CN117362047A - Polycrystalline cubic boron nitride composite sheet and preparation method thereof - Google Patents

Polycrystalline cubic boron nitride composite sheet and preparation method thereof Download PDF

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CN117362047A
CN117362047A CN202311157574.5A CN202311157574A CN117362047A CN 117362047 A CN117362047 A CN 117362047A CN 202311157574 A CN202311157574 A CN 202311157574A CN 117362047 A CN117362047 A CN 117362047A
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boron nitride
cubic boron
micro powder
polycrystalline cubic
ceramic binder
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张峰
李云升
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Langfang Supower Diamond Technology Co ltd
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Langfang Supower Diamond Technology Co ltd
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Abstract

The application relates to a polycrystalline cubic boron nitride composite sheet and a preparation method thereof. The polycrystalline cubic boron nitride composite sheet comprises a hard alloy substrate layer and a polycrystalline cubic boron nitride layer overlapped on the hard alloy substrate layer; based on the total weight of the preparation raw materials of the polycrystalline cubic boron nitride layer, the preparation raw materials of the polycrystalline cubic boron nitride layer comprise 55-70wt% of cubic boron nitride micro powder and 30-45wt% of ceramic binder micro powder, and the particle size of the ceramic binder micro powder is 50-180 nm. The ceramic binder in the polycrystalline cubic boron nitride composite sheet is a nano ceramic binder (particle size is 50-180 nm), and the ceramic binder with the size has the characteristics of small size, high activity and the like, so that gaps in the material can be easily filled, the density of the composite material can be remarkably increased, the bridging effect can be reduced or eliminated, the stress distribution in the material is more uniform, the expansion of cracks can be restrained, and the toughness of the PCBN composite sheet is further improved.

Description

Polycrystalline cubic boron nitride composite sheet and preparation method thereof
Technical Field
The application relates to the technical field of composite superhard materials, in particular to a polycrystalline cubic boron nitride composite sheet and a preparation method thereof.
Background
The Polycrystalline Cubic Boron Nitride (PCBN) composite sheet is a composite superhard material synthesized by cubic boron nitride micropowder, a binder and a hard alloy matrix at high temperature and high pressure, has excellent characteristics of high hardness, high wear resistance, high chemical stability and the like, and is mainly applied to processing various hard-cutting materials such as quenched steel, thermal spraying materials, chilled cast iron, cobalt-based and nickel-based materials above HRC35 and the like.
The existing PCBN sintered binders mainly comprise: metals of group IVB, VB, VIB of the periodic table and their nitrides, carbides or carbonitrides; aluminum, cobalt, nickel or alloys thereof. The PCBN compact can be divided from a binder into ceramic binder-like PCBN compact and metal binder-like PCBN compact. In general, the ceramic binder PCBN composite sheet has high heat resistance and is mainly used for cutting high-hardness metals such as quenched steel; the metal binder PCBN composite sheet has good toughness and is mainly used for cutting cast iron metals. From the content of cubic boron nitride micropowder, the PCBN composite sheet can be divided into a high-content PCBN composite sheet and a low-content PCBN composite sheet. Cubic boron nitride micropowder is generally referred to as high-content PCBN compact with a content of more than 80%, and low-content PCBN compact with a content of less than 80%.
For the low-content PCBN composite sheet, although the low-content PCBN composite sheet has high temperature resistance and high hardness and has great advantages in the aspect of processing quenched steel, the low-content PCBN is often synthesized by using a ceramic bond, so that the brittleness is generally high, and the cracking is easy to generate in the process of processing the quenched steel, thereby influencing the service life.
Therefore, the problem of poor toughness of the low-content PCBN composite sheet is urgently needed to be solved, and the cutting life of the PCBN composite sheet is prolonged.
Disclosure of Invention
In order to solve the defects of the prior art, the application provides a polycrystalline cubic boron nitride composite sheet, and the PCBN composite sheet is made of nano ceramic binder, so that the PCBN composite sheet has a more compact and fine microstructure, and further the problem of poor toughness of the low-content PCBN composite sheet can be solved to a certain extent, and the cutting life of the PCBN composite sheet is prolonged.
To this end, a first aspect of the present application provides a polycrystalline cubic boron nitride compact comprising a cemented carbide substrate layer and a polycrystalline cubic boron nitride layer superimposed on the cemented carbide substrate layer; the preparation raw materials of the polycrystalline cubic boron nitride layer comprise 55-70wt% of cubic boron nitride micro powder and 30-45wt% of ceramic binder micro powder, wherein the particle size of the ceramic binder micro powder is 50-180 nm, based on the total weight of the preparation raw materials of the polycrystalline cubic boron nitride layer.
