CN105671551B - Diamond composite coating, the gradient ultra-fine cemented carbide cutter with the composite coating and preparation method thereof - Google Patents

Diamond composite coating, the gradient ultra-fine cemented carbide cutter with the composite coating and preparation method thereof Download PDF

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Publication number
CN105671551B
CN105671551B CN201610083495.8A CN201610083495A CN105671551B CN 105671551 B CN105671551 B CN 105671551B CN 201610083495 A CN201610083495 A CN 201610083495A CN 105671551 B CN105671551 B CN 105671551B
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alloy
layer
matrix
layers
diamond
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CN105671551A (en
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伍尚华
陈健
邓欣
刘伟
刘汝德
陈少华
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Guangdong University of Technology
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Guangdong University of Technology
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Priority to PCT/CN2016/075362 priority patent/WO2017136972A1/en
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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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • 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
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/347—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with layers adapted for cutting tools or wear applications
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
    • B23B2228/04—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner applied by chemical vapour deposition [CVD]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
    • B23B2228/08—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner applied by physical vapour deposition [PVD]

Abstract

A kind of diamond composite coating, the gradient ultra-fine cemented carbide cutter with diamond composite coating and preparation method thereof.Alloy cutter is made up of tool matrix and diamond composite coating.Tool matrix is provided with normal group tissue layer, rich cobalt transition zone and poor cobalt richness cubic layer.Diamond composite coating includes the diamond layer as the Ti Al Si Cr alloy-layers of transition zone and as functional layer.The present invention has the gradient ultra-fine cemented carbide cutter of the diamond composite coating, and its tool matrix is good with diamond composite coating associativity, and solid tool has good abrasion-proof and temperature-resistant performance, and intensity is high, shock resistance is excellent.Diamond composite coating, it is good with tool matrix associativity, and adhesive force is good between the coating of composite coating, and its heat-resisting quantity, corrosion resistance, wearability are good.

Description

Diamond composite coating, the gradient ultra-fine cemented carbide cutter with the composite coating And preparation method thereof
Technical field
The present invention relates to hard alloy cutter technical field, is answered more particularly to a kind of diamond composite coating, with this Close gradient ultra-fine cemented carbide cutter of coating and preparation method thereof.
Background technology
Hard alloy cutter bears great mechanical load and thermic load in process, easily produces abrasion, so as to Its service life is influenceed, therefore, surface modification is carried out to cutter material, improves its surface property, this is to improving cutter material Service life has great importance.
TiN, TiN, TiCN or Al of thin layer are coated in carbide surface2O3Etc. high rigidity high-abrasive material, cutter can be improved Wearability simultaneously keep the good toughness of matrix, the service behaviour and service life of cutter material can be significantly improved.But apply Layer substantially hard brittle material, and, boundary coating and matrix between different with carbide matrix material thermal coefficient of expansion There is stress concentration phenomenon in face, usual crackle easily produces and to material failure caused by alloy diffusion inside in coating surface.
Although diamond has the characteristics that high rigidity, high thermal conductivity, low-friction coefficient, chemical stability are good, due to Adhesion between diamond coatings and hard alloy can not be solved effectively, limit diamond coatings in hard alloy cutter side The application in face.
Therefore, in view of the shortcomings of the prior art, providing a kind of diamond suitable for carbide tool surface performance enhancement Composite coating, there is gradient ultra-fine cemented carbide cutter of the composite coating and preparation method thereof to overcome prior art deficiency very For necessity.
The content of the invention
An object of the present invention is to provide a kind of gradient ultra-fine cemented carbide cutter with diamond composite coating And preparation method thereof, diamond composite coating and tool matrix associativity are good, and cutter abrasion-proof and temperature-resistant is good, and intensity is high, anti-impact Hit function admirable.
There is provided another object of the present invention is to avoid in place of the deficiencies in the prior art a kind of diamond composite coating and Its preparation method, diamond composite coating and tool matrix associativity are good, and the cutter abrasion-proof and temperature-resistant with the coating is good, by force Degree is high, and shock resistance is excellent.
The above-mentioned purpose of the present invention is realized by following technological means.
A kind of gradient ultra-fine cemented carbide cutter with diamond composite coating is provided, by tool matrix and is arranged at Diamond composite coating on tool matrix is formed；
The tool matrix includes normal group tissue layer, rich cobalt transition zone and poor cobalt richness cubic layer, the normal group tissue layer, Rich cobalt transition zone and poor cobalt richness cubic layer are arranged in order according to order from inside to outside；
The diamond composite coating includes being used to be deposited on Ti-Al- of the poor cobalt richness cubic layer surface as transition zone Si-Cr alloy-layers and it is deposited on the diamond layer on transition zone as functional layer.
The content of cobalt is 5-15wt.% in the upper tool matrix；
The normal group tissue layer is ultra-fine cemented carbide, and WC grain size is 1-10000nm；
The thickness of the normal group tissue layer is more than 2mm, and the thickness of the rich cobalt transition zone is 20-100 microns；The poor cobalt The thickness of rich cubic layer is 20-50 microns；
The thickness of the Ti-Al-Si-Cr alloy-layers is 2-3 microns, and the thickness of the diamond layer is 15-20 microns.
