CN110344005A - A kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable and the preparation method and application thereof - Google Patents

A kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable and the preparation method and application thereof Download PDF

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CN110344005A
CN110344005A CN201910605003.0A CN201910605003A CN110344005A CN 110344005 A CN110344005 A CN 110344005A CN 201910605003 A CN201910605003 A CN 201910605003A CN 110344005 A CN110344005 A CN 110344005A
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tialsin
micro
titanium alloy
tin
target
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张高会
梁文萍
缪强
孙自旺
汪阳
马海瑞
亓艳
李阳
赵子龙
黄朝军
林浩
易锦伟
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation

Abstract

The present invention discloses the preparation method and application of a kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable.Micro- lamination is deposited on TA15 titanium alloy surface by multi sphere ion plating technology, and micro- lamination is made of one layer of Ti transition zone and several layers TiN-TiAlSiN sedimentary；The Ti transition zone with a thickness of 0.5-1.0 μm；The TiN-TiAlSiN sedimentary with a thickness of 6-10 μm, outermost layer is TiAlSiN layers.Above-mentioned TA15 titanium alloy surface high-temperature wearable is micro- to be stacked in aircraft structure, especially applies in bearing high temperature and complex environment.The defects of micro- lamination of high-temperature wearable prepared by the present invention and matrix binding performance are superior, the obvious cavity of nothing, crackle can play the role of wear-resisting well under fretting wear environment.

Description

A kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable and its preparation Method and application
Technical field
The invention belongs to TA15 titanium alloy surface process fields, and in particular to a kind of TA15 titanium alloy surface high-temperature wearable is micro- Stack TiN-TiAlSiN and the preparation method and application thereof.
Background technique
The high-temperature stability and welding performance that TA15 titanium alloy not only has alpha titanium alloy excellent, and there is (alpha+beta) The good plastic deformation ability of Type Titanium Alloy, therefore TA15 titanium alloy especially exists particularly suitable for manufacturing various welding parts On space shuttle large-sized structural parts, TA15 titanium alloy is widely used, and most representative is Soviet Union 27.According to statistics, it revives The 27 titanium alloy blank qualities used reach 5.5t or so, account for the 16 ~ 18% of structural member total weight, and the single machine of TA15 titanium alloy Blank dosage can reach 70% or more of the total blank dosage of titanium alloy, become the important feature and selection feature of Advanced Aircraft Outstanding feature.But the soft of TA15 alloy, inductile shearing drag, coefficient of friction is big, have serious adhesive wear and The fretting wear of sensitivity, wear-resisting property relative deficiency, greatly affected the safety and reliability of titanium alloy structure part, significantly Limit its application development.Therefore TA15 titanium alloy is difficult to meet present and following technical requirements.
As the requirement to material surface property is higher and higher, consequent is the appearance of various ganoine thin films With it is various synthesis ganoine thin film technology Recent Progresses In The Development, also more embody the sufacing synthesis novel as one High use value possessed by sexology section.Mechanical property, chemical property and resistance to high temperature oxidation and anti-corruption on the surface of the material Corrosion can on have the ganoine thin film of many advantages especially noticeable.But single thin film is no longer satisfied applicable industry life The requirement of production, thin film system of new generation need developmental research, propose the concept of micro- lamination according to the shell structure of shell.
Micro- laminate film is the multi-layer thin for forming two kinds of different materials by certain interlamellar spacing and Thickness ratio intermeshing Film, hardness are resistant to the critical nature of plastic deformation.Be used to prepare micro- lamination high hardness material has transition metal nitride, carbon Material such as TiN/NbN, TiN/VN, TiN/CrN, Ni/TiC, TiN/TiAlSiN etc. that compound is formed.
The rub resistance service life of lamination hardness film is longer than single thin film and bilayer film, this can be explained by multiple solutions.It is first First, it is related with the average value of two kinds of materials that the rub resistance service life, which follows mixing rule,；Secondly because there are many interface, micro- lamination Service life be better than monomer coating material, and the rub resistance service life is inversely proportional with the number at interface.
