injector—see Installing the Crucible below.

Figure 7 GIS Crucible—Side View

Mounting flange O-ring (remove before installing shipping membrane)

Black shipping membrane:Used to cover new crucible out of shipping container. Transfer to empty crucible.Do not install on GIS unit.

Mounting screws (2-56 cap screws)go here

Valve O-ring

Reservoir (beneath spill guard)

Kalrez spill guard. Do not remove.

NO

TE Do not remove the

chemical spill guard from the top of the crucible.

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Platinum Deposition Replacing the Chemical Crucible


Replacing the Chemical Crucible Unpack a new chemical crucible in accordance with the instructions in “Unpacking the New Crucible” on page 23. Let the crucible stand for 5 minutes before installing it to allow the chemical to settle.

Installing the Crucible1. Confirm that the GIS valve is manually opened by tightening

the knurled valve adjustment knob until it will no longer turn when the locking screw is loose (see Figure 8). This retracts the GIS plunger and makes it possible to install the crucible.

2. Carefully remove the crucible shipping cap (chemical is liquid). Inspect the new crucible for contamination before installation.

3. Remove the black shipping membrane and inspect it for excess chemical. Ensure that the Kalrez® spill guard is still in place.

4. Using a lint-free swab or cloth, clean off excess chemical at the top of the crucible before installing the new O-ring.

5. Install the crucible mounting flange O-ring.

Figure 8 Loosen the Locking Screw

NO

TE

Keep the injector upright at all times. The chemical is liquid and can easily spill into the center hole and cause contamination.

Locking screw (3/32”)


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Platinum Deposition Replacing the Chemical Crucible


6. Verify that all three O-rings (shipping seal, plunger, and needle mounting) are installed as shown in Figure 9.

7. Using a lint-free cloth, clean the valve plunger before installing the new crucible to eliminate any residue that may cause contamination.

8. Place the new or refilled crucible over the valve plunger on the GIS injector.

Figure 9 Closeup of Crucible and Needle

Crucible

Needle

Shipping cap

Needle mounting O-ring

Shipping seal (replaced by O-ring during installation)

Kalrez spill guard

Aperture assembly

Plunger O-ring

CA

UT

ION Hold the GIS unit with the

needle pointing down at all times. This avoids a possible clog.

Valve plunger (hidden within crucible when crucible is mounted)

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Platinum Deposition Reinstalling the Gas Injector


9. Holding the crucible against the mating surface on the GIS injector, rotate the crucible so the screw holes are offset from the upper flange screws. Install the crucible mounting screws and tighten.

10. Install the aperture by screwing it into the end of the crucible.

11. Install the needle onto the crucible. Twist the needle clockwise to install it.

12. Once the crucible is installed, manually close the gas injection valve by turning the knurled valve adjustment knob on top of the GIS injector counterclockwise until you meet no resistance, then turn clockwise until you barely feel resistance. This is important in order to prevent gas from flowing out of the needle prior to installation.

Reinstalling the Gas InjectorUse the custom 5/32" Allen wrench (PN 16998) to reach the setscrews on top of the flange. For an illustration of the GIS injector, see Figure 4, “GIS Adjustment Features,” on page 18.

GIS Installation Procedure1. If the chamber is under vacuum, press VENT. When the

chamber is completely vented, remove the port cover from the GIS flange on the chamber. Save the port cover for future use.

2. Loosen the adjusting setscrews on the clamp.

3. Apply a thin film of high vacuum-compatible grease (FEI-recommended Braycote 803 grease) to the red Viton® O-ring. Install the GIS injector by inserting the crucible end through the GIS flange on the chamber.

Figure 10 Crucible Mounting Screws

Crucible

Needle

Crucible mounting screws

Upper flange screws

Mounting flange

See also

Aligning and Adjusting the Needle, 30

CA

UT

ION

Hold the GIS injector with the needle pointing down at all times.

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4. Install the two GIS clamps and screws (taken off during GIS injector removal).

5. Center the GIS injector in the clamps and tighten the clamp screws securely.

6. Tighten the adjusting setscrews until snug. You will later adjust these during needle alignment.

7. Install the air lines to the fittings. Ensure that the bottom fitting is connected to the black line, the middle is connected to the red line, and the top is connected to the green line.

