CN105088129B - The preparation method of micro-nano texturing titanium nitride solid lubricant film - Google Patents
The preparation method of micro-nano texturing titanium nitride solid lubricant film Download PDFInfo
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- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 239000007787 solid Substances 0.000 title claims abstract description 28
- 239000000314 lubricant Substances 0.000 title claims abstract description 27
- 239000011159 matrix material Substances 0.000 claims abstract description 33
- 238000012545 processing Methods 0.000 claims abstract description 27
- 238000005121 nitriding Methods 0.000 claims abstract description 25
- 230000004913 activation Effects 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 230000008595 infiltration Effects 0.000 claims abstract description 11
- 238000001764 infiltration Methods 0.000 claims abstract description 11
- 239000011859 microparticle Substances 0.000 claims abstract description 8
- 238000006396 nitration reaction Methods 0.000 claims abstract description 8
- 238000002203 pretreatment Methods 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 239000007789 gas Substances 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- 238000005498 polishing Methods 0.000 claims description 22
- 239000010936 titanium Substances 0.000 claims description 20
- 229910052719 titanium Inorganic materials 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000000758 substrate Substances 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 230000002000 scavenging effect Effects 0.000 claims description 4
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000002113 nanodiamond Substances 0.000 claims description 2
- 238000005461 lubrication Methods 0.000 abstract description 13
- 230000001050 lubricating effect Effects 0.000 abstract description 9
- 239000012528 membrane Substances 0.000 abstract description 4
- 239000010408 film Substances 0.000 description 42
- 238000005516 engineering process Methods 0.000 description 7
- 230000008859 change Effects 0.000 description 6
- 125000004433 nitrogen atom Chemical group N* 0.000 description 6
- 238000002791 soaking Methods 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- 229910010037 TiAlN Inorganic materials 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 150000003608 titanium Chemical class 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003831 antifriction material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of preparation method of micro-nano texturing titanium nitride solid lubricant film, it is characterised in that：Comprise the following steps：S01, the pre-treatment of matrix；S02, surface-texturing processing：Texturing processing is carried out to matrix surface using supersonic microparticle bombardment equipment；S03, the preparation of nitration case：Titanium nitride infiltration layer is prepared using the method for activation screen assisted glow ionic nitriding.A kind of preparation method for micro-nano texturing titanium nitride solid lubricant film that the present invention is provided, reduce the preparation condition of titanium nitride membrane, improve its preparation efficiency and quality, realize its metallurgical binding with matrix, film is with matrix without obvious combination interface, and in complete metallurgical binding, bond strength is high, and realize that it, to the universality for lubricating operating mode, meets the lubrication of plant equipment and wear-resistant protection requirements under Various Complex operating mode.
Description
Technical field
The present invention relates to a kind of preparation method of micro-nano texturing titanium nitride solid lubricant film, belong to metal material and component
Surface is modified and processing, fretting wear protection technology field.
Background technology
All the time, fretting wear is reduction equipment operating efficiency, causes energy consumption and generation environment to pollute
One of principal element, countries in the world are directed to the exploitation of New Friction-reducing anti-friction material, process for modifying surface and lubrication technology.Table
Face modification technology enjoys favor because of low cost, instant effect, simple operation.Except the various surface coating techniques of utilization are in material surface
Outside the wear resistance that hard coat is prepared to improve material, solid lubricant layer can be also prepared in material surface design effectively to be reduced
Fretting wear.Relative to traditional grease lubrication, solid lubricant layer can be in high temperature, high load capacity, ultralow temperature, ultrahigh vacuum, strong oxygen
Change effective realize under the special environment conditions such as reduction, intense radiation to lubricate, and in fields such as machinery, electronics and aerospace equipments
Obtain extensive use.
TiN (titanium nitride) ceramic membranes are set because of its excellent antifriction, anti-bonding, anti scuffing and decay resistance in machinery
Had broad application prospects in terms of the wear protection of standby and cutter.At present, the preparation and its burn into friction on TiAlN thin film
The existing more report such as characteristic research.
TiN film layer overview prepared by current method physically or chemically gets up to be primarily present following deficiency：Depositing temperature
High, matrix damage is big, around plating property is poor, film residual stress is high, film and substrate combinating strength is low, easy peeling, preparation efficiency are low,
High cost, be only applicable with size is small, simple in construction and surface smoothness is high workpiece, can not produce in enormous quantities.Meanwhile, as rubbing
When wiping lubricating layer, there is certain selectivity to lubrication operating mode.Abrasion resistance is lubricated generally under conditions of dry friction excellent, and
In water base or grease lubrication condition, its effect is then greatly reduced, and making the application field of TiAlN thin film has significant limitation.
