CN101498024A - Method for preparing ceramic film on titanium alloy surface - Google Patents
Method for preparing ceramic film on titanium alloy surface Download PDFInfo
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- CN101498024A CN101498024A CNA2009100713629A CN200910071362A CN101498024A CN 101498024 A CN101498024 A CN 101498024A CN A2009100713629 A CNA2009100713629 A CN A2009100713629A CN 200910071362 A CN200910071362 A CN 200910071362A CN 101498024 A CN101498024 A CN 101498024A
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- titanium alloy
- alloy surface
- ceramic film
- ceramic membrane
- preparing ceramic
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Abstract
The invention relates to a method for preparing a ceramic membrane, in particular to a method for preparing a ceramic membrane on a titanium alloy surface, which solves the problem that holes exist on titanium alloy surfaces in the prior art when ceramic membranes are prepared. The method comprises the following steps: polishing the titanium alloy surface to smooth, then washing and placing the titanium alloy surface in an electrolyte as an anode, using a stainless steel plate as a cathode and carrying out a constant-current energizing reaction before washing and drying a titanium alloy; and soaking the titanium alloy into a sodium silicate aqueous solution for depression treatment before drying the titanium alloy so as to obtain the ceramic membrane on the titanium alloy surface. The ceramic membrane prepared by the method has the advantages of compact surface structure, small holes and strong capabilities of resisting high temperature and oxidation. The method is simple and convenient to operate, is easy to obtain raw material and is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic membrane.
Background technology
Titanium alloy has advantages such as density is little, specific tenacity is high, corrosion-resistant as a kind of novel light metal material, is widely used in aerospace and civil area.But the working temperature of titanium alloy is lower, therefore is necessary to apply protective layer on its surface.Adopt the prepared ceramic film of method of differential arc oxidation can improve its high temperature resistant property to a certain extent, but reason owing to discharge channel in the differential arc oxidation process, the hole that has some amount inevitably at coatingsurface makes its high temperature oxidation resistance variation.
Summary of the invention
The objective of the invention is to have the problem of hole at the titanium alloy surface ceramic coating formed by micro-arc oxidation, and a kind of method of preparing ceramic film on titanium alloy surface is provided in order to solve prior art.
The method of preparing ceramic film on titanium alloy surface realizes according to the following steps: one, titanium alloy surface is polished to smooth surface, wash then 3～5min place again electrolytic solution as anodal, be negative pole with the stainless steel plate, the temperature of control electrolytic solution is a room temperature, is 10% in dutycycle, current density is 300～500A/m
2, frequency is to take out behind constant current energising reaction 20～40min under 1500～2500Hz condition, washing 3～5min, seasoning or 100 ℃ of oven dry down promptly get pertusate ceramic membrane; Two, the pertusate ceramic membrane immersion 100～200mL concentration with the step 1 preparation is in 200～400g/L sodium silicate aqueous solution, be to take out behind reduced pressure treatment 5～15min under the condition of 0.002～0.008MPa at sealing of hole pressure, drying is promptly prepared ceramic membrane at titanium alloy surface; Wherein every liter of electrolytic solution is formulated by the water of 4～8g sodium aluminate, 0.5～1g sodium hypophosphite and surplus in the step 1.
The product that the inventive method makes is after carrying out cyclic oxidation 500h under 500 ℃, and gain in weight is less than 0.5g/m
2, improved the high temperature oxidation resistance of sample significantly.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method for present embodiment preparing ceramic film on titanium alloy surface realizes according to the following steps: one, titanium alloy surface is polished to smooth surface, wash then 3～5min place again electrolytic solution as anodal, be negative pole with the stainless steel plate, the temperature of control electrolytic solution is a room temperature, is 10% in dutycycle, current density is 300～500A/m
2, frequency is to take out behind constant current energising reaction 20～40min under 1500～2500Hz condition, washing 3～5min, seasoning or 100 ℃ of oven dry down promptly get pertusate ceramic membrane; Two, the pertusate ceramic membrane immersion 100～200mL concentration with the step 1 preparation is in 200～400g/L sodium silicate aqueous solution, be to take out behind reduced pressure treatment 5～15min under the condition of 0.002～0.008MPa at sealing of hole pressure, drying is promptly prepared ceramic membrane at titanium alloy surface; Wherein every liter of electrolytic solution is formulated by the water of 4～8g sodium aluminate, 0.5～1g sodium hypophosphite and surplus in the step 1.
