JPWO2021105095A5 - - Google Patents
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- JPWO2021105095A5 JPWO2021105095A5 JP2022529919A JP2022529919A JPWO2021105095A5 JP WO2021105095 A5 JPWO2021105095 A5 JP WO2021105095A5 JP 2022529919 A JP2022529919 A JP 2022529919A JP 2022529919 A JP2022529919 A JP 2022529919A JP WO2021105095 A5 JPWO2021105095 A5 JP WO2021105095A5
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- Prior art keywords
- approximately
- oxygen
- ruthenium
- carried out
- containing layer
- Prior art date
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- 238000000034 method Methods 0.000 claims description 68
- 239000002243 precursor Substances 0.000 claims description 36
- 239000000376 reactant Substances 0.000 claims description 21
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 17
- 229910052707 ruthenium Inorganic materials 0.000 claims description 17
- 238000010926 purge Methods 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001882 dioxygen Inorganic materials 0.000 claims description 3
- 239000001272 nitrous oxide Substances 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- 150000003973 alkyl amines Chemical class 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229910001868 water Inorganic materials 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims 1
- 150000001350 alkyl halides Chemical class 0.000 claims 1
- -1 cyclic alkyl halides Chemical class 0.000 description 1
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 1
Description
本発明を、或る程度の詳細さをもって記載及び例示したが、この開示は例示として行ったものに過ぎないこと、及び各ステップの条件及び順番の数々の変化は、本発明の趣旨及び範囲から逸脱することなく、当業者によって採用できることが理解される。
本願は特許請求の範囲に記載の発明に係るものであるが、本願の開示は以下も包含する:
1. 次式I:
R
1、
R
2
、R
3
及びR
4
は、それぞれ独立して、置換されたもしくは置換されていないC
1
~C
20
線状もしくは分岐状もしくは環状アルキル、及び置換されたもしくは置換されていないC
1
~C
20
線状もしくは分岐状もしくは環状ハロゲン化アルキルの群から選択され;
nは2または3である]
で表され、但し、好ましくは、水、金属イオンまたは金属、及び有機不純物を実質的に含まない、ルテニウムを含むALDまたはALD類似前駆体。
2. R
1、
R
2
、R
3
及びR
4
が、それぞれ独立して、-CH
3
、-CH
2
CH
3
、-CH
2
CH
2
CH
3
、-CH(CH3)
2
、-CH
2
CH(CH
3
)
2
、-C(CH
3
)
3
、-CF
3
、-CF
2
CF
3
、-CF
2
CF
2
CF
3
、-CF(CF
3
)
2
、-C(CF
3
)
3
のうちの一つである、前記1.に記載の前駆体。
3. R
1
、R
2
、R
3
及びR
4
のうちの少なくとも一つが、置換されたもしくは置換されていないC
1
~C
8
パーフルオロアルキルである、前記1.に記載の前駆体。
4. nが2である、前記1.に記載の前駆体。
5. nが3である、前記1.に記載の前駆体。
6. R
1
、R
2
、R
3
及びR
4
がそれぞれ同じ基である、前記1.に記載の前駆体。
7. R
1
及びR
4
、またはR
2
及びR
3
がそれぞれ同じ基である、前記1.に記載の前駆体。
8. 次の構造を有する、前記1.に記載の前駆体。
14. 前記表面が、Al
2
O
3
、ZrO
2
、HfO
2
、SiO
2
、WN、WCN、TiN、Cu、Co、Mo、W及びこれらの組み合わせのうちの少なくとも一つを含む、前記13.に記載の方法。
15. おおよそ300℃未満の温度で行われる、前記13.に記載の方法。
16. おおよそ275℃未満の温度で行われる、前記13.に記載の方法。
17. おおよそ250℃未満の温度で行われる、前記13.に記載の方法。
18. おおよそ200℃からおおよそ300℃までの範囲の温度で行われる、前記13.に記載の方法。
19. おおよそ235℃からおおよそ300℃までの範囲の温度で行われる、前記13.に記載の方法。
20. 共反応体の使用を更に含む、前記13.に記載の方法。
21. 酸素不含共反応体の使用を更に含む、前記13.に記載の方法。
22. 酸素含有共反応体の使用を更に含む、前記13.に記載の方法。
23. 共反応体としてのH
2
