CN1451779A - Process for glow ion hydrogen-free carbonizing titanium surface - Google Patents
Process for glow ion hydrogen-free carbonizing titanium surface Download PDFInfo
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- CN1451779A CN1451779A CN 03119527 CN03119527A CN1451779A CN 1451779 A CN1451779 A CN 1451779A CN 03119527 CN03119527 CN 03119527 CN 03119527 A CN03119527 A CN 03119527A CN 1451779 A CN1451779 A CN 1451779A
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Abstract
A non-hydrogen glow ion process for carbonizing the surface of titanium (or Ti alloy) is characterized by that under the action of electric bias field and inert energy, the carbon ions (or atoms) sputted out from graphite electrode in glow plasmas reach to the surface of hot titanium workpiece, and under the action of thermal diffusion and ion bombardment the carbon ions (or atoms) come in the surface of titanium to form titanium carbide. Its advantages are high surface hardness (3000 HV) and antiwear nature, and deep carbonized layer.
Description
Affiliated technical field
A kind of titanium surface glow ion non-hydrogen carbonizing processing method relates to a kind of metal surface properties modification technology, the particularly modification technology on titanium or titanium alloy surface.
Background technology
The titanium material is owing to have advantages such as specific tenacity height, solidity to corrosion are good, is applied in increase constantly in all trades and professions.Begin to widely apply as fields such as Aeronautics and Astronautics, ocean, petrochemical complex and weapons.Used titanium or titanium alloy aboard in a large number, in aircraft engine, titanium material blade problems such as wearing and tearing, burn-back or burning can occur when work.Heavy lesson has been arranged on the airplane crash history.Problems such as not wear-resisting and easy burn-back also can take place in the titanium material when using as other functional materials.As the countermeasure of these problems, improve the surface abrasion resistance of titanium or titanium alloy exactly.For this reason, the technician to have carried out many be the Research on Surface Modification work of purpose to improve the titanium surface abrasion resistance.
The quick Ni-P coating of electroplating 500 μ m thickness that works out of Japan's Nishimoto English has been improved the wear resistance of titanium.Japanese kobe steel work out the Ni-P coating of modification on this basis, and called after KENI-COAT, surface hardness reaches 600～900HV, thickness can reach 700 μ m.All be better than electroless plating from toughness, anti-sliding capability, anti-rolling characteristics, impact resistance and lubricity aspect, disperse plating, nitrogenize, spraying and ion plating TiN rete.
Adopt ion implantation C
+Ion has also been realized the raising of the wear resisting property of titanium.But efficient is low, cost is high, is difficult to realize scale production.
The titanium surface cementation also can improve the wear resistance of titanium material, mainly contain following processing method in the titanium surface cementation: 1. liquid carburizing: liquid carburizing is to be main component with prussiates such as NaCN, KCN or K4Fe (CN) 6, add all the vessel in heating fusings of packing into of NaCI carburizing agent, iron and steel is immersed wherein salt bath.Prussiate decomposes and generates CO and N, and C and N infiltrate steel simultaneously.Should cry carbonitriding in fact.This method is simple to operate, and the low carburizing time of treatment temp is short, be out of shape for a short time, but this can generate severe toxicity when oozing method reaction, and working condition is harshness very.2. vacuum carburization: vacuum carburization is that workpiece is put into stove, and the stove internal gas pressure is reduced pressure about 1.33 handkerchiefs, directly feeds refine methane gas and carry out carburizing after 1040 ℃ of heat.3. plasma carburising: the ion carburizing, glowdischarge carburizing method is that hydrocarbon gas such as methane or propane are gone in the road in a vacuum, simultaneously between negative electrode and anode, add volts DS, make it produce glow discharge, and the generation plasma body, the carbon ion and the hydrogen ion that produce, under effect of electric field, bombardment is in the workpiece surface of negative electrode, has realized the carburizing on titanium surface.
Aspect patent, Zhu of Tsing-Hua University opens " ion bombardment ageing and surface strengthening method of titanium alloy " (patent No.: ZL99126286.7) relate to a kind of ion bombardment ageing and surface strengthening method of titanium alloy of school invention, at first titanium alloy is carried out solution treatment, place ion bombarding furnace again, electron-beam furnace is vacuumized, feed reactant gases, reactant gases is ammonia or ammonia+acetone steam, add bombarding voltage and carry out the ion bombardment timeliness, and infiltrate nitrogen or nitrogen carbon is the titanium alloy that timeliness of the present invention is held concurrently surface strengthening.Method of the present invention can make titanium alloy improve the hardness and the wear resistance on intensity and surface, and surface hardness can be increased to 800～1000HV.
