IP Library Granted Patent US 9,238,861
Granted Patent B2
US 9,238,861 · App. 13/467,789 · Granted Jan 19, 2016

Closed-space annealing process for production of CIGS thin-films

Inventors: Mariana Rodica Munteanu (Santa Clara, CA); Amith Kumar Murali (Fremont, CA); Brian Josef Bartholomeusz (Palo Alto, CA); Vardaan Chawla (Mountain View, CA)
Assignee: ZETTA RESEARCH AND DEVELOPMENT LLC—AQT SERIES
C23C14/0623C23C14/24C23C14/562H01L21/0256H01L21/02422H01L21/02557H01L21/02568H01L21/02614H01L31/0322Y02E10/541
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Quick Facts
Patent No.
US 9,238,861
App. No.
13/467,789
Granted
Jan 19, 2016
Kind
B2
Abstract

In one embodiment, a method includes depositing a CIGS precursor layer onto a substrate, introducing a source-material layer into proximity with the precursor layer, where the source-material layer includes one or more of Cu, In, or Ga, and one or more of S or Se, and annealing the precursor layer in proximity with of the source-material layer, where the annealing is performed in a constrained volume, and where the presence of the source-material layer reduces decomposition of volatile species from the precursor layer during annealing.

Claims (36)

1. A method comprising:

depositing a precursor layer onto a substrate, the precursor layer comprising a first layer comprising Cu, a second layer comprising one or more of In or Ga, and a third layer comprising one or more of S or Se;

introducing a source-material layer into proximity with the precursor layer, the source-material layer comprising one or more of Cu, In, or Ga, and one or more of S or Se; and

annealing the precursor layer in proximity with the source-material layer,

wherein the annealing is performed in a constrained volume,

wherein the presence of the source-material layer reduces decomposition of the volatile species from the precursor layer during annealing, and

wherein the precursor layer comprises approximately 5-50 atomic % Cu, approximately 5-50 atomic % In and Ga combined, and 5-50 atomic % S and Se combined.

2. The method of claim 1 , wherein the substrate comprises glass.

3. The method of claim 1 , wherein the precursor layer comprises Culn y Ga (1-y) (S z Se 1-z ) 2 , where y and z approximately satisfy 0≦y≦1, and 0≦z≦1.

4. The method of claim 1 , wherein the source-material layer comprises approximately 30-70 atomic % In and Ga combined, and approximately 30-70 atomic % S and Se combined.

5. The method of claim 1 , wherein the source-material layer comprises approximately 30-70 atomic % In and Ga combined, approximately 30-70 atomic % S, and approximately 30-70 atomic % Se.

6. The method of claim 1 , wherein the source-material layer comprises In 2 S 3 , In 2 Se 3 , Ga 2 S 3 , Ga 2 Se 3 , CuS, CuS 2 , CuSe, CuSe 2 , or any combination thereof.

7. The method of claim 1 , wherein the source-material layer evaporates or sublimes during the annealing to form gaseous sulfur, gaseous sulfur compounds, gaseous selenium, gaseous selenium compounds, or any combination thereof.

8. The method of claim 1 , wherein the precursor layer further comprises approximately less than or equal to 10 atomic % of Na, Sb, Bi, or any combination thereof.

9. The method of claim 1 , wherein the source-material layer further comprises approximately less than or equal to 10 atomic % of Li, Na, K, Rb, Cs, or any combination thereof.

10. The method of claim 1 , wherein In or Ga in the precursor layer is substituted in whole or in part with Al, Ag, or any combination thereof.

11. A method comprising:

depositing a precursor layer onto a substrate, the precursor layer comprising a first layer comprising Cu, a second layer comprising one or more of In or Ga, and a third layer comprising one or more of S or Se;

introducing a source-material layer into proximity with the precursor layer, the source-material layer comprising one or more of Cu, In, or Ga, and one or more of S or Se; and

annealing the precursor layer in proximity with the source-material layer,

wherein the annealing is performed in a constrained volume, and wherein the presence of the source-material layer reduces decomposition of the volatile species from the precursor layer during annealing, and

wherein the precursor layer comprises Cu x (In y Ga (1-y) ) α (S z Se 1-z ) β , where x, y, z, α and β approximately satisfy 0.1≦x≦0.7, 0≦y≦1, 0≦z≦1, 0.3≦α≦0.8, and β=1.

