CN113880082B - Preparation method of diamond micro powder for precision machining - Google Patents

Preparation method of diamond micro powder for precision machining Download PDF

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Publication number
CN113880082B
CN113880082B CN202111135856.6A CN202111135856A CN113880082B CN 113880082 B CN113880082 B CN 113880082B CN 202111135856 A CN202111135856 A CN 202111135856A CN 113880082 B CN113880082 B CN 113880082B
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micro powder
diamond micro
raw materials
precision machining
diamond
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CN113880082A (en
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陈强
花波波
张钲
王宬哲
王恒
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Henan Yalong Diamond Tools Co ltd
Zhengzhou Haocheng Superhard Tool Co ltd
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Henan Yalong Diamond Tools Co ltd
Zhengzhou Haocheng Superhard Tool Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/25Diamond
    • C01B32/28After-treatment, e.g. purification, irradiation, separation or recovery

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Polishing Bodies And Polishing Tools (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The invention discloses a preparation method of diamond micro powder for precision machining; adding a certain proportion of additives into the traditional diamond micro powder, and then granulating, roasting and post-treating to obtain a product; the method is simple to operate and easy to realize batch industrialization; compared with the traditional diamond micro powder, the diamond micro powder prepared by the method has the advantages of more cutting edges, good self-sharpening property, high grinding efficiency and the like, has fine grinding lines in operation, high processing precision and dispersed grinding stress, overcomes the defect that the traditional diamond micro powder has poor self-sharpening property and is easy to generate fine scratches, and is particularly suitable for precision machining in the fields of IT silicon wafers, red, sapphire, precision ceramics, optical products, optical fiber communication and the like.

Description

Preparation method of diamond micro powder for precision machining
Technical Field
The invention relates to the technical field of precision machining, in particular to a preparation method of diamond micro powder for precision machining.
Background
Diamond micropowder is the hardest superfine abrasive, and is an important processing raw material in the processing procedures of grinding, lapping, polishing and the like with the excellent performances of high hardness, high wear resistance, high compressive strength and good thermal conductivity, and has been widely used in the industrial departments of machinery, aerospace, optical instruments, glass, ceramics, electronics, petroleum, geology and military industry, particularly in the aspect of precise and ultra-precise processing, because of the high requirements on the grinding tool in the aspects of hardness, strength, thermal conductivity and the like, the grinding tool made of the diamond micropowder occupies the vast majority of the grinding tools.
At present, the traditional diamond micro powder manufacturing method mainly comprises two steps, wherein one is formed by taking monocrystalline diamond of an I-type material as a raw material and crushing, shaping and sorting the monocrystalline diamond. The diamond micro powder has high impurity content and low strength, and the cutting edge on the surface of the micro powder particles is large and hard, so that deep scratches are easily generated on a workpiece in high-precision machining, and the product requirement of a high-end market on diamond micro powder cannot be met. The other is a detonation method (polycrystalline diamond micropowder), and most of the diamond micropowder prepared by the method is nano-scale, has high impurity content and higher production cost. In addition, the diamond micro powder manufactured by the traditional method has the defects of poor isotropy and self-sharpening, sharp particles are easy to generate deeper vertical micro-breaking in the precise and ultra-precise machining process, and fine scratches can be generated on the machined surface, so that the precision of a device is affected.