The content of cobalt is 8-12wt.% in above-mentioned tool matrix；The WC grain size of the normal group tissue layer is 1nm- 400nm；The Ti-Al-Si-Cr alloy-layers are prepared by physical vaporous deposition, and the diamond layer passes through chemical vapor deposition It is prepared by area method.
The specific preparation method of above-mentioned Ti-Al-Si-Cr alloy-layers is as follows,
（1.1）Prepare Ti-Al-Si-Cr alloy target materials
（1.2）Physical gas-phase deposite method plated film
The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumize reach 0.5 × 10-1-1.5×10-1During Pa, arc source is opened, carries out Ions Bombardment, cleans hard alloy cutter matrix surface 2-5 minutes；
Then under conditions of bombardment bias 200-300V, arc power 50-90A, plated film 20-60 minutes；
Arc power is then shut off, makes vacuum chamber Slow cooling, 1-2 takes out sample after hour；Now, hard alloy cutter The poor cobalt richness cubic layer surface of matrix has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, being put into Learn in vapor deposition apparatus and prepare diamond layer, it is as follows to prepare the specific method of diamond layer,
（2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into chemical vapor depsotition equipment Vacuum chamber, make tool matrix apart from resistance wire 2mm-6mm；
（2.2) cooling water system is opened, 8-15 supports is first evacuated down to, then opens heater supply, slowly add electric current, electric current When reaching 500-650A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
（2.3) methane mass flow meter is opened after 3 minutes, flow reduces electric current after 100-300sccm, 1.5-3 hour, Methane flow meter is closed, electric current is zero after 15-30 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
（2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si- Cr alloyed layers are coated with the diamond layer that a layer thickness is 15-20 microns.
Further, the specific preparation method of above-mentioned Ti-Al-Si-Cr alloy-layers is as follows,
（1.1）The preparation of Ti-Al-Si-Cr alloy target materials
Using high-purity titanium sponge of purity 99.99%, the rafifinal of purity 99.99%, purity 99.99% HIGH-PURITY SILICON, 99.99% High Pure Chromium is as raw material, by weight percentage：Ti, which accounts for 70-80%, Al and accounts for 5-10%, Si and account for 5-10%, Cr, accounts for 10- 20% ratio carries out vacuum metling and obtains alloy pig, then alloy pig is processed into diameter 120mm, long 200mm cylindricality target As Ti-Al-Si-Cr alloy target materials；
（1.2）Physical gas-phase deposite method plated film
The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumizes and reach 1 × 10- 1During Pa, arc source is opened, carries out Ions Bombardment, cleaning hard alloy cutter matrix surface 3 minutes；
Then under conditions of bombardment bias 250V, arc power 60A, plated film 30-40 minutes；
Arc power is then shut off, makes vacuum chamber Slow cooling, sample is taken out after 1.5 hours；Now, tool matrix is poor Cobalt richness cubic layer surface has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, being put into Learn in vapor deposition apparatus and prepare diamond layer, it is as follows to prepare the specific method of diamond layer,
（2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into chemical vapor depsotition equipment Vacuum chamber, make tool matrix apart from resistance wire 3mm-4mm；
（2.2) cooling water system is opened, 10 supports is first evacuated down to, then opens heater supply, slowly plus electric current, electric current reach During to 600A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
（2.3) methane mass flow meter is opened after 3 minutes, flow 150-200sccm, reduces electric current after 2 hours, is closed Methane flow meter, electric current is zero after 20 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
（2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si- Cr alloyed layers are coated with the diamond layer that a layer thickness is 15-20 microns.
A kind of preparation method of the gradient ultra-fine cemented carbide cutter with diamond composite coating, including cutter are provided The preparation of matrix and prepare diamond composite coating on tool matrix surface；The preparation of diamond composite coating is to first pass through physics Vapour deposition process is coated with Ti-Al-Si-Cr alloy-layers on the poor cobalt richness cubic layer surface of tool matrix, and surface deposited Ti- The hard alloy cutter matrix of Al-Si-Cr alloy-layers is put into chemical vapor depsotition equipment with chemistry after the third intoxicated cleaning-drying Vapour deposition process prepares diamond layer.
