CN109972115A - Hard alloy cutter and preparation method thereof with micro-nano diamond coatings - Google Patents

Hard alloy cutter and preparation method thereof with micro-nano diamond coatings Download PDF

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CN109972115A
CN109972115A CN201711468369.5A CN201711468369A CN109972115A CN 109972115 A CN109972115 A CN 109972115A CN 201711468369 A CN201711468369 A CN 201711468369A CN 109972115 A CN109972115 A CN 109972115A
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hard alloy
alloy cutter
micro
nano diamond
preparation
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CN109972115B (en
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唐永炳
张松全
王陶
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Shenzhen Institute of Advanced Technology of CAS
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Shenzhen Institute of Advanced Technology of CAS
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02Pretreatment of the material to be coated
    • C23C16/0227Pretreatment of the material to be coated by cleaning or etching
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical 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
    • C23C16/26Deposition of carbon only
    • C23C16/27Diamond only
    • C23C16/271Diamond only using hot filaments
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56After-treatment

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The present invention provides a kind of hard alloy cutter and preparation method thereof with micro-nano diamond coatings, it is related to hard alloy cutter processing and manufacturing field, the preparation method of the hard alloy cutter with micro-nano diamond coatings, the following steps are included: preparing micron diamond coating in carbide tool surface, nano diamond coating is prepared on the surface layer of the micron diamond coating by etching later, obtain the hard alloy cutter with micro-nano diamond coatings, with alleviate the micro-nano diamond coatings obtained using the processing method of the prior art it is low with hard alloy cutter bond strength caused by the shorter technical problem of hard alloy cutter service life, the low nano diamond coating surface accuracy obtained using the processing method of the prior art and hardness can be alleviated simultaneously and the problem of wearability weakens, reach delay hard The effect of alloy cutter service life.

Description

Hard alloy cutter and preparation method thereof with micro-nano diamond coatings
Technical field
The present invention relates to hard alloy cutter processing and manufacturing technologies, have micro-nano diamond more particularly, to one kind Hard alloy cutter of coating and preparation method thereof.
Background technique
Diamond coatings are excellent such as high rigidity, high elastic modulus, good wearability due to good mechanical property Different corrosion resistance and thermoelectricity conductance etc. are widely used in the superhard protective coating of hard alloy cutter (such as lathe tool, milling cutter), To extend the overall processing service life of cutter.
At present mainly in one layer of carbide surface deposition growing certain thickness micron diamond coating in industrial application, Extend the service life of hard alloy cutter.It is subsequent also to need to adding since the surface roughness of micron diamond coating is higher Work workpiece surface is processed by shot blasting.Current Improving Measurements use nano diamond coating to be improved substantially, but due to Bond strength between the limitation of nano diamond coating performance itself, with hard alloy cutter matrix is weak, reduces the service life. For now, main by way of single layer nano diamond coating, composite diamond coating (micron-nanometer composite coating) To realize the surface accuracy for reducing diamond coatings surface roughness and improving workpieces processing.
Single layer nano diamond coating is directly in one layer of carbide tool surface deposition growing certain thick nanometer Diamond.Due to the limitation of existing preparation process and production equipment, prepared nano coating has weaker coating-Hard Alloy cutter bond strength, and its hardness and wearability are below micron diamond.The preparation method of entitled nano-diamond layer And in the patent of Nano diamond blade (105483643 A of CN), using chemical vapour deposition technique in hard alloy cutter matrix One layer of nano diamond coating of upper deposition growing, although improving coating surface precision, due to nano diamond coating with The bond strength of hard alloy cutter matrix is lower, and then can reduce the service life of hard alloy cutter.
