CN101418428A - Method for improving adhesive performance of SiC-C hydrogen (tritium) resistance coatings to matrix metal material - Google Patents
Method for improving adhesive performance of SiC-C hydrogen (tritium) resistance coatings to matrix metal material Download PDFInfo
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- CN101418428A CN101418428A CNA2008100463474A CN200810046347A CN101418428A CN 101418428 A CN101418428 A CN 101418428A CN A2008100463474 A CNA2008100463474 A CN A2008100463474A CN 200810046347 A CN200810046347 A CN 200810046347A CN 101418428 A CN101418428 A CN 101418428A
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Abstract
The invention discloses a method for improving the cohesiveness of a SiC-C hydrogen resisting coating to a matrix metal material, which belongs to the field of nuclear technology and application. When the SiC-C hydrogen (tritium) resisting coating is prepared on the matrix metal material, an intermediate transition layer is adopted to improve the cohesiveness of the coating to a matrix and to improve the hydrogen (tritium) resisting effect of the SiC-C coating. The method comprises the following steps: performing low-energy particle bombardment on the matrix of the metal material after the polishing and cleaning so as to further remove the surface contamination and activate the surface; and then using a physical vapor deposition technology to deposit the transition layer to further prepare the SiC-C coating on the basis of the transition layer. The method can be performed in a device for preparing the SiC-C coating, and the preparation of the intermediate transition layer can be directly matched with the preparation of the SiC-C coating. After the deposition of the intermediate transition layer, the SiC-C hydrogen (tritium) resisting coating not only can effectively improve the cohesiveness of the coating and the matrix material, but also is advantageous to improve the hydrogen resistance of the coating itself.
Description
Technical field
The invention belongs to the Nuclear Technology and Applications field, relate to a kind of employing deposition intermediate layer and improve the method for SiC-C resistance hydrogen (tritium) coating matrix metal material adhesive performance.
Background technology
It is present putative the safest nuclear waste disposal mode that nuke rubbish is embedded in the permanent disposal storehouse.Spent fuel after the nuclear reaction encapsulates with the stainless steel hold-up vessel.And the tritium that radiates in the spent fuel enters stainless steel base generation gathering easily and causes " hydrogen embrittlement ".Carry out the surface of stainless steel modification, deposition SiC-C resistance hydrogen (tritium) coating is a kind of method that prevents hydrogen embrittlement.And the SiC-C coating is a key factor that influences coating life to the adhesive performance of matrix.
The present disclosed method for preparing carbide mainly contains: publication number is the method that the patent of CN1273152A proposes to prepare with the forging sintering process iron base composite material, with ceramics powder and the component and the fusible alloy powder mixing that can generate carbide ceramics, and make pressed compact and be fixed in mo(U)ld face by the forming method of powder metallurgy, directly with the pressed compact sintering on the foundry goods parent, this coating is used for the reinforcement of piece surface.Publication number proposes to prepare carborundum films with the method for magnetron sputtering on silicon substrate for the CN1594648A patent.Publication number is that the patent of CN101138787A proposes the SiC particle is prefabricated into paste, this paste is adopted the method that the negative pressure casting is oozed to prepare SiC/ steel composite surface material on steel substrate, this coating is suitable for as the surface recombination wear-resistant material under the low-stress abrasive material erosive wear operating mode again.
The application's patent is that the SiC-C coating that adopts intermediate layer will hinder hydrogen (tritium) usefulness is adhered on the metallic matrix better, and can also further improve resistance hydrogen (tritium) effect of SiC-C coating.This amalgamation that is based on middle transition layer material such as copper and carbide ceramics is higher than iron, adds the interfacial bonding property matter that the copper transition layer can improve carbide and iron greatly like this.The preparation of transition layer and SiC-C coating preparation are carried out in same equipment in the method for the present invention, and transition layer can directly cooperate with the preparation of SiC-C coating.
Summary of the invention
The object of the present invention is to provide a kind of method that can improve the SiC-C coating to the metal matrix material adhesive performance.Method by physical vapor deposition deposition intermediate layer between film and matrix makes film mix the interfacial layer of formation composition graded with matrix element, improves the adhesive performance of SiC-C coating to matrix, increases its work-ing life.Find that simultaneously the deposition intermediate layer also helps the raising of SiC-C coating resistance hydrogen (tritium) effect.