Up to the present, sufacing focuses primarily upon signal layer coating and duplex coating in wear-resisting progress.Such as Nanjing Aero-Space University's Wang Fang etc. prepares Cr-Si composite cementation in TA15 alloy surface using double glow plasma surface alloying technology Layer, the results showed that, the nano hardness of Cr-Si compisite seeping layer is 10.371GPa, elasticity modulus 819.23GPa, compared with matrix point Nearly 4 times and 5 times are not improved.Such as Shanghai electronic information Vocationl Technical College wears Zhenyang and swashs in 45 steel surfaces preparation Ni-W-Si Light cladding coating, the results showed that, the hardness of coating is higher, and the wearability of machinery part surface increases substantially.But with painting The reduction of W content in layer, coating hardness decline, abrasion loss increase.But these methods all Shortcomings lack one kind at present can The method for effectively improving titanium alloy high-temperature wear resistance, and can be realized continuous effective protection matrix.
Summary of the invention
Present invention is generally directed under hot environment, the problem of titanium alloy wear resistance deficiency, main purpose be In providing a kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable and the preparation method and application thereof.I.e. in TA15 Titanium alloy surface prepares one layer of Ti transition zone and several layers TiN layer and TiAlSiN layers, and outermost layer is TiAlSiN layers, with nitridation The features such as high rigidity of object, high temperature resistant, plays the effect of Wear-resistant to titanium alloy surface.
A kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable, using multi sphere ion plating technology in TA15 Titanium alloy surface deposits micro- lamination, and micro- lamination successively includes Ti transition zone according to from the direction of TA15 titanium alloy surface outward With TiN-TiAlSiN sedimentary, the transition zone is one layer, and the TiN-TiAlSiN sedimentary is at least 2 layers, and TiN- It is located at outside for TiAlSiN layers in TiAlSiN sedimentary；The Ti transition zone with a thickness of 0.5-1 μm；The TiN- The overall thickness of TiAlSiN sedimentary is 6-10 μm.
The above-mentioned micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable the following steps are included:
Step 1, basis material pre-processes
Prepare TA15 titanium alloy, first bores pass through aperture in sample corner with small-bore bench drill, then use the sand paper of different model respectively It polished step by step matrix sample, next with mechanical polisher mirror surface be polished to the sample after polishing, be finally putting into and contain Have in the beaker of dehydrated alcohol and be cleaned by ultrasonic, is dried with spare；
Step 2, cleaning and placement workpiece
It polishes the inner wall and target material surface of vacuum drying oven, removes surface layer oxide film and impurity, then dipped with non-dust cloth anhydrous Ethyl alcohol is cleaned, and will be placed in vacuum drying oven with the sample face Ti target of drying；
Step 3, extracting vacuum furnace air to air pressure is 1 × 10-4Pa or less；Control cavity temperature is maintained at 200 ± 10 DEG C of models In enclosing, start to be passed through argon gas；
Step 4, aura cleans
Argon gas is opened until experiment terminates, while starting grid bias power supply cabinet, adjusting BP unipolar pulse is biased into 600V, furnace chamber air pressure It maintains within the scope of 2.0Pa-2.2Pa, continues 5-10min；
Step 5, Ti transition zone is prepared
It adjusts BP unipolar pulse and is biased into 200V-250V, open Ti target power supply and adjust electric current to 70A-80A, furnace chamber air pressure maintains Within the scope of 1.8Pa-2.2Pa, Ti target run duration 3min-7min；
Step 6, TiN layer is prepared
It keeps bias, size of current constant, is passed through N2Until experiment terminates, Ti target operation duration 3min-7min；
Step 7, TiAlSiN layers are prepared
Ti target power supply is closed, TiAlSi target power supply is opened and adjusts voltage to 75A-85A, open substrate spin button for sample rotates To face TiAlSi target, continue 3min-7min；TiAlSi target power supply is closed, Ti target power supply is opened, opens substrate spin button At sample rotates to face Ti target, continues 3min-7min, repeat the above steps, obtain at least 2 layers of TiN-TiAlSiN Sedimentary terminates experiment；
Step 8, pass hull closure
Successively close TiAlSi target power supply, grid bias power supply, gas cylinder switch, molecule switch pump, general supply.
It is that the sand of 180#, 280#, 320#, 400#, 500#, 600#, 800# model is successively used in step 1 as improved Paper polishes step by step to TA15 titanium alloy.
It is that the duration is determined as 6min in step 4 as improved.
It is that step 5 bias is determined as 250V as improved, Ti target current is determined as 80A, and the duration is determined as 5min。
It is Ti target duration 5min in step 6 as improved.
It is that TiAlSi target continues 5min in step 7 as improved, Ti target continues 5min.
The above-mentioned micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable is in the case where preparing hot environment or complex load The application on aerospace structural part to work in environment.
