JP6906220B2 - Processing method - Google Patents
Processing method Download PDFInfo
- Publication number
- JP6906220B2 JP6906220B2 JP2017036359A JP2017036359A JP6906220B2 JP 6906220 B2 JP6906220 B2 JP 6906220B2 JP 2017036359 A JP2017036359 A JP 2017036359A JP 2017036359 A JP2017036359 A JP 2017036359A JP 6906220 B2 JP6906220 B2 JP 6906220B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- treatment
- raw material
- processing apparatus
- mist
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000003672 processing method Methods 0.000 title claims description 8
- 239000000758 substrate Substances 0.000 claims description 57
- 238000011282 treatment Methods 0.000 claims description 56
- 239000003595 mist Substances 0.000 claims description 49
- 239000002994 raw material Substances 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 44
- 239000012159 carrier gas Substances 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 31
- 238000005530 etching Methods 0.000 claims description 26
- 230000015572 biosynthetic process Effects 0.000 claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 239000003607 modifier Substances 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
- 238000000889 atomisation Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 230000006837 decompression Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 description 76
- 239000000243 solution Substances 0.000 description 27
- 239000000463 material Substances 0.000 description 16
- 229910052751 metal Inorganic materials 0.000 description 15
- 239000002184 metal Substances 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- -1 tetraamyloxysilane Chemical compound 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 7
- 239000000470 constituent Substances 0.000 description 7
- 230000001771 impaired effect Effects 0.000 description 7
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
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- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
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- 229910010272 inorganic material Inorganic materials 0.000 description 4
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- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 4
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
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- 239000011147 inorganic material Substances 0.000 description 3
- 239000012212 insulator Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 229920001709 polysilazane Polymers 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
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- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
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- 239000011701 zinc Substances 0.000 description 3
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
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- 229910052581 Si3N4 Inorganic materials 0.000 description 2
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
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- 244000043261 Hevea brasiliensis Species 0.000 description 1
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- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B17/00—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups
- B05B17/04—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods
- B05B17/06—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods using ultrasonic or other kinds of vibrations
- B05B17/0607—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods using ultrasonic or other kinds of vibrations generated by electrical means, e.g. piezoelectric transducers
- B05B17/0615—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods using ultrasonic or other kinds of vibrations generated by electrical means, e.g. piezoelectric transducers spray being produced at the free surface of the liquid or other fluent material in a container and subjected to the vibrations
Landscapes
- Special Spraying Apparatus (AREA)
- Weting (AREA)
- Formation Of Insulating Films (AREA)
Description
本発明は、半導体装置や電子機器等の製造等に有用な処理方法に関し、より具体的には、基板上で原料溶液を含むミストまたは液滴を反応させることにより被処理物を処理する方法に関する。 The present invention relates to a treatment method useful for manufacturing semiconductor devices, electronic devices, and the like, and more specifically, to a method of treating an object to be treated by reacting a mist or droplets containing a raw material solution on a substrate. ..
基板または半導体膜もしくは絶縁膜等の被処理材に対する、エッチング、洗浄、表面改質、成膜等の処理を、液体材料を用いて行う技術が知られており、例えば、スプレー法等を用いたエッチング処理や、塗布法等を用いた成膜処理などの処理方法が一般的に知られている。中でも、霧化された液体原料(ミスト)を用いることにより、被処理物に対してエッチング処理、表面改質処理、成膜処理等を行う方法が検討されており、特に、ミストCVD法を用いて成膜処理等を行う方法が検討されている(特許文献1〜5)。
A technique is known in which a liquid material is used to perform processing such as etching, cleaning, surface modification, and film formation on a substrate or a material to be treated such as a semiconductor film or an insulating film, and for example, a spray method or the like is used. Treatment methods such as etching treatment and film formation treatment using a coating method or the like are generally known. Among them, a method of performing etching treatment, surface modification treatment, film formation treatment, etc. on an object to be treated by using an atomized liquid raw material (mist) has been studied, and in particular, a mist CVD method is used. A method of performing a film forming process or the like has been studied (
ミストCVD法については、特許文献1には、管状炉型のミストCVD装置が記載されている。特許文献2には、ファインチャネル型のミストCVD装置が記載されている。特許文献3には、リニアソース型のミストCVD装置が記載されている。また、特許文献4には、ミスト発生器の上方に基板を設置し、さらにサセプタがホットプレート上に備え付けられた回転ステージであるミストCVD装置が記載されている。
Regarding the mist CVD method,
ところで、シリコン酸化膜は絶縁膜としてMOSトランジスタのゲート絶縁膜などに幅広く使用されており、電子デバイス産業で重要な役割を果たしている。しかし、ファインチャネル型等の従来のミストCVD装置を用いて、このようなシリコン酸化膜を成膜した場合には、金型の大きさに基板サイズが依存し、さらに平板以外の形状には成膜が困難であるという問題があった。また、SiO2薄膜等の成膜においては、ミストCVD法では、成膜レートが低いという問題があった。他の手法も同様の問題があり、基体の種類によらず、良質な膜が得られ、さらに、成膜レートにも優れたミストCVD法による成膜方法が待ち望まれていた。 By the way, the silicon oxide film is widely used as an insulating film for a gate insulating film of a MOS transistor and the like, and plays an important role in the electronic device industry. However, when such a silicon oxide film is formed by using a conventional mist CVD apparatus such as a fine channel type, the substrate size depends on the size of the mold, and the shape other than the flat plate is formed. There was a problem that the membrane was difficult. Further, in the film formation of a SiO 2 thin film or the like, the mist CVD method has a problem that the film formation rate is low. Other methods have the same problem, and a film forming method by the mist CVD method, which can obtain a good quality film regardless of the type of the substrate and has an excellent film forming rate, has been desired.
本発明は、ミストを用いた処理でも、効率良く基体を処理することができる処理方法および処理装置を提供することを目的とする。 An object of the present invention is to provide a treatment method and a treatment apparatus capable of efficiently treating a substrate even in a treatment using mist.
本発明者らは、上記目的を達成すべく鋭意検討した結果、ミスト・デポジション法を用いて、ノズル角度を調節し、ノズル角度を、鉛直下向き方向に対し、1°〜30°の範囲内にして成膜を行うと、効率良く基板を処理することができることを知見し、特に、成膜処理を行う場合には、高い成膜速度で効率良く成膜処理を行うことができることを見出した。また、このような処理方法および処理装置が、上記した従来の問題を一挙に解決できるものであることを見出した。
また、本発明者らは、上記知見を得た後、さらに検討を重ねて、本発明を完成させるに至った。
As a result of diligent studies to achieve the above object, the present inventors adjusted the nozzle angle by using the mist deposition method, and set the nozzle angle within the range of 1 ° to 30 ° with respect to the vertically downward direction. It was found that the substrate can be processed efficiently when the film formation is performed, and in particular, it is found that the film formation process can be efficiently performed at a high film formation rate. .. Further, they have found that such a processing method and a processing apparatus can solve the above-mentioned conventional problems at once.
In addition, after obtaining the above findings, the present inventors have further studied and completed the present invention.
