CN112404435A - Diamond compact and preparation method thereof - Google Patents

Diamond compact and preparation method thereof Download PDF

Info

Publication number
CN112404435A
CN112404435A CN202011187945.0A CN202011187945A CN112404435A CN 112404435 A CN112404435 A CN 112404435A CN 202011187945 A CN202011187945 A CN 202011187945A CN 112404435 A CN112404435 A CN 112404435A
Authority
CN
China
Prior art keywords
cleaning
titanium
diamond
wear
diamond particles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202011187945.0A
Other languages
Chinese (zh)
Other versions
CN112404435B (en
Inventor
孔帅斐
张敏捷
李和鑫
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henan Fulaige Ultrahard Material Co ltd
Original Assignee
Henan Fulaige Ultrahard Material Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henan Fulaige Ultrahard Material Co ltd filed Critical Henan Fulaige Ultrahard Material Co ltd
Priority to CN202011187945.0A priority Critical patent/CN112404435B/en
Publication of CN112404435A publication Critical patent/CN112404435A/en
Application granted granted Critical
Publication of CN112404435B publication Critical patent/CN112404435B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
    • 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
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • 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
    • C23C16/44—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 method of coating
    • C23C16/4417—Methods specially adapted for coating powder
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • B22F2007/042—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Polishing Bodies And Polishing Tools (AREA)

Abstract

The invention provides a diamond compact which mainly comprises polycrystalline diamond particles, a wear-resistant metal compound coating and a metal adhesive, wherein the wear-resistant metal compound coating is formed on the surfaces of the polycrystalline diamond particles, and the metal adhesive is filled between the adjacent wear-resistant metal compound coatings. The invention also provides a preparation method of the diamond compact, which comprises the following steps: diamond particle pretreatment, wear-resistant metal compound coating formation, substrate cleaning and compact pressing and sintering. Specifically, the composite diamond particles are formed by depositing the wear-resistant metal compound coating with good wear resistance on the surfaces of the diamond particles, and after the composite diamond particles are uniformly mixed with the metal binder, the high-temperature and high-pressure sintering treatment is carried out on the surfaces of the clean hard alloy substrates to prepare the polycrystalline diamond compact.