Therefore, how to obtain diamond micro powder which has the advantages of simple operation, easy realization of batch production, good processing effect, high efficiency and low cost and meets the requirements of precision processing becomes a technical problem to be solved in the field.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of diamond micro powder for precision machining, which aims to solve the defects of poor machining effect, low efficiency and the like of the traditional diamond micro powder in precision and ultra-precision machining at present. The invention has simple operation and high output efficiency, and is easy to realize batch production.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of diamond micro powder for precision machining is characterized by comprising the following steps: adding a certain proportion of additives into the traditional diamond micro powder, and granulating, roasting and post-treating the mixture; the method specifically comprises the following steps:
(1) Mixing: weighing diamond micropowder raw materials, iron powder raw materials and graphite powder raw materials according to mass percent, putting the raw materials into an omnibearing planetary ball mill, uniformly mixing, wherein the rotation speed of a mixing tank is 100-200 rpm, the revolution speed is 50-100rpm, and the overturning speed of a carrying disc for carrying the mixing tank is 1.5rpm;
(2) Granulating: adding an organic solvent and a binder into the mixed materials, and granulating by a granulator;
(3) Roasting: placing the granulated material into a tube furnace, heating to 300-350 ℃, and preserving heat for 1-2h; then vacuuming to 1.0X10 -3 ~9.0×10 -3 Pa, heating to 500-650 ℃, and preserving heat for 1-2h; then heating to 800-900 ℃, preserving heat for 2-5 h, introducing oxygen for 1-3 times during the period, keeping the pressure in the furnace to normal pressure each time, maintaining for 10-20 minutes, and vacuumizing to 10Pa; cooling to room temperature after the whole heat preservation is finished;
(4) Post-treatment: and (3) pickling and drying the roasted material to obtain the diamond micro powder for precision machining.
Preferably, the weight percentages of the raw materials in the step (1) are 60-85% of the diamond micro powder raw material, 5-30% of the iron powder raw material and 5-20% of the graphite powder raw material.
Preferably, the step of mixing in the step (1) is to firstly load the iron powder raw material and the graphite powder raw material into a stainless steel mixing tank, ball-mill the stainless steel mixing tank on an omnibearing planetary ball mill for 2 to 3 hours, and then ball-mill the stainless steel mixing tank with the diamond micro powder raw material and the stainless steel spring as mixing media for 4 to 8 hours.
Further, the diameter of the stainless steel spring is 10mm.
Preferably, the mass ratio of the diamond micro powder to the stainless steel spring is 1:3-1:1.
Preferably, the organic solvent in step (2) is isopropanol or acetone.
Preferably, the binder in step (2) is WS-120 or GB-600.
Further, in the step (3), the tubular furnace is provided with a rotating device, and the rotating speed is 1-60 rpm.
The preparation method of the invention takes iron powder and graphite powder as additives, mixes diamond micro powder, iron powder and graphite powder according to a certain proportion, and obtains the diamond micro powder for precision machining through granulation, roasting and post-treatment.
According to the invention, the uniformity of materials in the mixing tank is ensured in a mode of rotation, revolution and 360-degree rotation of the space in the mixing aspect; meanwhile, the granulation process is assisted, so that mutual wrapping among the iron powder, the graphite powder and the diamond powder is realized.
According to the invention, iron which has better wettability to diamond and low cost is selected as an additive, C in diamond breaks away from diamond lattice to form graphite under the catalysis of iron at high temperature, and further C diffuses into the iron and undergoes dissolution reaction; and graphite powder is added into the diamond powder, so that the iron powder is effectively prevented from phagocytic dissolution of the diamond powder; meanwhile, the graphite powder and the iron powder cannot react in a vacuum state; in the area covered by the iron powder, the surface C of the diamond micro powder is gradually dissolved by the iron to form pits, and the diamond micro powder in the area covered by the graphite powder is kept as it is; finally, pits and new cutting edges with different sizes and depths are formed on the surface of the obtained diamond micro powder; in addition, the graphite powder can be used as a lubricant for the fine diamond powder in the fine machining process, and is more beneficial to the fine machining process.
The invention adds the procedure of artificial oxygen introduction during the roasting period, thereby effectively ensuring the full dissolution of the iron powder to the diamond part area and ensuring that the surface of the prepared diamond micro powder forms pits and cutting edges with proper size.
