CN205420524U - Titanium closes surface treatment device of compound nitridation of low pressure vacuum carburization - Google Patents
Titanium closes surface treatment device of compound nitridation of low pressure vacuum carburization Download PDFInfo
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- CN205420524U CN205420524U CN201520930506.2U CN201520930506U CN205420524U CN 205420524 U CN205420524 U CN 205420524U CN 201520930506 U CN201520930506 U CN 201520930506U CN 205420524 U CN205420524 U CN 205420524U
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Abstract
The utility model discloses a titanium closes surface treatment device of compound nitridation of low pressure vacuum carburization comprises high -purity nitrogen gas jar (5), high -purity argon gas jar (6), high -purity acetylene cylinder (7), gaseous buffer tank (2), relief pressure valve (1), vacuum tube heating furnace (3) and vacuum system (8), high -purity nitrogen gas jar (5), high -purity argon gas jar (6), high -purity acetylene cylinder (7) are connected with gaseous buffer tank (2) respectively through the stainless steel pipeline, relief pressure valve (1) is connected to the other end of gaseous buffer tank (2), reconnection flowmeter (4), the compound nitridation retort of flowmeter (4) relinking carbon nitrogen, the compound nitridation retort of carbon nitrogen is equipped with vacuum tube heating furnace (3) and heats the intensification, vacuum treatment is taken out in trailing end connection vacuum system (8) of the compound nitridation retort of carbon nitrogen. The utility model discloses this kind of device combines gas carburizing and gas nitriding, remedies not enough that independent gaseous carbonization brought.
Description
Technical field
This utility model relates to a kind of titanium alloy low-pressure vacuum carburization and is combined the surface processing device of nitriding, belongs to titanium alloy surface technical field of modification.
Background technology
Titanium alloy has the advantages such as high specific strength, good corrosion resistance, high temperature resistant and good biocompatibility, is widely used in the fields such as machinery, the energy, petrochemical industry, Aero-Space and biological engineering.But titanium alloy surface hardness is the highest, wearability and fatigue performance are poor, and easily with shortcomings such as the metal material generation adhesive wears of gas, thus its range is greatly limited.
In all of alloying element, nitrogen affects maximum to the hardness of titanium, the nitride of titanium has the advantages such as the highest hardness, excellent chemical stability, low coefficient of friction, excellent bio-compatibility and good electric conductivity, the nitride modified layer preparing titanium at titanium alloy surface is to improve its case hardness, improve its wearability, extend its service life, expand the effective measures of its range.At present, magnetron sputtering, glow discharge nitriding, laser gas nitriding and gas nitriding process is mainly used to prepare the nitride modified layer of titanium at titanium alloy surface.Magnetron sputtering technique can form certain thickness TiN film layer, improves hardness, improves wearability, but processes through magnetron sputtering method and there is sharp interface, poor bonding strength between film layer and matrix, and coating is thin, and many performance indications are less desirable.Glow discharge nitriding can significantly improve case hardness and the wearability of titanium alloy, but complex-shaped part can not be processed by glow discharge nitriding, and relatively costly.The tissue that laser nitriding is formed is relatively thin, and nitriding layer is tightly combined with matrix, but the quickly heating of high-energy-density laser beam and the chilling action of matrix, make cladding layer produces great thermal stress, easily crack.Meanwhile, under conditions of laser rapid solidification, when the gas in molten bath has little time effusion, easily forming pore, the crackle of laser treatment and pore always hinder the difficult point that this technology is applied, the most less use in actual production.Gas nitriding is simple, with low cost, can form nitride hard phase at titanium alloy surface, significantly improve anti-wear performance and corrosive nature.But the gas nitriding of titanium alloy conventional is along with the increase of nitride film thickness, nitrogen and titanium have the strongest affinity, fine and close nitration case will hinder going deep into of nitrogen, titanium alloy easily aoxidizes simultaneously, fine and close oxide-film also by hinder nitrogen to internal diffusion, the most existing gas nitriding technology also exists that nitriding velocity is slow, infiltration layer is thin, infiltration layer is crisp and processes the shortcomings such as overlong time.So existing titanium alloy surface gas nitriding technology or not ideal enough, it is impossible to meet the needs used.