Description

Diamond compact and preparation method thereof
Technical Field
The invention belongs to the technical field of superhard material processing, and particularly relates to a diamond compact and a preparation method thereof.
Background
Diamond is widely used in various fields because of its high hardness, high chemical stability, high wear resistance and low friction coefficient. The use efficiency is often reduced during processing and use due to processing graphitization. Diamond tools refer to finished products, such as grinding tools, cutters and drilling tools, which are made of diamond particles as cutting materials by pressing, sintering and processing with the aid of binders or other auxiliary materials into certain shapes and uses. Diamond has poor chemical affinity for some bonding metals or alloys during use and is not easily wetted by them, resulting in poor application properties. The diamond abrasive is easy to fall off during the use of the grinding tool due to the low bonding strength between the bonding agent and the abrasive, and the service life of the abrasive is shortened.
The chemical plating used at present is facing the challenge of updating because waste acid and waste alkali which can generate serious influence on environment in the process of preparing diamond. The vacuum micro-evaporation plating can carry out plating treatment on the surface of the diamond, but at present, metal plating is mainly carried out, and the treatment is usually nickel plating, titanium plating, tungsten plating, chromium plating and the like.
The coated cutting tool is characterized in that one or more layers of refractory metals or metal compounds with wear resistance are deposited on the surface of a superhard cutting blade made of ceramics, diamond or cubic boron nitride by utilizing a vapor deposition technology, although the wear resistance and the service life of the cutting tool can be improved to a certain extent by the method, the problem of bonding strength between a wear-resistant material and the superhard cutting blade still exists due to the fact that the wear-resistant material is formed on the surface of the superhard cutting blade, the wear-resistant material is also lost along with the use of the coated cutting tool, and when the wear-resistant material is lost to a certain extent, the service life of the coated cutting tool is still seriously influenced although the wear-resistant material is small in loss of the superhard cutting blade.
Disclosure of Invention
In view of this, the present invention provides a diamond compact and a method for manufacturing the same, so that the manufactured diamond compact has high performance, the utilization efficiency of the diamond compact is high, the cost can be saved, and the production cost of an enterprise can be reduced.
To this end, the present invention provides a diamond compact which is mainly composed of polycrystalline diamond particles, a wear-resistant metal compound coating layer formed on the surfaces of the polycrystalline diamond particles, and a metal binder filled between adjacent wear-resistant metal compound coating layers.
Based on the above, the wear-resistant metal compound coating is titanium carbide, chromium carbide, aluminum carbide, silicon carbide or any combination thereof.
The invention also provides a preparation method of the diamond compact, which comprises the following steps:
diamond particle pretreatment, namely performing acid-base treatment on diamond particles, and then performing ultrasonic water washing and drying to obtain clean diamond particles;
forming a wear-resistant metal compound coating and depositing the wear-resistant metal compound coating on the surface of the clean diamond particles to obtain composite diamond particles;
carrying out sand blasting treatment on a hard alloy matrix by matrix cleaning, and removing impurities and an oxide layer on the surface of the hard alloy matrix to obtain a first-time cleaned matrix; under the action of a water-based cleaning agent, cleaning the first cleaning substrate by using ultrasonic waves; vacuum drying to obtain a clean matrix;
pressing and sintering the composite sheet, and uniformly mixing the composite diamond particles and a metal binding agent according to the mass percentage of 75-85% and 15-25% to form a mixture; spreading the mixture on the surface of the clean matrix; and then sintering for 20-30 min under the conditions of 3.8-4.5 GPa and 1280-1350 ℃ to obtain the polycrystalline diamond compact.
Based on the above, the diamond particle pretreatment step comprises: respectively cooking diamond particles with the particle size of 7-40 mu m in 20-25% of nitric acid and 20-25% of sodium hydroxide solution by mass percent for 20-35 min, ultrasonically cleaning the cooked diamond particles in distilled water for 15-40 min, and then drying to obtain the clean diamond particles.
