CN103233219A - Metal TiN ceramic coating preparation process method - Google Patents
Metal TiN ceramic coating preparation process method Download PDFInfo
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- CN103233219A CN103233219A CN2013100964746A CN201310096474A CN103233219A CN 103233219 A CN103233219 A CN 103233219A CN 2013100964746 A CN2013100964746 A CN 2013100964746A CN 201310096474 A CN201310096474 A CN 201310096474A CN 103233219 A CN103233219 A CN 103233219A
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Abstract
According to the invention, a high energy micro-arc alloying technology and a glow plasma nitriding technology are combined to prepare a TiN coating on the surface of a metal. The process method comprises: adopting a high energy micro-arc alloying technology to deposit a layer of a pure Ti coating on the surface of a metal, wherein pure Ti with a certain specification is selected as a deposition electrode during the preparation process, and a variable thickness of the pure titanium layer can be achieved through controlling key technology parameters in the preparation process; and carrying out a nitriding treatment on the deposited pure titanium layer through a glow plasma nitriding technology to form a TiN layer, wherein during the treatment process, a furnace is adopted as an anode, the titanium layer is adopted as a cathode, ammonia gas or mixed gas of hydrogen gas and nitrogen gas is introduced, and nitrogen ions and nitrogen atoms generated from glow discharge are easily absorbed and permeated by the micro-crystallized Ti layer so as to form the TiN coating on the surface of the micro-crystallized Ti layer.
Description
Technical field
The present invention relates to a kind of modified technique of metallic surface, particularly a kind of preparation method of coating for metal surfaces.
Background technology
Current metallic substance is carried out surface modification, apply coating on its surface and improve the focus that its use properties is research.Wherein metal-ceramic coating shows higher engineering using value with its excellent erosion resistant, high-temperature oxidation resistant, low coefficient of thermal expansion, high rigidity height, wear resistance and thermal conductivity.The TiN coating is traditional metal-ceramic coating, and outward appearance shows as golden yellow, have the hardness height, wear-resistant, corrosion-resistant, anti-oxidant, fusing point is high and characteristics such as conductivity excellence.The protection of metallic surface be can be applied to, metallic surface hardness, wear resistance, solidity to corrosion and oxidation-resistance increased.Traditional TiN coating production often needs to synthesize in advance TiN, again TiN is carried out coating on metallic substrate surface.And in the operation of synthetic TiN, the nitrogen element penetrates into the infiltration effect among the pure Ti, and is undesirable often, and the combination of the coating that these methods obtain and matrix is poor, and tangible interface is arranged, and preparation time length, complex process, cost height.
Summary of the invention:
Technical problem to be solved by this invention is: in the prior art, in the operation of preparation metallic substrate surface TiN coating, often need to synthesize in advance TiN, again TiN is carried out coating on metallic substrate surface, and in the operation of synthetic TiN, the nitrogen element penetrates into the infiltration effect among the pure Ti, and is undesirable often.
For solving this technical problem, technical scheme provided by the invention is:
The invention provides a kind of method for preparing metallic surface TiN coating, this method is, at first by high energy differential of the arc alloying process in the pure Ti coating of metallic surface deposition one deck, will deposit the pure titanium layer of getting well then, carry out nitriding by the glow ion nitriding technology and handle, form the TiN layer.