If the GIS needle immediately starts to insert, this is a good indication that the red and black hoses have been switched and must be reconnected properly.

8. Mate the control cable connector to the GIS injector connector and tighten the screws.

Reconnecting the Compressed Air Source1. Open the main compressed air valve or regulator (previously

closed in Step 3 of “Turning off the Compressed Air Source” on page 16.)

2. Confirm it is set to its original pressure (60–80 psi).

3. Clear the “Compressed air low pressure” error message by clicking OK or CLOSE.

Figure 11 GIS Assembly (Upper Portion)

DA

NG

ER

!

Connect the green line only to the pneumatic fitting nearest the rear of the GIS, which is the GIS valve actuator. Connecting the wrong air line to the valve fitting will open the GIS valve in an unsafe situation, as during an open/vented specimen chamber.

CHEMICAL EXPOSURE


Insert air line (red)

Retract air line (black)

Heat control cable Locking screw (3/32”)


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Pumping Down the GIS Injector1. Click PUMP on the Startup page to begin evacuating the

chamber.

2. After the pump has run for approximately 1 minute, turn the knurled valve adjustment knob clockwise as far as it will go. Verify the locking screw is loose. This will manually open the valve of the GIS injector, allowing any excess pressure to be pumped out the crucible.

3. When the chamber pressure reaches approximately 5 x 10-5 mbar, close the valve by turning the knurled valve adjustment knob counterclockwise until it just begins to feel loose. Turn it back ½ turn (clockwise), then tighten the locking screw inside the knurled valve adjustment knob to lock the setting.

4. Align the needle as indicated in “Aligning and Adjusting the Needle” on page 30.

5. Adjust the GIS speed as described in “Adjusting the GIS Speed” on page 34.

6. Reset the GIS lifetime counter as described in “Resetting the GIS Lifetime Counter” on page 35.

CA

UT

ION Use care when adjusting

or securing these parts. Rocking the system could damage the turbo pump.

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Platinum Deposition Aligning and Adjusting the Needle


Aligning and Adjusting the NeedleA GIS needle must be positioned so that it is centered a specified distance from the center cross. In addition, needles must be positioned a safe distance from the surface of the sample at the stage eucentric position.

Figure 12 illustrates the correct alignment and orientation for conventional needles.

Table 3 provides alignment positions for the conventional needles used on FEI systems.

Figure 12 Aligned Conventional Needles

Table 3 Needle Alignment Positions1

1.These alignment positions are optimized for ion beam deposition. The gas flux may not be optimum for electron beam deposition.

Needle TypeSystem Types Needle Position

Conventional

200 TEM, Vectra™ 200, 201, 205

75 µm up and 150 µm from center position

235 150 µm up and 50 µm from center position

200 mm 100 µm up and 100 µm from center position

300 mm 100 µm up and 100 µm from center position

CA

UT


the needle position to avoid upsetting the motion-sensitive turbopump.

Field-of-view center for ion beam

Ion column

Conventional needle

Distance to center of viewDistance to stage-

eucentric position

Sample surface at eucentric position

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Coarse AlignmentCoarse alignment helps put the needle into the field of view of the ion beam.

1. With the specimen chamber at atmospheric pressure, confirm that the installed GIS is mounted in the center of its mounting clamps. This ensures that the adjustment range is not limited.

2. Slowly loosen the mounting clamp adjustment setscrews to an optimum starting point (not completely loose) to ensure full adjustment range during alignment.

3. Lower the stage to a safe location, well below the stage eucentric point.

4. Manually insert the GIS to be aligned and another, previously aligned GIS (if one exists). To manually insert the GIS, temporarily exchange the red and black air hoses.

5. Insert the new needle and roughly align it to the other. View the needles either by looking through an open port or the chamber door, or by using the optical microscope.

6. Return the manually inserted GIS to its original state.

7. Mount the system test sample onto the stage and pump the system down (if not already done).

8. Heat the GIS for at least 15 minutes to allow it to thermally stabilize. (Thermal expansion of the injector extends the needle slightly.)

9. Confirm that the stage is well below the eucentric point and insert the needle.

10. Start imaging, using a current of < 300 pA and the lowest magnification setting to locate the needle. Use low mag (10 kV accelerating voltage) if necessary.

