CN103572220B - A kind of preparation method of TiAlN niobium nitrogen gradient hard reaction film - Google Patents
A kind of preparation method of TiAlN niobium nitrogen gradient hard reaction film Download PDFInfo
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- CN103572220B CN103572220B CN201310515573.3A CN201310515573A CN103572220B CN 103572220 B CN103572220 B CN 103572220B CN 201310515573 A CN201310515573 A CN 201310515573A CN 103572220 B CN103572220 B CN 103572220B
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Abstract
A preparation method for TiAlN niobium nitrogen gradient hard reaction film, its preparation method comprises successively: 1, the determination of deposition technique and target material composition; 2, the selection of workpiece and pre-treatment; 3, the determination of pre-bombardment technique; 4, the determination of depositing operation; 5, vacuum heating treatment; 6, workpiece rotates.Present invention reduces coating cost, realize while ensure that rete high adhesive force, high rigidity and highly heatproof and shockproof, reduce rete internal stress, and there is satisfactory stability and repeatability.
Description
Technical field
The present invention relates to a kind of preparation method of nitrogen gradient hard reaction film, combination target is particularly adopted to prepare the method for multi-arc ion coating nitrogen gradient hard reaction film, such as the preparation method of TiAlN niobium nitrogen gradient hard reaction film (following use " TiAlNbN " replaces " TiAlN niobium ").
Background technology
Multi-arc ion coating is a kind of physical vacuum deposition technique being provided with multiple cathodic arc evaporation source that can simultaneously evaporate, and has the distinguishing features such as sedimentation velocity is fast, morphology is fine and close, strong adhesion, good uniformity.This technology is applicable to the preparation of hard films and hard reaction gradient film, and at titanium nitride, and the preparation aspect of TiAlN and more polynary hard reaction film succeeds application.TiAlN, the titanium based hard reaction films such as titanium niobium nitride have more development prospect due to respective characteristics such as hardness are high, frictional coefficient is little, thermotolerance is strong than titanium nitride film.
For individual layer with titanium be base multicomponent hard reaction film for, mainly there is following shortcoming: 1, the general easy contradiction occurred between film hardness and film adhesion, namely hardness and sticking power are difficult to meet simultaneously; 2, multicomponent alloy target market is not easily bought, usually need special melting, processing, not only cost is higher, and the cycle is longer; 3, easily in rete, produce larger internal stress, affect the thermal shock performance of hard films, and then affect result of use and work-ing life.
Summary of the invention
The object of this invention is to provide a kind of preparation method of TiAlN niobium (TiAlNbN) nitrogen gradient hard reaction film, this method reduce coating cost, realize while ensure that rete high adhesive force, high rigidity and highly heatproof and shockproof, reduce rete internal stress, and there is satisfactory stability and repeatability.
Technical scheme of the present invention is: a kind of preparation method of TiAlN niobium (TiAlNbN) nitrogen gradient hard reaction film comprises successively:
1, the determination of deposition technique and target material composition: determine the technology of preparing of multi-arc ion coating as TiAlNbN nitrogen gradient hard reaction film, select two different azimuth and become the arc source starting the arc simultaneously of 90 degree of configurations to deposit, one of them arc source is the commercial titanium-niobium alloy target of purity 99.9%, and the atomic ratio of titanium-niobium alloy target is Ti:Nb=75:25; Another arc source is the commercial titanium-aluminum alloy target of purity 99.9%, and the atomic ratio of titanium-aluminum alloy target is Ti:Al=50:50.
2, the selection of workpiece and pre-treatment: select commercial rapid steel as workpiece material, before putting into coating chamber and carrying out plated film, use to workpiece, metal detergent carries out that routine is deoiled, decontamination process carry out surface finish process, finally carry out ultrasonic cleaning with acetone and ethanol respectively, hair dryer dries up with for subsequent use.
3, the determination of pre-bombardment technique: refer to the ion bombardment technique of carrying out before the deposition for obtaining multi-arc ion coating TiAlNbN nitrogen gradient hard reaction film, when coating chamber back end vacuum tightness reaches 8.0 ' 10
-3handkerchief, temperature are filled with argon gas when reaching 200 ° of C, make coating chamber vacuum tightness reach 2.5 ' 10
-1handkerchief, opens two arc sources, keeps arc current at 55 ~ 56 amperes, carries out ion bombardment 10 ~ 12 minutes, and bombardment bias voltage is increased to 400 volts gradually from 350 volts.
