CN110129763A - It is a kind of based on the titanium-based diamond coatings binding force Enhancement Method being ultrasonically treated after carbonization - Google Patents

It is a kind of based on the titanium-based diamond coatings binding force Enhancement Method being ultrasonically treated after carbonization Download PDF

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Publication number
CN110129763A
CN110129763A CN201910547130.XA CN201910547130A CN110129763A CN 110129763 A CN110129763 A CN 110129763A CN 201910547130 A CN201910547130 A CN 201910547130A CN 110129763 A CN110129763 A CN 110129763A
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titanium
substrate surface
carbonization
substrate
chemical vapor
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徐锋
高继业
马震宇
施莉莉
王雪
左敦稳
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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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0254—Physical treatment to alter the texture of the surface, e.g. scratching or 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
    • C23C16/271—Diamond only using hot filaments

Abstract

It is a kind of based on the titanium-based diamond coatings binding force Enhancement Method being ultrasonically treated after carbonization, it is characterized in that its key step has: first using sand paper polishing titanium substrate surface to remove surface oxide layer and greasy dirt, it is cleaned by ultrasonic substrate surface later, secondly blasting treatment is carried out to substrate surface using sand-blasting machine, carbonization treatment is carried out to substrate using chemical vapor depsotition equipment later, then ultrasonic vibration in diadust acetone suspension is placed in the substrate after carbonization, finally, titanium substrate after ultrasonic cleaning and drying is placed in progress diamond coatings preparation in chemical vapor depsotition equipment.Present invention process is simple, and operation is easy, and relative to the methods of ultrasonic vibration pretreatment immediately after traditional sandblasting, film base binding performance is obviously improved.

