CN107217289A - It is a kind of to remove the method that titanium alloy differential arc oxidation film layer remains matrix - Google Patents
It is a kind of to remove the method that titanium alloy differential arc oxidation film layer remains matrix Download PDFInfo
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- CN107217289A CN107217289A CN201710321162.9A CN201710321162A CN107217289A CN 107217289 A CN107217289 A CN 107217289A CN 201710321162 A CN201710321162 A CN 201710321162A CN 107217289 A CN107217289 A CN 107217289A
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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
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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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
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F5/00—Electrolytic stripping of metallic layers or coatings
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The invention discloses a kind of specific method for removing the remaining matrix of titanium alloy differential arc oxidation film layer, one face mask layer of the sample after differential arc oxidation is polished off with sand paper, connect electrolytic fixture, being inlayed again with epoxy resin, its matrix is exposed after will be polished off after hardening of resin in face of the epoxy resin of matrix side with sand paper.Afterwards, the anodic solution of titanium matter matrix is carried out in mass fraction is 3.5% NaCl solution, and adds agitator being in the solution stirred, you can obtain complete arc differential oxide ceramic layer.The present invention is simple to operate, pollution-free, does not destroy film layer, obtained ceramic layer is pure and complete.SEM can be carried out to the film base interface of titanium matter differential arc oxidation film layer, EDS, XRD detection carries out the determination of observation and composition detection and the phase composition of microscopic appearance to film base interface, and the research to differential arc oxidation mechanism is very helpful.
Description
Technical field
The invention belongs to field of material surface modification, it is related to the separation side of a kind of differential arc oxidation film layer and its titanium matter matrix
Method.
Background technology
Titanium alloy is due to the features such as density is small, specific strength is high, corrosion resistance is good, frequently as aircraft and the primary structure of spacecraft
Material.But compared with ferrous materials, it is low that titanium alloy has hardness（Typically not greater than 350HV）, wear no resistance, thermal conductivity it is not high
The shortcomings of, " titanium fire " failure is also easy to produce in use, and these shortcomings seriously limit titanium alloy answering in aircraft industry
Use scope.Therefore, appropriate surface treatment need to be carried out to improve its hardness, improve its wearability.
Differential arc oxidation, also referred to as plasma electrolytic oxidation, are a kind of new surface modification technologies, greatly improve
The wearability and corrosion resistance of its matrix valve metal, and be most one of process for modifying surface of cost and environmental benefit advantage.
Because the metallurgical binding of film layer and matrix limits people to the observation at its film layer basal body interface, therefore it also counteracts that people couple
The further research of differential arc oxidation mechanism.Therefore, finding a kind of suitable method and obtaining complete differential arc oxidation film layer to enter
One step promote people to differential arc oxidation mechanism deeper into research.
The content of the invention
It is an object of the invention to provide a kind of safety simple to operate, efficiency high, free of contamination arc differential oxide ceramic layer with
The separation method of its titanium matter matrix.
The separation method of the present invention is as follows：A kind of separation method of differential arc oxidation film layer and its titanium matter matrix, its feature exists
It is as follows in method and step：
Step one：Prepared before separation：
（1）The one side of sample with differential arc oxidation film layer is polishing to titanium alloy substrate exposure with sand paper；
（2）The sample polished is connected into fixture and inlayed with epoxy resin；
（3）The sample inlayed is polished off towards the resin of the side of matrix with sand paper, its matrix is exposed；
（4）Configure the NaCl solution that electrolyte is mass fraction 1.5~10%；
（5）Agitator is added in the solution, and agitator speed is 650r/min；
（6）Connect circuit：By step（4）Institute's electrolyte is poured into electrolytic cell, and stainless steel passes through wire and power supply as negative electrode
Negative pole is connected, and is inlayed the sample after polishing and is connected as anode by wire with positive source, circuit needed for composition separation；
Step 2：Switch on power, using constant-voltage method, voltage is 15V, after taking out film layer after matrix all dissolving, in course of dissolution
The pH value of middle detection solution, and pH value is adjusted with watery hydrochloric acid, electrolytic solution is kept neutral；
Titanium base is removed using the method for anodic solution, the reaction equation of generation is：
Anode：Ti-4e→Ti4+, negative electrode： 4H2O+4e→2H2+4OH-, overall reaction：Ti+4H2O→Ti(OH)4+2H2。
Step 3：Taken out after the differential arc oxidation sample deionized water immersion 10min that step 2 is obtained, drying in case after
It is continuous to use.