In the prior art, micron-sized ceramic bond is often used as the binder of the low-content PCBN composite sheet, on one hand, the ceramic bond has poor activity, and certainly has poor affinity with cubic boron nitride micro powder, and the ceramic bond and the cubic boron nitride micro powder are basically only mechanically combined together at high temperature and high pressure. In addition, the use of coarse-grained ceramic binders results in a more pronounced "bridging effect" of the synthesized PCBN, which is prone to cracking. The nano ceramic binder with the particle size of 50-180 nm is creatively adopted as the binder in the polycrystalline cubic boron nitride layer in the polycrystalline cubic boron nitride composite sheet, and the ceramic binder with the size has the characteristics of small size, high activity and the like, so that gaps in the material can be easily filled, the density of the composite material can be remarkably increased, the bridging effect is reduced or eliminated, the stress distribution in the material is more uniform, the expansion of cracks can be restrained, and the toughness of the PCBN composite sheet is further improved.
In some embodiments, the particle size of the ceramic binder micropowder may be 50nm, 80nm, 100nm, 120nm, 150nm, 180nm, or the like.
In some preferred embodiments, the particle size of the ceramic binder micropowder is from 80 to 120nm. In some most preferred embodiments, the ceramic binder micropowder has a particle size of 100nm.
According to the method, the grain size of the ceramic binder micro powder is further controlled to be 80-120 nm, particularly 100nm, so that the obtained polycrystalline cubic boron nitride composite sheet has a more compact and fine microstructure, and the toughness of the PCBN composite sheet is further improved.
In some embodiments, the ceramic binder is selected from TiN, tiCN, tiC, al 2 O 3 、TiB 2 AlN and HfB 2 At least one of them.
In some preferred embodiments, the ceramic binder is selected from at least one of TiN, tiCN, and TiC. For example, the ceramic binder may be a mixture of TiN, tiCN, tiC, tiN and TiCN, a mixture of TiCN and TiC, a mixture of TiN and TiC, and a mixture of TiN, tiCN and TiC.
In some further preferred embodiments, the ceramic binder is a mixture of TiN and TiCN, a mixture of TiCN and TiC, a mixture of TiN and TiC, or a mixture of TiN, tiCN and TiC.
The binder plays an important role in the process of synthesizing the polycrystalline cubic boron nitride, and the addition of a proper amount of binder can reduce the sintering temperature and pressure and improve the performance of the prepared polycrystalline cubic boron nitride; and the effect of different binders on PCBN compact performance is also different. The ceramic binder of the type can be selected to enable the PCBN composite sheet to have better performance, and the toughness of the PCBN composite sheet is further improved.
In some embodiments, the cubic boron nitride micropowder includes coarse cubic boron nitride micropowder having a particle size of 2 to 5um and fine cubic boron nitride micropowder having a particle size of 0 to 1 um.
The granularity of the cubic boron nitride micro powder directly determines the density and the organization structure of the PCBN composite sheet. According to the method, the purpose that fine particles fill gaps among coarse particles can be achieved through selecting the cubic boron nitride micro powder with the mixed particle size in the particle size range, and then the density of initial powder can be effectively improved, and finally the density and the uniformity of a tissue structure of the synthesized PCBN composite sheet are improved, so that the PCBN composite sheet with more excellent toughness is obtained.
In some embodiments, the mass ratio of the coarse-particle size cubic boron nitride micropowder to the fine-particle size cubic boron nitride micropowder is (2-3): 1.
In some embodiments, the mass ratio of coarse-particle size cubic boron nitride micropowder to fine-particle size cubic boron nitride micropowder may be, for example, 2:1, 2.5:1, 3:1, or the like.
In some preferred embodiments, the mass ratio of coarse-particle size cubic boron nitride micropowder to fine-particle size cubic boron nitride micropowder is 2.5:1.
According to the method, the mass ratio of coarse-grain cubic boron nitride micro powder to fine-grain cubic boron nitride micro powder is controlled within the range, and especially when the mass ratio of the coarse-grain cubic boron nitride micro powder to the fine-grain cubic boron nitride micro powder is 2.5:1, the density and the uniformity of the tissue structure of the PCBN composite sheet can be further improved, and the toughness of the PCBN composite sheet is better.