すなわち、本発明は、以下の発明に関する。
[1] 原料溶液を霧化または液滴化し、得られたミストまたは液滴をキャリアガスで基体まで搬送し、ノズルから排出された前記ミストまたは前記液滴を前記基体上で反応させる処理方法であって、ノズル角度が、鉛直下向き方向に対し、1°〜30°の範囲内であることを特徴とする処理方法。
[2] ノズル角度が、16°〜28°の範囲内である前記[1]記載の処理方法。
[3] 前記霧化または液滴化を、超音波振動を用いて行う前記[1]または[2]に記載の処理方法。
[4] 前記原料溶液がエッチング剤、表面改質剤または成膜原料を含有し、前記処理が、それぞれエッチング処理、表面改質処理または成膜処理である前記[1]〜[3]のいずれかに記載の処理方法。
[5] 前記原料溶液が成膜原料を含有し、前記処理が、成膜処理である前記[1]〜[4]のいずれかに記載の処理方法。
[6] 前記反応を、大気圧下で行う前記[1]〜[5]のいずれかに記載の処理方法。
[7] 前記反応が、熱反応である前記[1]〜[6]のいずれかに記載の処理方法。
[8] 前記熱反応を、200℃以下の温度で行う前記[7]記載の処理方法。
[9] 原料溶液を霧化または液滴化する霧化・液滴化部、得られたミストまたは液滴をキャリアガスで基体まで搬送する搬送部、ノズルから排出された前記ミストまたは前記液滴を前記基体上で反応させる反応部を備える処理装置であって、ノズル角度が、鉛直下向き方向に対し、1°〜30°の範囲内であることを特徴とする処理装置。
[10] ノズル角度が、16°〜28°の範囲内である前記[9]記載の処理装置。
[11] 霧化・液滴化部に超音波振動子を備えており、前記の霧化または液滴化を、超音波振動を用いて行う前記[9]または[10]に記載の処理装置。
[12] エッチング処理装置、表面改質処理装置または成膜処理装置である前記[9]〜[11]のいずれかに記載の処理装置。
[13] 成膜処理装置である前記[9]〜[12]のいずれかに記載の処理装置。
[14] 真空装置または減圧装置を備えていない前記[9]〜[13]のいずれかに記載の処理装置。
[15] 反応部に加熱手段を備える前記[9]〜[14]のいずれかに記載の処理装置。
That is, the present invention relates to the following invention.
[1] A treatment method in which a raw material solution is atomized or dropletized, the obtained mist or droplet is conveyed to a substrate by a carrier gas, and the mist or droplet discharged from the nozzle is reacted on the substrate. Therefore, the processing method is characterized in that the nozzle angle is in the range of 1 ° to 30 ° with respect to the vertical downward direction.
[2] The processing method according to the above [1], wherein the nozzle angle is in the range of 16 ° to 28 °.
[3] The treatment method according to the above [1] or [2], wherein the atomization or droplet formation is performed using ultrasonic vibration.
[4] Any of the above [1] to [3], wherein the raw material solution contains an etching agent, a surface modifier or a film forming raw material, and the treatment is an etching treatment, a surface modification treatment or a film forming treatment, respectively. The processing method described in Crab.
[5] The treatment method according to any one of [1] to [4], wherein the raw material solution contains a film-forming raw material and the treatment is a film-forming treatment.
[6] The treatment method according to any one of [1] to [5], wherein the reaction is carried out under atmospheric pressure.
[7] The treatment method according to any one of the above [1] to [6], wherein the reaction is a thermal reaction.
[8] The treatment method according to the above [7], wherein the thermal reaction is carried out at a temperature of 200 ° C. or lower.
[9] An atomizing / droplet atomizing section for atomizing or dropletizing a raw material solution, a transport section for transporting the obtained mist or droplet to a substrate with a carrier gas, the mist or the droplet discharged from a nozzle. A processing device including a reaction unit for reacting the above-mentioned substrate, wherein the nozzle angle is in the range of 1 ° to 30 ° with respect to the vertically downward direction.
[10] The processing apparatus according to the above [9], wherein the nozzle angle is in the range of 16 ° to 28 °.
[11] The processing apparatus according to the above [9] or [10], wherein the atomizing / droplet atomizing portion is provided with an ultrasonic vibrator, and the atomizing or droplet forming is performed by using ultrasonic vibration. ..
[12] The processing apparatus according to any one of the above [9] to [11], which is an etching processing apparatus, a surface modification processing apparatus, or a film forming processing apparatus.
[13] The processing apparatus according to any one of the above [9] to [12], which is a film forming processing apparatus.
[14] The processing device according to any one of [9] to [13] above, which is not provided with a vacuum device or a decompression device.
[15] The processing apparatus according to any one of [9] to [14] above, wherein the reaction unit is provided with a heating means.
本発明の処理方法によれば、工業的有利に、効率良く基体を処理することができる。 According to the treatment method of the present invention, the substrate can be treated efficiently in an industrially advantageous manner.
本発明の処理方法は、原料溶液を霧化または液滴化し(霧化・液滴化工程)、得られたミストまたは液滴をキャリアガスで基体まで搬送し(搬送工程)、ノズルから排出された前記ミストまたは前記液滴を前記基体上で反応させる(反応工程)処理方法であって、ノズル角度が、鉛直下向き方向に対し、1°〜30°の範囲内であることを特長とする。 In the treatment method of the present invention, the raw material solution is atomized or dropleted (atomization / droplet atomization step), and the obtained mist or droplet is conveyed to the substrate by carrier gas (transport step) and discharged from the nozzle. It is a treatment method for reacting the mist or the droplets on the substrate (reaction step), and is characterized in that the nozzle angle is in the range of 1 ° to 30 ° with respect to the vertical downward direction.
(原料溶液)
前記原料溶液は、被処理物を処理する処理剤を含んでおり、霧化または液滴化が可能であれば、特に限定されない。前記処理剤は、液状であってもよいし、固体状であってもよいし、気体状であってもよい。ゲル状であってもよいし、ゾル状であってもよい。また、前記原料溶液は、無機材料を含んでいてもよいし、有機材料を含んでいてもよい。前記処理剤は、基体を処理できれば、特に限定されず、公知のものであってよい。前記処理剤としては、例えば、エッチング剤、表面改質剤、または成膜原料などが挙げられるが、本発明においては、前記処理剤が、成膜原料であるのが好ましい。
(Raw material solution)
The raw material solution contains a treatment agent for treating an object to be treated, and is not particularly limited as long as it can be atomized or dropletized. The treatment agent may be in a liquid state, a solid state, or a gaseous state. It may be in the form of a gel or in the form of a sol. Further, the raw material solution may contain an inorganic material or an organic material. The treatment agent is not particularly limited as long as it can treat the substrate, and may be a known one. Examples of the treatment agent include an etching agent, a surface modifier, and a film-forming raw material. In the present invention, the treatment agent is preferably a film-forming raw material.