の使用を更に含む、前記13.に記載の方法。
24. 共反応体としてのO
2
の使用を更に含む、前記13.に記載の方法。
25. おおよそ0.01トルとおおよそ20トルとの間の圧力で行われる、前記13.に記載の方法。
26. おおよそ1トルとおおよそ15トルとの間の圧力で行われる、前記13.に記載の方法。
27. おおよそ5トルとおおよそ15トルとの間の圧力で行われる、前記13.に記載の方法。
28. おおよそ5トルとおおよそ10トルとの間の圧力で行われる、前記13.に記載の方法。
29. おおよそ5トルの圧力で行われる、前記13.に記載の方法。
30. おおよそ10トルの圧力で行われる、前記13.に記載の方法。
31. おおよそ15トルの圧力で行われる、前記13.に記載の方法。
32. おおよそ1秒間からおおよそ15秒間までの前駆体パルス時間を用いて行われる、前記13.に記載の方法。
33. おおよそ5秒間からおおよそ10秒間までの前駆体パルス時間を用いて行われる、前記13.に記載の方法。
34. おおよそ10秒間の前駆体パルス時間を用いて行われる、前記13.に記載の方法。
35. おおよそ15秒間の前駆体パルス時間を用いて行われる、前記13.に記載の方法。
36. おおよそ1秒間からおおよそ20秒間までの前駆体パージ時間を用いて行われる、前記13.に記載の方法。
37. おおよそ5秒間からおおよそ15秒間までの前駆体パージ時間を用いて行われる、前記13.に記載の方法。
38. おおよそ10秒間からおおよそ15秒間の前駆体パージ時間を用いて行われる、前記13.に記載の方法。
39. おおよそ10秒間の前駆体パージ時間を用いて行われる、前記13.に記載の方法。
40. おおよそ15秒間の前駆体パージ時間を用いて行われる、前記13.に記載の方法。
41. おおよそ1秒間からおおよそ60秒間までの共反応体パルス時間を用いて行われる、前記13.に記載の方法。
42. おおよそ10秒間からおおよそ50秒間までの共反応体パルス時間を用いて行われる、前記13.に記載の方法。
43. おおよそ20秒間からおおよそ40秒間までの共反応体パルス時間を用いて行われる、前記13.に記載の方法。
44. おおよそ30秒間からおおよそ40秒間までの共反応体パルス時間を用いて行われる、前記13.に記載の方法。
45. おおよそ30秒間の共反応体パルス時間を用いて行われる、前記13.に記載の方法。
46. おおよそ40秒間の共反応体パルス時間を用いて行われる、前記13.に記載の方法。
47. おおよそ50秒間の共反応体パルス時間を用いて行われる、前記13.に記載の方法。
48. おおよそ1秒間からおおよそ90秒間までの共反応体パージ時間を用いて行われる、前記13.に記載の方法。
49. おおよそ10秒間からおおよそ80秒間までの共反応体パージ時間を用いて行われる、前記13.に記載の方法。
50. おおよそ20秒間からおおよそ70秒間までの共反応体パージ時間を用いて行われる、前記13.に記載の方法。
51. おおよそ30秒間からおおよそ60秒間までの共反応体パージ時間を用いて行われる、前記13.に記載の方法。
52. おおよそ50秒間の共反応体パージ時間を用いて行われる、前記13.に記載の方法。
53. おおよそ60秒間の共反応体パージ時間を用いて行われる、前記13.に記載の方法。
54. おおよそ70秒間の共反応体パージ時間を用いて行われる、前記13.に記載の方法。
55. 前記1.~12.のいずれか一つに記載の前駆体と少なくとも一種の酸素不含共反応体との反応生成物を含む、ALDまたはALD類似堆積膜。
56. 前記酸素不含共反応体が水素を含む、前記55.に記載のALDまたはALD類似堆積膜。
57. 前記酸素不含共反応体が窒素含有共反応体を含む、前記55.に記載のALDまたはALD類似堆積膜。
58. 前記酸素不含共反応体が、アンモニア、ヒドラジン、アルキルヒドラジン及びアルキルアミンのうちの一種以上を含む、前記55.に記載のALDまたはALD類似堆積膜。
59. 前記1.~12.のいずれか一つに記載の前駆体と少なくとも一種の酸素含有共反応体との反応生成物を含む、ALDまたはALD類似堆積膜。
60. 前記酸素含有共反応体が、酸素、過酸化水素及び亜酸化窒素のうちの一種以上を含む、前記59.に記載のALDまたはALD類似堆積膜。
61. 前記酸素含有共反応体が、オゾン、元素状酸素及び分子状酸素/O
2
のうちの一種以上を含む、前記59.に記載のALDまたはALD類似堆積膜。
62. 前記酸素含有共反応体がO
2
を含む、前記59.に記載のALDまたはALD類似堆積膜。
63. 前記13.に記載の方法であって、
(i)おおよそ245℃の温度で;
(ii)おおよそ10トルの圧力で;
(iii)おおよそ10秒間の前駆体パルス時間を用いて;
(iv)おおよそ15秒間の前駆体パージ時間を用いて;
(v)おおよそ40秒間の共反応体パルス時間を用いて;及び
(vi)おおよそ60秒間の共反応体パージ時間を用いて;
行われる、前記方法。
64. 前記共反応体がH
2
である、前記63.に記載の方法。
65. ALDまたはALD類似方法における、前記1~.12.のいずれか一つに記載の前駆体の使用。
Although the invention has been described and illustrated in some detail, it is understood that this disclosure is made by way of example only, and that numerous variations in the conditions and order of steps may be construed as departing from the spirit and scope of the invention. It is understood that it may be adopted by those skilled in the art without departing from this.
Although this application relates to the invention described in the claims, the disclosure of this application also includes the following:
1. Formula I:
R 1 , R 2 , R 3 and R 4 are each independently substituted or unsubstituted C 1 -C 20 linear or branched or cyclic alkyl, and substituted or unsubstituted C selected from the group of 1 to C20 linear or branched or cyclic alkyl halides;
n is 2 or 3]
ALD or ALD-like precursor containing ruthenium, preferably substantially free of water, metal ions or metals, and organic impurities.
2. R 1 , R 2 , R 3 and R 4 are each independently -CH 3 , -CH 2 CH 3 , -CH 2 CH 2 CH 3 , -CH(CH3) 2 , -CH 2 CH ( CH 3 ) 2 , -C(CH 3 ) 3 , -CF 3 , -CF 2 CF 3 , -CF 2 CF 2 CF 3 , -CF(CF 3 ) 2 , -C(CF 3 ) 3 Yes, above 1. Precursors described in.
3. 1. wherein at least one of R 1 , R 2 , R 3 and R 4 is substituted or unsubstituted C 1 -C 8 perfluoroalkyl; Precursors described in.
4. 1. above, where n is 2; Precursors described in.
5. 1. above, where n is 3; Precursors described in.
6. 1. above, wherein R 1 , R 2 , R 3 and R 4 are each the same group; Precursors described in.
7. 1. above, wherein R 1 and R 4 or R 2 and R 3 are each the same group; Precursors described in.
8. Said 1. having the following structure. Precursors described in.
14. 13. wherein the surface comprises at least one of Al 2 O 3 , ZrO 2 , HfO 2 , SiO 2 , WN, WCN, TiN, Cu, Co, Mo, W, and combinations thereof. The method described in.
15. 13 above, carried out at a temperature of approximately less than 300°C. The method described in.
16. 13 above, carried out at a temperature of approximately less than 275°C. The method described in.
17. 13 above, carried out at a temperature of approximately less than 250°C. The method described in.
18. 13 above, carried out at a temperature ranging from approximately 200°C to approximately 300°C. The method described in.
19. 13 above, carried out at a temperature ranging from approximately 235°C to approximately 300°C. The method described in.
20. 13 above, further comprising the use of a co-reactant. The method described in.
21. 13 above, further comprising the use of an oxygen-free co-reactant. The method described in.
22. 13 above, further comprising the use of an oxygen-containing co-reactant. The method described in.
23. 13 above, further comprising the use of H2 as a co-reactant . The method described in.
24. 13 above, further comprising the use of O2 as a coreactant . The method described in.
25. 13. conducted at a pressure between approximately 0.01 Torr and approximately 20 Torr. The method described in.
26. 13. carried out at a pressure between approximately 1 Torr and approximately 15 Torr. The method described in.
27. 13. conducted at a pressure between approximately 5 Torr and approximately 15 Torr. The method described in.
28. 13. carried out at a pressure between approximately 5 Torr and approximately 10 Torr. The method described in.
