JP2002519295A5 - - Google Patents
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- JP2002519295A5 JP2002519295A5 JP2000558027A JP2000558027A JP2002519295A5 JP 2002519295 A5 JP2002519295 A5 JP 2002519295A5 JP 2000558027 A JP2000558027 A JP 2000558027A JP 2000558027 A JP2000558027 A JP 2000558027A JP 2002519295 A5 JP2002519295 A5 JP 2002519295A5
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- 239000007789 gas Substances 0.000 description 45
- 239000000463 material Substances 0.000 description 20
- OZAIFHULBGXAKX-UHFFFAOYSA-N precursor Substances N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 7
- XYFCBTPGUUZFHI-UHFFFAOYSA-N phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 150000001340 alkali metals Chemical class 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- WMFOQBRAJBCJND-UHFFFAOYSA-M lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Inorganic materials [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- GQZXNSPRSGFJLY-UHFFFAOYSA-N Hypophosphorous acid Chemical compound OP=O GQZXNSPRSGFJLY-UHFFFAOYSA-N 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N N#B Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
Description
【特許請求の範囲】
【請求項１】 マイクロ波透過性で金属を含まずかつガス不浸透性で加圧された反応帯域を前駆体材料が通過する間に、マイクロ波放射と該前駆体材料との相互作用によってホスフィンガスを製造することを含む、高純度ホスフィンガスを生成する方法。
【請求項２】 前記前駆体材料は、水溶液中のＨ3ＰＯ2である、請求項１に記載の方法。
【請求項３】 前記前駆体材料は、水溶液中のＨ3ＰＯ3である、請求項１に記載の方法。
【請求項４】 前記前駆体材料は、結晶性Ｈ3ＰＯ2または結晶性Ｈ3ＰＯ3である、請求項１に記載の方法。
【請求項５】 前記前駆体材料は、水溶液中のＸＨ2ＰＯ2［式中、ＸはＬｉ、Ｎａ、及びＫからなるアルカリ金属群から選択される］の式を有する塩である、請求項１に記載の方法。
【請求項６】 前記前駆体材料は、水溶液中のＺ2（Ｈ2ＰＯ2）2［式中、ＺはＣａ、Ｍｇ、Ｓｒ、及びＢａからなるアルカリ金属群から選択される］の式を有する塩である、請求項１に記載の方法。
【請求項７】 前記前駆体材料は、水溶液中のＸＨ2ＰＯ3［式中、ＸはＬｉ、Ｎａ、及びＫからなるアルカリ金属群から選択される］の式を有する塩である、請求項１に記載の方法。
【請求項８】 前記前駆体材料は、アルカリ溶液中の赤リンのスラリーである、請求項１に記載の方法。
【請求項９】 前記アルカリ溶液は、水中に溶解したＮａＯＨ、ＫＯＨ、及びＬｉＯＨからなる群から選択されるかまたはこれらの組合せである、請求項８に記載の方法。
【請求項１０】 前記高純度ガスは１００ppmを超えない酸素または水蒸気を含む、請求項１に記載の方法。
【請求項１１】 マイクロ波放射の源と、マイクロ波透過性ガス気密バリアであって、該バリアを通して前記マイクロ波放射の源が向けられるバリアと、前記マイクロ波放射の源が向けられるマイクロ波反射性包囲体と、該包囲体から生成したガスを受け入れるのに適したガス供給用マニホルドと、前記生成したガスから溶媒蒸気を除去するのに適した溶媒蒸気除去装置と、前記生成したガス中のガス濃度を検知するためのガス濃度センサーと、前記包囲体内のガス生成速度を制御するためのフィードバック制御系と、で構成される、高純度ガス生成のための化学反応器系。
【請求項１２】 前記マイクロ波放射源は、周波数０．９GHzまたは２．４１〜１０GHzを有する、請求項１１に記載の系。
【請求項１３】 前記マイクロ波透過性バリアは、ポリテトラフルオロエチレン、溶融シリカ、二酸化ケイ素、窒化ホウ素、または黒鉛の群から選択される材料から構成される、請求項１１に記載の系。