The titanium alloy that present embodiment adopts is of a size of 1cm * 2cm.
The product that present embodiment makes is after carrying out cyclic oxidation 500h under 500 ℃, and gain in weight is less than 0.5g/m
2
Embodiment two: what present embodiment and embodiment one were different is that current density is 350～450A/m in the step 1
2Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is that current density is 400A/m in the step 1
2Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is that current density is 300A/m in the step 1
2Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is that current density is 500A/m in the step 1
2Other is identical with embodiment one.
Embodiment six: what present embodiment was different with embodiment one or two is that the step 1 medium frequency is 1800～2200Hz.Other is identical with embodiment one or two.
Embodiment seven: what present embodiment was different with embodiment one or two is that the step 1 medium frequency is 2000Hz.Other is identical with embodiment one or two.
Embodiment eight: what present embodiment was different with embodiment one or two is that the step 1 medium frequency is 1500Hz.Other is identical with embodiment one or two.
Embodiment nine: what present embodiment was different with embodiment one or two is that the step 1 medium frequency is 2500Hz.Other is identical with embodiment one or two.
Embodiment ten: what present embodiment and embodiment six were different is to react 25～35min in the step 1.Other is identical with embodiment six.
Embodiment 11: what present embodiment and embodiment six were different is to react 30min in the step 1.Other is identical with embodiment six.
Embodiment 12: what present embodiment and embodiment six were different is to react 20min in the step 1.Other is identical with embodiment six.
Embodiment 13: what present embodiment and embodiment six were different is to react 40min in the step 1.Other is identical with embodiment six.
Embodiment 14: what present embodiment and embodiment one, two or ten were different is that pressure is 0.004～0.006MPa in the step 2.Other is identical with embodiment one, two or ten.
Embodiment 15: what present embodiment and embodiment one, two or ten were different is that pressure is 0.005MPa in the step 2.Other is identical with embodiment one, two or ten.
Embodiment 16: what present embodiment and embodiment one, two or 12 were different is that pressure is 0.002MPa in the step 2.Other is identical with embodiment one, two or ten.
Embodiment 17: what present embodiment and embodiment one, two or ten were different is that pressure is 0.008MPa in the step 2.Other is identical with embodiment one, two or ten.
Embodiment 18: present embodiment and embodiment 14 are different is that the concentration of step 2 mesosilicic acid sodium water solution is 200g/L.Other is identical with embodiment 14.
The product that present embodiment makes is after carrying out cyclic oxidation 500h under 500 ℃, and gain in weight is 0.4g/m
2
Embodiment 19: present embodiment and embodiment 14 are different is that the concentration of step 2 mesosilicic acid sodium water solution is 400g/L.Other is identical with embodiment 14.
The product that present embodiment makes is after carrying out cyclic oxidation 500h under 500 ℃, and gain in weight is 0.05g/m
2
Embodiment 20: the method for present embodiment titanium alloy surface growth in situ ceramic membrane realizes according to the following steps: one, titanium alloy surface is polished to smooth surface, wash then 3min place again electrolytic solution as anodal, be negative pole with the stainless steel plate, the temperature of control electrolytic solution is a room temperature, is 10% in dutycycle, current density is 400A/m
2, frequency is to take out behind the constant current energising reaction 30min under the 2000Hz condition, washing 4min, seasoning promptly gets pertusate ceramic membrane; Two, the pertusate ceramic membrane of step 1 preparation being immersed 150mL concentration is in the 300g/L sodium silicate aqueous solution, at sealing of hole pressure is to take out behind the reduced pressure treatment 10min under the condition of 0.005MPa, and drying is promptly prepared ceramic membrane at titanium alloy surface; Wherein every liter of electrolytic solution is formulated by the water of 4g sodium aluminate, 0.5g sodium hypophosphite and surplus in the step 1.