The utility model has the advantages that
Compared with prior art, the micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable of the present invention uses multi sphere ion Micro- lamination of coating technology preparation, good with TA15 film-substrate cohesion, Ti transition zone effectively raises matrix and TiN-TiAlSiN Between binding performance.In high temperature wear environment, the micro- lamination of TiN/TiAlSiN can effectively accomplish that Wear-resistant acts on.
Detailed description of the invention
Fig. 1 is the SEM figure in the micro- lamination section being prepared under different parameters, a- embodiment 1, b- embodiment 2, c- implementation Example 3；
Fig. 2 is that be prepared under different parameters micro- is stacked in frictional wear experiment coefficient of friction figure, a- embodiment 1, and b- is implemented Example 2, c- embodiment 3；
Fig. 3 is that be prepared under different parameters micro- is stacked in fretting wear grinding defect morphology figure, a- embodiment 1, b- embodiment 2, C- embodiment 3.
Specific embodiment
The invention will be further described in the following with reference to the drawings and specific embodiments.
Embodiment 1
As shown in Fig. 1 (a), a kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable, using multi-arc ion coating skill Art is deposited on TA15 titanium alloy surface, at first depositing Ti transition zone, and outermost layer is TiAlSiN layers.Micro- scope of lamination gross thickness is 8.9 μ m；Ti transition region thickness is 0.9 μm, the TiN layer with a thickness of 0.8 μm, TiAlSiN layers with a thickness of 0.8 μm, i.e., the described TiN- TiAlSiN sedimentary is 5 layers.
Preparation method includes the following steps:
Step 1, basis material pre-processes
Prepare TA15 titanium alloy, is polished step by step with the sand paper of different model matrix sample respectively, next with mechanical throwing Ray machine polishes the sample after polishing, is finally putting into the beaker containing dehydrated alcohol and is cleaned by ultrasonic, spare；Sand paper Model use 180#, 280#, 320#, 400#, 500#, 600#, 800# respectively.
Step 2, cleaning and placement workpiece
It polishes the inner wall and target material surface of vacuum drying oven, removes surface layer oxide film and impurity, then dipped with non-dust cloth anhydrous Ethyl alcohol is cleaned, and will be placed in vacuum drying oven with the sample face Ti target of drying.
Step 3, vacuum furnace air is extracted, until air pressure is 1 × 10-4Pa is hereinafter, control cavity temperature is maintained at 200 DEG C It is interior；
Step 4, aura cleans
Argon gas is opened until experiment terminates, while starting grid bias power supply cabinet, adjusting BP unipolar pulse is biased into 600V, continues 6min；
Step 5, Ti transition zone is prepared
It adjusts BP unipolar pulse and is biased into 250V, open Ti target power supply and adjust electric current to 70A, duration 5min；
Step 6, TiN layer is prepared
It keeps bias, size of current constant, is passed through N2Until experiment terminates, Ti target continues working 5min；
Step 7, TiAlSiN layers are prepared
Ti target power supply is closed, TiAlSi target power supply is opened and adjusts voltage to 75A, open substrate spin button for sample rotates to just At TiAlSi target, continue 5min；TiAlSi target power supply is closed, Ti target power supply is opened, substrate spin button is opened and revolves sample It goes at face Ti target, continues 5min, repeat the above steps until experiment terminates；
Step 8, pass hull closure
Successively close TiAlSi target power supply, grid bias power supply, gas cylinder switch, molecule switch pump, general supply.
Friction-wear test is carried out to the micro- lamination prepared, the pattern after observing frictional wear experiment compares TA15 The coefficient of friction of titanium alloy substrate and the micro- lamination of TiN-TiAlSiN calculates wear volume and specific wear rate.As a result such as Fig. 2 a institute Show.
Micro- lamination made from the present embodiment ties up formula hardness and isHV, be matrix hardness (HV) 5.4 times；Micro- lamination Average friction coefficient under room temperature be 0.61, the average friction coefficient of the same terms lower substrate is 0.46, but micro- folded The friction coefficient curve of layer is more stable compared with matrix.Its specific wear rate is 7.35 × 10-6 mm3·N-1m-1, far below the ratio of matrix Wear rate (45.42 × 10-6 mm3·N-1m-1).And the specific wear rate of micro- lamination is 8.42 × 10 under 400 DEG C of hot conditions-6 mm3·N-1m-1, only the 32.8% of matrix.
