CN101892507B - Method for improving growth speed of titanium alloy microarc oxide film - Google Patents
Method for improving growth speed of titanium alloy microarc oxide film Download PDFInfo
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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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Abstract
The invention discloses a method for improving growth speed of a titanium alloy microarc oxide film, which is characterized by comprising the following steps of: 1) preparing microarc oxidation solution, wherein the formula of the microarc oxidation solution comprises the following components: 6g/L of Na2SiO3, 4g/L of NaAlO2 and 1g/L of NaOH; 2) adding 5mL/L OP-10 surfactant into the prepared microarc oxidation solution; 3) oscillating the solution in the step 2) in an ultrasonic oscillator for 10 minutes and adding 0.5 to 6 g/L nano Al powder or nano Cr powder, wherein the grain diameter of the Al powder or nano Cr powder ranges from 20 to 50 nm, and performing ultrasonic oscillation for 1 hour; and 4) taking the solution obtained in the step 3) out of the ultrasonic oscillator, stirring the solution up and down by using a mechanical oscillator, putting a sample and a stainless steel cathode into the solution, and connecting an anode and a cathode of a microarc oxidation power source by using a lead respectively for a microarc oxidation experiment, wherein the current density is 4 to 6A/dm<2>, and the time is 10 to 60 minutes. The method for improving the growth speed of the titanium alloy microarc oxide film has the advantages that the growth speed of the titanium alloy microarc oxide film can be improved by 0.1 to 3 times under the same deposition process condition.
Description
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
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.
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. method that improves growth speed of titanium alloy microarc oxide film is characterized in that method steps is:
1) preparation 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 for preparing, add 5mL/L OP-10;
3) with 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.
2. a kind of method that improves growth speed of titanium alloy microarc oxide film according to claim 1 is characterized in that this method is equally applicable to duraluminum and magnesiumalloy.
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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 oxidized 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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CN1487124A (en) * | 2002-08-30 | 2004-04-07 | 富士通株式会社 | Process for producing oxidic film with anodization magnesium material |
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CN1623013A (en) * | 2002-03-27 | 2005-06-01 | 岛屿涂层有限公司 | Process and device for forming ceramic coatings on metals and alloys, and coatings produced by this process |
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