Artificial texture technology causes the extensive of researcher as one of innovation forward position direction of tribological field in recent years
Pay attention to.The technology is to carry out micro forming design and then improvement to friction surface using technologies such as machinery, chemistry, electronics or optics
Its tribological property.At present, the research both at home and abroad on the optimization design and its tribology of texture has more report, but closes
It need to be goed deep into the complex effect of texture and solid lubricant film.If the excellent high temperature heavy load tribology of TiN solid films is special
Property be combined with the hydrodynamic lubrication of micro-nano texture, micro- storage and mechanical capture effect, will be expected to realize TiAlN thin film service life
Significantly extension and the expansion significantly of the scope of application, but be also rarely reported on the research of the design philosophy.Patent of invention " one kind tool
Have perforated membrane of TiN coatings and preparation method thereof " (CN102719691B) and " a kind of porous titanium nitride nano-array film and its
Preparation method " (CN102534630B) reports a kind of nitrogen plasma scanning method respectively and chemical synthesis in liquid phase method prepares porous knot
Structure TiN, both porous TiN have certain application prospect in sewage disposal, catalyst carrier, medical field, but technique is difficult
It is low with control, preparation efficiency, it is difficult to meet the protection requirements on engineering component especially wearing piece surface.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation condition of reduction titanium nitride membrane, improve its system
Standby efficiency and quality, realize its metallurgical binding with matrix, film and matrix are without obvious combination interface, in complete metallurgical junction
Close, bond strength is high, and realize its to the universality that lubricates operating mode, meet under Various Complex operating mode the lubrication of plant equipment and anti-
Grind the preparation method of the micro-nano texturing titanium nitride solid lubricant film of protection requirements；Further, the present invention provides a kind of improve
The reactivity of Ti, N atom, increases TiN equiax crystals；Meanwhile, plastic deformation drastically is introduced on the pole surface of matrix and is lacked
Fall into, the infiltration and diffusion for nitrogen-atoms provide passage, improve nitriding efficiency, the micro-nano texturing nitridation of refinement TiN crystallite dimensions
The preparation method of titanium solid lubricant film；Further, the present invention provides a kind of raising transmission of the nitrogen-atoms to matrix surface, subtracts
The damage that few ion sputtering is formed to matrix surface, while reducing the micro-nano texturing nitridation of the pollution of the other elements of matrix surface
The preparation method of titanium solid lubricant film.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
The preparation method of micro-nano texturing titanium nitride solid lubricant film, it is characterised in that：Comprise the following steps：
S01, the pre-treatment of matrix：It is base material from pure titanium or titanium alloy, then carries out surface preparation, surface preparation
Including going oxide film dissolving, metallographic polishing, polishing and cleaning；Rear skin drying is cleaned standby；
S02, surface-texturing processing：Texturing processing is carried out to matrix surface using supersonic microparticle bombardment equipment, Hong
Particulate is hit for SiO2Spheroidal particle, a diameter of 0.5~1mm；Carrier gas is high-purity argon gas, and purity is 99.9%；Speed is bombarded by gas
Body pressure is adjusted, and gas pressure is 0.5~2.0MPa；Bombardment time is 1~30min；After surface-texturing processing, through ultrasonic wave
It is standby after cleaning and drying, cleaned textured substrates are obtained, scavenging period is 30min, and medium is acetone；
S03, the preparation of nitration case：Titanium nitride infiltration layer is prepared using the method for activation screen assisted glow ionic nitriding；Activation
Screen is made up of industrial pure titanium TA2 thin plate and as auxiliary cathode, the thickness of slab of pure titanium TA2 thin plates is 0.5mm, and circular aperture is 5mm；
The objective table that textured substrates cleaned in S02 are inserted in activation screen, and keep insulation with auxiliary cathode；Then brightness is started
Photoion nitrogen treatment, technological parameter is：Nitriding temperature：680~890 DEG C, vacuum：6~7.5Pa, soaking time 6~10 is small
When, 22~27A of alternating current, 13~18A of DC current, 780~820V of voltage, nitrogen source：99.99% high pure nitrogen；Processing
After finishing, pass hull closure, nitrogen protection is with being furnace-cooled to room temperature.
The method for removing oxide film dissolving includes the method using abrasive machine or cutting.