Based on the above, the step of forming the wear-resistant metal compound coating comprises: depositing the wear-resistant metal compound coating on the surface of the clean diamond particles by a vacuum coating method at 530-610 ℃ in a mixed atmosphere of hydrogen and acetone to obtain the composite diamond particles; wherein, the material of the wear-resistant metal compound coating is titanium carbide, chromium carbide, aluminum carbide, silicon carbide or any combination thereof.
Based on the above, the step of forming the wear-resistant metal compound coating comprises:
placing the clean diamond particles on a substrate table of a coating machine chamber, and vacuumizing until the vacuum degree is 1 multiplied by 10-3～3×10-3Pa; heating the substrate table to 550-600 ℃, wherein the rotating speed of the substrate table is 10-15 rad/min, the deposition current is 100A, and hydrogen is introduced into the film plating machine at the flow rate of 50-65 sccm with acetone;
depositing for 1-2 h by using a titanium-aluminum target with the deposition power of 3000-4000W and a titanium target with the deposition power of 2000-2500W, and forming a composite coating of titanium carbide and aluminum carbide on the surface of the clean diamond particles;
simultaneously depositing for 1-2 h by using a titanium-aluminum target with the deposition power of 3000-4000W, a titanium-silicon target with the deposition power of 1000-1500W and a titanium target with the deposition power of 1000-1500W to form a composite coating of titanium carbide, aluminum carbide and silicon carbide on the titanium carbide and aluminum carbide alloy layer;
depositing for 1-2 hours by using a titanium-aluminum target with the deposition power of 3000-4000W, a titanium-chromium target with the deposition power of 1000-1500W and a titanium target with the deposition power of 1000-1500W to form a composite coating of chromium carbide, titanium carbide and an aluminum carbide layer on the composite coating of titanium carbide, aluminum carbide and silicon carbide;
and finally cooling to room temperature, decompressing and taking out the composite diamond particles.
Based on the above, the substrate cleaning step comprises:
placing the hard alloy matrix in a wet sand blasting machine to perform sand blasting treatment on the surface of the hard alloy matrix, and removing impurities and an oxidation layer on the surface of the hard alloy matrix to obtain a first-time cleaning matrix;
placing the first cleaning matrix in the water-based cleaning agent with higher concentration, cleaning for 10-15 min by adopting ultrasonic waves for the first time to peel off dirt on the surface of the first cleaning matrix, and then washing with tap water to obtain a second cleaning matrix;
placing the secondary cleaning matrix in the water-based cleaning agent with lower concentration, cleaning for 10-15 min by ultrasonic again to decompose and emulsify greasy dirt on the surface of the secondary cleaning matrix, and then washing with tap water to obtain a tertiary cleaning matrix;
placing the three-time cleaning substrate in high-purity water, and rinsing for 10-15 min by adopting ultrasonic waves for the third time to wash off the water-based cleaning agent remained on the surface of the three-time cleaning substrate, so as to obtain a four-time cleaning substrate;
and (3) drying the substrate cleaned for four times in a vacuum drying oven for 10-20 min to obtain the clean substrate.
Based on the above, the water-based cleaning agent comprises the following components in percentage by mass: 2.5-10% of alkanolamine neutralizing carbonic acid, 2.5-10% of alkaline carbonate, 2.5-10% of sodium silicate pentahydrate, 2.5-10% of polyalkoxylated fatty alcohol, less than or equal to 2.5% of monoethanolamine reactant, less than or equal to 2.5% of ethylhexyl sulfate, and the balance of water.
Based on the above, the mass fraction of the higher-concentration water-washing cleaning agent is 5% -7%, and the mass fraction of the lower-concentration water-washing cleaning agent is 3% -5%.
Based on the above, in the step of cleaning the substrate, the ultrasonic frequency range of each ultrasonic cleaning is 20-80 kHz, the ultrasonic power is 1800-3600W, and the tap water, the high purity water and the water-based cleaning agent are all heated to 50-60 ℃ when in use.
Based on the above, the cleaning substrate for four times is subjected to boriding treatment after being dried, so that the clean substrate is obtained.