The above carburizing process method of titanium exists the problem of serious environment pollution or hydrogen embrittlement.The admittedly molten limit of hydrogen in titanium has only tens PPm, under the temperature more than 80 ℃, the spread coefficient of hydrogen in titanium is very big, the performance of serious harm titanium, and harm mainly contains two aspects: the one, dissolving in of hydrogen causes very big crystal lattice stress and forms very crisp titanium hydride; The 2nd, hydrogen is easily assembled to the defect area of material, has reduced the concentration, particularly grain-boundary strength of defective, and brings out crackle and cause crack propagation.Directly translating into the plasticity of material and toughness and tensile strength descends greatly.A lot of titaniums having taken place in industry inhaled the accident of hydrogen, has lost huge.None is not relevant with protium for technologies such as gas carburizing, vacuum carburizing and plasma carburizing commonly used at present.In carburizing, always there is protium to penetrate in the matrix, hydrogen embrittlement occurs and ask body, have a strong impact on the carburizing quality of titanium material.
Summary of the invention
The present invention is exactly the deficiency that exists in the above raising titanium surface abrasion resistance Technology, a kind of requirement that can make the titanium or titanium alloy surface reach wear resisting property is provided, can not occurs the method for the titanium that technology is simple, cost is low, performance the is good surface glow ion non-hydrogen carbonizing of problems such as hydrogen embrittlement again.
Method of the present invention is achieved through the following technical solutions.
A kind of titanium surface glow ion non-hydrogen carbonizing processing method, it is characterized in that utilizing Graphite Electrodes in glow plasma by sputter, make the carbon ion that sputters out or carbon atom under the kinetic energy action of inertia of workpiece bias electric field and particle, arrive heated titanium workpiece surface, under the dual function of thermodiffusion and ion bombardment, make carbon penetrate into the titanium surface and form titanium carbide, the graphite source electrode, the glow discharge that produces between titanium workpiece and the vacuum chamber, the carbon of graphite source electrode is penetrated into surface through the titanium workpiece of well heater and hollow cathode effect heating, formed infiltration layer and the settled layer of TiC on the surface of titanium workpiece.
The equipment of titanium of the present invention surface aura non-hydrogen carbonizing, it is characterized in that vacuum chamber is by the vacuum acquiring system extracting vacuum, being provided with in the vacuum chamber can rotation and the work rest of revolution, graphite source electrode, the well heater with ac power supply unsettled with the idiostatic thermofin of vacuum chamber, the current potential of ground connection, at the dc bias power of vacuum chamber peripheral hardware argon gas feed system, the power supply of titanium workpiece, the direct current source electrode power supply and the temp measuring system of graphite source electrode power supply.
The processing parameter of titanium of the present invention surface aura non-hydrogen carbonizing is at partial pressure of ar gas 1 * 10
3～1 * 10
-1Pa, the temperature of titanium workpiece 4 is at 700～1300 ℃, the voltage 200～1200V of source electrode 1, the voltage 200～1000V of titanium workpiece 4 handled through 0.5～5 hour, and the infiltration layer on titanium workpiece 4 surfaces reaches 1～500 μ m, and deposit thickness reaches 1～100 μ m.
The structure of graphite source electrode 1 of the present invention is characterized in that graphite and the metal case that can produce hollow cathode effect constitute, and graphite and metal case are idiostatic.Graphite is high-purity karbate impervious graphite, and density is 75～99%.
Method of the present invention has overcome that the titanium wood property that is produced when there is hydrogen carbonizing on the titanium surface can descend and defectives such as crackle appear in the surface.Titanium material surface hardness with this art breading can reach 3000HV, and the infiltration layer on surface reaches 1～500 μ m, and deposit thickness reaches 1～100 μ m, and the wear resistance of titanium material is improved.
Description of drawings
Fig. 1 is the processing unit schematic diagram of method of the present invention.
