CN1074469C - Atomizing thermolysis process for preparing film - Google Patents
Atomizing thermolysis process for preparing film Download PDFInfo
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- CN1074469C CN1074469C CN98119488A CN98119488A CN1074469C CN 1074469 C CN1074469 C CN 1074469C CN 98119488 A CN98119488 A CN 98119488A CN 98119488 A CN98119488 A CN 98119488A CN 1074469 C CN1074469 C CN 1074469C
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Abstract
The present invention relates to a spraying pyrolysis method for preparing films. Firstly, the method prepares a required metal salt solution, and then the solution is atomized through an air compressing atomizer. The solution is injected in a container where a heated base plate is placed under the drive of current carrying gas, and a solvent is volatilized after a mist body is baked and is further decomposed and deposited on the base plate to be formed into a film. The present invention has the advantages of easy control of a ratio, favorable orientation and extensionality, low cost no need of filming for many times, no heat generation in atomization, stable mist quantity and no need of cooling devices. The method can prepare metal-oxide films.
Description
The present invention relates to a kind of atomizing thermolysis process for preparing film
The technology of preparing of film comprises: physical method, as evaporation, spatter establish, rheotaxy etc.; Chemical process, as chemical vapour deposition, metal organic salt deposition, sol-gel method etc., wherein sol-gel method is one of welcome preparation method.Vying each other of numerous technology promoted various Development of Preparation Technology.Spray heating decomposition is the new preparation method who is attempting at present.Compare with other preparation method, it has the advantage of sol-gel method: low growth temperature, big area deposition and the speed of growth, technology are easy to control stoichiometric ratio faster.In addition, it also has original advantage: good orientation and epitaxy, cost be low, do not need repeatedly plated film.
The object of the invention is the atomizing thermolysis process of the preparation film developed, at first prepare required metal salt solution, pass through Compressed Air Nebulizer then, make solution atomization, spirt is placed with (reaction chamber) in the container that is heated substrate under the drive of current-carrying gas, and the mist body desolvates and further decomposes through volatilization behind the overbaking and is deposited on film forming on the substrate.This method technology is easy to control that stoichiometric ratio, growth temperature are low, the film forming area big, can prepare orientation and epitaxial film, cost is low, do not need repeatedly plated film etc.Owing to adopt Compressed Air Nebulizer, do not need atomisation unit is cooled off, and the concentration of atomized soln is not had selectivity, adopt this method can prepare metal oxide film.
The atomizing thermolysis process of preparation film of the present invention, this method is at first prepared required metal salt solution, pass through Compressed Air Nebulizer then, make solution atomization, spirt is placed with in the container that is heated substrate under the drive of current-carrying gas, and the mist body desolvates and further decomposes through volatilization behind the overbaking and is deposited on film forming on the substrate; Raw materials usedly in the solution be: plumbic acetate, Zircosol ZN, tin protochloride, metatitanic acid four fourth fat; Solvent is methyl glycol, dehydrated alcohol, and additive is acetate, methyl ethyl diketone, hydrochloric acid; Substrate is silicon chip or wave carrier piece; Current-carrying gas is oxygen or nitrogen or air; Preparation PZT thin film solution,
Its component ratio is a mol ratio: plumbic acetate: Zircosol ZN: metatitanic acid four fourth fat=1.05: 0.4: 0.6-1.15: 0.6: 0.4, concentration is 0.1-0.4M, the mol ratio of additive and Pb-based lanthanumdoped zirconate titanates is 0.1-4.0, substrate temperature during thin film deposition is 300 ℃-800 ℃, depositing time 1-60 minute; The preparation tin oxide transparent conductive film, raw materials used tin protochloride, concentration is 0.1-0.4M, and the mol ratio of additive and tin protochloride is 0.1-4.0, and the substrate temperature during thin film deposition is 300 ℃-800 ℃, depositing time 1-60 minute; Adopt Compressed Air Nebulizer when the system film, under the drive of high velocity air, make that the sloped sides place slit in the compressed air atomizer of solution atomizes to the atomizer nozzle place, the mist body enters reaction chamber film forming on substrate.