The metallographic polishing is including the use of the polishing of multiple abrasive paper for metallograph.
The polishing agent used during the polishing is Nano diamond paste.
The cleaning is included using ultrasonic wave cleaning, and scavenging period is 30min, and medium is acetone.
As one kind preferably, the gas pressure is 1.2~1.5MPa；Bombardment time is 5~15min.
The activation screen is cylinder, and the circular port is evenly distributed with the activation screen.
S02 is in addition to it can produce texturing processing to substrate surface, moreover it is possible to beneficial activation is produced to it, is improved
The reactivity of Ti, N atom, increases TiN equiax crystals；Meanwhile, plastic deformation drastically is introduced on the pole surface of matrix and is lacked
Fall into, the infiltration and diffusion for nitrogen-atoms provide passage, improve nitriding efficiency, refine TiN crystallite dimensions.
The effect that pure activated titanium screen is used in S03 is to improve transmission of the nitrogen-atoms to matrix surface, reduces ion sputtering
Damage to matrix surface formation, while reducing the pollution of the other elements of matrix surface.
A kind of micro-nano texturing titanium nitride solid lubricant film, it is characterised in that：The matrix material being applicable is pure titanium or titanium
Alloy, it is anti-in the absorption on its surface, migration, diffusion and chemistry by nitrogen in nitridation process after being handled through surface-texturing
Texturing titanium nitride film should be formed, film is with matrix without obvious combination interface, and in complete metallurgical binding, bond strength is high.
The present invention is advantageous in that：The present invention proposes micro-nano texturing design on the basis of original TiN film
Thought, the increase for causing matrix surface activation, pole surface deformation and defect is on the one hand processed using texturing, nitriding bar is reduced
Part, improves nitriding efficiency, while being acted synergistically using the tribology of surface micro-nano texture and TiAlN thin film, further improves TiN film
The tribological property of layer, makes it be applicable not only to DRY SLIDING, can also meet the operating modes such as oil lubrication.On the other hand, using pure
Activated titanium screen assisted glow ion-nitridation method prepares titanium nitride infiltration layer, overcame in the past physically or chemically vapour deposition process and prepares nitrogen
The defect such as process conditions are higher, film substrate bond strength is low, Workpiece structure size and required precision height when changing titanium film layer, is more suitable for batch
Quantify low cost production and commercial Application.
Brief description of the drawings
Fig. 1 is the SEM shape appearance figures of the micro-nano texturing titanium nitride lubricating film prepared by embodiment 1~3；(a) embodiment 1；
(b) embodiment 2；(c) embodiment 3；
Fig. 2 is the XRD spectra of the micro-nano texturing titanium nitride lubricating film prepared by embodiment 1~3；
Fig. 3 is the micro-nano texturing titanium nitride lubricating film Cross Section Morphology figure prepared by embodiment 3
Fig. 4 is the micro-nano texturing titanium nitride lubricating film essential element line scanning figure prepared by embodiment 3；
Fig. 5 is friction factor figure of the micro-nano texturing titanium nitride lubricating film under different operating modes prepared by embodiment 3；
(a) dry friction；(b) PAO40 oil lubrications；
Fig. 6 is wear surface shape of the micro-nano texturing titanium nitride lubricating film under DRY SLIDING prepared by embodiment 3
Looks figure；(a) pure Titanium base；(b) texturing titanium nitride；
Fig. 7 is wear tables of the micro-nano texturing titanium nitride lubricating film under PAO40 Oil Lubrication Conditions prepared by embodiment 3
Face shape appearance figure；(a) pure Titanium base；(b) texturing titanium nitride.
Embodiment
The present invention is further described below in conjunction with the accompanying drawings.
