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CN101892507B - A method of increasing the growth rate of micro-arc oxidation film on titanium alloy - Google Patents

A method of increasing the growth rate of micro-arc oxidation film on titanium alloy Download PDF

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CN101892507B
CN101892507B CN2010102402580A CN201010240258A CN101892507B CN 101892507 B CN101892507 B CN 101892507B CN 2010102402580 A CN2010102402580 A CN 2010102402580A CN 201010240258 A CN201010240258 A CN 201010240258A CN 101892507 B CN101892507 B CN 101892507B
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arc oxidation
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titanium alloy
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CN101892507A (en
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冯长杰
赵晴
邵志松
杜楠
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Nanchang Hangkong University
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Abstract

一种提高钛合金微弧氧化膜生长速度的方法，其特征是方法步骤为：1)配置微弧氧化溶液：微弧氧化溶液配方如下：Na2SiO3 6g/L，NaAlO2 4g/L和NaOH 1g/L；2)向配置好的微弧氧化溶液中添加5mL/L OP-10表面活性剂；3)将步骤2溶液放在超声波震荡器中震荡10分钟后，加入0.5-6g/L的纳米Al粉或纳米Cr粉，Al粉或纳米Cr粉的粒径范围20-50nm，再超声振荡1h；4)将步骤3得到溶液从超声波震荡器中取出，使用机械震荡器上下搅拌溶液，将试样和不锈钢阴极放入溶液中，并用导线分别连接微弧氧化电源的阳极和阴极，进行微弧氧化实验，电流密度4-6A/dm2，时间10-60min。本发明的优点是：在相同的沉积工艺条件下，可使钛合金微弧氧化膜的生长速度提高0.1-3倍。

Figure 201010240258

A method for improving the growth rate of titanium alloy micro-arc oxidation film is characterized in that the method steps are: 1) configure the micro-arc oxidation solution: the formula of the micro-arc oxidation solution is as follows: Na 2 SiO 3 6g/L, NaAlO 2 4g/L and NaOH 1g/L; 2) Add 5mL/L OP-10 surfactant to the prepared micro-arc oxidation solution; 3) After shaking the solution in step 2 in an ultrasonic oscillator for 10 minutes, add 0.5-6g/L Nano-Al powder or nano-Cr powder, the particle size range of Al powder or nano-Cr powder is 20-50nm, and then ultrasonically oscillate for 1h; 4) Take out the solution obtained in step 3 from the ultrasonic oscillator, and use a mechanical oscillator to stir the solution up and down, Put the sample and stainless steel cathode into the solution, and connect the anode and cathode of the micro-arc oxidation power supply with wires respectively, and carry out the micro-arc oxidation experiment, the current density is 4-6A/dm 2 , and the time is 10-60min. The invention has the advantages that: under the same deposition process conditions, the growth rate of the titanium alloy micro-arc oxidation film can be increased by 0.1-3 times.

