CN116282003A - Preparation method of diamond powder for grinding and polishing superhard semiconductor substrate material - Google Patents

Preparation method of diamond powder for grinding and polishing superhard semiconductor substrate material Download PDF

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CN116282003A
CN116282003A CN202211466095.7A CN202211466095A CN116282003A CN 116282003 A CN116282003 A CN 116282003A CN 202211466095 A CN202211466095 A CN 202211466095A CN 116282003 A CN116282003 A CN 116282003A
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diamond
diamond powder
mixture
grinding
steps
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詹军
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Nanjing Fukexun New Material Co ltd
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Nanjing Fukexun New Material 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
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
    • C25B1/135Carbon

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Abstract

The invention discloses a preparation method of diamond powder for grinding and polishing a superhard semiconductor substrate material, and relates to the technical field of diamond powder preparation. The preparation method of diamond powder for grinding and polishing super-hard semiconductor substrate material comprises the steps of preprocessing primary diamond to obtain purified diamond particles, mixing the diamond particles with a ball mixture, performing ball milling treatment to obtain a mixture, purifying the mixture to obtain diamond powder, and performing organic treatment on the diamond powder to obtain modified diamond powder. The modified diamond powder is obtained by carrying out organic treatment on the diamond powder, more organic groups are introduced in the preparation process, and the lipophilicity of the diamond powder is increased, so that the diamond powder can be stabilized in suspension in the polishing solution and can not be agglomerated, the quality of the polishing solution can be ensured, the grinding and polishing quality can be improved, and the surface of the superhard semiconductor substrate material after grinding and polishing is smoother.

