CN101413103A - Method for infiltration plating platinum film on zirconium surface - Google Patents
Method for infiltration plating platinum film on zirconium surface Download PDFInfo
- Publication number
- CN101413103A CN101413103A CNA2008102324762A CN200810232476A CN101413103A CN 101413103 A CN101413103 A CN 101413103A CN A2008102324762 A CNA2008102324762 A CN A2008102324762A CN 200810232476 A CN200810232476 A CN 200810232476A CN 101413103 A CN101413103 A CN 101413103A
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- CN
- China
- Prior art keywords
- zirconium
- platinum
- workpiece
- negative bias
- plating
- 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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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 48
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 41
- 238000007747 plating Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000008595 infiltration Effects 0.000 title claims description 16
- 238000001764 infiltration Methods 0.000 title claims description 16
- 238000004544 sputter deposition Methods 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000717 platinum sputter deposition Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000000151 deposition Methods 0.000 abstract description 6
- 230000008021 deposition Effects 0.000 abstract description 5
- 238000009792 diffusion process Methods 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000007733 ion plating Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 28
- 239000000243 solution Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 229910001093 Zr alloy Inorganic materials 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- PKNLNPAQGSYBME-UHFFFAOYSA-N N[Pt]N.N(=O)O Chemical compound N[Pt]N.N(=O)O PKNLNPAQGSYBME-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N hydrofluoric acid Substances F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a method for carrying out diffusion plating on the surface of zirconium. The method comprises the following steps: a pretreated zirconium workpiece is positioned in a vacuum ion plating machine with a heating device; the workpiece is subjected to forvacuum to the pressure of 1*10<-3>Pa, is heated to a temperature of between 500 and 800 DEG C, is kept at the temperature for certain time and is accessed with argon gas; the vacuum degree is adjusted between 1*10<-1>Pa and 9 *10<-1>Pa; the workpiece is loaded with negative bias of between 800 and 2,000 V; a sputtering source with a platinum sputtering target is opened; the negative bias is adjusted between 100 and 500 V; the zirconium workpiece is deposited for certain period of time; the sputtering source is closed; and the zirconium workpiece is taken out till the temperature of the zirconium workpiece is lower than 100 DEG C. Through controlling the parameters of the film plating process, a platinum diffusion layer with thickness of between 0.1 and 10 mu m and a platinum deposition layer with thickness of between 0.1 and 50 mu m can be prepared; and the prepared platinum diffusion layer and a zirconium substrate have no obvious interface and are in metallurgical bonding.
Description
Technical field
The present invention relates to a kind of method of plating metallic film, particularly relate to a kind of method at zirconium surface infiltration plating platinum film.
Background technology
Zirconium is little with its thermal neutron absorption cross section, proper intensity and ductility, good solidity to corrosion become one of main nuclear matter of nuclear industry.Based on the raising that nuclear reactor safety and economy are required, in zirconium alloy surface-coated good conductivity, stablize anti-corrosion platinum coating and can further improve mechanical property and the erosion resistance of zirconium alloy under the reactor high burnup.Be coated with plating platinum film on the zirconium alloy surface and use as electrode, because the intensity height is corrosion-resistant, the catalytic activity height, range of application is also more and more widely in recent years.
The preparation technology of zirconium and alloy surface platinum coating thereof has methods such as electroless plating, aqueous solution plating and fused salt plating at present.As everyone knows, very easily generate stable passive film, coating and matrix can not be combined closely, easily cause defectives such as platinum film layer peeling cracking as the zirconium surface of rare refractory metal.Electroplatinizing all must be handled by the plating front activating, how to corrode with concentration higher nitric acid+hydrofluoric acid system or oxalic acid+sulfuric acid system at present, carries out platinum solution electroplatinizing afterwards.More sophisticated at present solution platinum plating technology is mainly divided acid and alkaline platinum plating two big classes.The main platinum plating solution system that adopts has: with two nitrous acid diamino platinum is that main salt is P salt platinum plating solution; With the hexahydroxy-potassium platinate is the platinum plating solution of main salt; And thionamic acid type platinum plating solution and vitriol platinum plating solution etc.Also have technologies such as prussiate fused salt platinum plating in addition.
