CN103233219B - Metal TiN ceramic coating preparation process method - Google Patents
Metal TiN ceramic coating preparation process method Download PDFInfo
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- CN103233219B CN103233219B CN201310096474.6A CN201310096474A CN103233219B CN 103233219 B CN103233219 B CN 103233219B CN 201310096474 A CN201310096474 A CN 201310096474A CN 103233219 B CN103233219 B CN 103233219B
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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 surface modification is carried out to metallic substance, apply coating on its surface and improve the focus that its use properties is research.Wherein metal-ceramic coating, wear resistance high with the erosion resistant of its excellence, high-temperature oxidation resistant, low coefficient of thermal expansion, high rigidity and thermal conductivity show higher engineer applied and are worth.TiN coating is traditional metal-ceramic coating, and appearance is golden yellow, the feature such as have that hardness is high, wear-resistant, corrosion-resistant, anti-oxidant, fusing point is high and conductivity is excellent.The protection of metallic surface can be applied to, increase metallic surface hardness, wear resistance, solidity to corrosion and oxidation-resistance.Traditional TiN coating production, often needs pre-synthesis TiN, then TiN is carried out coating in metallic substrate surface.And in the operation of synthesis TiN, nitrogen element penetrates into the infiltration effect in pure Ti, undesirable often, and the combination of the coating that these methods obtain and matrix is poor, has obvious interface, and preparation time length, complex process, cost are high.
Summary of the invention:
Technical problem to be solved by this invention is: in prior art, in the operation of preparation metallic substrate surface TiN coating, often need pre-synthesis TiN, again TiN is carried out coating in metallic substrate surface, and in the operation of synthesis TiN, nitrogen element penetrates into the infiltration effect in pure Ti, undesirable often.
For solving this technical problem, technical scheme provided by the invention is:
The invention provides a kind of method preparing metallic surface TiN coating, the method is, first deposits the pure Ti coating of one deck by high energy differential of the arc alloying process in metallic surface, the pure titanium layer then will deposited, carry out Nitrizing Treatment by glow ion nitriding technology, form TiN layer.
The concrete steps of above-mentioned preparation method are:
(1) pre-treatment of Ti electrode pole, anhydrates Ti electrode pole through acetone ultrasonic cleaning oil removing, ethanol, dries after distilled water cleaning,
Ti electrode diameter of the rod is 0.5-5mm, and purity is greater than 99.9wt%;
(2) pre-treatment of matrix metal material, by 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, finally dry,
Wherein, matrix metal is selected from stainless steel or titanium alloy, and these materials itself have good mechanical property, is material conventional in association area;
(3) high energy differential of the arc Alloying Treatment; using the Ti electrode pole that obtains in step (1) as depositing electrode; the operation of high energy differential of the arc alloying is carried out in metallic substrate surface; power supply selects unidirectional pulse AC power; deposition voltage is that 40-100V is adjustable; frequency is 200-600Hz; electric current pulsewidth is 100-500 μ s; output rating is 200-3000W, and adopt argon shield, depositing electrode constantly rotates vibrations; electrode rotary speed is 800r/min-4500r/min; by controlling depositing time, Ti coat-thickness can be realized 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 large, then can increase the burden of equipment,
This step is that the energy utilizing power supply to store passes through in short-term, electrode materials melts and deposits on metallic matrix by high-current pulse, and in coating forming procedure, electrode materials melts by high-current pulse, and forms metallurgical binding with matrix;
(4) glow ion nitriding process, the Ti coating obtained in step (3) is put into nitriding furnace, body of heater is as anode, Ti coating, as negative electrode, passes into the mixed gas of ammonia or hydrogen and nitrogen, and pressure is 400-1200Pa, nitriding temperature is 450-900 DEG C, nitriding time is 3-10 hour, generates TiN coating
In the mixed gas of hydrogen and nitrogen, the volume ratio of hydrogen and nitrogen is 3:1,
In Nitrizing Treatment process, body of heater is as anode, and titanium layer is as negative electrode, and Nitrogen ion, nitrogen-atoms adsorption and diffusion in the Ti coating of metallic surface that glow discharge produces, be easy to, by the Ti layer adsorption and permeation of micritization, generate one deck TiN coating in metallic surface.