29. 13 above, carried out at a pressure of approximately 5 Torr. The method described in.
30. 13 above, carried out at a pressure of approximately 10 Torr. The method described in.
31. 13 above, carried out at a pressure of approximately 15 Torr. The method described in.
32. 13. carried out using a precursor pulse time of approximately 1 second to approximately 15 seconds. The method described in.
33. 13. is carried out using a precursor pulse time of approximately 5 seconds to approximately 10 seconds. The method described in.
34. 13. carried out using a precursor pulse time of approximately 10 seconds. The method described in.
35. 13. carried out using a precursor pulse time of approximately 15 seconds. The method described in.
36. 13. conducted using a precursor purge time of approximately 1 second to approximately 20 seconds. The method described in.
37. 13. is carried out using a precursor purge time of approximately 5 seconds to approximately 15 seconds. The method described in.
38. 13. is carried out using a precursor purge time of approximately 10 seconds to approximately 15 seconds. The method described in.
39. 13 above, performed using a precursor purge time of approximately 10 seconds. The method described in.
40. 13. is performed using a precursor purge time of approximately 15 seconds. The method described in.
41. 13. carried out using a coreactant pulse time of approximately 1 second to approximately 60 seconds. The method described in.
42. 13. carried out using a coreactant pulse time of approximately 10 seconds to approximately 50 seconds. The method described in.
43. 13. carried out using a coreactant pulse time of approximately 20 seconds to approximately 40 seconds. The method described in.
44. 13. conducted using coreactant pulse times of approximately 30 seconds to approximately 40 seconds. The method described in.
45. 13. carried out using a coreactant pulse time of approximately 30 seconds. The method described in.
46. 13. carried out using a coreactant pulse time of approximately 40 seconds. The method described in.
47. 13. carried out using a coreactant pulse time of approximately 50 seconds. The method described in.
48. 13. conducted using a co-reactant purge time of approximately 1 second to approximately 90 seconds. The method described in.
49. 13. conducted using a co-reactant purge time of approximately 10 seconds to approximately 80 seconds. The method described in.
50. 13. is carried out using a co-reactant purge time of approximately 20 seconds to approximately 70 seconds. The method described in.
51. 13. is carried out using a co-reactant purge time of approximately 30 seconds to approximately 60 seconds. The method described in.
52. 13 above, performed using a coreactant purge time of approximately 50 seconds. The method described in.
53. 13 above, performed using a coreactant purge time of approximately 60 seconds. The method described in.
54. 13. is carried out using a coreactant purge time of approximately 70 seconds. The method described in.
55. Said 1. ~12. An ALD or ALD-like deposited film comprising a reaction product of a precursor according to any one of the preceding claims and at least one oxygen-free co-reactant.
56. 55 above, wherein said oxygen-free coreactant comprises hydrogen. ALD or ALD-like deposited film as described in .
57. 55 above, wherein said oxygen-free coreactant comprises a nitrogen-containing coreactant. ALD or ALD-like deposited film as described in .
58. 55 above, wherein the oxygen-free co-reactant comprises one or more of ammonia, hydrazine, alkylhydrazine and alkylamine. ALD or ALD-like deposited film as described in .
59. Said 1. ~12. An ALD or ALD-like deposited film comprising a reaction product of a precursor according to any one of the preceding paragraphs and at least one oxygen-containing co-reactant.
60. 59 above, wherein the oxygen-containing co-reactant comprises one or more of oxygen, hydrogen peroxide and nitrous oxide. ALD or ALD-like deposited film as described in .
61. 59 above, wherein the oxygen-containing co-reactant comprises one or more of ozone, elemental oxygen and molecular oxygen/ O2 . ALD or ALD-like deposited film as described in .
62. 59. above, wherein said oxygen-containing co-reactant comprises O2 . ALD or ALD-like deposited film as described in .
63. 13 above. The method described in
(i) at a temperature of approximately 245°C;
(ii) at a pressure of approximately 10 Torr;
(iii) using a precursor pulse time of approximately 10 seconds;
(iv) using a precursor purge time of approximately 15 seconds;
(v) using a coreactant pulse time of approximately 40 seconds; and
(vi) with a coreactant purge time of approximately 60 seconds;
Said method is carried out.
64. 63. above, wherein the co-reactant is H2 . The method described in.
