CN102560599A - Preparation method for in-situ growth of oxide film on titanium alloy surface - Google Patents
Preparation method for in-situ growth of oxide film on titanium alloy surface Download PDFInfo
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- CN102560599A CN102560599A CN2012100284593A CN201210028459A CN102560599A CN 102560599 A CN102560599 A CN 102560599A CN 2012100284593 A CN2012100284593 A CN 2012100284593A CN 201210028459 A CN201210028459 A CN 201210028459A CN 102560599 A CN102560599 A CN 102560599A
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Abstract
The invention belongs to the field of metal material surface treatment, particularly relates to the technical research on a titanium alloy surface treatment method, and more particularly relates to a preparation method for in-situ growth of an oxide film on the titanium alloy surface. The preparation method is characterized by comprising the following steps of: selecting deoiled and cleaned titanium alloy as an anode and a stainless steel electrolysis bath as a cathode, fixing and placing a titanium alloy specimen in an electrolyte, which is a sodium phosphate-sodium silicate system, simultaneously adding sodium wolframate and graphite to the electrolyte, setting electrolysis parameters and treating for 5-30min, so that a high-hardness, good-wear-resistance and strong-corrosion-resistance micro arc ceramic oxide layer is generated on the surface.
Description
Technical field
The invention belongs to the metal material surface process field, relate in particular to the technical study of titanium alloy surface treatment process, refer in particular to the preparation method of titanium alloy surface growth in situ sull.
Background technology
Titanium or titanium alloy is widely used in aerospace, chemical industry, physical culture and medical field with its higher specific tenacity and good solidity to corrosion; Its principal feature is that density is little; Specific tenacity is high, is 21.7 like the specific tenacity (tensile strength/density) of Ti6Al4V, almost is the highest in all metallic substance; Good corrosion resistance, the anti-nitric acid causticity like pure titanium during at 35 ℃ of corrosion resistance against sulfuric acid with at 100 ℃ is that annual corrosion rate is below 0.127mm; Any untoward reaction can not take place at body bone tissue in excellent biocompatibility; But titanium hardness is low under some condition, wearing no resistance makes solidity to corrosion descend greatly; Existing poor, the poor heat stability of titanium alloy surface coating's adhesion; Overcome above-mentioned these shortcomings; Developed the method for kinds of surface modification; Mainly containing plating Cr and Ni-P is wet type plating method, thermal diffusion method, welding method and the sputtering method of representative, in addition chemical vapor deposition (CVD) and physical vapor deposition (PVD) plasma spraying, ion implantation etc.; Yet there are various shortcomings and deficiencies in above-mentioned titanium alloy surface treatment process; Like PVD/CVD, ion implantation and thermal oxidation method needs maintenance high temperature in the coating prepn process, changed the structure of matrix and coating to a certain extent, the mechanical property of matrix is obviously degenerated; And the thermal oxidation method energy consumption is big, the time is long and labour intensity is big, and the coating that reaches is inhomogeneous, therefore is necessary to develop the coat preparing technology of new low-cost and high-performance; Differential arc oxidization technique receives people's attention just day by day as a kind of novel process for treating surface, and titanium alloy passes through differential arc oxidation, the ceramic membrane that matrix surface growth in situ one deck hardness is high, wear resistance is good, corrosion resistance nature is strong; So far; Many investigators have done a large amount of research to the titanium alloy differential arc oxidation; Mainly concentrate on about the micro-arc oxidation process Parameter Optimization; Like the system selection of electrolytic solution, current density, dutycycle, oxidization time etc., seldom see about in main electrolytic solution, adding report, the especially sodium wolframate of additive and the report that graphite adds simultaneously.
Summary of the invention
The object of the invention is to provide a kind of preparation method at titanium alloy substrate surface in situ growth one deck ceramic oxide rete; It is characterized in that: the titanium alloy after oil removing is cleaned is as anode; The stainless steel electrolytic groove is as negative electrode, the titanium alloy sample fixed place electrolytic solution, and electrolytic solution is sodium phosphate-water glass system; In electrolytic solution, add sodium wolframate and graphite simultaneously; Electrolytic parameter is set, handles 5-30min, the surface can generate the arc differential oxide ceramic layer that one deck hardness is high, wear resistance is good, solidity to corrosion is strong.