前記エッチング剤は、本発明の目的を阻害しない限り、特に限定されず、公知のエッチング剤であってよい。前記エッチング剤としては、例えば、公知の酸またはアルカリ等が挙げられる。前記酸としては、例えば、弗酸、塩酸、硫酸、リン酸、硝酸、酢酸、炭酸、蟻酸、安息香酸、亜塩素酸、次亜塩素酸、亜硫酸、次亜硫酸、亜硝酸、次亜硝酸、亜リン酸、次亜リン酸等のプロトン酸またはこれらの混合物等が挙げられる。また、前記アルカリとしては、例えば、水酸化ナトリウム、水酸化カリウム、水酸化カルシウムまたはこれらの混合物等が挙げられる。他のエッチング剤としては、金、銀、銅、パラジウム、白金などの金属のエッチングに使用されてきたもの(例えば、塩化第二鉄系エッチング剤、シアン酸塩/酸素系エッチング剤、フェロシアン酸塩/フェリシアン酸塩系エッチング剤、チオ尿素系エッチング剤、及びヨウ化カリウム/ヨウ素系エッチング剤(KI/I2;「三ヨウ化物」)またはこれらの組合せ)等が挙げられる。本発明においては、前記原料溶液に、前記エッチング剤を、1種類単独で用いてもよいし、2種類以上を用いてもよい。前記原料溶液中の前記エッチング剤の含有量は、特に限定されないが、好ましくは、0.001重量%〜80重量%であり、より好ましくは0.01重量%〜80重量%である。 The etching agent is not particularly limited and may be a known etching agent as long as the object of the present invention is not impaired. Examples of the etching agent include known acids and alkalis. Examples of the acid include phosphoric acid, hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, acetic acid, carbonic acid, formic acid, benzoic acid, chloric acid, hypochlorous acid, sulfite, hyposulfite, nitrite, hyponitrite, and sulphate. Examples thereof include protonic acids such as phosphoric acid and hypophosphorous acid, or mixtures thereof. Examples of the alkali include sodium hydroxide, potassium hydroxide, calcium hydroxide, or a mixture thereof. Other etching agents that have been used for etching metals such as gold, silver, copper, palladium, and platinum (eg, ferric chloride-based etching agents, cyanate / oxygen-based etching agents, ferrocyanic acid). Examples thereof include a salt / ferricyanate-based etching agent, a thiourea-based etching agent, and a potassium iodide / iodine-based etching agent (KI / I2; “triiodide”) or a combination thereof). In the present invention, the etching agent may be used alone or in combination of two or more in the raw material solution. The content of the etching agent in the raw material solution is not particularly limited, but is preferably 0.001% by weight to 80% by weight, and more preferably 0.01% by weight to 80% by weight.
前記表面改質剤は、本発明の目的を阻害しない限り、特に限定されず、公知のものであってよい。前記表面改質剤としては、例えば、アニオン系・カチオン系界面活性剤、ノニオン系界面活性剤、両性界面活性剤、高分子界面活性剤、顔料分散剤、アルコール類、脂肪酸、アミン類、アミド類、イミド類、金属せっけん、脂肪酸オリゴマー化合物、シランカップリング剤、チタネートカップリング剤、アルミネートカップリング剤、リン酸系カップリング剤、カルボン酸系カップリング剤、フッ素系界面活性剤、ホウ素系界面活性剤等が挙げられる。前記原料溶液は、前記表面改質剤を、1種類単独で含んでいてもよいし、2種類以上を含んでいてもよい。前記原料溶液中の前記表面改質剤の含有量は、特に限定されないが、好ましくは、0.001重量%〜80重量%であり、より好ましくは0.01重量%〜80重量%である。 The surface modifier is not particularly limited and may be a known one as long as the object of the present invention is not impaired. Examples of the surface modifier include anionic / cationic surfactants, nonionic surfactants, amphoteric surfactants, polymer surfactants, pigment dispersants, alcohols, fatty acids, amines, and amides. , Iimides, metal soap, fatty acid oligomer compounds, silane coupling agents, titanate coupling agents, aluminate coupling agents, phosphoric acid-based coupling agents, carboxylic acid-based coupling agents, fluorosurfactants, boron-based surfactants Activators and the like can be mentioned. The raw material solution may contain the surface modifier alone or in combination of two or more. The content of the surface modifier in the raw material solution is not particularly limited, but is preferably 0.001% by weight to 80% by weight, and more preferably 0.01% by weight to 80% by weight.
前記成膜原料は、本発明の目的を阻害しない限り、公知の成膜原料であってよく、無機材料であっても、有機材料であってもよい。本発明においては、前記成膜原料が、金属または金属化合物を含むのが好ましく、ガリウム、鉄、インジウム、アルミニウム、バナジウム、チタン、クロム、ロジウム、ニッケル、コバルト、亜鉛、マグネシウム、カルシウム、イットリウム、ストロンチウム、バリウムおよびケイ素から選ばれる1種または2種以上の金属を含むのがより好ましく、ケイ素含有化合物であるのが最も好ましい。前記ケイ素含有化合物は、少なくとも一つのケイ素を含む化合物であれば特に限定されない。前記ケイ素含有化合物としては、例えば、シラン、シロキサン、シラザン、ポリシラザンなどが挙げられる。前記シランとしては、例えば、モノシラン(SiH4)、アルコキシシランなどが挙げられる。前記アルコキシシランとしては、例えば、テトラエトキシシラン(TEOS)、テトラメトキシシラン、テトラプロポキシシラン、テトラブトキシシラン、テトラアミロキシシラン、テトラオクチルオキシシラン、テトラノニルオキシシラン、ジメトキシジエトキシシラン、ジメトキシジイソプロポキシシラン、ジエトキシジイソプロポキシシラン、ジエトキシジブトキシシラン、ジエトキシジトリチルオキシシランまたはこれらの混合物などが挙げられる。前記シロキサンとしては、例えばヘキサメチルジシロキサン、1,3−ジブチルテトラメチルジシロキサン、1,3−ジフェニルテトラメチルジシロキサン、1,3−ジビニルテトラメチルジシロキサン、ヘキサエチルジシロキサン及び3−グリシドキシプロピルペンタメチルジシロキサンなどが挙げられる。シラザンとしては、例えばヘキサメチルジシラザン及びヘキサエチルジシラザンなどが挙げられる。また、本発明においては、前記成膜原料が、前記金属を錯体または塩の形態で含むのも好ましい。前記錯体の形態としては、例えば、有機錯体などが挙げられ、より具体的には、例えば、アセチルアセトナート錯体、カルボニル錯体、アンミン錯体、ヒドリド錯体、キノリノール錯体等が挙げられる。前記塩の形態としては、例えば、ハロゲン化物などが挙げられ、より具体的には、例えば、塩化金属塩、臭化金属塩、ヨウ化金属塩などが挙げられる。原料溶液中の前記成膜原料の含有量は、特に限定されないが、好ましくは、0.001重量%〜80重量%であり、より好ましくは0.01重量%〜80重量%である。 The film-forming raw material may be a known film-forming raw material, and may be an inorganic material or an organic material as long as the object of the present invention is not impaired. In the present invention, the film-forming raw material preferably contains a metal or a metal compound, and gallium, iron, indium, aluminum, vanadium, titanium, chromium, rhodium, nickel, cobalt, zinc, magnesium, calcium, yttrium, and strontium. It is more preferable to contain one or more metals selected from, barium and silicon, and most preferably a silicon-containing compound. The silicon-containing compound is not particularly limited as long as it is a compound containing at least one silicon. Examples of the silicon-containing compound include silane, siloxane, silazane, polysilazane and the like. Examples of the silane include monosilane (SiH 4 ) and alkoxysilane. Examples of the alkoxysilane include tetraethoxysilane (TEOS), tetramethoxysilane, tetrapropoxysilane, tetrabutoxysilane, tetraamyloxysilane, tetraoctyloxysilane, tetranonyloxysilane, dimethoxydiethoxysilane, and dimethoxydiiso. Examples thereof include propoxysilane, diethoxydiisopropoxysilane, diethoxydibutoxysilane, diethoxyditrityloxysilane, and mixtures thereof. Examples of the siloxane include hexamethyldisiloxane, 1,3-dibutyltetramethyldisiloxane, 1,3-diphenyltetramethyldisiloxane, 1,3-divinyltetramethyldisiloxane, hexaethyldisiloxane and 3-glycid. Examples thereof include xipropylpentamethyldisiloxane. Examples of the silicate include hexamethyldisilazane and hexaethyldisilazane. Further, in the present invention, it is also preferable that the film-forming raw material contains the metal in the form of a complex or a salt. Examples of the form of the complex include an organic complex and the like, and more specific examples thereof include an acetylacetonate complex, a carbonyl complex, an ammine complex, a hydride complex, a quinolinol complex and the like. Examples of the form of the salt include halides and the like, and more specifically, for example, metal chloride salt, metal bromide salt, metal iodide salt and the like. The content of the film-forming raw material in the raw material solution is not particularly limited, but is preferably 0.001% by weight to 80% by weight, and more preferably 0.01% by weight to 80% by weight.