Description

It is a kind of based on the titanium-based diamond coatings binding force Enhancement Method being ultrasonically treated after carbonization
Technical field
The present invention relates to a kind of technology of preparing of diamond coatings, in particular to diamond coatings titanium substrate surface is first carbonized The method that ultrasonic vibration pretreatment substitution conventional pretreatment technology improves film base binding performance afterwards, it is specifically a kind of to be based on carbon The titanium-based diamond coatings binding force Enhancement Method being ultrasonically treated after change.
Background technique
Titanium, because of its low-density, high-tensile and highly corrosion resistant and be applied to aerospace, biological medicine and chemical work Many fields such as journey.The major defect of titanium is that its frictional behaviour is poor, wear-resisting in titanium surface deposition by chemical vapour deposition technique Diamond coatings can dramatically the wearability for improving titanium.Diamond coatings have high rigidity, excellent biocompatibility and corrosion-resistant The advantages that property, titanium is expanded in the application prospect of high-tech area.
Good film base binding performance is the basis that coating works normally, while the service life of coating also can be with combination The increase of performance and increase.However, the thermal expansion coefficient between diamond and titanium differs larger, coat inside meeting after deposition Generate great residual stress.Further, since titanium is carbide, be easy in the atmosphere of depositing diamond film and Carbonaceous active group reacts, therefore can be initially formed one layer of stable titanium carbide in substrate surface in film early growth period.So And this layer of titanium carbide be it is loose and porous, seriously affect the binding force between diamond coatings and titanium substrate.
In order to promote the film base binding performance of titanium-based diamond coatings, it is essential suitably to pre-process.Pretreatment can be with Substrate surface is cleaned, the forming core site of diamond film is provided, to increase Enhancing Nucleation Density, increases film-substrate cohesion.Sandblasting and super It is common preprocess method that acoustic shock, which is swung, can form a large amount of both macro and micro defect in substrate surface, mention high surface energy, benefit In forming core.Meanwhile the diadust of substrate surface absorption or insertion can become ready-made nucleation of diamond, and diamond film is added Growth course.When ultrasonic vibration pre-processes after using common first sandblasting, in the initial stage of deposition of diamond coatings, titanium It reacts between carbon-containing atmosphere and generates titanium carbide, the process of such a carbonization can make surface topography change while compare Surface area increases, to influence the pretreated treatment effect of ultrasonic vibration, is unfavorable for the forming core of subsequent diamond.
Summary of the invention
Object of the present invention is to coating and substrate binding performance possessed by being prepared for existing titanium-based diamond coatings compared with The problem of difference invents a kind of raising Enhancing Nucleation Density, is promoted and plants brilliant effect, the raising titanium-based diamond coatings for inhibiting titanium carbide to generate Ultrasonic vibration preprocess method after the first carbonization of film base binding performance.One kind is pre-processed based on ultrasonic vibration after being first carbonized, and is improved The method of the binding force of titanium-based diamond coatings,
The technical scheme is that
One kind is based on the pretreated titanium-based diamond coatings binding force Enhancement Method of ultrasonic vibration after being first carbonized, it is characterized in that it is wrapped Include following steps:
Step 1 is polished titanium substrate surface 10 minutes totally using the sand paper of 360 ~ 1000 mesh, then clear using dehydrated alcohol ultrasound It washes 10 minutes, it is preliminary to remove titanium substrate surface oxide layer, the pollutants such as greasy dirt；
Step 2, using sand-blasting machine to titanium substrate surface carry out blasting treatment, further purify substrate surface and obtain have compared with The substrate surface of bigger serface and exhibiting high surface defect；
Step 3 carries out carbonization treatment to substrate surface using chemical vapor depsotition equipment, sends out substrate surface and carbon-containing atmosphere Raw reaction generates titanium carbide, while the generation of titanium carbide occurs honey comb like porous micro- so that substrate surface topography changes Structure；