The present invention realizes that through following steps method steps is:
A: the titanium alloy of well cutting is polished with the sand paper of 400#, 600#, 1000# respectively step by step, sample is put into the ultrasonic auxiliary oil removing of acetone soln clean, use deionized water rinsing then, dry up subsequent use.
B: as anode, the stainless steel electrolytic groove is as negative electrode with titanium alloy, the titanium alloy sample fixed carry out differential arc oxidation in the electrolytic solution that is suspended in the stainless steel electrolytic groove; Sample must not contact with cell container, opens whisking appliance, and electrolytic solution is evenly stirred; Being suitable for circulating cooling system in the process of the test lowers the temperature to electrolytic solution; The electrolytic parameter that input is set, energized stops behind the differential arc oxidation.
C:: the sample behind the differential arc oxidation is clean with distilled water flushing, to remove the electrolytic solution of remained on surface, cleaned and placed oven drying.
The ultrasonic oil removing time is 3 ~ 5min in the said steps A.
Differential arc oxidation electrolytic solution among the said step B is basal liquid with water glass-sodium polyphosphate system; Add sodium wolframate and graphite, sodium polyphosphate 5 ~ 15g/L, water glass 10 ~ 20 g/L in the electrolytic solution, complexing stablizer EDTA disodium 1 ~ 5 g/L; Additive sodium wolframate 1 ~ 10g/L; Graphite 1 ~ 3g/L when preparation electrolytic solution, is noted that and treats just can add after every kind of material dissolves fully a kind of material down.
Electrolytic parameter among the said step B is: mao power source is the bidirectional pulse power supply, and power is that 5 ~ 6KW, voltage are that 300 ~ 500V, frequency are that 400 ~ 600HZ, dutycycle are 30% ~ 100%, current density is 0.05 ~ 0.5A/cm
2
The differential arc oxidation time among the said step B is 5 ~ 30min, and temperature remains on 10 ~ 50 ℃ in the whole differential arc oxidation process.
Drying temperature is at 50 ~ 100 ℃ among the said step C.
Beneficial effect of the present invention is: differential arc oxidation has overcome the deficiency of conventional titanium alloy process for treating surface, and at the ceramic membrane of titanium alloy surface growth in situ one deck high firmness, high-wearing feature, high anti-corrosion, and rete and matrix bond are good; Micro-arc oxidation process is simple, control easily, and low production cost and energy consumption are not polluted environment; The adding of additive exerts an influence to film performance from two aspects, and the one, directly getting into rete becomes the rete component, and the 2nd, improved electrolytic solution character, increased the oxidation filming ability of electrolytic solution, improved the performance of rete; The adding of sodium wolframate and graphite makes coating growth even; Thickness increases, and the film surface homogeneity improves, and hole density increases; The aperture reduces; It is Paint Gloss solid that the surface becomes, and little graphite granule finally is deposited on rete hole the inside and covers film surface, and the hardness of rete, wear resistance, corrosion resisting property are further improved.
Description of drawings
Fig. 1 is the surface and the cross section pattern of TC4 titanium alloy micro-arc oxidation films of gained in having or not additive solution;
Fig. 2 is the influence of additive to differential arc oxidation film layer hardness;
Fig. 3 is titanium alloy substrate and the polarization curve of differential arc oxidation film layer in 3.5%NaCl solution.
Can find among Fig. 1 not add sodium wolframate and graphite among Fig. 1 (a), coating porosity, the homogeneity of zone of oxidation is all not as after adding sodium wolframate and graphite, shown in Fig. 1 (b) coating porosity little, the also more all even densification of coating.
Fig. 2 is the influence of additive to differential arc oxidation film layer hardness, and wherein 1 is matrix; The 2nd, micro-arc oxidation films, but do not add sodium wolframate and graphite in the electrolytic solution; The 3rd, micro-arc oxidation films, but added sodium wolframate and graphite in the electrolytic solution; The hardness of coating increases after the data sheet of hardness can find the electrolytic solution to add graphite.