Above-mentioned preparation method's concrete steps are:
(1) pre-treatment of Ti electrode pole, with Ti electrode pole through acetone ultrasonic cleaning oil removing, ethanol anhydrate, distilled water dries after cleaning,
Ti electrode pole diameter is 0.5-5mm, and purity is greater than 99.9wt%;
(2) pre-treatment of matrix metal material is with the matrix metal material of well cutting, through 400,800,1000
#Sand paper polish step by step to surface-brightening, with acetone ultrasonic cleaning oil removing, ethanol anhydrate, distilled water cleans, dry at last,
Wherein, matrix metal is selected from stainless steel or titanium alloy, and these materials itself have the favorable mechanical performance, is material commonly used in the association area;
(3) high energy differential of the arc Alloying Treatment; with the Ti electrode pole that obtains in the step (1) as depositing electrode; carry out the operation of high energy differential of the arc alloying in metallic substrate surface; power supply is selected the unidirectional pulse AC power; deposition voltage is that 40-100V is adjustable; frequency is 200-600Hz; the electric current pulsewidth is 100-500 μ s; output rating is 200-3000W, adopts argon shield, and depositing electrode constantly rotates vibrations; the electrode speed of rotation is 800r/min-4500r/min; by the control depositing time, can realize that the Ti coat-thickness is adjustable
When adopting argon shield, the gas flow of argon gas is 5-30L/min,
Flow is too little, does not have provide protection, and flow is too big, then can increase the burden of equipment,
This step be utilize the power supply energy stored by in short-term, high-current pulse is with electrode materials fusing and deposit on the metallic matrix, high-current pulse melts electrode materials in coating forming procedure, and forms metallurgical binding with matrix;
(4) glow ion nitriding is handled, the Ti coating that obtains in the step (3) is put into nitriding furnace, body of heater is as anode, the Ti coating feeds the mixed gas of ammonia or hydrogen and nitrogen as negative electrode, and pressure is 400-1200Pa, nitriding temperature is 450-900 ℃, nitriding time is 3-10 hour, generates the TiN coating
In the mixed gas of hydrogen and nitrogen, the volume ratio of hydrogen and nitrogen is 3:1,
In the nitriding treating processes, body of heater is as anode, and titanium layer is as negative electrode, and nitrogen ion, nitrogen-atoms adsorption and diffusion in the Ti of metallic surface coating that glow discharge produces are easy to by the Ti layer adsorption and permeation of micritization, generate one deck TiN coating in the metallic surface.
The invention has the beneficial effects as follows: the present invention prepares metal Ti N ceramic coating, and operating procedure is simple, with low cost.Among the preparation technology of the present invention, do not need to synthesize in advance TiN, but by high energy differential of the arc alloying technology, utilize high-current pulse that electrode materials is melted, in the pure Ti coating of metallic substrate surface deposition one deck, make it to form metallurgical binding with matrix, post-depositional Ti coating generally has micritization or nanocrystalline structure, being conducive to the nitrogen element like this can be more even, penetrates into more fully in the Ti coating, thereby has guaranteed the use properties of TiN coating.
Embodiment
Embodiment 1:
(1) be 5mm with diameter, purity is put into acetone ultrasonic cleaning oil removing greater than the Ti electrode pole of 99.9wt%, and ethanol anhydrates again, cleans with distilled water at last and dries;
(2) select stainless steel as body material, be cut to 7mm * 10mm * 3mm shape, and polish step by step to surface-brightening with 400#, 800#, 1000#SiC sand paper successively, anhydrate with ethanol, after the acetone oil removing, clean and dry with distilled water flushing;
(3) adopt high energy differential of the arc alloying deposition technique, adjustment apparatus and process parameter is: it is 80V that deposition voltage is set, and frequency is 600Hz, and pulsewidth is 200 μ s, and the electrode speed of rotation is 1500r/min, and argon flow amount is 8L/min, and depositing time is 8min.Can generate the Ti coating that thickness is 16 μ m, titanium coatingsurface light, even compact at stainless steel surface.
(4) again the stainless steel of depositing Ti coating, put into that Wuhan glow plasma Equipment for Heating Processing company limited produces, model is in the nitriding furnace of MC-55AQK, carry out glow ion nitriding, selection gas is ammonia, and pressure is 400Pa, nitriding temperature is 450 ℃, and nitriding time is 4h.Treat that nitriding finishes the back and takes out sample, formed the TiN coating at stainless steel surface.
After tested, coating hardness is higher than 60HRC, and the compactness of coating is good, because ceramic coating itself is anti-corrosion, so corrosive nature is better; Be metallurgical binding with matrix in addition, because in the deposition process be the fusion mode, bonding force is good.