Fig. 2 is the structure iron of the graphite source electrode of processing unit of the present invention
Embodiment
A kind of titanium surface aura non-hydrogen carbonizing method is to utilize the glow discharge that produces between graphite source electrode 1, titanium workpiece 4 and the vacuum chamber 2, the carbon of graphite source electrode 1 is penetrated into surface through the titanium workpiece 4 of well heater 5 and hollow cathode effect heating, formed infiltration layer and the settled layer of TiC on the surface of titanium workpiece 4.The equipment of titanium of the present invention surface aura non-hydrogen carbonizing, vacuum chamber 2 is by vacuum acquiring system 10 extracting vacuum, be provided with in the vacuum chamber 2 can rotation and the work rest 4 of revolution, graphite source electrode 1, with the well heater 5 of unsettled usefulness AC power 6 power supplies of vacuum chamber 2 idiostatic thermofins 3, the current potential of ground connection, at the dc bias power 9 of vacuum chamber 2 peripheral hardware argon gas feed systems 7,4 power supplies of titanium workpiece, direct current source electrode power supply 8 and the temp measuring system that graphite source electrode 1 is powered.The processing parameter of titanium surface aura non-hydrogen carbonizing is at partial pressure of ar gas 1 * 10
3～1 * 10
-1Pa, the temperature of titanium workpiece 4 is at 700～1300 ℃, the voltage 200～1200V of source electrode 1, the voltage 200～1000V of titanium workpiece 4 handled through 0.5～5 hour, and the infiltration layer on titanium workpiece 4 surfaces reaches 1～500 μ m, and deposit thickness reaches 1～100 μ m.The structure of graphite source electrode 1 is characterized in that graphite 12 and the metal case 11 that can produce hollow cathode effect constitute, and graphite 12 is idiostatic with metal case 11.Graphite is high-purity karbate impervious graphite, and density is 75～99%.The principle of titanium surface glow ion non-hydrogen carbonizing technology is: feed the rare gas element argon gas in vacuum vessel, under partial pressure of ar gas reaches certain condition, utilize the glow discharge that produces between graphite source electrode, titanium workpiece and the vacuum chamber, the carbon that is activated on the graphite source electrode is spread the surface that penetrates into through the titanium workpiece 4 of well heater, cathode glow and the heating of hollow cathode effect by thermodiffusion and ion bombardment, form cementation zone on titanium material surface.The structure of titanium surface glow ion non-hydrogen carbonizing equipment is: vacuum chamber 2 is by vacuum acquiring system 10 extracting vacuum, be provided with in the vacuum chamber 2 can rotation and the work rest 4 of revolution, graphite source electrode 1, with the well heater 5 of unsettled usefulness AC power 6 power supplies of vacuum chamber 2 idiostatic thermofins 3, the current potential of ground connection, at the dc bias power 9 of vacuum chamber 2 peripheral hardware argon gas feed systems 7,4 power supplies of titanium workpiece, direct current source electrode power supply 8 and the temp measuring system that graphite source electrode 1 is powered.The structure of graphite source electrode 1 is to be made of graphite 12 and the metal case 11 that can produce hollow cathode effect, and graphite 12 is idiostatic with metal case 11.Graphite is high-purity karbate impervious graphite, and density is 75～99%.
The pure titanium sample of TA2 and graphite source electrode are packed in the vacuum chamber, vacuumize with the vacuum unit, vacuum reaches 5 * 10
-3Charge into high-purity argon gas with mass flowmeter behind the Pa, make partial pressure of ar gas reach 100Pa, add titanium workpiece bias voltage and 200V～700V source voltage simultaneously from 200V～700V, make and produce the hollow cathodic discharge between titanium workpiece and the source electrode, temperature according to titanium workpiece bias voltage and source voltage control workpiece, when the temperature of workpiece is controlled at 950 ℃, make the voltage of source electrode be elevated to 1200V, after titanium workpiece bias voltage is transferred to 700V, after the constant temperature 4 hours, furnace cooling is through check and analysis, carbon penetration mean thickness in the sample is 220 μ m, and surface hardness reaches 2080HV.
TC4 titanium alloy sample and graphite source electrode are packed in the vacuum chamber, vacuumize, vacuum reaches 5 * 10
-3Charge into high-purity argon gas with mass flowmeter behind the Pa, make partial pressure of ar gas reach 20Pa, add titanium workpiece bias voltage and the 200V～700V source voltage of 200V～700V simultaneously, make and produce the hollow cathodic discharge between titanium workpiece and the source electrode, temperature according to titanium workpiece bias voltage and source voltage control workpiece, carry out boosting with auxiliary heater simultaneously, when the temperature of workpiece is controlled at 1150 ℃, make the voltage of source electrode be elevated to 1200V, after titanium workpiece bias voltage is transferred to 800V, after the constant temperature 4 hours, furnace cooling.Through check and analysis, the carbon penetration mean thickness 496 μ m in the sample, surface hardness reaches 3000HV.
