CN106757216B - A kind of preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer and its product of preparation - Google Patents
A kind of preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer and its product of preparation Download PDFInfo
- Publication number
- CN106757216B CN106757216B CN201611153421.3A CN201611153421A CN106757216B CN 106757216 B CN106757216 B CN 106757216B CN 201611153421 A CN201611153421 A CN 201611153421A CN 106757216 B CN106757216 B CN 106757216B
- Authority
- CN
- China
- Prior art keywords
- vanadium
- vanadium alloy
- tritium
- alloy
- preparation
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/66—Electroplating: Baths therefor from melts
- C25D3/665—Electroplating: Baths therefor from melts from ionic liquids
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/12—Oxidising using elemental oxygen or ozone
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Electroplating Methods And Accessories (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention discloses a kind of preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer and its products of preparation, when purpose is to solve vanadium alloy as fusion reactor blanket structural material, radioactivity tritium easily passes through diffusion and penetrates into cladding structure material, or it is penetrated into other systems or environment by structural material, cause the radioactive pollution of tritium, waste of fuel, material hydrogen embrittlement and the crisp cause material plasticity of helium reduce, brittle fracture even occur, and hydrogen/tritium fires, and in certain situations it is desirable to vanadium-base alloy has the problem of certain insulation performance.Using the present invention, VAl/Al can be formed on vanadium-base alloy surface2O3Coating, the coating have both anti-tritium diffusion and electric insulation functions, effectively overcome defect present in existing alloy.It is prepared by the present invention to contain VAl/Al2O3The vanadium-base alloy of coating have preferable anti-tritium diffusion, be particularly suitable for fusion reactor produce tritium covering in vanadium-base alloy large-scale application demand, for fusion reactor tritium control oneself, economy, safety guarantee be of great significance.
Description
Technical field
The invention belongs to the surface treatment of vanadium alloy structural material in protective materials field, especially fusion reactor and national defence and
Protection field, the preparation method of specially a kind of vanadium alloy surface resistance tritium-permeation electric insulation coating layer and its product of preparation.This hair
The material coating of bright preparation has both resistance tritium infiltration and electrical insulation capability, is particularly suitable for fusion reactor and produces large scale, labyrinth covering
The surfaces externally and internally of component is handled, with good application prospect.
Background technique
Vanadium-base alloy not only has the advantages that fast neutron absorption cross-section is small, good to liquid metal corrosion stability, but also has good
The characteristics such as good intensity and plasticity, processing performance and Flouride-resistani acid phesphatase embrittlement/swelling, are times important in fusion reactor and national defence
Structural material is selected, is with a wide range of applications.Especially the ferromagnetism of RAFM steel can not to deuterium tritium plasma influence on system operation
Ignore and SiCfIn the case of the brittleness of/SiC ceramic matrix composite material can not receive, vanadium alloy will uniquely be had both nonferromagnetic and prolong
The fusion reactor structural material of malleability energy, thus get more and more people's extensive concerning.
However, can all face hydrogen and its same position whether using vanadium-base alloy as the first wall or cladding structure material
The invasion of plain deuterium, tritium.Since with low atomic radius and stronger reactivity, radioactivity tritium, which easily passes through to spread, penetrates into covering
Structural material, or penetrated into other systems or environment by structural material, cause the radioactive pollution, waste of fuel and material of tritium
The hydrogen embrittlement and helium of material are crisp etc., so as to cause material plasticity reduction, or even brittle fracture occur.Meanwhile tritium has easy as hydrogen
Combustion, explosive characteristic.More seriously, hydrogen isotope permeability in vanadium alloy is higher than RAFM and SiCfThe candidate knot such as/SiC
It is more than 2 orders of magnitude of structure material.Accordingly, it is considered to which the tritium to fusion reactor controls oneself, economy, safety and environment friendly are wanted
It asks, tritium and its isotope must be reduced or eliminated by the intrusion and infiltration of vanadium alloy.
Currently, coating resistance tritium coating on structural material surface is other than reliably containing and relating to the design of tritium system structure
Reduce one of the most effective measure of tritium-permeation.In addition, coating should also need have electrical insulating property in liquid lithium lead covering, with resistance
Hinder liquid lithium lead and structural material conductive, reduces magnetohydrodynamics (MHD) effect.
For this purpose, there is an urgent need to a kind of new materials or method, to solve the above problems.
