CN104630728A - Method for preparing palladium-copper alloy film - Google Patents
Method for preparing palladium-copper alloy film Download PDFInfo
- Publication number
- CN104630728A CN104630728A CN201510060213.8A CN201510060213A CN104630728A CN 104630728 A CN104630728 A CN 104630728A CN 201510060213 A CN201510060213 A CN 201510060213A CN 104630728 A CN104630728 A CN 104630728A
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- Prior art keywords
- film
- palladium
- matrix
- copper
- copper alloy
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
Abstract
The invention relates to a method for preparing an anti-corrosion alloy film and in particular relates to a method for preparing a palladium-copper alloy film. The method comprises the following steps: by selecting 316L stainless steel as a matrix, grinding and polishing the surface of the matrix, removing oil by using ethyl ether and alcohol, cleaning by using ultrasonic waves, drying, and depositing the film, especially, vacuumizing a vacuum chamber before the film is deposited, introducing high purity argon, accurately controlling the time of opening a baffle on the target by virtue of a computer so as to deposit a palladium film and a copper film; performing furnace cooling on the sample to room temperature after the film deposition is ended; adding the obtained film sample into an electric heating tube type atmosphere furnace, and alloying the metal palladium and metal copper on the 316L stainless steel matrix to form a uniform palladium-copper alloy film by virtue of heat treatment; and performing furnace cooling on the sample to room temperature after the heat treatment is ended. The method refers to a method for preparing the palladium-copper alloy film which is deposited by using a magnetron co-sputtering method and has the advantages of high corrosion resistance, high bonding strength and high temperature oxidation resistance. The film is applied to the stainless steel surface and belongs to the field of surface modification.
Description
Technical field
The present invention relates to a kind of preparation method of alloy firm, be specifically related to a kind of preparation method of palladium-copper alloy film.
Background technology
Stainless material has high chemical stability and excellent comprehensive mechanical performance, makes it in a lot of medium, all have excellent corrosion resistance characteristic, so be used widely at many industrial circles.But stainless solidity to corrosion and rustless property are relative, passivation film on stainless steel surface and the stainless solidity to corrosion of inactivating performance remarkably influenced thereof.Such as in many chemical production equipments, some inorganic acids such as working temperature of sulfuric acid etc. often reaches more than 85 degrees Celsius, because temperature raises, these mineral acids may be just reductibility by oxidative conversion, the passive film of such stainless steel surface will dissolve, and loses the ability of self-repair.The corrosion-resistant of stainless steel in high temperature non-oxygenated medium especially acidic medium is but the problem that annoying scholars always.
In order to solve this problem, Chinese scholars, through studying for many years, tentatively have found several solution, as electro-chemical protection technology, adds the methods such as alloying element; Electro-chemical protection technology relates to problem of environmental pollution, and Addition ofelements effect is not so good, and cost is higher.
For above problem, the present invention utilizes magnetic control co-sputtering coating system, metal refining palladium film and copper metal film is come by the thickness controlling palladium target and a copper target baffle plate opening time control unitary film, by thermal treatment, the palladium metal on stainless steel base and metallic copper alloy are turned to uniform palladium-copper alloy film, improve precision and also improve working efficiency simultaneously, working continuously for production line provides possibility.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of palladium-copper alloy film.The preparation method of the palladium-copper alloy film of high anti-corrosion, high bond strength and high temperature oxidation resisting that a kind of magnetic control co-sputtering method of the party's genealogy of law deposits.This film is applied to stainless steel surface, belongs to field of surface modification.
Technical scheme of the present invention is:
A preparation method for palladium-copper alloy film, a kind of preparation method of palladium-copper alloy film described in it, comprises the following steps:
1), select 316L stainless steel as matrix, matrix surface grinds through sand paper and is polished to 0.5 micron, then uses ether, alcohol and distilled water ultrasonic cleaning 20 minutes respectively, loads vacuum chamber and prepare deposit film after drying;
2), deposit film equipment choosing magnetic control co-sputtering coating system, pure metal palladium (99.99%) and pure metal copper (99.99%), aim at the matrix at upper center place, first by vacuum chamber to 3 × 10 before deposit film simultaneously
-4handkerchief, then passes into high-purity argon gas.The opening time accurately being controlled target overhead gage by computer carries out depositing Pd film and Copper thin film, and its deposition process conditions is: palladium target power output 50-150 watt, copper target power output 40-100 watt; Substrate negative voltage 0-150 lies prostrate, the distance 5-10 centimetre of target and matrix, operating air pressure 0.2-1 handkerchief, and substrate temperature is room temperature-500 degrees Celsius, and matrix rotational velocity is 5-25 rpm.Deposit film terminates rear film sample and cools to room temperature with the furnace;
3), the equipment choosing electrically heated tube-type atmosphere furnace of palladium Copper thin film alloying, obtained above-mentioned film sample is put into atmosphere furnace, be warmed up to 450-600 degree Celsius in argon gas atmosphere with 1 centigrade per minute rate program, keep after 5-10 hour furnace cooling to room temperature.