Description

Preparation method of diamond powder for grinding and polishing superhard semiconductor substrate material
Technical Field
The invention relates to the technical field of diamond powder preparation, in particular to a preparation method of diamond powder for grinding and polishing of superhard semiconductor substrate materials.
Background
Diamond powder, namely diamond powder, is a novel ultra-hard superfine abrasive formed by processing artificial diamond monocrystal through special process, is an ideal raw material for grinding and polishing hard alloy, ceramics, precious stone, optical glass and other high-hardness materials, and diamond products are tools and components manufactured by processing diamond materials, so that the diamond product has wide application, and in the field of semiconductors, polishing solution containing diamond powder is often used for grinding and polishing semiconductor substrates, and smooth and flat surfaces at grinding positions are favorable for obtaining semiconductor substrates with low roughness.
In the using process of the diamond powder polishing solution, the polishing solution is required to be uniform and stable in quality, but in the prior art, the diamond powder in the polishing solution is uneven in dispersion and poor in suspension, so that the problem of low polishing quality of a semiconductor substrate is caused.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of diamond powder for grinding and polishing a superhard semiconductor substrate material, which solves the problems of uneven dispersion and poor suspension property of diamond powder in polishing solution in the prior art, and causes the problem of low polishing quality of a semiconductor substrate.
Technical proposal
In order to achieve the above purpose, the invention is realized by the following technical scheme: the preparation method of diamond powder for grinding and polishing superhard semiconductor substrate material comprises the following steps:
s1, carrying out electrolytic treatment on a diamond rod to prepare primary diamond;
s2, preprocessing the primary diamond to obtain purified diamond particles;
s3, mixing diamond particles with the ball mixture, and performing ball milling treatment to obtain a mixture;
s4, purifying the mixture to obtain diamond powder;
s5, carrying out organic treatment on the diamond powder to obtain the modified diamond powder.
Further, the step S1 includes the steps of:
s11, crushing the diamond rod;
s12, placing the broken diamond rod into an acid electrolyte for electrolytic treatment to obtain the primary diamond.
Further, the pretreatment of the primary diamond in S2 specifically includes the following steps:
s21, grinding the primary diamond through a grinder, sieving the ground primary diamond, and grinding the primary diamond without sieving again;
s22, carrying out acid leaching treatment on the screened primary diamond, wherein the acid leaching time is 8-9 hours;
s23, performing heat treatment on the diamond subjected to acid leaching, and removing graphite and pyrophyllite in the primary diamond through screening and purifying to obtain purified diamond particles.
Further, the specific steps of preparing the mixture in S3 include:
s31, mixing the ball mixture with diamond particles, putting the mixed diamond particles and ball mixture into a ball mill, and simultaneously adding oxides into the ball mill tank;
s32, electrifying the ball milling tank, and crushing and shaping diamond particles in the ball milling tank through the ball mixture to obtain a mixture, wherein the crushing time is 1.5-2.5 hours.
Further, the ball mixture includes iron balls, zirconium dioxide balls, and tungsten steel balls.
Further, the step of preparing diamond powder in S4 includes:
s41, drying the mixture at a low temperature through a belt dryer, and placing the dried mixture into a stirrer for stirring;
s42, taking out the mixture from the stirrer, loading the mixture into a high-temperature sintering furnace, and carrying out high-temperature sintering on the mixture;
s43, after the mixture is cooled, purifying, and separating the mixture of balls from the diamond powder.
Further, the sintering furnace is a push rod type sintering furnace, the sintering temperature is 700-900 ℃, and nitrogen is used as a protective gas.
Further, the specific step of preparing the modified diamond powder in S5 comprises the following steps:
s51, immersing diamond powder in a strong acid or alkali solution, centrifuging, adjusting the diamond powder to be neutral by using a cleaning solution, and drying at a low temperature in a vacuum environment;
s52, placing the dried diamond powder into a preparation solution, stirring and heating, centrifuging, adjusting the diamond powder to be neutral by using a cleaning solution, and drying at a low temperature in a vacuum environment to obtain the modified diamond powder.
Further, the cleaning solution is a mixture of deionized water and absolute ethanol.
Further, the preparation process of the preparation solution comprises the following steps: 3-5 parts by mass of p-toluenesulfonamide is dissolved in 12-17 parts by mass of absolute ethanol and stirred until complete dissolution.
Advantageous effects
The invention has the following beneficial effects:
(1) According to the preparation method of diamond powder for grinding and polishing the superhard semiconductor substrate material, after the ball mixture is mixed with the diamond particles, the ball mixture is subjected to ball milling treatment, so that cracks can be formed on the surfaces of the diamond particles under the condition of a certain time, iron balls are contained in the ball mixture, and iron filings generated by collision can infiltrate into the cracks, so that more cutting edges can be generated on the surfaces and the inside of the diamond particles, and the grinding time of the diamond particles can be longer.
(2) According to the preparation method of diamond powder for grinding and polishing the superhard semiconductor substrate material, the diamond powder is subjected to organic treatment to obtain modified diamond powder, more organic groups are introduced in the preparation process, and the lipophilicity of the diamond powder is increased, so that the diamond powder can be stably suspended in polishing liquid and cannot be aggregated in solution, the quality of the polishing liquid can be ensured, the grinding and polishing quality can be improved, and the surface of the superhard semiconductor substrate material after grinding and polishing is smoother.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Drawings
FIG. 1 is a flow chart of the preparation method of the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be understood that the terms "open," "upper," "lower," "thickness," "top," "middle," "length," "inner," "peripheral," and the like indicate orientation or positional relationships, merely for convenience in describing the present invention and to simplify the description, and do not indicate or imply that the components or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
Referring to fig. 1, the embodiment of the invention provides a technical scheme: the preparation method of diamond powder for grinding and polishing superhard semiconductor substrate material comprises the following steps:
s1, carrying out electrolytic treatment on a diamond rod to prepare primary diamond;
s2, preprocessing the primary diamond to obtain purified diamond particles;
s3, mixing diamond particles with the ball mixture, and performing ball milling treatment to obtain a mixture;
s4, purifying the mixture to obtain diamond powder;
s5, carrying out organic treatment on the diamond powder to obtain the modified diamond powder.
Specifically, the step S1 includes the steps of:
s11, crushing the diamond rod;
s12, placing the broken diamond rod into an acid electrolyte for electrolytic treatment to obtain the primary diamond.
In this embodiment, the diamond rod is first crushed to become proper crushed grains, and the crushed grains are then set inside electrolyte with acid electrolyte for electrolysis treatment to obtain diamond.
Specifically, the pretreatment of the primary diamond in S2 specifically includes the following steps:
s21, grinding the primary diamond through a grinder, sieving the ground primary diamond, and grinding the primary diamond without sieving again;
s22, carrying out acid leaching treatment on the screened primary diamond, wherein the acid leaching time is 8-9 hours;
s23, performing heat treatment on the diamond subjected to acid leaching, and removing graphite and pyrophyllite in the primary diamond through screening and purifying to obtain purified diamond particles.
In this embodiment, diamond particles after electrolysis are placed in the grinder to grind, so that diamond particles are smaller, the ground diamond is screened by the screen, the diamond which is not screened needs to be ground again, the utilization rate is improved, diamond particles conforming to the size can be soaked in an acid solution for 8-9 hours, after acid leaching is finished, heat treatment is further carried out, moisture is volatilized, and then impurities such as graphite, pyrophyllite and the like are removed in a screening and purifying mode, so that diamond particles with high purity can be obtained, diamond powder is convenient to prepare, and the purity of polishing liquid is improved.
Specifically, the specific steps of preparing the mixture in S3 include:
s31, mixing the ball mixture with diamond particles, putting the mixed diamond particles and ball mixture into a ball mill, and simultaneously adding oxides into the ball mill tank;
s32, electrifying the ball milling tank, and crushing and shaping diamond particles in the ball milling tank through the ball mixture to obtain a mixture, wherein the crushing time is 1.5-2.5 hours;
the ball mixture comprises iron balls, zirconium dioxide balls and tungsten steel balls.
In this embodiment, the iron balls, zirconium dioxide balls and tungsten steel balls are mixed to form a ball mixture, the ball mixture is mixed with diamond particles, and then the mixture is added into a ball milling tank, and the ball milling tank is operated for 1.5-2.5 hours, so that the diamond particles are crushed and shaped, and the mixture is obtained.
Specifically, the step of preparing diamond powder in S4 includes:
s41, drying the mixture at a low temperature through a belt dryer, and placing the dried mixture into a stirrer for stirring;
s42, taking out the mixture from the stirrer, loading the mixture into a high-temperature sintering furnace, and carrying out high-temperature sintering on the mixture;
s43, after the mixture is cooled, purifying, and separating the mixture of balls from the diamond powder;
the sintering furnace is a push rod type sintering furnace, the sintering temperature is 700-900 ℃, and nitrogen is used as a shielding gas.
In the embodiment, the mixture obtained by ball milling tank treatment is dried at low temperature under the condition of urgent belt drying, the dried mixture is transported into a stirrer, the mixture is stirred to prevent dry agglomeration, the stirred mixture is placed into a high-temperature sintering furnace, nitrogen is used as protective gas for sintering the mixture, nitrogen is inert gas for preventing oxidation, the mixture is treated at a high temperature of 700-900 ℃, and after cooling, purification and separation are carried out to separate the spherical mixture from diamond powder;
based on the scheme, under the condition of controlling the collision time, the diamond particles can be slightly crushed, so that scrap iron generated in the collision process can infiltrate into cracks of the diamond particles, meanwhile, under the action of an oxidant, the iron shoe is converted into oxide, so that the oxide is tightly attached to the diamond particles, a polishing layer is formed on the surface of diamond, in the process of grinding and polishing the superhard semiconductor substrate material, even if the outer polishing layer is separated, the inner cutting edge can be used for continuously polishing, and the polishing solution can be used for a longer time.
Specifically, the specific step of preparing modified diamond powder in S5 includes:
s51, immersing diamond powder in a strong acid or alkali solution, centrifuging, adjusting the diamond powder to be neutral by using a cleaning solution, and drying at a low temperature in a vacuum environment;
s52, placing the dried diamond powder into a preparation solution, stirring and heating, centrifuging, adjusting the diamond powder to be neutral by using a cleaning solution, and drying at a low temperature in a vacuum environment to obtain modified diamond powder;
the cleaning solution is a mixture of deionized water and absolute ethanol.
The preparation process of the prepared solution comprises the following steps: 3-5 parts by mass of p-toluenesulfonamide is dissolved in 12-17 parts by mass of absolute ethanol and stirred until complete dissolution.
In the embodiment, diamond powder is soaked in strong acid or alkali solution for 3-5 hours, the centrifuged diamond powder is neutralized by using a cleaning solution, and is dried at low temperature in a vacuum environment after neutralization, wherein the cleaning solution is a mixture of deionized water and absolute ethyl alcohol, the diamond powder after the first vacuum drying is mixed with a preparation solution, the preparation solution is a mixture of 3-5 parts by mass of p-toluenesulfonamide and 12-17 parts by mass of absolute ethyl alcohol, the mixture is heated and stirred for 2-3 hours, and after centrifugation, the mixture is cleaned and neutralized by using the cleaning solution, and is subjected to secondary vacuum drying, so that modified diamond powder is finally obtained;
in the process of preparing the modified diamond powder, more organic groups are introduced, so that the lipophilicity of the diamond powder is increased, the diamond powder is easier to be worth of polishing liquid, the dispersibility of the diamond powder in oily solution is also enhanced, the diamond powder can be more stably declared in the polishing liquid, the high dispersion state can be kept for a long time, the agglomeration is prevented, the polishing quality can be improved, the surface of the superhard semiconductor substrate material is smoother, and the quality is improved.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.

Claims (10)

1. A preparation method of diamond powder for grinding and polishing superhard semiconductor substrate material is characterized by comprising the following steps: the method comprises the following steps:
s1, carrying out electrolytic treatment on a diamond rod to prepare primary diamond;
s2, preprocessing the primary diamond to obtain purified diamond particles;
s3, mixing diamond particles with the ball mixture, and performing ball milling treatment to obtain a mixture;
s4, purifying the mixture to obtain diamond powder;
s5, carrying out organic treatment on the diamond powder to obtain the modified diamond powder.
2. The method for preparing diamond powder for grinding and polishing superhard semiconductor substrate material according to claim 1, wherein the method comprises the following steps: the S1 comprises the following steps:
s11, crushing the diamond rod;
s12, placing the broken diamond rod into an acid electrolyte for electrolytic treatment to obtain the primary diamond.
3. The method for preparing diamond powder for grinding and polishing superhard semiconductor substrate material according to claim 1, wherein the method comprises the following steps: the pretreatment of the primary diamond in the step S2 specifically comprises the following steps:
s21, grinding the primary diamond through a grinder, sieving the ground primary diamond, and grinding the primary diamond without sieving again;
s22, carrying out acid leaching treatment on the screened primary diamond, wherein the acid leaching time is 8-9 hours;
s23, performing heat treatment on the diamond subjected to acid leaching, and removing graphite and pyrophyllite in the primary diamond through screening and purifying to obtain purified diamond particles.
4. The method for preparing diamond powder for grinding and polishing superhard semiconductor substrate material according to claim 1, wherein the method comprises the following steps: the specific steps for preparing the mixture by S3 comprise:
s31, mixing the ball mixture with diamond particles, putting the mixed diamond particles and ball mixture into a ball mill, and simultaneously adding oxides into the ball mill tank;
s32, electrifying the ball milling tank, and crushing and shaping diamond particles in the ball milling tank through the ball mixture to obtain a mixture, wherein the crushing time is 1.5-2.5 hours.
5. The method for preparing diamond powder for grinding and polishing superhard semiconductor substrate material according to claim 4, wherein the method comprises the following steps: the ball mixture comprises iron balls, zirconium dioxide balls and tungsten steel balls.
6. The method for preparing diamond powder for grinding and polishing superhard semiconductor substrate material according to claim 1, wherein the method comprises the following steps: the step of preparing diamond powder in the step S4 comprises the following steps:
s41, drying the mixture at a low temperature through a belt dryer, and placing the dried mixture into a stirrer for stirring;
s42, taking out the mixture from the stirrer, loading the mixture into a high-temperature sintering furnace, and carrying out high-temperature sintering on the mixture;
s43, after the mixture is cooled, purifying, and separating the mixture of balls from the diamond powder.
7. The method for preparing diamond powder for grinding and polishing superhard semiconductor substrate material according to claim 6, wherein the method comprises the following steps: the sintering furnace is a push rod type sintering furnace, the sintering temperature is 700-900 ℃, and nitrogen is used as a shielding gas.
8. The method for preparing diamond powder for grinding and polishing superhard semiconductor substrate material according to claim 1, wherein the method comprises the following steps: the specific step of preparing the modified diamond powder in S5 comprises the following steps:
s51, immersing diamond powder in a strong acid or alkali solution, centrifuging, adjusting the diamond powder to be neutral by using a cleaning solution, and drying at a low temperature in a vacuum environment;
s52, placing the dried diamond powder into a preparation solution, stirring and heating, centrifuging, adjusting the diamond powder to be neutral by using a cleaning solution, and drying at a low temperature in a vacuum environment to obtain the modified diamond powder.
9. The method for preparing diamond powder for grinding and polishing superhard semiconductor substrate material according to claim 8, wherein the method comprises the following steps: the cleaning solution is a mixture of deionized water and absolute ethanol.
10. The method for preparing diamond powder for grinding and polishing superhard semiconductor substrate material according to claim 8, wherein the method comprises the following steps: the preparation process of the prepared solution comprises the following steps: 3-5 parts by mass of p-toluenesulfonamide is dissolved in 12-17 parts by mass of absolute ethanol and stirred until complete dissolution.
CN202211466095.7A 2022-11-22 2022-11-22 Preparation method of diamond powder for grinding and polishing superhard semiconductor substrate material Withdrawn CN116282003A (en)

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CN202211466095.7A CN116282003A (en) 2022-11-22 2022-11-22 Preparation method of diamond powder for grinding and polishing superhard semiconductor substrate material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211466095.7A CN116282003A (en) 2022-11-22 2022-11-22 Preparation method of diamond powder for grinding and polishing superhard semiconductor substrate material

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CN116282003A true CN116282003A (en) 2023-06-23

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