CN106637354A - Preparation method of micro-arc oxidation film layer on surface of beryllium and beryllium-aluminum alloy - Google Patents
Preparation method of micro-arc oxidation film layer on surface of beryllium and beryllium-aluminum alloy Download PDFInfo
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- CN106637354A CN106637354A CN201611172981.3A CN201611172981A CN106637354A CN 106637354 A CN106637354 A CN 106637354A CN 201611172981 A CN201611172981 A CN 201611172981A CN 106637354 A CN106637354 A CN 106637354A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
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Abstract
The invention relates to a method for preparing a micro-arc oxidation film layer on the surface of beryllium and beryllium-aluminum alloy. The method is characterized by comprising the following steps: putting a beryllium or beryllium-aluminum alloy sample in an alkaline electrolyte of a phosphate or phosphate-silicate mixed system to serve as an anode; and regulating the current, pulse width, duty ratio, backward voltage (or current) and the like of a pulsed power supply to perform plasma discharge on the surface of the beryllium or beryllium-aluminum alloy so as to form the micro-arc oxidation film layer. The film layer formed in this way has typical micro-arc oxidation film layer features, and the film layer has the characteristics of favorable wear resistance and corrosion resistance, high insulativity and the like. The method can greatly improve the wear resistance, corrosion resistance and other properties of the beryllium and beryllium-aluminum alloy surface, prolong the service life and widen the application range.
Description
Technical field
The present invention relates to a kind of beryllium and beryllium alumin(i)um alloy differential arc oxidation film layer preparation method, belong to metal surface treatment technology neck
Domain.
Background technology
Beryllium has that density is low, fusing point is high, rigidity is high, thermal neutron absorption cross section is low, hot property is excellent, infrared reflection rate
It is high, the features such as X-ray penetrability is good, in fields such as strategic arms, Aero-Space, atomic energy, navigation instrument, weapon-shooting systems
It is unique or first-selected material.Used as a kind of plasticity beryllium-base alloy, not only the high-performance with beryllium, also has aluminium concurrently to beryllium alumin(i)um alloy
Good formability, and beryllium resource is saved, there is broad prospect of application in the slightly lower field of beryllium performance requirement.Aero-Space,
The fields such as navigation instrument, in order that beryllium or beryllium alumin(i)um alloy part meet use requirement, generally require to beryllium and beryllium alumin(i)um alloy part
Carry out surface modified to increase the performances such as its chemical stability, insulating properties, wear resistant corrosion resistant.From the modified technique on current beryllium surface
Maturity and applicable cases see that the modified work in the surface that foreign countries have tested successfully on beryllium has anodic oxidation, chemical nickel plating, electricity
The coatings such as various metals and sprayed wc are plated, up to the present there is not yet open source literature is reported with regard to beryllium or aluminizing surface by micro-arc
Oxidation technology；Differential arc oxidation be one kind the metals such as magnesium, aluminium, titanium and its alloy are placed in electrolyte solution, high temperature, high pressure,
The surface that material is made under the collective effects such as heat chemistry, plasma chemistry and electrochemistry produces spark discharge generation ceramic film
Method.The technology has a process is simple, and the features such as low in the pollution of the environment, efficiency high, and there is ceramic coating formed by micro-arc oxidation film base junction to close
Power is strong, wear-resistant, corrosion-resistant, high temperature oxidation resisting and the advantages of good insulating, hence with differential arc oxidization technique to fine aluminium and
Aluminium alloy carries out surface treatment and has good prospect.
The content of the invention
The invention aims to solve the above problems, a kind of beryllium and beryllium alumin(i)um alloy surface by micro-arc oxidation film layer are devised
Preparation method.
It is an object of the invention to a kind of process is simple, low cost can be provided can be simultaneously on beryllium and beryllium alumin(i)um alloy surface
The method for preparing the differential arc oxidation film layer of reliable in quality.
A kind of beryllium and beryllium alumin(i)um alloy surface by micro-arc oxidation ceramic film preparation method, the method comprises the steps:
Step one, beryllium and beryllium alumin(i)um alloy surface degreasing are cleaned
Test specimen is put in the NaOH or potassium hydroxide solution that concentration is 20-100g/L and is cleaned in 2-5min；
Step 2, washing
Beryllium or beryllium alumin(i)um alloy surface are cleaned with 50 DEG C -60 DEG C of warm water；
Step 3, differential arc oxidation process
Beryllium or beryllium alumin(i)um alloy Jing after step l) with 2) process, it is micro- with what is prepared with being put in electrolytic cell after aluminum steel connection
Arc oxidation treatment liquid carries out differential arc oxidation process, and power parameter is：Pulse frequency is 50 to 2000Hz, and pulse-width regulated scope is
50-5000 μ s, start stirring system and cooling system, adjust electric current, and current density is 2A/dm2-30A/dm2, and the working time is
5-60min, electrolyte temperature is controlled below 40 DEG C in processing procedure；
Step 4, is dried
Beryllium or beryllium alumin(i)um alloy after differential arc oxidation is processed, natural air drying or dries, and obtains beryllium or beryllium alumin(i)um alloy differential of the arc oxygen
Change film layer.
