CN111660211A - Polycrystalline diamond-like abrasive and preparation method thereof - Google Patents
Polycrystalline diamond-like abrasive and preparation method thereof Download PDFInfo
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- CN111660211A CN111660211A CN201911414671.1A CN201911414671A CN111660211A CN 111660211 A CN111660211 A CN 111660211A CN 201911414671 A CN201911414671 A CN 201911414671A CN 111660211 A CN111660211 A CN 111660211A
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- abrasive
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- polycrystalline diamond
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
- B24D3/20—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
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Abstract
The invention relates to a polycrystalline diamond-like abrasive and a preparation method thereof, belonging to the technical field of abrasives. The polycrystalline diamond-like abrasive material is a spherical structure formed by bonding diamond abrasive materials by using ceramic bonding agents, and the ceramic bonding agents are pyrolysis products of solidified liquid polysilazane. The polycrystalline diamond-like abrasive takes liquid polysilazane as an adhesive, and the liquid polysilazane is cured and pyrolyzed to form high-hardness ceramic, so that the polycrystalline diamond-like abrasive has high hardness and high processing efficiency. The invention also provides a preparation method of the polycrystalline diamond-like abrasive, which takes the liquid polysilazane as a bonding agent, completely wraps the diamond abrasive by the liquid polysilazane, isolates the contact between diamond and oxygen, can effectively ensure that the diamond abrasive is not oxidized during sintering, effectively avoids the influence of residual oxygen in a protective atmosphere, does not generate a melt flow phenomenon in the sintering process of the liquid polysilazane, and is beneficial to shape maintenance and post treatment of spherical particles.
Description
Technical Field
The invention relates to a polycrystalline diamond-like abrasive and a preparation method thereof, belonging to the technical field of abrasives.
Background
The artificial diamond abrasive has high hardness and high wear resistance, and the manufacturing cost is also increasingly reduced, and the proportion occupied in industrial processing is increasing. Diamond can be classified into single crystal diamond and polycrystalline diamond according to its crystal structure. The single crystal diamond crystal has anisotropy, large brittleness, few and large cutting edges and heavier processing traces; the polycrystalline diamond abrasive is mostly prepared by adopting a directional blasting method, crystals have isotropy, the particle toughness is large, the cutting edges are many and small, the self-sharpening performance is good, the processing efficiency is high, and a processed workpiece has better surface finish. However, the preparation method of the polycrystalline diamond is mainly a directional explosion method, and due to process limitation, the granularity is small, and the yield is not large, other methods are generated for preparing the abrasive particles with the characteristics similar to the characteristics of the polycrystalline diamond to replace the polycrystalline diamond.
The existing polycrystalline diamond-like abrasive materials on the market are mainly divided into the following parts, (1) after the surface of the single crystal diamond is treated, diamond particles with rough surfaces can be obtained, compared with the single crystal diamond particles, the diamond particles have more small cutting edges, but still have the characteristic of anisotropy, only the outermost layer of the particles has the cutting edges, and the grinding life of the particles is relatively short. (2) The method can obtain isotropic agglomerated abrasive particles, and the cutting edges of the inner layer and the outer layer of the particles are consistent, the service life is relatively long, but the strength of the glass binder is limited, so that the overall strength of the agglomerated particles is not very high. (3) The metal oxide glass binder needs to reach the melting point of glass to ensure that the glass has certain fluidity in the high-temperature sintering process, the process can cause the shape of spherical particles to change, and the bonding between the particles can occur, thereby having adverse effects on the shape maintenance of the particles and the post-treatment of the particles.
Disclosure of Invention
A first object of the present invention is to provide a polycrystalline diamond-like abrasive having a high hardness and a high processing efficiency.
The second purpose of the invention is to provide a preparation method of the polycrystalline diamond-like abrasive, which has simple operation and good controllability.
The technical scheme of the invention is as follows:
the polycrystalline diamond-like abrasive is a spherical structure formed by bonding diamond abrasives with ceramic bonding agents, and the ceramic bonding agents are pyrolysis products of solidified liquid polysilazane.