Embodiment 2:
The working method of step (1) and step (2) shown in embodiment 1,
(3) adopt high energy differential of the arc alloying deposition technique, adjustment apparatus and process parameter is: it is 90V that deposition voltage is set, and frequency is 400Hz, and pulsewidth is 150 μ s, and the electrode speed of rotation is 1000r/min, and argon flow amount is 5L/min, and depositing time is 6min.Can generate the Ti coating that thickness is 13 μ m, titanium coatingsurface light, even compact at stainless steel surface;
(4) again the stainless steel of depositing Ti coating, put into that Wuhan glow plasma Equipment for Heating Processing company limited produces, model is in the nitriding furnace of MC-55AQK, carry out glow ion nitriding, selecting gas is the mixed gas (hydrogen nitrogen volume ratio is 3:1) of hydrogen and nitrogen, pressure is 600Pa, and nitriding temperature is 550 ℃, and nitriding time is 8h.Treat that nitriding finishes the back and takes out sample, formed the TiN coating at stainless steel surface.
After tested, coating hardness is higher than 60HRC, and the compactness of coating is good, because ceramic coating itself is anti-corrosion, so corrosive nature is better; Be metallurgical binding with matrix in addition, because in the deposition process be the fusion mode, bonding force is good.
Embodiment 3:
Select the TC4 titanium alloy as body material, the working method of step (1) and step (2) shown in embodiment 1,
(3) adopt high energy differential of the arc alloying deposition technique, adjustment apparatus and process parameter is: it is 70V that deposition voltage is set, and frequency is 500Hz, and pulsewidth is 300 μ s, and the electrode speed of rotation is 1200r/min, and argon flow amount is 10L/min, and depositing time is 5min.Can generate thickness at the TC4 titanium alloy surface is the Ti coating of 11 μ m, titanium coatingsurface light, even compact;
(4) again the TC4 titanium alloy of depositing Ti coating, put into that Wuhan glow plasma Equipment for Heating Processing company limited produces, model is in the nitriding furnace of MC-55AQK, carry out glow ion nitriding, selection gas is ammonia, and pressure is 1100Pa, nitriding temperature is 900 ℃, and nitriding time is 3h.Treat that nitriding finishes the back and takes out sample, formed the TiN coating at the TC4 titanium alloy surface.
After tested, coating hardness is higher than 60HRC, and the compactness of coating is good, because ceramic coating itself is anti-corrosion, so corrosive nature is better; Be metallurgical binding with matrix in addition, because in the deposition process be the fusion mode, bonding force is good.
Embodiment 4:
Select the TC4 titanium alloy as body material, the working method of step (1) and step (2) shown in embodiment 1,
(3) adopt high energy differential of the arc alloying deposition technique, adjustment apparatus and process parameter is: it is 100V that deposition voltage is set, and frequency is 300Hz, and pulsewidth is 400 μ s, and the electrode speed of rotation is 1300r/min, and argon flow amount is 8L/min, and depositing time is 12min.Can generate thickness at the TC4 titanium alloy surface is the Ti coating of 22 μ m, titanium coatingsurface light, even compact;
(4) again the TC4 titanium alloy of depositing Ti coating, put into that Wuhan glow plasma Equipment for Heating Processing company limited produces, model is in the nitriding furnace of MC-55AQK, carry out glow ion nitriding, selecting gas is the mixed gas (hydrogen nitrogen volume ratio is 3:1) of hydrogen and nitrogen, pressure is 1200Pa, and nitriding temperature is 800 ℃, and nitriding time is 6h.Treat that nitriding finishes the back and takes out sample, formed the TiN coating at the TC4 titanium alloy surface.
After tested, coating hardness is higher than 60HRC, and the compactness of coating is good, because ceramic coating itself is anti-corrosion, so corrosive nature is better; Be metallurgical binding with matrix in addition, because in the deposition process be the fusion mode, bonding force is good.
Claims (6)
1. method for preparing metallic surface TiN coating, it is characterized in that: described method is, at first by high energy differential of the arc alloying process in the pure Ti coating of metallic surface deposition one deck, will deposit the pure titanium layer of getting well then, carry out nitriding by the glow ion nitriding technology and handle, form the TiN layer.