【請求項１４】 前記マイクロ波反射性包囲体は、少なくとも１０-3ohm/cmの導電率を有する導電性材料から構成される、請求項１１に記載の系。
【請求項１５】 前記マイクロ波反射性包囲体は、マイクロ波放射の波長の少なくとも２倍の最小寸法を有する、請求項１１に記載の系。
【請求項１６】 前記ガスを生成するための前駆体材料も備え、該前駆体材料は、次亜リン酸と、ハイポホリック酸と、赤リンのアルカリ性スラリーとからなる群から選択される、請求項１１に記載の系。
【請求項１７】 前記蒸気除去装置はシリカゲルを含む、請求項１１に記載の系。
【請求項１８】 前記フィードバック制御系は、原料供給ポンプへのマイクロプロセッサ制御温度フィードバックループと、マイクロ波放射源用電源とを含む、請求項１１に記載の系。
【請求項１９】 前記フィードバック制御系は、前記マイクロ波放射源への電力を調節して、一定のガス供給圧力を維持する、請求項１１に記載の系。
【請求項２０】 前記フィードバック制御系は、前記マイクロ波放射源への電力を調節して、可変のガス流量を提供する、請求項１１に記載の系。
【請求項２１】 前記フィードバック制御系は、前記マイクロ波放射周波数を調節して、反応生成物の選択性を制御する、請求項１１に記載の系。
【請求項２２】 生成物ガス流中のホスフィン対希釈用ガスの比を測定するための濃度モニタと；
前記生成物ガス流中のホスフィンガスの現在の濃度対所望の濃度を決定するための、マイクロプロセッサを基にしたコンパレータと；
前記決定に基づいて生成した信号に応じて、前記生成物ガス流中への希釈用ガスの導入を制御するためのガスフローコントローラと；
を備える、ホスフィン生成物ガスのための濃度制御系。
【請求項２３】 前記ホスフィンガスは、マイクロ波放射の影響下での前駆体材料の反応によって生成される、請求項２２に記載の系。
【請求項２４】 半導体加工用の高純度ガスを生成するための方法であって、マイクロ波透過性で金属を含まずかつガス不浸透性で加圧された反応帯域を前駆体材料が通過する間に、マイクロ波放射と該前駆体材料との相互作用によって前記ガスを製造することを含む、方法。
【請求項２５】 ガスを使用して半導体デバイスを製造するための方法であって、マイクロ波放射の影響下での前駆体材料の反応によって前記ガスを製造した時に前記ガスを使用することを特徴とする、方法。
【請求項２６】 マイクロ波放射を照射されているマイクロ波透過性反応チャンバ内への前記前駆体材料の連続的な導入及び反応によって、前記ガスを連続的に製造することと；
前記製造されたガスを、形成されたままで半導体製造プロセスに連続的に供給することと；
を含む、請求項２５に記載の方法。
【請求項２７】 前記ガスは、製造されたままで化学気相成長法用反応装置または酸化炉に連続的に供給される、請求項２６に記載の方法。
【請求項２８】 前記前駆体材料は液体であり、前記反応は前記ガスを含む２相系を生成する、請求項２４〜２７のいずれか１項に記載の方法。
【請求項２９】 前記ガスはホスフィンである、請求項２４〜２８のいずれか１項に記載の方法。
【請求項３０】 マイクロ波透過性反応チャンバと該反応チャンバ内に向けられるマイクロ波放射の源とを有し、ガスを生成するためのガス生成用反応器と；
該ガス生成用反応器に連結した化学気相成長法用反応装置または酸化炉と；
を備える、半導体デバイスの製造のための装置。
【請求項３１】 前記ガスはホスフィンである、請求項３０に記載の装置。
【請求項３２】 半導体の製造のための高純度ガス生成のための化学反応器系であって：
マイクロ波放射の源と；
圧力下で前記ガスを生成するのに適し、前記ガスを生成するための前駆体材料を受け入れるための反応チャンバと；
マイクロ波透過性ガス気密バリアであって、該バリアを通して前記マイクロ波放射の源が前記反応チャンバに向けられるバリアと；
前記マイクロ波放射の源が向けられるマイクロ波反射性包囲体と；
生成したガスを受け入れるのに適したガス供給用マニホルドと；
前記生成したガスから溶媒蒸気を除去するのに適した溶媒蒸気除去デバイスと；
で構成される、化学反応器系。
【請求項３３】 前記反応チャンバに連結した前駆体材料の供給源も備える、請求項３２に記載の系。
【請求項３４】 前記生成したガス中のガス濃度を検知するためのガス濃度センサーと；
前記反応チャンバ内のガス生成速度を制御するためのフィードバック制御系と；
も備える、請求項３３に記載の系。
[Claims]
1. Interaction of microwave radiation with a precursor material during passage of the precursor material through a microwave permeable, metal free and gas impermeable, pressurized reaction zone. A method for producing high purity phosphine gas, comprising producing a gas.