The product that present embodiment makes is after carrying out cyclic oxidation 500h under 500 ℃, and gain in weight is 0.2g/m
2
Claims (5)
1, the method for preparing ceramic film on titanium alloy surface, the method that it is characterized in that preparing ceramic film on titanium alloy surface realizes according to the following steps: one, titanium alloy surface is polished to smooth surface, wash then 3～5min place again electrolytic solution as anodal, be negative pole with the stainless steel plate, the temperature of control electrolytic solution is a room temperature, is 10% in dutycycle, current density is 300～500A/m
2, frequency is to take out behind constant current energising reaction 20～40min under 1500～2500Hz condition, washing 3～5min, seasoning or 100 ℃ of oven dry down promptly get pertusate ceramic membrane; Two, the pertusate ceramic membrane immersion 100～200mL concentration with the step 1 preparation is in 200～400g/L sodium silicate aqueous solution, be to take out behind reduced pressure treatment 5～15min under the condition of 0.002～0.008MPa at sealing of hole pressure, drying is promptly prepared ceramic membrane at titanium alloy surface; Wherein every liter of electrolytic solution is formulated by the water of 4～8g sodium aluminate, 0.5～1g sodium hypophosphite and surplus in the step 1.
2, the method for preparing ceramic film on titanium alloy surface according to claim 1 is characterized in that current density is 350～450A/m in the step 1
2
3,, it is characterized in that the step 1 medium frequency is 1800～2200Hz according to the method for claim 1,2 described preparing ceramic film on titanium alloy surface.
4, the method for preparing ceramic film on titanium alloy surface according to claim 3 is characterized in that constant current energising reaction 25～35min in the step 1.
5,, it is characterized in that sealing of hole pressure is 0.004～0.006MPa in the step 2 according to the method for claim 1,2 or 4 described preparing ceramic film on titanium alloy surface.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100713629A CN101498024A (en) | 2009-01-24 | 2009-01-24 | Method for preparing ceramic film on titanium alloy surface |
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|---|---|---|---|
| CNA2009100713629A CN101498024A (en) | 2009-01-24 | 2009-01-24 | Method for preparing ceramic film on titanium alloy surface |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194780A (en) * | 2013-04-01 | 2013-07-10 | 哈尔滨工业大学 | Preparation method of titanium alloy surface coating with low solar absorptivity and high emissivity |
| CN103320838A (en) * | 2013-06-03 | 2013-09-25 | 哈尔滨工业大学 | In-situ growth method of yellow ceramic coating on TC4 titanium alloy surface |
| CN106567116A (en) * | 2016-11-10 | 2017-04-19 | 长沙淮石新材料科技有限公司 | Heat-resisting moisture-preserving aluminum alloy and preparation method and application thereof |
| CN107653475A (en) * | 2017-09-12 | 2018-02-02 | 西安庄信新材料科技有限公司 | A kind of method that titanium alloy surface prepares high temperature composite coating using microarc oxidation solution |
| CN109518254A (en) * | 2018-11-27 | 2019-03-26 | 中国船舶重工集团公司第七二五研究所 | A kind of microarc oxidation solution, titanium alloy high rigidity micro-arc oxidation films and preparation and application |
-
2009
- 2009-01-24 CN CNA2009100713629A patent/CN101498024A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194780A (en) * | 2013-04-01 | 2013-07-10 | 哈尔滨工业大学 | Preparation method of titanium alloy surface coating with low solar absorptivity and high emissivity |
| CN103194780B (en) * | 2013-04-01 | 2016-03-02 | 哈尔滨工业大学 | A kind of preparation method of titanium alloy surface low sunlight absorptivity high emissivity coating |
| CN103320838A (en) * | 2013-06-03 | 2013-09-25 | 哈尔滨工业大学 | In-situ growth method of yellow ceramic coating on TC4 titanium alloy surface |
| CN106567116A (en) * | 2016-11-10 | 2017-04-19 | 长沙淮石新材料科技有限公司 | Heat-resisting moisture-preserving aluminum alloy and preparation method and application thereof |
| CN106567116B (en) * | 2016-11-10 | 2018-10-09 | 长沙淮石新材料科技有限公司 | A kind of heat-resisting moisturizing aluminium alloy and its preparation method and application |
| CN107653475A (en) * | 2017-09-12 | 2018-02-02 | 西安庄信新材料科技有限公司 | A kind of method that titanium alloy surface prepares high temperature composite coating using microarc oxidation solution |
| CN109518254A (en) * | 2018-11-27 | 2019-03-26 | 中国船舶重工集团公司第七二五研究所 | A kind of microarc oxidation solution, titanium alloy high rigidity micro-arc oxidation films and preparation and application |
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Open date: 20090805 |