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SUSTAINABILITY ANALYSIS OF METAL ASSISTED CHEMICAL ETCHING OF SILICON NANOWIRES Fenfen Wang, Chris Yingchun Yuan Department of Mechanical Engineering, UWM Understand the sustainability performance of metal assisted chemical etching (MACE) of silicon nanowires (SiNWs) for lithium ion batteries (LIBs). Research Object: MACE of Si wafer for synthesizing SiNWs Quantify material consumptions and establish material flows of the process Analyze both airborne and waterborne emissions involved in the process. Specifically, gas and gaseous particle emissions were tested using in-situ measurements and particle emissions (including size distributions, concentrations, morphologies, material compositions) in solutions were characterized by applying ex- situ measurements. Provide first-hand data and information support for future scale-up of MACE method for SiNWs and support the sustainable development of this technology. Etching parameters: 20 mM AgNO 3 and 0.3 M H 2 O 2 . OBJECTIVES EXPERIMENTAL CHARACTERIZATION EXPERIMENTAL CHARACTERIZATION (Cont.) Metal assisted chemical etching (MACE) of SiNWs has disadvantage of low productivity with high material consumptions including large amount of toxic chemicals. For example, for 1 g of SiNWs 39.6 g of Si wafer and 854.9 g of HF are consumed, which are both economical and environmental concerns. Gas emissions including H 2 and NO and large amount of gaseous particle emissions are produced during the etching process. Most of the gaseous particles are with diameters less than 100 nm. What is more, particle emissions are also found in the etching solutions, which exert serious environmental and human health impacts. Further work is needed to study the possibility for improving the sustainability performance of MACE of SiNWs by increasing its productivity and reducing wastes. CONCLUSION [1] Li, M., Li, Y., Liu, W., Yue, L., Li, R., Luo, Y., Trevor, M., Jiang, B., Bai, F., Fu, P., Metal-assisted chemical etching for designable monocrystalline silicon nanostructure. Materials Research Bulletin, 76, 436-449, 2016. BIBLIOGRAPHY Fenfen Wang, Email: [email protected] Chris Yingchun Yuan, Email: [email protected] CONTACT INFORMATION ACKNOWLEDGEMENT This study is financially supported by the National Science Foundation (CBET-3560) Sustainability issues about MACE method Nano-particle emissions Large amount of material consumptions including toxic chemicals Introduction Etching mechanism of MACE for SiNWs formation [1]: Experimental process of MACE for synthesizing SiNWs Ag nucleation Ag nanoparticle Si Si Ag + e Si SiO 2 SiF 6 2- F - Si Ag + e e Si HF+AgNO 3 HF+H 2 O 2 Experimental flow chart for synthesis of SiNWs Silicon wafer Acetone Ethanol DI-H 2 O 10 min Cleaning N 2 blowing Drying HF+AgNO 3 1 min Etching HF+H 2 O 2 60 min Etching Diluted HF 2 min Etching HNO 3 60 min Cleaning Removing Ag particles Rinsing &Drying SiNWs DI-H 2 O Synthesis process Material inputs Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) characterizations Waterborne particle emissions Morphologies and element compositions of particles in solutions were tested by SEM and energy-dispersive X-ray spectroscopy (EDS) Material consumptions for synthesizing 1 g of SiNWs Input Materials Mass (g) Si Wafer (etched) 39.6 Acetone 495.2 Ethanol 494.6 DI-H 2 O 11055.6 HF (48%) 854.9 AgNO 3 4.5 H 2 O 2 (30%) 177.4 HNO 3 (70%) 158.1 Output Mass (g) SiNWs 1 Ag nanoparticles involved in SiNWs Ag nanoparticles 600 nm Nanoparticle size distributions in etching solution 300 400 500 600 700 0 20 40 60 80 100 Intensity Diameter (nm) G (d) C (d) Gas emissions Gas emissions including H 2 and NO were tested using residual gas analyzer (RGA) 0 1000 2000 3000 4000 0.0 1.0x10 -5 2.0x10 -5 3.0x10 -5 H 2 NO 0.0 2.0x10 -8 4.0x10 -8 6.0x10 -8 8.0x10 -8 1.0x10 -7 1.2x10 -7 1.4x10 -7 1.6x10 -7 1.8x10 -7 Time (s) Pressure (Torr) Gaseous particle emissions during the etching process Concentrations and size distributions of gaseous particle emissions were tested by ultrafine Condensation Particle Counter (UCPC) and Scanning Mobility Particle Sizer (SMPS) 0 50 100 150 200 250 0 1x10 3 2x10 3 3x10 3 4x10 3 5x10 3 6x10 3 Concentrations (#/cm 3 ) Time (s) From HF + AgNO 3 (a) 0 1000 2000 3000 4000 0.0 2.0x10 4 4.0x10 4 6.0x10 4 8.0x10 4 1.0x10 5 Concentrations (#/cm 3 ) Time (s) From HF + H 2 O 2 (b) 0 1000 2000 3000 4000 0 1x10 5 2x10 5 3x10 5 4x10 5 5x10 5 6x10 5 Concentrations (#/cm 3 ) Time (s) From HNO 3 (c) 100 200 300 400 0% 1% 2% 3% 4% 5% 20 40 60 80 100 0% 1% 2% 3% 4% 5% Percentage Diameter (nm) Percentage Diameter (nm) From HF + AgNO 3 (a) 0 100 200 300 400 500 600 700 0% 1% 2% 3% 20 40 60 80 100 0% 1% 2% 3% Diameter (nm) Percentage Percentage Diameter (nm) (b) From HF + H 2 O 2 100 200 300 400 500 600 700 0% 10% 20% 30% 40% 50% 100 200 300 400 500 0% 1x10 -3 % 2x10 -3 % 3x10 -3 % 4x10 -3 % Diameter (nm) Percentage Percentage Diameter (nm) (c) From HNO 3 In HF+H 2 O 2 solution In HNO 3 solution In HF+AgNO 3 solution O Ag 100 m Ag O C BSE C 7 m O F C BSE Si F O Si C F Ag O 100 m F O C BSE Ag C