2. the method for preparing metallic surface TiN coating as claimed in claim 1, it is characterized in that: the concrete steps of described method are
(1) pre-treatment of Ti electrode pole, with Ti electrode pole through acetone ultrasonic cleaning oil removing, ethanol anhydrate, distilled water dries after cleaning;
(2) pre-treatment of matrix metal material is with the matrix metal material of well cutting, through 400,800,1000
#Sand paper polish step by step to surface-brightening, with acetone ultrasonic cleaning oil removing, ethanol anhydrate, distilled water cleans, dry at last;
(3) high energy differential of the arc Alloying Treatment, with the Ti electrode pole that obtains in the step (1) as depositing electrode, carry out the operation of high energy differential of the arc alloying in metallic substrate surface, power supply is selected the unidirectional pulse AC power, deposition voltage is that 40-100V is adjustable, frequency is 200-600Hz, the electric current pulsewidth is 100-500 μ s, output rating is 200-3000W, adopt argon shield, depositing electrode constantly rotates vibrations, and the electrode speed of rotation is 800r/min-4500r/min, by the control depositing time, can realize that the Ti coat-thickness is adjustable;
(4) glow ion nitriding is handled, the Ti coating that obtains in the step (3) is put into nitriding furnace, body of heater is as anode, the Ti coating is as negative electrode, feed the mixed gas of ammonia or hydrogen and nitrogen, pressure is 400-1200Pa, and nitriding temperature is 450-900 ℃, nitriding time is 3-10 hour, generates the TiN coating.
3. the method for preparing metallic surface TiN coating as claimed in claim 2, it is characterized in that: the Ti electrode pole diameter described in the step (1) is 0.5-5mm, and purity is greater than 99.9wt%.
4. the method for preparing metallic surface TiN coating as claimed in claim 2, it is characterized in that: the matrix metal described in the step (2) is selected from stainless steel or titanium alloy.
5. the method for preparing metallic surface TiN coating as claimed in claim 2, it is characterized in that: in the argon shield described in the step (3), gas flow is 5-30L/min.
6. the method for preparing metallic surface TiN coating as claimed in claim 2, it is characterized in that: in the mixed gas of the hydrogen described in the step (4) and nitrogen, the volume ratio of hydrogen and nitrogen is 3:1.
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Cited By (13)
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|---|---|---|---|---|
| CN103710695A (en) * | 2013-12-25 | 2014-04-09 | 长春金海硬质涂层有限公司 | Preparation method of titanium carbonitride protective coating used for metal workpiece surface |
| CN103990178A (en) * | 2014-06-07 | 2014-08-20 | 赵全明 | Preparation process of titanium nitride-coated artificial joint |
| CN104846398A (en) * | 2015-05-29 | 2015-08-19 | 华北水利水电大学 | Titanium-based TiNx/IrO2-Ta2O5 coating anode |
| CN105349944A (en) * | 2015-11-12 | 2016-02-24 | 浙江百纳橡塑设备有限公司 | Titanium nitride chromium coating and double glow plasma seepage preparing method thereof |
| CN105821459A (en) * | 2016-03-29 | 2016-08-03 | 常州大学 | Method for preparing boride coating on stainless steel surface |
| CN106435495A (en) * | 2016-08-31 | 2017-02-22 | 江苏华力金属材料有限公司 | Preparation method for TiN-Ti composite coating on surface of stainless steel sheet |
| CN106521419A (en) * | 2016-11-29 | 2017-03-22 | 大连圣洁真空技术开发有限公司开发区分公司 | Alloy surface titanizing technology |
| CN109371355A (en) * | 2018-11-21 | 2019-02-22 | 中国航发哈尔滨东安发动机有限公司 | A method of color at the control titanium alloy bearing insert class part angle of cut |