The polycrystalline diamond-like abrasive material is prepared by selecting liquid polysilazane as an adhesive, wherein a product obtained after the liquid polysilazane is cured and pyrolyzed is high-hardness ceramic which is higher than the hardness of a glass binder, and the obtained polycrystalline diamond-like abrasive material has high hardness, and has higher processing efficiency compared with the abrasive material obtained by a glass powder binder under the same diamond granularity in the same proportion.
Preferably, the grain size of the polycrystalline diamond-like abrasive is 10 times or more the grain size of the diamond abrasive; the average grain diameter of the polycrystalline diamond-like abrasive is 10 mu m-10 mm; the average grain diameter of the diamond abrasive is 0.05-100 mu m.
The kind of the diamond abrasive is not limited, and diamond abrasives commonly used in the art may be used, and preferably, the diamond abrasive is single crystal diamond powder, polycrystalline diamond powder, or single crystal diamond powder with a roughened particle surface.
The purity of the diamond abrasive is more than 99%.
A method of making a polycrystalline diamond-like abrasive, comprising the steps of:
(1) uniformly mixing the diamond abrasive with liquid polysilazane, curing, and sequentially crushing and granulating to obtain a ceramic precursor composite abrasive;
(2) and (3) sintering the ceramic precursor composite abrasive obtained in the step (1) in a protective atmosphere to obtain the polycrystalline diamond-like abrasive.
According to the preparation method of the polycrystalline diamond abrasive, the liquid polysilazane is used as a bonding agent, the diamond abrasive and the liquid polysilazane are uniformly mixed and then cured, and in the curing process, the liquid polysilazane completely wraps the diamond abrasive to isolate the contact between diamond and oxygen, so that the diamond abrasive is not oxidized during sintering, and the influence of residual oxygen in a protective atmosphere is effectively avoided. Meanwhile, in the invention, the liquid polysilazane is used as a bonding agent, and the liquid polysilazane does not melt and flow in the high-temperature cracking process of the spherical granular polycrystalline diamond-like abrasive material obtained by crushing and granulating after solidification, thereby being beneficial to shape maintenance and post-treatment of spherical granules.
The preparation method of the polycrystalline diamond-like abrasive material is simple to operate and easy to implement, and the polycrystalline diamond-like abrasive material can be obtained only by solidification, crushing, granulation and sintering. Meanwhile, the preparation method of the polycrystalline diamond abrasive material has good controllability, the grain size of the prepared polycrystalline diamond-like abrasive material can be controlled, the phenomenon of melt flow can not occur in the sintering process after the liquid polysilazane is solidified, and the spherical shape and the grain size of the ceramic precursor composite abrasive material can be maintained after sintering, so that the grain size of the ceramic precursor composite abrasive material can be determined according to the polycrystalline diamond-like abrasive material to be obtained, the grain size of the ceramic precursor composite abrasive material is obtained by crushing and granulating the uniformly mixed diamond abrasive material and the liquid polysilazane after being solidified, and the ceramic precursor composite abrasive material with a proper grain size can be obtained by controlling the crushed grain size and the granulated grain size.
Because the liquid polysilazane exists in a liquid state, the diamond abrasive and the liquid polysilazane can be mixed uniformly by directly adding the diamond abrasive into the liquid polysilazane and then mixing in a conventional mixing mode in the field, so that the bottom of the container is ensured to have no abrasive deposition, for example, the diamond abrasive can be uniformly dispersed in the liquid polysilazane by an ultrasonic wave stirring mode.
Since the liquid polysilazane can be crosslinked and cured at a high temperature, the uniformly mixed diamond abrasive and the liquid polysilazane can be cured by being placed in a high-temperature environment, and the type of the liquid polysilazane is not limited as long as the liquid polysilazane can be cured at a high temperature. Preferably, in the step (1), the liquid polysilazane has a trade name of liquid polysilazane 1800, and the curing temperature is 200-400 ℃. The liquid polysilazane 1800 can be smoothly crosslinked and cured within the temperature range of 200-400 ℃, and is coated around the diamond abrasive to form a solid.
Preferably, in the step (1), the curing time is 40-80 min.
Preferably, the temperature of the curing is 250 ℃; the curing time was 60 min.