Zirconium alloy electroplating surface platinum film existing problems are: (1) is difficult to remove the oxide film on zirconium surface, and galvanized Pt film bonding strength is low, the phenomenon of big area demoulding often occurs; (2) electroplating process is inhaled hydrogen easily, makes the zirconium matrix produce " hydrogen embrittlement "; (3) the electroplatinizing process all follows waste liquid, waste gas and waste sludge discharge to be difficult to solve, and environment is caused severe contamination.
For the method for existing physical vapor deposition (PVD) metallic film since film and body material the degree of mutual diffusion is very low mutually, so sedimentary film bonding strength is lower.This method can not satisfy requirement in nuclear power and electrolysis field at the Pt of zirconium surface deposition film.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and can accurately control platinum film thickness, the platinum that can prepare thickness 0.1～10 μ m expands the method at zirconium surface infiltration plating platinum film of infiltration layer and 0.1～50 μ m platinum settled layer.The platinum film and the zirconium matrix of this method preparation do not have tangible interface, are metallurgical binding, platinum film and zirconium substrate combinating strength height, and the membrane structure densification, defectives such as free of pinholes exist.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method at zirconium surface infiltration plating platinum film, with of the pre-treatment of zirconium workpiece surface through mechanical polishing, oil removing cleaning and dewatered drying, it is characterized in that: will insert the vaccum ion coater that has assisted heating device through pretreated zirconium workpiece, forvacuum to 1 * 10
-3Pa, heated parts to 500 ℃～800 ℃, insulation 10～40min feeds argon gas, regulates vacuum tightness to 1 * 10
-1Pa～9 * 10
-1Pa to workpiece loading negative bias 800～2000V, opens sputtering source 5～40min that the platinum sputtering target is housed; Regulate negative bias to 100～500V, deposit 10～200min again, the zirconium workpiece surface forms the platinum film that the platinum with 0.1～10 μ m expands infiltration layer and 0.1～50 μ m settled layer.
The present invention compared with prior art has the following advantages: the present invention can accurately control platinum film thickness by control rete depositing time, and the platinum that can prepare thickness 0.1～10 μ m expands infiltration layer and 0.1～50 μ m platinum settled layer; The platinum film and the matrix zirconium of preparation do not have tangible interface, are metallurgical binding, the membrane structure densification, and defectives such as free of pinholes exist.
Below by embodiment, the present invention is described in further detail.
Embodiment
Embodiment 1
To insert the vaccum ion coater that has assisted heating device, forvacuum to 1 * 10 through mechanical polishing, oil removing cleaning, the pretreated zirconium workpiece of dewatered drying
-3Pa, with zirconium workpiece heated parts to 500 ℃, insulation 10min feeds pure argon, regulates vacuum tightness to 1 * 10
-1Pa to workpiece loading negative bias 800V, opens the sputtering source 5min that the Pt sputtering target is housed, and the platinum for preparing 0.1 μ m expands infiltration layer; Regulate negative bias to 100V, open the sputtering source 10min that the Pt sputtering target is housed, deposition obtains thickness 0.1 μ m platinum film, closes sputtering source and assisted heating device, takes out after the zirconium workpiece temperature is lower than 100 ℃.After implementing above technological process, can form the platinum film that the platinum with 0.1 μ m expands infiltration layer and 0.1 μ m settled layer on the zirconium surface.
Embodiment 2
To insert the vaccum ion coater that has assisted heating device, forvacuum to 1 * 10 through mechanical polishing, oil removing cleaning, the pretreated zirconium workpiece of dewatered drying
-3Pa, with zirconium workpiece heated parts to 800 ℃, insulation 40min feeds high-purity argon gas, regulates vacuum tightness to 9 * 10
-11a to workpiece loading negative bias 2000V, opens the sputtering source 40min that the Pt sputtering target is housed, and the platinum for preparing 10 μ m expands infiltration layer; Regulate negative bias to 500V, open the sputtering source 200min that the Pt sputtering target is housed, deposition obtains thickness 50 μ m platinum films, closes sputtering source and assisted heating device, takes out after the zirconium workpiece temperature is lower than 100 ℃.After implementing above technological process, can form the platinum film that the platinum with 10 μ m expands infiltration layer and 50 μ m settled layers on the zirconium surface.