The preparation method of described a kind of palladium-copper alloy film, first by vacuum chamber to 3 × 10 before described deposit film
-4handkerchief, is then passing into high-purity argon gas, first metal refining palladium membranes on 316L stainless steel base.
The preparation method of described a kind of palladium-copper alloy film, the partial pressure of ar gas in described electrically heated tube-type atmosphere furnace 10 kPas, film sample is cooled to room temperature with atmosphere furnace.Advantage of the present invention and effect are:
Present method is the preparation method of the palladium-copper alloy film of a kind of high anti-corrosion, high bond strength and high temperature oxidation resisting.Film solidity to corrosion and pyro-oxidation resistance be all better than 316L stainless steel.Adopt magnetic control co-sputtering coating system, the method is simple and easy to do, improves production efficiency, for production line operation provides possibility.
Embodiment
By the following examples in detail the present invention is described in detail.
Embodiment 1
1), select 316L stainless steel as matrix, matrix surface grinds through sand paper and is polished to 0.5 micron, then uses ether, alcohol and distilled water ultrasonic cleaning 20 minutes respectively, loads vacuum chamber and prepare deposit film after drying;
2), deposit film equipment choosing magnetic control co-sputtering coating system, pure metal palladium (99.99%) and pure metal copper (99.99%), aim at the matrix at upper center place, first by vacuum chamber to 3 × 10 before deposit film simultaneously
-4handkerchief, then passes into high-purity argon gas.The opening time accurately being controlled target overhead gage by computer carries out depositing Pd film and Copper thin film, first on 316L stainless steel base, deposits layer of metal palladium membranes, and then deposits one deck Copper thin film.Its deposition process conditions is: palladium target power output 50 watts, copper target power output 40 watts; Substrate negative voltage 50 volts, the distance of target and matrix 5 centimetres, operating air pressure 0.2 handkerchief, substrate temperature is 100 degrees Celsius, and matrix rotational velocity is 5 rpms.Deposit film terminates rear film sample and cools to room temperature with the furnace;
3), the equipment choosing electrically heated tube-type atmosphere furnace of palladium Copper thin film alloying, obtain above-mentioned film sample and put into atmosphere furnace, be warmed up to 450 degrees Celsius in argon gas atmosphere with 1 centigrade per minute rate program, keep after 10 hours furnace cooling to room temperature.
Embodiment 2
1), select 316L stainless steel as matrix, matrix surface grinds through sand paper and is polished to 0.5 micron, then uses ether, alcohol and distilled water ultrasonic cleaning 20 minutes respectively, loads vacuum chamber and prepare deposit film after drying;
2), deposit film equipment choosing magnetic control co-sputtering coating system, pure metal palladium (99.99%) and pure metal copper (99.99%), aim at the matrix at upper center place, first by vacuum chamber to 3 × 10 before deposit film simultaneously
-4handkerchief, then passes into high-purity argon gas.The opening time accurately being controlled target overhead gage by computer carries out depositing Pd film and Copper thin film, first on 316L stainless steel base, deposits layer of metal palladium membranes, then deposits and deposit one deck Copper thin film again.Its deposition process conditions is: palladium target power output 100 watts, copper target power output 60 watts; Substrate negative voltage 100 volts, the distance of target and matrix 8 centimetres, operating air pressure 0.6 handkerchief, substrate temperature is 150 degrees Celsius, and matrix rotational velocity is 10 rpms.Deposit film terminates rear film sample and cools to room temperature with the furnace;
3), the equipment choosing electrically heated tube-type atmosphere furnace of palladium-copper alloy thin film alloys, the above-mentioned film sample obtained puts into atmosphere furnace, be warmed up to 500 degrees Celsius in argon gas atmosphere with 1 centigrade per minute rate program, keep after 8 hours furnace cooling to room temperature.
Embodiment 3
1), select 316L stainless steel as matrix, matrix surface grinds through sand paper and is polished to 0.5 micron, then uses ether, alcohol and distilled water ultrasonic cleaning 20 minutes respectively, loads vacuum chamber and prepare deposit film after drying;
2), deposit film equipment choosing magnetic control co-sputtering coating system, pure metal palladium (99.99%) and pure metal copper (99.99%), aim at the matrix at upper center place, first by vacuum chamber to 3 × 10 before deposit film simultaneously
-4handkerchief, then passes into high-purity argon gas.The opening time accurately being controlled target overhead gage by computer carries out depositing Pd film and Copper thin film, first on 316L stainless steel base, deposits layer of metal palladium membranes, then deposits and deposit one deck Copper thin film again.Its deposition process conditions is: palladium target power output 150 watts, copper target power output 90 watts; Substrate negative voltage 150 volts, the distance of target and matrix 10 centimetres, operating air pressure 1 handkerchief, substrate temperature is 450 degrees Celsius, and matrix rotational velocity is 15 rpms.Deposit film terminates rear film sample and cools to room temperature with the furnace;
3), the equipment choosing electrically heated tube-type atmosphere furnace of palladium-copper alloy thin film alloys, the above-mentioned film sample obtained puts into atmosphere furnace, be warmed up to 600 degrees Celsius in argon gas atmosphere with 1 centigrade per minute rate program, keep after 5 hours furnace cooling to room temperature.