Ti
3Al high-temperature titanium alloy sample and graphite source electrode are packed in the vacuum chamber, vacuumize, and vacuum reaches 5 * 10
-3Charge into high-purity argon gas with mass flowmeter behind the Pa, make partial pressure of ar gas reach 50Pa, add titanium workpiece bias voltage and the 200V～700V source voltage of 200V～700V simultaneously, make and produce the hollow cathodic discharge between titanium workpiece and the source electrode, according to the temperature of titanium workpiece bias voltage and source voltage control workpiece, when the temperature of workpiece is controlled at 1300 ℃, make the voltage of source electrode be elevated to 1200V, after titanium workpiece bias voltage is transferred to 1000V, after the constant temperature 3 hours, furnace cooling.Through check and analysis, the carbon penetration mean thickness 145 μ m in the sample, surface hardness reaches 2800HV.
Embodiment 4
The pure titanium sample of TA2 and graphite source electrode are packed in the vacuum chamber, vacuumize, vacuum reaches 5 * 10
-3Charge into high-purity argon gas with mass flowmeter behind the Pa, make partial pressure of ar gas reach 8 * 10
-3Pa, add titanium workpiece bias voltage and the 200V～550V source voltage of 200V～550V simultaneously, make and produce the hollow cathodic discharge between titanium workpiece and the source electrode, temperature according to titanium workpiece bias voltage and source voltage control workpiece, when the temperature of workpiece is controlled at 800 ℃, make the voltage of source electrode be elevated to 1000V, after titanium workpiece bias voltage is transferred to 500V, after the constant temperature time 2 hours, furnace cooling.Through check and analysis, the carbon penetration mean thickness 55 μ m in the sample, surface hardness reaches 640HV.
The pure titanium sample of TA2 and graphite source electrode are packed in the vacuum chamber, vacuumize, vacuum reaches 5 * 10
-3Charge into high-purity argon gas with mass flowmeter behind the Pa, make partial pressure of ar gas reach 35Pa, add titanium workpiece bias voltage and the 200V～500V source voltage of 200V～500V simultaneously, make and produce the hollow cathodic discharge between titanium workpiece and the source electrode, according to the temperature of titanium workpiece bias voltage and source voltage control workpiece, when the temperature of workpiece is controlled at 720 ℃, make the voltage of source electrode be elevated to 900V, after titanium workpiece bias voltage is transferred to 450V, after the constant temperature time 3 hours, furnace cooling.Through check and analysis, the carbon penetration mean thickness 5 μ m in the sample, surface hardness reaches 348HV.
Embodiment 6
TC6 titanium alloy sample and graphite source electrode are packed in the vacuum chamber, vacuumize, vacuum reaches 5 * 10
-3Charge into high-purity argon gas with mass flowmeter behind the Pa, make partial pressure of ar gas reach 50Pa, add titanium workpiece bias voltage and the 200V～700V source voltage of 200V～700V simultaneously, make and produce the hollow cathodic discharge between titanium workpiece and the source electrode, according to the temperature of titanium workpiece bias voltage and source voltage control workpiece, when the temperature of workpiece is controlled at 1020 ℃, make the voltage of source electrode be elevated to 1200V, after titanium workpiece bias voltage is transferred to 850V, after constant temperature was handled 0.5 hour, furnace cooling.Through check and analysis, the carbon penetration mean thickness 95 μ m in the sample, surface hardness reaches 2440HV.
Claims (4)
1. titanium surface glow ion non-hydrogen carbonizing processing method, it is characterized in that utilizing Graphite Electrodes in glow plasma by sputter, make the carbon ion that sputters out or carbon atom under the kinetic energy action of inertia of workpiece bias electric field and particle, arrive heated titanium workpiece surface, under the dual function of thermodiffusion and ion bombardment, make carbon penetrate into the titanium surface and form titanium carbide, the graphite source electrode, the glow discharge that produces between titanium workpiece and the vacuum chamber, the carbon of graphite source electrode is penetrated into surface through the titanium workpiece of well heater and hollow cathode effect heating, formed infiltration layer and the settled layer of TiC on the surface of titanium workpiece.
