CN1515705A - Method for in-situ growth of high hardness and wear-resistant ceramic coating on titanium alloy surface - Google Patents
Method for in-situ growth of high hardness and wear-resistant ceramic coating on titanium alloy surface Download PDFInfo
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- CN1515705A CN1515705A CNA031325866A CN03132586A CN1515705A CN 1515705 A CN1515705 A CN 1515705A CN A031325866 A CNA031325866 A CN A031325866A CN 03132586 A CN03132586 A CN 03132586A CN 1515705 A CN1515705 A CN 1515705A
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- titanium alloy
- hardness
- electrolyte
- ceramic coating
- wear
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000005524 ceramic coating Methods 0.000 title claims abstract description 19
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 10
- 239000003792 electrolyte Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 9
- 239000010935 stainless steel Substances 0.000 claims abstract description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 6
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims abstract description 3
- 229910000883 Ti6Al4V Inorganic materials 0.000 claims description 7
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 15
- 238000000576 coating method Methods 0.000 abstract description 15
- 239000011159 matrix material Substances 0.000 abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052719 titanium Inorganic materials 0.000 abstract description 6
- 239000010936 titanium Substances 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000005611 electricity Effects 0.000 abstract 1
- 239000008151 electrolyte solution Substances 0.000 description 13
- 229910000162 sodium phosphate Inorganic materials 0.000 description 6
- 239000001488 sodium phosphate Substances 0.000 description 6
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- YVBOZGOAVJZITM-UHFFFAOYSA-P ammonium phosphomolybdate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])=O.[O-][Mo]([O-])(=O)=O YVBOZGOAVJZITM-UHFFFAOYSA-P 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010285 flame spraying Methods 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005480 shot peening Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
钛合金表面原位生长高硬度耐磨陶瓷涂层方法，它涉及一种提高钛和钛合金表面硬度的方法。它的步骤是(1)用3－10克/升的铝酸钠、1－3克/升的次亚磷酸盐和水制成电解液；(2)以钛合金为基体并作为正极，以不锈钢板为负极并将两者置于电解液中，控制电解液温度在10－40℃；(3)接通脉冲电源，在五分钟内将电流密度调到400－800A/m2，通电反应90－240分钟；(4)取出试样经水洗、干燥即制成成品。本发明利用等离子体氧化法，在钛合金表面直接形成高硬度陶瓷涂层，有如下特点：1.可通过控制电参数和改变电解液成分调解涂层厚度、相组成，有目的提高其硬度、耐磨性能等；2.该方法由于是在基体上原位生长形成陶瓷涂层，因此与基体结合强度高。The invention discloses a method for in-situ growth of a high-hardness wear-resistant ceramic coating on the surface of a titanium alloy, which relates to a method for increasing the surface hardness of titanium and titanium alloys. Its steps are (1) use 3-10 g/L of sodium aluminate, 1-3 g/L of hypophosphite and water to make electrolyte; (2) use titanium alloy as the matrix and as the positive electrode, and The stainless steel plate is the negative electrode and the two are placed in the electrolyte, and the temperature of the electrolyte is controlled at 10-40°C; (3) Turn on the pulse power supply, and adjust the current density to 400-800A/m 2 within five minutes, and the electricity will react 90-240 minutes; (4) Take out the sample and wash it with water and dry it to make the finished product. The present invention uses the plasma oxidation method to directly form a high-hardness ceramic coating on the surface of the titanium alloy, which has the following characteristics: 1. The thickness and phase composition of the coating can be adjusted by controlling the electrical parameters and changing the composition of the electrolyte, so as to improve its hardness purposefully, 2. In this method, the ceramic coating is formed by in-situ growth on the substrate, so the bonding strength with the substrate is high.
Description
Technical field: the present invention relates to a kind of method that improves titanium and titanium alloy surface hardness.