And currently used micron-nanometer composite diamond coating is first high-quality in one layer of carbide tool surface growth Micron diamond coating is measured, then one layer of nano coating of growth in situ on micron diamond coating.This method although certain journey The bond strength of Bulk coat and hard alloy cutter is improved on degree, but equally introduces micron diamond coating and nanometer The problem of diamond coatings bed boundary bond strength, while also there is no alleviate the Nano diamond due to caused by deposition growing The problem of coating hardness and wearability weaken.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of preparation of hard alloy cutter with micro-nano diamond coatings Method, to alleviate the micro-nano diamond coatings obtained using the processing method of the prior art and hard alloy cutter bond strength The shorter technical problem of hard alloy cutter service life caused by low, while the processing method using the prior art can be alleviated The problem of obtained nano diamond coating surface accuracy is low and hardness and wearability weaken.
The second object of the present invention is to provide a kind of hard alloy cutter with micro-nano diamond coatings have table The advantages of face precision height and long service life.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A kind of preparation method of the hard alloy cutter with micro-nano diamond coatings, comprising the following steps:
Micron diamond coating is prepared in carbide tool surface, later by etching in the micron diamond coating Surface layer prepare nano diamond coating, obtain the hard alloy cutter with micro-nano diamond coatings.
Further, first hard alloy cutter is pre-processed, then prepares micron in carbide tool surface again Diamond coatings.
Further, the pretreatment includes the steps that carrying out chemical etching processing to the surface of hard alloy cutter.
Further, chemical etching processing is carried out again after carrying out blasting treatment to the surface of the hard alloy cutter;It can Hard alloy cutter is first cleaned up after blasting treatment and carries out chemical etching processing again by selection of land.
Further, the step of chemical etching includes: and is first performed etching to be performed etching with acid solution again with aqueous slkali.
Further, the aqueous slkali includes K3[Fe(CN)]6, KOH and water composition aqueous slkali;Optionally, the K3 [Fe(CN)]6, KOH and water mass ratio be (1~2): (1~2): 10;Optionally, the acid solution includes H2SO4And H2O2Group At acid solution;Optionally, the H2SO4And H2O2Volume ratio be (1~2): 10.
Further, the step of chemical etching includes: that hard alloy cutter is placed in K3[Fe(CN)]6, KOH and water It is performed etching in the aqueous slkali of composition, removes the aqueous slkali of carbide tool surface later, then be placed in H2SO4And H2O2Composition Acid solution in perform etching.
Further, the preparation method further includes carrying out by chemical etching treated carbide tool surface Pre- the step of planting crystal seed.
Further, the step of pre- plant crystal seed includes: that treated that hard alloy cutter is placed in gold by chemical etching It is ultrasonically treated in emery suspension.
Further, the concentration of the bortz powder suspension are as follows: 2~5wt%.
Further, the micron diamond coating being prepared with a thickness of 1.5-3 microns.
Further, the method for preparing micron diamond coating includes: to prepare micron diamond with chemical vapour deposition technique Coating.
Further, it includes: methane volumetric that the chemical vapour deposition technique, which prepares the technological parameter of micron diamond coating, Score is 2%-5%, air pressure 0.8-2.5kPa, 1800-2200 DEG C of temperature range, the temperature of hard alloy cutter when processing Range is 600-650 DEG C, and the processing time is 1-2.5h;Optimizing technology parameters are as follows: methane volumetric score is 3%-4%, and air pressure is 1.2-2kPa, 1900-2100 DEG C of temperature range, the temperature range of hard alloy cutter is 610-640 DEG C when processing, handles the time For 1.2-2.2h.
Further, the etching includes plasma etching.
Further, it includes: gas pressure in vacuum that using plasma etching, which prepares the technological parameter of nano diamond coating, The temperature range of hard alloy cutter is 600-650 DEG C, handles when range 1.5-2kPa, 2000-2200 DEG C of filament temperature, processing Time 10-30min, optimizing technology parameters are as follows: gas pressure in vacuum range 1.6-1.9kPa, 2000-2200 DEG C of filament temperature, processing When hard alloy cutter temperature range be 610-640 DEG C, processing time 15-25min, reaction gas is hydrogen.
A kind of hard alloy cutter with micro-nano diamond coatings, according to above-mentioned with micro-nano diamond coatings The preparation method of hard alloy cutter is prepared.