Based on the above, the gas for boriding treatment is B with the volume fraction of 10%2H6And 90% of H2The flow rate of the mixed gas is 10-15 sccm, the pressure is 8-10 kPa, and the reaction time is 3-5 h. Wherein, the flow rate in the step is selected to be 10-15 sccm, mainly because experiments show that when the gas flow is lower than 10 sccm, the thickness of the formed cobalt compound layer is small and cannot play the expected role of resisting Co diffusion; when the flow is too large, elemental boron will appear in the hard alloy matrix, and the bonding strength will be affected because the cleaning is difficult in the later period.
Based on the above, the metal binder is selected from two or more of titanium, aluminum, cobalt and chromium.
Based on the above, the polycrystalline diamond compact is subjected to centerless grinding to a required diameter size, and then surface polishing treatment is carried out to obtain the diamond compact.
Compared with the prior art, the diamond compact provided by the invention mainly comprises polycrystalline diamond particles, a wear-resistant metal compound coating and a metal adhesive, wherein the wear-resistant metal compound coating is formed on the surfaces of the polycrystalline diamond particles, the metal adhesive is filled between the adjacent wear-resistant metal compound coatings, the composite diamond particles are mainly formed by depositing the wear-resistant metal compound coating with good wear resistance on the surfaces of the polycrystalline diamond particles, and after the composite diamond particles are uniformly mixed with the metal adhesive, the composite diamond particles are subjected to high-temperature and high-pressure sintering treatment on the surfaces of clean hard alloy matrixes; the wear-resistant metal compound coating plated on the surfaces of the diamond particles, the metal binding agent and the diamond have good bonding strength simultaneously, the metal binding agent and the diamond particles can be connected, the holding force is enhanced, and early falling is prevented. In addition, the film coated on the surfaces of the diamond particles is a metal compound material with high wear resistance, the wear resistance of the polycrystalline diamond can be enhanced, and the polycrystalline diamond particles with the wear-resistant diamond compounds formed on the surfaces are uniformly dispersed in the diamond compact, so that the diamond compact provided by the invention has better wear resistance.
Further, in the preparation method provided by the invention, a vacuum coating method is adopted, acetone in a mixed atmosphere of hydrogen and acetone and under the action of high temperature of 530-610 ℃, the acetone in the mixed atmosphere is decomposed and chemically reacts with the metal target material to form a wear-resistant metal compound, and then the wear-resistant metal compound is uniformly deposited on the surfaces of the diamond particles, so that the wear-resistant metal compound coating is formed on the surfaces of the diamond particles.
Furthermore, the preparation method provided by the invention can remove oil stains on the surface of the hard alloy matrix and also remove an oxide layer and other impurities in the hard alloy matrix by sequentially carrying out sand blasting treatment and water-based cleaning agent combined ultrasonic cleaning on the hard alloy matrix; therefore, the surface cleanliness of the hard alloy substrate can be effectively improved, the bonding strength between the polycrystalline diamond compact and the hard alloy substrate is favorably improved, and the abrasion resistance of the subsequently prepared polycrystalline diamond compact is favorably improved.
Further, the preparation method provided by the invention also comprises the step of carrying out boronizing treatment on the hard alloy matrix, wherein the boronizing treatment is mainly used for forming CoWB and W2CoB2And d, reducing or avoiding the diffusion effect of Co in the hard alloy matrix by using the compounds, so as to further improve the bonding strength of the polycrystalline diamond compact and the hard alloy prepared subsequently and improve the wear resistance of the polycrystalline diamond compact.
Drawings
Fig. 1 is a photographic view of a diamond compact provided by an embodiment of the present invention.
Fig. 2 is a schematic view of the structure of the diamond compact shown in fig. 1.
Fig. 3 is a photograph of composite diamond particles formed during the practice of an embodiment of the present invention.
Wherein reference numerals in the figures denote: 1. polycrystalline diamond particles, 2, a wear-resistant metal compound coating, 3 and a metal binder.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