Fig. 3 is titanium alloy substrate and the polarization curve of differential arc oxidation film layer in 3.5%NaCl solution, and wherein 1 is matrix; The 2nd, micro-arc oxidation films, but do not add sodium wolframate and graphite in the electrolytic solution; The 3rd, micro-arc oxidation films; But sodium wolframate and graphite have been added in the electrolytic solution; If from figure, can find to have added in the electrolytic solution sodium wolframate and graphite; The solidity to corrosion of the differential arc oxidation coating that forms improves than the coating corrosion current potential of the electrolytic solution system of not adding additive, and corrosion current reduces, and explains that the corrosion resisting property of coating improves.
Embodiment
Handling sample is the TC4 titanium alloy, and size is the sheet of 40mm * 15 mm * 3 mm, further specifies the present invention through specific embodiment below.
Embodiment 1:
1) sample pretreatment: the titanium alloy of well cutting is polished with the sand paper of 400#, 600#, 1000# respectively step by step, sample is put into the ultrasonic auxiliary oil removing of acetone soln clean 3min, use deionized water rinsing then, dry up subsequent use.
2) differential arc oxidation is handled: electrolytic solution is basal liquid with water glass-sodium polyphosphate system, sodium polyphosphate 10g/L in the electrolytic solution, water glass 12g/L, EDTA disodium 1g/L, sodium wolframate 2g/L, graphite 1g/L; The titanium alloy that pre-treatment is good is as anode, and the stainless steel electrolytic groove is as negative electrode, the titanium alloy sample fixed place electrolytic solution to carry out differential arc oxidation; Sample must not contact with the stainless steel electrolytic groove, opens whisking appliance, and electrolytic solution is evenly stirred; Use circulating cooling system that electrolytic solution is lowered the temperature in the process of the test, temperature should maintain 40 ℃, and power supply adopts the bidirectional pulse mao power source; Power is that 5KW, voltage are 300V, and frequency is 500HZ, and current density is 0.1A/cm
2, dutycycle is 45%, the differential arc oxidation time is 15min.
3) sample aftertreatment: the sample behind the differential arc oxidation is clean with distilled water flushing, to remove the electrolytic solution of remained on surface, cleaned and be placed on oven drying, drying temperature is at 50 ℃.
Embodiment 2:
1) sample pretreatment: the titanium alloy of well cutting is polished with the sand paper of 400#, 600#, 1000# respectively step by step, sample is put into the ultrasonic auxiliary oil removing of acetone soln clean 5min, use deionized water rinsing then, dry up subsequent use.
2) differential arc oxidation is handled: electrolytic solution is basal liquid with water glass-sodium polyphosphate system, sodium polyphosphate 15g/L in the electrolytic solution, water glass 10g/L, EDTA disodium 5g/L, sodium wolframate 1g/L, graphite 3g/L; The titanium alloy that pre-treatment is good is as anode, and the stainless steel electrolytic groove is as negative electrode, the titanium alloy sample fixed place electrolytic solution to carry out differential arc oxidation; Sample must not contact with the stainless steel electrolytic groove, opens whisking appliance, and electrolytic solution is evenly stirred; Use circulating cooling system that electrolytic solution is lowered the temperature in the process of the test, temperature should maintain 30 ℃, and power supply adopts the bidirectional pulse mao power source; Power is that 6KW, voltage are 500V, and frequency is 500HZ, and current density is 0.3/cm
2, dutycycle is 65%, the differential arc oxidation time is 25min.
3) sample aftertreatment: the sample behind the differential arc oxidation is clean with distilled water flushing, to remove the electrolytic solution of remained on surface, cleaned and be placed on oven drying, drying temperature is at 100 ℃.
Embodiment 3:
1) sample pretreatment: the titanium alloy of well cutting is polished with the sand paper of 400#, 600#, 1000# respectively step by step, sample is put into the ultrasonic auxiliary oil removing of acetone soln clean 4min, use deionized water rinsing then, dry up subsequent use.