Summary of the invention
It is an object of the invention to: when for vanadium alloy as fusion reactor blanket structural material, radioactivity tritium easily passes through
Cladding structure material is penetrated into diffusion, or is penetrated into other systems or environment by structural material, causes the radioactive pollution of tritium,
Waste of fuel, material hydrogen embrittlement and the crisp cause material plasticity of helium reduce, even generation brittle fracture and hydrogen/tritium fires, Yi Ji
In some cases, it needs vanadium-base alloy to have the problem of certain insulation performance, it is exhausted to provide a kind of vanadium alloy surface resistance tritium-permeation electricity
The preparation method of edge coating and its product of preparation.Using method of the invention, it is possible in vanadium-base alloy surface formation VAl/
Al2O3Coating, the coating have both anti-tritium diffusion and electric insulation functions, effectively overcome defect present in existing alloy.System of the present invention
Standby contains VAl/Al2O3The vanadium-base alloy of coating has preferable anti-tritium diffusion, is particularly suitable for fusion reactor and produces vanadium base in tritium covering
The large-scale application demand of alloy, economy self-holding for the tritium of fusion reactor, safety and the guarantee of environment friendly have weight
Want meaning.And VAl/Al on vanadium-base alloy2O3The application that insulation performance possessed by coating is then able to satisfy liquid lithium lead covering needs
It asks, there is preferable application effect.Meanwhile production procedure of the present invention is simple, and it is easy to operate, it can satisfy industrialization and answer on a large scale
Demand, with good application prospect.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer, includes the following steps:
(1) it pre-processes
After carrying out oil removing, deoxidation film process respectively to fine aluminium, vanadium alloy, pretreatment is completed, it is spare；
(2) ionic liquid is aluminized
Using fine aluminium as anode, step (1) pretreated vanadium alloy is cathode, carries out permanent electricity using ionic liquid galvanoplastic
Galvanic electricity plating, the cathode after plating is cleaned, and obtains plating aluminum-vanadium alloy；
(3) it is heat-treated
Plating aluminum-vanadium alloy prepared by step (2) is subjected to diffusion into the surface heat treatment in air furnace, is formed on its surface VAl
Alloy coat, furnace are cold；
(4) oxidation processes
In reacting furnace, under the conditions of oxidizing atmosphere, the plating aluminum-vanadium alloy after step (3) heat treatment is subjected to the painting of VAl alloy
Layer high temperature oxidation process is to get product.
In the step 1, vanadium alloy is V-aCr-bTi alloy, and a is that 4~5, b is 4~5.
In the step 1, phosphoric acid, methanol, acetone and dehydrated alcohol ultrasonic cleaning is respectively adopted in fine aluminium, to remove fine aluminium table
The oxidation film layer and greasy dirt in face complete pretreatment.
In the step 1, when being activated to vanadium alloy, using vanadium alloy as anode, using fine aluminium as cathode, using ionic liquid
Body constantly rinses anode and cathode, the processing of constant potential anode activation is carried out, to remove the oxidation film on vanadium alloy surface.
In the step 1, when carrying out constant potential anode activation to vanadium alloy, the current potential of vanadium alloy matrix is greater than 1.25V
(Vs.Al), 30~60min of time is handled.
In the step (2), the current density of constant current plating is 16~24mA/cm2, electroplating time is 50~80min.
In the step (2), in constant current plating, ionic liquid is stirred, stirring rate is 100~200r/
min。
In the step (2), using step (1) pretreated fine aluminium as anode, step (1) pretreated vanadium alloy is
Cathode, constantly rinsed using ionic liquid anode and cathode carry out constant current plating, by the cathode after plating using organic solvent,
After deionized water is cleaned, plating aluminum-vanadium alloy is obtained.
In the step (2), with anhydrous AlCl3It is raw material with chlorination alkyl imidazole, stirs evenly after dissolving to get ion
Liquid electroplate liquid.
The AlCl3Molar ratio with chlorination alkyl imidazole is 1.5~2.5:1.
The chlorination alkyl imidazole is 1-ethyl-3-methyl-imidazolium chloride.
The AlCl3Molar ratio with chlorination alkyl imidazole is 2:1.
In the step 3, the temperature of heat treatment is 950~1050 DEG C, and heat treatment time is 1~2h.