Titanium alloy, after Carburization Treatment, can obtain uniform carburized layer, it is possible to obtains deeper carburized (case) depth and higher hardness.But carburizing temperature is higher under normal circumstances, part is susceptible to deformation, in atmosphere, active atoms of carbon concentration is higher simultaneously, absorption is at surface of the work, and along with the prolongation of carburizing time, the highest the closer to surface of the work concentration of carbon, carbon deposition phenomenon occurs, not only have impact on carburizing speed, in also resulting in depth of penetration, carbon content distribution is uneven, can only extend carburizing diffusion time or improve carburizing temperature, and its result is often to occur that carbide and martensite level are overproof after workpiece quenching, the carbon profile obtained is undesirable, affects the serviceability of workpiece.Think that the carbon black being deposited on piece surface stops the infiltration of active atoms of carbon, hinder the carrying out of carburizing process, make infiltration layer uneven.The carbon black being attached on retort wall reduces its heat conductivity, reduces service life of equipment etc..
At present, all there is certain defect in nitriding or the process for modifying surface of carburizing that titanium alloy is single, the most preferable to titanium alloy performance improvement, it is impossible to meets the needs used.Respective to nitriding and carburizing advantage is combined, in TiN, add C will form Ti (N, C) compound, when each atom reaches suitable stoichiometric proportion, available extreme hardness, high temperature resistant and wear-resistant all well Ti (C, N) compound, research and development titanium alloy surface carbon nitrogen MULTILAYER COMPOSITE gradient modified layer has far-reaching realistic meaning and vast potential for future development.
Utility model content
The purpose of this utility model is the defect overcoming the simple nitriding of traditional titanium alloy or carburizing to exist, it is provided that a kind of simple and convenient, steady quality, low cost, short-period titanium alloy surface intensifying device.
This utility model is to be realized by techniques below method:
It includes that alternate intermittent is passed through carburizing gas medium and nitriding gas medium, method Carburization Treatment and Nitrizing Treatment combined；It includes that the employing clearance-type cycle repeatedly inflates and bleeds to process and processes the combine carburizing formed or the method for nitriding inflation composite cementation process with carbo-nitriding.
nullConcrete，This utility model is achieved in that and need to titanium alloy sample to be processed or surface of the work be carried out after activation processing putting in sealing retort，In tank, first it is passed through argon to drive and to get rid of air in tank，Then evacuation and retort is warming up to regulation composite cementation temperature 800 DEG C～1200 DEG C，Keep certain time，Atmosphere in purification pot，It is then shut off vacuum pump and is passed through certain pressure and a certain proportion of carburizing or nitriding medium to retort，Carry out carburizing or after nitriding certain time，And then evacuation is diffused processing certain time，Row is passed through certain pressure and a certain proportion of carburizing or nitriding medium again，The gap period formula that inflation composite cementation/evacuation diffusion is so repeated processes，In tank, the pressure of gas medium is cycle reciprocating change，Gap period is 10min～120min，It is 0.005MPa～0.4MPa that carbon nitrogen is combined the pressure oozed altogether，The time oozed altogether is 1h～48h，Carry out after composite cementation processes the stipulated time according to this technique，Keep composite cementation pressure or evacuation diffusion in retort，Until temperature reduces by less than 200 DEG C，Taking-up titanium alloy sample or titanium alloy workpiece carry out detection and the performance test being correlated with，Complete that the carbon nitrogen of titanium alloy is compound oozes process altogether.
The medium of above-mentioned carbon nitrogen composite cementation is high purity acetylene gas or high purity acetylene+high-purity argon gas, high pure nitrogen or high pure nitrogen+high-purity argon gas；Airing form is carried out according to gap period formula method.
The purity of above-mentioned high pure nitrogen, high-purity argon gas and high purity acetylene is more than or equal to 99.9%.
