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1 KSC Efforts at Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned Earlier F. W. Adams / NASA / KSC Duke Follistein / NASA / KSC

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Page 1: Spectrometers Ruggedization of Mass Miniaturization and ... 3rd/Adams/adams.pdf · Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned ... Kisholoy

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KSC Efforts at Miniaturization and

Ruggedization of Mass Spectrometers

& Other Topics Not Mentioned Earlier

F. W. Adams / NASA / KSCDuke Follistein / NASA / KSC

Page 2: Spectrometers Ruggedization of Mass Miniaturization and ... 3rd/Adams/adams.pdf · Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned ... Kisholoy

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KSC RequirementsMass Analyzers (systems)

H2, He, N2, O2, Ar, CO2Background gas: Helium, Nitrogen or AirSensitivity to ppm’s at low concentrationWide dynamic range (10K - 100K)Small, Rugged, Reliable

Backing and High-Vacuum PumpsSample Delivery Systems and Components Point Sensors and Multiplexors

Page 3: Spectrometers Ruggedization of Mass Miniaturization and ... 3rd/Adams/adams.pdf · Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned ... Kisholoy

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Mass AnalyzersIonization

Solid State free-electron source (SBIR)Efficiency enhancement concept (TBD)Monolithic Block construction

Mass FilterSimplified Time-of-Flight (SBIR)Ortho Time of Flight (SBIR)Ion-Trap (Grant, U/F)

DetectorsMiniaturized electron multipliersRuggedized micro-channel plate assembliesMonolithic block construction

Page 4: Spectrometers Ruggedization of Mass Miniaturization and ... 3rd/Adams/adams.pdf · Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned ... Kisholoy

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Pumps (Backing, High-Vacuum)Miniaturization

JPL Miniature Pumps EffortRotary Backing Pumps (Summer Faculty)

RuggedizationCreare SBIR Turbo-molecular pumpSolid-State Free-electron SourceIonization-Efficiency enhancementIon Engine Concept

Page 5: Spectrometers Ruggedization of Mass Miniaturization and ... 3rd/Adams/adams.pdf · Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned ... Kisholoy

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Sample Delivery / ComponentsManifolds and Fittings

Fabrication and ReliabilityMiniature pressure regulators

Rugged, Reference against vacuumMiniature Valves

Reliable, Leak Tight, Low dead volumeMiniature Flow Controllers

Rugged, Reliable, Low dead volume

Page 6: Spectrometers Ruggedization of Mass Miniaturization and ... 3rd/Adams/adams.pdf · Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned ... Kisholoy

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Point Sensors (Reduced Sensitivity)

Cryo Operation Point Hydrogen, Oxygen sensorsReduce response time

Ground Support EquipmentCryo operationRoom temperature

Flight VehiclesOn-board, IVHM

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Funding Mechanisms (Historical)Small Business Innovation Research

Creare / Rugged, Miniature High-Vacuum PumpIonWerks / Solid-State Free Electron SourceIntelligent Optical Sensors / Fiber O2, H2 SensorsSouthwest Sciences, Inc / Unique TOF ApproachMakel Engineering, Inc. / Point Sensors H2 / O2

Internal FundingEngineering Technology Base (ETB)Space Launch Initiative / Second Generation RLV

PartnershipsLocal UniversitiesSummer Faculty Fellowships

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Funding / InternalEngineering Technology Base (ETB)Space Launch Initiative / 2nd Gen RLV3rd Gen Recently CancelledCenter Director’s Discretionary Fund (CDDF)Shuttle ProjectsAir Force, Navy, Army, etc.

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Funding, PartnershipsLocal Universities

Florida Solar Energy Center (MEMS Fab)Florida Institute of Technology (Fiber optics)University of Florida (Ion-Trap)

Summer Faculty FellowshipsConcept Generation and evaluationExperimental researchDetail design and performance evaluation

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SBIR / Phase-I / CREARECreare

Under a KSC-sponsored SBIR, Creare Inc. is building a highlyruggedized version of a recently developed 5 L/s turbomolecularpumpMiniaturized and rugged high vacuum systems are needed to complement recently developed portable mass spectrometersA key innovation of the new version is an “inside-out” electric motor that replaces the typical cantilevered rotor with one supported at both top and bottom, providing high tolerance to vibration and shockThe TMP will be combined with a modified version of a commercial rough pump to form a complete vacuum system

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SBIR / Phase-I / Creare

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SBIR / Phase-II / IonWerksIonWerksAl Schultz, Katrin Fuhrer, Marc Gonin

Solid-State Free Electron Source• Rugged• Reliable

Applications• Analyzer ionizer• Ion-engine based high vacuum pump

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SBIR / Phase-II / IonWerks

Goals-rugged-compact-high sampling speed

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SBIR / Phase-II / IonWerks

H2, He and Ar test gases in Nitrogen

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SBIR / Phase-II / IonWerks

10 0 20 08 0 00

10 0 00

12 0 00

14 0 00

tim e [s]