The process for preparation of the differential arc oxidation treatment fluid is first to take distilled water to pour in equipment, and reagent is added at room temperature,
Adding the concentration range of reagent is：Sodium phosphate (or sodium phosphate and sodium silicate mixture) 10g/L-100g/L, potassium hydroxide 0.5g/
L-4g/L, is stirred continuously in adding procedure, adds another kind of reagent again after a kind of reagent is completely dissolved, after addition is finished, after
Continuous stirring is completely dissolved to reagent；
Sodium phosphate (or the sodium phosphate and sodium silicate mixture) 10g/L-100g/L, potassium hydroxide 0.5g/L-4g/L's
Ratio is 1:1:1:1:1.
The chemical reagent is analyzes pure, and during configuration treatment fluid distilled water is all used.
Beryllium and beryllium alumin(i)um alloy surface by micro-arc oxidation ceramics film preparation concrete steps are described below：
A). the reagent for using is：
Main film forming agent：Phosphate or or phosphate and silicate mixture
PH value regulator；Potassium hydroxide or NaOH；
Can make to be suitably added other additives to improve film surface performance；
Chemical reagent used is analyzes pure, and during configuration treatment fluid distilled water is all used；
B). the equipment for using is：
DC pulse mao power source (power 5-300kW), electrolytic cell, stirring system and cooling system；
Material is beryllium or beryllium alumin(i)um alloy.
C). the preparation of differential arc oxidation treatment fluid
First take distilled water to pour in equipment, reagent is added at room temperature, adding the concentration range of reagent is：Sodium phosphate (or
Sodium phosphate and sodium silicate mixture) 10g/L-100g/L, potassium hydroxide 0.5g/L-4g/L, it is stirred continuously in adding procedure, treat
A kind of reagent adds again another kind of reagent after being completely dissolved, and after addition is finished, continues stirring to reagent and is completely dissolved；
The beryllium made using technical scheme and beryllium alumin(i)um alloy surface by micro-arc oxidation film layer preparation method, one kind will
The metals such as magnesium, aluminium, titanium and its alloy are placed in electrolyte solution, in high temperature, high pressure, heat chemistry, plasma chemistry and electrification
The surface that material is made under etc. collective effect produces the method that spark discharge generates ceramic film.The technology has process is simple,
The features such as low in the pollution of the environment, efficiency high, and ceramic coating formed by micro-arc oxidation has, and film-substrate cohesion is strong, wear-resistant, corrosion-resistant, high temperature resistant
The advantages of oxidation and good insulating, surface treatment is carried out to fine aluminium and aluminium alloy hence with differential arc oxidization technique and is had well
Prospect.
Description of the drawings
Fig. 1 is the process flow diagram of beryllium of the present invention and beryllium alumin(i)um alloy surface by micro-arc oxidation film layer preparation method；
Fig. 2 is the pure beryllium surface by micro-arc oxidation of beryllium of the present invention and beryllium alumin(i)um alloy surface by micro-arc oxidation film layer preparation method
Film layer XRD.
Specific embodiment
It is specifically described, as shown in Figure 1-2, a kind of beryllium and beryllium alumin(i)um alloy surface by micro-arc to the present invention below in conjunction with the accompanying drawings
Oxidation film layer preparation method,
Embodiment one：It is prepared by beryllium surface by micro-arc oxidation film layer
A) reagent for using is：
Main film forming agent：Sodium phosphate
PH value regulator；Potassium hydroxide；
Chemical reagent used is analyzes pure, and during configuration treatment fluid distilled water is all used；
B). the equipment for using is：
40kW DC pulse mao power sources, electrolytic cell, stirring system and cooling system；
Material is pure beryllium.