The deposition intermediate layer that the present invention proposes such as the method for copper layer can obviously be improved the interface structure between SiC-C coating and the Fe sill.This is because the amalgamation of copper and carbide ceramics is higher than iron, and iron and copper are the homogeneity metals.Simultaneously by ion beam mixing technology promptly under high energy ion bombardment, make transition layer respectively with the melange effect of SiC-C coating and Fe sill generation atom level, method of the present invention can improve the interfacial combined function of SiC-C coating to the Fe sill greatly.
The method for preparing intermediate layer that the present invention proposes comprises the steps:
1) grinding and polishing is carried out on the metal matrix material surface, use cleaning, drying, put into vacuum chamber, be evacuated down to the vacuum tightness of requirement;
2) with ion beam sputtering bombardment or electron beam heating method for scanning matrix surface is cleaned, remove the impurity of matrix surface zone of oxidation and absorption, and make the matrix surface activation;
3) ion beam mixing technology that uses direct current or medium frequency magnetron sputtering deposition to combine with ion beam bombardment prepares intermediate layer;
4) on intermediate layer, adopt similar method to prepare the SiC-C coating;
5) open vacuum chamber, take out sample.
Description of drawings
The second ion mass spectroscopy depth analysis of the SiC-C coating of Fig. 1, no Cu transition layer.
Fig. 2, the second ion mass spectroscopy depth analysis of the SiC-C coating of Cu transition layer is arranged.
SiC-C coating element enters in the transition layer Cu film from Fig. 2 more as can be seen of Fig. 1, Fig. 2, and matrix element Fe also enters in the Cu film, the existence that the Cu film is described makes coating and matrix carry out good atom level to mix, thereby effectively improves the adhesion strength of SiC-C coating to matrix.
Embodiment
Case study on implementation 1:
1) stainless material is a matrix, matrix surface is carried out conventional grinding and polishing after, with acetone, deionized water ultrasonic cleaning, oven dry, put into vacuum workshop then.
2) the base vacuum degree arrives 6 * 10
-4Behind the Pa, use Ar earlier
+Ionic fluid carries out sputter clean, Ar with the direction of miter angle to sample
+Ion beam energy is 3-5keV, and line is 5-10mA.
3) the Cu layer of the method deposition 20nm thickness of usefulness magnetically controlled DC sputtering uses argon ion bombardment to make the Cu element mix Ar with the Fe element
+Ion energy is 40keV, dosage 1 * 10
16Ions/cm
2.
3) the SiC-C coating of medium frequency magnetron sputtering deposition 40nm thickness, condition is: line 150mA, voltage 500-600V, dutycycle 62.5% is bombarded coating with ar-ion beam from vertical direction then, and ion energy is 40keV, bombardment dosage 1 * 10
16Ions/cm
2.
4) continue the film of deposition SiC-C, meet the requirements of thickness after, close the vacuum unit, take out sample.
Case study on implementation 2:
1) stainless material is a matrix, matrix surface is carried out conventional grinding and polishing after, after the ultrasonic cleaning, oven dry, put into vacuum workshop.
2) the base vacuum degree arrives 6 * 10
-4Behind the Pa, the mode that adds heat scan with electron beam is carried out sputter clean to sample. and the energy of electron beam is 20KeV, and beam current density is about 8 * 10
4W/cm
2, sweep velocity is 5mm/min
3) the Cu layer of the method deposition 10nm thickness of usefulness medium frequency magnetron sputtering uses argon ion bombardment then, and the Ar+ ion energy is 30keV, dosage 1 * 10
16Ions/cm
2.
3) the SiC-C coating of medium frequency magnetron sputtering deposition 40nm thickness, condition is: line 150mA, voltage 500-600V, dutycycle 80% is bombarded coating with ar-ion beam from vertical direction then, and ion energy is 40keV, bombardment dosage 1 * 10
16Ions/cm
2.
4) continue the film of deposition SiC-C, meet the requirements of thickness after, close the vacuum unit, take out sample.