In order to obtain the polycrystalline diamond-like abrasive material with the proper grain size, the solidified solid can be crushed and granulated according to the needs to obtain the ceramic precursor composite abrasive material with the proper grain size, and then the ceramic precursor composite abrasive material is sintered to obtain the polycrystalline diamond-like abrasive material with the target grain size. It can be understood that the grain size of the polycrystalline diamond-like abrasive is consistent with that of the ceramic precursor composite abrasive, and the grain size of the grains obtained after crushing is smaller than that of the ceramic precursor composite abrasive obtained by granulation. Preferably, in the step (1), the particle size of the particles obtained after crushing is 0.5-200 μm; the grain diameter of the ceramic precursor composite abrasive obtained after granulation is 10 mu m-10 mm.
The granulation method is not limited, and a dry granulation method or a wet granulation method, such as spray granulation, tumbling granulation, and boiling granulation, which are conventional in the art, may be selected as necessary. It can be understood that if the grain size of the ceramic precursor composite abrasive obtained after granulation is required to be small, for example, 20 to 60 μm, a spray granulation mode may be adopted, and if the grain size of the ceramic precursor composite abrasive obtained after granulation is required to be large, for example, 200 to 300 μm, a rolling granulation mode may be adopted.
And because of the hard characteristic of diamond, the grain diameter of the finally obtained polycrystalline diamond-like abrasive is far larger than that of the raw diamond abrasive. Preferably, the grain size of the polycrystalline diamond-like abrasive is 10 times or more the grain size of the diamond abrasive; the average grain diameter of the polycrystalline diamond-like abrasive is 10 mu m-10 mm; the average grain diameter of the diamond abrasive is 0.05-100 mu m. The particle size of the diamond abrasive is too small, the diamond abrasive is easy to agglomerate and is not easy to disperse uniformly when being mixed with liquid polysilazane, if the particle size of the diamond abrasive is too large, the particle size range of the prepared product is limited, for example, the particle size of the polycrystalline diamond-like abrasive prepared from the diamond abrasive of 200 micrometers is more than 2000 micrometers, and it can be understood that the diamond abrasive with the proper particle size range is selected when the polycrystalline diamond-like abrasive with the same particle size is prepared, and in the proper particle size range, the efficiency of preparing the polycrystalline diamond-like abrasive by taking the diamond abrasive with the large particle size as a raw material is higher.
The source of the diamond abrasive is not limited, and the diamond abrasive can be prepared by a method conventional in the field. For example, it may be a static pressure method or an explosion method.
It is understood that the protective atmosphere may be any protective gas conventional in the art, such as nitrogen, argon, and the like.
It should be understood that the relative amounts of the diamond abrasive and the liquid polysilazane are not limited as long as the diamond abrasive can be solidified and coated by the liquid polysilazane and sintered to obtain a polycrystalline diamond-like abrasive, and preferably, in step (1), the mass percentages of the diamond abrasive and the liquid polysilazane are as follows: 20 to 70 percent of diamond abrasive and 30 to 80 percent of liquid polysilazane.
Preferably, in the step (2), the sintering temperature is 1000-. The polycrystalline diamond-like abrasive can be obtained by reasonably adjusting the sintering temperature and time.
Detailed Description
The present invention will be further described with reference to the following embodiments.
First, specific examples of the polycrystalline diamond-like abrasive of the present invention are as follows:
example 1
In the polycrystalline diamond-like abrasive of the present embodiment, the polycrystalline diamond-like abrasive is a spherical structure formed by bonding diamond abrasives with a ceramic bond, and the ceramic bond is a pyrolysis product of liquid polysilazane 1800 after being cured.
The grain size of the polycrystalline diamond-like abrasive is 20 to 60 μm.
The average particle size of the diamond abrasive was 3 μm.
Example 2
In the polycrystalline diamond-like abrasive of the present embodiment, the polycrystalline diamond-like abrasive is a spherical structure formed by bonding diamond abrasives with a ceramic bond, and the ceramic bond is a pyrolysis product of liquid polysilazane 1800 after being cured.
The grain size of the polycrystalline diamond-like abrasive is 20 to 50 μm.
The average particle size of the diamond abrasive was 1 μm.
Example 3
In the polycrystalline diamond-like abrasive of the present embodiment, the polycrystalline diamond-like abrasive is a spherical structure formed by bonding diamond abrasives with a ceramic bond, and the ceramic bond is a pyrolysis product of liquid polysilazane 1800 after being cured.
The grain size of the polycrystalline diamond-like abrasive is 200-300 μm.
The average particle size of the diamond abrasive was 20 μm.
Secondly, the specific embodiment of the preparation method of the polycrystalline diamond-like abrasive material of the invention is as follows:
example 4
The method of making the polycrystalline diamond-like abrasive of this example produced the polycrystalline diamond-like abrasive of example 1, comprising the steps of:
(1) 3 mu m of diamond powder and liquid polysilazane (the trade name is liquid polysilazane 1800) are weighed, and according to the weight percentage, the 3 mu m of diamond powder is 50 percent, and the liquid polysilazane is 50 percent.
(2) Adding the diamond powder with the particle size of 3 mu m into the liquid polysilazane, stirring and ultrasonically dispersing for 15min to ensure that no abrasive material is precipitated at the bottom of the container.
The uniformly dispersed diamond suspension was cured by holding at 250 ℃ for 1 hour.
And crushing the solidified product into powder with the average particle size of 3.5-4.5 mu m, and performing spray granulation on the powder to obtain the spherical granular ceramic precursor composite abrasive with the particle size of 20-60 mu m.
(3) Under the protection of nitrogen, sintering the ceramic precursor composite abrasive at 1100 ℃ for 4 hours, and naturally cooling to room temperature to obtain the polycrystalline diamond-like abrasive with good sphericity.
The properties of the polycrystalline diamond-like abrasive obtained in this example were measured, and the following results were obtained:
preparing the prepared polycrystalline diamond-like abrasive into grinding fluid, processing a 2-inch sapphire wafer by matching with a grinding pad with Shore D hardness of about 75 degrees, and ensuring that the pressure per unit area is 200g/cm2The average removal rate of the wafer can reach 1.9 μm/min. Under the same condition, the same diamond powder and glass powder bonding agent (the glass powder bonding agent is borosilicate glass bonding agent, and mainly comprises SiO)2、B2O3、Al2O3、K2O and Na2O) the average removal rate of the wafer of the prepared spherical abrasive is about 1.6 mu m/min.
Example 5
The method of making the polycrystalline diamond-like abrasive of this example produced the polycrystalline diamond-like abrasive of example 2, comprising the steps of:
(1) weighing 1 micron of diamond powder and liquid polysilazane (the trade name is liquid polysilazane 1800), wherein the weight percentage of the 1 micron of diamond powder is 40 percent, and the weight percentage of the liquid polysilazane is 60 percent.
(2) Adding 1 micron diamond powder into liquid polysilazane, stirring and ultrasonically dispersing for 20min to ensure that no abrasive is precipitated at the bottom of the container.
The uniformly dispersed diamond suspension was cured by holding at 250 ℃ for 1 hour.
And crushing the solidified product into powder with the average particle size of 2-3 mu m, and carrying out rolling granulation on the powder to obtain the spherical granular ceramic precursor composite abrasive with the particle size of 20-50 mu m.
(3) Under the protection of nitrogen, sintering the ceramic precursor composite abrasive at 1100 ℃ for 4 hours, and naturally cooling to room temperature to obtain the polycrystalline diamond-like abrasive with good sphericity.
The properties of the polycrystalline diamond-like abrasive obtained in this example were measured, and the following results were obtained:
preparing the prepared polycrystalline diamond-like abrasive into grinding fluid, processing a 2-inch sapphire wafer, and preparingGrinding pad with Shore D hardness of about 75 degrees and unit area pressure of 200g/cm2The average removal rate of the wafer can reach 1.0 μm/min. Under the same condition, the same diamond powder and glass powder bonding agent (the glass powder bonding agent is borosilicate glass bonding agent, and mainly comprises SiO)2、B2O3、Al2O3、K2O and Na2O) the average removal rate of the wafer of the prepared spherical abrasive is about 0.8 mu m/min.
Example 6
The method of making the polycrystalline diamond-like abrasive of this example produced the polycrystalline diamond-like abrasive of example 3, comprising the steps of:
(1) 20 mu m of diamond powder and liquid polysilazane (with the trade name of liquid polysilazane 1800) are weighed, and according to the weight percentage, the 20 mu m of diamond powder is 60 percent, and the liquid polysilazane is 40 percent.
(2) Adding 20 mu m diamond powder into liquid polysilazane, stirring and ultrasonically dispersing for 10min to ensure that no abrasive material is precipitated at the bottom of the container.
The uniformly dispersed diamond suspension was cured by holding at 250 ℃ for 1 hour.
And crushing the solidified product into powder with the average particle size of 25-30 mu m, and carrying out rolling granulation on the powder to obtain the 200-300 mu m spherical granular ceramic precursor composite abrasive.
(3) Under the protection of nitrogen, sintering the ceramic precursor composite abrasive at 1400 ℃ for 4 hours, and naturally cooling to room temperature to obtain the polycrystalline diamond-like abrasive with good sphericity.
Claims (10)
1. The polycrystalline diamond-like abrasive is characterized in that the polycrystalline diamond-like abrasive is a spherical structure formed by bonding diamond abrasives by using a ceramic bond, and the ceramic bond is a product obtained by solidifying and pyrolyzing liquid polysilazane.
2. A polycrystalline diamond-like abrasive according to claim 1, wherein the grain size of the polycrystalline diamond-like abrasive is 10 times or more the grain size of the diamond abrasive; the average grain diameter of the polycrystalline diamond-like abrasive is 10 mu m-10 mm; the average grain diameter of the diamond abrasive is 0.05-100 mu m.
3. A polycrystalline diamond-like abrasive according to claim 1 or 2, wherein the diamond abrasive is single crystal diamond powder, polycrystalline diamond powder, or single crystal diamond powder with a roughened particle surface.
4. A method of producing a polycrystalline diamond-like abrasive according to any one of claims 1 to 3, comprising the steps of:
(1) uniformly mixing the diamond abrasive with liquid polysilazane, curing, and sequentially crushing and granulating to obtain a ceramic precursor composite abrasive;
(2) and (3) sintering the ceramic precursor composite abrasive obtained in the step (1) in a protective atmosphere to obtain the polycrystalline diamond-like abrasive.
5. The method for preparing the polycrystalline diamond-like abrasive material according to claim 4, wherein in the step (1), the mass percentages of the diamond abrasive material and the liquid polysilazane are as follows: 20 to 70 percent of diamond abrasive and 30 to 80 percent of liquid polysilazane.
6. The method for producing a polycrystalline diamond-like abrasive according to claim 4 or 5, wherein in the step (1), the liquid polysilazane is a liquid polysilazane 1800, and the curing temperature is 200 to 400 ℃.
7. The method of producing a polycrystalline diamond-like abrasive according to claim 6, wherein in the step (1), the time for solidification is 40 to 80 min.
8. A method for producing a polycrystalline diamond-like abrasive according to claim 4 or 5, wherein in the step (1), the particle size of the crushed particles is 0.5 μm to 200 μm; the grain diameter of the ceramic precursor composite abrasive obtained after granulation is 10 mu m-10 mm.
9. The method for preparing a polycrystalline diamond-like abrasive according to claim 4 or 5, wherein in the step (2), the sintering temperature is 1000-1500 ℃, and the sintering time is 3-6 h.
10. A method for producing a polycrystalline diamond-like abrasive according to claim 4 or 5, wherein the grain size of the polycrystalline diamond-like abrasive is 10 times or more the grain size of the diamond abrasive; the average grain diameter of the polycrystalline diamond-like abrasive is 10 mu m-10 mm; the average grain diameter of the diamond abrasive is 0.05-100 mu m.
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| CN113860301A (en) * | 2021-10-29 | 2021-12-31 | 河南联合精密材料股份有限公司 | Polycrystalline diamond-like powder with cracks on surface and preparation method thereof |
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