Referring to accompanying drawing
Fig. 1 is the present invention's thermolysis film coating apparatus of spraying
Fig. 2 is the enough synoptic diagram of spraying gun knot of the present invention
Embodiment 1 (on silicon substrate, depositing PZT thin film)
Preparation Pb-based lanthanumdoped zirconate titanates solution: take by weighing raw material (mol ratio) plumbic acetate: Zircosol ZN: metatitanic acid four fourth fat=1.05: 0.6: 0.4, solvent is a methyl glycol, concentration is 0.1M, the mol ratio of additive acetate and methyl ethyl diketone and Pb-based lanthanumdoped zirconate titanates is 0.1, mix, 300 ℃ of substrate temperatures, current-carrying gas oxygen, depositing time 1 minute, after the compressed air atomizer atomizing of the solution for preparing, under the drive of current-carrying gas, spirt is placed with (reaction chamber) in the container that is heated substrate, and the mist body volatilizees after toasting and desolvates and a step decomposes and to be deposited on film forming on the substrate.On silicon substrate, obtain the film of bright and clean.
Embodiment 2 (on silicon substrate, depositing PZT thin film)
Preparation Pb-based lanthanumdoped zirconate titanates solution: take by weighing raw material (mol ratio) plumbic acetate: Zircosol ZN: metatitanic acid four fourth fat=1.15: 0.4: 0.6, solvent is a dehydrated alcohol, concentration is 0.3M, the mol ratio of additive methyl ethyl diketone and Pb-based lanthanumdoped zirconate titanates is 2.0, mix, 550 ℃ of substrate temperatures, the current-carrying gas air, depositing time 30 minutes, after the compressed air atomizer atomizing of the solution for preparing, under the drive of current-carrying gas, spirt is placed with (reaction chamber) in the container that is heated substrate, and the mist body volatilizees after toasting and desolvates and a step decomposes and to be deposited on film forming on the substrate.On silicon substrate, obtain the film of bright and clean.
Embodiment 3 (on wave carrier piece, depositing tin oxide transparent conductive film)
Obtain solution: raw material is a tin protochloride, solvent is a dehydrated alcohol, and concentration is 0.4M, the mol ratio 4.0 of additive hydrochloric acid and tin protochloride, mix, 800 ℃ of substrate temperatures, current-carrying gas nitrogen, depositing time 60 minutes, after the compressed air atomizer atomizing of the solution for preparing, under the drive of current-carrying gas, spirt is placed with (reaction chamber) in the container that is heated substrate, and the mist body volatilizees after toasting and desolvates and a step decomposes and to be deposited on film forming on the substrate.On wave carrier piece, obtain the film of bright and clean.
Claims (5)
1, a kind of atomizing thermolysis process for preparing film, it is characterized in that, at first prepare required metal salt solution, pass through Compressed Air Nebulizer then, make solution atomization, spirt is placed with in the container that is heated substrate under the drive of current-carrying gas, and the mist body desolvates and further decomposes through volatilization behind the overbaking and is deposited on film forming on the substrate.
2, the atomizing thermolysis process of preparation film according to claim 1 is characterized in that, raw materials usedly in the solution is: plumbic acetate, Zircosol ZN, tin protochloride, metatitanic acid four fourth fat; Solvent is methyl glycol, dehydrated alcohol, and additive is acetate, methyl ethyl diketone, hydrochloric acid; Substrate is silicon chip or wave carrier piece; Current-carrying gas is oxygen or nitrogen or air.
3, the atomizing thermolysis process of preparation film according to claim 2, it is characterized in that, preparation PZT thin film solution, its component ratio is a mol ratio, plumbic acetate: Zircosol ZN: metatitanic acid four fourth fat=1.05: 0.4: 0.6-1.15: 0.6: 0.4, concentration is 0.1-0.4M, and additive is 0.1-4.0 for the mol ratio with Pb-based lanthanumdoped zirconate titanates; Substrate temperature during thin film deposition is 300 ℃-800 ℃, depositing time 1-60 minute.