Embodiment 1：
As shown in Fig. 1 (a)~2, the preparation method of micro-nano texturing titanium nitride solid lubricant film, it is characterised in that：Including
Following steps：
S01, the pre-treatment of matrix：By the wire cutting of TA2 industrially pure titaniums into 30mm × 15mm × 4mm print, surface coarse sand
After polishing, metallographic sanding and polishing is into minute surface, and then ultrasonic wave cleans 30min, dry for standby in medium-acetone；
S02, surface-texturing processing：Texturing processing is carried out to matrix surface using supersonic microparticle bombardment equipment, it is micro-
Grain is SiO2Spheroidal particle, a diameter of 0.5~1mm；Carrier gas is high-purity argon gas, and purity is 99.9%；Speed is bombarded by gas pressure
Power is adjusted, and gas pressure is 1.2MPa, and bombardment time is 5min, and ultrasonic wave cleans 30min and done in medium-acetone after processing
It is dry；
S03, the preparation of nitration case：TiN infiltration layers are prepared using the method for activation screen assisted glow ionic nitriding.Cylinder is living
Change screen to be made up of industrial pure titanium TA2 thin plate, as auxiliary cathode, thickness of slab is 0.5mm, and circular aperture is 5mm, and pitch of holes is
2.5mm；The objective table that cleaned textured substrates are inserted in activation screen, and keep insulation with auxiliary cathode；Then start
Glow discharge nitriding is handled, and main technologic parameters are：Nitriding temperature：850 DEG C, vacuum：6.2Pa, soaking time 8 hours is handed over
Flow electric current 23A, DC current 15A, voltage 800V, nitrogen source：99.99% high pure nitrogen；After being disposed, pass hull closure, nitrogen
Gas shielded is with being furnace-cooled to room temperature.
Titanium nitride film manufactured in the present embodiment is made up of equally distributed nick hole texture, and part texture has not yet been molded
It is whole；Film layer purity is very high, well-crystallized.
Embodiment 2：
As shown in Fig. 1 (b)~2, the preparation method of micro-nano texturing titanium nitride solid lubricant film, it is characterised in that：Including
Following steps：
S01, the pre-treatment of matrix：By the wire cutting of TA2 industrially pure titaniums into 30mm × 15mm × 4mm print, surface coarse sand
After polishing, metallographic sanding and polishing is into minute surface, and then ultrasonic wave cleans 30min, dry for standby in medium-acetone；
S02, surface-texturing processing：Texturing processing is carried out to matrix surface using supersonic microparticle bombardment equipment, it is micro-
Grain is SiO2Spheroidal particle, a diameter of 0.5~1mm；Carrier gas is high-purity argon gas, and purity is 99.9%；Speed is bombarded by gas pressure
Power is adjusted, and gas pressure is 1.5MPa, and bombardment time is 10min, and ultrasonic wave cleans 30min and done in medium-acetone after processing
It is dry；
S03, the preparation of nitration case：TiN infiltration layers are prepared using the method for activation screen assisted glow ionic nitriding.Cylinder is living
Change screen to be made up of industrial pure titanium TA2 thin plate, as auxiliary cathode, thickness of slab is 0.5mm, and circular aperture is 5mm, and pitch of holes is
2.5mm；The objective table that cleaned textured substrates are inserted in activation screen, and keep insulation with auxiliary cathode；Then start
Glow discharge nitriding is handled, and main technologic parameters are：Nitriding temperature：850 DEG C, vacuum：6.5Pa, soaking time 8 hours is handed over
Flow electric current 22A, DC current 18A, voltage 780V, nitrogen source：99.99% high pure nitrogen；After being disposed, pass hull closure, nitrogen
Gas shielded is with being furnace-cooled to room temperature.
Titanium nitride film manufactured in the present embodiment is made up of equally distributed nick hole texture, and film layer purity is very high, crystallization
Well.Moreover, relative to embodiment 1, due to the extension of gas pressure and time, show that texture shaping is complete, inwall is more smooth,
Boundary defect is reduced, and the crystallization degree of titanium nitride film is more preferable.
Embodiment 3：
As shown in Fig. 1 (c)~7, the preparation method of micro-nano texturing titanium nitride solid lubricant film, it is characterised in that：Including
Following steps：
S01, the pre-treatment of matrix：By the wire cutting of TA2 industrially pure titaniums into 30mm × 15mm × 4mm print, surface coarse sand
After polishing, metallographic sanding and polishing is into minute surface, and then ultrasonic wave cleans 30min, dry for standby in medium-acetone；
S02, surface-texturing processing：Texturing processing is carried out to matrix surface using supersonic microparticle bombardment equipment, it is micro-
Grain is SiO2Spheroidal particle, a diameter of 0.5~1mm；Carrier gas is high-purity argon gas, and purity is 99.9%；Speed is bombarded by gas pressure
Power is adjusted, and gas pressure is 1.2MPa, and bombardment time is 15min, and ultrasonic wave cleans 30min and done in medium-acetone after processing
It is dry.
