CN109748276B - Diamond core nano polycrystalline material, preparation method thereof and superhard cutter - Google Patents
Diamond core nano polycrystalline material, preparation method thereof and superhard cutter Download PDFInfo
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Abstract
The invention provides a diamond core nano polycrystalline material, a preparation method thereof and a superhard cutter, and belongs to the technical field of superhard materials. The diamond core nano polycrystalline material comprises an inner core and an outer shell, wherein the inner core comprises nano diamond, and the outer shell comprises B-C-N solid solution. The preparation method of the diamond core nano polycrystalline material comprises the following steps: filling nano-diamond powder or nano-carbon powder containing partial nano-diamond powder into a boron nitride nanotube under an ultrasonic condition through wet mixing to obtain a filling body, treating the filling body under a vacuum condition, and prepressing and forming to obtain a blank; and sintering the blank to perform solid solution strengthening to obtain the diamond core nano polycrystalline material. The diamond core nano polycrystalline material can solve the technical problems of low hardness of cubic boron nitride and cutting graphitization of diamond in the prior art, simultaneously improves the thermal stability and hardness, enhances the wear resistance, and can be used for preparing superhard cutters.
Description
Technical Field
The invention relates to the technical field of superhard materials, in particular to a diamond core nano polycrystalline material, a preparation method thereof and a superhard cutter.
Background
In the prior art, diamond alone or Cubic Boron Nitride (PCBN) alone is commonly used as the superhard cutter cutting material. Diamond starts to be oxidized at about 600 ℃ in air due to poor thermal stability, and the diamond is easy to generate chemical reaction with ferrous metal at high temperature, so that the diamond cannot be industrially applied to materials such as cutting hardened steel and the like; cubic boron nitride can be used for cutting hardened steel, but is rarely used for processing harder materials such as stone materials, and because the hardness of the cubic boron nitride is only half of that of diamond, the processing efficiency of high-hardness materials is low.
In the process of implementing the invention, the inventor finds that the prior art knowledge has the following problems: diamond is easily graphitized when cutting ferrous metals, and cubic boron nitride has a lower hardness than diamond, and thus has a poor cutting effect on high-hardness materials.
Disclosure of Invention
The embodiment of the invention aims to provide a diamond core nano polycrystalline material, a preparation method thereof and a superhard cutter, which form a core-shell structure, so that the thermal stability, chemical inertia and hardness of the material are improved, and the wear resistance is enhanced.
In a first aspect, embodiments of the present invention provide a diamond core nano-polycrystalline material comprising an inner core comprising nano-diamond and an outer shell comprising a B-C-N solid solution.
Because the nano-diamond core and the B-C-N solid solution shell are formed, in the process of metal cutting, the B-C-N solid solution of the shell is in contact with a metal material, the graphitization of diamond is avoided, and because the diamond is the core of the diamond core nano polycrystalline material, the nano-diamond of the matrix structure in the B-C-N solid solution cannot collapse in the process of cutting by using the diamond core nano polycrystalline material, the overall strength of the diamond core nano polycrystalline material is enhanced, the stability is improved, and the wear resistance is enhanced.
In combination with the first aspect, in one possible implementation manner, a three-dimensional network, dense shell structure with strong covalent bonds is formed among the nitrogen atoms, the boron atoms and the carbon atoms of the shell.
The connection between the B-C-N solid solution of the shell and the nano-diamond of the core is more stable, the grain boundary is tightly closed, a high atom density structure is formed among boron atoms, carbon atoms and nitrogen atoms, and the performance of the nano-polycrystalline material of the diamond core is further improved.
In a second aspect, an embodiment of the present invention provides a method for preparing a diamond core nano polycrystalline material, including the following steps:
filling the nano-diamond powder or the nano-carbon powder containing part of the nano-diamond powder into a boron nitride nanotube under an ultrasonic condition through wet mixing to obtain a filling body, then treating the filling body under a vacuum condition, and prepressing and forming to obtain a blank; and sintering the blank to perform solid solution strengthening to obtain the diamond core nano polycrystalline material.
