CN203602702U - Low-voltage-impulse vacuum nitriding device for titanium alloy - Google Patents
Low-voltage-impulse vacuum nitriding device for titanium alloy Download PDFInfo
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- CN203602702U CN203602702U CN201320590739.3U CN201320590739U CN203602702U CN 203602702 U CN203602702 U CN 203602702U CN 201320590739 U CN201320590739 U CN 201320590739U CN 203602702 U CN203602702 U CN 203602702U
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Abstract
The utility model discloses a low-voltage-impulse vacuum nitriding device. The low-voltage-impulse vacuum nitriding device comprises a heating furnace and an intelligent program temperature control instrument for controlling the temperature of the heating furnace, wherein a reactor is arranged in a hearth of the heating furnace and is respectively connected with a high-purity argon bottle and a high-purity nitrogen bottle by stainless-steel gas pipelines; the reactor is connected with a vacuum pump by an exhausting pipeline; a thermocouple is arranged on the heating furnace and is connected with the intelligent program temperature control instrument by a signal transmission line; pipelines of gas outlets of the high-purity argon bottle and the high-purity nitrogen bottle are respectively provided with a voltage meter; the gas outlet end of the high-purity argon bottle is provided with an argon control valve, and the gas outlet end of the high-purity nitrogen bottle is provided with a nitrogen control valve; and the exhausting pipeline for connecting the vacuum pump and the reactor is provided with a vacuum gauge and an exhausting control valve. The low-voltage-impulse vacuum nitriding device disclosed by the utility model not only has the advantages of simplicity in operation and suitability for batch production, but also has the advantages of high processing efficiency, good product quality and stable product quality and the like.
Description
Technical field
The utility model relates to a kind of titanium alloy action of low-voltage pulse vacuum nitriding device, belongs to titanium alloy nitridation technique field.
Background technology
Because titanium alloy has that specific tenacity is high, high temperature resistant, good corrosion resistance and there is the good advantage such as low-temperature flexibility and biocompatibility, thereby be widely used in the fields such as national defence, chemical industry, the energy, aerospace and biotechnology.But because titanium alloy surface hardness is not high, the shortcoming such as therefore there is wearability and resistance to fatigue is poor, easy and many material generation adhesive wears.
Process for modifying surface is the effective way that improves titanium alloy hardness, wear resistance and resistance to fatigue, from research both domestic and external, the process for modifying surface of titanium alloy has roughly experienced from strengthening as the tradition of representative take plating, electroless plating, thermodiffusion, plated film, arrives the development course of the modern surface strengthening technologies such as plasma body, ionic fluid, electron beam, laser.The coating that plating forms and the bonding strength of matrix are low, easily cause craze of coating, peel off.Vapour deposition CVD method generally will be carried out at higher temperature (1000～1100 ℃), easily causes the crystallization of matrix, the variation such as grow up again, and reduce the intensity of workpiece and affect workpiece geomery, and with high costs.The Ci that PVD ﹙ extensively adopts is at present controlled Jian She ﹚ method owing to there being obvious interface between rete and matrix, poor bonding strength, and coating is thin.After plasma spraying, coatingsurface is more coarse because spraying rate is high, spray wayward, more difficult to spraying complex part, easily produce intensive ultraviolet and pollute, simultaneously cost is also higher.The surface that titanium alloy surface laser reinforcing obtains is equally very coarse, and smooth finish is poor, and hardened layer is thin and inhomogeneous, and between coating and matrix, be easy to cause and melt cracking coating inside and also there will be pore and crackle melting, and apparatus expensive.Ionitriding surface hardness is good, and hardness is even, but cost is higher, and efficiency is low, has limited the application of this technology in actual production.
Gas nitriding is simple, with low cost, can form nitride hard phase at titanium alloy surface, significantly improves wear resisting property and corrosive nature.But the gas nitriding of titanium alloy conventional is along with the increase of nitrided film thickness, nitrogen and titanium have very strong avidity, fine and close nitride layer will hinder going deep into of nitrogen, titanium alloy is very easily oxidized simultaneously, fine and close oxide film also by hinder nitrogen to internal diffusion, therefore existing gas nitriding technology exists that nitriding velocity is slow, infiltration layer is thin, infiltration layer is crisp and the shortcoming such as the treatment time is long.So existing titanium alloy surface gas nitriding technology or not ideal enough, can not meet the needs of use.