2) differential arc oxidation is handled: electrolytic solution is basal liquid with water glass-sodium polyphosphate system, sodium polyphosphate 5g/L in the electrolytic solution, water glass 20g/L, EDTA disodium 3g/L, sodium wolframate 6g/L, graphite 2g/L; The titanium alloy that pre-treatment is good is as anode, and the stainless steel electrolytic groove is as negative electrode, the titanium alloy sample fixed place electrolytic solution to carry out differential arc oxidation; Sample must not contact with cell container, opens whisking appliance, and electrolytic solution is evenly stirred; Use circulating cooling system that electrolytic solution is lowered the temperature in the process of the test, temperature should maintain 10 ℃, and power supply adopts the bidirectional pulse mao power source; Power is that 5KW, voltage are 400V, and frequency is 400HZ, and current density is 0.5A/cm
2, dutycycle is 95%, the differential arc oxidation time is 30min.
3) sample aftertreatment: the sample behind the differential arc oxidation is clean with distilled water flushing, to remove the electrolytic solution of remained on surface, cleaned and be placed on oven drying, drying temperature is at 80 ℃.
Embodiment 4:
1) sample pretreatment: the titanium alloy of well cutting is polished with the sand paper of 400#, 600#, 1000# respectively step by step, sample is put into the ultrasonic auxiliary oil removing of acetone soln clean 5min, use deionized water rinsing then, dry up subsequent use.
2) differential arc oxidation is handled: electrolytic solution is basal liquid with water glass-sodium polyphosphate system, sodium polyphosphate 10g/L, water glass 15g/L, EDTA disodium 1g/L, sodium wolframate 10g/L, graphite 1g/L; The titanium alloy that pre-treatment is good is as anode, and the stainless steel electrolytic groove is as negative electrode, the titanium alloy sample fixed place electrolytic solution to carry out differential arc oxidation; Sample must not contact with cell container, opens whisking appliance, and electrolytic solution is evenly stirred; Use circulating cooling system that electrolytic solution is lowered the temperature in the process of the test, temperature should maintain 40 ℃, and power supply adopts the bidirectional pulse mao power source; Power is that 5KW, voltage are 400V, and frequency is 600HZ, and current density is 0.05A/cm
2, dutycycle is 30%, the differential arc oxidation time is 10min.
3) sample aftertreatment: the sample behind the differential arc oxidation is clean with distilled water flushing, to remove the electrolytic solution of remained on surface, cleaned and be placed on oven drying, drying temperature is at 70 ℃.
Claims (7)
1. the preparation method of titanium alloy surface growth in situ sull; Comprise the step of step, differential arc oxidation processed steps and the sample aftertreatment of titanium alloy sample pretreatment, it is characterized in that: the differential arc oxidation electrolytic solution that said differential arc oxidation is handled is to be basal liquid with water glass-sodium polyphosphate system, adds sodium wolframate and graphite; Sodium polyphosphate 5 ~ 15g/L, water glass 10 ~ 20 g/L in the electrolytic solution; Complexing stablizer EDTA disodium 1 ~ 5 g/L, additive sodium wolframate 1 ~ 10g/L, graphite 1 ~ 3g/L.
2. the preparation method of titanium alloy surface growth in situ sull as claimed in claim 1 is characterized in that: said differential arc oxidation processed steps is: as anode, the stainless steel electrolytic groove is as negative electrode with titanium alloy; The titanium alloy sample fixed carry out differential arc oxidation in the electrolytic solution that is suspended in the stainless steel electrolytic groove; Sample must not contact with cell container, opens whisking appliance, and electrolytic solution is evenly stirred; Being suitable for circulating cooling system in the process of the test lowers the temperature to electrolytic solution; The electrolytic parameter that input is set, energized stops behind the differential arc oxidation.