The specific preparation method of above-mentioned Ti-Al-Si-Cr alloy-layers is as follows,
（1.1）Prepare Ti-Al-Si-Cr alloy target materials
（1.2）Physical gas-phase deposite method plated film
The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumize reach 0.5 × 10-1-1.5×10-1During Pa, arc source is opened, carries out Ions Bombardment, cleans hard alloy cutter matrix surface 2-5 minutes；
Then under conditions of bombardment bias 200-300V, arc power 50-90A, plated film 20-60 minutes；
Arc power is then shut off, makes vacuum chamber Slow cooling, 1-2 takes out sample after hour；Now, hard alloy cutter The poor cobalt richness cubic layer surface of matrix has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, being put into Learn in vapor deposition apparatus and prepare diamond layer, it is as follows to prepare the specific method of diamond layer,
（2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into chemical vapor depsotition equipment Vacuum chamber, make tool matrix apart from resistance wire 2mm-6mm；
（2.2) cooling water system is opened, 8-15 supports is first evacuated down to, then opens heater supply, slowly add electric current, electric current When reaching 500-650A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
（2.3) methane mass flow meter is opened after 3 minutes, flow reduces electric current after 100-300sccm, 1.5-3 hour, Methane flow meter is closed, electric current is zero after 15-30 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
（2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si- Cr alloyed layers are coated with the diamond layer that a layer thickness is 15-20 microns.
Further, the specific preparation method of above-mentioned Ti-Al-Si-Cr alloy-layers is as follows,
（1.1）The preparation of Ti-Al-Si-Cr alloy target materials
Using high-purity titanium sponge of purity 99.99%, the rafifinal of purity 99.99%, purity 99.99% HIGH-PURITY SILICON, 99.99% High Pure Chromium is as raw material, by weight percentage：Ti, which accounts for 70-80%, Al and accounts for 5-10%, Si and account for 5-10%, Cr, accounts for 10- 20% ratio carries out vacuum metling and obtains alloy pig, then alloy pig is processed into diameter 120mm, long 200mm cylindricality target As Ti-Al-Si-Cr alloy target materials；
（1.2）Physical gas-phase deposite method plated film
The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumizes and reach 1 × 10- 1During Pa, arc source is opened, carries out Ions Bombardment, cleaning hard alloy cutter matrix surface 3 minutes；
Then under conditions of bombardment bias 250V, arc power 60A, plated film 30-40 minutes；
Arc power is then shut off, makes vacuum chamber Slow cooling, sample is taken out after 1.5 hours；Now, tool matrix is poor Cobalt richness cubic layer surface has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, being put into Learn in vapor deposition apparatus and prepare diamond layer, it is as follows to prepare the specific method of diamond layer,
（2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into chemical vapor depsotition equipment Vacuum chamber, make tool matrix apart from resistance wire 3mm-4mm；
（2.2) cooling water system is opened, 10 supports is first evacuated down to, then opens heater supply, slowly plus electric current, electric current reach During to 600A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
（2.3) methane mass flow meter is opened after 3 minutes, flow 150-200sccm, reduces electric current after 2 hours, is closed Methane flow meter, electric current is zero after 20 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
（2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si- Cr alloyed layers are coated with the diamond layer that a layer thickness is 15-20 microns.
A kind of diamond composite coating for gradient ultra-fine cemented carbide cutter is provided, including for being deposited on cutter base The poor cobalt richness cubic layer surface of body as transition zone Ti-Al-Si-Cr alloy-layers and be deposited on transition zone and be used as functional layer Diamond layer.
A kind of preparation method of diamond composite coating is provided, specific preparation method is as follows,
（1.1）The preparation of Ti-Al-Si-Cr alloy target materials
Using high-purity titanium sponge of purity 99.99%, the rafifinal of purity 99.99%, purity 99.99% HIGH-PURITY SILICON, 99.99% High Pure Chromium is as raw material, by weight percentage：Ti, which accounts for 70-80%, Al and accounts for 5-10%, Si and account for 5-10%, Cr, accounts for 10- 20% ratio carries out vacuum metling and obtains alloy pig, then alloy pig is processed into diameter 120mm, long 200mm cylindricality target As Ti-Al-Si-Cr alloy target materials；
（1.2）Physical gas-phase deposite method plated film
The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumizes and reach 1 × 10- 1During Pa, arc source is opened, carries out Ions Bombardment, cleaning hard alloy cutter matrix surface 3 minutes；
Then under conditions of bombardment bias 250V, arc power 60A, plated film 30-40 minutes；
Arc power is then shut off, makes vacuum chamber Slow cooling, sample is taken out after 1.5 hours；Now, tool matrix is poor Cobalt richness cubic layer surface has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, being put into Learn in vapor deposition apparatus and prepare diamond layer, it is as follows to prepare the specific method of diamond layer,
（2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into chemical vapor depsotition equipment Vacuum chamber, make tool matrix apart from resistance wire 3mm-4mm；
（2.2) cooling water system is opened, 10 supports is first evacuated down to, then opens heater supply, slowly plus electric current, electric current reach During to 600A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
（2.3) methane mass flow meter is opened after 3 minutes, flow 150-200sccm, reduces electric current after 2 hours, is closed Methane flow meter, electric current is zero after 20 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
（2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si- Cr alloyed layers are coated with the diamond layer that a layer thickness is 15-20 microns.
The present invention has the gradient ultra-fine cemented carbide cutter of the diamond composite coating, and its tool matrix is answered with diamond It is good to close coating adhesion, solid tool has good abrasion-proof and temperature-resistant performance, and intensity is high, shock resistance is excellent.Diamond is answered Coating is closed, it is good with tool matrix associativity, and adhesive force is good between the coating of composite coating, its heat-resisting quantity, corrosion-resistant Property, wearability are good.
Brief description of the drawings
Using accompanying drawing, the present invention is further illustrated, but the content in accompanying drawing does not form any limit to the present invention System.
Fig. 1 is a kind of schematic diagram of the gradient ultra-fine cemented carbide cutter with diamond composite coating of the present invention.
Fig. 2 is a kind of interlayer structure signal of gradient ultra-fine cemented carbide cutter with diamond composite coating of the present invention Figure.
Embodiment
The invention will be further described with the following Examples.
Embodiment 1.
A kind of gradient ultra-fine cemented carbide cutter with diamond composite coating, as shown in Figure 1 and Figure 2, by tool matrix Formed with the diamond composite coating being arranged on tool matrix.
Tool matrix includes normal group tissue layer, rich cobalt transition zone and poor cobalt richness cubic layer, normal group tissue layer, rich cobalt transition Layer and poor cobalt richness cubic layer are arranged in order according to order from inside to outside.The content of cobalt is 5-15wt.% in tool matrix, excellent The content for selecting cobalt is 8-12wt.%.Normal group tissue layer is ultra-fine cemented carbide, and WC grain size is 1-10000nm, and preferably WC is brilliant Particle size is 1-500nm.
Be rich in Emission in Cubic nitride or carbonitride in poor cobalt richness cubic layer, Emission in Cubic nitride in hard alloy and Therefore carbonitride has the hardness higher than the WC of close-packed hexagonal phase, the top layer of poor cobalt richness Emission in Cubic has higher hardness. Binder Phase is rich in rich cobalt transition zone,, can due to its good toughness when the crackle formed in coating is diffused into the region To absorb energy during crackle diffusion, therefore, it is possible to effectively prevent crackle to alloy diffusion inside, and can preferably inhale Impact energy during Tool in Cutting is received, thus has high toughness characteristic, and then is advantageous to improve the use of cutter material Life-span.Core is that rigid tissue regions are normal group tissue layer, and WC grain is evenly distributed and tiny, and average WC grain sizes are less than etc. In 500nm, there is the excellent mechanical property of ultra-fine cemented carbide.
The thickness of normal group tissue layer is more than 2mm, and the thickness of rich cobalt transition zone is 20-100 microns, poor cobalt richness cubic layer Thickness is 20-50 microns.
The overall thickness of diamond composite coating is 1-25 microns, preferably 2-10 microns.When coating layer thickness is less than 1 micron When, its wearability is poor, is worn quickly in cutting process, it is impossible to plays and is effectively improved Tool in Cutting performance and life-span Effect, and when coating layer thickness is more than 25 microns, the adhesion of coating and matrix is poor, and too high compression causes coating to be opened Split and peel off, shorten cutter life.The thickness of coating is controlled by adjusting sedimentation time.
The thickness of Ti-Al-Si-Cr alloy-layers is 2-3 microns, and the thickness of diamond layer is 15-20 microns.
The present invention sets one layer of Ti-Al-Si-Cr alloy-layer to be utilized as transition zone between tool matrix and diamond Titanium, chromium strong carbide form the characteristic of material, have good wellability and adhesion with matrix hard alloy and diamond, use With eliminate Film laminated coating and tool matrix because lattice mismatch, thermal expansion coefficient difference and caused by internal stress, both can be to prevent Blocking excessively penetrates into tool matrix, can prevent cobalt from being diffused to the surface from matrix depths again.It is rich vertical with poor cobalt that transition zone promotes it Adhesion between square phase layer, reduce internal stress.By transition zone, the depositing diamond layer on transition zone, hard both can guarantee that The original intensity of alloy cutter and sharpness, the wearability of cutter, processing effect by diamond coatings, can be increased substantially again Rate and service life.
The present invention has the gradient ultra-fine cemented carbide cutter of the diamond composite coating, and its tool matrix is answered with diamond It is good to close coating adhesion, solid tool has good abrasion-proof and temperature-resistant performance, and intensity is high, shock resistance is excellent.
Embodiment 2.
A kind of preparation method of the gradient ultra-fine cemented carbide cutter with diamond composite coating, including cutter base are provided The preparation of body and prepare diamond composite coating on tool matrix surface.
The specific preparation process of tool matrix is as follows：
(1) with refractory carbide, binding metal and TiCN and other powder such as TiC, TaC, or other strong nitridations Carbide, the carbonitride of thing formation element are raw material, pass through ball milling mixing, drying and screening, compressing and four steps of sintering Suddenly hard alloy substrate presoma is prepared.
(2) fine grinding processing is carried out to hard alloy substrate presoma.
(3) gradient sintering is carried out to the hard alloy substrate presoma after fine grinding processing, the poor cobalt in top layer is prepared With rich Emission in Cubic Graded-structure Cemented Carbides tool matrix.