S03, the preparation of nitration case：TiN infiltration layers are prepared using the method for activation screen assisted glow ionic nitriding.Cylinder is living
Change screen to be made up of industrial pure titanium TA2 thin plate, as auxiliary cathode, thickness of slab is 0.5mm, and circular aperture is 5mm, and pitch of holes is
2.5mm；The objective table that cleaned textured substrates are inserted in activation screen, and keep insulation with auxiliary cathode；Then start
Glow discharge nitriding is handled, and main technologic parameters are：Nitriding temperature：850 DEG C, vacuum：6.3Pa, soaking time 8 hours is handed over
Flow electric current 26A, DC current 17A, voltage 820V, nitrogen source：99.99% high pure nitrogen；After being disposed, pass hull closure, nitrogen
Gas shielded is with being furnace-cooled to room temperature.
As shown in Fig. 1 (c), the titanium nitride solid lubricant film inner surface of texture is in fiber tufted, and nick is handed between hole in prismatic
Connection.
As shown in figs. 34, the thicknesses of layers of the titanium nitride solid lubricant film of texture is uniform, about 30 μm, without substantially scarce
Fall into, be well combined with matrix, Ti, N element are in regular gradient distribution.
As shown in Fig. 5~7, using reciprocating friction abrasion tester respectively under dry friction and Oil Lubrication Condition to this implementation
Titanium nitride film prepared by example has carried out tribological property evaluation.
Experimental condition is：Dry friction, load 50N, speed 20mm/s；
Oil lubrication, load 20N, speed 20mm/s；
Friction factor and worn surface as shown in Fig. 5, Fig. 6~7, friction factor are dropped under DRY SLIDING respectively
Low by about 42%, under Oil Lubrication Condition, friction factor relatively reduces about 50%；Wear volume is smaller, and surface damage is slight.
Embodiment 4：
The preparation method of micro-nano texturing titanium nitride solid lubricant film, it is characterised in that：Comprise the following steps：
S01, the pre-treatment of matrix：By the wire cutting of TA2 industrially pure titaniums into 30mm × 15mm × 4mm print, surface coarse sand
After polishing, metallographic sanding and polishing is into minute surface, and then ultrasonic wave cleans 30min, dry for standby in medium-acetone；
S02, surface-texturing processing：Texturing processing is carried out to matrix surface using supersonic microparticle bombardment equipment, it is micro-
Grain is SiO2Spheroidal particle, a diameter of 0.5~1mm；Carrier gas is high-purity argon gas, and purity is 99.9%；Speed is bombarded by gas pressure
Power is adjusted, and gas pressure is 0.5MPa, and bombardment time is 1min, and ultrasonic wave cleans 30min and done in medium-acetone after processing
It is dry；
S03, the preparation of nitration case：TiN infiltration layers are prepared using the method for activation screen assisted glow ionic nitriding.Cylinder is living
Change screen to be made up of industrial pure titanium TA2 thin plate, as auxiliary cathode, thickness of slab is 0.5mm, and circular aperture is 5mm, and pitch of holes is
2.5mm；The objective table that cleaned textured substrates are inserted in activation screen, and keep insulation with auxiliary cathode；Then start
Glow discharge nitriding is handled, and main technologic parameters are：Nitriding temperature：680 DEG C, vacuum：6Pa, soaking time 6 hours, exchange
Electric current 22A, DC current 13A, voltage 780V, nitrogen source：99.99% high pure nitrogen；After being disposed, pass hull closure, nitrogen
Protection is with being furnace-cooled to room temperature.
Embodiment 5：
The preparation method of micro-nano texturing titanium nitride solid lubricant film, it is characterised in that：Comprise the following steps：
S01, the pre-treatment of matrix：By the wire cutting of TA2 industrially pure titaniums into 30mm × 15mm × 4mm print, surface coarse sand
After polishing, metallographic sanding and polishing is into minute surface, and then ultrasonic wave cleans 30min, dry for standby in medium-acetone；
S02, surface-texturing processing：Texturing processing is carried out to matrix surface using supersonic microparticle bombardment equipment, it is micro-
Grain is SiO2Spheroidal particle, a diameter of 0.5~1mm；Carrier gas is high-purity argon gas, and purity is 99.9%；Speed is bombarded by gas pressure
Power is adjusted, and gas pressure is 2.0MPa, and bombardment time is 30min, and ultrasonic wave cleans 30min and done in medium-acetone after processing
It is dry；
S03, the preparation of nitration case：TiN infiltration layers are prepared using the method for activation screen assisted glow ionic nitriding.Cylinder is living
Change screen to be made up of industrial pure titanium TA2 thin plate, as auxiliary cathode, thickness of slab is 0.5mm, and circular aperture is 5mm, and pitch of holes is
2.5mm；The objective table that cleaned textured substrates are inserted in activation screen, and keep insulation with auxiliary cathode；Then start
Glow discharge nitriding is handled, and main technologic parameters are：Nitriding temperature：890 DEG C, vacuum：7.5Pa, soaking time 10 hours is handed over
Flow electric current 27A, DC current 18A, voltage 820V, nitrogen source：99.99% high pure nitrogen；After being disposed, pass hull closure, nitrogen
Gas shielded is with being furnace-cooled to room temperature.