11. You may also need to make adjustments to the GIS to bring the needle into the field of view.

NO

TE

Do not overtighten the adjustment setscrews. This can limit the adjustment range and/or damage the setscrews.

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Fine Alignment1. Loosen the locking setscrew on the side of the GIS adjustment

collar about two turns.

2. Retract the needle. Coarsely adjust the needle insertion length by rotating the adjustment collar on the GIS body. Always retract the needle before rotating the GIS to avoid damage to the GIS. Do not use excessive force to rotate the collar.

3. Adjust the needle angle via the four small setscrews on the GIS clamps. Turning in the top two setscrews moves the needle down (towards the sample) and turning in the bottom two setscrews moves the needle up (away from the sample). Likewise, the left screws move the needle right, and vice versa. There will be some interaction between the insert position adjustment collar and the needle angle positioning setscrew, and you will need to alternate between the two modes.

4. Note the new Z position value with the sample lightly touching the needle (for example, 5250 µm) and compare it to the value for eucentric height (250 µm above eucentric).

Figure 13 Adjusting the Needle Angle

CA

UT

ION Apply only light tension to

the nylon-tipped setscrew. Do not turn the adjustment collar without first loosening the locking setscrew.

Locking setscrew

CA

UT


the needle position to avoid upsetting the motion-sensitive turbopump.

Move the needle away from the sample.

Move the needle to the right.

Move the needle to the left.

Move the needle towards the sample.

NOTE: Movement directions are port-dependent.

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5. Lower the stage several mm and make an adjustment to the needle length and angle that will set it the proper height above eucentric height (see Table 3, “Needle Alignment Positions,” on page 30. Carefully raise the sample again until it just touches the needle, and calculate the difference of the new Z position value from the eucentric position value.

6. If the position needs further adjustment, repeat the preceding step until the needle is the proper height above the sample eucentric height (Table 3). It may take several tries to get it in position.

7. When the needle is in the correct position, tighten the collar-locking setscrew. This might change the setting a little, so confirm that the position is still good and make corrections as necessary.

8. Retract the needle and reinsert it. Verify once more that the needle is in the proper position (Table 3).

Inspect the needle position once a week with the needle at operating temperature and adjust as necessary. If you experience difficulties with the GIS after replacing the crucible and needle, call FEI Customer Service at 1-866 MYFEICO (693-3426).

NO

TE Apply only light tension to

the nylon-tipped setscrew.

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Platinum Deposition Adjusting the GIS Speed


Adjusting the GIS SpeedThe gas injector should already be set to insert and retract slowly. Move the stage to its lowest Z position before proceeding.

To check the GIS speed:

1. Loosen locking collars on both air line connectors.

2. Click Needle IN and OUT to check the insert/retract speed, about 3–5 seconds each direction.

3. Turn the thumbscrew on the black hose to adjust the insert speed. Turn the thumbscrew on the red hose to adjust the retract speed. Refer to Figure 4, “GIS Adjustment Features,” on page 18.

4. Tighten the locking nut to secure the final position of the retract and insert thumbscrews.

NO

TE

Do not attempt to adjust the speed of the top pneumatic fitting. This is the GIS valve, which should be permanently set to full speed.

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Platinum Deposition Resetting the GIS Lifetime Counter


Resetting the GIS Lifetime CounterAfter you replace or refill a GIS, reset the lifetime counter. Log in as Supervisor. Select the Work page > GIS CONTROL > ZERO for the appropriate GIS injector.

Setting the Crucible TemperatureSP 1 (Setpoint 1), displayed on the Omega or Newport temperature controllers, specifies the crucible temperature.

The Newport temperature controller is a replacement for the Omega controller and performs the same basic functions. Both controllers may exist on a system. The Newport controller displays the temperature in 4 digits and has 4 buttons on the interface.

After clicking Heat ON, always wait 15 minutes before using the GIS for proper heat distribution.

For uniform gas flux, click Valve OPEN 2 minutes before initial deposition. At the end of 2 minutes, the vacuum pressure should no longer be dropping because of gas bursts.

Crucible Default TemperatureThe default temperature for platinum (Pt) is 45°C for the Newport controller and 40°C for the Omega controller.

Setting the Omega Controller SetpointTo change SP 1 on the Omega controller:

1. Press * and hold.

2. Press or to set the operating setpoint.

3. Release *.

WA

RN

ING

!