The invention has the beneficial effects as follows: the present invention prepares metal Ti N ceramic coating, operating procedure is simple, with low cost.In preparation technology of the present invention, do not need pre-synthesis TiN, but by high energy differential of the arc alloying technology, utilize high-current pulse to be melted by electrode materials, deposit the pure Ti coating of one deck in metallic substrate surface, make it to form metallurgical binding with matrix, post-depositional Ti coating generally has micritization or nanocrystalline structure, be conducive to like this nitrogen element can evenly, penetrate into more fully in Ti coating, thus ensure that the use properties of TiN coating.
Embodiment
Embodiment 1:
(1) be 5mm by diameter, the Ti electrode pole that purity is greater than 99.9wt% puts into acetone ultrasonic cleaning oil removing, then ethanol anhydrates, and finally cleans with distilled water and dries;
(2) select stainless steel as body material, be cut to 7mm × 10mm × 3mm shape, and carry out step by step polishing to surface-brightening with 400#, 800#, 1000#SiC sand paper successively, anhydrate with ethanol, after acetone oil removing, clean and dry with distilled water flushing;
(3) adopt high energy differential of the arc alloying deposition technique, adjustment technical parameter is: arranging deposition voltage is 80V, and frequency is 600Hz, and pulsewidth is 200 μ s, and electrode rotary speed is 1500r/min, and argon flow amount is 8L/min, and depositing time is 8min.The Ti coating that thickness is 16 μm can be generated, titanium coating surface-brightening, 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 DEG C, and nitriding time is 4h.After nitriding terminates, take out sample, define 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, therefore corrosive nature is better; Be metallurgical binding with matrix in addition, because in deposition process be fusion mode, bonding force is good.
Embodiment 2:
The working method of step (1) and step (2) as described in Example 1,
(3) adopt high energy differential of the arc alloying deposition technique, adjustment technical parameter is: arranging deposition voltage is 90V, and frequency is 400Hz, and pulsewidth is 150 μ s, and electrode rotary speed is 1000r/min, and argon flow amount is 5L/min, and depositing time is 6min.The Ti coating that thickness is 13 μm can be generated, titanium coating surface-brightening, even compact at stainless steel surface;
(4) again the stainless steel of depositing Ti coating, put into Wuhan glow plasma equipment for Heating Processing company limited produce, model is in the nitriding furnace of MC-55AQK, carry out glow ion nitriding, selection gas is the mixed gas (hydrogen nitrogen volume ratio is 3:1) of hydrogen and nitrogen, pressure is 600Pa, and nitriding temperature is 550 DEG C, and nitriding time is 8h.After nitriding terminates, take out sample, define 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, therefore corrosive nature is better; Be metallurgical binding with matrix in addition, because in deposition process be fusion mode, bonding force is good.
Embodiment 3:
Select TC4 titanium alloy as body material, the working method of step (1) and step (2) as described in Example 1,
(3) adopt high energy differential of the arc alloying deposition technique, adjustment technical parameter is: arranging deposition voltage is 70V, and frequency is 500Hz, and pulsewidth is 300 μ s, and electrode rotary speed is 1200r/min, and argon flow amount is 10L/min, and depositing time is 5min.The Ti coating that thickness is 11 μm can be generated, titanium coating surface-brightening, even compact at TC4 titanium alloy surface;
(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 DEG C, and nitriding time is 3h.After nitriding terminates, take out sample, define TiN coating at 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, therefore corrosive nature is better; Be metallurgical binding with matrix in addition, because in deposition process be fusion mode, bonding force is good.
Embodiment 4:
Select TC4 titanium alloy as body material, the working method of step (1) and step (2) as described in Example 1,
(3) adopt high energy differential of the arc alloying deposition technique, adjustment technical parameter is: arranging deposition voltage is 100V, and frequency is 300Hz, and pulsewidth is 400 μ s, and electrode rotary speed is 1300r/min, and argon flow amount is 8L/min, and depositing time is 12min.The Ti coating that thickness is 22 μm can be generated, titanium coating surface-brightening, even compact at TC4 titanium alloy surface;
(4) again the TC4 titanium alloy of depositing Ti coating, put into Wuhan glow plasma equipment for Heating Processing company limited produce, model is in the nitriding furnace of MC-55AQK, carry out glow ion nitriding, selection gas is the mixed gas (hydrogen nitrogen volume ratio is 3:1) of hydrogen and nitrogen, pressure is 1200Pa, and nitriding temperature is 800 DEG C, and nitriding time is 6h.After nitriding terminates, take out sample, define TiN coating at 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, therefore corrosive nature is better; Be metallurgical binding with matrix in addition, because in deposition process be fusion mode, bonding force is good.