Figure 201010240258

Description

A kind of method that improves growth speed of titanium alloy microarc oxide film
Technical field
The present invention relates to a kind of raising oxide growth method of velocity, relate in particular to a kind of method that improves growth speed of titanium alloy microarc oxide film.
Background technology
The middle and later periods nineties 20th century; Differential arc oxidization technique is introduced China by western developed countries such as Russia; It is on the basis of common anode oxidation, to grow up; Adopt high-voltage, high current density, utilize the reaction that arc discharge strengthens and activation upward takes place at anode (titanium alloy, duraluminum and magnesiumalloy etc.), thereby form ceramic coating; Can significantly improve hardness, wear resistance and the solidity to corrosion of matrix alloy, in industries such as space flight, aviation, automobile, electronics and machinery, have great application prospect.
Also do not have unified understanding at present both at home and abroad for the principle of differential arc oxidation, the research of differential arc oxidation is mainly concentrated on adjusting process parameter and solution composition on differential arc oxidation membrane structure and the Effect on Performance both at home and abroad.Research both at home and abroad shows, improves current density, adopts pulse or AC power, can improve the speed of growth of micro-arc oxidation films such as titanium alloy, duraluminum, in differential arc oxidation solution, adds some hard, nonconducting particulate, like Al 2O 3Deng, be similar to composite electroplated plating or electroless plating compound plating, these particulates are mixed in the micro-arc oxidation films, the speed of growth of micro-arc oxidation films is improved, the hardness or the solidity to corrosion of sull improve.
The present invention is nanometer Al powder or the nanometer Cr powder that in titanium alloy differential arc oxidation solution, adds 0.5-6g/L; Through stirring it is uniformly distributed in the solution, because metal nano powder conducts electricity, when it moves to specimen surface arc discharge regional; Can participate in arc discharge; Make arc light in the time lengthening that specimen surface stops, increased the temperature of top layer micro-arc oxidation films, the reaction of matrix alloy differential arc oxidation is quickened; Increased the speed of growth of micro-arc oxidation films, and the participation film forming of very small amount is not participated in or is had at metal powder or its oxide compound end.Do not find also at home and abroad at present that relevant Nano metal powder promotes the research report of differential arc oxidation layer-growth rate, relevant its mechanism also need be furtherd investigate.
Summary of the invention
The object of the present invention is to provide a kind of method that improves growth speed of titanium alloy microarc oxide film; This method is applicable to the speed of growth that improves titanium alloy, duraluminum and magnesium alloy differential arc oxidation film; The resource and the energy during for saving titanium alloy, duraluminum and magnesium alloy differential arc oxidation are significant, in industries such as space flight, aviation, automobile, electronics and machinery, have great application prospect.
The present invention realizes like this, it is characterized in that method steps is:
1) configuration differential arc oxidation solution: the differential arc oxidation solution formula is following: Na 2SiO 36g/L, NaAlO 24g/L and NaOH 1g/L;
2) in the differential arc oxidation solution that configures, add 5mL/L OP-10;
3) step 2 solution is placed in the ultrasonic oscillation device concussion after 10 minutes, adds nanometer Al powder or the nanometer Cr powder of 0.5-6g/L, the particle size range 20-50nm of nanometer Al powder or nanometer Cr powder, sonic oscillation 1h again;
4) step 3 being obtained solution takes out from the ultrasonic oscillation device; Use mechanical oscillator stirred solution up and down, sample and stainless steel cathode are put into solution, and connect the anode and the negative electrode of mao power source respectively with lead; Carry out the differential arc oxidation experiment, current density 4-6A/dm 2, time 10-60min.
This method is equally applicable to other duraluminum and magnesiumalloy.
Advantage of the present invention is: under identical deposition process conditions, can make the speed of growth of titanium alloy micro-arc oxidation films improve 0.1-3 doubly.
Description of drawings
Fig. 1 is the XRD figure behind the TC4 titanium alloy differential arc oxidation.
Fig. 2 is TC4 titanium alloy XRD figure behind the differential arc oxidation in the solution that contains 2g/L nanometer Cr powder.
Embodiment
Embodiment 1
Carry out the differential arc oxidation experiment to being of a size of 25mm * 50mm * 1mmTC4 titanium alloy test piece, experiment condition is following: Na 2SiO 36g/L, NaAlO 24g/L, NaOH 1g/L, nanometer Cr powder 0.5g/L or nanometer Al powder 0.5g/L,, OP-105ml/L, current density 4A/dm 2, time 10min, nanometer Cr or nanometer Al powder footpath scope 20nm.Measure the thickness of different micro-arc oxidation films with being prone to high 345 eddy current thickness meters after experiment finishes, experiment condition and experimental result are seen table 1.
Embodiment 2