0

3 00

2 5 pp m Ar(o n top o f ~ 5 0 pp m re sid u al A r )

2 5p pm He

coun

ts /

0.5s

8 00

1 0 00

1 2 00

25 pp m H2( on top o f ~ 5 0 pp m re sid u al H2)

25 ppm He, H2, and Ar 0.5 s measurements with 1 sigma

error bars

0

10

20

30

H2 He Ar

ppm

Page 16: Spectrometers Ruggedization of Mass Miniaturization and ... 3rd/Adams/adams.pdf · Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned ... Kisholoy

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SBIR / Phase-II / IonWerks

1000 1500 2000 2500 3000 3500-2000

0

20004000

60008000

1000012000

1400016000

N 2 cou

nts/

seco

nd

Source bias, V

Pressure 3x10-6

Double stack MCP voltage 2600V

Source-grid design with double/triple stack MCP electron current multiplier

1. Operation efficiency: comparable to that of the filament ionizer with 100nA electron emission current.2. Emission current stability about 3%.

Performance update

1. High gain/high maximum output (up to 100 µA) single channel electron current multiplier will be used.

2. High tension grid will be utilized in order to improve the emission stability.

3. Extra multiplication stage will be added if necessary.

Further improvements

1 2 1 6 2 0 2 4 2 8 3 2 3 6 4 0 4 4 4 8 5 2M a s s , a m u

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SBIR / Phase-II / IonWerks

•50’000 mass spectra per second

•0.1 s response time with capillary interface

•Spectra currently averaged over 0.5 s:25 ppm H2, He measured with 10% error in 0.5 s25 ppm Ar measured with 5% error in 0.5 s

•Filamentless ionizer under development for increased ruggedness

Future development:•Increase sampling speed•Shrink electronics•Implement filamentless ionizer

O-TOF: Current status

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SBIR / Phase-I / IOSKisholoy Goswami (PI)Intelligent Optical Sensors

Fiber H2, O2 SensorsMultiplex featuresFunctions demonstrated

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SBIR / Phase-I / IOSIntelligent Optical Systems (IOS) is now developing gas sensors for use on and around space launch vehicles

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SBIR / Phase-I / IOSProject Goals (Long-term, Phase III)

Demonstrate that H2 and O2 can be detected in real-time (within a second) in the ppm – 100% range.Establish that at least 20 sensors can be multiplexed at a cost of $10,000 or under.The sensors monitor these gases continuously.

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SBIR / Phase-I / IOS

PARAMETER O2 SENSOR H2 SENSOR

RANGE 0.1% TO 10% 0.1% TO 10%RESPONSE TIME ~ 1 Second ~ 1 SecondACCURACY ± 1% of Reading ± 1% of ReadingSENSITIVITY 0.10% 0.01%RESOLUTION 0.10% 0.01%SELECTIVITY 1-5% Nitrogen 1-5% Nitrogen

5% Carbon Dioxide 10% Oxygen75%-100% RH 75%-100% RH

TEMPERATURE RANGE 0°F - 140°F 0°F - 140°FDRIFT < 0.1% per Day < 0.1% per DayHALF LIFE OF SENSOR > I YEAR > I YEARFALSE ALARMS 0 0

Mixed, Phase I, II, III

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SBIR / Phase-I / IOS

Demonstrated performance of hydrogen sensors in the range of 0% to 10%

Demonstrated hydrogen sensor with no cross-sensitivity to nitrogen, helium, or air

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SBIR / Phase-I / IOS

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SBIR / Phase-I / IOS

OxygenSensitiveOptrode

TemperatureSensitive Optrode

HydrogenSensitive Optrode

Package1 cm long x 5 mm

diameter

CommunicationOptical Fibers

Fiber OpticRibbon Cable

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SBIR / Phase-I / IOS

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SBIR / Phase-II / MakelGARY W. HUNTER, Ph.D.

SENSORS AND ELECRONICS BRANCH INSTRUMENTATION AND CONTROLS DIVISION

NASA GLENN RESEARCH CENTER

PARTNERS

NASA GLENN RESEARCH CENTER NASA KENNEDY SPACE CENTER

MAKEL ENGINEERING, INC CASE WESTERN RESERVE UNIVERSITY

Page 27: Spectrometers Ruggedization of Mass Miniaturization and ... 3rd/Adams/adams.pdf · Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned ... Kisholoy

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SBIR / Phase-II / Makel Makel Engineering

Chemical H2, O2 Sensors• Reliable operation in Helium, Nitrogen or Air

Wide dynamic range• 100 ppm – 100%

Signal Processing • On-board sensor assembly

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SBIR / Phase-II / Makel

DEMONSTRATE STAND-ALONE SMART LEAK DETECTION SYSTEM WITH A SURFACE AREA THE SIZE OF POSTAGE STAMP

PROTOTYPE HYDROGEN/OXYGEN SENSOR SYSTEM WITH ELECTRONICS

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SBIR / Phase-II / MakelMICROFABRICATED GAS SENSORS

• COLLABORATIVE EFFORT BETWEEN NASA GRC AND CASE WESTERN RESERVE UNIVERSITY

• SENSOR DEVELOPMENT RESULTING FROM:

IMPROVEMENTS IN MICROFABRICATION AND MICROMACHINING TECHNOLOGYDEVELOPMENT OF SiC-BASED SEMICONDUCTOR TECHNOLOGY

• GAS DETECTION IN:

HARSH ENVIRONMENTSAPPLICATIONS BEYOND CAPABILITIES OF COMMERCIAL SENSORS TECHNOLOGY

• DEVELOPS PLATFORMS FOR A VARIETY OF MEASUREMENTS

SCHOTTKY DIODERESISTANCE BASEDELECTROCHEMICAL

• TARGET DETECTION OF GASES OF FUNDAMENTAL INTEREST

HYDROGEN (H2)HYDROCARBONS (CxHy)OXYGEN (O2)NITROGEN OXIDES (NOX) AND CARBON MONOXIDE (CO)CARBON DIOXIDE (CO2)

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SBIR / Phase-II / Makel

HYDROGEN EAK SENSOR TECHNOLOGY

1995 R&D 100 AWARD WINNER

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SBIR / Phase-II / Makel

RESISTOR

HEATER CONNECTOR

HEATERCONNECTOR

TEMPERATUREDETECTOR

CONNECTORS

Pd-ALLOY SCHOTTKY DIODE CONNECTORS

2.2 mm

WIDE CONCENTRATION RANGE HYDROGEN SENSORDESIGN

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SBIR / Phase-II / Makel

0

100

200

300

400

500

600

0 200 400 600 800TIME(SEC)

HYDR

OGEN

CON

CENT

RATI

ON (P

PM)

STS-95 Launch

Main Engine Cut Off (MECO)

STS-95 Hydrogen Sensor Flight Data

Page 33: Spectrometers Ruggedization of Mass Miniaturization and ... 3rd/Adams/adams.pdf · Miniaturization and Ruggedization of Mass Spectrometers & Other Topics Not Mentioned ... Kisholoy

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SBIR / Phase-II / Makel

• MICROFABRICATED AND MICROMACHINED FOR MINIMAL SIZE, WEIGHT AND POWER

CONSUMPTION (LESS THAN 2 W FOR 600 C OPERATION)

•AMPEROMETRIC OPERATION ALLOWS MEASUREMENT OF OXYGEN OVER A WIDE CONCENTRATION RANGE (0-100%)

• CHAMBER STRUCTURE CONTROLS OXYGEN DIFFUSION RATE

• INCORPORATION OF OXYGEN SENSOR WITH OTHER SENSORS (E.G. HYDROGEN) IN THE SAME PACKAGE PLANNED

Silicon

Silicon NitridePlatinum Zirconium Oxide

Silicon Dioxide

Not to scale:

4 micronTypical

ZrO2 Oxygen Sensor

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SBIR / Phase-II / Makel

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2nd Gen / MakelFocus is Ultra Miniaturization of Leak Detection Systems on 2nd Gen Vehicles Team is NASA GRC, NASA KSC, Makel Engineering, and Case Western Reserve UniversityProvide Simultaneous Measurement of Fuel and Oxidizer

Hydrocarbon, Oxygen, and Hydrogen SensorsReduce Power Consumption From 5W to approximately 100mW

enable battery or use of other low power sourceReduce Size Of Entire Sensor Module To Postage Stamp Size

enable large number of low cost sensors to be usedenable sensors to be incorporated into structures (composite valves, supports etc.)

Accomplishments - First Generation of Miniaturization Completed - Testing Being Conducted at KSC

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2nd Gen / Makel

Develop a multi-parameter smart sensor suitable for launch applications.Hydrogen, Oxygen, Pressure, and Temperature

Produce stand alone sensors suitable for future flight experiment or use on facilitiesTasks accomplished include:

thin film sensor optimization for hydrogen and oxygendevelopment of data logger module and flight power supply to enable autonomous flight experiments (i.e. No central data logger needed like IVHM experiments on STS-95 and STS-96)fabrication of prototypes to be delivered to NASA KSC in 2002

NASA Applications IncludeFlight Sensor For Space ShuttleLaunch Pad Facility SensorSensor for Grab Bottle Replacement

Commercial Spin Off of Product Being Tested by Non-NASA CustomersPEM Fuel Cell MonitoringFuel Cell Vehicle Leak Detection

H2 Sensor

O2 Sensor

Pressure Sensor

Single Chip MEMS SensorTechnology

Sensor Control/Interface Electronics- Single PCB 2”x2”

28 VDC Power

Digital Communications

Minature IntegratedSensor Head

Miniature Flight Electronics

Temperature Sensor

Oxygen Sensor

Hydrogen Sensor

Pressure Sensor

TempSensor

connector(on backof board)

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SBIR / Phase-I / SW SciencesSouth West Sciences

Special Time of Flight

40x10 -3

20

0

-20

Sign

al (V

)

120100806040200Mass (daltons)

ArN 2

H 2 and He