Embodiment 2
As shown in Fig. 1 (b), a kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable, using multi-arc ion coating Technology is deposited on TA15 titanium alloy surface, at first depositing Ti transition zone, and outermost layer is TiAlSiN layers.Micro- scope of lamination gross thickness is 6.9 μm；Ti transition region thickness is 0.9 μm, and TiN layer is with a thickness of 0.6 μm, and TiAlSiN layers with a thickness of 0.6 μm.
Preparation method includes the following steps:
Step 1, basis material pre-processes
Prepare TA15 titanium alloy, is polished step by step with the sand paper of different model matrix sample respectively, next with mechanical throwing Ray machine polishes the sample after polishing, is finally putting into the beaker containing dehydrated alcohol and is cleaned by ultrasonic, spare；Sand paper Model use 180#, 280#, 320#, 400#, 500#, 600#, 800# respectively.
Step 2, cleaning and placement workpiece
It polishes the inner wall and target material surface of vacuum drying oven, removes surface layer oxide film and impurity, then dipped with non-dust cloth anhydrous Ethyl alcohol is cleaned, and will be placed in vacuum drying oven with the sample face Ti target of drying.
Step 3, vacuum furnace air is extracted, until air pressure is 1 × 10-4Pa is hereinafter, control cavity temperature is maintained at 200 DEG C It is interior；
Step 4, aura cleans
Argon gas is opened until experiment terminates, while starting grid bias power supply cabinet, adjusting BP unipolar pulse is biased into 600V, furnace chamber internal pressure It is maintained at 2.0Pa by force, continues 6min；
Step 5, Ti transition zone is prepared
It adjusts BP unipolar pulse and is biased into 250V, open Ti target power supply and adjust electric current to 70A, duration 5min；
Step 6, TiN layer is prepared
Adjustment bias is 225V, and electric current 75A is passed through N2Until experiment terminates, Ti target operation duration 5min；
Step 7, TiAlSiN layers are prepared
Ti target power supply is closed, TiAlSi target power supply is opened and adjusts voltage to 80A, open substrate spin button for sample rotates to just At TiAlSi target, continue 5min；TiAlSi target power supply is closed, Ti target power supply is opened, substrate spin button is opened and revolves sample It goes at face Ti target, continues 5min, repeat the above steps until experiment terminates；
Step 8, pass hull closure
Successively close TiAlSi target power supply, grid bias power supply, gas cylinder switch, molecule switch pump, general supply.
Friction-wear test is carried out to the micro- lamination prepared, the pattern after observing frictional wear experiment compares TA15 The coefficient of friction of titanium alloy substrate and the micro- lamination of TiN/TiAlSiN calculates wear volume and specific wear rate.As a result such as Fig. 2 b institute Show.
The dimension formula hardness of micro- lamination made from the present embodiment is 1393HV, be matrix hardness (HV) 3.9 times；Micro- lamination Average friction coefficient under room temperature be 0.61, the average friction coefficient of the same terms lower substrate is 0.58, but micro- folded The friction coefficient curve of layer is more stable compared with matrix.Its specific wear rate is 7.47 × 10-6 mm3·N-1m-1, far below the ratio of matrix Wear rate (48.56 × 10-6 mm3·N-1m-1).And the specific wear rate of micro- lamination is 9.68 × 10 under 400 DEG C of hot conditions-6 mm3·N-1m-1, only the 35.2% of matrix.
Embodiment 3
As shown in Fig. 1 (c), a kind of micro- lamination of TA15 titanium alloy surface high-temperature wearable is deposited on using multi sphere ion plating technology TA15 titanium alloy surface, depositing Ti transition zone, outermost layer are TiAlSiN layers at first.Micro- scope of lamination gross thickness is 6.4 μm；Ti transition Layer is with a thickness of 0.9 μm, and TiN layer is with a thickness of 0.5 μm, and TiAlSiN layers with a thickness of 0.6 μm.
Preparation method includes the following steps:
Step 1, basis material pre-processes
Prepare TA15 titanium alloy, is polished step by step with the sand paper of different model matrix sample respectively, next with mechanical throwing Ray machine polishes the sample after polishing, is finally putting into the beaker containing dehydrated alcohol and is cleaned by ultrasonic, spare；Sand paper Model use 180#, 280#, 320#, 400#, 500#, 600#, 800# respectively.
Step 2, cleaning and placement workpiece
It polishes the inner wall and target material surface of vacuum drying oven, removes surface layer oxide film and impurity, then dipped with non-dust cloth anhydrous Ethyl alcohol is cleaned, and will be placed in vacuum drying oven with the sample face Ti target of drying.