本発明においては、前記原料溶液が、エッチング剤、表面改質剤または成膜原料を含有し、前記処理が、それぞれエッチング処理、表面改質処理または成膜処理であるのが好ましく、前記原料溶液が成膜原料を含有し、前記処理が、成膜処理であるのがより好ましい。 In the present invention, it is preferable that the raw material solution contains an etching agent, a surface modifier or a film forming raw material, and the treatments are an etching treatment, a surface modification treatment or a film forming treatment, respectively. Contains a film-forming raw material, and it is more preferable that the treatment is a film-forming treatment.
前記原料溶液は、さらに、溶媒を含んでいてもよい。前記溶媒は、特に限定されず、水等の無機溶媒であってもよいし、有機溶媒であってもよいし、無機溶媒と有機溶媒との混合溶媒であってもよい。本発明においては、前記溶媒が有機溶媒を含むのが好ましく、有機溶媒であるのがより好ましい。前記有機溶媒としては、例えば、エステル溶媒(例えば、酢酸エチル、酢酸プロピル、酢酸ブチル、プロピオン酸エチル、プロピオン酸プロピル、プロピオン酸ブチルなど)、エーテル溶媒(例えば、ジエチルエーテル、tert−ブチルメチルエーテル、ジグライム(例えば、ジエチレングリコールジメチルエーテル、ジエチレングリコールジブチルエーテル、ジエチレングリコールジエチルエーテル)、1,2−ジメトキシエタン、テトラヒドロフランなど)、アミド溶媒(例えば、N,N−ジメチルホルムアミド、N,N−ジメチルアセトアミド、N−メチルピロリドン、1,3−ジメチル−2−イミダゾリジノンなど)、ケトン溶媒(例えば、メチルイソブチルケトン、メチルエチルケトン、シクロヘキサノン、シクロペンタノンなど)、ニトリル溶媒(例えば、アセトニトリル、プロピオニトリルなど)、アルコール溶媒(例えば、メタノール、エタノール、1−プロパノール、2−プロパノール、1−ブタノール、2−ブタノールなど)、ハロゲン化溶媒(例えば、塩化メチレン、クロロホルムなど)、芳香族溶媒(例えば、トルエン、キシレン、クロロベンゼン、ニトロベンゼンなど)などが挙げられる。 The raw material solution may further contain a solvent. The solvent is not particularly limited, and may be an inorganic solvent such as water, an organic solvent, or a mixed solvent of an inorganic solvent and an organic solvent. In the present invention, the solvent preferably contains an organic solvent, and more preferably an organic solvent. Examples of the organic solvent include ester solvents (eg, ethyl acetate, propyl acetate, butyl acetate, ethyl propionate, propyl propionate, butyl propionate, etc.), ether solvents (eg, diethyl ether, tert-butyl methyl ether, etc.). Diglime (eg, diethylene glycol dimethyl ether, diethylene glycol dibutyl ether, diethylene glycol diethyl ether), 1,2-dimethoxyethane, tetrahydrofuran, etc.), amide solvent (eg, N, N-dimethylformamide, N, N-dimethylacetamide, N-methylpyrrolidone) , 1,3-dimethyl-2-imidazolidinone, etc.), ketone solvent (eg, methylisobutylketone, methylethylketone, cyclohexanone, cyclopentanone, etc.), nitrile solvent (eg, acetonitrile, propionitrile, etc.), alcohol solvent (eg, acetonitrile, propionitrile, etc.) For example, methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, etc., halogenated solvents (eg, methylene chloride, chloroform, etc.), aromatic solvents (eg, toluene, xylene, chlorobenzene, nitrobenzene, etc.) Etc.) and so on.
(霧化・液滴化工程)
霧化手段または液滴化手段は、前記原料溶液を霧化または液滴化できさえすれば特に限定されず、公知の手段であってよい。本発明においては、超音波振動を用いる霧化手段または液滴化手段が好ましい。超音波振動を用いて得られたミストまたは液滴は、初速度がゼロであり、空中に浮遊するので好ましく、例えば、スプレーのように吹き付けるのではなく、空間に浮遊してガスとして搬送することが可能なミストであるので衝突エネルギーによる損傷がなく、ミストの流路方向の制御も容易であるため、非常に好適である。ミストの液滴のサイズは、特に限定されず、数mm程度であってもよいが、好ましくは50μm以下であり、より好ましくは100nm〜10μmである。
(Atomization / droplet formation process)
The atomizing means or the droplet forming means is not particularly limited as long as the raw material solution can be atomized or dropletized, and may be a known means. In the present invention, atomizing means or droplet forming means using ultrasonic vibration is preferable. The mist or droplet obtained by using ultrasonic vibration is preferable because it has a zero initial velocity and floats in the air. For example, instead of spraying it like a spray, it floats in space and is transported as a gas. Since it is a mist that can be used, there is no damage due to collision energy, and it is easy to control the flow path direction of the mist, which is very suitable. The size of the mist droplets is not particularly limited and may be about several mm, but is preferably 50 μm or less, and more preferably 100 nm to 10 μm.