Through wet mixing and ultrasonic treatment, the potential barrier of the nano material can be overcome, the nano diamond powder or the nano carbon powder containing partial nano diamond powder is directionally filled into the boron nitride nano tube to form a filling body, and the treatment is carried out under the vacuum condition, the gas in the boron nitride tube is discharged, the connection between the nano-diamond powder or the nano-carbon powder containing partial nano-diamond powder and the boron nitride nanotube can be more compact, and the pre-pressing molding is carried out, so that the gaps among the initial material particles are reduced, the compactness between the nano-diamond powder or the nano-carbon powder containing partial nano-diamond powder and the boron nitride tube and between the filling material is improved, and sintering solid solution strengthening is carried out, so that the surface of the obtained diamond core nano polycrystalline material is a B-C-N solid solution, the core is nano diamond, and the surface is connected with the grain boundary of the core structure more compactly. The nano-particles are filled in the boron nitride tube, and finally the diamond core nano-polycrystalline material taking diamond as a core and B-C-N solid solution as a shell is directionally prepared, so that the overall strength of the diamond core nano-polycrystalline material is enhanced, the thermal stability and the chemical inertia are improved, and the wear resistance is enhanced.
In the prior art, the mechanical mixing of diamond and cubic boron nitride can cause that part of diamond without a solid solution surface layer or cubic boron nitride is exposed on the surface of a block material, or a diamond-cubic boron nitride alloy with lower strength and cubic boron nitride as a core can not achieve the effect of directional preparation.
With reference to the second aspect, in one possible implementation manner, the filling method includes filling a nano-diamond powder or a nano-carbon powder containing a part of the nano-diamond powder into a boron nitride nanotube under an ultrasonic condition by wet mixing to obtain a filling body, and includes: mixing 1-9 parts by weight of nano-diamond powder or nano-carbon powder containing part of nano-diamond powder with 1-9 parts by weight of boron nitride nanotubes to obtain a mixture, vibrating and wet-mixing the mixture under the condition that the ultrasonic frequency is 20Hz-200Hz to obtain a filler, and performing ultrasonic mixing to ensure that the filler is more uniformly filled.
Wherein, the grain diameter of the nano-diamond powder or the nano-carbon powder containing part of the nano-diamond powder can be 2-500nm, the inner diameter of the boron nitride nanotube can be 20-5000nm, when the nano-diamond powder or the nano-carbon powder containing part of the nano-diamond powder is uniformly mixed and filled, the grain diameter of the nano-diamond powder or the nano-carbon powder containing part of the nano-diamond powder is ensured to be smaller than the inner diameter of the boron nitride nanotube, so that the nano-diamond powder or the nano-carbon powder containing part of the nano-diamond powder can be filled into the boron nitride.
More nano-diamond powder or nano-carbon powder containing partial nano-diamond powder can be filled into the boron nitride nanotube, so that the finally obtained B-C-N solid solution shell is more tightly connected with the nano-diamond core, a B-C-N solid solution is formed between the core and the shell, the overall strength of the diamond core nano polycrystalline material is further enhanced, the stability is improved, and the wear resistance is enhanced.
In another possible implementation manner, in combination with the second aspect, the treatment is performed at a degree of vacuum of (4-10) × 10-3Pa, temperature of 800-1400 ℃ for 0.5-3 h.
The processing effect between the nano diamond powder or the nano carbon powder containing partial nano diamond powder and the boron nitride nanotube is better, the connection compactness is further improved, the overall strength of the diamond core nano polycrystalline material is enhanced, the stability is improved, and the wear resistance is enhanced.
With reference to the second aspect, in another possible implementation manner, the pre-pressing forming is performed for 1-20min under the condition that the pressure is 1-30MPa to obtain the blank.
The pre-pressing forming effect is better, the compactness between the diamond crystal and the B-C-N solid solution is further improved, the overall strength of the diamond core nano polycrystalline material is enhanced, the stability is improved, and the wear resistance is enhanced.
