CN110184606A - Diamond-coated tools and preparation method thereof - Google Patents

Diamond-coated tools and preparation method thereof Download PDF

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Publication number
CN110184606A
CN110184606A CN201910619791.9A CN201910619791A CN110184606A CN 110184606 A CN110184606 A CN 110184606A CN 201910619791 A CN201910619791 A CN 201910619791A CN 110184606 A CN110184606 A CN 110184606A
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China
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diamond
hard alloy
alloy substrate
coated tools
tialcn
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Inventor
孔帅斐
李翠
李和鑫
宜娟
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HENAN FULAIGE ULTRAHARD MATERIAL CO Ltd
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HENAN FULAIGE ULTRAHARD MATERIAL CO Ltd
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
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    • 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
    • C23C14/0605—Carbon
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    • 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
    • C23C14/0664—Carbonitrides
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    • 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
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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    • 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
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    • 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
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    • 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
    • C23C16/274—Diamond only using microwave discharges
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    • 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
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    • 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
    • C23C28/04—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 only coatings of inorganic non-metallic material
    • C23C28/044—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 only coatings of inorganic non-metallic material coatings specially adapted for cutting tools or wear applications
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    • 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
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    • 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
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    • 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
    • C23C28/343—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 at least one DLC or an amorphous carbon based layer, the layer being doped or not
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Abstract

The present invention provides a kind of diamond-coated tools, comprising: hard alloy substrate, the TiAlCN layer being formed on the hard alloy substrate are deposited on the diamond-like rock layers of the TiAlCN layer surface and are formed in the diamond coatings of the diamond-like layer surface.The present invention also provides a kind of preparation methods of above-mentioned diamond-coated tools, comprising: cleaning hard alloy substrate；Coating film treatment is carried out on the hard alloy substrate, forms TiAlCN layers and diamond-like rock layers；Using chemical vapour deposition technique the diamond-like rock layers surface deposition of diamond coatings.TiAlCN layer in above-mentioned diamond-coated tools is used as Co element shielded layer, and diamond-like rock layers are used as diamond kind crystal layer, enhance the bond strength of diamond coatings and hard alloy substrate, improve the cutting ability and service life of diamond-coated tools.In addition, above-mentioned diamond-coated tools are easy to industrialized production and preparation process is environmentally friendly.

Description

Diamond-coated tools and preparation method thereof
Technical field
The invention belongs to superhard material coated cutting tool field more particularly to a kind of diamond-coated tools and its preparation sides Method.
Background technique
Diamond-coated tools have high hardness and wearability, low-friction coefficient, high elastic modulus, highly thermally conductive, low Thermal expansion coefficient, and it is small with nonferrous metal affinity the advantages that, and can be made the geometry of various complexity, it is extensive Applied to every field.Especially processing nonferrous metal and alloy, fibre reinforced plastics, fibreglass-reinforced metal and graphite, The field of new materials such as ceramics, diamond-coated tools have not available for high-speed tool steel and hard alloy cutter advantageously Position.Diamond-coated tools mainly utilize the method for chemical vapor deposition to deposit certain thickness Buddha's warrior attendant on hard alloy substrate Made from stone film, the thickness of the diamond film coating layer is at 20 μm hereinafter, the hard alloy substrate used usually has toughness Well, the features such as intensity is high.At present cvd diamond cutting tool coated with hard alloy product there are the problem of one of be diamond thin and Carbide chip poor adhesion.The too early of diamond film coating layer falls off in process, and coated chip can be greatly reduced Cutting ability and service life, how to improve the caking property of diamond thin and hard alloy substrate, how to enhance diamond It is current problem to be solved in the nucleation rate of carbide surface.