4, the atomizing thermolysis process of preparation film according to claim 2 is characterized in that, the preparation tin oxide transparent conductive film, and raw materials used is tin protochloride, and concentration is 0.1-0.4M, and additive is 0.1-4.0 for the mol ratio with tin protochloride; Substrate temperature during thin film deposition is 300 ℃-800 ℃, depositing time 1-60 minute.
5, the atomizing thermolysis process of preparation film according to claim 1, it is characterized in that, when the system film, adopt Compressed Air Nebulizer, under the drive of high velocity air, make the sloped sides place slit in the compressed air atomizer of solution atomize to the atomizer nozzle place, the mist body enters reaction chamber film forming on substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98119488A CN1074469C (en) | 1998-10-14 | 1998-10-14 | Atomizing thermolysis process for preparing film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98119488A CN1074469C (en) | 1998-10-14 | 1998-10-14 | Atomizing thermolysis process for preparing film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1250823A CN1250823A (en) | 2000-04-19 |
| CN1074469C true CN1074469C (en) | 2001-11-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN98119488A Expired - Fee Related CN1074469C (en) | 1998-10-14 | 1998-10-14 | Atomizing thermolysis process for preparing film |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1293589C (en) * | 2003-07-23 | 2007-01-03 | 西安理工大学 | Method of making transparent electrode on optical fiber panel surface |
| CN100404142C (en) * | 2006-07-24 | 2008-07-23 | 南开大学 | Thermal decomposing nozzle for ultrasonic spraying |
| CN101245452B (en) * | 2007-12-27 | 2011-05-11 | 北京石油化工学院 | Equipment for producing thin film with whirl coating atomizing thermal decomposition |
| CN101759372B (en) * | 2009-12-31 | 2012-10-10 | 中国科学院广州能源研究所 | Integrative ultrasonic spray pyrolysis coating device |
| CN111293230A (en) * | 2018-12-10 | 2020-06-16 | 广东聚华印刷显示技术有限公司 | Thin film packaging layer and preparation method thereof, and preparation method of display panel |
| CN112813406B (en) * | 2020-12-30 | 2023-07-14 | 武汉工程大学 | Equipment and method for preparing three-dimensional metal simple substance film on surface of special-shaped piece based on CVD technology |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1075173A (en) * | 1992-12-28 | 1993-08-11 | 北京航空航天大学 | A kind of preparation method of Nano thin film |
| CN1090428A (en) * | 1993-01-15 | 1994-08-03 | 山东大学 | The preparation method of bismuth titanate ferro-electricity membrane |
| CN1128403A (en) * | 1994-10-25 | 1996-08-07 | 电子工业部第十二研究所自动工程研究所 | Laser-evaporated thin-film scandium series cathode and its preparation method |
| CN1156765A (en) * | 1996-02-10 | 1997-08-13 | 中国科学技术大学 | Metal organic chemistry vapour phase deposition process for preparing metal and alloy film |
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1998
- 1998-10-14 CN CN98119488A patent/CN1074469C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1075173A (en) * | 1992-12-28 | 1993-08-11 | 北京航空航天大学 | A kind of preparation method of Nano thin film |
| CN1090428A (en) * | 1993-01-15 | 1994-08-03 | 山东大学 | The preparation method of bismuth titanate ferro-electricity membrane |
| CN1128403A (en) * | 1994-10-25 | 1996-08-07 | 电子工业部第十二研究所自动工程研究所 | Laser-evaporated thin-film scandium series cathode and its preparation method |
| CN1156765A (en) * | 1996-02-10 | 1997-08-13 | 中国科学技术大学 | Metal organic chemistry vapour phase deposition process for preparing metal and alloy film |
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| CN1250823A (en) | 2000-04-19 |
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