Referring to fig. 1 and 2, the present embodiment provides a diamond compact, which mainly includes polycrystalline diamond particles 1, a wear-resistant metal compound coating 2 formed on the surface of the polycrystalline diamond particles, and a metal binder 3 filled in the adjacent wear-resistant metal compound coating 2. That is, the diamond compact provided in this embodiment mainly includes polycrystalline diamond composite particles and a metal binder 3 that connects adjacent polycrystalline diamond composite particles, and the polycrystalline diamond composite particles include polycrystalline diamond particles 1 and a wear-resistant metal compound coating layer 2 formed on the surface of the polycrystalline diamond particles.
The embodiment of the invention provides a preparation method of the diamond compact, which comprises the following steps:
firstly, diamond particle pretreatment
And (3) steaming and boiling the diamond particles with the particle size of 28-40 mu m in nitric acid with the mass percent of 25% and sodium hydroxide solution with the mass percent of 25% for 30 minutes in sequence. The boiled diamond was cleaned in distilled water using ultrasonic waves for minutes. And drying the diamond subjected to ultrasonic treatment to obtain clean diamond particles.
Secondly, forming a wear-resistant metal compound coating
Putting the clean diamond particles on a substrate table of a coating machine chamber, and vacuumizing until the vacuum degree is 1 multiplied by 10-3～3×10-3Pa; heating the substrate table to about 580 ℃, rotating the substrate table at 10-15 rad/min by taking titanium, titanium aluminum with the area ratio of 5:3, titanium silicon with the area ratio of 5:1 and titanium chromium with the area ratio of 5:2 as targets and enabling the diamond placed on the substrate table to freely roll,the deposition current is 100A, and the hydrogen is introduced into the film plating machine with acetone at the flow rate of about 60 sccm;
depositing for 2 hours under the deposition power of about 3500W of the titanium-aluminum target and about 2400W of the titanium target by taking the titanium-aluminum target and the titanium target as target materials, and uniformly forming a composite coating of titanium carbide and aluminum carbide on the surface of the clean diamond particles;
taking a titanium aluminum target, a titanium silicon target and a titanium target as target materials, simultaneously depositing for 1.5 h under the deposition power of about 3600W of the titanium aluminum target, about 1300W of the titanium silicon target and about 1200W of the titanium target, and uniformly forming a composite coating of titanium carbide, aluminum carbide and silicon carbide on the composite layer of the titanium carbide and the aluminum carbide;
then, taking a titanium-aluminum target, a titanium-chromium target and a titanium target as target materials, simultaneously depositing for 1 h under the deposition power of about 3500W of the titanium-aluminum target, about 1400W of the titanium-chromium target and about 1300W of the titanium target, and uniformly forming a composite coating of titanium carbide, aluminum carbide and chromium carbide on the composite coating of the titanium carbide, the aluminum carbide and the silicon carbide;
and finally, cooling to room temperature after deposition is finished, and decompressing and taking out the composite diamond particles, as shown in figure 3.
Thirdly, cleaning the substrate
And carrying out sand blasting treatment on the surface of the hard alloy matrix on a wet sand blasting machine to remove impurities and an oxide layer on the surface of the hard alloy matrix so as to obtain a first-time cleaning matrix.
Under the action of a water-based cleaning agent, the dirt on the surface of a cleaned substrate workpiece is peeled off and peeled off by adopting ultrasonic cleaning with the ultrasonic frequency range of 20-80 kHz and the ultrasonic power of 1800-3600W, and meanwhile, the greasy dirt can be decomposed and emulsified. The method specifically comprises two stages:
the first stage, placing a first cleaning matrix under 6% of water-based cleaning agent by mass, starting ultrasonic cleaning equipment to clean a workpiece to be cleaned for 17 min under the action of the water-based cleaning agent with the concentration and ultrasonic waves, stripping off dirt on the surface of the first cleaning matrix after the ultrasonic cleaning is finished, and then flushing away residual cleaning medium on the surface of the workpiece by using tap water to obtain a second cleaning matrix;
secondly, placing the secondary cleaning substrate under a water-based cleaning agent with the mass fraction of 4% for ultrasonic cleaning for 17 min again, decomposing and emulsifying greasy dirt on the surface of the secondary cleaning substrate after cleaning is finished, and then washing away residual cleaning medium again by using tap water to obtain a tertiary cleaning substrate;
placing the three-time cleaning substrate in high-purity water, and rinsing for 17 min by adopting ultrasonic waves to thoroughly wash off the cleaning medium remained on the surface of the hard alloy, thereby obtaining a four-time cleaning substrate;
placing the four-time cleaning matrix in a vacuum drying oven for drying for 17 min; putting the dried cleaned substrate of the fourth time into a vacuum tube type drying furnace for boriding treatment to obtain a clean substrate; wherein the atmosphere in the boriding treatment is B with a volume fraction of 10%2H6And 90% of H2The flow rate of the mixed gas is about 12 sccm, the pressure is about 10 kPa, and the reaction time is about 4 hours.
Tap water, high-purity water and the water-based cleaning agent adopted in the step of cleaning the substrate are all heated to 50-60 ℃ when in use.
The water-based cleaning agent comprises the following components in percentage by mass: 5% of alkanolamine neutralizing carbonic acid, 8% of alkaline carbonate, 6% of sodium pentahydrate, 9% of polyalkoxylated fatty alcohol, 2.5% of monoethanolamine reactant, 2% of ethylhexyl sulfate and the balance of water.
Fourthly, pressing and sintering the composite sheet
Uniformly mixing the composite diamond particles and a metal binder with a median particle size of 0.5 mu m according to the mass percentage of 80% and 20% respectively to obtain a mixture, wherein the metal binder consists of titanium, aluminum and cobalt in the mass ratio of 8:2: 1; then the clean matrix is placed in the pyrophyllite cavity, the calculated mixture is placed on the surface of the clean matrix, and the clean matrix is spread uniformly; and sintering the polycrystalline diamond compact for about 25 min at the temperature of about 4.2 GPa and about 1300 ℃ to obtain the polycrystalline diamond compact. And then, machining the obtained polycrystalline diamond to a required diameter size through centerless grinding, and polishing the surface to obtain the diamond compact shown in fig. 1.
Performance verification
Control group 1: control group 1 provided a diamond compact, which was prepared by a method that, compared with the preparation method provided by the present invention, mainly omitted the aforementioned "second, wear-resistant metal compound coating" step, i.e., no wear-resistant metal compound coating was formed on the surface of the diamond particles.
Control group 2: the TiAlCrC coating is deposited on the surface of the diamond compact provided by the control group 1 by adopting a PVD method.
The test conditions are as follows: the diamond compact provided by the embodiment of the invention and the diamond compacts provided by the control groups 1-2 are respectively subjected to abrasion ratio, impact resistance and hardness tests, and relevant test data are shown in table 1.
The test method of the abrasion ratio comprises the following steps: referring to JB-T3235-1999, under the specified conditions, the composite sheet is mixed with 80# grain ceramic bond grinding wheel silicon carbide parallel grinding wheel, and the abrasion loss M of the grinding wheels(g) And abrasion ratio M of composite sheetj(g) The ratio of the ratios is called the wear ratio E of the composite sheet, wherein E = Ms(g)/Mj(g)。
The test method of the impact resistance comprises the following steps: the usual method is the gradient method, first of all 10 samples are pretested to estimate the impact energy at 50% failure, on the basis of which an energy close to that at which the sample is impact-broken is selected, the first sample is impacted, it is observed whether the sample is broken, if it is broken, an energy value Δ E is decreased, the second sample is impacted, if it is not broken, a Δ E is added, and this is repeated and impact tests are carried out on at least 20 samples. Wherein the energy increment delta E can be increased according to 5-15% of the destruction energy of the pretest. E = H × g × M; m = M0+△M（A/N±0.5）；A=Σnizi; M0-The minimum drop weight mass of the experiment; the weight of the Delta M drop weight is increased and Kg; h, the falling height of the drop hammer; g, free acceleration; total number N of samples with or without N destructioniAt MiNumber of samples destroyed or not destroyed, ziFrom M0The number of mass increases is started.
Hardness test method: by pressing in, the indenter is very smallThe diamond cone of (2) and a square cone pressure head (Vikers pressure head) with the included angle of the conical surface of 136 degrees. The pressure head is vertically pressed into the surface of a tested sample to generate dents under the action of a certain load, and the pressure born by the unit area is the Vickers hardness. The calculation formula is as follows: hv =1854.4P/d2The preferred values in the formula, Hv-Vickers hardness, P-load (gf), and d-indentation diagonal length (. mu.m) are shown in the specification of the method of using the Vickers hardness tester.
Table 1 diamond compact performance test results
Figure DEST_PATH_IMAGE002
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.