Compared with the prior art, the invention has the following beneficial effects:
The present invention prepares one layer of certain thickness micron diamond coating in carbide tool surface by first, then passes through Etching prepares nano diamond coating in the surface layer of micron diamond coating, to obtain micro-nano diamond coatings.This Sample, which both ensure that, has stronger bond strength between micro-nano diamond coatings and the matrix of hard alloy cutter, in turn ensure micro- Nano diamond coating has lower surface roughness and higher surface accuracy.It can be to various height using the preparation method The hard alloy cutter of hardened material and composite material carries out Precision Machining, and can be reached simultaneously using the preparation method and be mentioned The purpose of high hard alloy cutter service life and machining accuracy, effectively reduces processing cost.
The hard alloy cutter with micron diamond coating obtained using preparation method provided by the invention, hardness For 95 ± 3GPa, Young's modulus is that its coefficient of friction is about 0.08 ± 0.005 under 1139.05 ± 362,10N load.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the surface topography map of the micro-nano diamond coatings for the carbide tool surface that embodiment 1 provides;
Fig. 2 is the friction system that the hard alloy cutter that embodiment 1 provides tests micro-nano diamond coatings under 10N load Number figure.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is The conventional products that can be obtained by commercially available purchase.
One aspect of the present invention provides a kind of preparation side of hard alloy cutter with micro-nano diamond coatings Method, comprising the following steps:
Micron diamond coating is prepared in carbide tool surface, later by etching in the micron diamond coating Surface layer prepare nano diamond coating, obtain the hard alloy cutter with micro-nano diamond coatings.
The present invention prepares one layer of certain thickness micron diamond coating in carbide tool surface by first, then passes through Etching prepares nano diamond coating in the surface layer of micron diamond coating, to obtain micro-nano diamond coatings.This Sample, which both ensure that, has stronger bond strength between micro-nano diamond coatings and the matrix of hard alloy cutter, in turn ensure micro- Nano diamond coating has lower surface roughness and higher surface accuracy.It can be to various height using the preparation method The hard alloy cutter of hardened material and composite material carries out Precision Machining, and can be reached simultaneously using the preparation method and be mentioned The purpose of high hard alloy cutter service life and machining accuracy, effectively reduces processing cost.
Micro-nano diamond coatings in the present invention are that micron diamond coating is answered with what nano diamond coating formed Close coating.
Hard alloy cutter in the present invention includes fluted drill, reamer, boring cutter, rose cutter, metal saw, taper milling Knife, indexable slotting cutter, indexable face milling cutter, indexable dovetail cutter and indexable three face sword etc..
As a preferred embodiment of the present invention, first hard alloy cutter is pre-processed, then again in hard alloy Tool surface prepares micron diamond coating.Hard alloy cutter is pre-processed, micro-nano diamond coatings can be improved With the bond strength of hard alloy cutter.
As a preferred embodiment of the present invention, the pretreatment includes carrying out chemical quarter to the surface of hard alloy cutter The step of erosion processing.It is handled by chemical etching, to process the defect generated conducive to diamond in carbide tool surface Position is conducive to subsequent diamond nucleation.
As a preferred embodiment of the present invention, first to the surface of the hard alloy cutter carry out after blasting treatment again into The processing of row chemical etching.Rough grinding processing can be carried out to carbide tool surface using blasting treatment, remove tool surface Grease etc., handled convenient for subsequent chemical etching.
As a preferred embodiment of the present invention, first use acetone and/or alcohol by hard alloy cutter after blasting treatment It cleans up and carries out chemical etching processing again.Carbide tool surface can be removed by carrying out cleaning with acetone and/or alcohol Dirt.
As a preferred embodiment of the present invention, the step of chemical etching includes: and is first performed etching again with aqueous slkali It is performed etching with acid solution.Processing is performed etching to carbide tool surface using aqueous slkali, so that hard alloy cutter table Face reaches roughening effect;It is performed etching later using acid to remove the cobalt Co of carbide tool surface, to prevent Co from destroying gold The surface bonding strength of hard rock coating and hard alloy cutter.