Background technology: titanium and titanium alloy are wide day by day because of its good solidity to corrosion Application Areas, but titanium or titanium alloy wears no resistance, and be particularly very responsive to the fretting wear damage.For guaranteeing the satisfied requirement of producing reality of titanium and titanium alloy, at the focus of process for modifying surface research the becoming researcher concern that improves the titanium alloy wear resisting property.Improve at present not following 10 kinds of the process for treating surface of the anti-fretting damage of titanium alloy: shot peening strengthening, conventional anodization, nitride laser, electrolytic coating, dry film lubrication layer, plasma spraying or detonation flame spraying layer, physical vapor deposition, organic coating, ion implantation etc.And wherein have impair the conventional fatigue property of titanium alloy base material (causing its conventional fatigue strength to reduce) up to 70% as electroplating Cr; Poor durability that has such as organic binder cemented MoS
2Or graphite dry film; What have causes titanium alloy brittle failure such as Ag or Cd coating.At present at solving Titanium Alloys at High Temperature wear resisting property difference and, being applied in the protection of titanium alloy based on solid film lubricant, hardened surface processing and this process for modifying surface of three types of soft metal coating to the fretting wear sensitive issue.But still have following subject matter: 1 titanium or titanium alloy is the metal to polymkeric substance, metal and ceramic coating poor adhesive force, and ceramic membrane that this forms with regard to making some introduce material from the outside or coating and high base strength are relatively poor.The means that 2 wet methods platings and some comprise high-temperature heat treatment process can cause hydrogen embrittlement---another hidden danger in the titanium alloy Secure Application of titanium alloy.3 wear-resisting and antifatigues are a pair of contradiction, a lot of method for surface hardening can improve hardness improves the titanium alloy wear resisting property, but having sacrificed the toughness of material, is to be cost with the conventional fatigue property (SF) that reduces titanium alloy and fretting fatigue performance (FF).
Summary of the invention: wear no resistance for solving existing titanium alloy, fretting wear is damaged very sensitive issue, the invention provides a kind of titanium alloy surface growth in situ high hardness wear-resisting ceramic coating method.The step of the inventive method is: (1), make electrolytic solution with the sodium aluminate of 3-10 grams per liter, the hypophosphite and the water of 1-3 grams per liter; (2), be matrix and with the titanium alloy as anodal, be negative pole with the stainless steel plate and both placed electrolytic solution that the control electrolyte temperature is at 10-40 ℃; (3), the make pulse power supply, in five minutes, current density is transferred to 400-800A/m
2, energising reaction 90-240 minute; (4), take out sample and promptly make finished product through washing, drying.Also can add additive phosphomolybdate or sodium wolframate in above-mentioned electrolytic solution, its add-on is the 0.3-0.5 grams per liter.Described titanium alloy is Ti-6Al-4V.Little plasma oxidation of the present invention is a new technology at metallic surface growth in situ ceramic membrane.It can directly become membrane of oxide ceramics to the matrix metal oxidation and sinter, does not introduce material from the outside, and different and general process for modifying surface makes the existing high rigidity of ceramic coating, has kept the bonding force of oxide film and matrix again.Performance evaluation of the present invention: the test of coating hardness is adopted Knoop indenter with HVS-1000 type digital display microscope sclerometer; The friction pair of the wear resisting property test of ceramic coating is a bearing steel.The present invention forms the high-hardness ceramic coating with little plasma oxidation method at the Ti-6Al-4V alloy surface, and the total thickness of ceramic coating reaches more than the 100 μ m, and wherein wearing layer thickness reaches 20-60 μ m.The maximum hardness of ceramic coating reaches 15GPa, and the frictional coefficient of bearing steel is reduced to the 1/5-1/3 of titanium alloy substrate, and abrasion loss approaches zero.The invention effect: the present invention utilizes the plasma oxidation method, directly form the high rigidity ceramic coating at titanium alloy surface, following characteristics are arranged: 1. can and change bath composition by the control electrical parameter and reconcile coat-thickness, phase composite, have purpose to improve its hardness, wear resisting property etc.; 2. this method is owing to being that growth in situ forms ceramic coating on matrix, therefore with the substrate combinating strength height.