3. the preparation method of titanium alloy surface growth in situ sull as claimed in claim 2; It is characterized in that: said electrolytic parameter is: mao power source is the bidirectional pulse power supply, and power is that 5 ~ 6KW, voltage are that 300 ~ 500V, frequency are that 400 ~ 600HZ, dutycycle are 30% ~ 100%, current density is 0.05 ~ 0.5A/cm
2
4. the preparation method of titanium alloy surface growth in situ sull as claimed in claim 2 is characterized in that: the differential arc oxidation time is 5 ~ 30min, and temperature remains on 10 ~ 50 ℃ in the whole differential arc oxidation process
The preparation method of titanium alloy surface growth in situ sull as claimed in claim 1; It is characterized in that: the step of said titanium alloy sample pretreatment is: titanium alloy is polished with the sand paper of 400#, 600#, 1000# respectively step by step; Sample is put into the ultrasonic auxiliary oil removing of acetone soln to be cleaned; Use deionized water rinsing then, dry up subsequent use.
5. the preparation method of titanium alloy surface growth in situ sull as claimed in claim 5 is characterized in that: the ultrasonic oil removing time is 3 ~ 5min.
6. the preparation method of titanium alloy surface growth in situ sull as claimed in claim 1; It is characterized in that: the step of said sample aftertreatment is: the sample behind the differential arc oxidation is clean with distilled water flushing; To remove the electrolytic solution of remained on surface, cleaned and placed oven drying.
7. the preparation method of titanium alloy surface growth in situ sull as claimed in claim 7 is characterized in that: said drying temperature is at 50 ~ 100 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104404600A (en) * | 2014-12-12 | 2015-03-11 | 南京理工大学 | Coating for frequency-adjustable high-sound-intensity soot blower sound production assembly, and preparation method for coating |
| CN104790016A (en) * | 2015-04-03 | 2015-07-22 | 昆明冶金研究院 | Method for preparing ceramic coating on surface of titanium alloy |
| CN106498477A (en) * | 2016-11-02 | 2017-03-15 | 上海航天设备制造总厂 | A kind of method for improving titanium alloy surface cementing strength |
| CN112663111A (en) * | 2020-12-04 | 2021-04-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of corrosion-resistant titanium alloy micro-arc oxidation coating |
| CN114088497A (en) * | 2021-12-02 | 2022-02-25 | 北京星航机电装备有限公司 | Preparation device and method of titanium alloy EBSD sample |
| CN114517322A (en) * | 2022-03-11 | 2022-05-20 | 西安理工大学 | In-situ preparation method of titanium alloy megaohm-grade high-impedance surface ceramic |
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| CN101994143A (en) * | 2010-10-27 | 2011-03-30 | 江苏科技大学 | Preparation method of titanium alloy/biological ceramic layer composite material |
| CN102021629A (en) * | 2010-12-30 | 2011-04-20 | 南昌航空大学 | Method for preparing titanium-alloy surface micro-arc oxidation antifriction compound film layer |
| CN102039408A (en) * | 2010-12-20 | 2011-05-04 | 哈尔滨工业大学 | Method for preparing bioactive ceramic coating on surface of porous titanium |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104404600A (en) * | 2014-12-12 | 2015-03-11 | 南京理工大学 | Coating for frequency-adjustable high-sound-intensity soot blower sound production assembly, and preparation method for coating |
| CN104790016A (en) * | 2015-04-03 | 2015-07-22 | 昆明冶金研究院 | Method for preparing ceramic coating on surface of titanium alloy |
| CN106498477A (en) * | 2016-11-02 | 2017-03-15 | 上海航天设备制造总厂 | A kind of method for improving titanium alloy surface cementing strength |
| CN112663111A (en) * | 2020-12-04 | 2021-04-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of corrosion-resistant titanium alloy micro-arc oxidation coating |
| CN114088497A (en) * | 2021-12-02 | 2022-02-25 | 北京星航机电装备有限公司 | Preparation device and method of titanium alloy EBSD sample |
| CN114088497B (en) * | 2021-12-02 | 2023-09-19 | 北京星航机电装备有限公司 | Preparation device and method of titanium alloy EBSD sample |
| CN114517322A (en) * | 2022-03-11 | 2022-05-20 | 西安理工大学 | In-situ preparation method of titanium alloy megaohm-grade high-impedance surface ceramic |
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Application publication date: 20120711 |