Embodiment 3
Will be through mechanical polishing, oil removing cleaning, the pretreated zirconium workpiece of dewatered drying are inserted the vaccum ion coater that has assisted heating device, forvacuum to 1 * 10
-3Pa, with zirconium workpiece heated parts to 500 ℃, insulation 25min feeds high-purity argon gas, regulates vacuum tightness to 6 * 10
-1Pa to workpiece loading negative bias 1200V, opens the sputtering source 30min that the Pt sputtering target is housed, and the platinum for preparing 8 μ m expands infiltration layer; Regulate negative bias to 300V, open the sputtering source 150min that the Pt sputtering target is housed, deposition obtains thickness 40 μ m platinum films, closes sputtering source and assisted heating device, takes out after the zirconium workpiece temperature is lower than 100 ℃.After implementing above technological process, can form the platinum film that the platinum with 8 μ m expands infiltration layer and 40 μ m settled layers on the zirconium surface.
The present invention can be implemented in zirconium surface preparation Au, precious metal plating films such as Ag, Pd by changing the platinum sputtering target material, realizes the modification on metal zirconium surface.
Claims (1)
1. method at zirconium surface infiltration plating platinum film, with of the pre-treatment of zirconium workpiece surface through mechanical polishing, oil removing cleaning and dewatered drying, it is characterized in that: will insert the vaccum ion coater that has assisted heating device through pretreated zirconium workpiece, forvacuum to 1 * 10
-3Pa, heated parts to 500 ℃～800 ℃, insulation 10～40min feeds argon gas, regulates vacuum tightness to 1 * 10
-1Pa～9 * 10
-1Pa to workpiece loading negative bias 800～2000V, opens sputtering source 5～40min that the platinum sputtering target is housed; Regulate negative bias to 100～500V, deposit 10～200min again, the zirconium workpiece surface forms the platinum film that the platinum with 0.1～10 μ m expands infiltration layer and 0.1～50 μ m settled layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102324762A CN101413103B (en) | 2008-11-28 | 2008-11-28 | Method for infiltration plating platinum film on zirconium surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102324762A CN101413103B (en) | 2008-11-28 | 2008-11-28 | Method for infiltration plating platinum film on zirconium surface |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101413103A true CN101413103A (en) | 2009-04-22 |
| CN101413103B CN101413103B (en) | 2010-09-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008102324762A Active CN101413103B (en) | 2008-11-28 | 2008-11-28 | Method for infiltration plating platinum film on zirconium surface |
Country Status (1)
| Country | Link |
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| CN (1) | CN101413103B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787514A (en) * | 2010-03-15 | 2010-07-28 | 南京航空航天大学 | Platinum-group metal coating on surface of refractory metal and preparation method thereof |
| CN111041412A (en) * | 2019-12-07 | 2020-04-21 | 西北有色金属研究院 | Preparation method of interface integrated zirconium or zirconium alloy cladding surface functional coating |
-
2008
- 2008-11-28 CN CN2008102324762A patent/CN101413103B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787514A (en) * | 2010-03-15 | 2010-07-28 | 南京航空航天大学 | Platinum-group metal coating on surface of refractory metal and preparation method thereof |
| CN111041412A (en) * | 2019-12-07 | 2020-04-21 | 西北有色金属研究院 | Preparation method of interface integrated zirconium or zirconium alloy cladding surface functional coating |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101413103B (en) | 2010-09-08 |
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Owner name: XI'AN SAIFUS MATERIAL PROTECTION CO., LTD. Free format text: FORMER OWNER: XIBEI NON-FERROUS METALS RESEARCH INST. Effective date: 20130423 |
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Effective date of registration: 20130423 Address after: Economic and Technological Development Zone Jingwei Metro New Material Industrial Park in Shaanxi Province Jing high road 710200 in the middle of Xi'an City Patentee after: XI'AN SURFACE MATERIAL PROTECTION CO., LTD. Address before: 710016 Shaanxi province Xi'an Weiyang Weiyang Road No. 96 Patentee before: Xibei Non-ferrous Metals Research Inst. |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A method of plating platinum film on zirconium surface Effective date of registration: 20200825 Granted publication date: 20100908 Pledgee: Weiyang sub branch of Shaanxi qinnong Rural Commercial Bank Co., Ltd Pledgor: XI'AN SURFACE MATERIAL PROTECTION Co.,Ltd. Registration number: Y2020610000130 |
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Date of cancellation: 20220216 Granted publication date: 20100908 Pledgee: Weiyang sub branch of Shaanxi qinnong Rural Commercial Bank Co.,Ltd. Pledgor: XI'AN SURFACE MATERIAL PROTECTION Co.,Ltd. Registration number: Y2020610000130 |
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