Embodiment one: the method for present embodiment is: be electrolytic solution with sodium aluminate 7 grams per liters, inferior sodium phosphate 1.5 grams per liters and water 1; 2, with Ti-6Al-4V be matrix and, be negative pole with the stainless steel plate and both are placed electrolytic solution that the control electrolyte temperature is at 10-40 ℃ as anodal; 3, make pulse power supply is set the wave head number and is 1, negative dutycycle 0.45, frequency 50Hz, and makes positive and negative current density reach 400A/M in five minutes
2, the 90 minutes reaction times of energising; 4, take out sample and promptly make finished product through washing, drying.The thickness that present embodiment forms coating is more than the 90 μ m, leans on the matrix internal layer with TiO
2, Al
2TiO
5Xiang Weizhu, superficies contain α-Al
2O
3Phase; The maximum hardness of coating reaches 14.5-15.2GPa; With substrate combinating strength greater than 17MPa; This ceramic coating is between the 0.35-0.6 to the frictional coefficient of bearing steel, and this moment, ceramic coating was not weightless substantially and more to the bearing steel surface scratch of mill.
Embodiment two: the method for present embodiment is: be electrolytic solution with sodium aluminate 7 grams per liters, inferior sodium phosphate 1.5 grams per liters and water 1; 2, with Ti-6Al-4V be matrix and, be negative pole with the stainless steel plate and both are placed electrolytic solution that the control electrolyte temperature is at 10-40 ℃ as anodal; 3, make pulse power supply is set the wave head number and is 1, negative dutycycle 0.45, frequency 50Hz, and makes positive and negative current density reach 800A/M in five minutes
2, the 90 minutes reaction times of energising; 4, take out sample and promptly make finished product through washing, drying.The thickness that present embodiment forms coating is that 80 μ m are above, maximum hardness 14.5GPa.
Embodiment three: the method for present embodiment is: be electrolytic solution with sodium aluminate 4 grams per liters, inferior sodium phosphate 2 grams per liters and water 1; 2, with Ti-6Al-4V be matrix and, be negative pole with the stainless steel plate and both are placed electrolytic solution that the control electrolyte temperature is at 10-40 ℃ as anodal; 3, make pulse power supply is set the wave head number and is 1, negative dutycycle 0.45, frequency 50Hz, and makes positive and negative current density reach 800A/M in five minutes
2, the 90 minutes reaction times of energising; 4, take out sample and promptly make finished product through washing, drying.The thickness that present embodiment forms coating is that 50 μ m are above, coating maximum hardness 8.5GPa.
Embodiment four: the method for present embodiment is: be electrolytic solution with sodium aluminate 7 grams per liters, inferior sodium phosphate 1.5 grams per liters, sodium wolframate 0.3 grams per liter (or ammonium phosphomolybdate 0.5 grams per liter) and water 1; 2, with Ti-6Al-4V be matrix and, be negative pole with the stainless steel plate and both are placed electrolytic solution that the control electrolyte temperature is at 10-40 ℃ as anodal; 3, make pulse power supply is set the wave head number and is 1, negative dutycycle 0.45, frequency 50Hz, and makes the positive current density reach 800A/M in five minutes
2, negative current density reaches 400A/M
2, the 90 minutes reaction times of energising; 4, take out sample and promptly make finished product through washing, drying.The result of present embodiment is identical with embodiment one, but the coating that forms contain α-Al
2O
3The phase thickness layer increases.
Embodiment five: what present embodiment and embodiment two were different is, is electrolytic solution with sodium aluminate 10 grams per liters, inferior sodium phosphate 1.5 grams per liters and water, and other parameter is identical with embodiment two.Its result is identical with embodiment two.
Embodiment six: what present embodiment and embodiment three were different is, is electrolytic solution with sodium aluminate 3 grams per liters, inferior sodium phosphate 1 grams per liter and water, and other parameter is identical with embodiment three.The thickness that present embodiment forms coating is more than the 50 μ m, and the coating maximum hardness is 6.5GPa.