Do not exceed the specified temperature. Exceeding these temperatures may void your warranty and service agreement.Increasing the setpoint for platinum will degrade/destroy the chemical.

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Platinum Deposition Setting the Crucible Temperature


Changing the Newport Controller SetpointTo change SP 1 on the Newport controller:

1. Press MENU. SP1 displays.

2. Press MAX to increase the first digit of the setpoint.

3. Press MIN to activate the next digit (it will be flashing).

4. Continue to use MAX and MIN to enter the 4-digit SP 1 value. For example, 40° C would be 040.0 and 35° C would be 035.0

5. Press ENTER when the value is correct.

NO

TE

You must open the electronics extension cabinet cover to access either controller. Be sure to turn off HT (high tension) before removing this cover.

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Platinum Deposition GIS Troubleshooting


GIS Troubleshooting Table 4 GIS Warning and Error Messages (1 of 2)

Condition Possible Cause Remedy

GIS needle does not insert or retract.

The insert/retract speed thumbscrews are too tight.

Loosen the insert/retract speed thumbscrews. See “Adjusting the GIS Speed” on page 34 and Figure 4, “GIS Adjustment Features,” on page 18.

GIS valve does not open.

The valve thumbscrews are too tight. Open the valve thumbscrews. See “Reinstalling the Gas Injector” on page 27 and Figure 4, “GIS Adjustment Features,” on page 18.

Heat Not Ready or Heat Not On error message

You selected OPEN from the GIS Control dialog box or you ran a pattern file and the gas injector heat was not on.

Click OK to close the dialog box; no patterning occurs. Turn on the GIS heat.

You heated a gas injector, but the proper heat was not reached and you attempted to open the valve or mill a pattern.

Click OK to close the dialog box; no patterning occurs. Wait for the Heat Ready light.

Inserted Needle Warning error message

One or more needles were inserted and you attempted to insert another from the Gas Injection group or the GIS Control dialog box.

Click OK to close the warning message and insert the selected needle. Click CANCEL to close the dialog box without inserting the needle.

Insufficient deposition

The GIS crucible might be empty. Verify the pressure rise. If the pressure is too low, the GIS may be empty. Review the GIS lifetime display for the affected beam chemistry (see “GIS Refill Procedures” on page 15).

Insufficient deposition

The needle might be misaligned. Check the distance from the sample to the needle. Ensure that the needle is aligned as described in “Aligning and Adjusting the Needle” on page 30.

Needle Not Inserted, Milling Aborted error message

You ran a pattern with a GIS selected and the relevant needle was not inserted.Message displays in Serial Patterning mode. The error message is given before any patterning starts and not when a pattern with such an error condition is reached.

Click OK to continue patterning. Click CANCEL to stop patterning. Insert the needle, verify the pattern position on the sample, then resume operation.

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Platinum Deposition GIS Troubleshooting


If you encounter difficulties not listed above, call FEI Customer Service at 1-866 MYFEICO (693-3426).

Vacuum Not OK error message

There is insufficient chamber vacuum to operate a GIS.

Click OK to close the dialog box; troubleshoot vacuum status.

Warning: Move too large - GIS needle(s) inserted error message

You requested a stage move through the user interface.

Click CANCEL to abort the stage move. Retract the needle. Move the stage to a safer height for the needle. Verify the eucentric height. Reinsert the needle.

Table 4 GIS Warning and Error Messages (2 of 2)

Condition Possible Cause Remedy

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Platinum Deposition Platinum (Methylcyclopentadienyl [Trimethyl] Platinum) MSDS


Platinum (Methylcyclopentadienyl [Trimethyl] Platinum) MSDS

M A T E R I A L S A F E T Y D A T A S H E E T

Page 1 of 6

Platinum Deposition

NFPA HMIS

2

0

0

HEALTH 2

FLAMMABILITY 0

REACTIVITY 0

PERSONAL PROTECTION J

1. Product And Company Identification

Supplier Manufacturer

Colonial Metals, Inc. Colonial Metals, Inc.