In combination with the second aspect, in another possible implementation manner, the solid solution strengthening is performed by sintering the blank at the temperature of 1000-3000 ℃ and the pressure of 5-30GPa for 10s-120 min.
The solid solution strengthening effect is better, the connection between the nano diamond and the B-C-N solid solution shell is further more compact, the overall strength of the diamond core nano polycrystalline material is enhanced, the stability is improved, and the wear resistance is enhanced.
In another possible implementation manner, in combination with the second aspect, the high-temperature high-pressure sintering device is a cubic press or any variant ultra-high-pressure device based on a cubic press.
In a further possible implementation in combination with the second aspect, the mixture is surface-treated with 3 to 5 parts by weight of a treating agent at a temperature of 50 to 200 ℃ before the treatment.
The method can remove the nano-diamond powder or the nano-carbon powder containing partial nano-diamond powder and the impurities on the surface of the boron nitride nanotube, avoid the influence of the impurities on the connection between the shell B-C-N solid solution and the core nano-diamond, further ensure the connection tightness between the nano-diamond and the B-C-N solid solution, enhance the overall strength of the diamond core nano polycrystalline material, improve the stability and enhance the wear resistance.
With reference to the second aspect, in another possible implementation manner, the treatment agent is selected from any one of hydrofluoric acid, aqua regia, hydrochloric acid, sulfuric acid, and nitric acid.
The removal effect of impurities (mainly some adsorbed organic matters) is better, for example: the removal effect on alcohol substances is better.
In another possible implementation manner in combination with the second aspect, the wet mixing is uniform wet mixing with 10 to 16 parts by weight of alcohol.
Through wet mixing, the nano-diamond powder or the nano-carbon powder containing part of the nano-diamond powder is easier to fill into the boron nitride nanotube, so that the subsequent preparation effect is better, and the finally obtained B-C-N solid solution shell is more tightly connected with the nano-diamond core.
In a third aspect, the embodiment of the invention provides a superhard cutting tool, and the manufacturing raw material of the superhard cutting tool comprises a diamond core nano polycrystalline material.
Firstly, processing the diamond core nano polycrystalline material into a cylinder with equal height, polishing two ends to be flat, processing into a triangular cylinder with side length and thickness of 2-3mm, and then processing into a triangular cylinder with vacuum degree of (1-10) multiplied by 10-3Alloy with metal under the conditions of Pa and temperature of 800-Welding the substrate, and then processing the substrate into a diamond core nano polycrystalline superhard cutter with a cutter point arc with the radius of 0.4-0.8mm by using laser.
The superhard cutter is made of a diamond core nano polycrystalline material, when metal is cut, the shell B-C-N solid solution is in contact with the metal, the nano diamond graphitization is avoided, the strength is high, the cutting effect is better, when stone such as granite is cut, the thermal stability and hardness of the cutter are improved, and the wear resistance is enhanced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments are briefly described below, it should be understood that the following drawings only illustrate some technical schematic diagrams of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without creative efforts, and the protection scope of the present invention also belongs to the protection scope of the present invention.
Fig. 1 is a technical schematic cross-sectional view of a diamond-cored nano-polycrystalline material of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The preparation method of the diamond core nano polycrystalline material comprises the following steps: filling the nano-diamond powder into a boron nitride nanotube under an ultrasonic condition through wet mixing to obtain a filler, treating the filler under a vacuum condition after strong acid treatment, and prepressing and forming to obtain a blank; and sintering the blank to perform solid solution strengthening to obtain the diamond core nano polycrystalline material.
Example 2
The preparation method of the diamond core nano polycrystalline material comprises the following steps:
(1) 1 part by weight of nano carbon powder with the grain diameter of 2-100nm and 9 parts by weight of boron nitride nano tube with the inner diameter of 20-1000nm are wet-mixed, and the nano carbon powder is filled into the boron nitride nano tube under the condition that the ultrasonic frequency is 20Hz to obtain the filling body.
(2) The packed body was evacuated to a vacuum of 4X 10-3Pa, at 1400 ℃ for 3h, and then prepressing under the pressure of 30MPa for 1min to obtain a blank.