In the step 4, the temperature of high temperature oxidation process is 950~1050 DEG C, 0.5~1h of oxidization time；
Oxidizing atmosphere refers to the gaseous mixture of oxygenous low vacuum environment or Ar and O2, and partial pressure of oxygen is 10~15Pa.
In the step 4, successively it is cleaned by ultrasonic, after drying using mechanical polishing, acetone and dehydrated alcohol, then to heat treatment
Plating aluminum-vanadium alloy afterwards carries out oxidation processes.
Using product prepared by preceding method, the surface of the vanadium-base alloy is provided with VAl/Al2O3Coating.
For foregoing problems, the present invention provide a kind of vanadium alloy surface resistance tritium-permeation electric insulation coating layer preparation method and its
The product of preparation.Applicant has found there is the Al of Al alloy transition layer when studying2O3Coating (AlM/Al2O3, M is matrix element) be
Comprehensive performance is good, most has the resistance tritium types of coatings of practical prospect.For this purpose, applicant combines the characteristics of vanadium alloy itself, pass through
The vanadium alloy with resistance tritium-permeation electric insulation coating layer of the invention is successfully prepared in mutual cooperation between step.Inventor is first
Vanadium alloy is pre-processed, then in the certain thickness aluminium layer of vanadium alloy electroplating surface, obtains VAl alloy-layer thereafter by heat treatment,
Then Al is prepared through peroxidating2O3Film, to obtain the VAl/Al for having both resistance tritium-permeation and electrical isolation2O3Coating.
In the present invention, vanadium alloy basis material is V- (4~5) Cr- (4~5) Ti alloy.Firstly, being pre-processed.Fine aluminium
Phosphoric acid, methanol, acetone and dehydrated alcohol ultrasonic cleaning need to be respectively adopted, remove the oxidation film layer and greasy dirt on surface.And vanadium alloy
Deoxidation film process is carried out after going oil processing, then with anode activation method.Wherein, anode activation method need to be using fine aluminium as cathode, vanadium
Based alloy is anode, constantly rinses anode and cathode using ionic liquid, carries out the processing of constant potential anode activation.It is preprocessed
Afterwards, it then carries out ionic liquid and aluminizes processing, obtain plating aluminum-vanadium alloy.While rinsing, ionic liquid is stirred, ion
The stirring rate of liquid is preferably 100~200r/min；Plating times are 50~80min.
Wherein, ionic liquid aluminize use ionic liquid with anhydrous AlCl3It is made after stirring evenly dissolution with organic salt.
Wherein, organic salt is chlorination alkyl imidazole.Preferably, chlorination alkyl imidazole is 1-ethyl-3-methyl-imidazolium chloride.Chlorination 1-
No. CAS of methyl -3- ethyl imidazol(e) are as follows: 65039-09-0, English abbreviation EMIC.
Then, diffusion into the surface heat treatment then by plating aluminum-vanadium alloy prepared by step (2) is carried out in air furnace, on its surface
VAl alloy coat is formed, and cooling in air furnace.Heat treatment temperature is 950~1050 DEG C, and heat treatment time is 1~2h.
Finally, under the conditions of oxidizing atmosphere, the plating aluminum-vanadium alloy after step (3) heat treatment is carried out VAl conjunction in reacting furnace
Gold plating high temperature oxidation process is to get product.Oxidizing temperature is 950~1050 DEG C, 0.5~1h of oxidization time.Oxidizing atmosphere: oxygen
10~15Pa is divided, the low vacuum environment of logical oxygen is can be, Ar and O can also be used2Gaseous mixture.
Preferably, first successively being mechanically polished, acetone and anhydrous second before vanadium alloy oxidation after step 3 heat treatment
Alcohol ultrasonic cleaning, drying.
Using the present invention, applicant's success prepares resistance tritium-permeation electric insulation coating layer on vanadium alloy surface, yet there are no
Vanadium-base alloy surface is about VAl/Al2O3Hinder the preparation of tritium coating and the relevant report of performance study and patent.Through practical application,
Using the present invention, the α-Al of V (Al, Cr, the Ti) diffusion layer and hundred nano-scale thickness by micron order thickness can be obtained2O3Outer layer composition
VAl/Al2O3Composite coating, compact structure are well combined with matrix；Coating make the deuterium permeability reduction 2 of V-5Cr-5Ti~
3 orders of magnitude, electrical insulation capability reach 102Ω.m2More than.The present invention, around plating property, is particularly suitable for fusion reactor production with excellent
The surfaces externally and internally processing of large scale, labyrinth cladding feature.Meanwhile the present invention provides the product using this method preparation, it should
Product is especially suitable for the demand that fusion reactor produces the large-scale production of tritium covering labyrinth surface coatings industryization, for ensureing fusion
The tritium of heap controls oneself, economy, safety and environment friendly are of great significance.