Said method to be realized, this utility model have employed such a kind of device: it is made up of High Purity Nitrogen gas tank, high-purity argon gas tank, high purity acetylene tank, gas buffer tank, air relief valve, electron tubes type heating furnace and vacuum system etc..High Purity Nitrogen gas tank, high-purity argon gas tank, high purity acetylene tank are connected with gas buffer tank respectively by rustless steel pipeline, the other end of gas buffer tank connects air relief valve, reconnect effusion meter, effusion meter reconnects compound carbonitriding nitrogen retort, compound carbonitriding nitrogen retort is carried out heat temperature raising by electron tubes type heating furnace, and the tail end of compound carbonitriding nitrogen retort connects vacuum system and carries out evacuation process.
Said apparatus gas buffer tank and air relief valve, mainly for accurately controlling gas pressure and flow, control the mixing ratio of gas before medium is heated by composite cementation simultaneously.
Said apparatus vacuum system is made up of molecular pump unit and vacuum pump.
Said apparatus is all separately installed with Pressure gauge on the pipeline of the gas outlet of high-purity argon gas cylinder, High Purity Nitrogen gas cylinder and high purity acetylene, and the outlet port at high-purity argon gas cylinder controls valve equipped with argon, at the outlet port of high pure nitrogen and high purity acetylene bottle equipped with gas gas control valve, the discharge duct connecting vacuum pump and reactor is provided with vacuum gauge and gas exhaust inspecting valve.Sealing ring is had at compound carbonitriding retort two ends.Molecular pump unit connects circulating water pipe.
This utility model has following technical effect that
First, it is different from the nitridation of traditional titanium alloy simple gas carbonization gentle body, simple gas carbonization, the carbon impregnation stage cycle is longer, and in atmosphere, active atoms of carbon concentration is higher, and absorption is at surface of the work, and along with the prolongation of carburizing time, the highest the closer to surface of the work concentration of carbon, produce carbon deposition phenomenon, and easily occur that crackle and carburizing are uneven；The gas nitriding of titanium alloy conventional is along with the increase of nitride film thickness, nitrogen and titanium have the strongest affinity, fine and close nitration case will hinder going deep into of nitrogen, titanium alloy easily aoxidizes simultaneously, fine and close oxide-film also by hinder nitrogen to internal diffusion, the most existing gas nitriding technology also exists that nitriding velocity is slow, infiltration layer is thin, infiltration layer is crisp and processes the shortcomings such as overlong time.Gas carburizing and gas nitriding are combined by this utility model, advanced row gas carburizing, and the micro-crack so produced at workpiece or specimen surface or gap can make the activated nitrogen atom in later stage expand further to ooze.Make up the deficiency that independent gas carbonization brings, the nitride for titanium so generated at titanium alloy surface, the carbide of titanium and the carbonitride of titanium, be more beneficial for improving its surface property.
Secondly, this utility model uses the clearance-type cycle repeatedly inflate and bleed, and the method has the advantage that under low pressure, carbon/nitrogen has higher carbon/nitrogen gesture, can produce more active atomic, and cycle batch (-type) repeatedly lead to/is bled.On the one hand, when furnace pressure is in low pressure, the atmosphere in slit and hole is discharged by force, adds live gas during inflation by force, and gas exchange can reach any position communicated with furnace gas.On the other hand, cycle exchange furnace gas, the remained gas thin layer at surface of the work is destroyed rapidly, and new atmosphere produces new active atomic, accelerate the active atomic collision at surface of the work, make infiltration element effectively improve in adsorption rate and the reaction rate of surface of the work.
Again, the medium of this utility model composite cementation is high purity acetylene gas or high purity acetylene+high-purity argon gas, high pure nitrogen or high pure nitrogen+high-purity argon gas.Pure during gas carburizing is to produce a large amount of white carbon blacks and produce hydrogen embrittlement in maximum problem, and traditional gas carburizing is easily to cause hydrogen embrittlement with the gas containing hydrogen such as methane, acetylene for/carbon source.In order to improve titanium alloy surface performance further and avoid hydrogen embrittlement, using acetylene gas to carry out carburizing at titanium alloy surface, acetylene is the gas that in alkanes gas, the few phosphorus content of hydrogen content is high, and is diluted reducing the generation of white carbon black with argon.