As a preferred embodiment of the present invention, the aqueous slkali includes K3[Fe(CN)]6, KOH and water composition alkali soluble Liquid;Optionally, the K3[Fe(CN)]6, KOH and water mass ratio be (1~2): (1~2): 10;Optionally, the acid solution Including H2SO4And H2O2The acid solution of composition;Optionally, the H2SO4And H2O2Volume ratio be (1~2): 10.Optionally, institute The step of stating chemical etching includes: that hard alloy cutter is placed in K3[Fe(CN)]6, KOH and water composition aqueous slkali in carry out Etching, removes the aqueous slkali of carbide tool surface later, then is placed in H2SO4And H2O2It is performed etching in the acid solution of composition. By the concentration of the concentration and acid solution of preferred aqueous slkali and acid solution and aqueous slkali, carbide tool surface can be made Pattern is easier to combine with diamond coatings.
As a preferred embodiment of the present invention, the preparation method further includes by chemical etching treated hard Alloy cutter surface carries out pre- the step of planting crystal seed.Nucleating point can be formed in carbide tool surface by planting crystal seed in advance, Be conducive to the nucleating growth of diamond coatings.
As a preferred embodiment of the present invention, the step of pre- plant crystal seed includes: that treated is hard by chemical etching Matter alloy cutter is placed in bortz powder suspension and is ultrasonically treated.Optionally, the concentration of the bortz powder suspension are as follows: 2~5wt%.
Wherein, ultrasonication is that diamond particles is allowed to collide tool surface by ultrasound, and tool surface is allowed to generate one A little subtle defects, and some diamond particles are embedded into tool surface.Bortz powder suspension is typical but non-limiting Concentration is for example are as follows: 2wt%, 3wt%, 4wt% or 5wt%.
As a preferred embodiment of the present invention, the micron diamond coating being prepared with a thickness of 1.5-3 microns.? In above-mentioned preferred embodiment, the typical but non-limiting thickness of micron diamond coating is for example are as follows: 1.5 microns, 2 microns, 2.5 microns or 3 microns.
As a preferred embodiment of the present invention, the method for preparing micron diamond coating includes: to use chemical vapor deposition Method prepares micron diamond coating.Micron diamond coating is prepared using vapour deposition process, traditional equipment is can use and carries out Processing reduces manufacturing cost and is easily achieved.
As a preferred embodiment of the present invention, the chemical vapour deposition technique prepares the technique ginseng of micron diamond coating It is 2%-5%, air pressure 0.8-2.5kPa that number, which includes: methane volumetric score, 1800-2200 DEG C of temperature range, hard when processing The temperature range of alloy cutter is 600-650 DEG C, and the processing time is 1-2.5h;Optimizing technology parameters are as follows: methane volumetric score is 3%-4%, air pressure 1.2-2kPa, 1900-2100 DEG C of temperature range, the temperature range of hard alloy cutter is 610- when processing 640 DEG C, the processing time is 1.2-2.2h.
As a preferred embodiment of the present invention, the etching includes plasma etching.It is obtained using plasma etching Nano diamond coating structure more evenly, surface accuracy is higher.
As a preferred embodiment of the present invention, using plasma etching prepares the technological parameter of nano diamond coating The temperature range of hard alloy cutter when including: gas pressure in vacuum range 1.5-2kPa, 2000-2200 DEG C of filament temperature, processing For 600-650 DEG C, processing time 10-30min, optimizing technology parameters are as follows: gas pressure in vacuum range 1.6-1.9kPa, filament temperature The temperature range of hard alloy cutter is 610-640 DEG C, handles time 15-25min, reaction gas when 2000-2200 DEG C, processing For hydrogen.
In obtained micro-nano diamond coatings using the preparation of above-mentioned preferred embodiment, the micron diamond coating The size of middle diamond particles is 1-1.5 microns, and the size of diamond particles is received in the nano diamond coating for 10-100 Rice.