Building 20 Building 20

505 Blue Ball Road 505 Blue Ball Road

Elkton, MD 21921 United States Elkton, MD 21921 United States

Company Contact: Wayne Sher Company Contact: Wayne Sher

Telephone Number: 410-398-7200 Telephone Number: 410-398-7200

FAX Number: 410-398-2918 FAX Number: 410-398-2918

E - M a i l : [email protected] E - M a i l : [email protected]

Web Site: colonialmetals.com Web Site: colonialmetals.com

Supplier Emergency Contacts & Phone Number Manufacturer Emergency Contacts & Phone Number

Chemtrac: 800-424-9300 Chemtrac: 800-424-9300

World Wide - Call COLLECT to U.S: 703-527-3887 World Wide - Call COLLECT to U.S: 703-527-3887

Issue Date: 08/18/2005

Product Name: Platinum Deposition

Chemical Name: Trimethyl [(1,2,3,4,5-ETA.)-1 Methyl 2, 4-Cyclopentadien-1-YL] Platinum

CAS Number: 94442-22-5

Chemical Family: Platinum Group Metal Organometallic Complex

Chemical Formula: C9H16Pt

MSDS Number: 80

Product Code: 0080

Synonyms

Trimethyl [(1,2,3,4,5-ETA.)-1 Methyl 2, 4-Cyclopentadien-1-YL] Platinum, Platinum Deposition

2. Composition/Information On Ingredients

Ingredient CAS Percent Of

Name Number Total Weight

Methylcyclopentadienyl (Trimethyl) Platinum 094442-22-2 100

EMERGENCY OVERVIEW

To the best of our knowledge the chemical, physical, and toxicological properties have not been thoroughly

investigated. Avoid air. Product incompatible with oxidizing agents and air. Can decompose toxic fumes of COx

and metal oxide.

40P N 4 0 3 5 2 7 2 2 1 8 5 1 - D 7 / 1 1 / 0 7




Page 2 of 6

Platinum Deposition

3. Hazards Identification

Primary Routes(s) Of Entry

Eye: Likely

Inhalation: Likely

Skin: Likely

Ingestion: Likely

Eye Hazards

May cause eye irritation.

Skin Hazards

May cause mild to moderate skin irritation.

Inhalation Hazards

Coughing, shortness of breath, wheezing.

Conditions Aggravated By Exposure

Any respiratory condition such as asthma. Maintain housekeeping and personal hygene to minimize exposure

and prevent sensitization. Platinum salts can cause a condition called Platnosis, effecting respiratory system.

Conditions Aggravated By Overexposure

May result in pulmonary fibrosis. To the best of our knowledge, the chemical, the physical, and toxicological

properties have not been thoroughly investigated.

First Aid (Pictograms)

4. First Aid Measures

Eye

Flush for 15 minutes with plenty of water. If discomfort occurs or persists, contact a physician.

Skin

Flush area for 15 minutes with water and wash with soap and water. If discomfort occurs or persists, contact a

physician.

Ingestion

If swallowed, contact a physician immediately. Do not give activated charcoal before or with syrup of ipecac. If

swallowed, do not induce vomiting unless directed...

Inhalation

Remove to fresh air immediately. If discomfort occurs or persists, contact a physician. If not breathing, give

artificial respiration.

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Page 3 of 6

Platinum Deposition

Fire Fighting (Pictograms)

5. Fire Fighting Measures

Flash Point: Non-flammable °F

Flash Point Method: NA

Flammability Class: NA

Fire And Explosion Hazards

Use proper safety equipment. Can decompose to emit toxic, irritating fumes of carbon monoxide, carbon dioxide

and metal oxide.

Extinguishing Media

Dry chemical powder, carbon dioxide, or sand.

Fire Fighting Instructions

Use NIOSH/MSHA approved self-contained breathing apparatus and full protective clothing.

6. Accidental Release Measures

Pick up mechanically, caution air sensitive and place in sealed container for reclaimination or disposal. Person

protected with full face shield and NIOSH approved respirator and cartridge for dust. Ventilate area and wash spill site

after pick-up is complete.

Handling & Storage (Pictograms)

7. Handling And Storage

Handling And Storage Precautions

Avoid contact with eyes, prolonged or repeated contact with skin. Use compatible chemical resistant gloves.

Wash hands thoroughly after handling.

Handling Precautions

Avoid breathing dust or vapor. Avoid contact with skin and clothing.

Storage Precautions

Store in a dry place. Do not store directly on ground..