4, the determination of depositing operation: refer to the depositing operation adopted for obtaining multi-arc ion coating TiAlNbN nitrogen gradient hard reaction film, coating process is divided into three phases, the first step, and the ar pressure in coating chamber is remained on 2.0 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 55 ~ 56 amperes, and workpiece bias is 150 ~ 200 volts, depositing time 5 minutes; Second step, passes into nitrogen in coating chamber, makes its partial pressure reach 1.0 ' 10
-1handkerchief, then adjusts argon flow amount, makes mixed gas total pressure remain on 2.5 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 55 ~ 56 amperes, and workpiece bias is 150 ~ 200 volts, depositing time 20 minutes; 3rd step, close Ar inlet, make argon flow amount be 0, partial pressure of ar gas is 0, and continues to increase nitrogen flow, makes its pressure reach 2.5 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 55 ~ 56 amperes, and workpiece bias is 150 ~ 200 volts, depositing time 30 minutes.
5, vacuum heating treatment: comprise workpiece heat and rete baking, workpiece heat mode adopts electric heating element Baking out, reaches 3.0 ' 10 in coating chamber back end vacuum
-2start workpiece heat during handkerchief, heat-up rate remain on 3 ~ 5 ° of C/minute, 200 ° of C can be reached after one hour; Rete baking refers to that deposition process terminates to carry out post-heating baking to deposited TiAlNbN nitrogen gradient hard reaction film afterwards, and adopt small area analysis to carry out micro-heating 10 ~ 15 minutes, electric current is reduced to 50 amperes from 70 amperes gradually.
6, workpiece rotates: in the whole process of workpiece heat, ion bombardment, film deposition, rete baking, holding workpiece rotates always, and rotating speed is 4 ~ 6 revs/min.
The method of multi-arc ion coating TiAlNbN nitrogen gradient hard reaction film is prepared according to employing titanium-niobium alloy target proposed by the invention and titanium-aluminum alloy target combination target, above-mentioned TiAlNbN nitrogen gradient hard reaction film can be obtained, the nitrogen content distribution gradient of this TiAlNbN nitrogen gradient hard reaction film, strong adhesion (3200N), hardness high (3HV3200), heat-shock resistance strong (650 ° of C thermal shock circulations reach 13 ~ 15 times).
Compared with the existing technology, the present invention determines the technology of preparing of conventional general multi-arc ion coating as TiAlNbN nitrogen gradient hard reaction film, determine commercial titanium-niobium alloy target and titanium-aluminum alloy target as arc source, avoid special smelting, prepare the limitation of titanium aluminium niobium alloy target, reduce coating cost; The present invention determines target material composition, quantity and configuration orientation, determine commercial rapid steel as workpiece material, determine workpiece pre-treating technology and depositing operation, realize while ensure that rete high rigidity, high adhesive force and high-heat resistance shock resistant, and there is satisfactory stability and repeatability, thus advantageously the friction durability of improving TiAlNbN nitrogen gradient hard reaction film, be more suitable for the application at Tool Industry.
Embodiment
embodiment 1
At commercial rapid steel (W18Cr4V) upper preparation TiAlNbN nitrogen gradient hard reaction film, its method is:
1, the determination of deposition technique and target material composition: determine the technology of preparing of multi-arc ion coating as TiAlNbN nitrogen gradient hard reaction film, select two different azimuth and become the arc source starting the arc simultaneously of 90 degree of configurations to deposit, one of them arc source is the commercial titanium-niobium alloy target of purity 99.9%, and the atomic ratio of titanium-niobium alloy target is Ti:Nb=75:25; Another arc source is the commercial titanium-aluminum alloy target of purity 99.9%, and the atomic ratio of titanium-aluminum alloy target is Ti:Al=50:50.
2, the selection of workpiece and pre-treatment: select commercial rapid steel (W18Cr4V) as workpiece material, before putting into coating chamber and carrying out plated film, use to workpiece, metal detergent carries out that routine is deoiled, decontamination process carry out surface finish process, finally carry out ultrasonic cleaning with acetone and ethanol respectively, hair dryer dries up with for subsequent use.
3, the determination of pre-bombardment technique: refer to the ion bombardment technique of carrying out before the deposition for obtaining multi-arc ion coating TiAlNbN nitrogen gradient hard reaction film, when coating chamber back end vacuum tightness reaches 8.0 ' 10
-3handkerchief, temperature are filled with argon gas when reaching 200 ° of C, make coating chamber vacuum tightness reach 2.5 ' 10
-1handkerchief, opens two arc sources, keeps arc current at 55 amperes, carries out ion bombardment 10 minutes, and bombardment bias voltage is increased to 400 volts gradually from 350 volts.