12. The method of claim 11 , wherein the precursor layer further comprises nanoparticles comprising Cu, one or more of In or Ga, and one or more of S or Se.

13. A method comprising:

depositing a precursor layer onto a substrate, the precursor layer comprising Cu, one or more of In or Ga, and one or more of S or Se;

introducing a source-material layer into proximity with the precursor layer, the source-material layer comprising one or more of Cu, In, or Ga, and one or more of S or Se; and

annealing the precursor layer in proximity with the source-material layer,

wherein the annealing is performed in a constrained volume, and wherein the presence of the source-material layer reduces decomposition of the volatile species from the precursor layer during annealing, and

wherein the precursor layer includes:

a first layer comprising (In y Ga (1-y) ) α Se z or (In y Ga (1-y) ) α S z , and where y, z and α appoximately satisfy 0≦y≦1, 0.5≦z≦1, and 0.05≦α≦1,

a second layer comprising Cu 2-x Se z , Cu 2-x S z , or any combination thereof, where x and z approximately satisfy 0≦x≦1.6, and z=1, and

a third layer comprising Cu x (In y Ga (1-y) ) α (S z Se 1-z ) β , and where x, y, z, α and β approximately satisfy 0.01≦x≦0.07, 0≦y≦1, 0≦z≦1, 0.3 ≦α≦0.08, and β=1.

14. The method of claim 13 , wherein the precursor layer further comprises Culn y Ga (1-y) (S z Se 1-z ) 2 , where y and z approximately satisfy 0≦y≦1, and 0≦z≦1.

15. The method of claim 13 , wherein the precursor layer further comprises nanoparticles comprising Cu, one or more of In or Ga, and one or more of S or Se.

16. The method of claim 13 , wherein the source-material layer comprises at least one of approximately 30-70 atomic % In and Ga combined, approximately 30-70 atomic % S, and approximately 30-70 atomic % Se, or the source-material layer comprises In 2 S 3 , In 2 Se 3 , Ga 2 S 3 , Ga 2 Se 3 , CuS, CUS 2 , CuSe, CuSe 2 , or any combination thereof.

17. The method of claim 13 , wherein the source-material layer evaporates or sublimes during the annealing to form gaseous sulfur, gaseous sulfur compounds, gaseous selenium, gaseous selenium compounds, or any combination thereof.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 17, 2013
From: AQT SOLAR, INC.
To: SWANSON, JOHN A.
Reel/Frame 029650/0366 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 17, 2013
From: SWANSON, JOHN A.
To: ZETTA RESEARCH AND DEVELOPMENT LLC - AQT SERIES
Reel/Frame 029650/0500 →
CORRECTIVE ASSIGNMENT TO CORRECT THE NAME OF INVENTOR BRIAN JOSEF BARTHOLOMEUSZ; INCORRECTLY IDENTIFIED AS BRAIN JOSEF BARTHOLOMEUSZ PREVIOUSLY RECORDED ON REEL 028183 FRAME 0434. ASSIGNOR(S) HEREBY CONFIRMS THE ENTIRE RIGHT OF INVENTION TO AQT SOLAR, INC. Recorded Jun 6, 2012
From: MUNTEANU, MARIANA RODICA; MURALI, AMITH KUMAR; BARTHOLOMEUSZ, BRIAN JOSEF; CHAWLA, VARDAAN
To: AQT SOLAR, INC.
Reel/Frame 028326/0666 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 9, 2012
From: MUNTEANU, MARIANA RODICA; MURALI, AMITH KUMAR; BARTHOLOMEUSZ, BRAIN JOSEF; CHAWLA, VARDAAN
To: AQT SOLAR, INC.
Reel/Frame 028183/0434 →
Continuity (3)
Continuation In Part 13401512 · Feb 21, 2012
Continuation In Part 13401558 · Feb 21, 2012
Related Publication 20130217214A1 · Aug 22, 2013