Carry out the differential arc oxidation experiment to being of a size of 25mm * 50mm * 1mmTA2 titanium alloy test piece, experiment condition is following: Na 2SiO 36g/L, NaAlO 24g/L, NaOH 1g/L, nanometer Cr powder 6g/L or nanometer Al powder 6g/L, OP-105ml/L, current density 6A/dm 2, time 60min nanometer Cr or nanometer Al powder footpath scope 100nm.Measure the thickness of different micro-arc oxidation films with being prone to high 345 eddy current thickness meters after experiment finishes, experiment condition and experimental result are seen table 2.
Embodiment 3
Carry out the differential arc oxidation experiment to being of a size of 25mm * 50mm * 1mm2024 duraluminum test piece, experiment condition is following: Na 2SiO 36g/L, NaAlO 24g/L, NaOH 1g/L, nanometer Cr powder 0.5-6g/L or nanometer Al powder 0.5-6g/L, OP-105ml/L, current density 5A/dm 2, time 10-60min, nanometer Cr or nanometer Al powder footpath scope 150-250nm.Measure the thickness of different micro-arc oxidation films with being prone to high 345 eddy current thickness meters after experiment finishes, experiment condition and experimental result are seen table 3.
Embodiment 4
Carry out the differential arc oxidation experiment to being of a size of 25mm * 50mm * 1mmAZ91D magnesiumalloy test piece, experiment condition is following: Na 2SiO 36g/L, NaAlO 24g/L, NaOH 1g/L, nanometer Cr powder 0.5-6g/L or nanometer Al powder 0.5-6g/L, OP-105ml/L, current density 5A/dm 2, time 10-60min, nanometer Cr or nanometer Al powder footpath scope 400-500nm.Measure the thickness of different micro-arc oxidation films with being prone to high 345 eddy current thickness meters after experiment finishes, experiment condition and experimental result are seen table 4.
Table 1 TC4 titanium alloy differential arc oxidation condition and experimental result
Sample Nanometer Al powder content (g/L) Nanometer Cr powder content (g/L) The differential arc oxidation time (min) Differential arc oxidation film thickness (μ m)
1 0 0 10 4.7
2 0 0 20 9.8
3 0 0 40 20.2
4 0 0 60 30.5
5 0.5 0 10 7.0
6 2 0 10 11.7
7 4 0 10 18.8
8 6 0 10 15.0
9 0 0.5 10 7.0
10 0 2 10 11.2
11 0 4 10 17.8
12 0 6 10 14.5
13 0.5 0 20 14.8
14 2 0 20 24.6
15 4 0 20 39.4
16 6 0 20 31.5
17 0 0.5 20 14.8
18 0 2 20 23.6
19 0 4 20 37.5
20 0 6 20 30.5
21 0.5 0 40 26.6
22 2 0 40 44.4
23 4 0 40 71.0
24 6 0 40 56.4
25 0 0.5 40 26.3
26 0 2 40 42.3
27 0 4 40 67.2
28 0 6 40 54.9
29 0.5 0 60 35.5
30 2 0 60 59.2
31 4 0 60 94.7
32 6 0 60 76.0
33 0 0.5 60 35.5
34 0 2 60 56.4
35 0 4 60 89.8
36 0 6 60 73.3
Table 2 TA2 titanium alloy differential arc oxidation condition and experimental result
Sample Nanometer Al powder content (g/L) Nanometer Cr powder content (g/L) The differential arc oxidation time (min) Differential arc oxidation film thickness (μ m)
1 0 0 10 6.7
2 0 0 20 14.1
3 0 0 40 28.9
4 0 0 60 43.7
5 0.5 0 10 10.0
6 2 0 10 16.8
7 4 0 10 26.5
8 6 0 10 21.5
9 0 0.5 10 10.7
10 0 2 10 14.8
11 0 4 10 25.5
12 0 6 10 20.1
13 0.5 0 20 21.1
14 2 0 20 34.9
15 4 0 20 55.1
16 6 0 20 45.0
17 0 0.5 20 20.8
18 0 2 20 33.6
19 0 4 20 52.4
20 0 6 20 43.7
21 0.5 0 40 37.6
22 2 0 40 63.2
23 4 0 40 100.9
24 6 0 40 82.1
25 0 0.5 40 37.6
26 0 2 40 60.5
27 0 4 40 94.2
28 0 6 40 76.7
29 0.5 0 60 50.4
30 2 0 60 84.1
31 4 0 60 135.6
32 6 0 60 108.7
33 0 0.5 60 50.4
34 0 ?2 60 80.7
35 0 4 60 127.8
36 0 6 60 103.6
Table 3 2024 aluminum alloy differential arc oxidation condition and experimental results
Sample Nanometer Al powder content (g/L) Nanometer Cr powder content (g/L) The differential arc oxidation time (min) Differential arc oxidation film thickness (μ m)
1 0 0 10 5.5
2 0 0 20 11.6
3 0 0 40 23.8
4 0 0 60 36.0
5 0.5 0 10 8.3
6 2 0 10 13.8
7 4 0 10 22.0
8 6 0 10 17.7
9 0 0.5 10 8.5
10 0 2 10 12.7
11 0 4 10 21.0
12 0 6 10 16.8
13 0.5 0 20 17.4
14 2 0 20 28.9
15 4 0 20 45.9
16 6 0 20 37.1
17 0 0.5 20 17.3
18 0 2 20 27.8
19 0 4 20 43.7
20 0 6 20 36.0
21 0.5 0 40 31.2
22 2 0 40 52.2
23 4 0 40 83.4
24 6 0 40 67.0
25 0 0.5 40 31.1
26 0 2 40 49.8
27 0 4 40 78.3
28 0 6 40 63.9
29 0.5 0 60 41.7
30 2 0 60 69.5
31 4 0 60 111.6
32 6 0 60 89.5
33 0 0.5 60 41.7
34 0 2 60 66.4
35 0 4 60 105.5
36 0 6 60 85.8
Table 4 AZ91D magnesium alloy differential arc oxidation condition and experimental result
Sample Nanometer Al powder content (g/L) Nanometer Cr powder content (g/L) The differential arc oxidation time (min) Differential arc oxidation film thickness (μ m)
1 0 0 10 4.5
2 0 0 20 9.5
3 0 0 40 19.5
4 0 0 60 29.5
5 0.5 0 10 6.8
6 2 0 10 9.9
7 4 0 10 13.6
8 6 0 10 12.7
9 0 0.5 10 7.0
10 0 2 10 10.4
11 0 4 10 14.9
12 0 6 10 12.2
13 0.5 0 20 11.8
14 2 0 20 20.4
15 4 0 20 28.1
16 6 0 20 26.3
17 0 0.5 20 12.7
18 0 2 20 19.9
19 0 4 20 30.4
20 0 6 20 24.9
21 0.5 0 40 22.7
22 2 0 40 32.2
23 4 0 40 49.4
24 6 0 40 44.0
25 0 0.5 40 20.8
26 0 2 40 36.3
27 0 4 40 51.7
28 0 6 40 47.8
29 0.5 0 60 29.6
30 2 0 60 47.8
31 4 0 60 73.3
32 6 0 60 55.2
33 0 0.5 60 29.6
34 0 2 60 45.4
35 0 4 60 63.8
36 0 6 60 56.7
As shown in Figure 1, visible TC4 micro-arc oxidation films is by a spot of amorphous phase and anatase structured TiO 2Form.Micro-arc oxidation process with the prescription as follows: Na 2SiO 36g/L, NaAlO 24g/L, NaOH 1g/L, OP-105ml/L, current density 4A/dm 2, time 10min.
As shown in Figure 2, visible TC4 micro-arc oxidation films is by the TiO of a spot of amorphous phase, anatase structured and rutile structure 2Form, the main peak of matrix is low than among Fig. 1 also, anatase octahedrite TiO 2Diffraction peak than the height of Fig. 1, and more anatase octahedrite TiO is arranged 2Generate, explain that sull is thicker than Fig. 1, and do not find Cr or Cr 2O 3Diffraction peak explains that nanometer Cr does not participate in film forming, and perhaps Cr content seldom is not enough to monitor with XRD in the micro-arc oxidation films.Micro-arc oxidation process with the prescription as follows: Na 2SiO 36g/L, NaAlO 24g/L, NaOH 1g/L, nanometer Cr powder 2g/L, OP-105ml/L, current density 4A/dm 2, time 10min.