4, the determination of depositing operation: refer to the depositing operation adopted for obtaining multi-arc ion coating TiAlNbN nitrogen gradient hard reaction film, coating process is divided into three phases, the first step, and the ar pressure in coating chamber is remained on 2.0 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 55 amperes, and workpiece bias is 200 volts, depositing time 5 minutes; Second step, passes into nitrogen in coating chamber, makes its partial pressure reach 1.0 ' 10
-1handkerchief, then adjusts argon flow amount, makes mixed gas total pressure remain on 2.5 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 55 amperes, and workpiece bias is 200 volts, depositing time 20 minutes; 3rd step, close Ar inlet, make argon flow amount be 0, partial pressure of ar gas is 0, and continues to increase nitrogen flow, makes its pressure reach 2.5 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 55 amperes, and workpiece bias is 200 volts, depositing time 30 minutes.
5, vacuum heating treatment: comprise workpiece heat and rete baking, workpiece heat mode adopts electric heating element Baking out, reaches 3.0 ' 10 in coating chamber back end vacuum
-2start workpiece heat during handkerchief, heat-up rate remain on 3 ~ 5 ° of C/minute, reach 200 ° of C after one hour; Rete baking refers to that deposition process terminates to carry out post-heating baking to deposited TiAlNbN nitrogen gradient hard reaction film afterwards, and adopt small area analysis to carry out micro-heating 12 minutes, electric current is reduced to 50 amperes from 70 amperes gradually.
6, workpiece rotates: in the whole process of workpiece heat, ion bombardment, film deposition, rete baking, holding workpiece rotates always, and rotating speed is 5 revs/min.
Test the TiAlNbN nitrogen gradient hard reaction film using aforesaid method to prepare, the nitrogen content distribution gradient of this TiAlNbN nitrogen gradient hard reaction film, sticking power reaches 200N, and hardness reaches HV3400, and anti-650 ° of C thermal shock cycle indexes reach 14 times.
Embodiment 2
At commercial rapid steel (W6Mo5Cr4V2) upper preparation TiAlNbN nitrogen gradient hard reaction film, its method is:
1, the determination of deposition technique and target material composition: determine the technology of preparing of multi-arc ion coating as TiAlNbN nitrogen gradient hard reaction film, select two different azimuth and become the arc source starting the arc simultaneously of 90 degree of configurations to deposit, one of them arc source is the commercial titanium-niobium alloy target of purity 99.9%, and the atomic ratio of titanium-niobium alloy target is Ti:Nb=75:25; Another arc source is the commercial titanium-aluminum alloy target of purity 99.9%, and the atomic ratio of titanium-aluminum alloy target is Ti:Al=50:50.
2, the selection of workpiece and pre-treatment: select commercial rapid steel (W6Mo5Cr4V2) as workpiece material, before putting into coating chamber and carrying out plated film, use to workpiece, metal detergent carries out that routine is deoiled, decontamination process carry out surface finish process, finally carry out ultrasonic cleaning with acetone and ethanol respectively, hair dryer dries up with for subsequent use.
3, the determination of pre-bombardment technique: refer to the ion bombardment technique of carrying out before the deposition for obtaining multi-arc ion coating TiAlNbN nitrogen gradient hard reaction film, when coating chamber back end vacuum tightness reaches 8.0 ' 10
-3handkerchief, temperature are filled with argon gas when reaching 200 ° of C, make coating chamber vacuum tightness reach 2.5 ' 10
-1handkerchief, opens two arc sources, keeps arc current at 56 amperes, carries out ion bombardment 10 minutes, and bombardment bias voltage is increased to 400 volts gradually from 350 volts.
4, the determination of depositing operation: refer to the depositing operation adopted for obtaining multi-arc ion coating TiAlNbN nitrogen gradient hard reaction film, coating process is divided into three phases, the first step, and the ar pressure in coating chamber is remained on 2.0 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 56 amperes, and workpiece bias is 150 volts, depositing time 5 minutes; Second step, passes into nitrogen in coating chamber, makes its partial pressure reach 1.0 ' 10
-1handkerchief, then adjusts argon flow amount, makes mixed gas total pressure remain on 2.5 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 56 amperes, and workpiece bias is 150 volts, depositing time 20 minutes; 3rd step, close Ar inlet, make argon flow amount be 0, partial pressure of ar gas is 0, and continues to increase nitrogen flow, makes its pressure reach 2.5 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 56 amperes, and workpiece bias is 150 volts, depositing time 30 minutes.
5, vacuum heating treatment: comprise workpiece heat and rete baking, workpiece heat mode adopts electric heating element Baking out, reaches 3.0 ' 10 in coating chamber back end vacuum
-2start workpiece heat during handkerchief, heat-up rate remain on 3 ~ 5 ° of C/minute, reach 200 ° of C after one hour; Rete baking refers to that deposition process terminates to carry out post-heating baking to deposited TiAlNbN nitrogen gradient hard reaction film afterwards, and adopt small area analysis to carry out micro-heating 10 minutes, electric current is reduced to 50 amperes from 70 amperes gradually.
