CN113860301B - Polycrystalline diamond-like powder with cracks on surface and preparation method thereof - Google Patents
Polycrystalline diamond-like powder with cracks on surface and preparation method thereof Download PDFInfo
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- CN113860301B CN113860301B CN202111272109.7A CN202111272109A CN113860301B CN 113860301 B CN113860301 B CN 113860301B CN 202111272109 A CN202111272109 A CN 202111272109A CN 113860301 B CN113860301 B CN 113860301B
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Abstract
The invention provides a quasi-polycrystalline diamond powder with cracks on the surface and a preparation method thereof. The invention enables the abrasive to form microcracks on the surface only without being broken through the collision between the ball and the abrasive; the oxidation of the oxidant is used to generate the oxide, one part of the oxide is in close contact with the surface of the milled powder, and the other part of the oxide permeates into the generated gap, so that rich cutting edges can be generated inside and outside the milled powder.
Description
Technical Field
The invention relates to the field of superhard abrasives, in particular to polycrystalline diamond-like powder with cracks on the surface and a preparation method thereof.
Background
In recent years, artificial diamond micropowder used as an "industrial tooth" has been widely used in industries such as semiconductor chips, photovoltaic solar silicon chips, mobile phones, tablet computers and the like. Moreover, with the continuous progress of science and technology, the application of various hard and brittle materials which are difficult to process puts higher and higher requirements on the processing of grinding and polishing. The traditional single crystal diamond has anisotropy, large brittleness, few and large cutting edges, is easy to scratch and can not meet the processing requirements; polycrystalline diamond has isotropy, large particle toughness, more and small cutting edges, good self-sharpening property and high processing efficiency, but the wider application of the polycrystalline diamond is limited due to the special process, smaller production particle size and low productivity.
Summary of the invention
Aiming at the technical problems, the invention provides the polycrystalline diamond-like powder with cracks on the surface and the preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the polycrystalline diamond-like powder with cracks on the surface is prepared by mixing an abrasive and a ball mixture, and then performing ball milling crushing, high-temperature sintering and purification treatment.
A method for preparing a polycrystalline diamond-like powder having a crack in the surface thereof according to any one of the above aspects, comprising the steps of:
s1, mixing iron balls and zirconia balls according to a ratio to obtain a ball mixture;
s2, selecting single-crystal diamond micro powder as an abrasive, mixing the abrasive and the ball mixture, and filling the mixture into a ball milling tank;
s3, adding an oxidant into the ball milling tank in the step S2;
s4, opening a ball milling tank switch to mix and crush to obtain a mixture A;
s5, pouring out the mixture A, drying at a low temperature, putting into a high-temperature furnace, vacuumizing, and performing high-temperature sintering treatment to obtain a mixture B;
s6, purifying the mixture B.
Preferably, the ball mixture in the step S1 comprises an iron ball with the diameter of 0.2 to 25mm and a zirconia ball with the diameter of 0.1 to 5mm.
Preferably, the ball mixture in the step S1 is prepared from 83.3% -92.8% by mass of iron balls and zirconia balls: 7.1-16.7 percent of the total weight of the components.
Preferably, the grinding material in the step S2 is single crystal diamond micro powder with the granularity of 3-120 mu m.
Preferably, the grinding material in the step S2 is mixed with the ball mixture according to the mass fraction of 12.5% -30.7%.
Preferably, the rotation speed of ball milling and crushing in the ball milling tank in the step S4 is 20 to 80r/min, and the crushing and shaping time is 10 to 180min.
Preferably, the sintering temperature in the step S5 is 800 to 1100 ℃, and the heat preservation is carried out for 2 to 4 hours.
Preferably, the oxidant in step S3 is hydrogen peroxide.
The invention has the beneficial effects that:
1. the invention utilizes the collision between the iron ball and the diamond to produce the following effects: the collision time is controlled, so that the diamond can be subjected to micro-crushing, micro-cracks are formed on the surface of the diamond only, and the diamond is not crushed; iron filings can be generated in the collision process, and meanwhile, part of iron-containing oxides generated on the surface of the iron ball is in close contact with the surface of the diamond by using the oxidation action of hydrogen peroxide, and the other part of iron-containing oxides permeates into generated gaps, so that rich cutting edges can be generated inside and outside the diamond;
2. in the grinding and polishing process, after the outer layer particles fall off, the inner layer particles can still have rich cutting edges, so that the grinding time is more durable;
3. when the bonded abrasive tool is processed, the rich cutting edges on the surface can keep high removal rate, and the surface cracks can increase the holding force of abrasive particles and a bonding agent.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The invention relates to a polycrystalline diamond-like powder with cracks on the surface and a preparation method thereof, wherein an iron ball with the diameter of 0.2-25mm and a zirconia ball with the diameter of 0.1-5 mm are firstly mixed according to the proportion of 83.3% -92.8%: 7.1-16.7% of ball mixture, wherein the required grinding material can be single crystal diamond micro powder with the particle size of 3-120 μm, the ball mixture and the ball mixture are mixed according to the mass fraction of 12.5-30.7% and are filled in a ball milling tank, and a certain amount of hydrogen peroxide is added as an oxidant. And opening a switch of the ball milling tank, and rotating at the speed of 20-80r/min for 10-180min.
After mixing, pouring out the required mixed materials, drying at low temperature, loading into a high-temperature furnace, and vacuumizing. And carrying out high-temperature sintering treatment, wherein the sintering temperature is 800-1100 ℃, and the heat preservation is carried out for 2-4h. And purifying the mixture after the heat treatment to obtain the composite material.
Example 2
The single crystal diamond micro powder has the granularity of 3 mu m, the weight of 200g, the diameter of an iron ball of 0.2mm, the weight of 500g, the diameter of a zirconia ball of 0.25mm and the weight of 50g, hydrogen peroxide of 20ml is added, the rotating speed is adjusted to be 20r/min, and the crushing and shaping time is 10min;
drying the crushed powder, briquetting, placing in a vacuum furnace, heating to 800 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 2 hours; naturally cooling to room temperature, taking out, and purifying to obtain the final product.
Preparing the prepared similar polycrystalline diamond powder into grinding fluid, processing a 2-inch sapphire substrate sheet, wherein the unit area pressure is 200g/cm & lt 2 & gt, the average removal rate of the wafer can reach 1.0 mu m/min, and the roughness Ra value is 0.04 mu m; under the same condition, the average removal rate of the wafer is about: 0.6 μm/min, roughness Ra 0.08. Mu.m.
Example 3
The granularity of the monocrystalline diamond micro powder is 25 mu m, the weight is about 600g, the diameter of an iron ball is 1mm, the weight is about 2000g, the diameter of a zirconia ball is 1mm, the weight is about 400g, about 50ml of hydrogen peroxide is added, the rotating speed is adjusted to 50r/min, the crushing and shaping time is 90min, the sintering temperature is 1000 ℃, and the heat preservation time is 2.5h;
drying the crushed powder, briquetting, placing in a vacuum furnace, heating to 1000 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 2.5h; naturally cooling to room temperature, taking out, and purifying to obtain the final product.
Preparing the prepared similar polycrystalline diamond powder into grinding fluid, processing a 2.5-inch sapphire substrate sheet, wherein the unit area pressure is 200g/cm < 2 >, the average removal rate of a wafer can reach 5.6 mu m/min, and the roughness Ra value is 0.09 mu m; under the same condition, the average removal rate of the wafer is about: 2.9 μm/min, roughness Ra 0.13. Mu.m.
Example 4
The granularity of the monocrystal diamond micro powder is 65 mu m, the weight is about 1500g, the diameter of an iron ball is 10mm, the weight is about 6000g, the diameter of a zirconia ball is 5mm, the weight is about 800g, about 100ml of hydrogen peroxide is added, the rotating speed is adjusted to 60r/min, the crushing and shaping time is 240min, the sintering temperature is 1100 ℃, and the heat preservation time is 3h;
drying the crushed powder, briquetting, placing in a vacuum furnace, heating to 1100 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 3h; naturally cooling to room temperature, taking out, and purifying to obtain the final product.
Preparing the prepared similar polycrystalline diamond powder into a polishing pad, processing microcrystalline glass at 100r/min, wherein the average removal rate can reach 180 mu m/min, and the roughness Ra value is 0.7 mu m; under the same condition, the average removal rate of the diamond powder is about: 100 μm/min, roughness Ra 0.8. Mu.m.
Example 5
The single crystal diamond micro powder has the granularity of 120 mu m, the weight of 2200g, the diameter of an iron ball of 25mm, the weight of 8000g, the diameter of a zirconia ball of 5mm and the weight of 2000g, hydrogen peroxide of 200ml is added, the rotating speed is adjusted to 80r/min, the crushing and shaping time is 15min, the sintering temperature is 1000 ℃, and the heat preservation time is 4h;
drying the crushed powder, briquetting, placing in a vacuum furnace, heating to 1100 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 4 hours; naturally cooling to room temperature, taking out, and purifying to obtain the final product.
Preparing the prepared similar polycrystalline diamond powder into a polishing pad, processing a ceramic back plate, wherein the average removal rate of 120r/min can reach 200 mu m/min, and the roughness Ra value is 0.8 mu m; under the same condition, the average removal rate of the diamond powder is about: 120 μm/min, roughness Ra value of 0.9 μm.
Example 6
The single crystal diamond micro powder has the granularity of 3 mu m, the weight of 100g, the diameter of an iron ball of 0.5mm, the weight of 650g, the diameter of a zirconia ball of 0.1mm and the weight of 50g, hydrogen peroxide of 20ml is added, the rotating speed is adjusted to be 25r/min, and the crushing and shaping time is 10min;
drying the crushed powder, briquetting, placing in a vacuum furnace, heating to 800 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 2 hours; naturally cooling to room temperature and taking out. Purifying to obtain the product.
Preparing the prepared similar polycrystalline diamond powder into grinding fluid, processing a 2-inch sapphire substrate sheet with the unit area pressure of 200g/cm 2 The average removal rate of the wafer can reach 1.0 mu m/min, and the roughness Ra value is 0.04 mu m; under the same conditions, gold is adoptedThe average removal rate of the diamond powder, wafer, was about: 0.6 μm/min, roughness Ra 0.08 μm.
Example 7
The single crystal diamond micro powder has the granularity of 10 mu m, the weight of 200g, the diameter of an iron ball of 0.5mm, the weight of 1000g, the diameter of a zirconia ball of 0.25mm and the weight of 100g, hydrogen peroxide of 30ml is added, the rotating speed is adjusted to 25r/min, and the crushing and shaping time is 60min;
drying the crushed powder, briquetting, placing in a vacuum furnace, heating to 900 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 2 hours; naturally cooling to room temperature and taking out. Purifying to obtain the product.
Preparing the prepared similar polycrystalline diamond powder into grinding fluid, processing a 2.5-inch sapphire substrate sheet, and processing the sapphire substrate sheet with the unit area pressure of 200g/cm 2 The average removal rate of the wafer can reach 1.6 mu m/min, and the roughness Ra value is 0.06 mu m; under the same condition, the average removal rate of the wafer is about: 0.6 μm/min, roughness Ra 0.09 μm.
Example 8
The granularity of the monocrystalline diamond micro powder is 25 mu m, the weight is about 600g, the diameter of an iron ball is 1mm, the weight is about 2000g, the diameter of a zirconia ball is 1mm, the weight is about 400g, about 50ml of hydrogen peroxide is added, the rotating speed is adjusted to 50r/min, the crushing and shaping time is 90min, the sintering temperature is 1000 ℃, and the heat preservation time is 2.5h;
drying the crushed powder, briquetting, placing in a vacuum furnace, heating to 1000 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 2.5h; naturally cooling to room temperature and taking out. Purifying to obtain the product.
Preparing the prepared similar polycrystalline diamond powder into grinding fluid, processing a 2.5-inch sapphire substrate sheet, wherein the unit area pressure is 200g/cm & lt 2 & gt, the average removal rate of the wafer can reach 5.6 mu m/min, and the roughness Ra value is 0.09 mu m; under the same condition, the average removal rate of the wafer is about: 2.9 μm/min, roughness Ra 0.13. Mu.m.
Example 9
The granularity of the monocrystal diamond micro powder is 65 mu m, the weight is about 1500g, the diameter of an iron ball is 10mm, the weight is about 6000g, the diameter of a zirconia ball is 5mm, the weight is about 800g, about 100ml of hydrogen peroxide is added, the rotating speed is adjusted to 60r/min, the micro crushing time is 120min, the sintering temperature is 1100 ℃, and the temperature is kept for 3h;
drying the crushed powder, briquetting, placing in a vacuum furnace, heating to 1100 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 3h; naturally cooling to room temperature and taking out. Purifying to obtain the product.
Preparing the prepared polycrystal-like diamond powder into a polishing pad, processing microcrystalline glass at 100r/min, wherein the average removal rate can reach 180 mu m/min, and the roughness Ra value is 0.7 mu m; under the same condition, the average removal rate of the diamond powder is about: 100 μm/min, roughness Ra value of 0.8 μm.
Example 10
The granularity of the monocrystalline diamond micro powder is 120 mu m, the weight is about 4000g, the diameter of an iron ball is 25mm, the weight is about 8000g, the diameter of a zirconia ball is 5mm, the weight is about 960g, about 200ml of hydrogen peroxide is added, the rotating speed is adjusted to 80r/min, and the micro-crushing time is 180min;
drying the crushed powder, briquetting, placing in a vacuum furnace, heating to 1100 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 4 hours; naturally cooling to room temperature and taking out. Purifying to obtain the product.
Preparing the prepared similar polycrystalline diamond powder into a polishing pad, processing a ceramic back plate, wherein the average removal rate of 120r/min can reach 200 mu m/min, and the roughness Ra value is 0.8 mu m; under the same condition, the average removal rate of the diamond powder is about: 120 μm/min, roughness Ra value of 0.9 μm.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The preparation method of the quasi-polycrystalline diamond powder with cracks on the surface is characterized in that the quasi-polycrystalline diamond powder is prepared by mixing an abrasive and a ball mixture and then performing ball milling, crushing, high-temperature sintering and purification treatment; the preparation method of the polycrystalline diamond-like powder with cracks on the surface comprises the following steps:
s1, mixing iron balls and zirconia balls according to a ratio to obtain a ball mixture;
s2, selecting single-crystal diamond micro powder as an abrasive, mixing the abrasive and the ball mixture, and filling the mixture into a ball milling tank;
s3, adding an oxidant into the ball milling tank in the step S2;
s4, opening a switch of the ball milling tank to mix and crush to obtain a mixture A;
s5, pouring out the mixture A, drying at a low temperature, putting into a high-temperature furnace, vacuumizing, and performing high-temperature sintering treatment to obtain a mixture B;
s6, purifying the mixture B;
the rotation speed of ball milling and crushing in the ball milling tank in the step S4 is 20 to 80r/min, and the crushing and shaping time is 10 to 180min;
the oxidant in the step S3 is hydrogen peroxide.
2. The method for preparing a polycrystalline diamond-like powder having cracks on the surface according to claim 1, wherein the ball mixture in the step S1 comprises iron balls with a diameter of 0.2 to 25mm and zirconia balls with a diameter of 0.1 to 5 mm.
3. The method for preparing a polycrystalline diamond-like powder having a cracked surface according to claim 2, wherein the ball mixture in step S1 is prepared from iron balls and zirconia balls in a mass fraction of 83.3% to 92.8%:7.1% -16.7% of the above-mentioned raw materials.
4. The method for preparing the polycrystalline diamond-like powder with the cracked surface according to any one of claims 1~3, wherein the abrasive in the step S2 is single-crystal diamond micro powder with the grain size of 3-120 μm.
5. The method for preparing a polycrystalline diamond-like powder having a cracked surface according to claim 4, wherein the abrasive in the step S2 is mixed with the ball mixture in a proportion of 12.5 to 30.7% by mass.
6. The method for preparing the polycrystalline diamond-like powder with cracks on the surface according to any one of claims 1~3 and 5, wherein the sintering temperature in the step S5 is 800-1100 ℃, and the temperature is kept for 2-4h.
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| CN101228095A (en) * | 2005-07-21 | 2008-07-23 | 住友电气工业株式会社 | High-hardness polycrystalline diamond and process for producing the same |
| CN102757044A (en) * | 2012-07-23 | 2012-10-31 | 河南省联合磨料磨具有限公司 | High-cutting-force diamond micro powder and preparation method thereof |
| CN104853837A (en) * | 2012-06-15 | 2015-08-19 | 第六元素研磨剂股份有限公司 | Multi-layered polycrystalline diamond structure |
| CN111660211A (en) * | 2019-12-31 | 2020-09-15 | 河南联合精密材料股份有限公司 | Polycrystalline diamond-like abrasive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005065809A1 (en) * | 2003-12-11 | 2005-07-21 | Sumitomo Electric Industries, Ltd. | High-hardness conductive diamond polycrystalline body and method for producing same |
| GB201122365D0 (en) * | 2011-12-28 | 2012-02-01 | Element Six Abrasives Sa | Method of making polycrystalline diamond material |
| GB201622472D0 (en) * | 2016-12-31 | 2017-02-15 | Element Six (Uk) Ltd | Superhard constructions & methods of making same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101228095A (en) * | 2005-07-21 | 2008-07-23 | 住友电气工业株式会社 | High-hardness polycrystalline diamond and process for producing the same |
| CN104853837A (en) * | 2012-06-15 | 2015-08-19 | 第六元素研磨剂股份有限公司 | Multi-layered polycrystalline diamond structure |
| CN102757044A (en) * | 2012-07-23 | 2012-10-31 | 河南省联合磨料磨具有限公司 | High-cutting-force diamond micro powder and preparation method thereof |
| CN111660211A (en) * | 2019-12-31 | 2020-09-15 | 河南联合精密材料股份有限公司 | Polycrystalline diamond-like abrasive and preparation method thereof |
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