Another aspect of the present invention provides a kind of hard alloy cutter with micro-nano diamond coatings, according to upper The preparation method for stating the hard alloy cutter with micro-nano diamond coatings is prepared.
The hard alloy cutter with micron diamond coating obtained using preparation method provided by the invention, hardness For 95 ± 3GPa, Young's modulus is that its coefficient of friction is about 0.08 ± 0.005 under 1139.05 ± 362,10N load.
Below in conjunction with embodiment and comparative example, the present invention will be further described in detail.
Embodiment 1
The present embodiment is a kind of hard alloy cutter with micro-nano diamond coatings, and preparation method includes following step It is rapid:
Step a): blasting treatment: the YG6 indexable face milling cutter sold using on domestic market first uses white fused alumina as matrix Wet abrasive blasting processing is carried out to matrix, pressure when blasting treatment is 200kPa, and grit size is 800 mesh, after blasting treatment Hard alloy cutter-indexable face milling cutter is placed in the mixed solution of acetone and alcohol and is cleaned by ultrasonic 15min;
Step b): hard alloy cutter of the surface clean after dry chemical etching processing: is statically placed in K3[Fe(CN)]6、 10min is stood in the Murakami aqueous slkali of KOH and water composition, wherein K3[Fe(CN)]6, KOH and water mass ratio be 1:1: 10, then be respectively placed in deionized water and ethanol solution and be cleaned by ultrasonic 10min, remove remaining lye and surface adhesion Object;Hard alloy cutter is statically placed in H later2SO4And H2O210s in the acid solution of composition, wherein H2SO4And H2O2Volume ratio For 1:10, be rinsed with water be placed on be cleaned by ultrasonic 20min in dehydrated alcohol after dried up with argon gas;
Step c): micron diamond coating is prepared: using hot filament CVD, using hydrogen and methane as reaction gas Body deposits micron diamond coating, process conditions when hot-wire chemical gas-phase deposition are as follows: the total gas volume of volume Zhan of methane 5%, gas pressure in vacuum 2kPa, filament temperature are 2200 DEG C, and the temperature of hard alloy cutter is 650 DEG C, and the processing time is 2.5h, the micron diamond coating being prepared by above-mentioned technique with a thickness of 3 microns;
Step d): nano diamond coating is prepared: using in-situ plasma lithographic method in micron diamond coating Prepare nano diamond coating, the process conditions of plasma etching in surface layer are as follows: reaction gas is that purity is greater than 99.999% High-purity hydrogen, gas pressure in vacuum 2kPa, filament temperature is 2200 DEG C, and the temperature of hard alloy cutter is 650 when processing DEG C, the processing time is 30min, and the nano particle size after processing in gained nano diamond coating is about 80nm.
Embodiment 2
The present embodiment is a kind of hard alloy cutter with micro-nano diamond coatings, and preparation method includes following step It is rapid:
Step a): chemical etching processing: the YG6 indexable face milling cutter sold using on domestic market is as matrix, by surface Hard alloy cutter after cleaning-drying is statically placed in K3[Fe(CN)]6, KOH and water composition Murakami aqueous slkali in stand 8min, wherein K3[Fe(CN)]6, KOH and water mass ratio be 2:1:10, then be respectively placed in deionized water and ethanol solution Middle ultrasonic cleaning 10min removes remaining lye and surface adhesion object;Hard alloy cutter is statically placed in H later2SO4And H2O2 10s in the acid solution of composition, wherein H2SO4And H2O2Volume ratio be 2:10, be rinsed with water that be placed in dehydrated alcohol ultrasound clear It is dried up after washing 20min with argon gas;
Step b): micron diamond coating is prepared: using hot filament CVD, using hydrogen and methane as reaction gas Body deposits micron diamond coating, process conditions when hot-wire chemical gas-phase deposition are as follows: the total gas volume of volume Zhan of methane 3%, gas pressure in vacuum 2kPa, filament temperature are 2000 DEG C, and the temperature of hard alloy cutter is 650 DEG C, and the processing time is 2.5h, the micron diamond coating being prepared by above-mentioned technique with a thickness of 3 microns;
Step c): nano diamond coating is prepared: using in-situ plasma lithographic method in micron diamond coating Prepare nano diamond coating, the process conditions of plasma etching in surface layer are as follows: reaction gas is that purity is greater than 99.999% High-purity hydrogen, gas pressure in vacuum 1.9kPa, filament temperature is 2000 DEG C, and the temperature of hard alloy cutter is 640 when processing DEG C, the processing time is 20min, and the nano particle size after processing in gained nano diamond coating is about 80nm.