C). the preparation of differential arc oxidation treatment fluid
First take distilled water to pour in equipment, reagent is added at room temperature, adding the concentration of reagent is：Sodium phosphate 30g/L, hydrogen
Potassium oxide 2g/L, is stirred continuously in adding procedure, adds another kind of reagent, addition to finish again after a kind of reagent is completely dissolved
Afterwards, continue to stir to reagent to be completely dissolved；
D). the enforcement of micro-arc oxidation process
1). pure beryllium surface degreasing cleaning
Test specimen is put in the sodium hydroxide solution that concentration is 30g/L and is cleaned in 2min；
2). washing
Pure beryllium surface is cleaned with 50 DEG C -60 DEG C of warm water；
3). differential arc oxidation process
Pure beryllium Jing after step l) with 2) process, with being put in electrolytic cell after aluminum steel connection, uses the differential of the arc of step c) preparations
Oxidation treatment liquid carries out differential arc oxidation process, and power parameter is：Frequency 500Hz, dutycycle 10% starts stirring system and cooling
System, adjusts electric current, and current density is 10A/dm2, and the working time is 20min, and electrolyte temperature is controlled 40 in processing procedure
Below DEG C；
4). it is dried
Pure beryllium after differential arc oxidation is processed, natural air drying or dries, and obtains pure beryllium surface by micro-arc oxidation ceramic membrane.Obtain
Film layer XRD it is as shown in Figure 1.Film layer main component is crystal phase BeO.
Embodiment two：It is prepared by beryllium alumin(i)um alloy surface by micro-arc oxidation film layer
A) reagent for using is：
Main film forming agent：Sodium phosphate-sodium silicate mixture
PH value regulator；NaOH；
Chemical reagent used is analyzes pure, and during configuration treatment fluid distilled water is all used；
B) equipment for using is：
40kW mao power sources, electrolytic cell, stirring system and cooling system；
Material is beryllium alumin(i)um alloy.
C) preparation of differential arc oxidation treatment fluid
First take distilled water to pour in equipment, reagent is added at room temperature, adding the order and concentration range of reagent is：Phosphoric acid
Sodium 20g/L, sodium metasilicate 20g/L, NaOH 1g/L, sodium fluoride 5g/L, and be stirred continuously in adding procedure, treat a kind of reagent
Add another kind of reagent, after addition is finished, continue stirring to reagent and be completely dissolved after being completely dissolved again；
D). the enforcement of micro-arc oxidation process
1). beryllium alumin(i)um alloy surface degreasing is cleaned
Test specimen is put in the sodium hydroxide solution that concentration is 40g/L and is cleaned in 4min；
2). washing
Beryllium alumin(i)um alloy surface is cleaned with 50 DEG C -60 DEG C of warm water；
3). differential arc oxidation process
Beryllium alumin(i)um alloy Jing after step l) with 2) process, with being put in electrolytic cell after aluminum steel connection, uses what step c) was prepared
Differential arc oxidation treatment fluid carries out differential arc oxidation process, and power parameter is：Frequency 1000Hz, dutycycle 30%, starts stirring system
And cooling system, electric current is adjusted, current density is 15A/dm2, and the working time is 30min, electrolyte temperature control in processing procedure
System is below 40 DEG C；
4). it is dried
Beryllium alumin(i)um alloy after differential arc oxidation is processed, natural air drying or dries, and obtains beryllium alumin(i)um alloy ceramic coating formed by micro-arc oxidation,
More than 250 megaohms of film surface insulaion resistance.
It is that beryllium or beryllium alumin(i)um alloy sample are placed in into phosphate or phosphate-silicate mixing that the characteristics of the present embodiment is
As anode in the alkaline electrolyte of system, by adjust the pulse power electric current, pulsewidth, duty when backward voltage (or electricity
Stream) etc., make that plasma discharge formation differential arc oxidation film layer occurs in beryllium or beryllium alumin(i)um alloy surface.The film layer being consequently formed has
Typical differential arc oxidation film layer feature, film layer has the characteristics such as good wear resistant corrosion resistant, high insulation.The present invention is greatly improved
The performance such as wear-resisting, corrosion-resistant on beryllium and beryllium alumin(i)um alloy surface, extends its service life, expands its range of application.
Above-mentioned technical proposal only embodies the optimal technical scheme of technical solution of the present invention, those skilled in the art
Some of which part is made some variation embody the present invention principle, belong to protection scope of the present invention it
It is interior.
Claims (3)
1. a kind of beryllium and beryllium alumin(i)um alloy surface by micro-arc oxidation ceramic film preparation method, it is characterised in that the method includes following step
Suddenly:
Step one, beryllium and beryllium alumin(i)um alloy surface degreasing are cleaned
Test specimen is put in the NaOH or potassium hydroxide solution that concentration is 20-100g/L and is cleaned in 2-5min；
Step 2, washing
Beryllium or beryllium alumin(i)um alloy surface are cleaned with 50 DEG C -60 DEG C of warm water；
Step 3, differential arc oxidation process
Beryllium or beryllium alumin(i)um alloy Jing after step l) with 2) process, with being put in electrolytic cell after aluminum steel connection, with the differential of the arc oxygen prepared
Changing treatment fluid carries out differential arc oxidation process, and power parameter is：Pulse frequency is 50 to 2000Hz, and pulse-width regulated scope is 50-
5000 μ s, start stirring system and cooling system, adjust electric current, and current density is 2A/dm2-30A/dm2, and the working time is 5-
60min, electrolyte temperature is controlled below 40 DEG C in processing procedure；
Step 4, is dried
Beryllium or beryllium alumin(i)um alloy after differential arc oxidation is processed, natural air drying or dries, and obtains beryllium or beryllium alumin(i)um alloy micro-arc oxidation films
Layer.
The process for preparation of the differential arc oxidation treatment fluid is first to take distilled water to pour in equipment, and reagent is added at room temperature, is added
The concentration range of reagent is：Sodium phosphate (or sodium phosphate and sodium silicate mixture) 10g/L-100g/L, potassium hydroxide 0.5g/L-
4g/L, is stirred continuously in adding procedure, adds another kind of reagent again after a kind of reagent is completely dissolved, and after addition is finished, continues
Stir to reagent and be completely dissolved.
2. beryllium according to claim 1 and beryllium alumin(i)um alloy surface by micro-arc oxidation ceramic film preparation method, it is characterised in that institute
Sodium phosphate (or sodium phosphate and sodium silicate mixture) 10g/L-100g/L is stated, the ratio of potassium hydroxide 0.5g/L-4g/L is 1:1:
1:1:1。
3. beryllium according to claim 2 and beryllium alumin(i)um alloy surface by micro-arc oxidation ceramic film preparation method, it is characterised in that institute
State chemical reagent be analysis it is pure, configuration treatment fluid when all use distilled water.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107740084A (en) * | 2017-09-30 | 2018-02-27 | 中国科学院长春光学精密机械与物理研究所 | A kind of beryllium alumin(i)um alloy and preparation method thereof |
| CN108193252A (en) * | 2017-12-28 | 2018-06-22 | 西北稀有金属材料研究院宁夏有限公司 | A kind of new method of beryllium alumin(i)um alloy anodic oxidation |
| CN108754360A (en) * | 2018-06-20 | 2018-11-06 | 陈国荣 | A kind of particle reinforced aluminum alloy New energy automobile motor shell |
| CN108754359A (en) * | 2018-06-20 | 2018-11-06 | 陈国荣 | A kind of manufacturing method of motor in electric automobile shell |
| CN109943875A (en) * | 2019-04-30 | 2019-06-28 | 北京航天控制仪器研究所 | A kind of beryllium and its alloy surface differential arc oxidization processing method and processing device |
| CN110923777A (en) * | 2019-09-10 | 2020-03-27 | 西北稀有金属材料研究院宁夏有限公司 | Method for conducting oxidation on surface of beryllium-aluminum alloy |
| CN114808079A (en) * | 2022-05-22 | 2022-07-29 | 王海建 | Surface treatment process for aluminum material |
| CN114892170A (en) * | 2022-05-22 | 2022-08-12 | 王海建 | Metal coating material |
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- 2016-12-18 CN CN201611172981.3A patent/CN106637354A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107740084A (en) * | 2017-09-30 | 2018-02-27 | 中国科学院长春光学精密机械与物理研究所 | A kind of beryllium alumin(i)um alloy and preparation method thereof |
| CN108193252A (en) * | 2017-12-28 | 2018-06-22 | 西北稀有金属材料研究院宁夏有限公司 | A kind of new method of beryllium alumin(i)um alloy anodic oxidation |
| CN108193252B (en) * | 2017-12-28 | 2019-12-17 | 西北稀有金属材料研究院宁夏有限公司 | Novel method for anodizing beryllium-aluminum alloy |
| CN108754360A (en) * | 2018-06-20 | 2018-11-06 | 陈国荣 | A kind of particle reinforced aluminum alloy New energy automobile motor shell |
| CN108754359A (en) * | 2018-06-20 | 2018-11-06 | 陈国荣 | A kind of manufacturing method of motor in electric automobile shell |
| CN109943875A (en) * | 2019-04-30 | 2019-06-28 | 北京航天控制仪器研究所 | A kind of beryllium and its alloy surface differential arc oxidization processing method and processing device |
| CN110923777A (en) * | 2019-09-10 | 2020-03-27 | 西北稀有金属材料研究院宁夏有限公司 | Method for conducting oxidation on surface of beryllium-aluminum alloy |
| CN114808079A (en) * | 2022-05-22 | 2022-07-29 | 王海建 | Surface treatment process for aluminum material |
| CN114892170A (en) * | 2022-05-22 | 2022-08-12 | 王海建 | Metal coating material |
| CN114808079B (en) * | 2022-05-22 | 2023-09-29 | 山西钰沙新材料科技有限公司 | Surface treatment process of aluminum material |
| CN114892170B (en) * | 2022-05-22 | 2023-10-24 | 江苏鑫氟天科技有限公司 | Metal coating material |
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