The above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. the preparation method of micro-nano texturing titanium nitride solid lubricant film, it is characterised in that：Comprise the following steps：
S01, the pre-treatment of matrix：It is base material from pure titanium or titanium alloy, then carries out surface preparation, surface preparation includes
Go oxide film dissolving, metallographic polishing, polishing and clean；Rear skin drying is cleaned standby；
S02, surface-texturing processing：Texturing processing is carried out to matrix surface using supersonic microparticle bombardment equipment, bombarded micro-
Grain is SiO2Spheroidal particle, a diameter of 0.5 ~ 1mm；Carrier gas is high-purity argon gas, and purity is 99.9%；Speed is bombarded by gas pressure
Regulation, gas pressure is 0.5 ~ 2.0MPa；Bombardment time is 1 ~ 30min；After surface-texturing processing, clean and do through ultrasonic wave
It is dry rear standby, cleaned textured substrates are obtained, scavenging period is 30min, and medium is acetone；
S03, the preparation of nitration case：Titanium nitride infiltration layer is prepared using the method for activation screen assisted glow ionic nitriding；Activation screen by
Industrial pure titanium TA2 thin plate is made and as auxiliary cathode, the thickness of slab of pure titanium TA2 thin plates is 0.5mm, and circular aperture is 5mm, Kong Jian
Away from for 2.5mm；The objective table that textured substrates cleaned in S02 are inserted in activation screen, and keep insulation with auxiliary cathode；
Then glow discharge nitriding processing is started, technological parameter is：Nitriding temperature：680 ~ 890 DEG C, vacuum：6 ~ 7.5Pa, during insulation
Between 6 ~ 10 hours, 22 ~ 27A of alternating current, 13 ~ 18A of DC current, 780 ~ 820V of voltage, nitrogen source：99.99% high pure nitrogen；
After being disposed, pass hull closure, nitrogen protection is with being furnace-cooled to room temperature.
2. the preparation method of micro-nano texturing titanium nitride solid lubricant film according to claim 1, it is characterised in that：It is described
Going the method for oxide film dissolving includes the method using abrasive machine or cutting.
3. the preparation method of micro-nano texturing titanium nitride solid lubricant film according to claim 1, it is characterised in that：It is described
Metallographic polishing is including the use of the polishing of multiple abrasive paper for metallograph.
4. the preparation method of micro-nano texturing titanium nitride solid lubricant film according to claim 1, it is characterised in that：It is described
The polishing agent used during polishing is Nano diamond paste.
5. the preparation method of micro-nano texturing titanium nitride solid lubricant film according to claim 1, it is characterised in that：It is described
Cleaning is included using ultrasonic wave cleaning, and scavenging period is 30min, and medium is acetone.
6. the preparation method of micro-nano texturing titanium nitride solid lubricant film according to claim 1, it is characterised in that：As
A kind of preferred, the gas pressure is 1.2 ~ 1.5MPa；Bombardment time is 5 ~ 15min.
7. the preparation method of micro-nano texturing titanium nitride solid lubricant film according to claim 1, it is characterised in that：It is described
Activation screen is cylinder, and the circular port is evenly distributed with the activation screen.
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| CN107962356B (en) * | 2017-11-25 | 2019-11-08 | 中国地质大学（北京） | A kind of preparation method of space flight titanium alloy TC 4 surface anti-friction wear-resistant strengthening layer |
| CN108179374A (en) * | 2018-01-30 | 2018-06-19 | 哈尔滨工程大学 | A kind of method for making Nano surface for accelerating vacuum carburization rate |
| CN111485233A (en) * | 2020-04-17 | 2020-08-04 | 安徽科蓝特铝业有限公司 | Method for preparing thick titanium nitride modified layer on surface of aluminum alloy |
| CN112522663A (en) * | 2020-11-05 | 2021-03-19 | 浙江工业大学 | Titanium alloy surface texturing synchronous nitriding process based on scanning galvanometer |
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