65. In ALD or an ALD-like method, 1 to . 12. Use of a precursor according to any one of the following.
Claims (31)
(i) 前記基材の表面を前駆体に曝すステップであって、前記前駆体が、次式I:
R1、R2、R3及びR4は、それぞれ独立して、置換されたもしくは置換されていないC1~C20線状もしくは分岐状アルキル、及び置換されたもしくは置換されていないC1~C20線状もしくは分岐状ハロゲン化アルキルの群から選択され;
nは2または3である]
で表され、但し、水、金属イオンまたは金属、及び有機不純物を実質的に含まない、ルテニウムを含むALDまたはALD類似前駆体である、ステップ、
(ii) その後、前記基材の表面を一種以上の共反応体に曝すステップ、
を含み、おおよそ200℃からおおよそ300℃未満までの範囲の温度で行われる、前記方法。 An ALD or ALD-like method for depositing a ruthenium-containing layer on a substrate, the method comprising:
(i) exposing the surface of the substrate to a precursor, the precursor having the following formula I:
R 1 , R 2 , R 3 and R 4 are each independently substituted or unsubstituted C 1 -C 20 linear or branched alkyl , and substituted or unsubstituted C 1 selected from the group of ~ C20 linear or branched alkyl halides ;
n is 2 or 3]
is an ALD or ALD-like precursor containing ruthenium, substantially free of water , metal ions or metals, and organic impurities,
(ii) thereafter exposing the surface of said substrate to one or more co-reactants;
and carried out at a temperature ranging from about 200<0>C to less than about 300<0>C.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201962940524P | 2019-11-26 | 2019-11-26 | |
US62/940,524 | 2019-11-26 | ||
PCT/EP2020/083152 WO2021105095A1 (en) | 2019-11-26 | 2020-11-24 | Ruthenium pyrazolate precursor for atomic layer deposition and similar processes |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2023502764A JP2023502764A (en) | 2023-01-25 |
JPWO2021105095A5 true JPWO2021105095A5 (en) | 2023-11-21 |
Family
ID=73598078
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JP2022529919A Pending JP2023502764A (en) | 2019-11-26 | 2020-11-24 | Ruthenium pyrazolate precursors and similar methods for atomic layer deposition |
Country Status (8)
Country | Link |
---|---|
US (1) | US20220341039A1 (en) |
EP (1) | EP4065743A1 (en) |
JP (1) | JP2023502764A (en) |
KR (1) | KR20220104805A (en) |
CN (1) | CN114667367A (en) |
IL (1) | IL293077A (en) |
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US20110198756A1 (en) * | 2005-11-28 | 2011-08-18 | Thenappan Ue | Organometallic Precursors and Related Intermediates for Deposition Processes, Their Production and Methods of Use |
TWI425110B (en) * | 2007-07-24 | 2014-02-01 | Sigma Aldrich Co | Methods of forming thin metal-containing films by chemical phase deposition |
TW200951241A (en) * | 2008-05-30 | 2009-12-16 | Sigma Aldrich Co | Methods of forming ruthenium-containing films by atomic layer deposition |
JP2013530304A (en) * | 2010-04-19 | 2013-07-25 | レール・リキード−ソシエテ・アノニム・プール・レテュード・エ・レクスプロワタシオン・デ・プロセデ・ジョルジュ・クロード | Ruthenium-containing precursors for CVD and ALD |
WO2013117955A1 (en) * | 2012-02-07 | 2013-08-15 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method for the deposition of a ruthenium containing film using arene diazadiene ruthenium(0) precursors |
WO2017009948A1 (en) * | 2015-07-14 | 2017-01-19 | リサーチ コーオペレーション ファウンデーション オブ ヨンナム ユニバーシティ | Method for forming ruthenium thin film by atomic layer deposition |
KR102638657B1 (en) * | 2016-11-08 | 2024-02-19 | 메르크 파텐트 게엠베하 | Metal complexes containing cyclopentadienyl ligands |
TWI790320B (en) * | 2017-12-16 | 2023-01-21 | 美商應用材料股份有限公司 | Selective atomic layer deposition of ruthenium |
US11976352B2 (en) * | 2018-02-12 | 2024-05-07 | Merck Patent Gmbh | Methods of vapor deposition of ruthenium using an oxygen-free co-reactant |
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