Detailed description of the invention
Examples of the present invention will be described by way of reference to the accompanying drawings, in which:
Fig. 1 is Al coating cross-section photograph in the embodiment of the present invention 1.
Fig. 2 is the VAl layer cross section photo of sample after being heat-treated in the embodiment of the present invention 1.
Fig. 3 is the VAl/Al of sample after aoxidizing in the embodiment of the present invention 12O3Coating cross sections photo.
Fig. 4 is the object phase testing result of sample after aoxidizing in the embodiment of the present invention 1.
Fig. 5 is the resistance tritium-permeation performance test results of sample after aoxidizing in the embodiment of the present invention 1.
Fig. 6 is VAl/Al after aoxidizing in the embodiment of the present invention 22O3Coating cross sections photo.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other
Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
?.
Embodiment 1 is in the surface V-5Cr-5Ti prepares coating
The specific operation process of the present embodiment is as follows.
1) taking long and width is 20mm, with a thickness of the V-5Cr-5Ti piece of 2mm, after first using conventional method degreasing, by sample
The AlCl being put into argon gas gloves for protection case3- EMIC (molar ratio 2:1) solution (i.e. ionic liquid) carries out at 25 DEG C of room temperature
Anodization, current potential 1.25V (Vs.Al) activate 60min deoxidation film.Wherein, it when being activated to vanadium alloy, is closed with vanadium
Gold is anode, using fine aluminium as cathode, constantly rinses anode and cathode using ionic liquid, carries out the processing of constant potential anode activation,
To remove the oxidation film on vanadium alloy surface.
2) the V-5Cr-5Ti alloy after step 1 anodization is put into AlCl3- EMIC (molar ratio 2:1) solution,
At 25 DEG C of room temperature, aluminize.Reaction condition is as follows: current density 24mA/cm2, ionic liquid stirring rate 200r/min, plating
Cover 50min.After plating, obtaining aluminium coat thickness is about 20 μm (Fig. 1), and coating is excellent in conjunction with matrix.
3) sample prepared by step 2 is heat-treated, 950 DEG C of temperature in air furnace, keeps the temperature 2h, obtains VAl alloy
Layer, the thickness of the Val alloy-layer is about 30 μm (Fig. 2).
4) by the sample after step 3 heat treatment 1.2 × 105Under Ar gas (partial pressure of oxygen 10Pa) protection of Pa, 950 DEG C of oxidations
1h obtains VAl/Al2O3Coating (as shown in Figure 3), it can be seen that VAl/Al2O3Coating structure is fine and close, is well combined with matrix
Such as, by V (Al, Cr, the Ti) diffusion layer of micron order thickness and the α-Al of hundred nano-scale thickness2O3Outer layer composition such as Fig. 4.
After measured, in the present embodiment, VAl/Al2O3Coating makes 2~3 orders of magnitude of deuterium permeability reduction of V-5Cr-5Ti such as
Fig. 5, electrical insulating property reach 102Ω.m2More than.
Embodiment 2 is in the surface V-4Cr4Ti prepares coating
The specific operation process of the present embodiment is as follows.
1) taking long and width is 20mm, with a thickness of the V-4Cr-4Ti piece of 2mm, after first using conventional method degreasing, by sample
The AlCl being put into argon gas gloves for protection case3- EMIC (molar ratio 2:1) solution carries out anodization at 25 DEG C of room temperature, electricity
Position 1.25V (Vs.Al) activates 30min deoxidation film.Wherein, when being activated to vanadium alloy, using vanadium alloy as anode, with pure
Aluminium is cathode, constantly rinses anode and cathode using ionic liquid, the processing of constant potential anode activation is carried out, to remove vanadium alloy table
The oxidation film in face.