| CN109972080A (en) * | 2019-04-26 | 2019-07-05 | 常州大学 | A kind of titanium enhancing high-effect ionic nitriding method |
| CN110760788A (en) * | 2019-10-29 | 2020-02-07 | 长春奥普光电技术股份有限公司 | Modification treatment method for surface hardness of cast titanium alloy |
| CN113308694A (en) * | 2021-06-30 | 2021-08-27 | 广东牧人王电器有限公司 | Titanium-nitrogen co-permeation process and one-hundred-year unbreakable pot processed by same |
| CN114164400A (en) * | 2021-12-17 | 2022-03-11 | 沈阳博尔雅生物科技有限公司 | Nickel-titanium alloy root canal file without nickel on surface and preparation method thereof |
| CN114214620A (en) * | 2021-12-17 | 2022-03-22 | 沈阳博尔雅生物科技有限公司 | Preparation method of root canal file nano TiN coated film |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710695A (en) * | 2013-12-25 | 2014-04-09 | 长春金海硬质涂层有限公司 | Preparation method of titanium carbonitride protective coating used for metal workpiece surface |
| CN103710695B (en) * | 2013-12-25 | 2016-02-03 | 长春金海硬质涂层有限公司 | A kind of preparation method for surface of workpiece titanium carbonitride protective coating |
| CN103990178A (en) * | 2014-06-07 | 2014-08-20 | 赵全明 | Preparation process of titanium nitride-coated artificial joint |
| CN104846398A (en) * | 2015-05-29 | 2015-08-19 | 华北水利水电大学 | Titanium-based TiNx/IrO2-Ta2O5 coating anode |
| CN105349944A (en) * | 2015-11-12 | 2016-02-24 | 浙江百纳橡塑设备有限公司 | Titanium nitride chromium coating and double glow plasma seepage preparing method thereof |
| CN105821459B (en) * | 2016-03-29 | 2018-06-26 | 常州大学 | A kind of method for preparing boride coating in stainless steel surface |
| CN105821459A (en) * | 2016-03-29 | 2016-08-03 | 常州大学 | Method for preparing boride coating on stainless steel surface |
| CN106435495A (en) * | 2016-08-31 | 2017-02-22 | 江苏华力金属材料有限公司 | Preparation method for TiN-Ti composite coating on surface of stainless steel sheet |
| CN106435495B (en) * | 2016-08-31 | 2019-01-22 | 江苏华力金属材料有限公司 | The preparation method of Thin Stainless Steel plate surface TiN-Ti composite coating |
| CN106521419A (en) * | 2016-11-29 | 2017-03-22 | 大连圣洁真空技术开发有限公司开发区分公司 | Alloy surface titanizing technology |
| CN109371355A (en) * | 2018-11-21 | 2019-02-22 | 中国航发哈尔滨东安发动机有限公司 | A method of color at the control titanium alloy bearing insert class part angle of cut |
| CN109972080A (en) * | 2019-04-26 | 2019-07-05 | 常州大学 | A kind of titanium enhancing high-effect ionic nitriding method |
| CN110760788A (en) * | 2019-10-29 | 2020-02-07 | 长春奥普光电技术股份有限公司 | Modification treatment method for surface hardness of cast titanium alloy |
| CN113308694A (en) * | 2021-06-30 | 2021-08-27 | 广东牧人王电器有限公司 | Titanium-nitrogen co-permeation process and one-hundred-year unbreakable pot processed by same |
| CN113308694B (en) * | 2021-06-30 | 2023-09-01 | 广东牧人王电器有限公司 | Titanium-nitrogen co-permeation process and hundred-year-old non-rotting pot for processing same |
| CN114164400A (en) * | 2021-12-17 | 2022-03-11 | 沈阳博尔雅生物科技有限公司 | Nickel-titanium alloy root canal file without nickel on surface and preparation method thereof |
| CN114214620A (en) * | 2021-12-17 | 2022-03-22 | 沈阳博尔雅生物科技有限公司 | Preparation method of root canal file nano TiN coated film |
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Denomination of invention: A process method for preparing metal tin ceramic coating Effective date of registration: 20220426 Granted publication date: 20150603 Pledgee: Jiangsu Rudong Rural Commercial Bank Co.,Ltd. Nankan sub branch Pledgor: Nantong Hongsheng gloves Co.,Ltd. Registration number: Y2022320000194 |