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Page 1: SUSTAINABILITY ANALYSIS OF METAL ASSISTED - UWMwebman.ceas.uwm.edu/poster/sites/default/files/webform/FFWPoster... · SUSTAINABILITY ANALYSIS OF METAL ASSISTED CHEMICAL ETCHING OF

SUSTAINABILITY ANALYSIS OF METAL ASSISTED

CHEMICAL ETCHING OF SILICON NANOWIRESFenfen Wang, Chris Yingchun YuanDepartment of Mechanical Engineering, UWM

Understand the sustainability performance of metal assisted chemical etching

(MACE) of silicon nanowires (SiNWs) for lithium ion batteries (LIBs).

Research Object: MACE of Si wafer for synthesizing SiNWs

•Quantify material consumptions and establish material flows of the process

•Analyze both airborne and waterborne emissions involved in the process.

Specifically, gas and gaseous particle emissions were tested using in-situ

measurements and particle emissions (including size distributions, concentrations,

morphologies, material compositions) in solutions were characterized by applying ex-

situ measurements.

•Provide first-hand data and information support for future scale-up of MACE

method for SiNWs and support the sustainable development of this technology.

➢ Etching parameters: 20 mM AgNO3 and 0.3 M H2O2.

OBJECTIVES EXPERIMENTAL CHARACTERIZATION EXPERIMENTAL CHARACTERIZATION (Cont.)

➢ Metal assisted chemical etching (MACE) of SiNWs has disadvantage of low

productivity with high material consumptions including large amount of toxic

chemicals. For example, for 1 g of SiNWs 39.6 g of Si wafer and 854.9 g of HF are

consumed, which are both economical and environmental concerns.

➢ Gas emissions including H2 and NO and large amount of gaseous particle emissions

are produced during the etching process. Most of the gaseous particles are with

diameters less than 100 nm. What is more, particle emissions are also found in the

etching solutions, which exert serious environmental and human health impacts.

➢ Further work is needed to study the possibility for improving the sustainability

performance of MACE of SiNWs by increasing its productivity and reducing

wastes.

CONCLUSION

• [1] Li, M., Li, Y., Liu, W., Yue, L., Li, R., Luo, Y., Trevor, M., Jiang, B., Bai, F., Fu, P.,

Metal-assisted chemical etching for designable monocrystalline silicon nanostructure.

Materials Research Bulletin, 76, 436-449, 2016.