Claims (14)

1. A diamond compact is characterized by mainly comprising polycrystalline diamond particles, a wear-resistant metal compound coating and a metal adhesive, wherein the wear-resistant metal compound coating is formed on the surfaces of the polycrystalline diamond particles, and the metal adhesive is filled between the adjacent wear-resistant metal compound coatings.
2. The diamond compact of claim 1, wherein the wear resistant metal compound coating is titanium carbide, chromium carbide, aluminum carbide, silicon carbide, or any combination thereof.
3. A method for preparing a diamond compact, comprising the steps of:
diamond particle pretreatment, namely performing acid-base treatment on diamond particles, and then performing ultrasonic water washing and drying to obtain clean diamond particles;
forming a wear-resistant metal compound coating and depositing the wear-resistant metal compound coating on the surface of the clean diamond particles to obtain composite diamond particles;
carrying out sand blasting treatment on a hard alloy matrix by matrix cleaning, and removing impurities and an oxide layer on the surface of the hard alloy matrix to obtain a first-time cleaned matrix; under the action of a water-based cleaning agent, cleaning the first cleaning substrate by using ultrasonic waves; vacuum drying to obtain a clean matrix;
pressing and sintering the composite sheet, and uniformly mixing the composite diamond particles and a metal binding agent according to the mass percentage of 75-85% and 15-25% to form a mixture; spreading the mixture on the surface of the clean matrix; and then sintering for 20-30 min under the conditions of 3.8-4.5 GPa and 1280-1350 ℃ to obtain the polycrystalline diamond compact.
4. The method of making a diamond compact of claim 3, wherein the diamond particle pre-treatment step comprises: respectively cooking diamond particles with the particle size of 7-40 mu m in 20-25% of nitric acid and 20-25% of sodium hydroxide solution by mass percent for 20-35 min, ultrasonically cleaning the cooked diamond particles in distilled water for 15-40 min, and then drying to obtain the clean diamond particles.
5. The method of making a diamond compact of claim 3, wherein the step of forming a wear resistant metal compound coating comprises: depositing the wear-resistant metal compound coating on the surface of the clean diamond particles by a vacuum coating method at 530-610 ℃ in a mixed atmosphere of hydrogen and acetone to obtain the composite diamond particles; wherein, the material of the wear-resistant metal compound coating is titanium carbide, chromium carbide, aluminum carbide, silicon carbide or any combination thereof.
6. The method of making a diamond compact of claim 5, wherein the step of forming a wear resistant metal compound coating comprises:
placing the clean diamond particles on a substrate table of a coating machine chamber, and vacuumizing until the vacuum degree is 1 multiplied by 10-3～3×10-3Pa; heating the substrate table to 550-600 ℃, wherein the rotating speed of the substrate table is 10-15 rad/min, the deposition current is 100A, and hydrogen is introduced into the film plating machine at the flow rate of 50-65 sccm with acetone;
depositing for 1-2 h by using a titanium-aluminum target with the deposition power of 3000-4000W and a titanium target with the deposition power of 2000-2500W, and forming a composite coating of titanium carbide and aluminum carbide on the surface of the clean diamond particles;
simultaneously depositing for 1-2 h by using a titanium-aluminum target with the deposition power of 3000-4000W, a titanium-silicon target with the deposition power of 1000-1500W and a titanium target with the deposition power of 1000-1500W to form a composite coating of titanium carbide, aluminum carbide and silicon carbide on the titanium carbide and aluminum carbide alloy layer;
depositing for 1-2 hours by using a titanium-aluminum target with the deposition power of 3000-4000W, a titanium-chromium target with the deposition power of 1000-1500W and a titanium target with the deposition power of 1000-1500W to form a composite coating of chromium carbide, titanium carbide and an aluminum carbide layer on the composite coating of titanium carbide, aluminum carbide and silicon carbide;
and finally cooling to room temperature, decompressing and taking out the composite diamond particles.
7. The method of making a diamond compact according to any of claims 3 to 6, wherein the step of cleaning the substrate comprises:
placing the hard alloy matrix in a wet sand blasting machine to perform sand blasting treatment on the surface of the hard alloy matrix, and removing impurities and an oxidation layer on the surface of the hard alloy matrix to obtain a first-time cleaning matrix;
placing the first cleaning matrix in the water-based cleaning agent with higher concentration, cleaning for 10-15 min by adopting ultrasonic waves for the first time to peel off dirt on the surface of the first cleaning matrix, and then washing with tap water to obtain a second cleaning matrix;
placing the secondary cleaning matrix in the water-based cleaning agent with lower concentration, cleaning for 10-15 min by ultrasonic again to decompose and emulsify greasy dirt on the surface of the secondary cleaning matrix, and then washing with tap water to obtain a tertiary cleaning matrix;
placing the three-time cleaning substrate in high-purity water, and rinsing for 10-15 min by adopting ultrasonic waves for the third time to wash off the water-based cleaning agent remained on the surface of the three-time cleaning substrate, so as to obtain a four-time cleaning substrate;
and (3) drying the substrate cleaned for four times in a vacuum drying oven for 10-20 min to obtain the clean substrate.
8. The preparation method of the diamond compact of claim 7, wherein the water-based cleaning agent comprises the following components in percentage by mass: 2.5-10% of alkanolamine neutralizing carbonic acid, 2.5-10% of alkaline carbonate, 2.5-10% of sodium silicate pentahydrate, 2.5-10% of polyalkoxylated fatty alcohol, less than or equal to 2.5% of monoethanolamine reactant, less than or equal to 2.5% of ethylhexyl sulfate, and the balance of water.
9. The method of claim 8, wherein the higher concentration of the water-washing cleaning agent is 5-7% by mass, and the lower concentration of the water-washing cleaning agent is 3-5% by mass.
10. The method for preparing a diamond compact according to claim 8, wherein in the step of cleaning the substrate, the ultrasonic frequency range of each ultrasonic cleaning is 20 to 80 kHz, the ultrasonic power is 1800 to 3600W, and the tap water, the high purity water and the water-based cleaning agent are all heated to 50 to 60 ℃ when in use.
11. The method of claim 8, wherein the four times of cleaning the substrate after drying is boronized to obtain the clean substrate.
12. The method of making a diamond compact of claim 11, wherein the boronizing gas is 10 volume percent B2H6And 90% of H2The flow rate of the mixed gas is 10-15 sccm, the pressure is 8-10 kPa, and the reaction time is 3-5 h.
13. The method of manufacturing a diamond compact according to claim 3 or 12, wherein the metal binder is selected from two or more of titanium, aluminum, cobalt, and chromium.
14. The method of claim 13, wherein the polycrystalline diamond compact is centerless ground to a desired diameter and then surface polished to obtain the diamond compact.
CN202011187945.0A 2020-10-30 2020-10-30 Diamond compact and preparation method thereof Active CN112404435B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011187945.0A CN112404435B (en) 2020-10-30 2020-10-30 Diamond compact and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011187945.0A CN112404435B (en) 2020-10-30 2020-10-30 Diamond compact and preparation method thereof