2. The method of claim 1, wherein said precursor material is H 3 PO 2 in an aqueous solution.
3. The method of claim 1, wherein said precursor material is H 3 PO 3 in an aqueous solution.
4. The method of claim 1, wherein said precursor material is crystalline H 3 PO 2 or crystalline H 3 PO 3 .
5. The precursor material is a salt having the formula XH 2 PO 2 in an aqueous solution, wherein X is selected from the group of alkali metals consisting of Li, Na, and K. 2. The method according to 1.
6. The precursor material has a formula of Z 2 (H 2 PO 2 ) 2 in an aqueous solution, wherein Z is selected from an alkali metal group consisting of Ca, Mg, Sr, and Ba. The method according to claim 1, which is a salt having the compound.
7. The precursor material is a salt having the formula XH 2 PO 3 in an aqueous solution, wherein X is selected from the group of alkali metals consisting of Li, Na, and K. 2. The method according to 1.
8. The method of claim 1, wherein said precursor material is a slurry of red phosphorus in an alkaline solution.
9. The method of claim 8, wherein the alkaline solution is selected from the group consisting of NaOH, KOH, and LiOH dissolved in water, or a combination thereof.
10. The method of claim 1, wherein said high purity gas comprises no more than 100 ppm of oxygen or water vapor.
11. A microwave radiation source, a microwave transparent gas-tight barrier, a barrier that is directed source of the microwave radiation through the barrier, the microwave reflective said source of microwave radiation is directed An enclosure, a gas supply manifold suitable for receiving gas generated from the enclosure, a solvent vapor removal device suitable for removing solvent vapor from the generated gas, A chemical reactor system for producing high-purity gas, comprising: a gas concentration sensor for detecting gas concentration; and a feedback control system for controlling a gas production rate in the enclosure.
12. The system according to claim 11, wherein the microwave radiation source has a frequency of 0.9 GHz or 2.41 to 10 GHz.
13. The system of claim 11, wherein said microwave transparent barrier is comprised of a material selected from the group of polytetrafluoroethylene, fused silica, silicon dioxide, boron nitride, or graphite.
14. The system of claim 11, wherein said microwave reflective enclosure is comprised of a conductive material having a conductivity of at least 10-3 ohm / cm.
15. The system of claim 11, wherein said microwave reflective enclosure has a minimum dimension of at least twice the wavelength of microwave radiation.
16. The method according to claim 16, further comprising a precursor material for producing the gas, wherein the precursor material is selected from the group consisting of hypophosphorous acid, hypophoric acid, and an alkaline slurry of red phosphorus. Item 12. The system according to Item 11.
17. The system of claim 11, wherein said vapor removal device comprises silica gel.
18. The system of claim 11, wherein the feedback control system includes a microprocessor controlled temperature feedback loop to a feed pump and a power source for a microwave radiation source.
19. The system of claim 11, wherein the feedback control system regulates power to the microwave radiation source to maintain a constant gas supply pressure.
20. The system of claim 11, wherein the feedback control system adjusts power to the microwave radiation source to provide a variable gas flow.
21. The system of claim 11, wherein said feedback control system adjusts said microwave radiation frequency to control the selectivity of a reaction product.
22. A concentration monitor for measuring the ratio of phosphine to diluent gas in the product gas stream;
A microprocessor-based comparator for determining a current concentration of the phosphine gas in the product gas stream versus a desired concentration;
A gas flow controller for controlling introduction of a diluting gas into the product gas stream in response to a signal generated based on the determination;
A concentration control system for a phosphine product gas, comprising:
23. The system of claim 22, wherein said phosphine gas is generated by reaction of a precursor material under the influence of microwave radiation.
24. A method for producing a high-purity gas for semiconductor processing, wherein a precursor material passes through a microwave-permeable, metal-free, gas-impermeable, pressurized reaction zone. In the meantime, a method comprising producing the gas by interaction of microwave radiation with the precursor material.
25. A method for manufacturing a semiconductor device using a gas, the method comprising using the gas when the gas is manufactured by reacting a precursor material under the influence of microwave radiation. And the way.