BIBLIOGRAPHY

• Fenfen Wang, Email: [email protected]

• Chris Yingchun Yuan, Email: [email protected]

CONTACT INFORMATIONACKNOWLEDGEMENT

• This study is financially supported by the National Science Foundation (CBET-3560)

➢ Sustainability issues about MACE method

• Nano-particle emissions

• Large amount of material consumptions including toxic chemicals

Introduction

➢ Etching mechanism of MACE for SiNWs formation [1]:

➢ Experimental process of MACE for synthesizing SiNWs

Ag nucleation Ag nanoparticle

SiSi

Ag+

e

Si

SiO2

SiF62-

F-

Si

Ag+

e

e

Si

HF+AgNO3 HF+H2O2

Experimental flow chart for synthesis of SiNWs

Silicon

wafer

Acetone

Ethanol

DI-H2O

10 min

Cleaning

N2 blowing

Drying

HF+AgNO3

1 min

Etching

HF+H2O2

60 min

Etching

Diluted HF

2 min

Etching

HNO3

60 min

Cleaning

Removing Ag particles

Rinsing

&DryingSiNWs

DI-H2O

Synthesis process

Material inputs

➢ Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) characterizations

➢ Waterborne particle emissions

• Morphologies and element compositions of particles in solutions were

tested by SEM and energy-dispersive X-ray spectroscopy (EDS)

Material consumptions for synthesizing

1 g of SiNWs

Input Materials Mass (g)

Si Wafer (etched) 39.6

Acetone 495.2

Ethanol 494.6

DI-H2O 11055.6

HF (48%) 854.9

AgNO3 4.5

H2O2 (30%) 177.4

HNO3 (70%) 158.1

Output Mass (g)

SiNWs 1

Ag nanoparticles involved in SiNWs

Ag nanoparticles

600 nm

Nanoparticle size distributions in etching solution

300 400 500 600 700

0

20

40

60

80

100

Inte

nsity

Diameter (nm)

G (d)

C (d)

➢ Gas emissions

• Gas emissions including H2 and NO were tested using residual gas analyzer (RGA)

0 1000 2000 3000 4000

0.0

1.0x10-5

2.0x10-5

3.0x10-5

H2

NO

0.0

2.0x10-8

4.0x10-8

6.0x10-8

8.0x10-8

1.0x10-7

1.2x10-7

1.4x10-7

1.6x10-7

1.8x10-7

Time (s)

Pre

ssu

re (

To

rr)

➢ Gaseous particle emissions during the etching process

• Concentrations and size distributions of gaseous particle emissions were tested by ultrafine

Condensation Particle Counter (UCPC) and Scanning Mobility Particle Sizer (SMPS)

0 50 100 150 200 250

0

1x103

2x103

3x103

4x103

5x103

6x103

Co

nce

ntr

atio

ns (

#/c

m3)

Time (s)

From HF + AgNO3

(a)

0 1000 2000 3000 4000

0.0

2.0x104

4.0x104

6.0x104

8.0x104

1.0x105

Co

nce

ntr

atio

ns (

#/c

m3)

Time (s)

From HF + H2O2

(b)

0 1000 2000 3000 4000

0

1x105

2x105

3x105

4x105

5x105

6x105

Co

nce

ntr

atio

ns (

#/c

m3)

Time (s)

From HNO3

(c)

100 200 300 4000%

1%

2%

3%

4%

5%

20 40 60 80 1000%

1%

2%

3%

4%

5%

Perc

enta

ge

Diameter (nm)

Pe

rce

nta

ge

Diameter (nm)

From HF + AgNO3

(a)

0 100 200 300 400 500 600 7000%

1%

2%

3%

20 40 60 80 1000%

1%

2%

3%

Diameter (nm)

Pe

rce

nta

ge

Pe

rce

nta

ge

Diameter (nm)

(b)

From HF + H2O2

100 200 300 400 500 600 7000%

10%

20%

30%

40%

50%

100 200 300 400 5000%

1x10-3%

2x10-3%

3x10-3%

4x10-3%

Diameter (nm)

Pe

rce

nta

ge

Pe

rce

nta

ge

Diameter (nm)

(c)

From HNO3

In HF+H2O2 solution

In HNO3 solution

In HF+AgNO3 solution

O Ag

100 mAgOCBSE

C

7 mO FCBSE Si

F O Si

C

FAgO

100 mF OCBSE Ag

C