Publications (2)

Publication Number Publication Date
CN112404435A true CN112404435A (en) 2021-02-26
CN112404435B CN112404435B (en) 2023-07-18

Family

ID=74828247

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011187945.0A Active CN112404435B (en) 2020-10-30 2020-10-30 Diamond compact and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112404435B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7318172B1 (en) * 2022-05-25 2023-08-01 住友電工ハードメタル株式会社 Sintered body and cutting tool

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5030276A (en) * 1986-10-20 1991-07-09 Norton Company Low pressure bonding of PCD bodies and method
US5585175A (en) * 1990-12-21 1996-12-17 Sandvik Ab Diamond-impregnated hard materials
US5833021A (en) * 1996-03-12 1998-11-10 Smith International, Inc. Surface enhanced polycrystalline diamond composite cutters
US20020095875A1 (en) * 2000-12-04 2002-07-25 D'evelyn Mark Philip Abrasive diamond composite and method of making thereof
CN103722174A (en) * 2013-12-30 2014-04-16 中原工学院 Self-sharpening polycrystalline diamond compact and preparation method thereof
CN104131256A (en) * 2014-07-25 2014-11-05 广东工业大学 Multilayer nanometer composite cutting tool coating and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5030276A (en) * 1986-10-20 1991-07-09 Norton Company Low pressure bonding of PCD bodies and method
US5585175A (en) * 1990-12-21 1996-12-17 Sandvik Ab Diamond-impregnated hard materials
US5833021A (en) * 1996-03-12 1998-11-10 Smith International, Inc. Surface enhanced polycrystalline diamond composite cutters
US20020095875A1 (en) * 2000-12-04 2002-07-25 D'evelyn Mark Philip Abrasive diamond composite and method of making thereof
CN103722174A (en) * 2013-12-30 2014-04-16 中原工学院 Self-sharpening polycrystalline diamond compact and preparation method thereof
CN104131256A (en) * 2014-07-25 2014-11-05 广东工业大学 Multilayer nanometer composite cutting tool coating and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7318172B1 (en) * 2022-05-25 2023-08-01 住友電工ハードメタル株式会社 Sintered body and cutting tool
WO2023228324A1 (en) * 2022-05-25 2023-11-30 住友電工ハードメタル株式会社 Sintered body and cutting tool

Also Published As

Publication number Publication date
CN112404435B (en) 2023-07-18

Similar Documents

Publication Publication Date Title
JP5757232B2 (en) Surface coated cutting tool with excellent chipping resistance and wear resistance due to hard coating layer
CN105349965B (en) A kind of composite polycrystal-diamond and preparation method thereof
US5660881A (en) Method of manufacturing CVD diamond coated cutting tools
JPH04232282A (en) Diamond having multilayer coating and its manufacture
JP2012213852A (en) Method of manufacturing coated cutting tool
CN108527182A (en) The method that the diamond abrasive tool of abrasive grain ordered arrangement is prepared using mask plate
CN109913796A (en) TiAlN composite coating on surface of titanium alloy and preparation method thereof
CN113548909B (en) Diamond-metal interface structure, composite material and preparation method
CN109207996A (en) Titanium alloy surface wear-resistant ceramic composite coating and preparation method thereof
CN112404435B (en) Diamond compact and preparation method thereof
CN111041448B (en) Method for preparing diamond coating on surface of cobalt-containing hard alloy and tool and die with diamond coating
JP2001511219A (en) Coating of cemented carbide substrate or carbide-containing cermet substrate with hard material
JP4653922B2 (en) Method of attaching a coating to a substrate composed of diamond or a diamond-containing material
CN111254394B (en) Surface metallization diamond composite particle
CN114774841B (en) Hard alloy surface boronizing treatment method
JP2001293603A (en) Cutting tool coated with vapor phase synthetic diamond
CN115233173A (en) Hard wear-resistant anti-oxidation high-entropy alloy coating and preparation method thereof
CN111705311B (en) Method for plating nickel on surface of diamond micro powder
CN109628884B (en) Surface metallization process of diamond
CN113336576A (en) Preparation method of SiC nanowire toughened HfC-SiC complex phase coating by chemical vapor codeposition
JP2009255234A (en) Surface coated cutting tool
JP2011051890A (en) Adhesive composite coating film for diamond and for diamond-containing material, and method for producing the same
JP2002275571A (en) cBN-BASE SINTERED COMPACT, AND COATED TOOL CONSISTING THEREOF
CN109082640B (en) Nitrogen-doped high-adhesion high-hardness nano-structure W-based coating and preparation method thereof
CN113564551B (en) Multiphase BN-Y/CrAlN composite coating and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant