CN105483643A - Preparation method of nano-diamond layer and nano-diamond blade - Google Patents
Preparation method of nano-diamond layer and nano-diamond blade Download PDFInfo
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- CN105483643A CN105483643A CN201510830744.0A CN201510830744A CN105483643A CN 105483643 A CN105483643 A CN 105483643A CN 201510830744 A CN201510830744 A CN 201510830744A CN 105483643 A CN105483643 A CN 105483643A
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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
- C23C16/22—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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
- B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B2222/00—Materials of tools or workpieces composed of metals, alloys or metal matrices
- B23B2222/28—Details of hard metal, i.e. cemented carbide
Abstract
The invention provides a preparation method of a nano-diamond layer. The preparation method comprises the following steps that a hard alloy matrix is firstly subjected to acid pickling treatment, then cleaned with water and dried, and a clean hard alloy matrix is obtained; the clean hard alloy matrix is put into ultra-nano-diamond suspension liquid to be subjected to ultrasonic cleaning for 10-40 min, and then dried for 10-30 min at the temperature of 80-150 DEG C, a hard alloy pretreatment body is obtained, and the ultra-nano-diamond suspension liquid comprises ultra-nano-diamond particles with the particle size of 4-100 nm; and the nano-diamond layer is formed on the hard alloy pretreatment body through a chemical vapor deposition method. The invention further provides a nano-diamond blade which comprises the nano-diamond layer deposited through the method. The bonding force of the nano-diamond layer prepared through the method and the hard alloy matrix is high, and therefore the nano-diamond blade is higher in precision and longer in service life.
Description
Technical field
The invention belongs to technical field of superhard material, be specifically related to a kind of preparation method and Nano diamond blade of Nano diamond layer.
Background technology
Along with the kind of superhard material gets more and more, and also get more and more as the coated cutting tool of processing cutting industry.Diamond-coated tools is owing to having the highest hardness and the highest thermal conductivity, and extremely low frictional coefficient and thermal expansivity.Make it still to have overwhelming superiority in work material industry, be such as processed with non-ferrous metal, carbon fiber, graphite and ceramic field etc.But along with the requirement of processing industry to working accuracy improves constantly, make general diamond cutter be difficult to meet present situation, desirable finishing tool is that requirement tool surface needs are extremely smooth, enables to improve working accuracy in work material process.
Nano diamond coating cutter, not only maintains the advantage of hardness that block diamond has and thermal conductivity, shows in cutting process to have very high hardness, ensure that the work-ing life of diamond cutter; Also have some characteristics of nano material concurrently, as even curface smooth finish more, Nano diamond is structurally main with SP
3certain reticulated structure that hybrid bond is formed by connecting, ensure that the precision in working angles, has lower surfaceness, lower frictional coefficient, be more suitable for precision work field compared to micron diamond coating.But there is the not strong problem of the bonding force of nanometer or super nano diamond coating and hard alloy substrate in the nanometer adopting existing coating process to prepare or super nano diamond coating, thus making the precision of existing diamond-coated tools good not, work-ing life is shorter.
Summary of the invention
By Given this, necessary preparation method and the Nano diamond blade providing a kind of Nano diamond layer of the present invention, to solve the problem.
For solving the problem, technical scheme provided by the invention is mainly by before the non-depositing nano diamond layer of hard alloy substrate, described hard alloy substrate forms super Nano diamond particle in advance, to increase the nucleation amount of the Nano diamond layer of follow-up formation.Particularly, the invention provides a kind of preparation method of Nano diamond layer, comprise the following steps:
Pickling: first cleanup acid treatment is carried out to hard alloy substrate, more also dry with water cleaning, obtain clean hard alloy substrate;
Ultrasonic cleaning: described clean hard alloy substrate is placed in super nanodiamond suspension and carries out ultrasonic cleaning 10 ~ 40min, then at the temperature of 80 DEG C ~ 150 DEG C, dry 10 ~ 30min, obtain Wimet pre-treatment body, wherein, described super nanodiamond suspension comprises the super Nano diamond particle that particle diameter is 4 ~ 100nm;
Deposition: adopt chemical Vapor deposition process to form Nano diamond layer on described Wimet pre-treatment body.
" super Nano diamond particle " herein refers to that median size is the Nano diamond particle of 4 ~ 100nm." particle diameter " herein mainly refers to the median size of Nano diamond particle.
Based on above-mentioned, described super nanodiamond suspension is 10 by first preparing super Nano diamond numbers of particles concentration
16~ 10
19the dense super nanodiamond suspension of/g, to get again in the high purity water of dense super nanodiamond suspension instillation 10 ~ 50ml described in 2ml and stir and carry out diluting obtaining, wherein, described dense super nanodiamond suspension pH value is at normal temperatures 3 ~ 5, and described high-purity resistivity of water is at more than 15M CM.
The present invention also provides a kind of Nano diamond blade, and it comprises hard alloy substrate and adopts aforesaid method to be deposited on Nano diamond layer on described hard alloy substrate, and the median size of the Nano diamond particle in described Nano diamond layer is 30 ~ 800nm.
Based on above-mentioned, the surperficial arithmetic average roughness (Ra) of described Nano diamond layer is 50 ~ 600nm.
Compared with prior art, the preparation method of Nano diamond layer provided by the invention, mainly by before depositing nano diamond layer, first adopts in described super nanodiamond suspension and carries out ultrasonic cleaning and obtained to hard alloy substrate; Because the particle diameter of the super Nano diamond particle in described super nanodiamond suspension is smaller, hard alloy substrate passes through the ultrasonic cleaning of super nanodiamond suspension, easily at the super Nano diamond particle of the surface adsorption small particle size of this hard alloy substrate; So, the super Nano diamond particle being adsorbed on described carbide surface can as Nano diamond layer crystal core described in subsequent deposition, be conducive to the nucleation of Nano diamond, increase the nucleation amount of Nano diamond, be conducive to the deposition of Nano diamond layer, and then increase the bonding force of Nano diamond layer and hard alloy substrate.Therefore, Nano diamond blade provided by the invention comprises above-mentioned Nano diamond layer can increase the precision of described Nano diamond blade, wear resistance and work-ing life.
Test proves: adopt digital display micro Vickers (VTD512) to do impression test to the Nano diamond layer prepared by method provided by the invention, mode is departed from from diamond film, impression circumferential crack, impression radius three aspect analyze diamond film with the bonding force of substrate, though described Nano diamond layer has Indentation Damage but impression is not obvious and radius is less than 30 μm, impression periphery flawless, imply that the remarkable decline of intrinsic stress and thermal stresses, therefore, Nano diamond layer and the hard alloy substrate prepared by method provided by the invention have stronger bonding force.
In addition, specify, behind 1/2 depth of cut place, knife face weares and teares bandwidth VB as blunt standard, the blunt standard VB=0.4mm of inserted tool for WC-6%wt.Co with international standard ISO.Turning equipment: CK6136I digital controlled lathe, turning material: ZAlSi12, turning speed V=200m/min, amount of feed f=24mm/min, turning degree of depth ap=0.5mm, under abrasion loss VB=0.4mm, the life-span of Nano diamond blade provided by the invention is 300 ~ 500min.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
The invention provides a kind of preparation method of Nano diamond layer, comprise the following steps:
Pickling: first cleanup acid treatment is carried out to hard alloy substrate, more also dry with water cleaning, obtain clean hard alloy substrate;
Ultrasonic cleaning: described clean hard alloy substrate is placed in super nanodiamond suspension and carries out ultrasonic cleaning 10 ~ 40min, then dry 10 ~ 30min at the temperature of 80 DEG C ~ 150 DEG C, obtain Wimet pre-treatment body, wherein, described super nanodiamond suspension comprises the super Nano diamond particle that particle diameter is 4 ~ 100nm;
Deposition: adopt chemical Vapor deposition process to form Nano diamond layer on described Wimet pre-treatment body.
Described acid pickling step is the acid cleaning process adopting existing hard alloy substrate, such as: get the concentrated sulfuric acid solution 10ml that massfraction is 95% ~ 98%, with distilled water diluting to 100ml, described hard alloy substrate is put into sulfuric acid diluent 1 ~ 5min, clean up with distilled water afterwards and drying, obtain described clean hard alloy substrate.Wherein, described hard alloy substrate can be tungsten cobalt alloy, tungsten titanium-cobalt alloy or tungsten titanium tantalum alloy.
In the step of described ultrasonic pickling, described super nanodiamond suspension is 10 by first preparing super Nano diamond numbers of particles concentration
16~ 10
19the dense super nanodiamond suspension of/g, to get again in the high purity water of dense super nanodiamond suspension instillation 10 ~ 50ml described in 2ml and stir and carry out diluting obtaining, wherein, described dense super nanodiamond suspension pH value is at normal temperatures 3 ~ 5, and described high-purity resistivity of water is at more than 15M CM.In this step, why adopting high purity water to dilute described dense super nanodiamond suspension is in order to avoid affecting Nano diamond granular absorption on described clean hard alloy substrate because introducing impurity.
After the step of described ultrasonic pickling, do not need, again with water cleaning, directly to carry out subsequent step.The main purpose of the step of described ultrasonic pickling is to clean described hard alloy substrate further, Nano diamond granular absorption will be surpassed in described clean cemented carbide substrate surfaces, for described in subsequent deposition, Nano diamond layer provides nucleus, be conducive to the nucleation of Nano diamond, increase the nucleation amount of Nano diamond, be conducive to the deposition of Nano diamond layer, and then increase the bonding force of Nano diamond layer and hard alloy substrate.Described super nanodiamond suspension is mainly in order to provide super Nano diamond particle; That is, no matter what the concrete composition of described super nanodiamond suspension is, as long as in described super nanodiamond suspension containing particle diameter be the Nano diamond particle of 4 ~ 100nm, and can stably be adsorbed on hard substrate alloy under ultrasonic effect, just can reach object of the present invention.
The method of ultrasonic cleaning is adopted in described ultrasonic acid pickling step, the super Nano diamond particle in described super nanodiamond suspension can be made to divide equally dispersion, and be formed uniformly on described clean hard alloy substrate, avoid super Nano diamond particle to reunite on the surface of described clean hard alloy substrate.
The step of described deposition adopts existing chemical Vapor deposition process to deposit described Nano diamond layer on described Wimet pre-treatment body.
Test proves: adopt digital display micro Vickers (VTD512) to do impression test to the Nano diamond layer prepared by method provided by the invention, depart from mode from diamond film, diamond film is analyzed in impression circumferential crack, impression radius three aspect and the bonding force of substrate, though described Nano diamond layer has Indentation Damage but impression is not obvious and radius is less than 30 μm, impression periphery flawless, imply that the remarkable decline of intrinsic stress and thermal stresses, therefore, described Nano diamond layer has stronger bonding force with hard alloy substrate.
The present invention also provides a kind of Nano diamond blade, and it comprises hard alloy substrate and adopts aforesaid method to be deposited on Nano diamond layer on described hard alloy substrate, and the median size of the Nano diamond particle in described Nano diamond layer is 30 ~ 800nm.Wherein, the surperficial arithmetic average roughness (Ra) of described Nano diamond layer is 50 ~ 600nm.
Test proves: specify, behind 1/2 depth of cut place, knife face weares and teares bandwidth VB as blunt standard, the blunt standard VB=0.4mm of inserted tool for WC-6%wt.Co with international standard ISO.Turning equipment: CK6136I digital controlled lathe, turning material: ZAlSi12, turning speed V=200m/min, amount of feed f=24mm/min, turning degree of depth ap=0.5mm, under abrasion loss VB=0.4mm, the life-span of described Nano diamond blade is 300 ~ 500min.
Below with specific embodiment, explain further and the present invention is described.
Embodiment 1
The embodiment of the present invention 1 provides a kind of preparation method of Nano diamond layer, comprises the following steps:
Pickling: get the concentrated sulfuric acid solution 10ml that massfraction is 96%, with distilled water diluting to 100ml, puts into sulfuric acid diluent 3min by tungsten cobalt alloy matrix, clean up afterwards and drying, obtain described clean tungsten cobalt alloy matrix with distilled water;
Ultrasonic cleaning: first provide super Nano diamond numbers of particles concentration to be 6 × 10
18the dense super nanodiamond suspension of/g, the median size of the Nano diamond particle in wherein said dense super nanodiamond suspension is 10 ~ 16nm, then stirs and carry out diluting and super nanodiamond suspension after the dilution of concentration needed for obtain in the high purity water getting dense super nanodiamond suspension instillation 25ml described in 2ml; Wherein, described super nanodiamond suspension comprises the Nano diamond particle that particle diameter is 5 ~ 100nm, and described dense super nanodiamond suspension pH value is at normal temperatures 4.5, and described high-purity resistivity of water is at more than 15M CM; Described clean tungsten cobalt alloy matrix is placed in super nanodiamond suspension and carries out ultrasonic cleaning 25min, then dry 20min at the temperature of 115 DEG C, obtains tungsten cobalt alloy pre-treatment body;
Deposition: at temperature is 750 DEG C, with H
2, CH
4for reacting gas source, utilize chemical Vapor deposition process to react 6 hours, described Wimet pre-treatment body forms Nano diamond layer.Wherein, the surfaceness of described Nano diamond layer is 80 ~ 150nm, and the median size of the Nano diamond particle in described Nano diamond layer is 70 ~ 120nm.
Simultaneous test 1
Simultaneous test 1 provides a kind of preparation method of Nano diamond layer, this preparation method is substantially identical with the preparation method that embodiment 1 provides, difference is: simultaneous test 1 does not comprise the step of above-mentioned ultrasonic cleaning, tungsten cobalt alloy matrix, after the step through above-mentioned pickling, directly enters the step of above-mentioned deposition.
Adopt digital display micro Vickers (VTD512) to do impression test to diamond film, analyze the Nano diamond layer of embodiment 1 and simultaneous test 1 and the bonding force of tungsten cobalt alloy matrix from diamond film disengaging mode, impression circumferential crack, impression radius three aspect.The Nano diamond layer obtained by simultaneous test 1 is by after the test of impression instrument, and Nano diamond layer directly comes off, and impression is obviously visible and indentation edge crackle has the gesture expanded, and impression radius reaches 150 μm; Though and the Nano diamond layer obtained by embodiment 1 has Indentation Damage but impression is not obvious and radius is less than 30 μm, impression periphery flawless imply that the remarkable decline of intrinsic stress and thermal stresses.As can be seen here, the preparation method of Nano diamond layer that the embodiment of the present invention 1 provides can significantly improve the bonding force intensity of Nano diamond layer and matrix.
Embodiment 2
The embodiment of the present invention 2 provides a kind of Nano diamond blade, and it comprises tungsten cobalt alloy matrix and adopts the method that provides of embodiment 1 to be deposited on Nano diamond layer on described tungsten cobalt alloy matrix.
Simultaneous test 2
Documents 2 provides a kind of Nano diamond blade, and it method comprising tungsten cobalt alloy matrix and employing simultaneous test 1 is deposited on the Nano diamond layer on described tungsten cobalt alloy matrix.
Specify, behind 1/2 depth of cut place, knife face weares and teares bandwidth VB as blunt standard, the blunt standard VB=0.4mm of inserted tool for WC-6%wt.Co with international standard ISO.Turning equipment: CK6136I digital controlled lathe, turning material: ZAlSi12, turning speed V=200m/min, amount of feed f=24mm/min, the turning degree of depth, ap=0.5mm.Under identical abrasion loss VB=0.4mm, the cutter life that embodiment 2 provides is 450min, and the cutter life that simultaneous test 2 provides is 225min.
Embodiment 3
The embodiment of the present invention 3 provides a kind of preparation method of Nano diamond layer, this preparation method is substantially identical with the preparation method that embodiment 1 provides, difference is: in described ultrasonic cleaning step, the median size of the Nano diamond particle in the described super nanodiamond suspension adopted is 42 ~ 50nm, described clean tungsten cobalt alloy matrix after the ultrasonic cleaning time is 10min, dry 30min at the temperature of 80 DEG C; The surfaceness of the Nano diamond layer finally obtained is 180 ~ 400nm, and the median size of the Nano diamond particle in described Nano diamond layer is 300 ~ 600nm.
The method identical with embodiment 1 is adopted to do impression test to the Nano diamond layer prepared by embodiment 3: though the Nano diamond layer obtained by embodiment 3 has Indentation Damage impression not obvious and radius is less than 70 μm, impression periphery flawless imply that the remarkable decline of intrinsic stress and thermal stresses.
Embodiment 4
The embodiment of the present invention 4 provides a kind of Nano diamond blade, and it comprises tungsten cobalt alloy matrix and adopts the method that provides of embodiment 3 to be deposited on Nano diamond layer on described tungsten cobalt alloy matrix.
The method identical with embodiment 2 is adopted to do cutting test to the Nano diamond layer prepared by embodiment 4: the cutter life that embodiment 4 provides is 400min.
Embodiment 5
The embodiment of the present invention 5 provides a kind of preparation method of Nano diamond layer, and this preparation method is substantially identical with the preparation method that embodiment 1 provides, and difference is: the hard alloy substrate adopted in described acid pickling step is tungsten titanium-cobalt alloy matrix; In described ultrasonic cleaning step, the median size of the Nano diamond particle in the described super nanodiamond suspension adopted is 30 ~ 36nm, described clean tungsten cobalt alloy matrix after the ultrasonic cleaning time is 25min, dry 18min at the temperature of 120 DEG C; The surfaceness of the Nano diamond layer finally obtained is 100 ~ 180nm, and the median size of the Nano diamond particle in described Nano diamond layer is 100 ~ 220nm.
The method identical with embodiment 1 is adopted to do impression test to the Nano diamond layer prepared by embodiment 5: though the Nano diamond layer obtained by embodiment 3 has Indentation Damage impression not obvious and radius is less than 45 μm, impression periphery flawless imply that the remarkable decline of intrinsic stress and thermal stresses.
Embodiment 6
The embodiment of the present invention 6 provides a kind of Nano diamond blade, and it comprises tungsten titanium-cobalt alloy matrix and adopts the method that provides of embodiment 3 to be deposited on Nano diamond layer on described tungsten titanium-cobalt alloy matrix.
The method identical with embodiment 2 is adopted to do cutting test to the Nano diamond layer prepared by embodiment 6: the cutter life that embodiment 6 provides is 430min.
Embodiment 7
The embodiment of the present invention 7 provides a kind of preparation method of Nano diamond layer, this preparation method is substantially identical with the preparation method that embodiment 5 provides, difference is: in described ultrasonic cleaning step, the median size of the Nano diamond particle in the described super nanodiamond suspension adopted is 4.2 ~ 5.0nm, described clean tungsten titanium-cobalt alloy matrix after the ultrasonic cleaning time is 30min, dry 10min at the temperature of 130 DEG C; In described deposition step, the temperature of chemical vapour deposition is 720 DEG C ~ 760 DEG C, and reacting gas source is H
2and C
2h
4, the reaction times is the surfaceness of the Nano diamond layer obtained for 5 hours is 50 ~ 110nm, and the median size of the Nano diamond particle in described Nano diamond layer is 30 ~ 90nm.
The method identical with embodiment 1 is adopted to do impression test to the Nano diamond layer prepared by embodiment 7: though the Nano diamond layer obtained by embodiment 7 has Indentation Damage impression not obvious and radius is less than 50 μm, impression periphery flawless imply that the remarkable decline of intrinsic stress and thermal stresses.
Embodiment 8
The embodiment of the present invention 8 provides a kind of Nano diamond blade, and it comprises tungsten cobalt alloy matrix and adopts the method that provides of embodiment 3 to be deposited on Nano diamond layer on described tungsten cobalt alloy matrix.
The method identical with embodiment 2 is adopted to do cutting test to the Nano diamond layer prepared by embodiment 8: the cutter life that embodiment 8 provides is 500min.
Embodiment 9
The embodiment of the present invention 9 provides a kind of preparation method of Nano diamond layer, this preparation method is substantially identical with the preparation method that embodiment 7 provides, difference is: in described ultrasonic cleaning step, the median size of the Nano diamond particle in the described super nanodiamond suspension adopted is 80 ~ 100nm, described clean tungsten titanium-cobalt alloy matrix after the ultrasonic cleaning time is 20min, dry 10min at the temperature of 130 DEG C; In described deposition step, the temperature of chemical vapour deposition is 720 DEG C ~ 760 DEG C, and reacting gas source is H
2and C
2h
4, the reaction times is the surfaceness of the Nano diamond layer obtained for 5 hours is 350 ~ 600nm, and the median size of the Nano diamond particle in described Nano diamond layer is 550 ~ 800nm.
The method identical with embodiment 1 is adopted to do impression test to the Nano diamond layer prepared by embodiment 9: though the Nano diamond layer obtained by embodiment 9 has Indentation Damage impression not obvious and radius is less than 100 μm, impression periphery flawless imply that the remarkable decline of intrinsic stress and thermal stresses.
Embodiment 10
The embodiment of the present invention 10 provides a kind of Nano diamond blade, and it comprises tungsten cobalt alloy matrix and adopts the method that provides of embodiment 3 to be deposited on Nano diamond layer on described tungsten cobalt alloy matrix.
The method identical with embodiment 2 is adopted to do cutting test to the Nano diamond layer prepared by embodiment 10: the cutter life that embodiment 10 provides is 300min.
Therefore, the Nano diamond layer that the embodiment of the present invention provides and hard alloy substrate have stronger bonding force, described Nano diamond blade has higher precision and stronger work-ing life, mainly because at employing chemical Vapor deposition process on hard alloy substrate between depositing nano diamond layer, super Nano diamond particle has been adsorbed in advance on hard alloy substrate, nucleus is provided for subsequent reactions generates described Nano diamond layer, be convenient to growth in situ Nano diamond on described super Nano diamond particle, with the precision of the bonding force and Nano diamond blade that increase described Nano diamond layer and work-ing life.In other words, no matter use which kind of reacting gas source, great temperature of reaction during follow-up employing chemical vapor deposition Nano diamond layer, as long as adopt super Nano diamond particle suspension liquid process hard alloy substrate in advance, object of the present invention can be reached.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request of the present invention protection.
Claims (4)
1. a preparation method for Nano diamond layer, comprises the following steps:
Pickling: first cleanup acid treatment is carried out to hard alloy substrate, more also dry with water cleaning, obtain clean hard alloy substrate;
Ultrasonic cleaning: described clean hard alloy substrate is placed in super nanodiamond suspension and carries out ultrasonic cleaning 10 ~ 40min, then at the temperature of 80 DEG C ~ 150 DEG C, dry 10 ~ 30min, obtain Wimet pre-treatment body, wherein, described super nanodiamond suspension comprises the super Nano diamond particle that particle diameter is 4 ~ 100nm;
Deposition: adopt chemical Vapor deposition process to form Nano diamond layer on described Wimet pre-treatment body.
2. the preparation method of Nano diamond layer according to claim 1, is characterized in that: described super nanodiamond suspension is 10 by first preparing super Nano diamond numbers of particles concentration
16~ 10
19the dense super nanodiamond suspension of/g, to get again in the high purity water of dense super nanodiamond suspension instillation 10 ~ 50ml described in 2ml and stir and carry out diluting obtaining, wherein, described dense super nanodiamond suspension pH value is at normal temperatures 3 ~ 5, and described high-purity resistivity of water is at more than 15M CM.
3. a Nano diamond blade, it comprises hard alloy substrate and is deposited on the Nano diamond layer on described hard alloy substrate, it is characterized in that: described Nano diamond layer is prepared by the preparation method of the Nano diamond layer described in claim 1 or 2, and the median size of the Nano diamond particle in described Nano diamond layer is 30 ~ 800nm.
4. Nano diamond blade according to claim 3, is characterized in that: the surperficial arithmetic average roughness of described Nano diamond layer is 50 ~ 600nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591799A (en) * | 2016-12-28 | 2017-04-26 | 富耐克超硬材料股份有限公司 | Preparation method of diamond coating layer and diamond coating layer blade |
| CN108149219A (en) * | 2017-12-14 | 2018-06-12 | 富耐克超硬材料股份有限公司 | A kind of diamond composite coating cutter and preparation method thereof |
| WO2018176217A1 (en) * | 2017-03-28 | 2018-10-04 | 深圳先进技术研究院 | Method of preparing high-density diamond thin film |
| CN110387534A (en) * | 2019-09-05 | 2019-10-29 | 蓬莱市超硬复合材料有限公司 | A kind of preparation method of nano diamond coating cemented carbide material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220462A (en) * | 2008-01-25 | 2008-07-16 | 南京航空航天大学 | Gradient method preprocessing technique for depositing CVD diamond film on hard metal surface |
| CN101830733A (en) * | 2009-03-13 | 2010-09-15 | 王兵 | Method for preparing ultra nanometer diamond coating of ceramic valve core |
-
2015
- 2015-11-25 CN CN201510830744.0A patent/CN105483643B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220462A (en) * | 2008-01-25 | 2008-07-16 | 南京航空航天大学 | Gradient method preprocessing technique for depositing CVD diamond film on hard metal surface |
| CN101830733A (en) * | 2009-03-13 | 2010-09-15 | 王兵 | Method for preparing ultra nanometer diamond coating of ceramic valve core |
Non-Patent Citations (2)
| Title |
|---|
| A. KROMKA等: "Early stage of diamond growth at low temperature", 《DIAMOND & RELATED MATERIALS》 * |
| 薛海鹏: "纳米金刚石膜的晶粒生长控制及其刀具涂层应用的基础研究", 《中国优秀硕士学位论文全文数据库（电子期刊）》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591799A (en) * | 2016-12-28 | 2017-04-26 | 富耐克超硬材料股份有限公司 | Preparation method of diamond coating layer and diamond coating layer blade |
| CN106591799B (en) * | 2016-12-28 | 2019-02-22 | 富耐克超硬材料股份有限公司 | The preparation method and diamond coatings blade of diamond coatings |
| WO2018176217A1 (en) * | 2017-03-28 | 2018-10-04 | 深圳先进技术研究院 | Method of preparing high-density diamond thin film |
| CN108149219A (en) * | 2017-12-14 | 2018-06-12 | 富耐克超硬材料股份有限公司 | A kind of diamond composite coating cutter and preparation method thereof |
| CN110387534A (en) * | 2019-09-05 | 2019-10-29 | 蓬莱市超硬复合材料有限公司 | A kind of preparation method of nano diamond coating cemented carbide material |
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