Embodiment 3
The present embodiment is a kind of hard alloy cutter with micro-nano diamond coatings, and preparation method includes following step It is rapid:
Step a): pretreatment: the YG6 indexable face milling cutter sold using on domestic market is as matrix, by carbide cutter tool Tool-indexable face milling cutter, which is placed in the mixed solution of acetone and alcohol, is cleaned by ultrasonic 15min;
Step b): hard alloy cutter of the surface clean after dry chemical etching processing: is statically placed in K3[Fe(CN)]6、 10min is stood in the Murakami aqueous slkali of KOH and water composition, wherein K3[Fe(CN)]6, KOH and water mass ratio be 1:2: 10, then be respectively placed in deionized water and ethanol solution and be cleaned by ultrasonic 10min, remove remaining lye and surface adhesion Object;Hard alloy cutter is statically placed in H later2SO4And H2O210s in the acid solution of composition, wherein H2SO4And H2O2Volume ratio For 1.5:10, be rinsed with water be placed on be cleaned by ultrasonic 20min in dehydrated alcohol after dried up with argon gas;
Step c): micron diamond coating is prepared: using hot filament CVD, using hydrogen and methane as reaction gas Body deposits micron diamond coating, process conditions when hot-wire chemical gas-phase deposition are as follows: the total gas volume of volume Zhan of methane 4%, gas pressure in vacuum 0.8kPa, filament temperature are 2200 DEG C, and the temperature of hard alloy cutter is 600 DEG C, and the processing time is 2.5h, the micron diamond coating being prepared by above-mentioned technique with a thickness of 2 microns;
Step d): nano diamond coating is prepared: using in-situ plasma lithographic method in micron diamond coating Prepare nano diamond coating, the process conditions of plasma etching in surface layer are as follows: reaction gas is that purity is greater than 99.999% High-purity hydrogen, gas pressure in vacuum 1.6kPa, filament temperature is 2100 DEG C, and the temperature of hard alloy cutter is 600 when processing DEG C, the processing time is 10min, and the nano particle size after processing in gained nano diamond coating is about 10nm.
Embodiment 4
The present embodiment is a kind of hard alloy cutter with micro-nano diamond coatings, and preparation method includes following step It is rapid:
Step a): blasting treatment: the YG6 indexable face milling cutter sold using on domestic market first uses white fused alumina as matrix Wet abrasive blasting processing is carried out to matrix, pressure when blasting treatment is 180kPa, and grit size is 1000 mesh, and blasting treatment terminates Hard alloy cutter-indexable face milling cutter is placed in afterwards in the mixed solution of acetone and alcohol and is cleaned by ultrasonic 10min;
Step b): hard alloy cutter of the surface clean after dry chemical etching processing: is statically placed in K3[Fe(CN)]6、 15min is stood in the Murakami aqueous slkali of KOH and water composition, wherein K3[Fe(CN)]6, KOH and water mass ratio be 2:2: 10, then be respectively placed in deionized water and ethanol solution and be cleaned by ultrasonic 8min, remove remaining lye and surface adhesion object; Hard alloy cutter is statically placed in H later2SO4And H2O220s in the acid solution of composition, wherein H2SO4And H2O2Volume ratio be 1: 10, be rinsed with water be placed in dehydrated alcohol be cleaned by ultrasonic 15min after dried up with argon gas;
Step c): pre- to plant crystal seed processing: by chemical etching, treated that hard alloy cutter is placed in the gold that concentration is 2wt% 30min is ultrasonically treated in emery suspension;
Step d): micron diamond coating is prepared: using hot filament CVD, using hydrogen and methane as reaction gas Body deposits micron diamond coating, process conditions when hot-wire chemical gas-phase deposition are as follows: the total gas volume of volume Zhan of methane 2%, gas pressure in vacuum 1.5kPa, filament temperature are 1800 DEG C, and the temperature of hard alloy cutter is 620 DEG C, and the processing time is 1.5h, the micron diamond coating being prepared by above-mentioned technique with a thickness of 3 microns;
Step e): nano diamond coating is prepared: using in-situ plasma lithographic method in micron diamond coating Prepare nano diamond coating, the process conditions of plasma etching in surface layer are as follows: reaction gas is that purity is greater than 99.999% High-purity hydrogen, gas pressure in vacuum 1.5kPa, filament temperature is 2100 DEG C, and the temperature of hard alloy cutter is 640 when processing DEG C, the processing time is 25min, and the nano particle size after processing in gained nano diamond coating is about 90nm.