Step 3, vacuum furnace air is extracted, until air pressure is 1 × 10-4Pa is hereinafter, control cavity temperature is maintained at 200 DEG C It is interior；
Step 4, aura cleans
Argon gas is opened up to off-test, while starting grid bias power supply cabinet, BP unipolar pulse is adjusted and is biased into 600V, continue 6min；
Step 5, Ti transition zone is prepared
It adjusts BP unipolar pulse and is biased into 250V, open Ti target power supply and adjust electric current to 70A, duration 5min；
Step 6, TiN layer is prepared
Adjustment bias is 200V, and electric current 80A is passed through N2Until off-test, Ti target operation duration 5min；
Step 7, TiAlSiN layers are prepared
Ti target power supply is closed, TiAlSi target power supply is opened and adjusts voltage to 85A, open substrate spin button for sample rotates to just At TiAlSi target, continue 5min；TiAlSi target power supply is closed, Ti target power supply is opened, substrate spin button is opened and revolves sample It goes at face Ti target, continues 5min, repeat the above steps until experiment terminates；
Step 8, pass hull closure
Successively close TiAlSi target power supply, grid bias power supply, gas cylinder switch, molecule switch pump, general supply.
Friction-wear test is carried out to the micro- lamination prepared, the pattern after observing frictional wear experiment compares TA15 The coefficient of friction of titanium alloy substrate and the micro- lamination of TiN/TiAlSiN calculates wear volume and specific wear rate.As a result such as Fig. 2 c institute Show.
The dimension formula hardness of micro- lamination made from the present embodiment is 1943HV, be matrix hardness (HV) 5.4 times；Micro- lamination Average friction coefficient under room temperature be 0.61, the average friction coefficient of the same terms lower substrate is 0.60, but micro- folded The friction coefficient curve of layer is more stable compared with matrix.Its specific wear rate is 6.82 × 10-6 mm3·N-1m-1, far below the ratio of matrix Wear rate (50.67 × 10-6 mm3·N-1m-1).And the specific wear rate of micro- lamination is 7.19 × 10 under 400 DEG C of hot conditions-6 mm3·N-1m-1, only the 36.8% of matrix.
Comparative example 1
Step 1, prepare TA15 titanium alloy, polished step by step with the sand paper of different model matrix sample, next used respectively Mechanical polisher polishes the sample after polishing, is finally putting into the beaker containing dehydrated alcohol and is cleaned by ultrasonic, standby With；The model of sand paper uses 180#, 280#, 320#, 400#, 500#, 600#, 800# respectively.
Step 2, cleaning and placement workpiece
It polishes the inner wall and target material surface of vacuum drying oven, removes surface layer oxide film and impurity, then dipped with non-dust cloth anhydrous Ethyl alcohol is cleaned, and will be placed in vacuum drying oven with the sample face Ti target of drying.
Step 3, vacuum furnace air is extracted, until air pressure is 1 × 10-4Pa is hereinafter, be continually fed into argon gas；
Step 4, aura cleans
Start grid bias power supply cabinet, adjusts BP unipolar pulse and be biased into 600V, continue 6min；
Step 5, Ti transition zone is prepared
It adjusts BP unipolar pulse and is biased into 250V, open Ti target power supply and adjust electric current to 70A, duration 5min；
Step 6, TiN layer is prepared
Adjustment bias is 200V, and electric current 80A is passed through N2Continue 50min；
Step 7, pass hull closure
Successively close Ti target power supply, grid bias power supply, gas cylinder switch, molecule switch pump, general supply.
Single layer TiN layer made from this comparative example with a thickness of 5.9 μm, dimension formula hardness be 1013HV, be matrix hardness ( HV) 2.9 times；TiN layer average friction coefficient under room temperature is 0.46, and specific wear rate is 15.6 × 10-6 mm3·N- 1m-1, lower than the specific wear rate (50.67 × 10 of matrix-6 mm3·N-1m-1), but it is higher than the specific wear rate (6.82 × 10 of micro- lamination-6 mm3·N-1m-1).The specific wear rate of TiN layer is 16 × 10 under the conditions of 400 DEG C-6 mm3·N-1m-1, it is much higher than under the same terms The specific wear rate of the micro- lamination of TiN-TiAlSiN.By embodiment and comparative example, the wear resistance of micro- lamination is found more It is good.