Claims (2)

1.一种提高钛合金微弧氧化膜生长速度的方法，其特征是方法步骤为：1. A method for improving the growth rate of titanium alloy micro-arc oxidation film is characterized in that the method steps are: 1)配制微弧氧化溶液：微弧氧化溶液配方如下：Na2SiO3 6g/L，NaAlO2 4g/L和NaOH 1g/L；1) Prepare the micro-arc oxidation solution: the formula of the micro-arc oxidation solution is as follows: Na 2 SiO 3 6g/L, NaAlO 2 4g/L and NaOH 1g/L; 2)向配制好的微弧氧化溶液中添加5mL/L OP-10；2) Add 5mL/L OP-10 to the prepared micro-arc oxidation solution; 3)将步骤2)溶液放在超声波震荡器中震荡10分钟后，加入0.5-6g/L的纳米Al粉或纳米Cr粉，纳米Al粉或纳米Cr粉的粒径范围20-50nm，再超声振荡1h；3) Put the solution in step 2) in an ultrasonic oscillator for 10 minutes, add 0.5-6g/L nano-Al powder or nano-Cr powder, the particle size range of nano-Al powder or nano-Cr powder is 20-50nm, and then ultrasonic Oscillate for 1h; 4)将步骤3)得到溶液从超声波震荡器中取出，使用机械震荡器上下搅拌溶液，将试样和不锈钢阴极放入溶液中，并用导线分别连接微弧氧化电源的阳极和阴极，进行微弧氧化实验，电流密度4-6A/dm2，时间10-60min。4) Take the solution obtained in step 3) out of the ultrasonic oscillator, use a mechanical oscillator to stir the solution up and down, put the sample and stainless steel cathode into the solution, and connect the anode and cathode of the micro-arc oxidation power supply with wires, and perform micro-arc oxidation. Oxidation experiment, current density 4-6A/dm 2 , time 10-60min. 2.根据权利要求1所述的一种提高钛合金微弧氧化膜生长速度的方法，其特征是该方法同样适用于铝合金和镁合金。2. A method for improving the growth rate of titanium alloy micro-arc oxidation film according to claim 1, characterized in that the method is also applicable to aluminum alloys and magnesium alloys.
CN2010102402580A 2010-07-29 2010-07-29 A method of increasing the growth rate of micro-arc oxidation film on titanium alloy Expired - Fee Related CN101892507B (en)

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CN102424998A (en) * 2011-11-27 2012-04-25 西北有色金属研究院 Method for reducing surface roughness of micro-arc oxidation ceramic layer
CN103060881B (en) * 2013-01-25 2016-01-20 北京科技大学 Titanium alloy surface black high temperature coatings preparation method
CN109267136B (en) * 2018-09-26 2020-09-25 西安理工大学 Titanium bolt surface ceramic method based on in-situ growth
CN111172573A (en) * 2018-11-13 2020-05-19 北京艾路浦科技发展有限公司 Preparation method of micro-arc oxidation ceramic membrane

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