Accompanying drawing explanation
Fig. 1 is the structural representation that this utility model uses device；
Fig. 2 is the corrosion polarization curve contrast of titanium alloy sample and former state and simple gas nitriding in the present embodiment 1；
Fig. 3 is acetylene metallographic comparison diagram after the independent nitriding of titanium alloy sample and titanium alloy elder generation nitrogen in embodiment 2；
Fig. 4 is titanium alloy hardness gradient figure at infiltration layer interface after composite cementation in embodiment 3.
Being labeled as in accompanying drawing 1: 1-air relief valve, 2-gas buffer tank, 3-electron tubes type heating furnace, 4-effusion meter, 5-High Purity Nitrogen gas tank, 6-high-purity argon gas tank, 7-high purity acetylene tank, 8-vacuum system.
Detailed description of the invention
With embodiment, this utility model is further described below in conjunction with the accompanying drawings.
As shown in Figure 1, the surface processing device of a kind of titanium alloy compound carbonitriding that this utility model uses is made up of High Purity Nitrogen gas tank 5, high-purity argon gas tank 6, high purity acetylene tank 7, gas buffer tank 2, air relief valve 1, electron tubes type heating furnace 3 and vacuum system 8, and electron tubes type heating furnace 3 is arranged in compound carbonitriding nitrogen retort；High Purity Nitrogen gas tank 5, high-purity argon gas tank 6, high purity acetylene tank 7 are connected with gas buffer tank 2 respectively by rustless steel pipeline, the other end of gas buffer tank 2 connects air relief valve 1, reconnect effusion meter 4, effusion meter 4 reconnects compound carbonitriding nitrogen retort, compound carbonitriding nitrogen retort carries out heat temperature raising by its interior electron tubes type heating furnace 3, and the tail end of compound carbonitriding nitrogen retort connects vacuum system 8 and carries out evacuation process.
Using said apparatus, processing method of the present utility model is to sequentially include the following steps: the titanium alloy sample or titanium alloy workpiece needing to carry out Nitrizing Treatment
nullFirst titanium alloy sample or titanium alloy workpiece removing surface totally and are put into after activation processing in the reactor tank inner chamber of vacuum nitriding device，Then reactor tank is sealed，Evacuation is carried out after air in argon eliminating tank leak detection，Reactor tank is heated simultaneously，It is warming up to the composite cementation temperature 800 DEG C～1200 DEG C of regulation，Then in reactor tank, it is passed through carburizing or nitriding gas medium，After insulation carries out compound nitriding certain time，Then evacuation diffusion certain time，Capable carburizing/the nitriding medium that is passed through carries out compound nitriding again，I.e. use ventilation、Close and keep、Bleed、Close the aerating mode keeping ventilating again and be repeatedly periodically added into carburizing/nitriding gas medium，So that the carburizing/nitriding gas medium in reactor tank inner chamber is clearance-type mechanical periodicity，The clearance-type cycle is 10 minutes～200 minutes，The pressure change simultaneously making the carburizing in reactor tank inner chamber/nitriding gas medium is maintained at the scope of 0MPa～0.050MPa，Its Nitrizing Treatment time controls at 1 hour～48 hours，After nitriding reaches the required time，Reactor tank inner chamber is carried out evacuation process or is filled with above-mentioned carburizing/nitriding pressure medium，After temperature drops to below 200 DEG C, i.e. can be taken off titanium alloy sample or titanium alloy workpiece carries out detecting and performance evaluation，Thus complete compound carbonitridingization and process.
The medium of composite cementation is high purity acetylene gas or high purity acetylene+high-purity argon gas, high pure nitrogen or high pure nitrogen+high-purity argon gas；Airing form is resting period formula.
Carrying out in such as the device of Fig. 1 of above-mentioned titanium alloy compound carbonitriding, this device includes air supply system, heating system and vacuum system composition, air supply system includes that High Purity Nitrogen gas tank, high-purity argon gas tank, high purity acetylene tank, gas buffer tank, decompressor valve form, heating system is made up of retort, electron tubes type heating furnace, vacuum systems is made up of vacuum pump, cooling line, and whole device is connected by rustless steel pipeline and pipe joint.
