CN107598174B - Integral sintered polycrystalline diamond ball tooth and preparation method thereof - Google Patents

Integral sintered polycrystalline diamond ball tooth and preparation method thereof Download PDF

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CN107598174B
CN107598174B CN201710949266.4A CN201710949266A CN107598174B CN 107598174 B CN107598174 B CN 107598174B CN 201710949266 A CN201710949266 A CN 201710949266A CN 107598174 B CN107598174 B CN 107598174B
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resistant layer
powder
outer wear
inner impact
diamond
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CN107598174A (en
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刘书锋
崔卫民
李启泉
张旺玺
张素梅
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Zhengzhou Berlt Hard Materials Co ltd
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Abstract

The invention discloses an integrally sintered polycrystalline diamond ball tooth, which consists of an outer wear-resistant layer and an inner impact-resistant layer, wherein the outer wear-resistant layer is positioned on the outer layer of the inner impact-resistant layer, and the outer wear-resistant layer is prepared from the following raw materials in percentage by mass: 70-95% of diamond micro powder, 1-5% of nickel powder, 1-15% of silicon powder and 3-20% of cobalt powder; the inner impact-resistant layer is prepared from the following raw materials in percentage by mass: 40-70% of diamond micro powder, 1-10% of nickel powder, 5-15% of silicon powder and 10-40% of cobalt powder. The invention aims at the future development demand, and provides the integral sintered polycrystalline diamond ball tooth, the raw material of the material is artificially synthesized, and the price of the material is continuously reduced along with the progress of the technology, so that the material has great prospect in the future.

Description

Integral sintered polycrystalline diamond ball tooth and preparation method thereof
Technical Field
The invention belongs to the technical field of buttons, and particularly relates to an integrally sintered polycrystalline diamond button and a preparation method thereof.
Background
At present, a large amount of buttons are used for geological exploration, coal exploitation, petroleum exploitation and the like, so that the working efficiency is improved. The ball tooth material is various, and high-speed steel is used in the past, and most of hard alloy is used at present, and diamond composite ball teeth are adopted as parts. The high-speed steel has the advantages that the wear resistance is insufficient, the service life is short, the stage is exited, the hard alloy buttons are replaced, the processing of raw materials of hard alloy is always increased in recent years, the stock of the hard alloy is limited and is not renewable, so that the price of the hard alloy can be continuously increased in the future, and the cost is greatly increased. The appearance of the diamond composite buttons is to cope with the exploration of harder rock stratum, so that the service life and the working efficiency of a drill bit can be improved, but the diamond composite buttons take hard alloy as a matrix, a polycrystalline diamond composite layer is compounded on the hard alloy, most of the polycrystalline diamond composite layer is hard alloy, and the problem of scarcity of hard alloy raw materials is faced in the future.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art and provides an integrally sintered polycrystalline diamond button and a preparation method thereof.
The object of the invention is achieved in the following way:
an integrally sintered polycrystalline diamond ball tooth, wherein the ball tooth consists of an external wear-resistant layer and an internal impact-resistant layer, the external wear-resistant layer is positioned on the outer layer of the internal impact-resistant layer, and the external wear-resistant layer is prepared from the following raw materials in percentage by mass: 70-95% of diamond micro powder, 1-5% of nickel powder, 1-15% of silicon powder and 3-20% of cobalt powder; the inner impact-resistant layer is prepared from the following raw materials in percentage by mass: 40-70% of diamond micro powder, 1-10% of nickel powder, 5-15% of silicon powder and 10-40% of cobalt powder.
The granularity of the diamond micro powder of the outer wear-resistant layer and the diamond micro powder of the inner impact-resistant layer are W40-W10.
The particle sizes of the nickel powder of the external wear-resistant layer and the nickel powder of the internal impact-resistant layer are less than or equal to 300 meshes.
The grain diameters of the silica powder of the outer wear-resistant layer and the inner impact-resistant layer are all smaller than or equal to 400 meshes.
The particle sizes of cobalt powder of the outer wear-resistant layer and the inner impact-resistant layer are all smaller than or equal to 400 meshes.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at a temperature of 650-750 ℃;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral top press, sintering for 3-6min at the pressure of 5-8GPa and the temperature of 1100-1500 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
And (3) in the step (5), the volume ratio of the hydrogen to the argon is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles is 0.5-2.0mm.
The novel diamond button provided by the invention has the advantages that the hardness is far higher than that of a hard alloy button, the impact toughness is better than that of the hard alloy button, the service life is tens times longer than that of the hard alloy button, the time for replacing a large number of buttons is reduced, the drilling speed is higher, and therefore, the production efficiency can be greatly improved. Meanwhile, the invention avoids the problems of layering and breakage of the diamond composite buttons in the use process. The preparation process adopts compression molding to improve the initial density of the blank, so that the polycrystalline diamond sintered body with higher density can be obtained, and the material performance is greatly improved.
Compared with the prior art, the invention provides the integral sintered polycrystalline diamond ball tooth aiming at the future development demand, the raw material of the material is artificially synthesized, and the price of the material is continuously reduced along with the progress of the technology, so that the material has great prospect in the future.
Drawings
Fig. 1 is a schematic longitudinal cross-sectional view of one of the integrally sintered polycrystalline diamond buttons produced in accordance with the present invention.
Fig. 2 is a schematic cross-sectional view of one of the integrally sintered polycrystalline diamond buttons produced in accordance with the present invention.
Fig. 3 is a schematic longitudinal cross-sectional view of a second integrally sintered polycrystalline diamond button made in accordance with the present invention.
Fig. 4 is a schematic cross-sectional view of a second integrally sintered polycrystalline diamond button made in accordance with the present invention.
Fig. 5 is a schematic longitudinal cross-sectional view of a third one of the integrally sintered polycrystalline diamond buttons produced in accordance with the present disclosure.
Fig. 6 is a schematic cross-sectional view of a third one of the integrally sintered polycrystalline diamond buttons made in accordance with the present disclosure.
Fig. 7 is a schematic longitudinal cross-sectional view of a fourth integrally sintered polycrystalline diamond button made in accordance with the present disclosure.
Fig. 8 is a schematic cross-sectional view of a fourth integrally sintered polycrystalline diamond button made in accordance with the present disclosure.
Wherein 1 is an outer wear layer; 2 is an inner impact resistant layer.
Detailed Description
The process of electroplating nickel powder on the surface of the diamond micro powder can require that a diamond micro powder manufacturer directly electroplate a layer of nickel powder after preparing the diamond micro powder, namely the diamond micro powder with electroplated nickel powder on the market.
As shown in fig. 1-8, the different molds produced the different configurations of buttons.
The buttons are cylindrical as shown in fig. 1.
The lower part of the spherical tooth is a cylinder, the upper part of the spherical tooth is a hemisphere, the diameter of the hemisphere is equal to that of the upper surface of the cylinder, and the center of the sphere of the hemisphere is the same as the center of the circle of the upper surface of the cylinder, as shown in fig. 3.
The buttons are bullet-shaped as shown in fig. 7.
The lower part of the spherical tooth is a cylinder, the upper part of the spherical tooth is a cone, the diameter of the bottom surface circle of the cone is equal to that of the upper surface circle of the cylinder, and the center of the bottom surface circle of the cone is the same as that of the upper surface circle of the cylinder, as shown in figure 5.
The cross section of the interface of the outer wear layer 1 and the inner impact layer 2 is circular or circular with wavy teeth, as shown in fig. 2, 4, 6, 8.
The wave teeth are rectangular, triangular or semicircular.
Example 1:
an integrally sintered polycrystalline diamond ball tooth, wherein the ball tooth consists of an outer wear-resistant layer 1 and an inner impact-resistant layer 2, the outer wear-resistant layer 1 is positioned on the outer layer of the inner impact-resistant layer 2, and the outer wear-resistant layer 1 is prepared from the following raw materials in percentage by mass: 70-95% of diamond micro powder, 1-5% of nickel powder, 1-15% of silicon powder and 3-20% of cobalt powder; the inner impact-resistant layer 2 is made of the following raw materials in mass fraction: 40-70% of diamond micro powder, 1-10% of nickel powder, 5-15% of silicon powder and 10-40% of cobalt powder.
The granularity of the diamond micro powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is W40-W10.
The particle size of the nickel powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is less than or equal to 300 meshes.
The grain diameters of the silica powder of the outer wear-resistant layer 1 and the silica powder of the inner impact-resistant layer 2 are all smaller than or equal to 400 meshes.
The particle size of cobalt powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is less than or equal to 400 meshes.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at a temperature of 650-750 ℃; removing impurities, oxygen and the like in the button entity;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral top press, sintering for 3-6min at the pressure of 5-8GPa and the temperature of 1100-1500 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
The volume ratio of hydrogen to argon in the step (5) is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles are 0.5-2.0mm.
Example 2:
an integrally sintered polycrystalline diamond button, wherein the button consists of an outer wear-resistant layer 1 and an inner impact-resistant layer 2, and the outer wear-resistant layer 1 is prepared from the following raw materials in percentage by mass: 90% of diamond micro powder, 1% of nickel powder, 2% of silicon powder and 7% of cobalt powder; the inner impact-resistant layer 2 is made of the following raw materials in mass fraction: 70% of diamond micro powder, 2% of nickel powder, 7% of silicon powder and 21% of cobalt powder.
The granularity of the diamond micro powder of the outer wear-resistant layer 1 is W40, and the granularity of the diamond micro powder of the inner impact-resistant layer 2 is W40.
The particle size of the nickel powder of the outer wear layer 1 and the inner impact layer 2 was 300 mesh.
The grain sizes of the silica powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 are 400 meshes.
The particle size of the cobalt powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 400 mesh.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at the temperature of 650 ℃; removing impurities, oxygen and the like in the button entity;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral press, sintering for 5min at the pressure of 7GPa and the temperature of 1300 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
The volume ratio of hydrogen to argon in the step (5) is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles are 0.5-2.0mm.
Example 3:
an integrally sintered polycrystalline diamond button, wherein the button consists of an outer wear-resistant layer 1 and an inner impact-resistant layer 2, and the outer wear-resistant layer 1 is prepared from the following raw materials in percentage by mass: 84% of diamond micro powder, 2% of nickel powder, 11% of silicon powder and 3% of cobalt powder; the inner impact-resistant layer 2 is made of the following raw materials in mass fraction: 65% of diamond micro powder, 9% of nickel powder, 10% of silicon powder and 16% of cobalt powder.
The granularity of the diamond micro powder of the outer wear-resistant layer 1 is W40, and the granularity of the diamond micro powder of the inner impact-resistant layer 2 is W40.
The particle size of the nickel powder of the outer wear layer 1 and the inner impact layer 2 was 325 mesh.
The grain sizes of the silica powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 are 460 meshes.
The particle size of the cobalt powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 460 mesh.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at a temperature of 670 ℃; removing impurities, oxygen and the like in the button entity;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral press, sintering for 4min at the pressure of 6GPa and the temperature of 1200 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
The volume ratio of hydrogen to argon in the step (5) is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles are 0.5-2.0mm.
Example 4:
an integrally sintered polycrystalline diamond button, wherein the button consists of an outer wear-resistant layer 1 and an inner impact-resistant layer 2, and the outer wear-resistant layer 1 is prepared from the following raw materials in percentage by mass: 70% of diamond micro powder, 5% of nickel powder, 10% of silicon powder and 15% of cobalt powder; the inner impact-resistant layer 2 is made of the following raw materials in mass fraction: 56% of diamond micro powder, 10% of nickel powder, 13% of silicon powder and 21% of cobalt powder.
The diamond micropowder of the outer wear-resistant layer 1 has a particle size W28 and the diamond micropowder of the inner impact-resistant layer 2 has a particle size W20.
The particle size of the nickel powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 was 400 mesh.
The grain sizes of the silica powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 are 540 meshes.
The particle size of the cobalt powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 540 meshes.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at 690 ℃; removing impurities, oxygen and the like in the button entity;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral press, sintering for 6min at the pressure of 7GPa and the temperature of 1200 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
The volume ratio of hydrogen to argon in the step (5) is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles are 0.5-2.0mm.
Example 5:
an integrally sintered polycrystalline diamond button, wherein the button consists of an outer wear-resistant layer 1 and an inner impact-resistant layer 2, and the outer wear-resistant layer 1 is prepared from the following raw materials in percentage by mass: 75% of diamond micro powder, 3% of nickel powder, 6% of silicon powder and 16% of cobalt powder; the inner impact-resistant layer 2 is made of the following raw materials in mass fraction: 49% of diamond micro powder, 6% of nickel powder, 15% of silicon powder and 30% of cobalt powder.
The diamond micropowder of the outer wear-resistant layer 1 has a particle size W20 and the diamond micropowder of the inner impact-resistant layer 2 has a particle size W10.
The particle size of the nickel powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 460 mesh.
The grain sizes of the silica powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 are 650 meshes.
The particle size of the cobalt powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 650 meshes.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at 710 ℃; removing impurities, oxygen and the like in the button entity;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral press, sintering for 3min at the pressure of 8GPa and the temperature of 1400 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
The volume ratio of hydrogen to argon in the step (5) is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles are 0.5-2.0mm.
Example 6:
an integrally sintered polycrystalline diamond button, wherein the button consists of an outer wear-resistant layer 1 and an inner impact-resistant layer 2, and the outer wear-resistant layer 1 is prepared from the following raw materials in percentage by mass: 80% of diamond micro powder, 1% of nickel powder, 15% of silicon powder and 4% of cobalt powder; the inner impact-resistant layer 2 is made of the following raw materials in mass fraction: 40% of diamond micro powder, 10% of nickel powder, 10% of silicon powder and 40% of cobalt powder.
The diamond micropowder of the outer wear-resistant layer 1 has a particle size of W14, and the diamond micropowder of the inner impact-resistant layer 2 has a particle size of W14.
The particle size of the nickel powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 540 mesh.
The grain sizes of the silica powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 are 800 meshes.
The particle size of the cobalt powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 800 meshes.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at the temperature of 730 ℃; removing impurities, oxygen and the like in the button entity;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral top press, sintering for 5min at the pressure of 5GPa and the temperature of 1300 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
The volume ratio of hydrogen to argon in the step (5) is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles are 0.5-2.0mm.
Example 7:
an integrally sintered polycrystalline diamond button, wherein the button consists of an outer wear-resistant layer 1 and an inner impact-resistant layer 2, and the outer wear-resistant layer 1 is prepared from the following raw materials in percentage by mass: 86% of diamond micro powder, 2% of nickel powder, 4% of silicon powder and 8% of cobalt powder; the inner impact-resistant layer 2 is made of the following raw materials in mass fraction: 60% of diamond micro powder, 4% of nickel powder, 5% of silicon powder and 31% of cobalt powder.
The diamond micropowder of the outer wear-resistant layer 1 has a particle size W20 and the diamond micropowder of the inner impact-resistant layer 2 has a particle size W10.
The particle size of the nickel powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 650 meshes.
The grain sizes of the silica powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 are 900 meshes.
The particle size of the cobalt powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 900 meshes.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at 750 ℃; removing impurities, oxygen and the like in the button entity;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral press, sintering for 4min at the pressure of 8GPa and the temperature of 1500 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
The volume ratio of hydrogen to argon in the step (5) is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles are 0.5-2.0mm.
Example 8:
an integrally sintered polycrystalline diamond button, wherein the button consists of an outer wear-resistant layer 1 and an inner impact-resistant layer 2, and the outer wear-resistant layer 1 is prepared from the following raw materials in percentage by mass: 95% of diamond micro powder, 1% of nickel powder, 1% of silicon powder and 3% of cobalt powder; the inner impact-resistant layer 2 is made of the following raw materials in mass fraction: 68% of diamond micro powder, 1% of nickel powder, 0% of silicon powder and 21% of cobalt powder.
The diamond micropowder of the outer wear-resistant layer 1 has a particle size W10 and the diamond micropowder of the inner impact-resistant layer 2 has a particle size W20.
The particle size of the nickel powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 was 400 mesh.
The grain sizes of the silica powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 are 540 meshes.
The particle size of the cobalt powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 540 meshes.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at 690 ℃; removing impurities, oxygen and the like in the button entity;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral press, sintering for 5min at the pressure of 6GPa and the temperature of 1100 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
The volume ratio of hydrogen to argon in the step (5) is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles are 0.5-2.0mm.
Example 9:
an integrally sintered polycrystalline diamond button, wherein the button consists of an outer wear-resistant layer 1 and an inner impact-resistant layer 2, and the outer wear-resistant layer 1 is prepared from the following raw materials in percentage by mass: 70% of diamond micro powder, 5% of nickel powder, 5% of silicon powder and 20% of cobalt powder; the inner impact-resistant layer 2 is made of the following raw materials in mass fraction: 65% of diamond micro powder, 10% of nickel powder, 15% of silicon powder and 10% of cobalt powder.
The diamond micropowder of the outer wear-resistant layer 1 has a particle size of W10, and the diamond micropowder of the inner impact-resistant layer 2 has a particle size of W10.
The particle size of the nickel powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 was 400 mesh.
The grain sizes of the silica powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 are 540 meshes.
The particle size of the cobalt powder of the outer wear-resistant layer 1 and the inner impact-resistant layer 2 is 540 meshes.
The preparation method of the integral sintered polycrystalline diamond button comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at 690 ℃; removing impurities, oxygen and the like in the button entity;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral press, sintering for 6min at the temperature of 1400 ℃ under the pressure of 7GPa, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
The volume ratio of hydrogen to argon in the step (5) is 3:7.
The particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles are 0.5-2.0mm.
Comparative example 1 is a conventional commercially available cemented carbide button, and comparative example 2 is a conventional commercially available cemented carbide, polycrystalline diamond compact button.
The results of the impact times for examples 2-9 and comparative examples 1-2 are shown in Table 1.
Figure 301083DEST_PATH_IMAGE002
The method for measuring the impact resistance times comprises the following steps: the weight is 30kg, the height is 1.5 meters, the ball teeth are placed on the bottom base plate, the round head or the conical head faces upwards, the weight is put down at the height of 1.5 meters, the weight falls freely until the ball teeth are hit, the operation is repeated, the number of times of the ball teeth can be tested, and the number of times of the hit is recorded.
As can be seen from Table 1, the impact toughness of the polycrystalline diamond ball tooth is higher than that of the existing hard alloy ball tooth and diamond composite ball tooth, so that the polycrystalline diamond ball tooth can adapt to the situation of worse geological conditions and has longer service life.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that it will be apparent to those skilled in the art that several changes and modifications can be made without departing from the general inventive concept, and these should also be regarded as the scope of the invention.

Claims (8)

1. An integrally sintered polycrystalline diamond button, characterized in that: the ball tooth consists of an outer wear-resistant layer (1) and an inner impact-resistant layer (2), wherein the outer wear-resistant layer (1) is positioned on the outer layer of the inner impact-resistant layer (2), and the outer wear-resistant layer (1) is prepared from the following raw materials in percentage by mass: 70-95% of diamond micro powder, 1-5% of nickel powder, 1-15% of silicon powder and 3-20% of cobalt powder; the inner impact-resistant layer (2) is prepared from the following raw materials in percentage by mass: 40-70% of diamond micro powder, 1-10% of nickel powder, 5-15% of silicon powder and 10-40% of cobalt powder.
2. The integrally sintered polycrystalline diamond button of claim 1, wherein: the granularity of the diamond micro powder of the outer wear-resistant layer (1) and the inner impact-resistant layer (2) is W40-W10.
3. The integrally sintered polycrystalline diamond button of claim 1, wherein: the particle sizes of nickel powder of the outer wear-resistant layer (1) and the inner impact-resistant layer (2) are less than or equal to 300 meshes.
4. The integrally sintered polycrystalline diamond button of claim 1, wherein: the grain diameters of the silica powder of the outer wear-resistant layer (1) and the silica powder of the inner impact-resistant layer (2) are smaller than or equal to 400 meshes.
5. The integrally sintered polycrystalline diamond button of claim 1, wherein: the particle sizes of cobalt powder of the outer wear-resistant layer (1) and the inner impact-resistant layer (2) are all smaller than or equal to 400 meshes.
6. A method of preparing an integrally sintered polycrystalline diamond button as claimed in any one of claims 1 to 5, wherein: the method comprises the following specific steps:
(1) Outer wear layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1%, wetting, and granulating to obtain external wear-resistant layer particles;
(2) Inner impact resistant layer particles: firstly electroplating nickel powder on the surface of diamond micro powder, uniformly mixing nickel-plated diamond micro powder, silicon powder and cobalt powder, adding PVA aqueous solution with the mass fraction of 1% for wetting, and granulating to obtain internal impact-resistant layer particles;
(3) Filling the external wear-resistant layer particles into a mould, and compacting by using a pressure head;
(4) Filling the internal impact-resistant layer particles into a mould, compacting by using a pressure head, and removing the mould to obtain a spherical tooth entity;
(5) Placing the spherical tooth entity into a vacuum furnace, and preserving heat for 1h in a mixed gas environment of hydrogen and argon at a temperature of 650-750 ℃;
(6) And (3) assembling the spherical tooth entity, the pyrophyllite and the steel ring which are taken out of the vacuum furnace, putting the assembled spherical tooth entity, the pyrophyllite and the steel ring into a hexahedral top press, sintering for 3-6min at the pressure of 5-8GPa and the temperature of 1100-1500 ℃, taking out, and performing sand blasting and excircle processing to form the integrally sintered polycrystalline diamond spherical tooth.
7. The method of preparing integrally sintered polycrystalline diamond buttons according to claim 6, wherein: and (3) in the step (5), the volume ratio of the hydrogen to the argon is 3:7.
8. The method of preparing integrally sintered polycrystalline diamond buttons according to claim 6, wherein: the particle size of the outer wear-resistant layer particles and the inner impact-resistant layer particles is 0.5-2.0mm.
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