In some embodiments, the thickness of the hard alloy matrix layer in the polycrystalline cubic boron nitride composite sheet is 1.0-6.0 mm, and the thickness of the polycrystalline cubic boron nitride layer is 0.5-1.5 mm.
The hard alloy matrix adopted by the application is a cobalt-containing hard alloy, and the content range of cobalt in the hard alloy can be 8-16 wt%. For example, commercially available cemented carbide YG8-YG16 can be used.
A second aspect of the present application provides a method for preparing a polycrystalline cubic boron nitride compact according to the first aspect of the present application, the method comprising the steps of:
s1, drying mixed powder obtained by mixing the polycrystalline cubic boron nitride micro powder and the ceramic binder micro powder, and then placing the dried mixed powder into a vacuum furnace for reduction to obtain reduced powder;
s2, packaging the reduced mixed powder and the hard alloy matrix, and sintering under high-temperature and high-pressure conditions to obtain the polycrystalline cubic boron nitride composite sheet.
The preparation method of the polycrystalline cubic boron nitride composite sheet is simple, the nano ceramic bond is added in the preparation process, so that the prepared PCBN composite sheet has the characteristics of high density, good toughness and strong impact resistance, the crack ratio generated in the laser cutting process can be greatly reduced, the impact resistance can be obviously improved in the cutting process of quenched steel, and the service life is far longer than that of other materials of the same type in the market.
In some embodiments, in step S1, the mixing is performed by a wet mixing method, the dispersing agent used in the wet mixing process is alcohol, and the ratio of the total mass of the cubic boron nitride micro powder and the ceramic binder micro powder to the mass of the dispersing agent is (2-3): 1.
The application adopts the wet mixing method to enable the mixture to be mixed more uniformly, and the dosage of powder (cubic boron nitride micro powder and ceramic binder micro powder) and dispersing agent (alcohol) in the wet mixing process is controlled within the range, so that the uniformity of the mixture is improved.
In some embodiments, the drying is performed in a vacuum oven, the conditions of the drying being: drying at 50-60 deg.c for 1.5-2 hr and then at 130-150 deg.c for 1-2 hr.
In some embodiments, the conditions of the drying are: drying at 50deg.C for 2 hr, and drying at 150deg.C for 1 hr.
The vacuum degree in the vacuum oven can be (1-5) multiplied by 10 -2 Pa, e.g. 3X 10 -2 Pa。
In some embodiments, in step S1, the process of reduction is: in (3-8) x 10 -3 Heating the mixed powder under the vacuum degree of Pa; the heating process comprises the following steps: heating to 550-600 ℃ within 25-30 min, and preserving heat for 120-150 min.
In some embodiments, the process of reduction is: at 5X 10 -3 Heating the mixed powder under the vacuum degree of Pa; the heating process comprises the following steps: heating to 600 ℃ for 30min, and preserving heat for 120min.
In some embodiments, in step S2, the sintering is performed at a pressure of 4.0 to 5.5Gpa, a temperature of 1300 to 1600 ℃, and a time of 5 to 20 minutes.
Under the sintering condition, the packaged green body can be effectively compounded to prepare the PCBN composite sheet with better comprehensive performance.
The beneficial technical effects of this application are: the ceramic binder in the polycrystalline cubic boron nitride layer in the polycrystalline cubic boron nitride composite sheet is a nano ceramic binder (particle size is 50-180 nm), and the ceramic binder with the size has the characteristics of small size, high activity and the like, so that gaps in the material can be easily filled, the density of the composite material can be remarkably increased, the bridging effect is reduced or eliminated, the stress distribution in the material is more uniform, crack expansion can be restrained, and the toughness of the PCBN composite sheet is further improved. Meanwhile, the preparation method of the polycrystalline cubic boron nitride composite sheet is simple, and the obtained PCBN composite sheet has the characteristics of high density, good toughness and strong impact resistance, the crack ratio generated in the laser cutting processing process can be greatly reduced, the impact resistance can be obviously improved in the cutting processing of quenched steel, and the service life is far longer than that of other materials of the same type on the market.
Detailed Description
In order that the present application may be more readily understood, the following examples are presented in conjunction with the following detailed description, which are intended to be illustrative only and are not intended to limit the scope of application of the present application. The starting materials or components used in the present application may be prepared by commercial or conventional methods unless specifically indicated.
Example 1: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 30wt% of 100nm TiN ceramic binder micro powder; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1.
The cemented carbide substrate in the cemented carbide substrate layer was cemented carbide YG12 having a cobalt content of 12 wt%.