The present invention has advantages below：1st, it is simple to operate, it is effectively, pollution-free.2nd, because Titanium base is during electrolysis
The black product depended on matrix surface is easily produced, black product can be made to depart from sample in the presence of agitator.3rd, inlay
Sample after embedding firmly can be attached on epoxy resin, and in the case where there is agitator effect, sample will not be with the flowing of electrolyte
And depart from resin.4th, titanium alloy substrate is dissolved using the method for anodic solution, obtained film layer is complete and pure.
Brief description of the drawings
Fig. 1 is that the embodiment of the present invention 1 is the XRD diffraction patterns for removing sample before matrix.
Fig. 2 is the XRD diffraction patterns that the embodiment of the present invention 1 removes sample after matrix.
The shape appearance figure for the film surface that Fig. 3 obtains for the sample that the embodiment of the present invention 1 does not remove matrix under ESEM.
At the film layer and basal body interface that Fig. 4 obtains for the sample after the removal matrix of the embodiment of the present invention 1 under ESEM
Shape appearance figure.
Embodiment
Embodiment 1
By rectangle（20×20×1.5mm）One face ceramic layer of the titanium matter thin plate with ceramic coating formed by micro-arc oxidation is ground off with sand paper,
Expose matrix；Upper fixture is pressed from both sides afterwards, fixture and sample one are reinstated into epoxy resin and inlayed, and the sample inlayed is faced into matrix
The resin of side polished off with sand paper and expose its matrix, then the positive pole of sample and power supply is connected；By what is prepared
Mass fraction is that 3.5%NaCl solution is poured into electrolytic cell, is connected with stainless steel with power cathode as negative electrode, composition separation institute
Circuit is needed, agitator is added in the solution, mixing speed is 650r/min；Switch on power, using constant-potential electrolysis, voltage is 15V,
Detected in course of dissolution and adjust pH value, electrolyte is kept neutral, taken out after after matrix all dissolving；After being finally electrolysed
Differential arc oxidation film layer with deionized water immersion 10min take out, in case subsequently using after drying.
As shown in figure 1, because the film layer of differential arc oxidation is relatively thin, the presence of matrix diffraction maximum is had, the detection to film layer phase
There is interference in analysis, poor because diffraction maximum is too small and mixes and can not determine with diffraction noise in film layer in addition；
As shown in Fig. 2 the diffraction maximum of matrix is not present after matrix is eliminated, can be with due to eliminating interference of the matrix to film layer phase
It was found that the content that can not be determined in Fig. 1 very low thing has mutually obtained obvious embodiment herein, therefore, it is possible to more accurately obtain
The diffraction maximum of matrix has also been not present in the phase composition of film layer simultaneously；As shown in figure 3, being the film surface shape seen under surface sweeping Electronic Speculum
Looks；As shown in figure 4, for the clearly film layer and the pattern of basal body interface seen under Flied emission Electronic Speculum, Fig. 3 and Fig. 4 pattern are deposited
In greatest differences, illustrate that separation membrane layer has great Research Significance for research differential arc oxidation mechanism.
Embodiment 2
By rectangle（20×20×1.5mm）One face ceramic layer of the titanium matter thin plate with ceramic coating formed by micro-arc oxidation is ground off with sand paper,
Expose matrix；Upper fixture is pressed from both sides afterwards, fixture and sample one are reinstated into epoxy resin and inlayed, and the sample inlayed is faced into matrix
The resin of side polished off with sand paper and expose its matrix, then the positive pole of sample and power supply is connected；By what is prepared
Mass fraction is that 1.5%NaCl solution is poured into electrolytic cell, is connected with stainless steel with power cathode as negative electrode, composition separation institute
Circuit is needed, agitator is added in the solution, mixing speed is 650r/min；Switch on power, using constant-potential electrolysis, voltage is 15V,
Detected in course of dissolution and adjust pH value, electrolyte is kept neutral, taken out after after matrix all dissolving；After being finally electrolysed
Differential arc oxidation film layer with deionized water immersion 10min take out, in case subsequently using after drying.