For this purpose, rich Nike provides a kind of deposition cvd diamond in the patent of invention application No. is CN2016112474099 Coated substrate oil removing takes off cobalt method, and step includes: to impregnate hard alloy substrate using anhydrous propanone solution first, obtains pre- place Manage hard alloy substrate；Then the pretreatment hard alloy substrate is cleaned using alkaline cleaner, obtains alkali cleaning hard alloy Matrix；Sandblasting successively finally is carried out to the alkali cleaning hard alloy substrate, oxygen plasma cleaning treatment obtains hard alloy and removes Then oil base body carries out pickling to the hard alloy oil removing matrix using the mixed acid containing perchloric acid and takes off cobalt processing, thus Obtain the deposition cvd diamond coated substrate that clean deposition cvd diamond coated substrate is made clean.The patent of invention is main Hard alloy substrate is handled using chemical erosion liquid ablution, cost is relatively low, is easy to industrial applications, however chemistry is invaded Erosion liquid ablution generallys use acid & alkali liquid and is cleaned, and generates a large amount of acid-base waste fluid and pollutes the environment.
In addition, having in the prior art using the method enhancing diamond of diadust suspension ultrasonic cleaning in hard The nucleation rate of alloy surface, although the diadust as crystal seed that this method can be formed on diamond body, crystal seed Quantity is uncontrollable, and can generate a large amount of diadust suspension waste liquid, and waste is serious.
Summary of the invention
In view of this, the present invention is applied it is necessory to provide a kind of diamond-coated tools and preparation method thereof, the diamond Layer cutter has preferable cutting ability and longer service life, and easy to industrialized production and preparation process is environmentally friendly.
For this purpose, technical solution provided by the invention are as follows: a kind of diamond-coated tools, comprising: hard alloy substrate, formation TiAlCN layer on the hard alloy substrate is deposited on the diamond-like rock layers of the TiAlCN layer surface and is formed in described The diamond coatings of diamond-like layer surface.Wherein, the hard alloy substrate is hard alloy cutter.
Based on above-mentioned, described TiAlCN layers with a thickness of 200~400nm.Described TiAlCN layers primarily serves Co element screen Layer is covered, the Co element in hard alloy substrate is mainly shielded and forms compound prevention Co element with Co element and expand to surface It dissipates, in order to avoid finally influence the bond strength of diamond thin and hard alloy substrate.So TiAlCN layers of the thickness cannot It is too thin, it is also It is not necessary to too thick, and too thick will increase cost.
Based on above-mentioned, the diamond-like rock layers with a thickness of 5~30nm.The diamond-like rock layers play diamond seeds layer Effect, mainly provide crystal seed for subsequent CVD method depositing diamond film.
Based on above-mentioned diamond-coated tools, further include be formed in the hard alloy substrate and it is TiAlCN layers described between CrAl layer, and described CrAl layers with a thickness of 50~250nm.Described CrAl layers mainly as the hard alloy substrate and institute State TiAlCN layers of transition zone, the too thin connection hard alloy substrate and TiAlCN layers described of cannot preferably playing of thickness Effect, it is also It is not necessary to too thick, and too thick will increase cost.
The present invention also provides a kind of preparation methods of above-mentioned diamond-coated tools, including firstly, cleaning carbide matrix Body；Coating film treatment is carried out on the hard alloy substrate again, forms TiAlCN layers and diamond-like rock layers；Then, using chemistry Surface deposition of diamond coatings of the vapour deposition process in the diamond-like rock layers.
Based on above-mentioned, the step of the coating film treatment further include: form the TiAlCN on the hard alloy substrate Before layer, CrAl layers are plated on the surface of the hard alloy substrate.
Based on above-mentioned, the method for the coating film treatment is arc ion plating method or magnetron sputtering embrane method.
Based on above-mentioned, the step of coating film treatment, includes:
The hard alloy substrate after cleaning is placed in coating machine, the intracorporal pressure of plated film chamber of the coating machine is 1 ×10-3~5 × 10-3Pa, back bias voltage be 80~100V, turntable speed be 0.3~0.6rpm, and temperature control 700 DEG C~ 800℃；
It is passed through argon gas into the plated film cavity with the flow of 120~180mln, selects CrAl composition target for CrAl coating Sputtering target material, the CrAl composition target power be 3000~4000W under conditions of, splashed on the surface of the hard alloy substrate 10~30min of deposition is penetrated, forms the CrAl layer with a thickness of 50~250nm, wherein the face of Cr and Al in the CrAl composition target Product is than being 5:3；
Nitrogen is passed through the plated film cavity with the flow and argon gas of 80~120mln with the flow of 40~60mln simultaneously It is interior, the sputtering target material of graphite target, TiAl composition target and titanium target as TiAlCN coating is selected, and in the power of the graphite target The item that power for 800~1200W, the TiAl composition target is 2500~3500W and the power of the titanium target is 250~350W Under part, 10~30min is deposited on CrAl layers of the surface, forms the TiAlCN layer with a thickness of 200~400nm, wherein described The area ratio of Al and Ti in TiAl composition target are 3:5；
Argon gas is passed through in the plated film cavity with the flow of 180~250mln, selects the graphite target for diamond-like The sputtering target material of layer, and under conditions of the power of the graphite target is 250~350W, it is heavy on TiAlCN layers of the surface 10~30min of product, forms the diamond-like rock layers with a thickness of 5~30nm.
Based on above-mentioned, the chemical vapour deposition technique is hot filament CVD or microwave plasma chemical gas phase Sedimentation.
Wherein, the step of diamond coatings being prepared using hot filament CVD are as follows: pressure be 0.5- 1.5kPa, under the conditions of temperature is 680-820 DEG C, using hot filament CVD, with H2And CH4It is reacting gas source in institute It states to precipitate on hard alloy substrate and reacts 16-32 hours formation nano diamond coatings on pre-treatment body, wherein CH4Gas body Product is the 1%~5% of overall reaction gas volume source.
The step of diamond coatings are prepared using MPCVD method are as follows: pressure be 0.5- 1.3k Pa, under the conditions of temperature is 700-800 DEG C, using MPCVD method, with H2And CH4For reaction gas 10-20 hours formation nano diamond coatings are reacted on processing body before the tungsten-cobalt alloy precipitates in body source, wherein microwave power For 6~9kW, CH4Gas volume in overall reaction gas volume source 1%~5%.
Based on above-mentioned, the step of cleaning hard alloy substrate includes: that the hard alloy substrate first successively exists It is ultrasonically treated in acetone, dehydrated alcohol and distilled water, is then dried in an oven again respectively.
Compared with prior art, TiAlCN is formed on the hard alloy substrate of diamond-coated tools provided by the invention Layer and diamond-like rock layers, the Co element shielded in the hard alloy substrate by described TiAlCN layer and with Co element formationization It closes object and prevents diffusion into the surface of the Co element to diamond-like rock layers, and the diamond-like rock layers can mention for diamond coatings growth For kind of a crystalline substance, so that the combination for enhancing the diamond coatings and hard alloy substrate prepared using chemical vapour deposition technique is strong Degree, so, diamond-coated tools provided by the invention have preferable cutting ability and longer service life.Further, The hard alloy substrate and it is TiAlCN layers described between be provided as the CrAl layer of transition zone, closed for enhancing the hard Auri body and it is TiAlCN layers described between binding force, to be further conducive to enhance the diamond coatings and carbide matrix The bond strength of body, to be conducive to improve the cutting ability and service life of diamond-coated tools.
The preparation method of diamond-coated tools provided by the invention, which mainly passes through, first cleans hard alloy substrate again hard CrAl layers, TiAlCN layers and diamond-like rock layers etc. are plated on matter alloy substrate, then use chemical vapor deposition diamond Coating, the preparation method avoid just can be reduced or avoid Co element to prepare chemical vapour deposition technique using a large amount of acid & alkali liquid Diamond coatings and hard alloy substrate bond strength influence, method is simple, and environmental protection, it is easy to industrialized production. Further, the present invention using arc ion plating method or magnetron sputtering embrane method plated on hard alloy substrate CrAl layers, TiAlCN layers and diamond-like rock layers etc., in particular by high-power impulse magnetron sputtering coating method formed it is CrAl layers described, TiAlCN layers and diamond-like rock layers, energy conservation and environmental protection.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the diamond-coated tools that the embodiment of the present invention 1 provides.
Fig. 2 is the structural schematic diagram for the diamond-coated tools that the embodiment of the present invention 2 provides.
Wherein, in each figure: hard alloy substrate 11, TiAlCN layer 13, diamond-like rock layers 14, diamond coatings 15, CrAl Layer 22.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention will be described in further detail.
Embodiment 1
Referring to Fig. 1, the embodiment of the present invention 1 provides a kind of diamond-coated tools, it is made of, specifically includes four-layer structure Hard alloy substrate 11, the TiAlCN layer 13 for being formed in 11 upper surface of hard alloy substrate, be deposited on it is TiAlCN layers described The diamond-like rock layers 14 of upper surface and the diamond coatings 15 for being formed in 14 surface of diamond-like rock layers, wherein the present embodiment In, the hard alloy substrate 11 is tungsten-cobalt alloy single dege blade.The TiAlCN layer 13 with a thickness of 400nm, the eka-gold Hard rock layer 14 with a thickness of 25nm.Wherein, the TiAlCN layer 13 mainly shields the Co element in hard alloy substrate 11 simultaneously Forming compound with Co element prevents Co element from spreading to the upper surface of hard alloy substrate 11, in order to avoid finally influence subsequent chemistry The bond strength of diamond thin and hard alloy substrate 11 that vapour deposition process deposition is prepared；The diamond-like rock layers 14 are main If providing crystal seed for subsequent chemistry vapour deposition process depositing diamond film.The thickness of the diamond coatings 15 is unlimited, excellent Be selected as 1~20 μm, depending on actual demand, in the present embodiment, the diamond coatings 15 with a thickness of 1 μm.Therefore, Above-mentioned diamond-coated tools provided in this embodiment have preferable cutting ability and longer service life.
The present embodiment also provides a kind of preparation method of above-mentioned diamond-coated tools, comprising steps of
Cleaning hard alloy substrate 11 surpasses the hard alloy substrate 11 respectively in acetone, dehydrated alcohol and distilled water Then the hard alloy substrate 11 is placed in baking oven and dries by sound 15min, the hard alloy substrate after being cleaned；
Hard alloy substrate 11 after the cleaning is placed in high-power impulse magnetron sputtering coating machine by coating film treatment, described The intracorporal pressure of plated film chamber of coating machine is 2 × 10-3Pa, back bias voltage 80V, turntable speed is 0.3rpm, and temperature control exists 700℃；
Argon gas is passed through in the plated film cavity with the flow and nitrogen of 120mln with the flow of 60mln simultaneously, selects stone The sputtering target material of black target, TiAl composition target and titanium target as TiAlCN coating, and the power of the graphite target be 800W, institute Under conditions of the power for stating TiAl composition target is 2500W and the power of the titanium target is 250W, in the hard alloy substrate 11 Upper surface deposit 30min, form the TiAlCN layer 13 with a thickness of 400nm, wherein Al's and Ti in the TiAl composition target Area ratio is 3:5；The purity of the sputtering target material of TiAlCN coating in this step is 99.999%, the purity of nitrogen and argon gas It is 99.999%；
Argon gas is passed through in the plated film cavity with the flow of 250mln, selects the graphite target splashing for diamond-like rock layers It shoots at the target material, and under conditions of the power of the graphite target is 250W, in the upper surface of the TiAlCN layer 13 deposition 25min forms the diamond-like rock layers 14 with a thickness of 25nm；
It is heavy on the surface of the diamond-like rock layers using MPCVD method to prepare diamond coatings The product diamond coatings are specifically that 0.5kPa utilizes microwave plasma chemical under the conditions of temperature is 700 DEG C in pressure Vapour deposition process, with H2And CH4React 7h formation on the hard alloy substrate for reacting gas source with a thickness of 1 μm of Buddha's warrior attendant Stone coating 15, wherein microwave power 9kW, CH4Gas volume in overall reaction gas volume source 3%.
Wherein, during above-mentioned coating film treatment, the purity of the various targets used is 99.999%, nitrogen and argon gas Purity be 99.999%.
Above-mentioned preparation method provided in this embodiment pre-processes hard alloy substrate using PVD method, in its table TiAlCN layers of face formation and diamond-like rock layers, the kind crystal layer of shielded layer and diamond thin respectively as hard alloy substrate, Method is simple, effects of energy conservation and environmental protection.
Embodiment 2
Referring to Fig. 2, the diamond-coated tools are five-layer structure the present embodiment provides a kind of diamond-coated tools, The main distinction of its diamond-coated tools provided with embodiment 1 is: diamond-coated tools provided in this embodiment are also Including the CrAl layer 22 being set between the hard alloy substrate 11 and TiAlCN layer 13, the CrAl layer 22 with a thickness of 200nm, the CrAl layer 22 are mainly used as transition zone, to increase the combination of the hard alloy substrate 11 and TiAlCN layer 13 Power；In the present embodiment, the superhard alloy matrix 11 be common alloy double bladed knife tool, the TiAlCN layer 13 with a thickness of 300nm, the diamond-like rock layers 14 with a thickness of 20nm, the diamond layer 15 with a thickness of 8 μm.
The present embodiment also provides a kind of preparation method of above-mentioned diamond-coated tools, comprising:
Cleaning hard alloy substrate 11 surpasses the hard alloy substrate 11 respectively in acetone, dehydrated alcohol and distilled water Then the hard alloy substrate 11 is placed in baking oven and dries by sound 15min, the hard alloy substrate after being cleaned；
Hard alloy substrate 11 after the cleaning is placed in high-power impulse magnetron sputtering coating machine by coating film treatment, described The intracorporal pressure of plated film chamber of coating machine is 2 × 10-3Pa, back bias voltage 90V, turntable speed is 0.5rpm, and temperature control exists 750℃；
It is passed through argon gas into the plated film cavity with the flow of 100mln, selects CrAl composition target for transition zone CrAl coating Sputtering target material, the CrAl composition target power be 3500W under conditions of, in the surface sputtering sedimentation of the hard alloy substrate 20min forms the CrAl layer 22 with a thickness of 200nm, wherein the area ratio of Cr and Al in the CrAl composition target are 5:3；
Nitrogen is passed through in the plated film cavity with the flow and argon gas of 100mln with the flow of 50mln simultaneously, selects stone The sputtering target material of black target, TiAl composition target and titanium target as TiAlCN coating, and the power of the graphite target be 1000W, Under conditions of the power of the TiAl composition target is 3000W and the power of the titanium target is 300W, in the upper of the CrAl layer 22 Surface deposits 20min, forms the TiAlCN layer 13 with a thickness of 300nm, wherein the area of Al and Ti in the TiAl composition target Than for 3:5；
Argon gas is passed through in the plated film cavity with the flow of 200mln, selects the graphite target splashing for diamond-like rock layers It shoots at the target material, and under conditions of the power of the graphite target is 300W, in the upper surface of the TiAlCN layer 13 deposition 20min forms the diamond-like rock layers 14 with a thickness of 20nm；
It prepares diamond coatings and Buddha's warrior attendant is deposited on the surface of the diamond-like rock layers 14 using hot filament CVD Stone coating 15, specifically: being 0.5kPa in pressure, under the conditions of temperature is 700 DEG C, using hot filament CVD, with H2 And CH4React 20h formation on the hard alloy substrate for reacting gas source with a thickness of 8 μm of diamond coatings 15, wherein CH4Gas volume in overall reaction gas volume source 3%.
Wherein, during above-mentioned coating film treatment, the purity of the various targets used is 99.999%, nitrogen and argon gas Purity be 99.999%.
Embodiment 3
The present embodiment provides a kind of diamond-coated tools and preparation method thereof, apply with the diamond that embodiment 2 provides The structure of layer cutter and preparation method thereof is essentially identical, and it is different with the thickness of diamond layer that difference essentially consists in each coating； Specifically, in the present embodiment, described CrAl layers with a thickness of 250nm, sedimentation time 15min；Described TiAlCN layers with a thickness of 200nm, sedimentation time 10min；The diamond-like rock layers with a thickness of 10nm, sedimentation time 10min；The thickness of the diamond layer Degree is 10 μm, reaction time 20h.
Embodiment 4
The present embodiment provides a kind of diamond-coated tools and preparation method thereof, apply with the diamond that embodiment 2 provides Layer cutter and preparation method thereof is essentially identical, and the thickness that difference essentially consists in each coating is different；Specifically, the present embodiment In, described CrAl layers with a thickness of 100nm, sedimentation time 10min；The diamond-like rock layers with a thickness of 15nm, sedimentation time 13min；The diamond layer with a thickness of 15 μm, the reaction time is for 24 hours.
Hard alloy substrate in the various embodiments described above is common various specifications hard alloy cutter, e.g., hard alloy Two sword ball knife of two blade milling cutters or hard alloy.It is applied below by performance verification verification experimental verification diamond provided in an embodiment of the present invention The performance of layer cutter.
The diamond-coated tools that 4 embodiment samples of subjects and corresponding 4 control samples provide
Embodiment sample:, should respectively using 4 kinds of hard alloy cutters shown in table 1 as the diamond-coated tools of matrix The structure of coated cutting tool is identical as the structure of diamond-coated tools that the embodiment of the present invention 2 provides.
Control sample: 4 kinds of hard alloy substrates shown in table 1 after the de- Co of soda acid processing, are in pressure respectively 0.5kPa, under conditions of temperature is 700 DEG C, using hot filament CVD, with H2、CH4For reacting gas source, in de- Co The surface of hard alloy substrate afterwards forms the diamond coatings that thickness is about 8 μm, obtains control group diamond-coated tools, Wherein, CH4Gas volume in overall reaction gas volume source 3%.The detailed process of the soda acid processing are as follows: (1) exist Ultrasonic vibration 20min in Murakami reagent, solution quality proportion are m (KOH) ︰ m (K3[Fe(CN)6]) ︰ m (H2O)=1 1 ︰ of ︰ 10；(2)H2SO4+H2O2Ultrasonic vibration 20s, liquor capacity proportion are V (H2SO4) ︰ V (H2O2The ︰ of)=3 7, then, in acetone soln Middle ultrasonic cleaning 5min simultaneously dries, to have the function that remove surface smut and reach de- Co.
The material and specification of 1 hard alloy substrate of table
Serial number Title Material Specification
1 Two blade milling cutter of alloy Tungsten-cobalt series hard alloy D0.81*2*D4*50*2F
2 Two blade milling cutter of alloy Tungsten-cobalt series hard alloy D0.8*0.6*3*D4*50*2F
3 Two blade milling cutter of alloy Tungsten-cobalt series hard alloy D0.8*1.6*D0.75*5*D4*50*2F
4 Two sword ball knife of alloy Tungsten-cobalt series hard alloy R1.5*15*D3*60L*2F
(1) adhesion strength checking test method provides above-mentioned 4 embodiment samples and 4 control samples using scratching instrument Diamond-coated tools do impression test, test result is as shown in table 2.
The adhesion strength observed result of 2 diamond-coated tools of table
As can be seen from Table 2: the binding force of diamond-coated tools provided in an embodiment of the present invention and traditional soda acid The binding force for handling the coated cutting tool of preparation is suitable, therefore, provides the diamond coatings in diamond-coated tools by the present invention There is stronger binding force with hard alloy substrate.
(2) it cutting ability checking test method: is applied respectively using the diamond that 4 pairs of embodiment samples and control sample provide Layer cutter is processed workpieces processing, by the cutting for testing workpieces processing quantity validation each group diamond-coated tools Performance, test result are as shown in table 6.
3 diamond-coated tools cutting ability test result of table
As can be seen from Table 3: other than workpieces processing is ceramics, the diamond-coated tools that control sample provides can Workpieces processing, which is processed into the quantity that surface roughness is R0.8 and the diamond-coated tools that embodiment sample provides, to incite somebody to action Workpieces processing be processed into surface roughness be R0.6 quantity it is essentially identical, workpieces processing be ceramics when, control group coated cutting tool Processing quantity significantly lower than sample sets coated cutting tool, so, it is in workpieces processing and the surface roughness of workpiece difference identical Under conditions of, the workpieces processing quantity for the diamond-coated tools that embodiment sample provides can be significantly hotter than control sample offer Thus the workpieces processing quantity of diamond-coated tools illustrates the cutting ability for the diamond-coated tools that embodiment sample provides The cutting ability and service life of the diamond-coated tools of control sample offer are provided with service life.
Finally it should be noted that: the above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；To the greatest extent The present invention is described in detail with reference to preferred embodiments for pipe, it should be understood by those ordinary skilled in the art that: still It can modify to a specific embodiment of the invention or some technical features can be equivalently replaced；Without departing from this hair The spirit of bright technical solution should all cover within the scope of the technical scheme claimed by the invention.

Claims (10)

1. a kind of diamond-coated tools characterized by comprising hard alloy substrate is formed in the hard alloy substrate On TiAlCN layer, be deposited on the diamond-like rock layers of the TiAlCN layer surface and be formed in the gold of the diamond-like layer surface Hard rock coating.
2. diamond-coated tools according to claim 1, which is characterized in that described TiAlCN layers with a thickness of 200~ 400 nm。
3. diamond-coated tools according to claim 1, which is characterized in that the diamond-like rock layers with a thickness of 5~ 30 nm。
4. diamond-coated tools according to claim 1 or 2 or 3, which is characterized in that further include being formed in the hard Alloy substrate and it is TiAlCN layers described between CrAl layer, and described CrAl layers with a thickness of 50~250 nm.
5. a kind of preparation method of the described in any item diamond-coated tools of Claims 1 to 4, comprising: firstly, cleaning hard Alloy substrate；Coating film treatment is carried out on the hard alloy substrate again, forms TiAlCN layers and diamond-like rock layers；Then, it adopts With chemical vapour deposition technique the diamond-like rock layers surface deposition of diamond coatings.
6. the preparation method of diamond-coated tools according to claim 5, which is characterized in that the step of the coating film treatment It suddenly further include before plating TiAlCN film on the hard alloy substrate, plating CrAl on the surface of the hard alloy substrate Layer.
7. the preparation method of diamond-coated tools according to claim 6, which is characterized in that the side of the coating film treatment Method is arc ion plating method or magnetron sputtering embrane method.
8. the preparation method of diamond-coated tools according to claim 7, which is characterized in that the step of the coating film treatment Suddenly include:
The hard alloy substrate after cleaning is placed in coating machine, the intracorporal pressure of plated film chamber of the coating machine is 1 × 10-3 ~5 × 10-3Pa, back bias voltage are 80~100 V, and turntable speed is 0.3~0.6 rpm, and temperature control is 700 DEG C~800 ℃；
It is passed through argon gas into the plated film cavity with the flow of 120~180 mln, selects CrAl composition target splashing for CrAl coating It shoots at the target material, which sputters under conditions of power is 3000~4000 W on the surface of the hard alloy substrate 10~30 min are deposited, form the CrAl layer with a thickness of 50~250 nm, wherein the face of Cr and Al in the CrAl composition target Product is than being 5:3；
Nitrogen is passed through in the plated film cavity with the flow and argon gas of 80~120 mln with the flow of 40~60 mln simultaneously, The sputtering target material of graphite target, TiAl composition target and titanium target as TiAlCN coating is selected, and is in the power of the graphite target 800~1200 W, the TiAl composition target power be 2500~3500 W and the power of the titanium target is 250~350 W Under the conditions of, 10~30 min are deposited on CrAl layers of the surface, form the TiAlCN layer with a thickness of 200~400 nm, wherein The area ratio of Al and Ti in the TiAl composition target are 3:5；
Argon gas is passed through in the plated film cavity with the flow of 180~250 mln, selects the graphite target for diamond-like rock layers Sputtering target material, and under conditions of the power of the graphite target is 250~350 W, it is deposited on TiAlCN layers of the surface 10~30 min form the diamond-like rock layers with a thickness of 5~30 nm.
9. according to the preparation method of the described in any item diamond-coated tools of claim 5~8, which is characterized in that describedization Learning vapour deposition process is hot filament CVD or MPCVD method.
10. the preparation method of diamond-coated tools according to claim 9, which is characterized in that the cleaning is described hard The step of matter alloy substrate includes: that the hard alloy substrate first successively carries out in acetone, dehydrated alcohol and distilled water respectively Ultrasonic treatment, is then dried in an oven again.
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