Claims (3)
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| CN 03132586 CN1255579C (en) | 2003-08-29 | 2003-08-29 | Method for in situ growing high-hardness wear resistant ceramic coating layer on titanium alloy surface |
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|---|---|---|---|
| CN 03132586 CN1255579C (en) | 2003-08-29 | 2003-08-29 | Method for in situ growing high-hardness wear resistant ceramic coating layer on titanium alloy surface |
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| Publication Number | Publication Date |
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| CN1515705A true CN1515705A (en) | 2004-07-28 |
| CN1255579C CN1255579C (en) | 2006-05-10 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709470B (en) * | 2009-11-30 | 2011-04-20 | 中国科学院金属研究所 | Preparation method of composite coating containing in situ generated diffusion barrier |
| CN101219707B (en) * | 2006-12-27 | 2011-12-28 | 雅马哈发动机株式会社 | Propeller for watercraft and the method for producing the same, outboard motor and watercraft |
| 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 |
| CN103409786A (en) * | 2013-07-09 | 2013-11-27 | 中国船舶重工集团公司第七二五研究所 | Preparation method of nanometer coating for reducing marine organism adhesion on titanium alloy surface |
| CN103409785A (en) * | 2013-07-09 | 2013-11-27 | 中国船舶重工集团公司第七二五研究所 | Preparation method of nano coating with reduced marine organism attachment on surface of titanium alloy |
| CN104195616A (en) * | 2014-09-04 | 2014-12-10 | 攀钢集团成都钢钒有限公司 | Micro-arc oxidation treatment method of titanium alloy tubing coupling surface |
| CN107841777A (en) * | 2017-11-01 | 2018-03-27 | 西南交通大学 | A kind of preparation method of witch culture Nano tube array of titanium dioxide |
| CN108950646A (en) * | 2018-07-20 | 2018-12-07 | 南京理工大学 | A kind of titanium alloy surface self-lubricating antiwear composite ceramic coating and preparation method thereof |
| CN113943964A (en) * | 2020-07-15 | 2022-01-18 | 中国科学院上海硅酸盐研究所 | Thermal control wear-resistant coating on titanium alloy surface and preparation method thereof |
-
2003
- 2003-08-29 CN CN 03132586 patent/CN1255579C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219707B (en) * | 2006-12-27 | 2011-12-28 | 雅马哈发动机株式会社 | Propeller for watercraft and the method for producing the same, outboard motor and watercraft |
| CN101709470B (en) * | 2009-11-30 | 2011-04-20 | 中国科学院金属研究所 | Preparation method of composite coating containing in situ generated diffusion barrier |
| 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 |
| CN103409786A (en) * | 2013-07-09 | 2013-11-27 | 中国船舶重工集团公司第七二五研究所 | Preparation method of nanometer coating for reducing marine organism adhesion on titanium alloy surface |
| CN103409785A (en) * | 2013-07-09 | 2013-11-27 | 中国船舶重工集团公司第七二五研究所 | Preparation method of nano coating with reduced marine organism attachment on surface of titanium alloy |
| CN103409786B (en) * | 2013-07-09 | 2015-12-02 | 中国船舶重工集团公司第七二五研究所 | A kind ofly reduce the nano coating preparation method of sea organism attachment at titanium alloy surface |
| CN103409785B (en) * | 2013-07-09 | 2015-12-23 | 中国船舶重工集团公司第七二五研究所 | A kind of titanium alloy surface reduces the nano coating preparation method of sea organism attachment |
| CN104195616A (en) * | 2014-09-04 | 2014-12-10 | 攀钢集团成都钢钒有限公司 | Micro-arc oxidation treatment method of titanium alloy tubing coupling surface |
| CN107841777A (en) * | 2017-11-01 | 2018-03-27 | 西南交通大学 | A kind of preparation method of witch culture Nano tube array of titanium dioxide |
| CN107841777B (en) * | 2017-11-01 | 2019-11-01 | 西南交通大学 | A kind of preparation method of witch culture Nano tube array of titanium dioxide |
| CN108950646A (en) * | 2018-07-20 | 2018-12-07 | 南京理工大学 | A kind of titanium alloy surface self-lubricating antiwear composite ceramic coating and preparation method thereof |
| CN113943964A (en) * | 2020-07-15 | 2022-01-18 | 中国科学院上海硅酸盐研究所 | Thermal control wear-resistant coating on titanium alloy surface and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1255579C (en) | 2006-05-10 |
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