Comparative example 1
This comparative example is a kind of hard alloy cutter with micro-nano diamond coatings, preparation method are as follows: directly exist The certain thick Nano diamond of hard alloy cutter-one layer of indexable face milling cutter surface deposition growing.
Comparative example 2
This comparative example is a kind of hard alloy cutter with micro-nano diamond coatings, preparation method are as follows: first hard Matter alloy cutter-indexable face milling cutter surface grows one layer of high quality micron diamond coating, then in micron diamond coating One layer of nano coating of upper growth in situ.
Comparative test:
To the hardness, Young's modulus and coefficient of friction of the coating of the hard alloy cutter in embodiment 1-4 and comparative example 1-2 It is tested for the property, also, cutting polishing is carried out to identical substance with the hard alloy cutter in each embodiment and comparative example Test, the service life of hard alloy cutter, every test result are listed in table 1 when record damages.Wherein, coefficient of friction be The coefficient of friction tested under the action of 10N power.
The performance test results of each embodiment and comparative example of table 1
From table 1 it follows that the hardness of the micro-nano diamond coatings in embodiment 1-4 will be much higher than 1 He of comparative example 2, also, the service life index of the hard alloy cutter in embodiment 1-4 is also much higher than comparative example 1 and 2, illustrates using this hair The hard alloy cutter that the preparation method of bright offer is prepared, the combination between micro-nano diamond coatings and hard alloy cutter Intensity will be got well.
In addition, the service life index of the hard alloy cutter in embodiment 1 and 4 is higher than embodiment 2 and 3, illustrate pre- Sandblasting in treatment process can improve the bond strength between micro-nano diamond coatings and hard alloy cutter, to improve hard The access times of alloy cutter.
Compared with Example 4, the service life in embodiment 4 illustrates to plant at crystal seed in advance embodiment 1 also above embodiment 1 Science and engineering skill will increase the bond strength between micro-nano diamond coatings and hard alloy cutter, to provide service life.
In conclusion the hard alloy cutter being prepared using preparation method provided by the present invention, micro-nano gold The surface of hard rock coating and hard alloy cutter has excellent bond strength, while micro-nano diamond coatings are with higher Surface hardness and extremely low surface roughness, coefficient of friction are lower than 0.1, therefore, are obtained using preparation method provided by the invention The hard alloy cutter with micro-nano diamond coatings integrate longer service life and higher precision, have pole The strong market competitiveness.
In preparation method provided by the invention, simple process can be completed processing and manufacturing using conventional equipment, be conducive to save About processing cost.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims Including belonging to all such changes and modifications in the scope of the invention.

Claims (10)

1. a kind of preparation method of the hard alloy cutter with micro-nano diamond coatings, which is characterized in that including following step It is rapid:
Micron diamond coating is prepared in carbide tool surface, later by etching the table in the micron diamond coating Layer prepares nano diamond coating, obtains the hard alloy cutter with micro-nano diamond coatings.