The preparation process comprises the following steps: mixing the polycrystalline cubic boron nitride micro powder and the ceramic binder micro powder by adopting a wet mixing method, wherein a dispersing agent adopted in the wet mixing process is alcohol, and the mass ratio of the powder (the polycrystalline cubic boron nitride micro powder and the ceramic binder micro powder) to the dispersing agent is 2:1. Placing the wet mixed powder in a vacuum oven for drying, wherein the drying process is as follows: drying at 50deg.C for 2 hr, heating to 150deg.C, and drying for 1 hr under vacuum degree of 3×10 -2 Pa. Placing the dried mixed powder in a vacuum furnace for vacuum reduction to remove oxygen and water in the mixed powder, wherein the concrete process comprises the following steps: sequentially starting vacuum pumps of each stage of the vacuum furnace to perform vacuumizing treatment until reaching 5×10 -3 High vacuum degree of Pa; heating under the vacuum degree, wherein the heating process comprises the following steps: heating to 600 ℃ for 30min, and preserving heat for 120min. The reduced mixed powder and the hard powder are mixedAnd (3) packaging a matrix of the mass alloy, and roasting the packaged blank for 20 minutes under the conditions of the pressure of 5.0Gpa and the temperature of 1500 ℃ for compounding to prepare the polycrystalline cubic boron nitride composite sheet. The thickness of the polycrystalline cubic boron nitride layer in the polycrystalline cubic boron nitride composite sheet is 1.0mm, and the thickness of the hard alloy substrate layer is 3.0mm.
Example 2: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 30wt% of TiC ceramic binder micro powder with the wavelength of 100 nm; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1.
The procedure is as in example 1.
Example 3: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 30wt% of TiNC ceramic binder micropowder with the wavelength of 100 nm; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1.
The procedure is as in example 1.
Example 4: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; tiB of 100nm 2 30wt% of ceramic binder micropowder; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1.
The procedure is as in example 1.
Example 5: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 15wt% of 100nm TiN ceramic binder micro powder; 15wt% of TiC ceramic binder micro powder with the wavelength of 100 nm; the content of the cubic boron nitride micro powder in the raw materials is 70wt%, the content of the ceramic binder micro powder is 30wt%, the mass ratio of coarse-granularity cubic boron nitride micro powder to fine-granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1, and the mass ratio of the TiN ceramic binder micro powder to the TiC ceramic binder micro powder is 1:1.
The procedure is as in example 1.
Example 6: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 10wt% of 100nm TiN ceramic binder micropowder; 10wt% of TiC ceramic binder micropowder with the wavelength of 100 nm; 10wt% of TiNC ceramic binder micropowder with the wavelength of 100 nm; the content of the cubic boron nitride micro powder in the raw materials is 70wt%, the content of the ceramic binder micro powder is 30wt%, the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1, and the mass ratio of the TiN ceramic binder micro powder to the TiC ceramic binder micro powder to the TiNC ceramic binder micro powder is 1:1:1.
The procedure is as in example 1.
Example 7: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 30wt% of 50nm TiC ceramic binder micro powder; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1.
The procedure is as in example 1.
Example 8: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 30wt% of TiC ceramic binder micro powder with the particle size of 180 nm; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1.
The procedure is as in example 1.
Example 9: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 30wt% of TiC ceramic binder micro powder with the wavelength of 250 nm; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1.
The procedure is as in example 1.
Example 10: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 50wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 20wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 30wt% of TiC ceramic binder micro powder with the wavelength of 20 nm; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 2.5:1.
The procedure is as in example 1.
Example 11: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 52.5wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 17.5wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 30wt% of TiC ceramic binder micro powder with the wavelength of 100 nm; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 3:1.
The procedure is as in example 1.
Example 12: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 35wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 35wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 30wt% of TiC ceramic binder micro powder with the wavelength of 100 nm; the content of the cubic boron nitride micro powder in the raw material is 70wt%, the content of the ceramic binder micro powder is 30wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 1:1.
The procedure is as in example 1.
Example 13: preparation of polycrystalline cubic boron nitride composite sheet
The polycrystalline cubic boron nitride layer comprises the following raw materials: 45wt% of coarse-grained cubic boron nitride micro powder with the granularity of 2-5 um; 15wt% of fine granularity cubic boron nitride micro powder of 0-1 um; 40wt% of TiC ceramic binder micro powder with the wavelength of 100 nm; the content of the cubic boron nitride micro powder in the raw material is 60wt%, the content of the ceramic binder micro powder is 40wt%, and the mass ratio of the coarse granularity cubic boron nitride micro powder to the fine granularity cubic boron nitride micro powder in the cubic boron nitride micro powder is 3:1.