The beneficial effects of the invention are that
The method for preparing the diamond micro powder for precision machining is simple to operate and easy to realize batch industrialization; compared with the traditional diamond micro powder, the prepared diamond micro powder has the advantages of more cutting edges, good self-sharpening property, high grinding efficiency and the like, has fine grinding lines during operation, high processing precision and dispersed grinding stress, solves the problem that the traditional diamond micro powder has poor self-sharpening property and is easy to generate fine scratches, and is suitable for precision machining in the fields of IT silicon wafers, red, sapphires, precision ceramics, optical products, optical fiber communication and the like.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below in connection with specific embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. The methods described in the examples are conventional methods unless otherwise specified, and the starting materials described are commercially available unless otherwise specified; while the following examples are provided for illustration of the invention, they should not be construed as limiting the scope of the invention.
Example 1
The preparation method of the diamond micro powder for precision machining specifically comprises the following steps:
(1) Mixing: weighing 60% of diamond micro powder, 30% of iron powder and 10% of graphite powder according to mass percentage, firstly loading the iron powder and the graphite powder into a stainless steel mixing tank, ball milling for 3 hours on an omnibearing planetary ball mill, and then adding the diamond micro powder and a stainless steel spring with the diameter of 10mm for ball milling for 8 hours, wherein the mass ratio of the diamond micro powder to the stainless steel spring is 1:3. the rotation speed of the mixing tank during ball milling is set to be 200rpm, the revolution rotation speed is set to be 100rpm, and the overturning drilling speed of the carrying disc carrying the mixing tank is 1.5rpm.
(2) Granulating: isopropanol and WS-120 were added to the mixed material, and granulation was performed by a granulator.
(3) Roasting: the granulated material was placed in a rotatable tube furnace at 20rpm. Heating to 320 ℃, and preserving heat for 1.5h. Mainly used for volatilizing the isopropanol and WS-120 in the granulation. Then vacuuming to 1.0X10 -3 Pa, heating to 550 ℃, keeping the temperature for 2 hours, then heating to 830 ℃, keeping the temperature for 4 hours, introducing oxygen 3 times during the heat preservation, keeping the pressure in the furnace to normal pressure each time, keeping for 10 minutes, and vacuumizing to 10Pa. And cooling to room temperature after the whole heat preservation is finished.
(4) Post-treatment: and (3) pickling and drying the roasted material to obtain the product.
The diamond micropowder prepared in this example and conventional diamond micropowder of the same quality were placed in a MODEL 920 polishing machine to carry out silicon carbide wafer polishing experiments, the rotation speed of a polishing disk was 80r/min, the polishing pressure was 6.35kPa, the polishing time was 20min, and the polishing efficiency was as shown in Table 1:
table 1.
As can be seen from the data in Table 1, the removal rate of the diamond micro powder prepared in this example is about 2.1 times that of the conventional diamond micro powder, and the roughness value Ra of the polished wafer is about 25% of that of the conventional diamond particles, so that the polishing efficiency and accuracy of the silicon carbide wafer can be remarkably improved.
Example 2
The preparation method of the diamond micro powder for precision machining specifically comprises the following steps:
(1) Mixing: weighing 85% of diamond micro powder, 10% of iron powder and 5% of graphite powder according to mass percentage, firstly loading the iron powder and the graphite powder into a stainless steel mixing tank, ball milling for 1 hour on an omnibearing planetary ball mill, and then adding the diamond micro powder and a stainless steel spring with the diameter of 10mm for ball milling for 4 hours, wherein the mass ratio of the diamond micro powder to the stainless steel spring is 1:1. The rotation speed of the mixing tank during ball milling is set to be 100rpm, the revolution rotation speed is set to be 50rpm, and the overturning drilling speed of the carrying disc carrying the mixing tank is 1.5rpm.
(2) Granulating: adding isopropanol and GB-600 into the mixed materials, and granulating by a granulator.