2. the preparation method of the hard alloy cutter according to claim 1 with micro-nano diamond coatings, feature It is, first hard alloy cutter is pre-processed, then prepares micron diamond coating in carbide tool surface again.
3. the preparation method of the hard alloy cutter according to claim 2 with micro-nano diamond coatings, feature It is, the pretreatment includes the steps that carrying out chemical etching processing to the surface of hard alloy cutter;
Preferably, chemical etching processing is carried out again after carrying out blasting treatment to the surface of the hard alloy cutter;
Preferably, first hard alloy cutter is cleaned up after blasting treatment and carries out chemical etching processing again.
4. the preparation method of the hard alloy cutter according to claim 3 with micro-nano diamond coatings, feature It is, the step of chemical etching includes: first to be performed etching to be performed etching with acid solution again with aqueous slkali.
5. the preparation method of the hard alloy cutter according to claim 4 with micro-nano diamond coatings, feature It is, the aqueous slkali includes K3[Fe(CN)]6, KOH and water composition aqueous slkali;
Preferably, the K3[Fe(CN)]6, KOH and water mass ratio be (1~2): (1~2): 10;
Preferably, the acid solution includes H2SO4And H2O2The acid solution of composition;
Preferably, the H2SO4And H2O2Volume ratio be (1~2): 10;
Preferably, the step of chemical etching includes: that hard alloy cutter is placed in K3[Fe(CN)]6, KOH and water composition It is performed etching in aqueous slkali, removes the aqueous slkali of carbide tool surface later, then be placed in H2SO4And H2O2The acid of composition is molten It is performed etching in liquid.
6. the preparation method of the hard alloy cutter according to claim 3 with micro-nano diamond coatings, feature It is, the preparation method further includes carrying out the pre- step for planting crystal seed by chemical etching treated carbide tool surface Suddenly;
Preferably, the step of pre- plant crystal seed includes: that treated that hard alloy cutter is placed in bortz powder by chemical etching It is ultrasonically treated in suspension;
Preferably, the concentration of the bortz powder suspension are as follows: 2~5wt%.
7. the preparation side of the hard alloy cutter according to claim 1-6 with micro-nano diamond coatings Method, which is characterized in that the micron diamond coating being prepared with a thickness of 1.5-3 microns.
8. the preparation side of the hard alloy cutter according to claim 1-6 with micro-nano diamond coatings Method, which is characterized in that the method for preparing micron diamond coating includes: to prepare micron diamond with chemical vapour deposition technique to apply Layer;
Preferably, it includes: that methane volumetric score is that the chemical vapour deposition technique, which prepares the technological parameter of micron diamond coating, 2%-5%, air pressure 0.8-2.5kPa, 1800-2200 DEG C of temperature range, the temperature range of hard alloy cutter is when processing 600-650 DEG C, the processing time is 1-2.5h;Optimizing technology parameters are as follows: methane volumetric score is 3%-4%, air pressure 1.2- 2kPa, 1900-2100 DEG C of temperature range, the temperature range of hard alloy cutter is 610-640 DEG C when processing, and the processing time is 1.2-2.2h。
9. the preparation side of the hard alloy cutter according to claim 1-6 with micro-nano diamond coatings Method, which is characterized in that the etching includes plasma etching;
Preferably, it includes: gas pressure in vacuum range that using plasma etching, which prepares the technological parameter of nano diamond coating, The temperature range of hard alloy cutter is 600-650 DEG C, handles the time when 1.5-2kPa, 2000-2200 DEG C of filament temperature, processing 10-30min, optimizing technology parameters are as follows: hard when gas pressure in vacuum range 1.6-1.9kPa, 2000-2200 DEG C of filament temperature, processing The temperature range of matter alloy cutter is 610-640 DEG C, handles time 15-25min, and reaction gas is hydrogen.
10. a kind of hard alloy cutter with micro-nano diamond coatings, which is characterized in that -9 is any according to claim 1 The preparation method of the hard alloy cutter with micro-nano diamond coatings described in is prepared.
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