(搬送工程)
搬送工程では、キャリアガスおよび所望により供給管等を用いて、前記ミストまたは前記液滴を前記基体へ搬送する。
前記キャリアガスは、本発明の目的を阻害しない限り、特に限定されず、例えば、酸素、オゾン、窒素やアルゴン等の不活性ガス、または水素ガスやフォーミングガス等の還元ガスなどが好適な例として挙げられる。また、キャリアガスの種類は1種類であってよいが、2種類以上であってもよく、流量を下げた希釈ガス(例えば10倍希釈ガス等)などを、第2のキャリアガスとしてさらに用いてもよい。また、キャリアガスの供給箇所も1箇所だけでなく、2箇所以上あってもよい。キャリアガスの流量は、特に限定されないが、0.01〜20L/分であるのが好ましく、1〜10L/分であるのがより好ましい。希釈ガスの場合には、希釈ガスの流量が、0.001〜20L/分であるのが好ましく、0.1〜10L/分であるのがより好ましい。
(Transport process)
In the transfer step, the mist or the droplet is transferred to the substrate by using a carrier gas and, if desired, a supply pipe or the like.
The carrier gas is not particularly limited as long as the object of the present invention is not impaired, and for example, an inert gas such as oxygen, ozone, nitrogen or argon, or a reducing gas such as hydrogen gas or forming gas is a suitable example. Can be mentioned. Further, the type of the carrier gas may be one type, but may be two or more types, and a diluted gas having a reduced flow rate (for example, a 10-fold diluted gas) or the like is further used as the second carrier gas. May be good. Further, the carrier gas may be supplied not only at one location but also at two or more locations. The flow rate of the carrier gas is not particularly limited, but is preferably 0.01 to 20 L / min, and more preferably 1 to 10 L / min. In the case of a diluting gas, the flow rate of the diluting gas is preferably 0.001 to 20 L / min, more preferably 0.1 to 10 L / min.
(基体)
前記基体は、前記被処理物を支持できるものであれば特に限定されない。前記基体の材料も、本発明の目的を阻害しない限り特に限定されず、公知の基体であってよく、有機化合物であってもよいし、無機化合物であってもよい。多孔質構造体であってもよい。前記基体の形状としては、どのような形状のものであってもよく、あらゆる形状に対して有効であり、例えば、平板や円板等の板状、繊維状、棒状、円柱状、角柱状、筒状、螺旋状、球状、リング状などが挙げられるが、本発明においては、基板が好ましい。基板の厚さは、本発明においては特に限定されないが、10μm〜100mmが好ましく、100μm〜10mmがより好ましい。
(Hypokeimenon)
The substrate is not particularly limited as long as it can support the object to be treated. The material of the substrate is not particularly limited as long as it does not impair the object of the present invention, and may be a known substrate, an organic compound, or an inorganic compound. It may be a porous structure. The shape of the substrate may be any shape and is effective for any shape, for example, plate-like, fibrous, rod-like, columnar, prismatic, such as a flat plate or a disk. Cylindrical, spiral, spherical, ring-shaped and the like can be mentioned, but in the present invention, a substrate is preferable. The thickness of the substrate is not particularly limited in the present invention, but is preferably 10 μm to 100 mm, more preferably 100 μm to 10 mm.
前記基板は、板状であって、前記ミストまたは前記液滴を反応させることにより処理可能なものであれば、特に限定されない。前記基板の材料も本発明の目的を阻害しない限り特に限定されず、公知の材料であってよい。絶縁体基板であってもよいし、半導体基板であってもよいし、金属基板や導電性基板であってもよい。また、本発明においては、前記基板の一部または全部の上に、金属膜、半導体膜、導電性膜および絶縁性膜の少なくとも1種の膜が形成されているものも、前記基板として好適に用いることができる。前記金属膜の構成金属としては、例えば、ガリウム、鉄、インジウム、アルミニウム、バナジウム、チタン、クロム、ロジウム、ニッケル、コバルト、亜鉛、マグネシウム、カルシウム、シリコン、イットリウム、ストロンチウムおよびバリウムから選ばれる1種または2種以上の金属などが挙げられる。半導体膜の構成材料としては、例えば、シリコン、ゲルマニウムのような元素単体、周期表の第3族〜第5族、第13族〜第15族の元素を有する化合物、金属酸化物、金属硫化物、金属セレン化物、または金属窒化物、ペロブスカイト等が挙げられる。また、前記導電性膜の構成材料としては、例えば、スズドープ酸化インジウム(ITO)、フッ素ドープ酸化インジウム(FTO)、酸化亜鉛(ZnO)、アルミニウムドープ酸化亜鉛(AZO)、ガリウムドープ酸化亜鉛(GZO)、酸化スズ(SnO2)、酸化インジウム(In2O3)、酸化タングステン(WO3)などが挙げられる。前記絶縁性膜の構成材料としては、例えば、酸化アルミニウム(Al2O3)、酸化チタン(TiO2)、酸化シリコン(SiO2)、窒化シリコン(Si3N4)、酸窒化シリコン(Si4O5N3)などが挙げられるが、絶縁性酸化物からなる絶縁性膜であるのが好ましく、チタニア膜であるのがより好ましい。 The substrate is not particularly limited as long as it has a plate shape and can be processed by reacting the mist or the droplets. The material of the substrate is not particularly limited as long as it does not interfere with the object of the present invention, and may be a known material. It may be an insulator substrate, a semiconductor substrate, a metal substrate, or a conductive substrate. Further, in the present invention, a substrate in which at least one of a metal film, a semiconductor film, a conductive film and an insulating film is formed on a part or all of the substrate is also suitable as the substrate. Can be used. As the constituent metal of the metal film, for example, one selected from gallium, iron, indium, aluminum, vanadium, titanium, chromium, rhodium, nickel, cobalt, zinc, magnesium, calcium, silicon, yttrium, strontium and barium, or one of them. Two or more kinds of metals and the like can be mentioned. Examples of the constituent materials of the semiconductor film include elemental substances such as silicon and germanium, compounds having elements of groups 3 to 5 and groups 13 to 15 of the periodic table, metal oxides, and metal sulfides. , Metal selenium, metal nitride, perovskite and the like. Examples of the constituent material of the conductive film include tin-doped indium oxide (ITO), fluorine-doped indium oxide (FTO), zinc oxide (ZnO), aluminum-doped zinc oxide (AZO), and gallium-doped zinc oxide (GZO). , Tin oxide (SnO 2 ), indium oxide (In 2 O 3 ), tungsten oxide (WO 3 ) and the like. Examples of the constituent materials of the insulating film include aluminum oxide (Al 2 O 3 ), titanium oxide (TiO 2 ), silicon oxide (SiO 2 ), silicon nitride (Si 3 N 4 ), and silicon oxynitride (Si 4). Examples thereof include O 5 N 3 ), and an insulating film made of an insulating oxide is preferable, and a titania film is more preferable.
なお、金属膜、半導体膜、導電性膜および絶縁性膜の形成手段は、特に限定されず、公知の手段であってよい。このような形成手段としては、例えば、ミストCVD法、スパッタ法、CVD法(気相成長法)、SPD法(スプレー熱分解堆積法)、蒸着法、ALD(原子層堆積)法、塗布法(例えばディッピング、滴下、ドクターブレード、インクジェット、スピンコート、刷毛塗り、スプレー塗装、ロールコーター、エアーナイフコート、カーテンコート、ワイヤーバーコート、グラビアコート、インクジェット塗布等)などが挙げられる。 The means for forming the metal film, the semiconductor film, the conductive film and the insulating film is not particularly limited and may be a known means. Examples of such forming means include a mist CVD method, a sputtering method, a CVD method (vapor deposition method), an SPD method (spray thermal decomposition deposition method), a vapor deposition method, an ALD (atomic layer deposition) method, and a coating method ( For example, dipping, dripping, doctor blade, inkjet, spin coating, brush coating, spray coating, roll coater, air knife coating, curtain coating, wire bar coating, gravure coating, inkjet coating, etc.).