Summary of the invention
The purpose of this utility model is: a kind of simple to operate, steady quality is provided, is suitable for the titanium alloy action of low-voltage pulse vacuum nitriding device of batch production, to overcome the deficiencies in the prior art.
The utility model is to form like this: a kind of action of low-voltage pulse vacuum nitriding device of the present utility model is, this device comprises process furnace and controls the intelligent program temperature controller of furnace temp, in the burner hearth of process furnace, be provided with reactor, reactor is connected with high-purity argon gas cylinder and High Purity Nitrogen gas cylinder respectively by stainless steel gas pipeline, on reactor, be connected with vacuum pump by gas exhaust duct, thermopair for testing temperature in process furnace burner hearth is installed on process furnace, and thermopair is connected with intelligent program temperature controller by signal transmission line, on the pipeline of the air outlet of high-purity argon gas cylinder and High Purity Nitrogen gas cylinder, be all separately installed with tensimeter, and end is equipped with argon gas by-pass valve control in the air outlet of high-purity argon gas cylinder, in the air outlet of High Purity Nitrogen gas cylinder, end is equipped with nitrogen by-pass valve control, on the gas exhaust duct that connects vacuum pump and reactor, vacuum gauge and gas exhausting valve door are installed.
Above-mentioned reactor is made up of reactor tank, reactor cap and ring flange, the tank body of reactor tank is arranged in the burner hearth of process furnace, ring flange is fixed on the port of reactor tank, reactor cap is connected on ring flange and by the port closed of reactor tank by joint bolt, and stainless steel gas pipeline and gas exhaust duct are connected on reactor cap and with the inner chamber of reactor tank and are communicated with.
Between above-mentioned reactor cap and ring flange, be also lined with sealing-ring.
On above-mentioned ring flange, be provided with the circulating water pipe that can be connected with cooling water source.
Above-mentioned thermopair is arranged in process furnace burner hearth and the position of stacking titanium alloy sample or titanium alloy workpiece near reactor tank.
Above-mentioned argon gas by-pass valve control, nitrogen by-pass valve control or gas exhausting valve door is manual control valve or is electric control valve.
Owing to having adopted technique scheme, adopt the utility model, can on the surface of titanium alloy workpiece, form one deck densification, high rigidity, corrosion-resistant and anti abrasive nitride layer, prove through test and practical probation, the utlity model has following advantage and disadvantage:
1, vacuum nitriding technology is that while utilizing heating under vacuum, the feature such as clean, the non-oxidation of workpiece surface is carried out nitriding, can prevent the tissue defects such as interior oxidation, hydrogen embrittlement, loose and black.When vacuum nitriding, on the one hand, other gases and the bur of workpiece surface absorption will be discharged out of the furnace by desorption, reduce the obstacle in impurity and hole, workpiece surface is cleaned, active increasing, promotes the absorption of activated nitrogen atom in nitriding process, thereby improves adsorptive power and the velocity of diffusion of nitrogen-atoms at workpiece surface; On the other hand, can reduce the objectionable impurities in atmosphere, effectively stop other gases to form adsorption layer at workpiece surface, purify furnace atmosphere.
2, under low pressure, nitriding has higher nitrogen gesture, can produce more activated nitrogen atom, the nitrogen gesture of low pressure nitriding improves approximately 40% than ordinary gas nitridation, and furnace pressure is in the time of low pressure, furnace atmosphere is even, can solve band slit, aperture (micropore), deep hole, the inhomogeneous difficult problem of blind hole workpiece infiltration layer.Pulse nitridation technique be with the cycle repeatedly intermittent type logical/air suction mode carries out nitriding.On the one hand, furnace pressure is in the time of low pressure, and the atmosphere in slit and hole is discharged by force, adds by force again live gas when inflation, and gaseous interchange can reach any position communicating with furnace gas.On the other hand, recurrence interval exchange furnace gas, is destroyed rapidly at the retained gas thin layer of workpiece surface, and new atmosphere produces new active atomic, accelerate the collision of active atomic at workpiece surface, made to infiltrate element and effectively improve in rate of adsorption and the speed of reaction of workpiece surface.