2) sample after step 1 anodization is put into AlCl3In-EMIC (molar ratio 2:1) solution, at room temperature,
It aluminizes.When plating aluminum, fine aluminium is anode, and step (1) pretreated vanadium alloy is cathode, is constantly rushed using ionic liquid
It washes anode and cathode and carries out constant current plating；While rinsing, ionic liquid is stirred.Plating conditions are as follows: electric current
Density 16mA/cm2, ionic liquid stirring rate 100r/min, plating 80min.After plating, obtaining aluminium coat thickness is about
20 μm, coating is excellent in conjunction with matrix.
3) sample prepared by step 2 is heat-treated, 1050 DEG C of temperature in air furnace, keeps the temperature 1h, obtains VAl alloy
Layer, the thickness of the Val alloy-layer is about 30 μm.
4) by the sample after step 3 heat treatment 1.5 × 104Under Ar gas (partial pressure of oxygen 15Pa) protection of Pa, 1050 DEG C of oxygen
Change 1h, obtains VAl/Al2O3Coating.
After measured, in the present embodiment, VAl/Al2O3The XRD testing result of coating is similar to Example 1, still by micron order thickness
V (Al, Cr, Ti) diffusion layer and hundred nano-scale thickness α-Al2O3Outer layer forms (as shown in Figure 6).VAl/Al2O3Coating makes V-
2~3 orders of magnitude of deuterium permeability reduction of 5Cr-5Ti, electrical insulating property reach 102Ω.m2More than.
Embodiment 3 is in the surface column V-5Cr-5Ti prepares coating
The specific operation process of the present embodiment is as follows.
1) diameter 20mm, the column V-5Cr-5Ti of height 50mm are taken, first using after conventional method degreasing, sample is put into
AlCl in argon gas gloves for protection case3- EMIC (molar ratio 2:1) solution carries out anodization, current potential at 25 DEG C of room temperature
1.25V (Vs.Al) activates 60min deoxidation film.Wherein, when being activated to vanadium alloy, using vanadium alloy as anode, with fine aluminium
For cathode, anode and cathode is constantly rinsed using ionic liquid, the processing of constant potential anode activation is carried out, to remove vanadium alloy surface
Oxidation film.
2) sample after step 1 anodization is put into AlCl3In-EMIC (molar ratio 2:1) solution, at room temperature,
It aluminizes.When plating aluminum, using fine aluminium as anode, step (1) pretreated vanadium alloy is cathode, continuous using ionic liquid
It rinses anode and cathode and carries out constant current plating；While rinsing, ionic liquid is stirred.Plating conditions are as follows: electricity
Current density 20mA/cm2, ionic liquid stirring rate 200r/min, plating 60min obtain 20 μm of aluminium coats, coating and matrix knot
It closes excellent.
3) sample prepared by step 2 is heat-treated, 950 DEG C of temperature in air furnace, keeps the temperature 2h, obtains VAl alloy
Layer, the thickness of the Val alloy-layer is about 30 μm.
4) by the sample after step 3 heat treatment 1.2 × 105Under Ar gas (partial pressure of oxygen 10Pa) protection of Pa, 950 DEG C of oxidations
1h obtains VAl/Al2O3Coating.
After measured, in the present embodiment, the coating interface and XRD and section testing result of sample are similar to Example 1, VAl/
Al2O3Coating makes 2 orders of magnitude of deuterium permeability reduction of V-5Cr-5Ti, and electrical insulation capability reaches 102Ω.m2。
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (5)
1. a kind of preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer, which comprises the steps of:
(1) it pre-processes
After carrying out oil removing, deoxidation film process respectively to fine aluminium, vanadium alloy, pretreatment is completed, it is spare；
(2) ionic liquid is aluminized
Using fine aluminium as anode, step (1) pretreated vanadium alloy is cathode, carries out constant current electricity using ionic liquid galvanoplastic
Plating, the cathode after plating is cleaned, and obtains plating aluminum-vanadium alloy；
(3) it is heat-treated
Plating aluminum-vanadium alloy prepared by step (2) is subjected to diffusion into the surface heat treatment in air furnace, is formed on its surface the conjunction of vanadium aluminium
Gold plating, furnace are cold；
(4) oxidation processes
In reacting furnace, under the conditions of oxidizing atmosphere, it is high that the plating aluminum-vanadium alloy after step (3) heat treatment is subjected to vananum coating
Warm oxidation processes are to get product；
In the step (1), vanadium alloy is V-aCr-bTi alloy, and a is that 4~5, b is 4~5:
In the step (2), the current density of constant current plating is 16~24mA/cm2, electroplating time is 50~80min；
In the step (2), with anhydrous AlCl3It is raw material with chlorination alkyl imidazole, stirs evenly after dissolving to get ionic liquid
Electroplate liquid；
In the step (2), in constant current plating, ionic liquid is stirred, stirring rate is 100~200r/min；
In the step (3), the temperature of heat treatment is 950~1050 DEG C, and heat treatment time is 1~2h；
In the step (4), the temperature of high temperature oxidation process is 950~1050 DEG C, 0.5~1h of oxidization time；
Oxidizing atmosphere refers to oxygenous low vacuum environment or Ar and O2Gaseous mixture, partial pressure of oxygen be 10~15Pa.
