CN112047740B - Preparation method of aluminum nitride/diamond polycrystalline material - Google Patents
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Abstract
The invention belongs to the technical field of preparation and processing of diamond composite materials, and relates to a preparation method of a novel aluminum nitride/diamond polycrystalline material. The preparation method comprises the steps of fully mixing aluminum nitride powder, sintering aid and conductive metal powder, respectively carrying out cold pressing forming on the mixture and the diamond/cobalt composite layer, and preparing the novel aluminum nitride/diamond polycrystalline material by adopting a high-temperature high-pressure sintering method. The prepared aluminum nitride/diamond polycrystalline material has firm combination, controllable thickness, high grinding efficiency and good heat resistance, and the heat conductivity of the aluminum nitride matrix is far higher than that of a hard alloy matrix used by the traditional diamond polycrystalline composite sheet, so that the aluminum nitride/diamond polycrystalline material can be widely applied to the fields of automobiles, aerospace, energy sources and the like, and the requirement of high-speed precision processing of the material is met.
Description
Technical Field
The invention belongs to the technical field of preparation and processing of diamond composite materials, and particularly relates to a preparation method of a novel aluminum nitride/diamond polycrystalline material.
Background
Diamond has been used for hundreds of years as a superhard cutting tool material for cutting machining. In the seventies of the twentieth century, people use a high-pressure synthesis technology to synthesize polycrystalline diamond (PCD), so that the problems of rare quantity and high price of natural diamond are solved, and the application range of the diamond cutter is expanded to a plurality of fields such as aviation, aerospace, automobiles, electronics, stone and the like. The diamond cutter has the characteristics of high hardness, high compressive strength, good heat conductivity, good wear resistance and the like, and can obtain high processing precision and processing efficiency in high-speed cutting.
The traditional polycrystalline diamond material is mostly a hard alloy substrate and plays a good role in fixation and bonding. However, the heat conductivity of the hard alloy is not high and is only 65-80W/m.K, and in the process of processing and grinding the diamond cutter, heat is accumulated, the heat dissipation efficiency is poor, and the diamond is frequently carbonized at high temperature and failed in the working process, so that the heat dissipation problem of the diamond cutter substrate is always a critical point which needs to be solved urgently.
The aluminum nitride has high thermal conductivity, low dielectric constant and dielectric loss, high volume resistivity, good insulating property, high temperature resistance, no toxicity, good mechanical property and the like. The thermal conductivity can reach 320W/m.K, is close to BeO and SiC and is Al2O3More than 5 times, aluminum nitride is often used in electronic packaging materials. In addition, the hardness of the aluminum nitride is high, and the aluminum nitride is superior to the traditional aluminum oxide, is a novel wear-resistant ceramic material and can play an effective grinding role.
Disclosure of Invention
The invention aims to prepare a novel aluminum nitride/diamond polycrystalline material, and effectively solves the problem of poor heat dissipation of a diamond polycrystalline material substrate on the premise of ensuring the hardness of the substrate.
A preparation method of an aluminum nitride/diamond polycrystalline material is characterized by comprising the following preparation steps:
1) weighing aluminum nitride powder and sintering aid in a certain proportion, uniformly mixing by a ball milling method, drying and sieving to obtain mixed powder;
2) weighing a certain proportion of mixed powder and conductive metal powder, and uniformly mixing to obtain aluminum nitride composite powder;
3) weighing diamond micro powder and cobalt powder in a certain proportion, and uniformly mixing to obtain diamond composite powder;
4) weighing a certain amount of aluminum nitride composite powder according to the thickness and the diameter of the required diamond polycrystalline material, flatly paving the aluminum nitride composite powder in a graphite mold, carrying out cold press molding, and removing the mold to obtain an aluminum nitride sheet;
5) then weighing a certain amount of diamond composite powder, flatly paving the diamond composite powder in a graphite mould, carrying out cold press molding, and removing the mould to obtain a diamond sheet;
6) placing an aluminum nitride sheet on the lower layer, placing a diamond sheet on the upper layer, stacking and combining the aluminum nitride sheet and the diamond sheet into an aluminum nitride/diamond composite block, and placing the aluminum nitride sheet and the diamond sheet into a pyrophyllite closed block;
7) and finally, sintering the pyrophyllite sealing block obtained by the combination at high temperature and high pressure to obtain the novel aluminum nitride/diamond polycrystalline material.
Further, the aluminum nitride powder in the step 1) is commercial or laboratory synthetic aluminum nitride powder; the sintering aid comprises one or more of lanthanum oxide, yttrium oxide, cerium oxide, calcium oxide, lanthanum fluoride, yttrium fluoride, cerium fluoride and calcium fluoride, and accounts for 0.5-10% of the mixed powder by mass; the ball milling and mixing time is 1h-48 h.
Further, the conductive metal powder in the step 2) comprises silver powder, gold powder, copper powder, aluminum powder, zinc powder, molybdenum powder, tungsten powder, cobalt powder, nickel powder, iron powder, platinum powder, tin powder, chromium powder, titanium powder and the like, and accounts for 1% -20% of the mass of the aluminum nitride composite powder.
Further, the granularity range of the diamond micro powder in the step 3) is as follows: 0.2-60 μm; the cobalt powder is commercial or laboratory self-made cobalt powder; the cobalt powder accounts for 0.05-5% of the mass of the diamond composite powder.
Further, the thickness of the aluminum nitride/diamond polycrystalline material in the step 4) is 2mm-10mm, wherein the thickness of the aluminum nitride sheet is 1mm-7 mm.
Further, the thickness of the diamond sheet in the step 5) ranges from 1mm to 3 mm; the aluminum nitride sheet in the step 4) and the diamond sheet in the step 5) are both round sheets; the inner diameter range of the graphite grinding tool is 20mm-150 mm; the cold pressing pressure is 15MPa-60MPa, and the pressure maintaining time is 15s-300 s.
Further, the number of the aluminum nitride/diamond composite blocks in the pyrophyllite sealing block in the step 6) can be 1 or more; the diameter of the inner hole of the pyrophyllite sealing block is the same as the inner diameter of the graphite mould in the steps 4) and 5).
Further, the sintering pressure adopted by the high-temperature high-pressure sintering in the step 7) is as follows: 3GPa-50 GPa; the sintering temperature is as follows: 1100-1400 ℃.
The material obtained by the invention is a diamond polycrystalline material taking aluminum nitride as a matrix. The prepared aluminum nitride/diamond polycrystalline material is wear-resistant and sharp and has excellent heat-conducting property, and the problems that the heat conduction of a hard alloy matrix in the traditional diamond polycrystalline material is poor and a diamond working layer is carbonized and failed at high temperature can be effectively solved. The prepared aluminum nitride/diamond polycrystalline material has firm combination, controllable thickness, high grinding efficiency and good heat resistance, and the heat conductivity of the aluminum nitride matrix is far higher than that of a hard alloy matrix used by the traditional diamond polycrystalline composite sheet, so that the aluminum nitride/diamond polycrystalline material can be widely applied to the fields of automobiles, aerospace, energy sources and the like, and the requirement of high-speed precision processing of the material is met.
Detailed Description
Example 1
This example provides a method for preparing an aluminum nitride/polycrystalline diamond material with a diameter of 50mm and a thickness of 4mm, wherein the thickness of the aluminum nitride matrix layer is 2.5mm, and the thickness of the polycrystalline diamond layer is 1.5 mm. The method comprises the following specific steps: 490g of aluminum nitride powder, 8g of calcium oxide and 2g of yttrium fluoride are placed in a ball mill, ball-milled and mixed for 2 hours, and the mixture is dried and sieved to obtain mixed powder. And (3) placing 450g of mixed powder and 50g of iron powder in a ball mill, carrying out ball milling and mixing for 2h, drying and sieving to obtain the aluminum nitride composite powder. 298.5g of diamond micro powder with the diameter of 5 mu m and 1.5g of commercial cobalt powder are uniformly mixed to obtain the diamond composite powder. And pouring a proper amount of aluminum nitride composite powder into a graphite die with the inner diameter of 50mm (the thickness of the powder is about 4mm after the powder is tiled), and performing cold pressing and shaping, wherein the cold pressing pressure is 40MPa, and the pressure maintaining time is 180s, so as to obtain the aluminum nitride sheet. And then taking a proper amount of diamond composite powder, and repeating the operation (the thickness of the split body is about 2.5mm after the diamond composite powder is spread flatly) to obtain the diamond sheet. Placing the obtained aluminum nitride sheet at the lower layer, placing the diamond sheet at the upper layer, transferring the diamond sheet to the inner cavity of the pyrophyllite closed block with the inner diameter of 50mm, and sintering and forming by adopting a high-temperature high-pressure sintering method, wherein the sintering pressure is 6GPa, and the sintering temperature is 1200 ℃. After the pyrophyllite embryo is removed, the aluminum nitride/diamond polycrystalline material is obtained through subsequent processing such as grinding, polishing and excircle grinding.
Example 2
This example provides a method for preparing an aluminum nitride/diamond polycrystalline material with a diameter of 40mm and a thickness of 5mm, wherein the thickness of the aluminum nitride matrix layer is 3mm and the thickness of the diamond polycrystalline layer is 2 mm. The method comprises the following specific steps: 490g of aluminum nitride powder, 5g of calcium oxide and 5g of calcium fluoride are placed in a ball mill, ball-milled and mixed for 2 hours, and the mixture is dried and sieved to obtain mixed powder. And (3) placing 450g of mixed powder and 50g of nickel powder in a ball mill, carrying out ball milling and mixing for 2h, drying and sieving to obtain the aluminum nitride composite powder. 298.5g of diamond micro powder with the diameter of 10 mu m and 1.5g of commercial cobalt powder are uniformly mixed to obtain the diamond composite powder. And pouring a proper amount of aluminum nitride composite powder into a graphite die with the inner diameter of 40mm (the thickness of the powder is about 4mm after the powder is tiled), and performing cold pressing and shaping, wherein the cold pressing pressure is 35MPa, and the pressure maintaining time is 200s, so as to obtain the aluminum nitride sheet. And then taking a proper amount of diamond composite powder, and repeating the operation (the thickness of the split body is about 3mm after the diamond composite powder is spread flatly) to obtain the diamond sheet. Placing the obtained aluminum nitride sheet at the lower layer, placing the diamond sheet at the upper layer, transferring the diamond sheet to the inner cavity of the pyrophyllite closed block with the inner diameter of 40mm, and sintering and forming by adopting a high-temperature high-pressure sintering method, wherein the sintering pressure is 5.5GPa, and the sintering temperature is 1260 ℃. After the pyrophyllite embryo is removed, the aluminum nitride/diamond polycrystalline material is obtained through subsequent processing such as grinding, polishing and excircle grinding.
Claims (7)
1. A preparation method of an aluminum nitride/diamond polycrystalline material is characterized by comprising the following preparation steps:
1) weighing aluminum nitride powder and sintering aid in a certain proportion, uniformly mixing by a ball milling method, drying and sieving to obtain mixed powder;
2) weighing a certain proportion of mixed powder and conductive metal powder, and uniformly mixing to obtain aluminum nitride composite powder;
3) weighing diamond micro powder and cobalt powder in a certain proportion, and uniformly mixing to obtain diamond composite powder;
4) weighing a certain amount of aluminum nitride composite powder according to the thickness and the diameter of the required diamond polycrystalline material, flatly paving the aluminum nitride composite powder in a graphite mold, carrying out cold press molding, and removing the mold to obtain an aluminum nitride sheet;
5) then weighing a certain amount of diamond composite powder, flatly paving the diamond composite powder in a graphite mould, carrying out cold press molding, and removing the mould to obtain a diamond sheet;
6) placing an aluminum nitride sheet on the lower layer, placing a diamond sheet on the upper layer, stacking and combining the aluminum nitride sheet and the diamond sheet into an aluminum nitride/diamond composite block, and placing the aluminum nitride sheet and the diamond sheet into a pyrophyllite closed block;
7) finally, sintering the pyrophyllite sealing block obtained by the combination at high temperature and high pressure to obtain a novel aluminum nitride/diamond polycrystalline material;
and 7), sintering pressure adopted by the high-temperature high-pressure sintering is as follows: 5.5GPa-50 GPa; the sintering temperature is as follows: 1100-1400 ℃.
2. The method for preparing the aluminum nitride/diamond polycrystalline material according to claim 1, wherein the aluminum nitride powder in step 1) is a commercial or laboratory synthetic aluminum nitride powder; the sintering aid comprises one or more of lanthanum oxide, yttrium oxide, cerium oxide, calcium oxide, lanthanum fluoride, yttrium fluoride, cerium fluoride and calcium fluoride, and accounts for 0.5-10% of the mixed powder by mass; the ball milling and mixing time is 1h-48 h.
3. The method for preparing the aluminum nitride/diamond polycrystalline material according to claim 1, wherein the conductive metal powder in the step 2) comprises silver powder, gold powder, copper powder, aluminum powder, zinc powder, molybdenum powder, tungsten powder, cobalt powder, nickel powder, iron powder, platinum powder, tin powder, chromium powder and titanium powder, and accounts for 1-20% of the mass of the aluminum nitride composite powder.
4. The method for preparing the aluminum nitride/diamond polycrystalline material according to claim 1, wherein the grain size of the diamond micropowder obtained in the step 3) is within the following range: 0.2-60 μm; the cobalt powder is commercial or laboratory self-made cobalt powder; the cobalt powder accounts for 0.05-5% of the mass of the diamond composite powder.
5. The method for preparing the aluminum nitride/diamond polycrystalline material according to claim 1, wherein the thickness of the aluminum nitride/diamond polycrystalline material in the step 4) is 2mm-10mm, and the thickness of the aluminum nitride sheet is 1mm-7 mm.
6. The method for preparing the aluminum nitride/diamond polycrystalline material according to claim 1, wherein the thickness of the diamond sheet in the step 5) is 1mm to 3 mm; the aluminum nitride sheet in the step 4) and the diamond sheet in the step 5) are both round sheets; the inner diameter range of the graphite grinding tool is 20mm-150 mm; the cold pressing pressure is 15MPa-60MPa, and the pressure maintaining time is 15s-300 s.
7. The method for preparing the aluminum nitride/diamond polycrystalline material according to claim 1, wherein 1 or more aluminum nitride/diamond composite blocks in the pyrophyllite sealing block in the step 6) are provided; the diameter of the inner hole of the pyrophyllite sealing block is the same as the inner diameter of the graphite mould in the steps 4) and 5).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7132309B2 (en) * | 2003-04-22 | 2006-11-07 | Chien-Min Sung | Semiconductor-on-diamond devices and methods of forming |
| CN104014280B (en) * | 2014-06-18 | 2016-05-04 | 吉林大学 | A kind of polycrystalline diamond sintering method |
| CN105642191A (en) * | 2014-11-13 | 2016-06-08 | 吕艳 | Polycrystalline diamond composite sheet preparation process |
| CN206845104U (en) * | 2017-04-10 | 2018-01-05 | 泉州君寻贸易有限公司 | A kind of polycrystalline diamond compact bit of good heat dissipation effect |
| CN107098704A (en) * | 2017-05-08 | 2017-08-29 | 中原工学院 | A kind of preparation method of polycrystalline cubic boron nitride sintered material |
| CN109750204A (en) * | 2017-11-03 | 2019-05-14 | 河南海纳德新材料有限公司 | A kind of polycrystalline cubic boron nitride-diamond multilayer composite sheet and preparation method thereof |
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