本発明においては、前記基板上に、直接または他の層を介して、凹部または凸部からなる凹凸部が形成されているのも好ましい。前記凹凸部は、凸部または凹部からなるものであれば特に限定されず、凸部からなる凹凸部であってもよいし、凹部からなる凹凸部であってもよいし、凸部および凹部からなる凹凸部であってもよい。また、前記凹凸部は、規則的な凸部または凹部から形成されていてもよいし、不規則な凸部または凹部から形成されていてもよい。本発明においては、前記凹凸部が周期的に形成されているのが好ましく、周期的かつ規則的にパターン化されているのがより好ましい。前記凹凸部の形状としては、特に限定されず、例えば、ストライプ状、ドット状、メッシュ状またはランダム状などが挙げられるが、本発明においては、ストライプ状またはドット状が好ましい。なお、ドット状に凹凸部を形成する場合には、例えば正方格子、斜方格子、三角格子、六角格子などの格子位置に、周期的かつ規則的に、三角形、四角形(例えば正方形、長方形若しくは台形等)、五角形若しくは六角形等の多角形状、円状、楕円状などの凹凸部を配置することができる。前記凹凸部の凹部または凸部の断面形状としては、特に限定されないが、例えば、コの字型、U字型、逆U字型、波型、または三角形、四角形(例えば正方形、長方形若しくは台形等)、五角形若しくは六角形等の多角形等が挙げられる。 In the present invention, it is also preferable that a concavo-convex portion composed of a concave portion or a convex portion is formed on the substrate directly or via another layer. The concavo-convex portion is not particularly limited as long as it is composed of a convex portion or a concave portion, and may be a concavo-convex portion composed of a convex portion, a concavo-convex portion composed of a concave portion, or a convex portion and a concave portion. It may be an uneven portion. Further, the uneven portion may be formed from a regular convex portion or a concave portion, or may be formed from an irregular convex portion or a concave portion. In the present invention, it is preferable that the uneven portion is formed periodically, and it is more preferable that the uneven portion is periodically and regularly patterned. The shape of the uneven portion is not particularly limited, and examples thereof include a striped shape, a dot shape, a mesh shape, and a random shape. In the present invention, the striped shape or the dot shape is preferable. When forming the uneven portion in a dot shape, for example, a triangle, a quadrangle (for example, a square, a rectangle, or a trapezoid) is periodically and regularly arranged at a grid position such as a square grid, an oblique grid, a triangular grid, or a hexagonal grid. Etc.), polygonal shapes such as pentagons and hexagons, and concavo-convex parts such as circles and ellipses can be arranged. The cross-sectional shape of the concave or convex portion of the uneven portion is not particularly limited, and is, for example, U-shaped, U-shaped, inverted U-shaped, corrugated, or triangular, quadrangular (for example, square, rectangular, trapezoidal, etc.). ), Polygons such as pentagons and hexagons, etc.
前記原料溶液が、エッチング剤を含み、前記処理が、エッチング処理である場合、前記基板の構成材料としては、好適には例えば、半導体材料、絶縁体材料、金属材料等の固体材料が挙げられる。前記半導体材料としては、例えば、シリコン(単結晶シリコン、多結晶シリコン、アモルファスシリコン等)、ゲルマニウム、シリコンゲルマニウム、シリコンカーバイド(SiC)、ガリウムヒ素、ガリウムアルミニウムヒ素、インジウムリン、インジウムアンチモン、窒化ガリウム、窒化アルミニウム、酸化ガリウムなどが挙げられる。前記絶縁体材料としては、例えば、酸化ジルコニウム、酸化ハフニウム、酸化タンタル、酸化アルミニウム、酸化チタン、酸化クロムなどの金属酸化物及びこれらのシリケート、二酸化ケイ素、石英などのシリコン酸化物、シリコン窒化物、サファイアなどが挙げられる。前記金属材料としては、例えば、金(Au)、銀(Ag)、白金(Pt)、銅(Cu)、鉄(Fe)、マンガン(Mn)、ニッケル(Ni)、パラジウム(Pd)、コバルト(Co)、ロジウム(Rh)、ルテニウム(Ru)、クロム(Cr)、モリブデン(Mo)、タングステン(W)およびアルミニウム(Al)から選ばれる1種または2種以上の金属等が挙げられる。 When the raw material solution contains an etching agent and the treatment is an etching treatment, the constituent material of the substrate is preferably a solid material such as a semiconductor material, an insulator material, or a metal material. Examples of the semiconductor material include silicon (single crystal silicon, polycrystalline silicon, amorphous silicon, etc.), germanium, silicon germanium, silicon carbide (SiC), gallium arsenide, gallium aluminum arsenide, indium phosphide, indium antimony, gallium nitride, and the like. Examples include aluminum nitride and gallium oxide. Examples of the insulator material include metal oxides such as zirconium oxide, hafnium oxide, tantalum oxide, aluminum oxide, titanium oxide and chromium oxide, silicates thereof, silicon oxides such as silicon dioxide and quartz, and silicon nitride. Examples include sapphire. Examples of the metal material include gold (Au), silver (Ag), platinum (Pt), copper (Cu), iron (Fe), manganese (Mn), nickel (Ni), palladium (Pd), and cobalt (Pd). Examples thereof include one or more metals selected from Co), rhodium (Rh), ruthenium (Ru), chromium (Cr), molybdenum (Mo), tungsten (W) and aluminum (Al).
前記原料溶液が、表面改質剤を含み、前記処理が、表面改質処理である場合、前記基板の構成材料としては、好適には例えば、シリコンゴム、フッ素ゴム、天然ゴム、ネオプレンゴム、クロロプレンゴム、ウレタンゴム、アクリルゴムなどのゴム類、各種ポリエチレン樹脂、ポリプロピレン樹脂、変性ポリプロピレン樹脂、ポリメチルペンテン樹脂、ポリエステル樹脂、ポリカーボネート樹脂、エポキシ樹脂、フェノール樹脂、シアネート樹脂、尿素樹脂、グアナミン樹脂等の高分子材料、アルミニウム、マグネシウム、ステンレス、ニッケル、クロム、タングステン、金、銅、鉄、銀、亜鉛、スズ、鉛等の金属材料、酸化チタン、酸化ジルコニウム、酸化亜鉛、酸化インジウム、酸化スズ、シリカ、タルク、炭酸カルシウム、石灰、ゼオライト、半田、ガラス、セラミック材料等が挙げられる。 When the raw material solution contains a surface modifier and the treatment is a surface modification treatment, the substrate constituent material is preferably, for example, silicon rubber, fluororubber, natural rubber, neoprene rubber, chloroprene. Rubbers such as rubber, urethane rubber, acrylic rubber, various polyethylene resins, polypropylene resins, modified polypropylene resins, polymethylpentene resins, polyester resins, polycarbonate resins, epoxy resins, phenol resins, cyanate resins, urea resins, guanamine resins, etc. Polymer materials, aluminum, magnesium, stainless steel, nickel, chromium, tungsten, gold, copper, iron, silver, zinc, tin, lead and other metal materials, titanium oxide, zirconium oxide, zinc oxide, indium oxide, tin oxide, silica , Rubber, calcium carbonate, lime, zeolite, solder, glass, ceramic materials and the like.
前記原料溶液が、成膜原料を含み、前記処理が、成膜処理である場合、前記基板の構成材料としては、好適には例えば、石英、ガラス、サファイア、チタニア等の無機材料、ポリエチレンテレフタレート、ポリエチレンナフタレート、ポリエーテルスルホン、ポリイミド、ナイロン、ポリスチレン、ポリビニルアルコール、エチレンビニルアルコール共重合体、フッ素樹脂、塩化ビニル、ポリエチレンのようなポリオレフィン、セルロース、ポリ塩化ビニリデン、アラミド、ポリフェニレンスルフィド、ポリウレタン、ポリカーボネート、ポリアリレート、ポリノルボルネン、エポキシ樹脂等の有機材料、紙、合成紙等の紙材料、ステンレス、チタン、アルミニウム等の金属に絶縁性を付与する層等を塗布又は積層した複合材料等が挙げられる。 When the raw material solution contains a film-forming raw material and the treatment is a film-forming treatment, the constituent material of the substrate is preferably, for example, an inorganic material such as quartz, glass, sapphire, or titania, polyethylene terephthalate, or the like. Polyethylene naphthalate, polyether sulfone, polyimide, nylon, polystyrene, polyvinyl alcohol, ethylene vinyl alcohol copolymer, fluororesin, vinyl chloride, polyolefins such as polyethylene, cellulose, polyvinylidene chloride, aramid, polyphenylene sulfide, polyurethane, polycarbonate , Organic materials such as polyarylate, polynorbornene, epoxy resin, paper materials such as paper and synthetic paper, composite materials coated or laminated with layers that impart insulation to metals such as stainless steel, titanium and aluminum. ..
(反応工程)
反応工程では、ノズルから排出された前記ミストまたは前記液滴を前記基体上で反応させる。ここで、ノズル角度は、鉛直下向き方向に対し、1°〜30°の範囲内であるが、本発明においては、成膜レートがより向上するので、前記ノズル角度が2°〜29°の範囲内であるのが好ましく、10°〜29°の範囲内であるのがより好ましく、16°〜28°の範囲内であるのが最も好ましい。また、本発明においては、成膜速度がさらに格段に向上するとの観点から、前記ノズル角度が、20°〜27°の範囲内であるのが好ましく、20°〜25°の範囲内であるのがより好ましい。前記ノズル角度は、鉛直下向き方向と、ノズル内の前記基体に向けてキャリアガスとともに流れる前記ミストまたは前記液滴の流れ方向とのなす角である。図2にノズル角度の例を示す。図2は、本発明の反応装置における反応部の一態様を示す。図2の反応部は、ノズル7、ホットプレート8、基板10、ステージ11および支柱12からなる。支柱12は、鉛直下向き方向に立っており、ノズル7内の基板に向けてキャリアガスとともに流れる前記ミストまたは前記液滴の流れ方向とのなす角がノズル角度となる。図2中、ノズル角度をθで示す。
(Reaction process)
In the reaction step, the mist or the droplets discharged from the nozzle are reacted on the substrate. Here, the nozzle angle is in the range of 1 ° to 30 ° with respect to the vertical downward direction, but in the present invention, the film formation rate is further improved, so that the nozzle angle is in the range of 2 ° to 29 °. It is preferably in the range of 10 ° to 29 °, more preferably in the range of 16 ° to 28 °, and most preferably in the range of 16 ° to 28 °. Further, in the present invention, the nozzle angle is preferably in the range of 20 ° to 27 °, preferably in the range of 20 ° to 25 °, from the viewpoint of further significantly improving the film formation rate. Is more preferable. The nozzle angle is an angle formed by a vertically downward direction and a flow direction of the mist or droplets flowing together with the carrier gas toward the substrate in the nozzle. FIG. 2 shows an example of the nozzle angle. FIG. 2 shows an aspect of a reaction unit in the reaction apparatus of the present invention. The reaction section of FIG. 2 includes a
ノズルの形状は特に限定されないが、前記ミストまたは前記液滴の流れに指向性を与えることができ、かつ前記基体に均一に前記ミストまたは前記液滴を搬送することができる形状であるのが好ましい。例えば、リニアソース型ノズルなどが挙げられる。 The shape of the nozzle is not particularly limited, but it is preferable that the shape is such that directivity can be given to the flow of the mist or the droplet and the mist or the droplet can be uniformly conveyed to the substrate. .. For example, a linear source type nozzle and the like can be mentioned.
前記反応は、前記基体上で、前記ミストまたは液滴が反応さえすればそれでよく、物理的な反応であってもよいし、化学的な反応であってもよい。乾燥による反応であってもよいが、熱による熱反応が好ましく、熱反応は、熱でもって前記ミストまたは液滴が反応すればそれでよく、反応条件等も本発明の目的を阻害しない限り特に限定されない。本発明では、前記熱反応を、通常、650℃以下で行うが、本発明においては、200℃以下が好ましく、75℃以下がより好ましい。本発明においては、このような低温であっても、効率良く前記基体を処理することができる。下限については、本発明の目的を阻害しない限り特に限定されないが、60℃以上が好ましい。また、前記反応は、本発明の目的を阻害しない限り、真空下、非酸素雰囲気下、還元ガス雰囲気下および酸素雰囲気下のいずれの雰囲気下で行われてもよいが、非酸素雰囲気下または酸素雰囲気下で行われるのが好ましい。また、大気圧下、加圧下および減圧下のいずれの条件下で行われてもよいが、本発明においては、大気圧下で行われるのが好ましい。なお、前記処理が成膜処理である場合、成膜する膜の膜厚は、成膜時間を調整することにより、設定することができる。 The reaction may be a physical reaction or a chemical reaction as long as the mist or droplets react on the substrate. Although it may be a reaction by drying, a thermal reaction by heat is preferable, and the thermal reaction may be any reaction as long as the mist or droplets react with heat, and the reaction conditions and the like are particularly limited as long as the object of the present invention is not impaired. Not done. In the present invention, the thermal reaction is usually carried out at 650 ° C. or lower, but in the present invention, 200 ° C. or lower is preferable, and 75 ° C. or lower is more preferable. In the present invention, the substrate can be efficiently treated even at such a low temperature. The lower limit is not particularly limited as long as the object of the present invention is not impaired, but 60 ° C. or higher is preferable. Further, the reaction may be carried out in any of a vacuum, a non-oxygen atmosphere, a reducing gas atmosphere and an oxygen atmosphere as long as the object of the present invention is not impaired, but the reaction may be carried out in a non-oxygen atmosphere or oxygen. It is preferably performed in an atmosphere. Further, it may be carried out under any conditions of atmospheric pressure, pressurization and depressurization, but in the present invention, it is preferably carried out under atmospheric pressure. When the process is a film forming process, the film thickness of the film to be formed can be set by adjusting the film forming time.