Work/Hygienic Practices

Use good personal hygiene. Wash thoroughly after handling. Wash thoroughly with soap and water after handling.

Other Precautions

0.01 ppm high efficiency particular respirator/supplied air respirator/self-contained breathing apparatus; 0.2 ppm same

as above with full face piece; 1 ppm powdered air purifying respirator with high efficiency filter/type C supplied air

respirator operated in pressure demand mode.

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Page 4 of 6

Platinum Deposition

7. Handling And Storage - Continued

Work/Hygienic Practices - Continued

Store in sealed container, plastic or plastic liners, in a cool, well ventilated, dry area away from air. Store under inert

gas.

Protective Clothing (Pictograms)

8. Exposure Controls/Personal Protection

Engineering Controls

Ventilation: Local Exhaust:Required in handling area

Mechanical: Desirable to insure concentration

of material below TLV/TWA levels

Other: Closed Ventilation system

Eye/Face Protection

ANSI approved safety glasses/goggles

Skin Protection

Rubber/Neoprene (use compatible chemical-resistant gloves).

Respiratory Protection

NIOSH approved chemical cartridge respirator for particulates and dust or self-contained breathing apparatus

with full face shield.

Other/General Protection

Lab coat/apron, flame and chemical resistant protective clothing, eye wash, safety shower, and hygiene facilities

for washing.

Ingredient(s) - Exposure Limits

Methylcyclopentadienyl (Trimethyl) Platinum

Platinum Only::

NIOSH Exposure Limits: 0.002 mg/m3

OSHA: TWA 1 mg/m3

ACGIH: 0.002 mg/m3

9. Physical And Chemical Properties

Appearance

Off-white powder

Odor

None

Chemical Type: Mixture

Physical State: Solid

Melting Point: 30-31 °C

Boiling Point: Sublimes °C

43P N 4 0 3 5 2 7 2 2 1 8 5 1 - D 7 / 1 1 / 0 7




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Platinum Deposition

9. Physical And Chemical Properties - Continued

Odor - Continued

Specific Gravity: NE

Molecular Weight: 319.34

Vapor Pressure: 0.053 mmHg

Vapor Density: NE

pH Factor: NA

S o l u b i l i t y : Insoluble

Evaporation Rate: NE

10. Stability And Reactivity

S t a b i l i t y : Stable

Hazardous Polymerization: Will not occur

Conditions To Avoid (Stability)

Air (store under inert gas)

Incompatible Materials

Mixing with oxidizing agents and air

Hazardous Decomposition Products

Toxic fumes of COx and metal oxide

11. Toxicological Information

No Data Available...

12. Ecological Information

No Data Available...

13. Disposal Considerations

Consult Federal EPA, State and local regulations for proper disposal/recycle/reclamation

NOTE: Chemical additions, processing, or otherwise altering this material may make the waste management

information presented above incomplete, inaccurate, or otherwise inappropriate.

RCRA Information

NL

14. Transport Information

Proper Shipping Name

Non-Hazardous

Additional Shipping Paper Description

IATA Regulations: Non-Hazardous

15. Regulatory Information

U.S. Regulatory Information

TSCA: Yes

Canadian Regulatory Information

This prodcut has been classified in accordance with the hazard criteria of CPR, and the MSDS contains all the information required by the CPR.

44P N 4 0 3 5 2 7 2 2 1 8 5 1 - D 7 / 1 1 / 0 7




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Platinum Deposition

15. Regulatory Information - Continued

European Union (EU) Regulatory Information

Information not available.

16. Other Information

NFPA Rating

H e a l t h : 2

F i r e : 0

R e a c t i v i t y : 0

HMIS Rating

H e a l t h : 2

F i r e : 0

R e a c t i v i t y : 0

Personal Protection: J

Revision/Preparer Information

MSDS Preparer: Wayne Sher

MSDS Preparer Phone Number: 410-398-7200

This MSDS Supercedes A Previous MSDS Dated: 02/25/2002

Disclaimer

In compliance with the OSHA Hazard Communication Standard, 29 C.F.R 1910.1200, we are providing you with a

Materials Safety Data Sheet (MSDS) for the hazardous material you are purchasing.

It is your responsibility to educate your employees on the safe use of the hazardous material. With this in mind, a

copy should be forwarded to the supervisor of the user or to the user themselves, and copy should be retained in

your files for future reference.

Colonial Metals, Inc. makes no presentation as to the accuracy of the information in the MSDS. The information

is believed to be correct; however, you (the customer), should perform your own investigation and independent

verification. If you resell the product, you are responsible to forward the information in the MSDS to your

customer.

Colonial Metals, Inc.Printed Using MSDS Generator™ 2000

45P N 4 0 3 5 2 7 2 2 1 8 5 1 - D 7 / 1 1 / 0 7

Platinum Deposition


46P N 4 0 3 5 2 7 2 2 1 8 5 1 - D 7 / 1 1 / 0 7

Platinum Deposition


47P N 4 0 3 5 2 7 2 2 1 8 5 1 - D 7 / 1 1 / 0 7

C O N F I D E N T I A LFEI Limited Rights Data

Index

Aair lines 17, 28alignment

coarse 31fine 32GIS needle 31, 32

Bbeam current 1

and electrostatic discharge 13beam current/pattern area 3

Ccarbon content in platinum deposition 5circuit edit applications 5clamp screws 19coarse alignment 31

GIS needle 31coatings and current density 13compressed air source

reconnecting 28turning off 16

compressed air, low pressure, error message 17, 28control cable 18controller

Newport 36Omega 35

crucibledefault temperature 35disposal 24heating 35installation 25 – 27mounting screws 27removal 21 – 22setpoint 35, 36side view 24temperature 1unpacking a new one 23

customer maintenance training 14Customer Service contact information 14

Ddeposition 1

efficiency, illustrated 2factors 1fast scanning and layer growth 2finding resistance 3insufficient 37net rate 2rate 3, 10

with required resistance 4dwell time 2

Eelectron beam deposition 5 – 9electrostatic discharge 13error messages 37

Ffast scanning and layer growth 2fine alignment, GIS needle 32

Ggas flux and deposition rate 1GIS (gas injection system)

patterning and milling 1GIS components illustrated 18GIS heating 31GIS lifetime counter 35GIS maintenance 14 – 36

equipment required 16training 14

GIS speed, adjusting 34GIS troubleshooting 37

Iinjector

compressed air sourcereconnecting 28turning off 16

handling 16heat warning message 37installation 27 – 34

illustration 22pumping down 29refill procedure 15removal 16 – 21returning empty 21

inserting the needle, warning message 37installation

crucible 25 – 27diagram 22injector 27 – 34

insufficient deposition 37Insulator Deposition III (HMCHS) MSDS 39

Llayer growth 2lifetime 15

4848P N 4 0 3 5 2 7 2 2 1 8 5 1 - D 7 / 1 1 / 0 7

Index M-W

C O N F I D E N T I A L FEI Limited Rights Data

Mmaterial files

for electron beam deposition 8pt_high_mag.mtr 10pt_low.mtr 10pt_mag.mtr 10pt_tem.mtr 10pt_via.mtr 10smarter, Sidewinder column 10

mounting screws 27

Nneedle

alignment 31, 32angle 32coarse alignment 31diameter 1insertion warning 37position 1, 26, 30warning message 37

net deposition rate 2Newport temperature controller 35

setpoint 36

OOmega temperature controller 35

setpoint 35O-ring 26, 27

Ppatterning mode for electron beam deposition 8photoresist exposure matrices 5platinum

default temperature 35finding resistance for deposition 3

pressure 37pt_high_mag.mtr 10pt_low.mtr 10pt_mag.mtr 10pt_tem.mtr 10pt_via.mtr 10

Rrate

deposition 3, 10sputtering 10

removalcrucible 21 – 22gas injector 16 – 21

resistance 3formula 4

Ssafety precautions 14

clothing 16, 17scan area 1scan speed 1serial patterning error message 37setpoint, changing 35, 36smarter material files, Sidewinder ion column 10sputtering rate 2, 10stage tilt for electron beam deposition 7

TTEM sample preparation 5temperature

controllers 35crucible 1crucible defaults 35

training, customer maintenance 14troubleshooting

GIS does not insert or retract 37GIS does not open 37insufficient deposition 37Warning, Move too large 38

Vvacuum warning message 38

Wwarning message, compressed air low pressure 17,

28workstand 20

platinum deposition technical note - michigan … · 5350 ne dawson creek drive hillsboro, oregon...

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