Substrate after carbonization is placed in diadust acetone suspension progress ultrasonic vibration processing by step 4, substrate with Scraping effect between diadust can make substrate surface a large amount of microdefect occur, while plant crystalline substance, then in dehydrated alcohol Middle ultrasonic cleaning is finally dried up using compressed nitrogen；
Titanium substrate Jing Guo series of preprocessing is placed in chemical vapor depsotition equipment the system for carrying out diamond coatings by step 5 It is standby.
The parameter used when carrying out carbonization treatment to substrate surface using hot-filament chemical vapor deposition equipment are as follows: real It tests the intracavitary base vacuum in initial vacuum and is evacuated to 1Pa hereinafter, to reduce the influence of foreign gas, reaction gas CH4、H2And TMB, C/H is that 1 ~ 6%, B/C is 0 ~ 8000ppm, and heated filament selects tungsten wire, and hot-wire temperature is 2200 ~ 2300 DEG C, and silk bottom is away from 8 ~ 12mm, substrate 750 ~ 850 DEG C of temperature, reaction pressure 1.5KPa, 5 ~ 20min of carbonization time.Other chemical vapor depsotition equipments can also be used to carry out Substrate silicon carbide processing.
For diadust used in the titanium substrate ultrasound pretreatment having a size of 0.2 ~ 1 μm, concentration is 3 ~ 6g gold Hard rock micro mist/100ml acetone, ultrasonic 30 ~ 60min of pretreatment time, dehydrated alcohol are cleaned by ultrasonic the time for 1min, are dried with nitrogen It is spare.
It is described using hot-filament chemical vapor deposition equipment deposition of diamond coatings when the parameter that uses are as follows: in vacuum chamber this Bottom vacuum 1Pa is hereinafter, reaction gas is CH4、H2And it is 0 ~ 8000ppm that TMB, C/H, which are 1 ~ 6%, B/C, heated filament selects tungsten wire, heated filament Temperature is 2200 ~ 2300 DEG C, and silk bottom is away from 8 ~ 12mm, 750 ~ 850 DEG C of underlayer temperature, 0.5 ~ 2KPa of reaction pressure, diamond nucleation 30 ~ 60min of time, later, methane concentration are down to 0.5 ~ 3%, and reaction pressure rises to 1 ~ 4KPa, and diamond coatings grow 6 ~ 12h. Other chemical vapor depsotition equipment deposition of diamond coatings can also be used.
The beneficial effects of the present invention are:
The present invention considerably increases Enhancing Nucleation Density using ultrasonic vibration pretreating process after being first carbonized, and improves the brilliant effect of plant, promotees Into fine and close and thin carburization zone is generated, the film base binding performance of titanium-based diamond coatings is improved.
Present invention process is simple, operation is easy, is at low cost, and coating adhesion can be promoted obviously.
Ultrasonic vibration preprocess method after first carbonization proposed by the present invention is that ultrasonic vibration is located in advance after common first sandblasting On the basis of reason, exchange carbonization and the pretreated sequence of ultrasonic vibration, i.e., first sandblasting is rear to be carbonized, then ultrasonic vibration, to avoid Influence of the variation of surface topography to ultrasonic vibration treatment effect.This method considerably increases Enhancing Nucleation Density, and Enhancing Nucleation Density mentions Film base contact area can be effectively increased by rising, to promote film base binding performance；Improve the brilliant effect of plant, the substrate table after carbonization Face has a large amount of holes of uniform size, can be very good capture diadust；Inhibit the generation of titanium carbide, high forming core One layer of fine and close diamond can be more quickly formed in density, stop the contact of carbon-containing atmosphere and titanium substrate, to inhibit carbonization The generation of titanium.
Detailed description of the invention
Fig. 1 is diamond coatings grain morphology figure of the invention.
Fig. 2 is the substrate surface topography figure after carbonization.
Fig. 3 is the shape appearance figure for being first carbonized and planting brilliant pretreatment backsight bottom surface forming core 10min afterwards.
Fig. 4 is titanium-based diamond coatings sectional view.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
Embodiment 1.
As shown in Figs 1-4.
One kind is pre-processed based on ultrasonic vibration after being first carbonized, the method for improving the binding force of titanium-based diamond coatings, including Following steps:
1. use 2mm thickness titanium sheet, use 360 mesh respectively, 600 mesh, 1000 mesh sand paper to surface carry out it is total polish 10 minutes with Oxide on surface, the pollutants such as greasy dirt are removed, while obtaining even curface, are cleaned by ultrasonic 20min using dehydrated alcohol, into one Step removal metal substrate surface greasy dirt, adsorbate etc..
2. using sand-blasting machine to titanium substrate surface carry out blasting treatment, further purify substrate surface and obtain have compared with The substrate surface of bigger serface and exhibiting high surface defect.