(3) Roasting: the granulated material was placed in a rotatable tube furnace at 50rpm. Heating to 350 ℃, and preserving heat for 1h. Mainly used for volatilizing isopropanol and GB-600 in the pelletization, and then vacuumized to 5.0X10 -3 Pa, heating to 650 ℃, preserving heat for 1h, then heating to 880 ℃, preserving heat for 2h, introducing oxygen for 1 time, maintaining the pressure in the furnace to normal pressure each time, maintaining for 15 minutes, and vacuumizing to 10Pa. And cooling to room temperature after the whole heat preservation is finished.
(4) Post-treatment: and (3) pickling and drying the roasted material to obtain the product.
The diamond micropowder prepared in this example and conventional diamond micropowder of the same quality were placed in a MODEL 920 polishing machine to carry out silicon carbide wafer polishing experiments, the rotation speed of a polishing disk was 80r/min, the polishing pressure was 6.35kPa, the polishing time was 20min, and the polishing efficiency was as shown in Table 2:
table 2.
As can be seen from the data in Table 2, the removal rate of the diamond micro powder prepared in this example is about 1.9 times that of the conventional diamond micro powder, and the roughness value Ra of the polished wafer is about 27% of that of the conventional diamond particles, so that the polishing efficiency and accuracy of the silicon carbide wafer can be remarkably improved.
Example 3
The preparation method of the diamond micro powder for precision machining specifically comprises the following steps:
(1) Mixing: weighing 75% of diamond micro powder, 5% of iron powder and 20% of graphite powder according to mass percentage, firstly loading the iron powder and the graphite powder into a stainless steel mixing tank, ball milling for 2 hours on an omnibearing planetary ball mill, and then adding the diamond micro powder and a stainless steel spring with the diameter of 10mm for ball milling for 6 hours, wherein the mass ratio of the diamond micro powder to the stainless steel spring is 1:2. The rotation speed of the mixing tank during ball milling is set to 150rpm, the revolution rotation speed is set to 75rpm, and the overturning drilling speed of the carrying tray carrying the mixing tank is 1.5rpm.
(2) Granulating: adding isopropanol and GB-600 into the mixed materials, and granulating by a granulator.
(3) Roasting: the granulated material was placed in a rotatable tube furnace at 35rpm. Heating to 300 ℃, and preserving heat for 2 hours. Is mainly used for volatilizing the isopropanol and GB-600 in the granulation. Then vacuuming to 9.0X10 -3 Pa, heating to 600 ℃, preserving heat for 1.5h, then heating to 850 ℃, preserving heat for 3h, introducing oxygen 2 times during the heat preservation, maintaining the pressure in the furnace to normal pressure for 15 minutes after each time of introducing the oxygen, and vacuumizing to 10Pa. And cooling to room temperature after the whole heat preservation is finished.
(4) Post-treatment: and (3) pickling and drying the roasted material to obtain the product.
The diamond micropowder prepared in this example and conventional diamond micropowder of the same quality were placed in a MODEL 920 polishing machine to carry out silicon carbide wafer polishing experiments, the rotation speed of a polishing disk was 80r/min, the polishing pressure was 6.35kPa, the polishing time was 20min, and the polishing efficiency was as shown in Table 3:
table 3.
As can be seen from the data in Table 3, the removal rate of the diamond micro powder prepared in this example is about 2 times that of the conventional diamond micro powder, and the wafer roughness value Ra after grinding is about 26% of that of the conventional diamond particles, so that the grinding and polishing efficiency and accuracy of the silicon carbide wafer can be remarkably improved.
Comparative example 1
The preparation method of diamond micro powder for precision machining in comparative example 1 is basically the same as that in example 1, except that no artificial introduction of oxygen is performed during the calcination in step (3);
the diamond micro powder prepared in comparative example 1 has fewer pits and cutting edges on the surface compared with the diamond micro powder prepared in example 1, the diamond micro powder prepared in comparative example 1 and the conventional diamond micro powder with the same quality as that of example 1 are placed in a MODEL 920 grinding polisher to carry out silicon carbide wafer grinding experiments, the rotating speed of a grinding disc is 80r/min, the grinding pressure is 6.35kPa, the grinding time is 20min, and the recorded grinding and polishing efficiencies are shown in Table 4:
table 4.