上記のようにして処理することにより、工業的有利に、効率良く前記基体を処理することができる。 By treating as described above, the substrate can be treated efficiently in an industrially advantageous manner.
本発明においては、上記の各工程を、原料溶液を霧化または液滴化する霧化・液滴化部、得られたミストまたは液滴をキャリアガスで基体まで搬送する搬送部、ノズルから排出された前記ミストまたは前記液滴を前記基体上で反応させる反応部を備える処理装置であって、ノズル角度が、鉛直下向き方向に対し、1°〜30°の範囲内である処理装置を用いて行うのが好ましい。以下、本発明の処理装置について、成膜材料を用いて成膜処理した例を具体的に挙げて説明する。 In the present invention, each of the above steps is discharged from an atomization / droplet atomization unit that atomizes or droplets the raw material solution, a transport unit that transports the obtained mist or droplets to the substrate with a carrier gas, and a nozzle. Using a processing device including a reaction unit for reacting the mist or the droplets on the substrate, the nozzle angle of which is in the range of 1 ° to 30 ° with respect to the vertical downward direction. It is preferable to do so. Hereinafter, the processing apparatus of the present invention will be specifically described with reference to an example in which a film forming process is performed using a film forming material.
以下、本発明の実施例を説明するが、本発明はこれらに限定されるものではない。 Hereinafter, examples of the present invention will be described, but the present invention is not limited thereto.
(実施例1)
1.処理装置
図1を用いて、本実施例で用いた成膜装置1を説明する。成膜装置1は、キャリアガスを供給するキャリアガス供給源2aと、キャリアガス供給源2aから送り出されるキャリアガスの流量を調節するための流量調節弁3aと、キャリアガス(希釈)を供給するキャリアガス(希釈)供給源2bと、キャリアガス(希釈)供給源2bから送り出されるキャリアガス(希釈)の流量を調節するための流量調節弁3bと、原料液4aが収容されるミスト発生源4と、水5aが入れられる容器5と、容器5の底面に取り付けられた超音波振動子6と、ホットプレート8と、ホットプレート8上に載置された基板10と、ミスト発生源4からノズル7までをつなぐ供給管9と、供給管9と基板10近傍までをつなぐノズル7とを備えている。なお、ノズル7のノズル角度を20°とした。
(Example 1)
1. 1. Processing apparatus The
2.原料溶液の作製
ポリシラザンを酢酸ブチルに混合して希釈したポリシラザン溶液を調整し、さらに、過酸化水素水を体積比で6%含有させて溶液を調整し、これを原料溶液とした。
2. Preparation of raw material solution A polysilazane solution diluted by mixing polysilazane with butyl acetate was prepared, and a solution was prepared by adding 6% by volume of hydrogen peroxide solution, which was used as a raw material solution.
3.成膜準備
上記2.で得られた原料溶液4aをミスト発生源4内に収容した。次に、基板10として、ガラス基板をホットプレート8上に設置し、ホットプレート8を作動させて基板10の温度を75℃にまで昇温させた。次に、流量調節弁3aおよび3bを開いて、キャリアガス供給源2aから供給されるキャリアガスの流量を3.0L/分に、キャリアガス(希釈)供給源2bから供給されるキャリアガス(希釈)の流量を2.0L/分に調節した。なお、キャリアガスとして窒素を用いた。
3. 3. Preparation for film formation 2. The
4.成膜処理
次に、超音波振動子6を2.4MHzで振動させ、その振動を、水5aを通じて原料液4aに伝播させることによって、原料液4aを霧化させてミストを生成した。このミスト4bを、キャリアガスによって、供給管9内およびノズル7を通って、基板10へと搬送し、大気圧下、75℃にて、基板10近傍でミスト4bを反応させ、基板10上にシリコン酸化膜を成膜した。なお、成膜処理時間は15分間であり、膜厚は8.6μmであった。
4. Film formation treatment Next, the ultrasonic vibrator 6 was vibrated at 2.4 MHz, and the vibration was propagated to the
(実施例2)
ノズル7のノズル角度を25°としたこと以外は、実施例1と同様にして、成膜処理を行った。得られた膜の膜厚は、15.68μmであった。
(Example 2)
The film formation process was performed in the same manner as in Example 1 except that the nozzle angle of the
(比較例1)
ノズル7のノズル角度を0°としたこと以外は、実施例1と同様にして、成膜処理を行った。得られた膜の膜厚は、1.0μmであった。
(Comparative Example 1)
The film formation process was performed in the same manner as in Example 1 except that the nozzle angle of the
(実施例3)
ノズル7のノズル角度を5°としたこと以外は、実施例1と同様にして、成膜処理を行った。得られた膜の膜厚は、6.7μmであった。
(Example 3)
The film formation process was performed in the same manner as in Example 1 except that the nozzle angle of the
(実施例4)
ノズル7のノズル角度を10°としたこと以外は、実施例1と同様にして、成膜処理を行った。得られた膜の膜厚は、3.4μmであった。
(Example 4)
The film formation process was performed in the same manner as in Example 1 except that the nozzle angle of the
(実施例5)
ノズル7のノズル角度を15°としたこと以外は、実施例1と同様にして、成膜処理を行った。得られた膜の膜厚は、6.3μmであった。
(Example 5)
The film formation process was performed in the same manner as in Example 1 except that the nozzle angle of the
(実施例6)
ノズル7のノズル角度を30°としたこと以外は、実施例1と同様にして、成膜処理を行った。得られた膜の膜厚は、2.1μmであった。
(Example 6)
The film formation process was performed in the same manner as in Example 1 except that the nozzle angle of the
図3に、実施例1〜6および比較例1における、ノズル角度と膜厚との関係を示す。図3から明らかなように、実施例1〜6ではいずれも成膜速度が優れており、効率良く成膜処理が行うことができることがわかる。 FIG. 3 shows the relationship between the nozzle angle and the film thickness in Examples 1 to 6 and Comparative Example 1. As is clear from FIG. 3, it can be seen that the film forming speed is excellent in each of Examples 1 to 6, and the film forming process can be efficiently performed.
本発明の処理方法は、工業的有利に、効率良く基体を処理することができるため、半導体装置、電子機器等の種々の製造分野に利用可能である。 Since the processing method of the present invention can efficiently process the substrate in an industrially advantageous manner, it can be used in various manufacturing fields such as semiconductor devices and electronic devices.
1 成膜装置
2a キャリアガス供給源
2b キャリアガス(希釈)供給源
3a 流量調節弁
3b 流量調節弁
4 ミスト発生源
4a 原料溶液
4b ミスト
5 容器
5a 水
6 超音波振動子
7 ノズル
8 ホットプレート
9 供給管
10 基板
11 ステージ
12 支柱
1
Claims (15)
The processing apparatus according to any one of claims 9 to 14, wherein the reaction unit includes a heating means.
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