(3) And sintering the blank at 2000 ℃ under the pressure of 20GPa for solid solution strengthening for 10min to obtain the diamond core nano polycrystalline material.
Example 3
The preparation method of the diamond core nano polycrystalline material comprises the following steps:
(1) and mixing 9 parts by weight of the 500nm diamond nanopowder and the graphene nanopowder with the particle size of 100-.
(2) Adding 3 parts by weight of treating agent into the raw materials at the temperature of 50 ℃ for surface treatment, dissolving impurities in the nano-diamond powder, the nano-graphene powder and the boron nitride nanotube, washing the mixture to be neutral by deionized water, drying the mixture, uniformly wet mixing the mixture by 10 parts by weight of alcohol, and vibrating the mixture by using an ultrasonic vibrator with the ultrasonic frequency of 200Hz to fill the nano-diamond powder and the nano-graphene powder into the boron nitride nanotube to obtain the filling body.
(3) The packed body was placed under a vacuum of 10X 10-3Pa, at 800 ℃ for 0.5h, and prepressing at room temperature under the pressure of 1MPa for 20min without adding any binder to obtain a blank.
(4) And putting the pre-pressed blank assembly sintering unit into a cubic press, and sintering and solid solution strengthening for 10s under the conditions that the temperature is 1900 ℃ and the pressure is 25GPa to obtain the diamond core nano polycrystalline material.
Example 4
The preparation method of the diamond core nano polycrystalline material comprises the following steps:
(1) 5 parts by weight of nano diamond powder with the particle size of 100-400nm and nano carbon powder are mixed with 5 parts by weight of boron nitride nano tube with the inner diameter of 500-4000 nm.
(2) Adding 5 parts by weight of treating agent (such as hydrofluoric acid or aqua regia or hydrochloric acid or sulfuric acid or nitric acid) into the raw materials at the temperature of 200 ℃ for surface treatment, dissolving impurities in the nano-diamond powder, the nano-carbon powder and the boron nitride nanotube, washing the mixture to be neutral by using deionized water, drying the mixture, uniformly wet mixing the mixture by using 16 parts by weight of alcohol, and vibrating the mixture by using an ultrasonic vibrator with the ultrasonic frequency of 100Hz to fill the nano-diamond powder and the nano-carbon powder into the boron nitride nanotube to obtain the filler.
(3) The packed body was then evacuated to a vacuum of 6X 10-3Pa, at 1000 deg.C for 1h, and prepressing at room temperature under 10MPa for 10min without adding any binder to obtain blank.
(4) And putting the pre-pressed blank assembly sintering unit into a cubic press, and sintering and solid solution strengthening for 30min under the conditions that the temperature is 2000 ℃ and the pressure is 10GPa to obtain the diamond core nano polycrystalline material.
Example 5
The preparation method of the diamond core nano polycrystalline material comprises the following steps:
(1) 4 parts by weight of nano diamond powder with the particle size of 20-200nm and 6 parts by weight of boron nitride nano tube with the inner diameter of 400-1000nm are mixed.
(2) Adding 4 parts by weight of hydrofluoric acid into the raw materials at the temperature of 100 ℃ for surface treatment, dissolving impurities in the nano-diamond powder and the boron nitride nanotube, washing the raw materials to be neutral by deionized water, drying the raw materials, uniformly wet-mixing the raw materials by 12 parts by weight of alcohol, and vibrating the raw materials by using an ultrasonic vibrator with the ultrasonic frequency of 100Hz to fill the nano-diamond powder into the boron nitride nanotube to obtain the filling body.
(3) The packed body was then evacuated to a vacuum of 6X 10-3Pa, at 1000 deg.C for 1h, and prepressing at room temperature under 10MPa for 10min without adding any binder to obtain blank.
(4) And putting the pre-pressed blank assembly sintering unit into a cubic press, and sintering and solid solution strengthening for 50min under the conditions that the temperature is 2000 ℃ and the pressure is 17GPa to obtain the diamond core nano polycrystalline material.