The foregoing is only a preferred embodiment of the present invention, the scope of protection of the present invention is not limited to this, it is any ripe Know those skilled in the art within the technical scope of the present disclosure, the letter for the technical solution that can be become apparent to Altered or equivalence replacement are fallen within the protection scope of the present invention.

Claims (8)

1. a kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable, which is characterized in that use multi-arc ion coating skill Art deposits micro- lamination in TA15 titanium alloy surface, and micro- lamination successively includes according to from the direction of TA15 titanium alloy surface outward Ti transition zone and TiN-TiAlSiN sedimentary, the transition zone are one layer, and the TiN-TiAlSiN sedimentary is at least 2 layers, And in TiN-TiAlSiN sedimentary TiAlSiN layers be located at outside；The Ti transition zone with a thickness of 0.5-1.0 μm；It is described The overall thickness of TiN-TiAlSiN sedimentary is 6-10 μm.
2. the system based on a kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable as stated in claim 1 Preparation Method, which comprises the following steps:
Step 1, basis material pre-processes
Prepare TA15 titanium alloy, first bores pass through aperture in sample corner with small-bore bench drill, then use the sand paper of different model respectively It polished step by step matrix sample, next with mechanical polisher mirror surface be polished to the sample after polishing, be finally putting into and contain Have in the beaker of dehydrated alcohol and be cleaned by ultrasonic, is dried with spare；
Step 2, cleaning and placement workpiece
It polishes the inner wall and target material surface of vacuum drying oven, removes surface layer oxide film and impurity, then dipped with non-dust cloth anhydrous Ethyl alcohol is cleaned, and will be placed in vacuum drying oven with the sample face Ti target of drying；
Step 3, empty furnace air to air pressure is 1 × 10-4Pa or less；Control cavity temperature is maintained within the scope of 200 ± 10 DEG C, Start to be passed through argon gas；
Step 4, aura cleans
Argon gas is opened until experiment terminates, while starting grid bias power supply cabinet, adjusting BP unipolar pulse is biased into 600V, furnace chamber air pressure It maintains within the scope of 2.0Pa-2.2Pa, continues 5-10min；
Step 5, Ti transition zone is prepared
It adjusts BP unipolar pulse and is biased into 200V-250V, open Ti target power supply and adjust electric current to 70A-80A, furnace chamber air pressure maintains Within the scope of 1.8Pa-2.2Pa, Ti target operation duration 3min-7min；
Step 6, TiN layer is prepared
It keeps bias, size of current constant, is passed through N2Until experiment terminates, Ti target operation duration 3min-7min；
Step 7, TiAlSiN layers are prepared
Ti target power supply is closed, TiAlSi target power supply is opened and adjusts voltage to 75A-85A, open substrate spin button for sample rotates To face TiAlSi target, continue 3min-7min；TiAlSi target power supply is closed, Ti target power supply is opened, opens substrate spin button At sample rotates to face Ti target, continues 3min-7min, repeat the above steps, obtain at least 2 layers of TiN-TiAlSiN Sedimentary terminates experiment；
Step 8, pass hull closure
Successively close TiAlSi target power supply, grid bias power supply, gas cylinder switch, molecule switch pump, general supply.
3. according to a kind of system of the micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable described in claim requirement 2 Preparation Method, which is characterized in that the sand paper pair of 180#, 280#, 320#, 400#, 500#, 600#, 800# model is successively used in step 1 TA15 titanium alloy is polished step by step.
4. according to a kind of system of the micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable described in claim requirement 2 Preparation Method, which is characterized in that the duration is determined as 6min in step 4.
5. according to a kind of system of the micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable described in claim requirement 2 Preparation Method, which is characterized in that step 5 bias is determined as 250V, and Ti target current is determined as 80A, and the duration is determined as 5min.
6. according to a kind of system of the micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable described in claim requirement 2 Preparation Method, which is characterized in that Ti target duration 5min in step 6.
7. according to a kind of system of the micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable described in claim requirement 2 Preparation Method, which is characterized in that TiAlSi target continues 5min in step 7, and Ti target continues 5min.
8. preparing high temperature ring based on the micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable described in claim 1 The application on aerospace structural part to work under border or in complex load environment.
CN201910605003.0A 2019-07-05 2019-07-05 A kind of micro- stack TiN-TiAlSiN of TA15 titanium alloy surface high-temperature wearable and the preparation method and application thereof Pending CN110344005A (en)

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