26. continuously producing said gas by continuous introduction and reaction of said precursor material into a microwave permeable reaction chamber being irradiated with microwave radiation;
Continuously supplying the produced gas to a semiconductor production process as formed;
26. The method of claim 25, comprising:
27. The method of claim 26, wherein the gas is continuously supplied as produced to a chemical vapor deposition reactor or an oxidation furnace.
28. The method according to claim 24, wherein the precursor material is a liquid and the reaction produces a two-phase system comprising the gas.
29. The method according to claim 24, wherein the gas is phosphine.
30. A gas producing reactor having a microwave permeable reaction chamber and a source of microwave radiation directed into the reaction chamber for producing a gas;
A reactor for chemical vapor deposition or an oxidation furnace connected to the reactor for gas generation;
An apparatus for manufacturing a semiconductor device, comprising:
31. The apparatus of claim 30, wherein said gas is phosphine.
32. A chemical reactor system for producing high-purity gas for semiconductor production, comprising:
A source of microwave radiation;
A reaction chamber suitable for producing the gas under pressure and for receiving a precursor material for producing the gas;
A microwave permeable gas tight barrier through which the source of microwave radiation is directed to the reaction chamber;
A microwave reflective enclosure to which the source of microwave radiation is directed ;
A gas supply manifold suitable for receiving the generated gas;
A solvent vapor removal device suitable for removing solvent vapor from the produced gas;
A chemical reactor system composed of
33. The system of claim 32, further comprising a source of precursor material coupled to said reaction chamber.
34. A gas concentration sensor for detecting a gas concentration in the generated gas;
A feedback control system for controlling a gas generation rate in the reaction chamber;
34. The system of claim 33, further comprising:
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US9173798P | 1998-07-06 | 1998-07-06 | |
| US60/091,737 | 1998-07-06 | ||
| PCT/US1999/015181 WO2000001615A1 (en) | 1998-07-06 | 1999-07-06 | Method and apparatus for the preparation of high purity phosphine or other gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2002519295A JP2002519295A (en) | 2002-07-02 |
| JP2002519295A5 true JP2002519295A5 (en) | 2006-11-02 |
Family
ID=22229425
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000558027A Pending JP2002519295A (en) | 1998-07-06 | 1999-07-06 | Method and apparatus for producing high purity phosphine or other gas |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP2002519295A (en) |
| CN (1) | CN100374365C (en) |
| WO (1) | WO2000001615A1 (en) |
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|---|---|---|---|---|
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| CN108773838A (en) * | 2018-08-15 | 2018-11-09 | 马杰 | A kind of preparation method and its preparation facilities of phosphine |
| CN113161535B (en) * | 2021-03-30 | 2022-10-25 | 华南理工大学 | Method and material for improving discharge specific capacity and cycling stability of lithium-rich cathode material through gas-phase surface phosphating treatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5474659A (en) * | 1989-04-18 | 1995-12-12 | At&T Corp. | Process and apparatus for generating precursor gases used in the manufacture of semiconductor devices |
| JPH0659293B2 (en) * | 1990-04-27 | 1994-08-10 | 川崎重工業株式会社 | Medical waste treatment method and device |
| US5158656A (en) * | 1991-03-22 | 1992-10-27 | Electron Transfer Technologies, Inc. | Method and apparatus for the electrolytic preparation of group IV and V hydrides |
| CA2137074A1 (en) * | 1992-06-05 | 1993-12-23 | Colin J. Waterford | Formulations, method and apparatus for the controlled generation of phosphine |
| US5480947A (en) * | 1993-02-24 | 1996-01-02 | Mitsui Toatsu Chemicals, Inc. | Diguanamines and preparation process, derivatives and use thereof |
| US5451302A (en) * | 1994-05-03 | 1995-09-19 | Cha; Chang Y. | Process for microwave catalysis of chemical reactions using waveguide liquid films |
| JP3889813B2 (en) * | 1995-12-06 | 2007-03-07 | エレクトロン・トランスファー・テクノロジーズ・インコーポレーテッド | Method and apparatus for supplying hydride gas for semiconductor processing with a constant composition |
| US5951831A (en) * | 1997-07-11 | 1999-09-14 | Albright & Wilson Americas Limited | Condensation polymerization of phosphorus containing compounds |
-
1999
- 1999-07-06 CN CNB998101699A patent/CN100374365C/en not_active Expired - Fee Related
- 1999-07-06 JP JP2000558027A patent/JP2002519295A/en active Pending
- 1999-07-06 WO PCT/US1999/015181 patent/WO2000001615A1/en active Application Filing
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