It is presented herein below and uses several specific embodiments of the present utility model:
Embodiment 1: acetylene+nitrogen:
TC4 titanium alloy sample is oozed front pretreatment (arrangement of sample, clear up and activation etc.), sample through pretreatment is loaded in reactor tank, retort is sealed, hunts leak and after air-discharging by vacuum system 8 evacuation, by the electron tubes type heating furnace 3 in reactor tank, reactor is heated.
Its carbon nitrogen composite cementation concrete operations are: the argon (0.1MPa) that titanium alloy sample enters in stokehold high-purity argon to be used gas tank 6 carries out twice aerofluxus to it, aerofluxus for the first time is used for the gas hunted leak and discharge in vacuum response tank, aerofluxus for the second time is used for ensureing that the air gas in pyroreaction still has been drained off totally, preventing workpiece from aoxidizing.After aerofluxus start evacuation and furnace temperature is raised to 900 DEG C insulation 1h be de-gassed and purify, the valve being then shut off vacuum pump stops evacuation and opens charging valve and be filled with high purity acetylene gas (0.01MPa) from high purity acetylene tank 7, insulation 30min followed by evacuation insulation 30min, after being filled with high pure nitrogen (0.01MPa) insulation 30min by High Purity Nitrogen gas tank 5 again, row evacuation is incubated 30min again, intermittent cycle is so repeated take out/inflate compound carbonitriding nitrogen and process after 8h, continuing to keep the high pure nitrogen pressure medium in reactor tank is 0.01MPa, and the titanium alloy sample that takes out rear below the greenhouse cooling in reactor tank to 200 DEG C is carried out coherent detection, complete whole compound carbonitriding operation.
Fig. 2 is the sample after the present embodiment 1 compound carbonitriding processes and the Tafel polarization curve that measures in Fluohydric acid. and nitric acid mixed system of former state.As seen from the figure, titanium alloy is through compound carbonitriding nitrogen process post-etching electromotive force apparently higher than titanium alloy former state, and corrosion current reduces 3 orders of magnitude, and after the present embodiment compound carbonitriding processes, its corrosive nature is obviously improved.
Embodiment 2: nitrogen+(acetylene+argon):
TC4 titanium alloy sample is oozed front pretreatment (arrangement of sample, cleaning and activation processing etc.), sample through pretreatment is loaded in reactor tank, and pass through vacuum system 8 evacuation after reactor tank sealing, leak detection, aerofluxus, by the electron tubes type heating furnace 3 in reactor tank, retort is heated.
Its carbon nitrogen composite cementation concrete operations are: the argon (0.1MPa) that vacuum response still enters in stokehold high-purity argon gas tank 6 carries out twice aerofluxus to it, aerofluxus for the first time is used for hunting leak and discharging air in retort, air gas emptying in the pyroreaction tank of aerofluxus principal security for the second time, prevents workpiece from aoxidizing.After aerofluxus start evacuation and furnace temperature is raised to 900 DEG C insulation 1h be de-gassed and purify, it is then shut off the valve of vacuum pump stop evacuation and open charging valve and be filled with high pure nitrogen gas (0.01MPa) by High Purity Nitrogen gas tank 5, insulation 30min followed by evacuation insulation 30min, after high purity acetylene (0.01MPa) insulation 30min inflated by high purity acetylene tank 7, row evacuation is incubated 30min more again, intermittent cycle is so repeated take out/inflate compound carbonitriding nitrogen and process after 8h, continuing to keep the high purity acetylene pressure medium in reactor tank is 0.01MPa, and the titanium alloy sample that takes out rear below the greenhouse cooling in reactor tank to 200 DEG C is carried out coherent detection, complete whole compound carbonitriding operation.
Fig. 3 is metallographic microstructure and the test impression of hardened layer hardness gradient of sample after the present embodiment 2 compound carbonitriding processes.As seen from the figure, the carbon nitrogen defining certain depth through the present embodiment compound carbonitriding process rear surface is combined co-penetration layer, and hardness is significantly improved, and case hardness reaches more than HV1000, and case depth is more than 100 μm.
Embodiment 3:(acetylene+argon)+(nitrogen+argon):
TC4 titanium alloy sample is oozed front pretreatment (arrangement of sample, clear up and activation etc.), sample through pretreatment is loaded in reactor tank, retort is sealed, hunts leak and after aerofluxus by vacuum system 8 evacuation, by the electron tubes type heating furnace 3 in reactor tank, retort is heated.
Its carbon nitrogen composite cementation concrete operations are: the argon (0.1MPa) that titanium alloy sample enters in stokehold high-purity argon to be used gas tank 6 carries out twice aerofluxus to it, aerofluxus for the first time is used for the gas hunted leak and discharge in vacuum response tank, aerofluxus for the second time is used for ensureing that the air gas in pyroreaction still has been drained off totally, preventing workpiece from aoxidizing.Start evacuation after aerofluxus and furnace temperature is raised to 900 DEG C of insulation 1h is de-gassed and purifies, being then shut off the valve of vacuum pump and stop evacuation and open charging valve and be filled with high purity acetylene gas and high-purity argon (in molar ratio for the high purity acetylene+high-purity argon gas of 1:1；Pressure is 0.01MPa), insulation 30min followed by evacuation insulation 30min, reinflated high pure nitrogen and high-purity argon gas (are the high pure nitrogen+high-purity argon gas of 1:1 in molar ratio；Pressure is 0.01MPa) insulation 30min after again row evacuation insulation 30min, intermittent cycle is so repeated take out/inflate compound carbonitriding nitrogen and process after 8h, continue to keep the high pure nitrogen in reactor tank and high-purity argon gas medium (being the high pure nitrogen+high-purity argon gas of 1:1 in molar ratio), pressure is 0.01MPa, take out titanium alloy sample after greenhouse cooling to less than 200 DEG C and carry out coherent detection, complete whole compound carbonitriding operation.
Fig. 4 is sample and the wear-resisting curve of former state after the present embodiment 3 compound carbonitriding processes, and as seen from the figure, after the present embodiment compound carbonitriding processes, coefficient of friction is significantly less than the coefficient of friction of former state, and wearability is greatly improved.
Certainly, being more than concrete exemplary applications of the present utility model, this utility model also has the technical scheme that other embodiment, all employing equivalents or equivalent transformation are formed, within all falling within the protection domain required by this utility model.
Claims (1)
1. a titanium closes low-pressure vacuum carburization and is combined the surface processing device of nitriding, it is characterised in that: it is made up of High Purity Nitrogen gas tank (5), high-purity argon gas tank (6), high purity acetylene tank (7), gas buffer tank (2), air relief valve (1), electron tubes type heating furnace (3) and vacuum system (8)；High Purity Nitrogen gas tank (5), high-purity argon gas tank (6), high purity acetylene tank (7) are connected with gas buffer tank (2) respectively by rustless steel pipeline, the other end of gas buffer tank (2) connects air relief valve (1), reconnect effusion meter (4), effusion meter (4) reconnects compound carbonitriding nitrogen retort, compound carbonitriding nitrogen retort is provided with electron tubes type heating furnace (3) and carries out heat temperature raising, and the tail end of compound carbonitriding nitrogen retort connects vacuum system (8) and carries out evacuation process.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106904986A (en) * | 2017-02-23 | 2017-06-30 | 辽宁奥亿达新材料有限公司 | A kind of manufacture method of high-performance composite carbon fiber insulation board |
| CN114622155A (en) * | 2021-11-01 | 2022-06-14 | 杭州永磁集团有限公司 | Vacuum nitriding method of samarium iron nitrogen powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106904986A (en) * | 2017-02-23 | 2017-06-30 | 辽宁奥亿达新材料有限公司 | A kind of manufacture method of high-performance composite carbon fiber insulation board |
| CN114622155A (en) * | 2021-11-01 | 2022-06-14 | 杭州永磁集团有限公司 | Vacuum nitriding method of samarium iron nitrogen powder |
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