2. the preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer according to claim 1, which is characterized in that described
In step (1), when being activated to vanadium alloy, using vanadium alloy as anode, using fine aluminium as cathode, constantly rinsed using ionic liquid
Anode and cathode carries out the processing of constant potential anode activation, to remove the oxidation film on vanadium alloy surface.
3. the preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer according to claim 1, which is characterized in that described
In step (1), when carrying out constant potential anode activation to vanadium alloy, the current potential of vanadium alloy matrix is greater than 1.25V Vs.Al, when processing
Between 30~60min.
4. the preparation method of any one vanadium alloy surface resistance tritium-permeation electric insulation coating layer according to claim 1~3, feature
It is, the AlCl3Molar ratio with chlorination alkyl imidazole is 1.5~2.5:1.
5. the surface of the vanadium-base alloy is provided with V- using product prepared by any one of preceding claims 1-4 the method
Al/Al2O3Coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611153421.3A CN106757216B (en) | 2016-12-14 | 2016-12-14 | A kind of preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer and its product of preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611153421.3A CN106757216B (en) | 2016-12-14 | 2016-12-14 | A kind of preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer and its product of preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106757216A CN106757216A (en) | 2017-05-31 |
| CN106757216B true CN106757216B (en) | 2019-03-19 |
Family
ID=58888677
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611153421.3A Active CN106757216B (en) | 2016-12-14 | 2016-12-14 | A kind of preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer and its product of preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106757216B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109451605B (en) * | 2018-10-29 | 2021-03-16 | 温州科博达汽车部件有限公司 | Surface treatment method for electric heating belt of preheater |
| CN113978056A (en) * | 2021-10-15 | 2022-01-28 | 北京科技大学 | Vanadium alloy |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0508479B1 (en) * | 1991-04-10 | 1995-10-25 | Kawasaki Steel Corporation | Corrosion resistant Zn or part-Zn plated steel sheet and method of producing the same |
| CN101845645A (en) * | 2009-07-30 | 2010-09-29 | 浙江大学 | Method for preparing hydrogen permeation preventing coating by aluminizing by adopting room temperature fused salt |
| CN103422039A (en) * | 2012-05-22 | 2013-12-04 | 核工业西南物理研究院 | Method for reinforcing V-4Cr-4Ti alloy |
| CN104499013A (en) * | 2014-12-19 | 2015-04-08 | 中国工程物理研究院材料研究所 | Room temperature ionic liquids electroplating method for electroplating aluminum on RAFM (Reduced Activation Ferritic/martensitic) steel surface |
| CN105154878A (en) * | 2015-07-24 | 2015-12-16 | 中国科学院等离子体物理研究所 | Method for preparing alpha-Al2O3 hydrogen permeation prevention and corrosion-resistant insulation layer |
-
2016
- 2016-12-14 CN CN201611153421.3A patent/CN106757216B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0508479B1 (en) * | 1991-04-10 | 1995-10-25 | Kawasaki Steel Corporation | Corrosion resistant Zn or part-Zn plated steel sheet and method of producing the same |
| CN101845645A (en) * | 2009-07-30 | 2010-09-29 | 浙江大学 | Method for preparing hydrogen permeation preventing coating by aluminizing by adopting room temperature fused salt |
| CN103422039A (en) * | 2012-05-22 | 2013-12-04 | 核工业西南物理研究院 | Method for reinforcing V-4Cr-4Ti alloy |
| CN104499013A (en) * | 2014-12-19 | 2015-04-08 | 中国工程物理研究院材料研究所 | Room temperature ionic liquids electroplating method for electroplating aluminum on RAFM (Reduced Activation Ferritic/martensitic) steel surface |
| CN105154878A (en) * | 2015-07-24 | 2015-12-16 | 中国科学院等离子体物理研究所 | Method for preparing alpha-Al2O3 hydrogen permeation prevention and corrosion-resistant insulation layer |
