CN103726028B - A kind of UVCVD prepares ZrO 2the method of coating - Google Patents
A kind of UVCVD prepares ZrO 2the method of coating Download PDFInfo
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- CN103726028B CN103726028B CN201310309133.2A CN201310309133A CN103726028B CN 103726028 B CN103726028 B CN 103726028B CN 201310309133 A CN201310309133 A CN 201310309133A CN 103726028 B CN103726028 B CN 103726028B
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Abstract
The invention provides a kind of method preparing zirconia coating, by with chemical vapor deposition unit, zirconia coating is being prepared under the condition of ultraviolet and nearly vacuum, using the rare gas element such as nitrogen or argon gas as carrier gas, depositing temperature is less than 300 DEG C, and its presoma can be ZrCl (tmhd)
3, ZrCl
2(tmhd)
2(wherein tmhd=2,2,6,6-tetramethyl--3,5-heptane polyester), Zr (OR)
4or ZrCl
4+ H
2one in O, the substrate requirements fusing point of reaction is greater than the metal of 300 DEG C or second-order transition temperature is greater than 300 DEG C of non-metallic material, and ultraviolet wavelength range used is 150nm ~ 400nm.Major advantage of the present invention is: (1) can prepare zirconia coating at a lower temperature, extends the range of choice of matrix, and then also extends the range of application of zirconia coating; (2) started and termination reaction by switch UV-light generating unit, make reaction controllability very strong, be also just conducive to the thickness of coating itself and the control of shape characteristic, be conducive to the preparation of multilayer material; (3) technique is simple, and cheap, practicality is very strong.
Description
Technical field
The present invention relates to a kind of preparation method of coating, particularly a kind of UVCVD prepares ZrO
2the method of coating.
Background technology
Zirconium white (ZrO
2) be a kind of excellent coated material, because it has a series of features such as coefficient of linear expansion is high, thermal conductivity is little, fusing point is high, hardness is large, density is lower, be often used as high-strength abrasion-proof coating and the thermal barrier coating of high-quality, so ZrO
2the preparation of coating receives great concern.
Prepare zirconia coating and have a variety of method, as electrochemical plating, chemical Vapor deposition process, physical vaporous deposition etc. respectively have its relative merits, this wherein chemical Vapor deposition process because having, deposited film device is simple, coating density and purity controlled, easy acquisition gradient deposition thing or mixing coating, the advantage such as easily to carry out at a lower temperature and day by day receive the concern of people.
The Chinese patent of patent No. CN1798618A discloses a kind of ultraviolet and plasma assisted MOCVD system, prepare the method for high-temperature superconducting coating with achieving the continuous high production of Metalorganic Chemical Vapor Deposition, but present method is only applicable to metal organic chemical vapor deposition, precursor is that inorganic salts is then no longer applicable, moreover the present invention does not relate to ZrO yet
2the preparation of coating, so for ZrO
2the preparation of coating then needs to should be regarded as a different matter.
Stable pure monoclinic zirconia coating production and application under the Chinese patent of patent No. CN101219239A also discloses a kind of low temperature, successfully achieve the preparation that less than 100 DEG C preparations have the zirconia coating of biological fitness, but present method needs the particle etc. of ball milling and screening certain diameter, operating procedure is complicated, be difficult to realize industrial quantity-produced requirement, practice have certain limitation.
The chemical gas phase technology described in " UVCVD/UHVCVD technology prepares SiGeHBT material " literary composition of the people such as Dai Xianying with ultraviolet and ultravacuum are assisted prepares SiGe/Si material, there is the feature of low temperature depositing and there is controllability, but what kind of situation the preparation for zirconia material is then needs to should be regarded as a different matter, so this patent uses ultraviolet lower pressure to prepare zirconia coating, not only expand the selectable range as base material when chemical vapour deposition technique prepares zirconia coating, and make the thickness of coating and shape characteristic be more prone to control, coating no longer has the defect caused because of phase transformation, required performance more easily realizes.
Summary of the invention
The invention provides a kind of method preparing zirconia coating, by with chemical vapor deposition unit, zirconia coating is being prepared under the condition of ultraviolet and nearly vacuum, using the rare gas element such as nitrogen or argon gas as carrier gas, depositing temperature is less than 300 DEG C, and its presoma can be ZrCl (tmhd)
3, ZrCl
2(tmhd)
2(wherein tmhd=2,2,6,6-tetramethyl--3,5-heptane polyester), Zr (OR)
4or ZrCl
4+ H
2one in O, the substrate requirements fusing point of reaction is greater than the metal of 300 DEG C or second-order transition temperature is greater than 300 DEG C of non-metallic material, and ultraviolet wavelength range used is 150nm ~ 400nm.
The invention provides a kind of method that UVCVD prepares ZrO2 coating, it is characterized in that the step comprising following order:
(1) ultrasonic cleaning substrate 10 ~ 20min, adds acetone or alcohol during cleaning, dry up after cleaning with nitrogen;
(2) substrate is put into sample table, after first vacuumizing 10 ~ 20min to 10Pa with mechanical pump, then vacuumize 20 ~ 30min to 0.01Pa closure molecule pump with molecular pump;
(3) UV-light generating unit is opened, and logical carrier gas and precursor substance, the flow controlling carrier gas is 30 ~ 400ml/min, and precursor is 1 with the ratio of the flow of carrier gas: (0.5 ~ 15), under 150 ~ 300 DEG C of conditions, deposit 1 ~ 5min;
(4) ZrO is waited until
2coating reaches thickness and the pattern just closedown UV-light generating unit of many requirements, and stops heating, to be cooled to room temperature, taking-up sample.
Major advantage of the present invention is: (1) can prepare zirconia coating at a lower temperature, extends the range of choice of matrix, and then also extends the range of application of zirconia coating; (2) started and termination reaction by switch UV-light generating unit, make reaction controllability very strong, be also just conducive to the thickness of coating itself and the control of shape characteristic, be conducive to the preparation of multilayer material; (3) technique is simple, and cheap, practicality is very strong.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims and limited.
Embodiment 1
Under the condition of ultraviolet and nearly vacuum, preparing zirconia coating, nitrogen buffer gas, depositing temperature is 150 DEG C, and its presoma is ZrCl (tmhd)
3(wherein tmhd=2,2,6,6-tetramethyl--3,5-heptane polyester), the substrate of reaction is thermostable phenolic resin, and ultraviolet wavelength range used is 150nm ~ 400nm.
The invention provides a kind of method that UVCVD prepares ZrO2 coating, it is characterized in that the step comprising following order:
(1) ultrasonic cleaning substrate 10min, adds acetone during cleaning, dries up after cleaning with nitrogen;
(2) substrate is put into sample table, after first vacuumizing 15min to 10Pa with mechanical pump, then vacuumize 20min to 0.01Pa closure molecule pump with molecular pump;
(3) UV-light generating unit is opened, and logical carrier gas and precursor substance, the flow controlling carrier gas is 80ml/min, and precursor is 1: 2 with the ratio of the flow of carrier gas, under 150 DEG C of conditions, deposit 3min;
(4) ZrO is waited until
2coating reaches thickness and the pattern just closedown UV-light generating unit of many requirements, and stops heating, to be cooled to room temperature, taking-up sample.
Embodiment 2
Under the condition of ultraviolet and nearly vacuum, preparing zirconia coating, take argon gas as carrier gas, depositing temperature is 250 DEG C, and its presoma is ZrCl
4+ H
2o (ZrCl4 and H
2in the mixture of O, both amount of substance ratios are 1: 1.5 ~ 3), the substrate of reaction is copper, and ultraviolet wavelength range used is 150nm ~ 400nm.
The invention provides a kind of method that UVCVD prepares ZrO2 coating, it is characterized in that the step comprising following order:
(1) ultrasonic cleaning substrate 15min, adds acetone during cleaning, dries up after cleaning with nitrogen;
(2) substrate is put into sample table, after first vacuumizing 20min to 10Pa with mechanical pump, then vacuumize 25min to 0.01Pa closure molecule pump with molecular pump;
(3) UV-light generating unit is opened, and logical carrier gas and precursor substance, the flow controlling carrier gas is 80ml/min, and precursor is 1: 4 with the ratio of the flow of carrier gas, under 250 DEG C of conditions, deposit 2min;
(4) ZrO is waited until
2coating reaches thickness and the pattern just closedown UV-light generating unit of many requirements, and stops heating, to be cooled to room temperature, taking-up sample.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited thereto, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content not departing from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (4)
1. a UVCVD prepares ZrO
2the method of coating, is characterized in that by with chemical vapor deposition unit, using nitrogen or argon gas as carrier gas, with ZrCl (tmhd)
3, ZrCl
2(tmhd)
2, Zr (OR)
4or ZrCl
4+ H
2one in O is presoma, is less than 300 DEG C, synthesizes ZrO under the nearly vacuum condition of the UV-light of wavelength region 150nm ~ 400nm at depositing temperature
2coating.
2. UVCVD according to claim 1 prepares ZrO
2the method of coating, is characterized in that if use ZrCl
4+ H
2o as precursors, then ZrCl
4with H
2in the mixture of O, both amount of substance ratios are 1: 1.5 ~ 3.
3. UVCVD according to claim 1 prepares ZrO
2the method of coating, is characterized in that the substrate of reacting is the non-metallic material that fusing point is less than the metal of 300 DEG C or second-order transition temperature and is less than 300 DEG C.
4. UVCVD according to claim 1 prepares Z
ro
2the method of coating, is characterized in that the step comprising following order:
(1) ultrasonic cleaning substrate 10 ~ 20min, adds acetone or alcohol during cleaning, dry up after cleaning with nitrogen;
(2) substrate is put into sample table, after first vacuumizing 10 ~ 20min to 10Pa with mechanical pump, then vacuumize 20 ~ 30min to 0.01Pa closure molecule pump with molecular pump;
(3) UV-light generating unit is opened, and logical carrier gas and precursor substance, the flow controlling carrier gas is 30 ~ 400ml/min, and precursor is 1 with the ratio of the flow of carrier gas: (0.5 ~ 15), under 150 ~ 300 DEG C of conditions, deposit 1 ~ 5min;
(4) ZrO is waited until
2coating meets the requirements of thickness and pattern just closes UV-light generating unit, and stops heating, to be cooled to room temperature, takes out sample.
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|---|---|---|---|
| CN201310309133.2A CN103726028B (en) | 2013-07-23 | 2013-07-23 | A kind of UVCVD prepares ZrO 2the method of coating |
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|---|---|---|---|
| CN201310309133.2A CN103726028B (en) | 2013-07-23 | 2013-07-23 | A kind of UVCVD prepares ZrO 2the method of coating |
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| CN103726028A CN103726028A (en) | 2014-04-16 |
| CN103726028B true CN103726028B (en) | 2016-04-06 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1417844A (en) * | 2002-12-10 | 2003-05-14 | 西安电子科技大学 | SiGe/Si Chemical vapor deposition growth process |
| CN2567234Y (en) * | 2002-09-05 | 2003-08-20 | 西安电子科技大学 | Luminous window device for light chemical vapour deposition equipment |
| CN2568672Y (en) * | 2002-09-05 | 2003-08-27 | 西安电子科技大学 | Photochemical gas phase deposition appts. |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5940523A (en) * | 1982-08-31 | 1984-03-06 | Toshiba Corp | Manufacture of semiconductor thin film |
| JPS628519A (en) * | 1985-07-04 | 1987-01-16 | Nec Corp | Formation of impurity diffused layer |
| JP3455171B2 (en) * | 2000-08-30 | 2003-10-14 | 宮崎沖電気株式会社 | Method for manufacturing interlayer insulating film by vacuum ultraviolet light CVD |
-
2013
- 2013-07-23 CN CN201310309133.2A patent/CN103726028B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2567234Y (en) * | 2002-09-05 | 2003-08-20 | 西安电子科技大学 | Luminous window device for light chemical vapour deposition equipment |
| CN2568672Y (en) * | 2002-09-05 | 2003-08-27 | 西安电子科技大学 | Photochemical gas phase deposition appts. |
| CN1417844A (en) * | 2002-12-10 | 2003-05-14 | 西安电子科技大学 | SiGe/Si Chemical vapor deposition growth process |
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| CN103726028A (en) | 2014-04-16 |
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Addressee: TAICANG PAIOU TECHNOLOGY CONSULTATION SERVICE CO., LTD. Document name: Notification of Passing Preliminary Examination of the Application for Invention |
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Address after: 215400 Chengxiang City, Taicang Province town of the People South Road, No. 162, No. Patentee after: TAICANG PAIOU TECHNOLOGY CONSULTATION SERVICE CO., LTD. Address before: Taicang City, Suzhou City, Jiangsu Province, and 215400 Metro Jianxiong Road No. 20 South Road 2 Patentee before: TAICANG PAIOU TECHNOLOGY CONSULTATION SERVICE CO., LTD. |