Claims (9)
1, the method that adopts the energy particle bombardment to combine with physical gas-phase deposition prepares intermediate layer, this sedimentary intermediate layer not only improves the adhesive performance of SiC-C coating to matrix, and helps the raising of resistance hydrogen (tritium) effect of SiC-C coating.Its feature comprise following some:
1). substrate material surface carries out conventional cleaning, drying to eliminate surperficial foul behind grinding and polishing, put into vacuum chamber, and vacuum chamber base vacuum degree reaches 6 * 10
-4More than the Pa.
2). adopt the physical sputtering method to clean to matrix surface, eliminate surface contamination such as natural oxide film, and activate.
3). adopt physical gas-phase deposite method deposition intermediate layer, after reaching certain thickness, the ion with certain energy bombards again, and this layer material is mixed with matrix.
4). deposit certain thickness SiC-C then, use Ar
+Ion bombardment makes the SiC-C layer mix with transition layer.
5). proceed the preparation of SiC-C coating, to reach desired thickness.
2, method according to claim 1 is characterized in that the matrix metal material can be the Fe sill, also can be nonferrous materials.
3, method according to claim 1 is characterized in that: the material that intermediate layer is used not only can adopt Cu, can also adopt W, Mo etc.
4, method according to claim 1, the cleaning again that it is characterized in that putting into the specimen surface behind the vacuum chamber is by ion beam sputtering cleaning or electron beam scanning heated wash.
5, method according to claim 4, ion beam energy is 20-30KeV when it is characterized in that the ion beam sputtering cleaning, beam current density is at 10mA/cm
2About.
6, method according to claim 4, energy is 15～30KeV when it is characterized in that electron beam scanning cleaning matrix surface, power density is 5 * 10
4～1 * 10
5W/cm
2
7, according to the method for the described deposition transition layer of claim 1, can adopt magnetically controlled DC sputtering when it is characterized in that depositing, also can adopt medium frequency magnetron sputtering, the ion beam mixing technology deposition intermediate layer of ion bombardment is adopted in the deposition back.
8, according to the method for the described deposition transition layer of claim 1, it is characterized in that depositing the transition layer of 10-20nm left and right thickness, be the Ar of 30-80KeV then with energy
+Ion or other inert gas ions bombard, and make transition layer carry out mixing of atom level with matrix.
9, method according to claim 1 when it is characterized in that depositing behind the transition layer the about 30nm of the deposit thickness of SiC-C coating, is used the Ar about 40KeV again
+Ion bombardment makes itself and the mixing of transition layer generation atom level.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100463474A CN101418428A (en) | 2008-10-22 | 2008-10-22 | Method for improving adhesive performance of SiC-C hydrogen (tritium) resistance coatings to matrix metal material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100463474A CN101418428A (en) | 2008-10-22 | 2008-10-22 | Method for improving adhesive performance of SiC-C hydrogen (tritium) resistance coatings to matrix metal material |
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|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102505066A (en) * | 2011-12-26 | 2012-06-20 | 上海工程技术大学 | Method for increasing binding force between titanium nitride coating and steel substrate |
| EP3990954A4 (en) * | 2019-06-26 | 2023-08-02 | Applied Materials, Inc. | Flexible multi-layered cover lens stacks for foldable displays |
-
2008
- 2008-10-22 CN CNA2008100463474A patent/CN101418428A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102505066A (en) * | 2011-12-26 | 2012-06-20 | 上海工程技术大学 | Method for increasing binding force between titanium nitride coating and steel substrate |
| EP3990954A4 (en) * | 2019-06-26 | 2023-08-02 | Applied Materials, Inc. | Flexible multi-layered cover lens stacks for foldable displays |
| US11789300B2 (en) | 2019-06-26 | 2023-10-17 | Applied Materials, Inc. | Flexible multi-layered cover lens stacks for foldable displays |
| EP3990955A4 (en) * | 2019-06-26 | 2023-11-29 | Applied Materials, Inc. | Flexible multi-layered cover lens stacks for foldable displays |
| US11934056B2 (en) | 2019-06-26 | 2024-03-19 | Applied Materials, Inc. | Flexible multi-layered cover lens stacks for foldable displays |
| US11940683B2 (en) | 2019-06-26 | 2024-03-26 | Applied Materials, Inc. | Flexible multi-layered cover lens stacks for foldable displays |
| US11940682B2 (en) | 2019-06-26 | 2024-03-26 | Applied Materials, Inc. | Flexible multi-layered cover lens stacks for foldable displays |
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Open date: 20090429 |