3. carrying out carbonization treatment to substrate surface using hot-filament chemical vapor deposition equipment.The parameter used are as follows: before experiment Base vacuum in vacuum chamber is evacuated to 1Pa hereinafter, to reduce the influence of foreign gas, reaction gas CH4And H2, C/H 3%, Heated filament selects tungsten wire, and hot-wire temperature is 2300 DEG C, and silk bottom is away from 10mm, and 800 DEG C of underlayer temperature, reaction pressure 0.5KPa, when carbonization Between 5min.As shown in Figure 2.
4. the substrate after carbonization is placed in diadust acetone suspension and carries out ultrasonic pretreatment.The gold used Hard rock micro mist is having a size of 1 μm, and concentration is 6g diadust/100ml acetone, ultrasonic pretreatment time 60min, and dehydrated alcohol is super Sound scavenging period is 1min, is dried with nitrogen spare.As shown in Figure 3.
5. the titanium substrate Jing Guo series of preprocessing is placed in hot-filament chemical vapor deposition equipment and carries out diamond coatings Growth.The parameter used are as follows: base vacuum 1Pa in vacuum chamber is hereinafter, reaction gas is CH4And H2, C/H 3%, heated filament choosing With tungsten wire, hot-wire temperature is 2300 DEG C, and silk bottom is away from 10mm, 800 DEG C of underlayer temperature, reaction pressure 0.5KPa, when diamond nucleation Between 60min, later, methane concentration is down to 1.5%, and reaction pressure rises to 1KPa, and diamond coatings grow 8h.Obtained Buddha's warrior attendant Stone coated grains shape appearance figure is as shown in Figure 1, titanium-based diamond coatings sectional view is as shown in Figure 4.
Embodiment 2.
1. using 2mm thickness titanium sheet, 360 mesh, 600 mesh are used respectively, and 1000 mesh sand paper carry out total polish 10 points to surface Clock obtains even curface to remove oxide on surface, the pollutants such as greasy dirt, is cleaned by ultrasonic 20min using dehydrated alcohol, Further remove metal substrate surface greasy dirt, absorption mist etc..
2. using sand-blasting machine to titanium substrate surface carry out blasting treatment, further purify substrate surface and obtain have compared with The substrate surface of bigger serface and exhibiting high surface defect.
3. carrying out carbonization treatment to substrate surface using hot-filament chemical vapor deposition equipment.The parameter used are as follows: before experiment Base vacuum in vacuum chamber is evacuated to 1Pa hereinafter, to reduce the influence of foreign gas, reaction gas CH4、H2And TMB, C/H are 2%, B/C 4000ppm, heated filament select tungsten wire, and hot-wire temperature is 2250 DEG C, and silk bottom is away from 10mm, and 750 DEG C of underlayer temperature, reaction gas Press 1.5KPa, carbonization time 10min.
4. the substrate after carbonization is placed in diadust acetone suspension and carries out ultrasonic pretreatment.The gold used For hard rock micro mist having a size of 0.2 μm, concentration is 3g diadust/100ml acetone, ultrasonic pretreatment time 60min, dehydrated alcohol The ultrasonic cleaning time is 1min, is dried with nitrogen spare.
5. the titanium substrate Jing Guo series of preprocessing is placed in hot-filament chemical vapor deposition equipment and carries out diamond coatings Growth.The parameter used are as follows: base vacuum 1.5Pa in vacuum chamber is hereinafter, reaction gas is CH4、H2And TMB, C/H 2%, B/ C is 4000ppm, and heated filament selects tungsten wire, and hot-wire temperature is 2250 DEG C, and silk bottom is away from 10mm, 750 DEG C of underlayer temperature, reaction pressure 1KPa, diamond nucleation time 60min, later, methane concentration are down to 1%, and reaction pressure rises to 3KPa, diamond coatings growth 12h。
Embodiment 3.
1. using 2mm thickness titanium sheet, 360 mesh, 600 mesh are used respectively, and 1000 mesh sand paper carry out total polish 10 points to surface Clock obtains even curface to remove oxide on surface, the pollutants such as greasy dirt, is cleaned by ultrasonic 20min using dehydrated alcohol, Further remove metal substrate surface greasy dirt, absorption mist etc..
2. using sand-blasting machine to titanium substrate surface carry out blasting treatment, further purify substrate surface and obtain have compared with The substrate surface of bigger serface and exhibiting high surface defect.
3. carrying out carbonization treatment to substrate surface using hot-filament chemical vapor deposition equipment.The parameter used are as follows: before experiment Base vacuum in vacuum chamber is evacuated to 1Pa hereinafter, to reduce the influence of foreign gas, reaction gas CH4、H2And TMB, C/H are 4%, B/C 2000ppm, heated filament select tungsten wire, and hot-wire temperature is 2200 DEG C, and silk bottom is away from 8mm, and 850 DEG C of underlayer temperature, reaction gas Press 1KPa, carbonization time 20min.
4. the substrate after carbonization is placed in diadust acetone suspension and carries out ultrasonic pretreatment.The gold used For hard rock micro mist having a size of 0.5 μm, concentration is 6g diadust/100ml acetone, ultrasonic pretreatment time 30min, dehydrated alcohol The ultrasonic cleaning time is 1min, is dried with nitrogen spare.
5. the titanium substrate Jing Guo series of preprocessing is placed in hot-filament chemical vapor deposition equipment and carries out diamond coatings Growth.The parameter used are as follows: base vacuum 1Pa in vacuum chamber is hereinafter, reaction gas is CH4、H2And TMB, C/H 4%, B/C For 2000ppm, heated filament selects tungsten wire, and hot-wire temperature is 2200 DEG C, and silk bottom is away from 8mm, and 850 DEG C of underlayer temperature, reaction pressure 1KPa, Diamond nucleation time 30min, later, methane concentration are down to 2%, and reaction pressure rises to 2KPa, and diamond coatings grow 10h.
Embodiment 4.
1. using 2mm thickness titanium sheet, 360 mesh, 600 mesh are used respectively, and 1000 mesh sand paper carry out total polish 10 points to surface Clock obtains even curface to remove oxide on surface, the pollutants such as greasy dirt, is cleaned by ultrasonic 10min using dehydrated alcohol, Further remove metal substrate surface greasy dirt, absorption mist etc..
2. using sand-blasting machine to titanium substrate surface carry out blasting treatment, further purify substrate surface and obtain have compared with The substrate surface of bigger serface and exhibiting high surface defect.
3. carrying out carbonization treatment to substrate surface using hot-filament chemical vapor deposition equipment.The parameter used are as follows: before experiment Base vacuum in vacuum chamber is evacuated to 1Pa hereinafter, to reduce the influence of foreign gas, reaction gas CH4、H2And TMB, C/H are 1%, B/C 8000ppm, heated filament select tungsten wire, and hot-wire temperature is 2200 DEG C, and silk bottom is away from 12mm, and 850 DEG C of underlayer temperature, reaction gas Press 1KPa, carbonization time 20min.
4. the substrate after carbonization is placed in diadust acetone suspension and carries out ultrasonic pretreatment.The gold used For hard rock micro mist having a size of 0.5 μm, concentration is 4.5g diadust/100ml acetone, ultrasonic pretreatment time 45min, anhydrous second Alcohol is cleaned by ultrasonic the time for 1min, is dried with nitrogen spare.
5. the titanium substrate Jing Guo series of preprocessing is placed in hot-filament chemical vapor deposition equipment and carries out diamond coatings Growth.The parameter used are as follows: base vacuum 1Pa in vacuum chamber is hereinafter, reaction gas is CH4、H2And TMB, C/H 1%, B/C For 8000ppm, heated filament selects tungsten wire, and hot-wire temperature is 2200 DEG C, and silk bottom is away from 12mm, and 850 DEG C of underlayer temperature, reaction pressure 2KPa, diamond nucleation time 45min, later, methane concentration are down to 3%, and reaction pressure rises to 4KPa, diamond coatings growth 6h。
Embodiment 5.
1. using 2mm thickness titanium sheet, 360 mesh, 600 mesh are used respectively, and 1000 mesh sand paper carry out total polish 10 points to surface Clock obtains even curface to remove oxide on surface, the pollutants such as greasy dirt, is cleaned by ultrasonic 10min using dehydrated alcohol, Further remove metal substrate surface greasy dirt, absorption mist etc..
2. using sand-blasting machine to titanium substrate surface carry out blasting treatment, further purify substrate surface and obtain have compared with The substrate surface of bigger serface and exhibiting high surface defect.
3. carrying out carbonization treatment to substrate surface using hot-filament chemical vapor deposition equipment.The parameter used are as follows: before experiment Base vacuum in vacuum chamber is evacuated to 1Pa hereinafter, to reduce the influence of foreign gas, reaction gas CH4、H2And TMB, C/H are 6%, B/C 8000ppm, heated filament select tungsten wire, and hot-wire temperature is 2200 DEG C, and silk bottom is away from 12mm, and 850 DEG C of underlayer temperature, reaction gas Press 1KPa, carbonization time 20min.
4. the substrate after carbonization is placed in diadust acetone suspension and carries out ultrasonic pretreatment.The gold used For hard rock micro mist having a size of 0.5 μm, concentration is 4.5g diadust/100ml acetone, ultrasonic pretreatment time 45min, anhydrous second Alcohol is cleaned by ultrasonic the time for 1min, is dried with nitrogen spare.
5. the titanium substrate Jing Guo series of preprocessing is placed in hot-filament chemical vapor deposition equipment and carries out diamond coatings Growth.The parameter used are as follows: base vacuum 1Pa in vacuum chamber is hereinafter, reaction gas is CH4、H2And TMB, C/H 6%, B/C For 8000ppm, heated filament selects tungsten wire, and hot-wire temperature is 2200 DEG C, and silk bottom is away from 12mm, and 850 DEG C of underlayer temperature, reaction pressure 2KPa, diamond nucleation time 45min, later, methane concentration are down to 0.5%, and reaction pressure rises to 4KPa, and diamond coatings are raw Long 10h.
Part that the present invention does not relate to is same as the prior art or can be realized by using the prior art.

Claims (4)

1. it is a kind of based on the titanium-based diamond coatings binding force Enhancement Method being ultrasonically treated after carbonization, it is characterized in that it includes following Step:
Step 1 is polished titanium substrate surface 10 minutes totally using the sand paper of 360 ~ 1000 mesh, then clear using dehydrated alcohol ultrasound It is washed till 10 minutes few, preliminary removal titanium substrate surface oxide layer, the pollutants such as greasy dirt；
Step 2, using sand-blasting machine to titanium substrate surface carry out blasting treatment, further purify substrate surface and obtain have compared with The substrate surface of bigger serface and exhibiting high surface defect；
Step 3 carries out carbonization treatment to substrate surface using chemical vapor depsotition equipment, sends out substrate surface and carbon-containing atmosphere Raw reaction generates titanium carbide, while the generation of titanium carbide occurs honey comb like porous micro- so that substrate surface topography changes Structure；
Substrate after carbonization is placed in diadust acetone suspension progress ultrasonic vibration processing by step 4, substrate with Scraping effect between diadust can make substrate surface a large amount of microdefect occur, while plant crystalline substance, then in dehydrated alcohol Middle ultrasonic cleaning is finally dried up using compressed nitrogen；
Titanium substrate Jing Guo series of preprocessing is placed in chemical vapor depsotition equipment the system for carrying out diamond coatings by step 5 It is standby.
2. according to the method described in claim 1, it is characterized in that described uses hot-filament chemical vapor deposition equipment to substrate table Face carries out the parameter used when carbonization treatment are as follows: the intracavitary base vacuum in experiment initial vacuum is evacuated to 1Pa hereinafter, to reduce impurity gas The influence of body, reaction gas CH4、H2And it is 0 ~ 8000ppm that TMB, C/H, which are 1 ~ 6%, B/C, heated filament selects tungsten wire, hot-wire temperature It is 2200 ~ 2300 DEG C, silk bottom is away from 8 ~ 12mm, and 750 ~ 850 DEG C of underlayer temperature, reaction pressure 0.5-1.5KPa, carbonization time 5 ~ 20min；Other chemical vapor depsotition equipments can also be used to carry out substrate silicon carbide processing.
3. according to the method described in claim 1, it is characterized in that titanium substrate ultrasound pre-processes used diadust size It is 0.2 ~ 1 μm, concentration is 3 ~ 6g diadust/100ml acetone, ultrasonic 30 ~ 60min of pretreatment time, dehydrated alcohol ultrasound Scavenging period is 1min, is dried with nitrogen spare.
4. according to the method described in claim 1, it is characterized in that described deposits Buddha's warrior attendant using hot-filament chemical vapor deposition equipment The parameter used when stone coating are as follows: base vacuum 1Pa in vacuum chamber is hereinafter, reaction gas is CH4、H2And TMB, C/H are 1 ~ 6%, B/C is 0 ~ 8000ppm, and heated filament selects tungsten wire, and hot-wire temperature is 2200 ~ 2300 DEG C, silk bottom away from 8 ~ 12mm, underlayer temperature 750 ~ 850 DEG C, 0.5 ~ 2KPa of reaction pressure, 30 ~ 60min of diamond nucleation time, later, methane concentration is down to 0.5 ~ 3%, reaction gas Pressure rises to 1 ~ 4KPa, and diamond coatings grow 6 ~ 12h；Other chemical vapor depsotition equipment deposition of diamond coatings can also be used.
CN201910547130.XA 2019-06-24 2019-06-24 It is a kind of based on the titanium-based diamond coatings binding force Enhancement Method being ultrasonically treated after carbonization Pending CN110129763A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111300275A (en) * 2019-11-28 2020-06-19 张威男 Sand blasting process for titanium metal container
CN114540791A (en) * 2022-03-04 2022-05-27 杭州超然金刚石有限公司 Artificial diamond preparation process and equipment thereof

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CN104233216A (en) * 2014-10-09 2014-12-24 南京航空航天大学 Preparation method of titanium-based boron-doped diamond electrode provided with nano-structure array on surface
CN105256278A (en) * 2015-11-13 2016-01-20 浙江工业大学 Method for preparing diamond film on stainless steel surface

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CN104233216A (en) * 2014-10-09 2014-12-24 南京航空航天大学 Preparation method of titanium-based boron-doped diamond electrode provided with nano-structure array on surface
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111300275A (en) * 2019-11-28 2020-06-19 张威男 Sand blasting process for titanium metal container
CN111300275B (en) * 2019-11-28 2021-09-10 张威男 Sand blasting process for titanium metal container
CN114540791A (en) * 2022-03-04 2022-05-27 杭州超然金刚石有限公司 Artificial diamond preparation process and equipment thereof
CN114540791B (en) * 2022-03-04 2023-05-09 杭州超然金刚石有限公司 Process and equipment for preparing artificial diamond

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Application publication date: 20190816