Claims (5)
1. prepare a method for metallic surface TiN coating, it is characterized in that: described method is, first deposit the pure Ti coating of one deck by high energy differential of the arc alloying process in metallic surface, then the pure titanium layer will deposited, carry out Nitrizing Treatment by glow ion nitriding technology, form TiN layer
The concrete steps of described method are,
(1) pre-treatment of Ti electrode pole, anhydrates Ti electrode pole through acetone ultrasonic cleaning oil removing, ethanol, dries after distilled water cleaning;
(2) pre-treatment of matrix metal material, by 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, finally dry;
(3) high energy differential of the arc Alloying Treatment, using the Ti electrode pole that obtains in step (1) as depositing electrode, the operation of high energy differential of the arc alloying is carried out in metallic substrate surface, power supply selects unidirectional pulse AC power, deposition voltage is that 40-100V is adjustable, frequency is 200-600Hz, electric current pulsewidth is 100-500 μ s, output rating is 200-3000W, adopt argon shield, depositing electrode constantly rotates vibrations, and electrode rotary speed is 800r/min-4500r/min, by controlling depositing time, Ti coat-thickness can be realized adjustable;
(4) glow ion nitriding process, the Ti coating obtained in step (3) is put into nitriding furnace, body of heater is as anode, Ti coating is as negative electrode, pass into the mixed gas of ammonia or hydrogen and nitrogen, pressure is 400-1200Pa, and nitriding temperature is 450-900 DEG C, nitriding time is 3-10 hour, generates TiN coating.
2. prepare the method for metallic surface TiN coating as claimed in claim 1, it is characterized in that: the Ti electrode diameter of the rod described in step (1) is 0.5-5mm, and purity is greater than 99.9wt%.
3. prepare the method for metallic surface TiN coating as claimed in claim 1, it is characterized in that: the matrix metal described in step (2) is selected from stainless steel or titanium alloy.
4. prepare the method for metallic surface TiN coating as claimed in claim 1, it is characterized in that: in the argon shield described in step (3), gas flow is 5-30L/min.
5. prepare the method for metallic surface TiN coating as claimed in claim 1, it is characterized in that: in the mixed gas of the hydrogen described in step (4) and nitrogen, the volume ratio of hydrogen and nitrogen is 3:1.
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| 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 |
| CN104846398B (en) * | 2015-05-29 | 2017-08-01 | 华北水利水电大学 | A kind of titanium-based TiNx/IrO2‑Ta2O5Coated 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 |
| 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 |
| 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 |
| 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 |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101994077A (en) * | 2010-10-27 | 2011-03-30 | 江苏科技大学 | High-temperature oxidation resisting intermetallic compound coating and preparation method thereof |
| CN101922037B (en) * | 2010-09-26 | 2012-02-15 | 武汉大学 | Method for preparing nitrogen-doped titanium dioxide nanotube array |
| CN102732832A (en) * | 2012-06-28 | 2012-10-17 | 南京航空航天大学 | Titanium alloy surface high temperature oxidation resistance and wear resistance oxide gradient coat, and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101922037B (en) * | 2010-09-26 | 2012-02-15 | 武汉大学 | Method for preparing nitrogen-doped titanium dioxide nanotube array |
| CN101994077A (en) * | 2010-10-27 | 2011-03-30 | 江苏科技大学 | High-temperature oxidation resisting intermetallic compound coating and preparation method thereof |
| CN102732832A (en) * | 2012-06-28 | 2012-10-17 | 南京航空航天大学 | Titanium alloy surface high temperature oxidation resistance and wear resistance oxide gradient coat, and preparation method thereof |
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Effective date of registration: 20201117 Address after: 307 Yuxi Road, Dayu Town, Rudong County, Nantong City, Jiangsu Province Patentee after: Nantong Hongsheng gloves Co., Ltd Address before: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Patentee before: CHANGZHOU University |
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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 |