The procedure is as in example 11.
Example 14: preparation of polycrystalline cubic boron nitride composite sheet
The materials of the polycrystalline cubic boron nitride layer and the cemented carbide base layer were the same as in example 1.
The preparation process comprises the following steps: mixing the polycrystalline cubic boron nitride micro powder and the ceramic binder micro powder by adopting a wet mixing method, wherein a dispersing agent adopted in the wet mixing process is alcohol, and the mass ratio of the powder (the polycrystalline cubic boron nitride micro powder and the ceramic binder micro powder) to the dispersing agent is 2:1. Placing the wet mixed powder in a vacuum oven for drying, wherein the drying process is as follows: drying at 150deg.C for 2 hr, and vacuum degree of oven is 3×10 -2 Pa. Placing the dried mixed powder in a vacuum furnace for vacuum reduction to remove oxygen and water in the mixed powder, and specifically performing the processThe method comprises the following steps: sequentially starting vacuum pumps of each stage of the vacuum furnace to perform vacuumizing treatment until reaching 2×10 -3 High vacuum degree of Pa; heating under the vacuum degree, wherein the heating process comprises the following steps: heating to 400 ℃ for 20min, preserving heat for 30min, heating to 800 ℃ for 30min, and preserving heat for 120min. Packaging the reduced mixed powder and a hard alloy matrix, and roasting the packaged green body for 20min under the conditions of 5.0Gpa of pressure and 1500 ℃ for compounding to prepare the polycrystalline cubic boron nitride composite sheet. The thickness of the polycrystalline cubic boron nitride layer in the polycrystalline cubic boron nitride composite sheet is 1.0mm, and the thickness of the hard alloy substrate layer is 3.0mm.
Example 15: preparation of polycrystalline cubic boron nitride composite sheet
The materials of the polycrystalline cubic boron nitride layer and the cemented carbide base layer were the same as in example 1.
The preparation process comprises the following steps: mixing the polycrystalline cubic boron nitride micro powder and the ceramic binder micro powder by adopting a wet mixing method, wherein a dispersing agent adopted in the wet mixing process is alcohol, and the mass ratio of the powder (the polycrystalline cubic boron nitride micro powder and the ceramic binder micro powder) to the dispersing agent is 2:1. Placing the wet mixed powder in a vacuum oven for drying, wherein the drying process is as follows: drying at 50deg.C for 2 hr, heating to 150deg.C, and drying for 1 hr under vacuum degree of 3×10 -2 Pa. Placing the dried mixed powder in a vacuum furnace for vacuum reduction to remove oxygen and water in the mixed powder, wherein the concrete process comprises the following steps: sequentially starting vacuum pumps of each stage of the vacuum furnace to perform vacuumizing treatment until reaching 2×10 -3 High vacuum degree of Pa; heating under the vacuum degree, wherein the heating process comprises the following steps: heating to 500 ℃ for 30min, and preserving heat for 140min. Packaging the reduced mixed powder and a hard alloy matrix, and roasting the packaged green body for 20min under the conditions of 5.0Gpa of pressure and 1500 ℃ for compounding to prepare the polycrystalline cubic boron nitride composite sheet. The thickness of the polycrystalline cubic boron nitride layer in the polycrystalline cubic boron nitride composite sheet is 1.0mm, and the thickness of the hard alloy substrate layer is 3.0mm.
Test case
The polycrystalline cubic boron nitride compacts prepared in examples 1 to 15 were tested for density, fracture toughness, and impact toughness using a drainage method, fracture toughness was calculated from the length of extended cracks at four corners of a pit pressed by a vickers indenter, and impact toughness was tested for flexural strength by a three-point bending method. The specific detection results are shown in Table 1.
Table 1: polycrystalline cubic boron nitride composite sheet performance detection result
As can be seen from the test results in Table 1, the density of the polycrystalline cubic boron nitride composite sheet synthesized in examples 1 to 15 of the present application is 3.78 to 4.12g/m 3 Fracture toughness of 5.3-6.7 MPa/m 2 Impact toughness of 36-50 KJ/m 2 The polycrystalline cubic boron nitride composite sheet provided by the application has higher density and excellent fracture toughness and impact toughness.
From the test results of examples 1 to 6, it is understood that the density and toughness of the finally produced polycrystalline cubic boron nitride composite sheet can be improved when the ceramic binder used is at least one selected from TiN, tiCN and TiC, particularly at least two selected from TiN, tiCN and TiC.