2. method according to claim 1, the vacuum chamber that it is characterized in that used titanium surface aura non-hydrogen carbonizing equipment is by the vacuum acquiring system extracting vacuum, being provided with in the vacuum chamber can rotation and the work rest of revolution, graphite source electrode, the well heater with ac power supply unsettled with the idiostatic thermofin of vacuum chamber, the current potential of ground connection, at the dc bias power of vacuum chamber peripheral hardware argon gas feed system, the power supply of titanium workpiece, the direct current source electrode power supply and the temp measuring system of graphite source electrode power supply.
3. method according to claim 1 is characterized in that: the processing parameter of titanium surface aura non-hydrogen carbonizing is a partial pressure of ar gas 1 * 10
3～1 * 10
-1Pa, the temperature of titanium workpiece 4 is at 700～1300 ℃, the voltage 200～1200V of source electrode 1, the voltage 200～1000V of titanium workpiece 4 handled through 0.5～5 hour, and the infiltration layer on titanium workpiece 4 surfaces reaches 1～500 μ m, and deposit thickness reaches 1～100 μ m.
4. method according to claim 1, the structure that it is characterized in that the graphite source electrode are that graphite and the metal case that can produce hollow cathode effect constitute, and graphite and metal case are idiostatic, and graphite is high-purity karbate impervious graphite, and density is 75～99%.
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| CN 03119527 CN1451779A (en) | 2002-03-11 | 2003-03-10 | Process for glow ion hydrogen-free carbonizing titanium surface |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100516286C (en) * | 2004-12-24 | 2009-07-22 | 鸿富锦精密工业（深圳）有限公司 | Method for hard coating thin film of generic diamond |
| CN104805325A (en) * | 2015-05-07 | 2015-07-29 | 太原理工大学 | Preparation method of nitriding nano-porous Ti-Ag |
| CN106350764A (en) * | 2016-11-25 | 2017-01-25 | 大连圣洁热处理科技发展有限公司 | Controllable-atmosphere thin-layer carburizing process |
| CN109701948A (en) * | 2019-01-28 | 2019-05-03 | 西安建筑科技大学 | A kind of preparation method of high-wearing feature high-hardness titanium alloy probing bar |
| CN110257756A (en) * | 2019-07-23 | 2019-09-20 | 海南中航特玻科技有限公司 | A kind of preparation method of surface carbonation titanium metal products |
| CN111477899A (en) * | 2020-02-27 | 2020-07-31 | 太原理工大学 | Conductive corrosion-resistant metal bipolar plate for fuel cell and preparation method thereof |
| CN113293350A (en) * | 2021-05-26 | 2021-08-24 | 南京信息工程大学 | Titanium alloy surface modification method |
-
2003
- 2003-03-10 CN CN 03119527 patent/CN1451779A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100516286C (en) * | 2004-12-24 | 2009-07-22 | 鸿富锦精密工业（深圳）有限公司 | Method for hard coating thin film of generic diamond |
| CN104805325A (en) * | 2015-05-07 | 2015-07-29 | 太原理工大学 | Preparation method of nitriding nano-porous Ti-Ag |
| CN106350764A (en) * | 2016-11-25 | 2017-01-25 | 大连圣洁热处理科技发展有限公司 | Controllable-atmosphere thin-layer carburizing process |
| CN106350764B (en) * | 2016-11-25 | 2018-11-20 | 大连圣洁热处理科技发展有限公司 | Controlled atmosphere thin layer carburizing technique |
| CN109701948A (en) * | 2019-01-28 | 2019-05-03 | 西安建筑科技大学 | A kind of preparation method of high-wearing feature high-hardness titanium alloy probing bar |
| CN110257756A (en) * | 2019-07-23 | 2019-09-20 | 海南中航特玻科技有限公司 | A kind of preparation method of surface carbonation titanium metal products |
| CN111477899A (en) * | 2020-02-27 | 2020-07-31 | 太原理工大学 | Conductive corrosion-resistant metal bipolar plate for fuel cell and preparation method thereof |
| CN111477899B (en) * | 2020-02-27 | 2022-12-09 | 太原理工大学 | Conductive corrosion-resistant metal bipolar plate for fuel cell and preparation method thereof |
| CN113293350A (en) * | 2021-05-26 | 2021-08-24 | 南京信息工程大学 | Titanium alloy surface modification method |
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