Claims (4)
1. a preparation method for palladium-copper alloy film, is characterized in that, said method comprising the steps of:
1), select 316L stainless steel as matrix, matrix surface, after sand paper grinding also polishing, cleans with ether, alcohol and distilled water ultrasonic sound appratus, deposit film after drying respectively;
2), deposit film equipment choosing magnetic control co-sputtering coating system, pure metal palladium and pure metal copper aim at the matrix at upper center place simultaneously, first by vacuum chamber before plated film, then pass into high-purity argon gas; The opening time accurately being controlled target overhead gage by computer carries out depositing Pd film and Copper thin film, and its deposition process conditions is: palladium target power output 50-150 watt, copper target power output 40-100 watt; Substrate negative voltage 0-150 lies prostrate, the distance 5-10 centimetre of target and matrix, operating air pressure 0.2-1 handkerchief, and substrate temperature is room temperature-500 degrees Celsius, and matrix rotational velocity is 5-25 rpm, and plated film terminates rear sample and cools to room temperature with the furnace;
3), the equipment choosing electrically heated tube-type atmosphere furnace of palladium Copper thin film alloying, atmosphere furnace put into by the above-mentioned sample obtained, be warmed up to 450-600 degree Celsius in argon gas atmosphere with 1 centigrade per minute rate program, keep after 5-10 hour furnace cooling to room temperature.
2. the preparation method of a kind of palladium-copper alloy film according to claim 1, is characterized in that, described 316L stainless steel base surface finish to 0.5 micron, then uses ether, alcohol and distilled water ultrasonic cleaning 20 minutes respectively.
3. the preparation method of a kind of palladium-copper alloy film according to claim 1, is characterized in that, first by vacuum chamber to 3 × 10-4 handkerchief before described deposit film, is then passing into high-purity argon gas, first metal refining palladium membranes on 316L stainless steel base.
4. the preparation method of a kind of palladium-copper alloy film according to claim 1, is characterized in that, the partial pressure of ar gas in described electrically heated tube-type atmosphere furnace 10 kPas, film sample is cooled to room temperature with atmosphere furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510060213.8A CN104630728A (en) | 2015-02-05 | 2015-02-05 | Method for preparing palladium-copper alloy film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510060213.8A CN104630728A (en) | 2015-02-05 | 2015-02-05 | Method for preparing palladium-copper alloy film |
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| CN104630728A true CN104630728A (en) | 2015-05-20 |
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| CN201510060213.8A Pending CN104630728A (en) | 2015-02-05 | 2015-02-05 | Method for preparing palladium-copper alloy film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110249225A (en) * | 2017-02-10 | 2019-09-17 | 伊士曼化工公司 | Electrode for electrochemical sensor |
Citations (4)
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|---|---|---|---|---|
| US20080164613A1 (en) * | 2007-01-10 | 2008-07-10 | International Business Machines Corporation | ULTRA-THIN Cu ALLOY SEED FOR INTERCONNECT APPLICATION |
| EP2261905A1 (en) * | 2009-06-12 | 2010-12-15 | Thomson Licensing | Compatible optical recording medium |
| CN102120150A (en) * | 2010-12-08 | 2011-07-13 | 南京工业大学 | Gear type hydrogen-permeable palladium or palladium alloy film and hydrogen separator |
| CN102154635A (en) * | 2011-02-24 | 2011-08-17 | 南京工业大学 | Preparation process of porous stainless steel load-type palladium or palladium alloy membrane |
-
2015
- 2015-02-05 CN CN201510060213.8A patent/CN104630728A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080164613A1 (en) * | 2007-01-10 | 2008-07-10 | International Business Machines Corporation | ULTRA-THIN Cu ALLOY SEED FOR INTERCONNECT APPLICATION |
| EP2261905A1 (en) * | 2009-06-12 | 2010-12-15 | Thomson Licensing | Compatible optical recording medium |
| CN102120150A (en) * | 2010-12-08 | 2011-07-13 | 南京工业大学 | Gear type hydrogen-permeable palladium or palladium alloy film and hydrogen separator |
| CN102154635A (en) * | 2011-02-24 | 2011-08-17 | 南京工业大学 | Preparation process of porous stainless steel load-type palladium or palladium alloy membrane |
Non-Patent Citations (2)
| Title |
|---|
| J.Y.YANG ET AL.: "Preparation and characterization of Pd-Cu/V-15Ni composite membrane for hydrogen permeation", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 乔爱玲: "钯铜合金复合膜的研制及其性能测试", 《中国优秀硕士学位论文全文数据库》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110249225A (en) * | 2017-02-10 | 2019-09-17 | 伊士曼化工公司 | Electrode for electrochemical sensor |
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Application publication date: 20150520 |