From the detection results of examples 1 and 7-10, it is known that when the particle size of the ceramic binder micro powder is 50-180 nm, especially 100nm, the density and toughness of the polycrystalline cubic boron nitride composite sheet can be further improved, and the service performance of the polycrystalline cubic boron nitride composite sheet can be further improved.
From the detection results of examples 1 and 11-12, it is found that the mass ratio of coarse-grain cubic boron nitride micro powder to fine-grain cubic boron nitride micro powder in the adopted cubic boron nitride micro powder is (2-3): 1, especially 2.5, is more favorable for improving the density and toughness of the polycrystalline cubic boron nitride composite sheet.
It should be noted that the above-described embodiments are only for explaining the present application, and do not constitute any limitation to the present application. The present application has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the present application as defined within the scope of the claims of the present application, and the invention may be modified without departing from the scope and spirit of the present application. Although the present application is described herein with reference to particular methods, materials and embodiments, the present application is not intended to be limited to the particular examples disclosed herein, but rather, the present application is intended to extend to all other methods and applications having the same functionality.

Claims (10)

1. The polycrystalline cubic boron nitride composite sheet is characterized by comprising a hard alloy substrate layer and a polycrystalline cubic boron nitride layer superposed on the hard alloy substrate layer; based on the total weight of the preparation raw materials of the polycrystalline cubic boron nitride layer, the preparation raw materials of the polycrystalline cubic boron nitride layer comprise 55-70wt% of cubic boron nitride micro powder and 30-45wt% of ceramic binder micro powder, and the particle size of the ceramic binder micro powder is 50-180 nm.
2. The polycrystalline cubic boron nitride compact according to claim 1, wherein the particle size of the ceramic binder micro powder is 80-120 nm.
3. The polycrystalline cubic boron nitride compact according to claim 1 or 2, wherein the ceramic binder is selected from TiN, tiCN, tiC, al 2 O 3 、TiB 2 AlN and HfB 2 At least one of them.
4. The polycrystalline cubic boron nitride compact according to claim 1 or 2, wherein the cubic boron nitride micro powder comprises coarse cubic boron nitride micro powder with a granularity of 2-5 um and fine cubic boron nitride micro powder with a granularity of 0-1 um.
5. The polycrystalline cubic boron nitride compact according to claim 4, wherein the mass ratio of the coarse-grain cubic boron nitride fine powder to the fine-grain cubic boron nitride fine powder is (2-3): 1.
6. The polycrystalline cubic boron nitride compact according to claim 1 or 2, wherein the thickness of the cemented carbide matrix layer in the polycrystalline cubic boron nitride compact is 1.0-6.0 mm, and the thickness of the polycrystalline cubic boron nitride layer is 0.5-1.5 mm.
7. A method of preparing a polycrystalline cubic boron nitride compact according to any one of claims 1 to 6, the method comprising the steps of:
s1, drying mixed powder obtained by mixing the polycrystalline cubic boron nitride micro powder and the ceramic binder micro powder, and then placing the dried mixed powder into a vacuum furnace for reduction to obtain reduced powder;
s2, packaging the reduced mixed powder and the hard alloy matrix, and sintering under high-temperature and high-pressure conditions to obtain the polycrystalline cubic boron nitride composite sheet.
8. The method according to claim 7, wherein in the step S1, the mixing method is a wet mixing method, the dispersant used in the wet mixing process is alcohol, and the ratio of the total mass of the cubic boron nitride micro powder and the ceramic binder micro powder to the mass of the dispersant is (2-3): 1;
the drying is carried out in a vacuum oven, and the conditions of the drying are as follows: drying at 50-60 ℃ for 1.5-2 hours, and then drying at 130-150 ℃ for 1-2 hours.
9. The method according to claim 7 or 8, wherein in step S1, the process of reduction is: in (3-8) x 10 -3 Heating the mixed powder under the vacuum degree of Pa; the heating process comprises the following steps: heating to 550-600 ℃ within 25-30 min, and preserving heat for 120-150 min.
10. The method according to claim 7 or 8, wherein in step S2, the sintering is performed at a pressure of 4.0 to 5.5Gpa, a temperature of 1300 to 1600 ℃ and a time of 5 to 20min.
CN202311157574.5A 2023-09-08 2023-09-08 Polycrystalline cubic boron nitride composite sheet and preparation method thereof Pending CN117362047A (en)

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