Embodiment 3
By rectangle（20×20×1.5mm）One face ceramic layer of the titanium matter thin plate with ceramic coating formed by micro-arc oxidation is ground off with sand paper,
Expose matrix；Upper fixture is pressed from both sides afterwards, fixture and sample one are reinstated into epoxy resin and inlayed, and the sample inlayed is faced into matrix
The resin of side polished off with sand paper and expose its matrix, then the positive pole of sample and power supply is connected；By what is prepared
Mass fraction is that 10%NaCl solution is poured into electrolytic cell, is connected with stainless steel with power cathode as negative electrode, composition separation institute
Circuit is needed, agitator is added in the solution, mixing speed is 650r/min；Switch on power, using constant-potential electrolysis, voltage is 15V,
Detected in course of dissolution and adjust pH value, electrolyte is kept neutral, taken out after after matrix all dissolving；After being finally electrolysed
Differential arc oxidation film layer with deionized water immersion 10min take out, in case subsequently using after drying.
Claims (1)
1. a kind of remove the method that titanium alloy differential arc oxidation film layer remains matrix, it is characterised in that：
（1）Prepared before separation；
1. the one side with sample after differential arc oxidation is polishing to titanium alloy substrate exposure with sand paper；
2. the sample polished is connected into upper fixture and inlayed with epoxy resin；
3. the epoxy of matrix side is polished off with sand paper, and exposes its matrix；
4. configuration electrolyte is the NaCl solution of mass fraction 1.5~10%；
5. agitator is added in the solution, and it is 650r/min to make agitator speed；
6. circuit is connected：By step, 4. institute's electrolyte is poured into electrolytic cell, and stainless steel is born as negative electrode by wire and power supply
Pole is connected, and is inlayed the sample after polishing and is connected as anode by wire with positive source, circuit needed for composition separation；
（2）Switch on power, using constant-voltage method, voltage is 15V, after taking out film layer after matrix all dissolving, examined in course of dissolution
The pH value of solution is surveyed, and pH value is adjusted with watery hydrochloric acid, electrolytic solution is kept neutral；
（3）By step（2）The differential arc oxidation sample of acquisition deionized water is soaked to be taken out after 10min, is dried in case subsequently using.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113564662A (en) * | 2021-08-17 | 2021-10-29 | 北京石油化工学院 | Preparation method of magnesium alloy self-supporting micro-arc oxidation film layer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820832A (en) * | 2014-03-12 | 2014-05-28 | 湖南大学 | Two-step micro-arc oxidation method for producing super wear-resistant coating on surface of aluminium alloy |
| CN104018202A (en) * | 2014-05-30 | 2014-09-03 | 燕山大学 | Method of separating micro-arc oxidation ceramic layer from aluminium substrate thereof |
| CN104959045A (en) * | 2015-06-16 | 2015-10-07 | 陕西科技大学 | Method for manufacturing polyvinylidene fluoride nano array pore membranes |
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2017
- 2017-05-09 CN CN201710321162.9A patent/CN107217289A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820832A (en) * | 2014-03-12 | 2014-05-28 | 湖南大学 | Two-step micro-arc oxidation method for producing super wear-resistant coating on surface of aluminium alloy |
| CN104018202A (en) * | 2014-05-30 | 2014-09-03 | 燕山大学 | Method of separating micro-arc oxidation ceramic layer from aluminium substrate thereof |
| CN104959045A (en) * | 2015-06-16 | 2015-10-07 | 陕西科技大学 | Method for manufacturing polyvinylidene fluoride nano array pore membranes |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113564662A (en) * | 2021-08-17 | 2021-10-29 | 北京石油化工学院 | Preparation method of magnesium alloy self-supporting micro-arc oxidation film layer |
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Application publication date: 20170929 |