(4) after carrying out Chemical cleaning to tool matrix, then in its surface depositing diamond composite coating.
In diamond composite coating, Ti-Al-Si-Cr alloy-layers are prepared by physical vaporous deposition, the diamond layer Prepared by chemical vapour deposition technique.
The preparation of diamond composite coating is the poor cobalt richness cubic layer for first passing through physical vaporous deposition in tool matrix Surface is coated with Ti-Al-Si-Cr alloy-layers, and the hard alloy cutter matrix that surface deposited Ti-Al-Si-Cr alloy-layers is intoxicated through third After cleaning-drying, it is put into chemical vapor depsotition equipment and diamond layer is prepared with chemical vapour deposition technique.
The specific preparation method of Ti-Al-Si-Cr alloy-layers is as follows：
（1.1）Prepare Ti-Al-Si-Cr alloy target materials
（1.2）Physical gas-phase deposite method plated film
The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumize reach 0.5 × 10-1-1.5×10-1During Pa, arc source is opened, carries out Ions Bombardment, cleans hard alloy cutter matrix surface 2-5 minutes；
Then under conditions of bombardment bias 200-300V, arc power 50-90A, plated film 20-60 minutes；
Arc power is then shut off, makes vacuum chamber Slow cooling, 1-2 takes out sample after hour；Now, hard alloy cutter The poor cobalt richness cubic layer surface of matrix has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns.
Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, being put into Learn in vapor deposition apparatus and prepare diamond layer, the specific method for preparing diamond layer is as follows：
（2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into chemical vapor depsotition equipment Vacuum chamber, make tool matrix apart from resistance wire 2mm-6mm；
（2.2) cooling water system is opened, 8-15 supports is first evacuated down to, then opens heater supply, slowly add electric current, electric current When reaching 500-650A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
（2.3) methane mass flow meter is opened after 3 minutes, flow reduces electric current after 100-300sccm, 1.5-3 hour, Methane flow meter is closed, electric current is zero after 15-30 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
（2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si- Cr alloyed layers are coated with the diamond layer that a layer thickness is 15-20 microns.
The preparation method of the present invention uses first is coated with one layer of Ti-Al-Si-Cr with PVD methods on hard alloy cutter matrix Layer is used as transition zone, then uses CVD method depositing diamond layer on transition zone again.The composition of target is determined by concrete technology And preparation method, by the selection and control of specific PVD parameter, avoid film layer internal stress mistake caused by heating is too fast Explosion or obscission occur greatly, makes that there is good adhesive force between film layer and tool matrix.The present invention passes through transition zone Be coated with, then prepare diamond layer, the final gradient ultra-fine cemented carbide cutter for obtaining function admirable.
The gradient ultra-fine cemented carbide cutter with the diamond composite coating prepared by the present invention, its tool matrix with Diamond composite coating associativity is good, and solid tool has good abrasion-proof and temperature-resistant performance, and intensity is high, shock resistance is excellent.
Embodiment 3.
A kind of preparation method of the gradient ultra-fine cemented carbide cutter with diamond composite coating, including cutter base are provided The preparation of body and prepare diamond composite coating on tool matrix surface.
Tool matrix is formed by each component sintering of following mass percent：5-15% TiC, 2-5% TaC, 10-15% Alloy bonding phase, surplus WC.Alloy bonding is mutually made up of the powder of following mass percent：0.5-5.5% Cr, 0.5- 5.5% Mo, 0.5-5.5% B, 0.5-5.5% Al, 0.5-5.5% V, 0.5-5.5% Y, 0.5-5.5% Si, surplus are Co, and Cr, Mo, B, Al, V, Y and Si quality sum are the 7-20% of alloy bonding phase quality in alloy bonding phase.
The preparation method of tool matrix, comprises the following steps：
S1, prepare alloy bonding phase：Weigh eight kinds of powders of Cr, Mo, B, Al, V, Y, Si, Co respectively by mass percentage, will Eight kinds of powders are well mixed, and obtain alloy bonding phase.It is preferred that eight kinds of powders are placed in ball mill, with hard alloy mill ball ball milling 72 hours, and just suspend ball milling 10min per ball milling 1h, obtain alloy bonding phase.
S2, prepare blank：Weigh tetra- kinds of alloy bonding phase, TiC, TaC, WC components, four kinds of groups respectively by mass percentage It is grouped into material powder；Paraffin is weighed by the 1.5-2.5% of material powder gross mass, and paraffin is well mixed with material powder, Obtain blank.
S3, pressing blank：Blank is compressing, obtain base substrate.
Can be first compressing by blank with molding press, obtain just base substrate；Just base substrate is further suppressed with cold isostatic press again, is obtained Base substrate.
S4, sintering：Base substrate is placed in sintering furnace, 1200-1250 DEG C is warming up to 5-8 DEG C/min speed, is incubated 18- 22min, and keep 10-3Below Pa vacuum；Then nitrogen is filled with into sintering furnace and is warming up to 1-3 DEG C/min speed 1420-1450 DEG C, it is incubated 55-65min and keeps more than 0.2MPa pressure；Then it is cooled to again with 2-6 DEG C/min speed 1000-1200 DEG C, 110-130min is incubated, and keep more than 0.2MPa pressure；Followed by base substrate furnace cooling, and keep More than 0.2MPa pressure, case-hardened gradient hard alloy is made.
Pre-sintering step can be carried out, the pre-sintering step is that base substrate is placed in sintering furnace, in inertia before step S4 Under gas atmosphere, with 1400 DEG C of sintering 10min；Refine base substrate profile after base substrate furnace cooling.
The content of cobalt is 5-15wt.%.% in the tool matrix of hard alloy prepared by this method.Normal group tissue layer is super Thin hard alloy, WC grain size are 1-10000nm.Tool matrix has excellent mechanical property, improves hard alloy Red hardness.Crystal grain in carbide matrix body is tiny, is normal group tissue layer；The top layer richness Emission in Cubic of hard alloy and poor Binder Phase I.e. poor cobalt richness Emission in Cubic, and the transition zone of an also rich alloy Binder Phase is rich cobalt transition zone under top layer, so that hard closes Gold utensil has excellent hardness, wearability and toughness.
After the completion of prepared by alloy substrate, Chemical cleaning is carried out to it, then in its surface depositing diamond composite coating.
The preparation of diamond composite coating is the poor cobalt richness cubic layer for first passing through physical vaporous deposition in tool matrix Surface is coated with Ti-Al-Si-Cr alloy-layers, and the hard alloy cutter matrix that surface deposited Ti-Al-Si-Cr alloy-layers is intoxicated through third After cleaning-drying, it is put into chemical vapor depsotition equipment and diamond layer is prepared with chemical vapour deposition technique.
The specific preparation method of Ti-Al-Si-Cr alloy-layers is as follows,
（1.1）The preparation of Ti-Al-Si-Cr alloy target materials
Using high-purity titanium sponge of purity 99.99%, the rafifinal of purity 99.99%, purity 99.99% HIGH-PURITY SILICON, 99.99% High Pure Chromium is as raw material, by weight percentage：Ti, which accounts for 70-80%, Al and accounts for 5-10%, Si and account for 5-10%, Cr, accounts for 10- 20% ratio carries out vacuum metling and obtains alloy pig, then alloy pig is processed into diameter 120mm, long 200mm cylindricality target As Ti-Al-Si-Cr alloy target materials；
（1.2）Physical gas-phase deposite method plated film
The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumizes and reach 1 × 10- 1During Pa, arc source is opened, carries out Ions Bombardment, cleaning hard alloy cutter matrix surface 3 minutes；
Then under conditions of bombardment bias 250V, arc power 60A, plated film 30-40 minutes；
Arc power is then shut off, makes vacuum chamber Slow cooling, sample is taken out after 1.5 hours；Now, tool matrix is poor Cobalt richness cubic layer surface has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, being put into Learn in vapor deposition apparatus and prepare diamond layer, it is as follows to prepare the specific method of diamond layer,
（2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into chemical vapor depsotition equipment Vacuum chamber, make tool matrix apart from resistance wire 3mm-4mm；
（2.2) cooling water system is opened, 10 supports is first evacuated down to, then opens heater supply, slowly plus electric current, electric current reach During to 600A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
（2.3) methane mass flow meter is opened after 3 minutes, flow 150-200sccm, reduces electric current after 2 hours, is closed Methane flow meter, electric current is zero after 20 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
（2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si- Cr alloyed layers are coated with the diamond layer that a layer thickness is 15-20 microns.
The preparation method of the present invention uses first is coated with one layer of Ti-Al-Si-Cr with PVD methods on hard alloy cutter matrix Layer is used as transition zone, then uses CVD method depositing diamond layer on transition zone again.The composition of target is determined by concrete technology And preparation method, by the selection and control of specific PVD parameter, avoid film layer internal stress mistake caused by heating is too fast Explosion or obscission occur greatly, makes that there is good adhesive force between film layer and tool matrix.The present invention passes through transition zone Be coated with, then prepare diamond layer, the final gradient ultra-fine cemented carbide cutter for obtaining function admirable.
The gradient ultra-fine cemented carbide cutter with the diamond composite coating prepared by the present invention, its tool matrix with Diamond composite coating associativity is good, and solid tool has good abrasion-proof and temperature-resistant performance, and intensity is high, shock resistance is excellent.
Embodiment 4.
It is any in a kind of diamond composite coating for gradient ultra-fine cemented carbide cutter, its structure and embodiment 1-3 Diamond composite coating in one is identical, including for being deposited on the poor cobalt richness cubic layer surface of tool matrix as transition Layer Ti-Al-Si-Cr alloy-layers and be deposited on the diamond layer on transition zone as functional layer.
Diamond composite coating prepared by the present invention, it is good with tool matrix associativity, between the coating of composite coating Adhesive force is good, and its heat-resisting quantity, corrosion resistance, wearability are good, and intensity is high, shock resistance is excellent.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected The limitation of scope, although being explained in detail with reference to preferred embodiment to the present invention, one of ordinary skill in the art should manage Solution, can modify or equivalent substitution to technical scheme, without departing from technical solution of the present invention essence and Scope.

Claims (5)

  1. A kind of 1. gradient ultra-fine cemented carbide cutter with diamond composite coating, it is characterised in that：
    It is made up of tool matrix and the diamond composite coating being arranged on tool matrix；
    The tool matrix includes normal group tissue layer, rich cobalt transition zone and poor cobalt richness cubic layer, the normal group tissue layer, rich cobalt Transition zone and poor cobalt richness cubic layer are arranged in order according to order from inside to outside；
    The diamond composite coating includes being used to be deposited on Ti-Al-Si-Cr of the poor cobalt richness cubic layer surface as transition zone Alloy-layer and it is deposited on the diamond layer on transition zone as functional layer；
    The content of cobalt is 5-15wt.% in the tool matrix；
    The normal group tissue layer is ultra-fine cemented carbide, and WC grain size is 1-10000nm；
    The thickness of the normal group tissue layer is more than 2mm, and the thickness of the rich cobalt transition zone is 20-100 microns；The poor cobalt is rich vertical The thickness of square phase layer is 20-50 microns；
    The thickness of the Ti-Al-Si-Cr alloy-layers is 2-3 microns, and the thickness of the diamond layer is 15-20 microns；
    The content of cobalt is 8-12wt.% in the tool matrix；The WC grain size of the normal group tissue layer is 1nm-400nm；Institute State Ti-Al-Si-Cr alloy-layers to prepare by physical vaporous deposition, the diamond layer is prepared by chemical vapour deposition technique.
  2. 2. the gradient ultra-fine cemented carbide cutter according to claim 1 with diamond composite coating, it is characterised in that：
    The specific preparation method of the Ti-Al-Si-Cr alloy-layers is as follows,
    （1.1）Prepare Ti-Al-Si-Cr alloy target materials
    （1.2）Physical gas-phase deposite method plated film
    The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumizes and reach 0.5 × 10-1- 1.5×10-1During Pa, arc source is opened, carries out Ions Bombardment, cleans hard alloy cutter matrix surface 2-5 minutes；
    Then under conditions of bombardment bias 200-300V, arc power 50-90A, plated film 20-60 minutes；
    Arc power is then shut off, makes vacuum chamber Slow cooling, 1-2 takes out sample after hour；Now, hard alloy cutter matrix Poor cobalt richness cubic layer surface has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
    Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, be put into chemical gas Diamond layer is prepared in phase depositing device, it is as follows to prepare the specific method of diamond layer,
    （2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into the vacuum of chemical vapor depsotition equipment Room, make tool matrix apart from resistance wire 2mm-6mm；
    （2.2) cooling water system is opened, 8-15 supports is first evacuated down to, then opens heater supply, slowly plus electric current, electric current reach During 500-650A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
    （2.3) methane mass flow meter is opened after 3 minutes, flow reduces electric current after 100-300sccm, 1.5-3 hour, close Methane flow meter, electric current is zero after 15-30 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
    （2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si-Cr is closed Layer gold surface is coated with the diamond layer that a layer thickness is 15-20 microns.
  3. 3. the gradient ultra-fine cemented carbide cutter according to claim 2 with diamond composite coating, it is characterised in that：
    The specific preparation method of the Ti-Al-Si-Cr alloy-layers is as follows,
    （1.1）The preparation of Ti-Al-Si-Cr alloy target materials
    Using high-purity titanium sponge of purity 99.99%, the rafifinal of purity 99.99%, the HIGH-PURITY SILICON of purity 99.99%, 99.99% High Pure Chromium as raw material, by weight percentage：Ti, which accounts for 70-80%, Al and accounts for 5-10%, Si, accounts for the ratio that 5-10%, Cr account for 10-20% Example carries out vacuum metling and obtains alloy pig, and alloy pig then is processed into diameter 120mm, long 200mm cylindricality target as Ti- Al-Si-Cr alloy target materials；
    （1.2）Physical gas-phase deposite method plated film
    The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumizes and reach 1 × 10-1During Pa, Arc source is opened, carries out Ions Bombardment, cleaning hard alloy cutter matrix surface 3 minutes；
    Then under conditions of bombardment bias 250V, arc power 60A, plated film 30-40 minutes；
    Arc power is then shut off, makes vacuum chamber Slow cooling, sample is taken out after 1.5 hours；Now, the poor cobalt of tool matrix is rich Cubic layer surface has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
    Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, be put into chemical gas Diamond layer is prepared in phase depositing device, it is as follows to prepare the specific method of diamond layer,
    （2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into the vacuum of chemical vapor depsotition equipment Room, make tool matrix apart from resistance wire 3mm-4mm；
    （2.2) cooling water system is opened, 10 supports is first evacuated down to, then opens heater supply, slowly plus electric current, electric current reach During 600A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
    （2.3) methane mass flow meter is opened after 3 minutes, flow 150-200sccm, reduces electric current after 2 hours, closes methane Flowmeter, electric current is zero after 20 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
    （2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si-Cr is closed Layer gold surface is coated with the diamond layer that a layer thickness is 15-20 microns.
  4. 4. the gradient ultra-fine cemented carbide cutter with diamond composite coating as described in claims 1 to 3 any one Preparation method, it is characterised in that：
    Preparation including tool matrix and prepare diamond composite coating on tool matrix surface；The preparation of diamond composite coating It is to first pass through physical vaporous deposition to be coated with Ti-Al-Si-Cr alloy-layers, table on the poor cobalt richness cubic layer surface of tool matrix Face deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, be put into chemical vapor deposition Diamond layer is prepared with chemical vapour deposition technique in equipment；
    The specific preparation method of the Ti-Al-Si-Cr alloy-layers is as follows,
    （1.1）Prepare Ti-Al-Si-Cr alloy target materials
    （1.2）Physical gas-phase deposite method plated film
    The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumizes and reach 0.5 × 10-1- 1.5×10-1During Pa, arc source is opened, carries out Ions Bombardment, cleans hard alloy cutter matrix surface 2-5 minutes；
    Then under conditions of bombardment bias 200-300V, arc power 50-90A, plated film 20-60 minutes；
    Arc power is then shut off, makes vacuum chamber Slow cooling, 1-2 takes out sample after hour；Now, hard alloy cutter matrix Poor cobalt richness cubic layer surface has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
    Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, be put into chemical gas Diamond layer is prepared in phase depositing device, it is as follows to prepare the specific method of diamond layer,
    （2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into the vacuum of chemical vapor depsotition equipment Room, make tool matrix apart from resistance wire 2mm-6mm；
    （2.2) cooling water system is opened, 8-15 supports is first evacuated down to, then opens heater supply, slowly plus electric current, electric current reach During 500-650A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
    （2.3) methane mass flow meter is opened after 3 minutes, flow reduces electric current after 100-300sccm, 1.5-3 hour, close Methane flow meter, electric current is zero after 15-30 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
    （2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si-Cr is closed Layer gold surface is coated with the diamond layer that a layer thickness is 15-20 microns.
  5. 5. the preparation method of the gradient ultra-fine cemented carbide cutter with diamond composite coating as claimed in claim 4, its It is characterised by：
    The specific preparation method of the Ti-Al-Si-Cr alloy-layers is as follows,
    （1.1）The preparation of Ti-Al-Si-Cr alloy target materials
    Using high-purity titanium sponge of purity 99.99%, the rafifinal of purity 99.99%, the HIGH-PURITY SILICON of purity 99.99%, 99.99% High Pure Chromium as raw material, by weight percentage：Ti, which accounts for 70-80%, Al and accounts for 5-10%, Si, accounts for the ratio that 5-10%, Cr account for 10-20% Example carries out vacuum metling and obtains alloy pig, and alloy pig then is processed into diameter 120mm, long 200mm cylindricality target as Ti- Al-Si-Cr alloy target materials；
    （1.2）Physical gas-phase deposite method plated film
    The hard alloy cutter matrix cleaned through ultrasonic wave is put into the vacuum chamber of PVD equipment, vacuumizes and reach 1 × 10-1During Pa, Arc source is opened, carries out Ions Bombardment, cleaning hard alloy cutter matrix surface 3 minutes；
    Then under conditions of bombardment bias 250V, arc power 60A, plated film 30-40 minutes；
    Arc power is then shut off, makes vacuum chamber Slow cooling, sample is taken out after 1.5 hours；Now, the poor cobalt of tool matrix is rich Cubic layer surface has been coated with the Ti-Al-Si-Cr alloy-layers that a layer thickness is 2-3 microns；
    Surface deposited the hard alloy cutter matrix of Ti-Al-Si-Cr alloy-layers after the third intoxicated cleaning-drying, be put into chemical gas Diamond layer is prepared in phase depositing device, it is as follows to prepare the specific method of diamond layer,
    （2.1) the hard alloy cutter matrix for being coated with Ti-Al-Si-Cr alloy-layers is put into the vacuum of chemical vapor depsotition equipment Room, make tool matrix apart from resistance wire 3mm-4mm；
    （2.2) cooling water system is opened, 10 supports is first evacuated down to, then opens heater supply, slowly plus electric current, electric current reach During 600A, hydrogen quality flowmeter, flow 900-1000sccm are opened；
    （2.3) methane mass flow meter is opened after 3 minutes, flow 150-200sccm, reduces electric current after 2 hours, closes methane Flowmeter, electric current is zero after 20 minutes, now closes hydrogen flowmeter, keeps cooling system to run well；
    （2.4) cooling system is closed after 1-1.5 hours, opens door for vacuum chamber, takes out solid tool, now, Ti-Al-Si-Cr is closed Layer gold surface is coated with the diamond layer that a layer thickness is 15-20 microns.
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