Non-Patent Citations (5)
| Title |
|---|
| An advance process ofaluminum rich coating as tritium permeation barrier on 321 steel workpiece;Zhang GK et al;《Fusion Engineering and Design》;20120418(第87期);第1370-1375页 |
| Fabrication and characterization of aluminide coating on V-5Cr-5Ti by electrodeposition and subsequent heat treating";Xuexing Peng et al;《International Journal of HYDROGEN ENERGY》;20160430(第41期);第8935-8945页 |
| FeAl-Al2O3阻氚层的制备新方法与性能;张桂凯 等;《稀有金属材料与工程》;20110615;第40卷(第6期);第1120-1124页 |
| Tritium permeation barrier-aluminized coating prepared by Al-plating and subsequent oxidation process;Zhang Guikai et al;《Journal of Nuclear Materials》;20110101(第417期);第1245-1248页 |
| V-5Cr-5Ti在AlC3-EMIC离子液体中的阳极活化及表面铝沉积;彭雪星 等;《原子能科学技术》;20161015;第50卷(第10期);第1902-1908页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106757216A (en) | 2017-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xia et al. | Electrochemical studies of AC/DC anodized Mg alloy in NaCl solution | |
| Bockris et al. | Comprehensive treatise of electrochemistry | |
| CN108570703B (en) | Preparation method of tungsten/copper laminated composite material based on tungsten sheet surface nanocrystallization | |
| CN106757216B (en) | A kind of preparation method of vanadium alloy surface resistance tritium-permeation electric insulation coating layer and its product of preparation | |
| CN104562128B (en) | A kind of method for preparing thermal protection ceramic layer on metal or metallic composite surface | |
| CN110359044A (en) | A kind of preparation method of steel matrix surface ultra-hydrophobic water film | |
| Zhan-Fang et al. | Super-hydrophobic coating used in corrosion protection of metal material: review, discussion and prospects | |
| CN105350049A (en) | Preparing method for graphene oxide composite coating on surface of magnesium alloy | |
| Partovi-Nia et al. | Corrosion of cold spray deposited copper coating on steel substrates | |
| Zhu et al. | Effect of the Cu content on the microstructure and corrosion behavior of PEO coatings on Al–xCu alloys | |
| Wang et al. | Ti/Cr (III) conversion coating on aluminium foil for lithium-ion battery package | |
| CN103147112B (en) | A kind of electrolytic solution and for the preparation of the purposes of nuclear fuel rod zirconium alloy cladding micro-arc oxidation films and method | |
| CN105063715A (en) | Preparation method for anodic oxide film on B4C-A1-based composite surface and oxide film prepared through preparation method | |
| Zhang et al. | Effect of Fe3+ and F− on black micro‐arc oxidation ceramic coating of magnesium alloy | |
| CN104499013A (en) | Room temperature ionic liquids electroplating method for electroplating aluminum on RAFM (Reduced Activation Ferritic/martensitic) steel surface | |
| CN103469278B (en) | A kind of electrolyte of preparing for zirconium alloy cladding diaphragm and micro-arc oxidation process | |
| CN105543823A (en) | Method for preparing titanium/selenium multicolour composite conversion film on surface of aluminium alloy | |
| Zhang et al. | Modification and durability of carbon paper gas diffusion layer in proton exchange membrane fuel cell | |
| CN113265609B (en) | Method for rapidly preparing aluminum oxide on surface of 316L stainless steel aluminide tritium-resistant coating | |
| CN106521494A (en) | Ni, S codoped TiO2 film, application and preparation method thereof | |
| Wang et al. | Hydrogen interaction characteristics of a Cr2O3Y2O3 coating formed on stainless steel in an ultra-low oxygen environment | |
| Yerokhin et al. | Anodising of light alloys | |
| CN111926366B (en) | Sintered neodymium-iron-boron magnet surface corrosion-resistant coating and preparation method thereof | |
| CN113151829A (en) | Aluminum alloy surface heat cracking resistance treatment method and product | |
| CN111020655B (en) | Preparation method and application of zirconium alloy material with chromium coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |