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NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide NASA Aeronautics Research Mission Directorate (ARMD) 2014 Seedling Technical Seminar February 19–27, 2014 Robert S. Okojie, PhD NASA Glenn Research Center, Cleveland OH Email: [email protected]; phone: (216)433-6522

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Page 1: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in

Silicon Carbide

NASA Aeronautics Research Mission Directorate (ARMD)

2014 Seedling Technical Seminar

February 19–27, 2014

Robert S. Okojie, PhD

NASA Glenn Research Center, Cleveland OH

Email: [email protected]; phone: (216)433-6522

Page 2: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

Outline

Reactive Ion Etching: The Basics

Observed Phenomenon

Technical Approach

Results

Innovation and Impact on Mission

Next Steps

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 2

Page 3: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

Reactive Ion Etching (RIE): The Basics

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 3

Halogen based gas (i.e., SF6) is ionized to create F

ions and

neutrals. Neutrals react chemically with target. F ions accelerate toward the target substrate under E-field and are adsorbed. F ions assist neutrals chemical reaction, leading to enhanced chemical etching of target. With argon added and ionized, Ar

+ physical bombardment of

target causes erosion. Results in increased chemical reaction and higher etch rate.

E-Field

F- F

- F- F

- F

-

P.H. Yih et al.: A Review of SiC Reactive Ion Etching in Fluorinated Plasmas, phys. stat. sol. (b)202, 605 (1997)

Neutrals

Page 4: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

Observed Phenomenon

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 4

Hole

Etched diaphragm in semi-insulating SiC

Boss

Free standing, 2 m highly doped

n-type SiC resistor

Semi-Insulating

SiC substrate

Hole due to over-etch

Free standing, 2 m highly doped n-type

SiC resistor

Unintentional rupture of micro diaphragms was observed during routine RIE

(with SF6 + Ar) of semi-insulated (SI) 4H-SiC substrate.

Observed free standing 2µm thick “cantilevers” of the patterned highly doped

n-type homoepitaxially grown 4H-SiC piezoresistor layer on the SI SiC.

Etch selectivity between SI and highly doped n-type SiC is proposed

RIE

Page 5: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

Technical Approach

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 5

SF6= Flow Rate (sccm) SI N-Type(Nd=3.8 x 1019 cm-3) 45 3 8 60 4 9 75 5 10

Calibration patterns etched in n-type and semi-

insulating SiC samples.

Fixed process conditions: RF Power=400 W; Base Pressure = 25 mT; Etch Time=2 hours

Photolithography and Al pattern definition with

calibration mask

RIE

Al mask stripped off and performed depth profile

measurement

Depth Profile

Page 6: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 6

Etching selectivity between SI and highly doped n-type

substrates in SF6 gas only.

Selectivity Between SI and N-Type 4H-SiC

480

500

520

540

560

580

30 40 50 60 70 80

Etc

h R

ate

(Å/m

in)

SF6 Flow Rate (sccm)

SI-SiC N-Type SiC (3.8 x 10^19 cm^-3)

RF Power = 400 WBase Pressure = 25 mT

Higher doping increases

selectivity

Page 7: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 7

Etching selectivity between highly doped p- and n-type 4H-SiC

substrates in SF6 gas only.

600

650

700

750

800

850

900

950

1000

30 40 50 60 70 80 90

Etc

h R

ate

(Å/m

in)

SF6 Flow Rate (sccm)

DH0852-14 (p-2e20), 0.5 µm epi BQ0339-10 (n>2e19), 2 µm epi

RF Power = 400 WBase Pressure = 25 mT

Selectivity Between N- and P-Type 4HSiC

Higher doping increases

selectivity

Page 8: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

500

600

700

800

900

30 40 50 60 70 80 90

Etc

h R

ate

(Å/m

in)

SF6 Flow Rate (sccm)

2 x 10^19 cm^-3 3.8 x 10^19 cm^-3

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 8

Selectivity in N-Type Concentrations

Selectivity increasing with

increased dopant

concentration

Page 9: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

DSRIE Release of N-Type Cantilevers

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 9

Suspended 2 µm

thick single crystal

SiC piezoresistor

Proof mass

suspended by 2 µm

thick single crystal

SiC piezoresistor

SEM paste!

Suspended 2 µm

thick single crystal

SiC piezoresistor

Page 10: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

~220 µm

~3 µm

DSRIE Release of N-Type Cantilevers

Page 11: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

Innovation and Impact on Mission

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 11

Mission Challenges: Thermoacoustic instabilities in combustors are known to be precursor to flame-out or damage to engine components. Existing instability prediction models have high uncertainty margins. Need environmentally robust and reliable pressure sensors for model validation and improvement.

Existing Technology Gap: SoA sensors placed feet from test article-limits frequency bandwidth; Water cooling adds “vortex noise” to corrupt signal. Robust and reliable sensors needed for direct (no water cooling) measurement of sub-psi dynamics at >500 ºC. 600 ºC SiC pressure sensor technology currently exists, but SiC fabrication technology cannot produce the ultra-thin diaphragms to achieve the high sensitivity needed to resolve sub-psi pressure dynamics.

Innovation: DSRIE will result in ultra-thin (< 10 µm) SiC diaphragms to accurately resolve sub-psi dynamics at temperatures in excess of 500 ºC (current capability).

Flush mounted

SiC dynamic sensor

Benefit of SiC Etch Stop Mechanism

~5 µm etch stop diaphragm

Semi Insulating SiC

Page 12: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

Next Steps

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 12

Improve further understanding of the DSRIE mechanism -Investigate various doping levels and other halides to optimize etch selectivity

Demonstrate 5-10 µm thick diaphragm SiC pressure sensors -Based on circular plate theory, maximum deflection (for deflections << thickness) of a clamped circular plate is expressed as:

Where: =maximum deflection (m); P=applied pressure (Pa); r=diaphragm radius (m); E=Young’s Modulus (Pa); h=diaphragm thickness (m); =Poisson ratio

For E =475 GPa for SiC; h =5 µm; r =1 mm; = 0.212

The predicted ~ 1 µm and applied pressure is ~345 Pa (0.05 psi)

~5 µm etch stop diaphragm

Page 13: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

Summary/Conclusion

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 13

Confirmed existence of dopant and conductivity selectivity in SiC during reactive ion etching with SF6 gas;

While the etch selectivity ratio between the SI and n-type SiC using SF6 gas is < 2, free standing n-type cantilever structures were realized;

Validation of this proof of concept allows the investigation of other halides in which the etch selectivity ratio may be higher.

More experimental data is needed to determine the effective role of doping concentration and conductivity.

Page 14: Concept Demonstration of Dopant ... - nari.arc.nasa.gov · NASA Aeronautics Research Institute Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

NASA Aeronautics Research Institute

Acknowledgement

February 19–27, 2014

NASA Aeronautics Research Mission Directorate 2014 Seedling Technical Seminar 14

Kimala Laster/Ariana Miller - sample fabrication Beth Osborn-Sample preparation Laura Evans and Pete Bonacuse - SEM images Kelley Moses and David Spry- RIE system health maintenance Sponsor: ARMD Seedling Fund