So compared with prior art, that the utility model not only has advantages of the utility model is simple to operate, be suitable for batch production, but also have that working (machining) efficiency is high, the advantage such as good product quality and constant product quality.
Accompanying drawing explanation
Fig. 1 is the structural representation of the utility model device;
Fig. 2 is structural representation when reactor is arranged on process furnace in Fig. 1;
Fig. 3 is the surperficial XRD figure spectrum contrast of titanium alloy sample and no pulse vacuum nitriding sample in embodiment 1;
Fig. 4 is titanium alloy nitride layer interface SEM pattern picture in embodiment 2;
Fig. 5 is titanium alloy and relatively SEM pattern picture (wherein Fig. 5 (a) is undressed titanium alloy polishing scratch, and Fig. 5 (b) is through embodiment 3 titanium alloy polishing scratch after treatment) of undressed titanium alloy polishing scratch in embodiment 3.
Description of reference numerals: 1, high-purity argon gas cylinder; 2, High Purity Nitrogen gas cylinder; 3, stainless steel gas pipeline; 4, argon gas by-pass valve control; 5, tensimeter; 6, nitrogen by-pass valve control; 7, intelligent program temperature controller; 8, thermopair; 9, process furnace; 10, reactor; 11, vacuum gauge; 12, gas exhausting valve door; 13, vacuum pump; 14, gas exhaust duct; 15, titanium alloy sample or titanium alloy workpiece.10-1, reactor tank; 10-2, reactor cap; 10-3, joint bolt; 10-4, circulating water pipe; 10-5, sealing-ring; 10-6, ring flange.
Embodiment
Below in conjunction with drawings and Examples, the utility model is further described.
In the time that the titanium alloy sample to conventional or titanium alloy workpiece carry out nitriding and process, can adopt the utility model to process it, the utility model is constructed according to a kind of following titanium alloy action of low-voltage pulse vacuum nitriding method, the method is that titanium alloy sample or the titanium alloy workpiece to carrying out nitriding processing carries out according to the following steps: first will after titanium alloy sample or titanium alloy workpiece removing surface totally, put into the reactor tank inner chamber of action of low-voltage pulse vacuum nitriding device, then reactor tank is sealed, after leak detection, vacuumize, reactor tank is heated simultaneously, make the temperature of its inner chamber remain on 700 ℃～1000 ℃, then in reactor tank inner chamber, adopt the mode of pulse aerating to add nitriding gas medium, adopt ventilation, close maintenance, bleed, close the aerating mode that maintenance ventilates again and repeatedly periodically add nitriding gas medium, thereby the rectangular pulse mode of nitriding gas pressure medium in reactor tank inner chamber is changed, the periodic regime of this square topped pulse is 10 minutes～200 minutes, make the pressure change of the nitriding gas medium in reactor tank inner chamber remain on the scope of 0MPa～0.050MPa simultaneously, its nitriding treatment time is controlled at 2 hours～and 72 hours, until reach required time by the mode of this action of low-voltage pulse vacuum nitriding processing after, can be keeping the nitriding gas pressure medium in reactor tank inner chamber or again reactor tank inner chamber vacuumized on the basis of processing, after below the temperature of reactor tank inner chamber is dropped to 300 ℃, can take out titanium alloy sample or titanium alloy workpiece, thereby complete nitriding treatment.Nitriding gas medium used can adopt the mixed gas of high pure nitrogen of the prior art or high pure nitrogen+high-purity argon gas, in this gas mixture by molar weight proportioning, the shared molar weight proportioning of each gas is, high pure nitrogen: high-purity argon gas=1:1～5:1, high pure nitrogen used or the purity of high-purity argon gas are more than or equal to 99.9%.
The structural representation of the of the present utility model a kind of action of low-voltage pulse vacuum nitriding device building according to aforesaid method as depicted in figs. 1 and 2, this device comprises process furnace 9 and controls the intelligent program temperature controller 7 of furnace temp, its process furnace 9 can adopt middle temperature cabinet-type electric furnace of the prior art or tube type resistance furnace, its intelligent program temperature controller 7 can directly adopt finished product of the prior art, by traditional temperature automatically controlled mode of connection, intelligent program temperature controller 7 is connected with process furnace 9 and thermopair 8 by wire simultaneously, in the burner hearth of process furnace 9, establish the device 10 that directly responds, reactor 10 is connected with high-purity argon gas cylinder 1 and High Purity Nitrogen gas cylinder 2 respectively by stainless steel gas pipeline 3, on reactor 10, connect a vacuum pump 13 by gas exhaust duct 14, thermopair 8 for testing temperature in process furnace 9 burner hearths is installed on process furnace 9, and thermopair 8 is connected with intelligent program temperature controller 7 by signal transmission line, on the pipeline of the air outlet of high-purity argon gas cylinder 1 and High Purity Nitrogen gas cylinder 2, be all separately installed with tensimeter 5, and end is equipped with argon gas by-pass valve control 4 in the air outlet of high-purity argon gas cylinder 1, in the air outlet of High Purity Nitrogen gas cylinder 2, end is equipped with nitrogen by-pass valve control 6, on the gas exhaust duct 14 that connects vacuum pump 13 and reactor 10, vacuum gauge 11 and gas exhausting valve door 12 are installed, its reactor 10 is made up of reactor tank 10-1, reactor cap 10-2 and ring flange 10-6, the tank body of reactor tank 10-1 is arranged in the burner hearth of process furnace 9, ring flange 10-6 is fixed on the port of reactor tank 10-1, reactor cap 10-2 is connected to ring flange 10-6 by joint bolt 10-3 and above and by the port closed of reactor tank 10-1 lives, and stainless steel gas pipeline 3 and gas exhaust duct 14 are connected to reactor cap 10-2 above and are communicated with the inner chamber of reactor tank 10-1, in order to reach better sealing effectiveness, can between reactor cap 10-2 and ring flange 10-6, pad a resistant to elevated temperatures sealing-ring 10-5, for the ease of control that reactor tank 10-1 is lowered the temperature, the circulating water pipe 10-4 that an energy is connected with cooling water source can be installed on ring flange 10-6, in the time that thermopair 8 is installed, be preferably arranged in process furnace 9 burner hearths and the position of stacking titanium alloy sample or titanium alloy workpiece 15 near reactor tank 10-1, its argon gas by-pass valve control 4 used, nitrogen by-pass valve control 6 or gas exhausting valve door 12 can directly adopt manual control valve of the prior art or are electric control valve according to the needs that use, in the time adopting electric control valve, can adopt micro-chip of the prior art or PLC(programcontrol unit), and after micro-chip or PLC being connected with electric control valve and intelligent program temperature controller 7 by traditional automatic control linkage mode, can realize full automatic control nitriding processing.
To adopt several specific embodiments of the present utility model below:
Embodiment 1: TC4 titanium alloy sample is oozed to the front pre-treatment (arrangement of sample, cleaning etc.), to pack in the reactor tank of reactor through pretreated sample or workpiece, and will after reactor tank sealing, leak detection, vacuumize, by process furnace, reactor is heated, its vacuum nitriding processing parameter is: the high-purity N that 800 ℃ of temperature, nitriding medium are 99.999%
2, the nitriding medium pressure in reactor tank is changed between 0 MPa～0.015MPa, first fill high-purity N by device of the present utility model
2after gas 30min, close the at this moment high-purity N in reactor tank of nitrogen by-pass valve control 15 min(
2pressure remains on 0.015MPa), then open rapidly gas exhausting valve door and vacuumize at this moment nitrogen by-pass valve control maintenance of 30min(closing condition), then close after gas exhausting valve door 5 min, then open rapidly nitrogen by-pass valve control and fill high-purity N in reactor tank
230min(at this moment gas exhausting valve door keeps closing condition); After iterative cycles like this 8 times, the treatment stage of can completing action of low-voltage pulse vacuum nitriding, at this moment continuing to keep the nitriding medium pressure in reactor tank is 0.015MPa, and by ℃ following rear titanium alloy sample that takes out of the greenhouse cooling to 300 in reactor tank, can complete so whole nitriding treatment operation.Fig. 3 is the surperficial XRD figure spectrum contrast of titanium alloy sample and no pulse vacuum nitriding sample in the present embodiment.
Embodiment 2: TC4 titanium alloy sample is oozed to the front pre-treatment (arrangement of sample, cleaning etc.), to pack in the reactor tank of reactor through pretreated sample or workpiece, and will after reactor tank sealing, leak detection, vacuumize, by process furnace, reactor is heated, its vacuum nitriding processing parameter is: 850 ℃ of temperature, nitriding medium are to be the high-purity N of 1:1 in molar ratio
2+ high-purity Ar, nitriding medium pressure in reactor tank is changed between 0 MPa～0.015MPa, by device of the present utility model first fill close after nitriding medium 30min simultaneously nitrogen by-pass valve control and argon gas by-pass valve control 15 min(at this moment the nitriding medium pressure in reactor tank remain on 0.015MPa), then open rapidly gas exhausting valve door and vacuumize at this moment nitrogen by-pass valve control and argon gas by-pass valve control maintenance closing condition of 30min(), then close after gas exhausting valve door 5 min, open rapidly again nitrogen by-pass valve control and argon gas by-pass valve control and fill at this moment gas exhausting valve door maintenance of nitriding medium 30min(closing condition in reactor tank), after iterative cycles like this 6 times, the treatment stage of can completing action of low-voltage pulse vacuum nitriding, at this moment continuing to keep the nitriding medium pressure in reactor tank is 0.015MPa, and by ℃ following rear titanium alloy sample that takes out of the greenhouse cooling to 300 in reactor tank, can complete so whole nitriding treatment operation.This sample is observed after 10% HF corrosive fluid corrosion to the microscopic appearance of its diffusion layer organization, as shown in the SEM picture of Fig. 4.
Embodiment 3: TC4 titanium alloy sample is oozed to the front pre-treatment (arrangement of sample or workpiece, cleaning etc.), to pack in the reactor tank of reactor through pretreated sample or workpiece, and will after reactor tank sealing, leak detection, vacuumize, by process furnace, reactor is heated, its vacuum nitriding processing parameter is: 800 ℃ of temperature, nitriding medium are 99.999% high-purity N
2, the nitriding medium pressure in reactor tank is changed between 0 MPa～0.020MPa, first fill and close the at this moment high-purity N in reactor tank of nitrogen by-pass valve control 15 min(after nitriding medium 30min by device of the present utility model
2pressure remains on 0.020MPa), then open rapidly gas exhausting valve door and vacuumize at this moment nitrogen by-pass valve control maintenance of 30min(closing condition), then close after gas exhausting valve door 5 min, then open rapidly nitrogen by-pass valve control and fill at this moment gas exhausting valve door maintenance of nitriding medium 30min(closing condition in reactor tank); After iterative cycles like this 8 times, the treatment stage of can completing action of low-voltage pulse vacuum nitriding, at this moment continuing to keep the nitriding medium pressure in reactor tank is 0.020MPa, and by ℃ following rear titanium alloy sample that takes out of the greenhouse cooling to 300 in reactor tank, can complete so whole nitriding treatment operation.The body material of the titanium alloy sample of on dish pin formula friction wear testing machine, employing the utility model embodiment 3 being processed and untreated titanium alloy sample carries out the end face sliding friction test of 30min, by scanning electron microscopic observation surface of friction microscopic appearance, picture as shown in Figure 5, wherein Fig. 5 (a) is undressed titanium alloy polishing scratch, and Fig. 5 (b) is through the present embodiment 3 titanium alloy polishing scratch after treatment.
Collection of illustrative plates or picture from above-described embodiment are known, after by the utility model, titanium alloy sample or titanium alloy workpiece being processed, can on the surface of its titanium alloy workpiece, form one deck densification, high rigidity, corrosion-resistant and anti abrasive nitride layer.Therefore, the surface quality of the workpiece by the utility model processing is better than the workpiece surface quality that adopts existing mode processing greatly.
Claims (6)
1. an action of low-voltage pulse vacuum nitriding device, comprise the intelligent program temperature controller (7) of process furnace (9) and control furnace temp, it is characterized in that: in the burner hearth of process furnace (9), be provided with reactor (10), reactor (10) is connected with high-purity argon gas cylinder (1) and High Purity Nitrogen gas cylinder (2) respectively by stainless steel gas pipeline (3), above be connected with vacuum pump (13) by gas exhaust duct (14) at reactor (10), thermopair (8) for testing temperature in process furnace (9) burner hearth is installed on process furnace (9), and thermopair (8) is connected with intelligent program temperature controller (7) by signal transmission line, on the pipeline of the air outlet of high-purity argon gas cylinder (1) and High Purity Nitrogen gas cylinder (2), be all separately installed with tensimeter (5), and at the air outlet end of high-purity argon gas cylinder (1), argon gas by-pass valve control (4) is housed, at the air outlet end of High Purity Nitrogen gas cylinder (2), nitrogen by-pass valve control (6) is housed, on the gas exhaust duct (14) that connects vacuum pump (13) and reactor (10), vacuum gauge (11) and gas exhausting valve door (12) are installed.
2. action of low-voltage pulse vacuum nitriding device according to claim 1, it is characterized in that: reactor (10) is by reactor tank (10-1), reactor cap (10-2) and ring flange (10-6) composition, the tank body of reactor tank (10-1) is arranged in the burner hearth of process furnace (9), ring flange (10-6) is fixed on the port of reactor tank (10-1), reactor cap (10-2) is connected to ring flange (10-6) by joint bolt (10-3) and above and by the port closed of reactor tank (10-1) lives, stainless steel gas pipeline (3) and gas exhaust duct (14) are connected to reactor cap (10-2) above and are communicated with the inner chamber of reactor tank (10-1).
3. action of low-voltage pulse vacuum nitriding device according to claim 2, is characterized in that: between reactor cap (10-2) and ring flange (10-6), be also lined with sealing-ring (10-5).
4. action of low-voltage pulse vacuum nitriding device according to claim 2, is characterized in that: on ring flange (10-6), be provided with the circulating water pipe (10-4) that can be connected with cooling water source.
5. action of low-voltage pulse vacuum nitriding device according to claim 2, is characterized in that: thermopair (8) is arranged in process furnace (9) burner hearth and the position of stacking titanium alloy sample or titanium alloy workpiece (15) near reactor tank (10-1).
6. action of low-voltage pulse vacuum nitriding device according to claim 1, is characterized in that: described argon gas by-pass valve control (4), nitrogen by-pass valve control (6) or gas exhausting valve door (12) is manual control valve or is electric control valve.
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| CN201320590739.3U CN203602702U (en) | 2013-09-24 | 2013-09-24 | Low-voltage-impulse vacuum nitriding device for titanium alloy |
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| CN201320590739.3U CN203602702U (en) | 2013-09-24 | 2013-09-24 | Low-voltage-impulse vacuum nitriding device for titanium alloy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103469147A (en) * | 2013-09-24 | 2013-12-25 | 贵州师范大学 | Low-pressure pulse vacuum nitriding method and low-pressure pulse vacuum nitriding device for titanium alloy |
| CN110747430A (en) * | 2019-10-25 | 2020-02-04 | 西南交通大学 | Low-pressure gas rapid nitriding method |
-
2013
- 2013-09-24 CN CN201320590739.3U patent/CN203602702U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103469147A (en) * | 2013-09-24 | 2013-12-25 | 贵州师范大学 | Low-pressure pulse vacuum nitriding method and low-pressure pulse vacuum nitriding device for titanium alloy |
| CN103469147B (en) * | 2013-09-24 | 2015-10-28 | 贵州师范大学 | A kind of titanium alloy action of low-voltage pulse vacuum nitriding method and device |
| CN110747430A (en) * | 2019-10-25 | 2020-02-04 | 西南交通大学 | Low-pressure gas rapid nitriding method |
| CN110747430B (en) * | 2019-10-25 | 2020-12-15 | 西南交通大学 | Low-pressure gas rapid nitriding method |
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