As can be seen from the data in table 4, the removal rate of diamond micropowder and the wafer roughness value Ra after grinding of comparative example 1 were 1.23 times and 84.3 times as high as those of conventional diamond micropowder, and 59% and 3.4 times as high as those of the diamond micropowder of example 1. Compared with example 1, the removal rate of the diamond micropowder ground wafer obtained in comparative example 1 without manual oxygen ventilation operation is remarkably reduced, the roughness of the wafer is remarkably increased, and the grinding and polishing efficiency and precision improvement effect on the wafer are not obvious compared with the conventional diamond micropowder. Therefore, the process of adding artificial oxygen introduction in the preparation method is very important for improving the grinding and polishing efficiency of the diamond micro powder.
Finally, it is to be understood that the foregoing embodiments are merely preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any simple changes or equivalent alternatives of the technical solutions that may be obvious to those skilled in the art within the scope of the present invention are within the scope of the present invention.

Claims (7)

1. The preparation method of the diamond micro powder for precision machining is characterized in that the traditional diamond micro powder is added with additives and then is subjected to granulation, roasting and post-treatment; the method specifically comprises the following steps:
(1) Mixing: weighing diamond micropowder raw materials, iron powder raw materials and graphite powder raw materials according to mass percent, putting the raw materials into an omnibearing planetary ball mill, uniformly mixing, wherein the rotation speed of a mixing tank is 100-200 rpm, the revolution speed is 50-100rpm, and the overturning speed of a carrying disc for carrying the mixing tank is 1.5rpm;
(2) Granulating: adding an organic solvent and a binder into the mixed materials, and granulating by a granulator;
(3) Roasting: placing the granulated material into a tube furnace, heating to 300-350 ℃, and preserving heat for 1-2h; then vacuuming to 1.0X10 -3 ~9.0×10 -3 Pa, heating to 500-650 ℃, and preserving heat for 1-2h; then heating to 800-900 ℃, preserving heat for 2-5 h, introducing oxygen for 1-3 times during the period, keeping the pressure in the furnace to normal pressure each time, maintaining for 10-20 minutes, and vacuumizing to 10Pa; cooling to room temperature after the whole heat preservation is finished;
(4) Post-treatment: acid washing and drying the roasted material to obtain diamond micro powder for precision machining;
the weight percentages of the raw materials in the step (1) are 60-85% of diamond micropowder raw materials, 5-30% of iron powder raw materials and 5-20% of graphite powder raw materials.
2. The method for preparing diamond micro powder for precision machining according to claim 1, wherein in the step (1), the various raw materials are put into an omnibearing planetary ball mill to be uniformly mixed, specifically, firstly, iron powder raw materials and graphite powder raw materials are put into a stainless steel mixing tank, ball milling is carried out on the omnibearing planetary ball mill for 2-3 hours, and then, the diamond micro powder raw materials and a stainless steel spring are added as mixing media to carry out ball milling for 4-8 hours.
3. The method for preparing diamond micro powder for precision machining according to claim 2, wherein the diameter of the stainless steel spring is 10mm.
4. The method for producing diamond micro powder for precision machining according to claim 2, wherein the mass ratio of the diamond micro powder to the stainless steel spring is 1:3 to 1:1.
5. The method of producing diamond micro powder for precision machining according to claim 1, wherein the organic solvent in the step (2) is isopropyl alcohol or acetone.
6. The method of producing diamond micro powder for precision machining according to claim 1, wherein the binder in the step (2) is WS-120 or GB-600.
7. The method for producing diamond fine powder for precision machining according to claim 1, wherein the tubular furnace in step (3) is provided with a rotating device at a rotational speed of 1 to 60rpm.
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