Experimental example 1
Example 5 a technical schematic cross-sectional view of a diamond-cored nano-polycrystalline material is obtained as shown in fig. 1. As can be seen from fig. 1, the nano polycrystalline material with the diamond core is of a core-shell structure, wherein the core, that is, the inner core is a diamond core, and the shell is a B-N-C solid solution, wherein the black sphere is a C atom, the light gray sphere is a B atom, the dark gray sphere is a N atom, the connection between the B-N-C solid solution and the nano diamond of the inner core is more stable, the grain boundary is tightly closed, so that a dense structure with a high atomic density structure, a three-dimensional network shape and a strong covalent bond is formed among boron atoms, carbon atoms and nitrogen atoms, the overall strength of the nano polycrystalline material with the diamond core is enhanced, the stability is improved, and the wear resistance is enhanced.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (8)
1. A preparation method of a diamond-core nano polycrystalline material is characterized in that the diamond-core nano polycrystalline material comprises an inner core and an outer shell, the inner core comprises nano diamond, the outer shell comprises a B-C-N solid solution, and a three-dimensional network dense shell structure with strong covalent bonds is formed among nitrogen atoms, boron atoms and carbon atoms of the outer shell; the preparation method comprises the following steps:
filling nano-diamond powder or nano-carbon powder containing partial nano-diamond powder into a boron nitride nanotube under an ultrasonic condition through wet mixing to obtain a filler, treating the filler under a vacuum condition, and prepressing and forming to obtain a blank; and sintering the blank to perform solid solution strengthening to obtain the diamond core nano polycrystalline material.
2. The preparation method according to claim 1, wherein the filling of the nano-diamond powder or the nano-carbon powder containing a part of the nano-diamond powder into the boron nitride nanotube under the ultrasonic condition by wet mixing to obtain the filling body comprises: mixing 1-9 parts by weight of the nano-diamond powder or nano-carbon powder containing part of the nano-diamond powder with 1-9 parts by weight of the boron nitride nanotube to obtain a mixture, and vibrating and wet-mixing the mixture under the condition that the ultrasonic frequency is 20Hz-200Hz to obtain the filling body.
3. The method according to claim 1, wherein the treatment is carried out under a vacuum of (4 to 10). times.10-3Pa, temperature of 800-1400 ℃ for 0.5-3 h.
4. The production method according to claim 1, wherein the preliminary press molding is performed for 1 to 20min under a pressure of 1 to 30MPa to obtain a blank.
5. The method according to claim 1, wherein the solid solution strengthening is performed by sintering the blank at 3000 ℃ and 5-30GPa for 10s-120 min.
6. The method according to claim 2, wherein the mixture is subjected to a surface treatment with 3 to 5 parts by weight of a treating agent at a temperature of 50 to 200 ℃ before the treatment.
7. The method according to claim 6, wherein the treating agent is any one selected from hydrofluoric acid, aqua regia, hydrochloric acid, sulfuric acid, and nitric acid.
8. The production method according to claim 6, wherein the wet-mixing is a uniform wet-mixing with 10 to 16 parts by weight of alcohol.
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| JP4029158B2 (en) * | 2004-01-30 | 2008-01-09 | 独立行政法人物質・材料研究機構 | Magnesium peroxide-containing boron nitride nanotubes and method for producing the same |
| TW200616907A (en) * | 2004-11-26 | 2006-06-01 | Hon Hai Prec Ind Co Ltd | A mold and a method of making the same |
| CN101899713B (en) * | 2009-05-31 | 2014-09-24 | 北京清大微纳科技有限公司 | Polycrystalline superhard material with gradient nano-micro structure and synthesis method thereof |
| CN102719220B (en) * | 2012-06-21 | 2014-10-29 | 南京航空航天大学 | Composite abrasive grain in grain/alumina core-shell structure and preparation method and application of composite abrasive grain |
| CN104759240A (en) * | 2015-04-14 | 2015-07-08 | 四川大学 | Diamond-cubic boron nitride type universal superhard cutter material, cutter and preparation method of material |
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