6, workpiece rotates: in the whole process of workpiece heat, ion bombardment, film deposition, rete baking, holding workpiece rotates always, and rotating speed is 5 revs/min.
Test the TiAlNbN nitrogen gradient hard reaction film using aforesaid method to prepare, the nitrogen content distribution gradient of this TiAlNbN nitrogen gradient hard reaction film, sticking power reaches 200N, and hardness reaches HV3300, and anti-650 ° of C thermal shock cycle indexes reach 15 times.
Claims (1)
1. the preparation method of a TiAlN niobium nitrogen gradient hard reaction film, it is characterized in that: its preparation method comprises successively: the determination of (1), deposition technique and target material composition: determine the technology of preparing of multi-arc ion coating as TiAlNbN nitrogen gradient hard reaction film, select two different azimuth and become the arc source starting the arc simultaneously of 90 degree of configurations to deposit, one of them arc source is the commercial titanium-niobium alloy target of purity 99.9%, and the atomic ratio of titanium-niobium alloy target is Ti:Nb=75:25; Another arc source is the commercial titanium-aluminum alloy target of purity 99.9%, and the atomic ratio of titanium-aluminum alloy target is Ti:Al=50:50; (2), the selection of workpiece and pre-treatment: select commercial rapid steel as workpiece material, before putting into coating chamber and carrying out plated film, use to workpiece, metal detergent carries out that routine is deoiled, decontamination process carry out surface finish process, finally carry out ultrasonic cleaning with acetone and ethanol respectively, hair dryer dries up with for subsequent use; (3), the determination of pre-bombardment technique: refer to the ion bombardment technique of carrying out before the deposition for obtaining multi-arc ion coating TiAlNbN nitrogen gradient hard reaction film, when coating chamber back end vacuum tightness reaches 8.0 ' 10
-3handkerchief, temperature are filled with argon gas when reaching 200 ° of C, make coating chamber vacuum tightness reach 2.5 ' 10
-1handkerchief, opens two arc sources, keeps arc current at 55 ~ 56 amperes, carries out ion bombardment 10 ~ 12 minutes, and bombardment bias voltage is increased to 400 volts gradually from 350 volts; (4), the determination of depositing operation: refer to the depositing operation adopted for obtaining multi-arc ion coating TiAlNbN nitrogen gradient hard reaction film, coating process is divided into three phases, the first step, and the ar pressure in coating chamber is remained on 2.0 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 55 ~ 56 amperes, and workpiece bias is 150 ~ 200 volts, depositing time 5 minutes; Second step, passes into nitrogen in coating chamber, makes its partial pressure reach 1.0 ' 10
-1handkerchief, then adjusts argon flow amount, makes mixed gas total pressure remain on 2.5 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 55 ~ 56 amperes, and workpiece bias is 150 ~ 200 volts, depositing time 20 minutes; 3rd step, close Ar inlet, make argon flow amount be 0, partial pressure of ar gas is 0, and continues to increase nitrogen flow, makes its pressure reach 2.5 ' 10
-1handkerchief, the arc current of titanium-aluminum alloy target and titanium-niobium alloy target is all placed in 55 ~ 56 amperes, and workpiece bias is 150 ~ 200 volts, depositing time 30 minutes; (5), vacuum heating treatment: comprise workpiece heat and rete baking, workpiece heat mode adopts electric heating element Baking out, reaches 3.0 ' 10 in coating chamber back end vacuum
-2start workpiece heat during handkerchief, heat-up rate remain on 3 ~ 5 ° of C/minute, 200 ° of C can be reached after one hour; Rete baking refers to that deposition process terminates to carry out post-heating baking to deposited TiAlNbN nitrogen gradient hard reaction film afterwards, and adopt small area analysis to carry out micro-heating 10 ~ 15 minutes, electric current is reduced to 50 amperes from 70 amperes gradually; (6), workpiece rotates: in the whole process of workpiece heat, ion bombardment, film deposition, rete baking, holding workpiece rotates always, and rotating speed is 4 ~ 6 revs/min.
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| CN104726823A (en) * | 2015-04-14 | 2015-06-24 | 沈阳大学 | Method for preparation of titanium aluminum zirconium niobium/titanium aluminum zirconium niobium nitride quaternary-nitrogen gradient films |
| CN104726824A (en) * | 2015-04-14 | 2015-06-24 | 沈阳大学 | Titanium nitride-aluminium-zirconium/titanium nitride-aluminium-zirconium-silicon quaternary double layer nitride film preparation method |
| CN106011753B (en) * | 2016-07-15 | 2019-02-22 | 沈阳大学 | A kind of preparation method of metal composite hard films |
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