CN113683962A - Preparation method of silicon dioxide grinding and polishing agent - Google Patents
Preparation method of silicon dioxide grinding and polishing agent Download PDFInfo
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- CN113683962A CN113683962A CN202111010321.6A CN202111010321A CN113683962A CN 113683962 A CN113683962 A CN 113683962A CN 202111010321 A CN202111010321 A CN 202111010321A CN 113683962 A CN113683962 A CN 113683962A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C09K3/1436—Composite particles, e.g. coated particles
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K3/1463—Aqueous liquid suspensions
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Abstract
A preparation method of a silicon dioxide grinding and polishing agent comprises a preparation step of an abrasive crystal seed, a preparation step of high-purity saturated silica sol liquid, a preparation step of an abrasive crystal nucleus with loose silicon dioxide crystal particles deposited, and a preparation step of an abrasive crystal nucleus mixed emulsion wrapped by the silica sol layer. Through the steps, the silicon dioxide grinding and polishing agent which has passivated edges and corners, has high-hardness abrasive crystal nuclei with loose silicon dioxide crystal particles on the surfaces and is wrapped by a silica sol layer can be prepared. The method determines the cutting capacity of the grinding polishing agent by selecting the abrasive material seed crystals of different specifications; silicon dioxide crystal particles with different cutting capacities can be obtained by adjusting the mass percentage concentration of silicon dioxide in the high-purity saturated silica sol solution and controlling the deposition crystallization conditions and time of the silicon dioxide; and silica sol layers with different thicknesses which are wrapped outside the abrasive crystal nucleus and used as lubricating and filling materials can be obtained by controlling the rehydration conditions and time of the silica crystal particles.
Description
Technical Field
The invention relates to a preparation method of a grinding polishing agent, in particular to a preparation method of a silicon dioxide grinding polishing agent, and belongs to the technical field of production and preparation of grinding and polishing materials.
Background
An abrasive polishing agent or so-called abrasive polishing solution is another type of "abrasive tool" different from a bonded abrasive tool or a coated abrasive tool, and is an "abrasive tool" formed by uniformly and freely distributing abrasives in a dispersing agent, and the abrasive polishing agent can be divided into an abrasive and a polishing agent, wherein the abrasive is generally used for rough grinding, the polishing agent is used for precise grinding, the polishing agent is generally used for the next process of the abrasive, and the polishing agent is also called as an abrasive or a polishing agent in the industry.
Because the components and the mixing proportion of the dispersing agent and the auxiliary material are different, the grinding polishing agent also has various different forms such as liquid, paste and solid.
Commonly used abrasives include corundum, silicon carbide, boron carbide and synthetic diamond as well as iron oxide, chromium oxide and cerium oxide, and the like; common dispersing agents include kerosene, engine oil, animal oil, glycerin, alcohol, water and the like, and the dispersing agents play roles in uniformly dispersing the grinding materials, diluting, lubricating, cooling and the like; the auxiliary materials comprise stearic acid, fatty acid, ethylene oxide, triethanolamine, paraffin, oleic acid, hexadecanol and the like, play roles of emulsification, lubrication and adsorption in the grinding and polishing process, and also play roles of promoting the surface of a workpiece to generate chemical change and generating an oxidation film or a vulcanization film which is easy to fall off so as to improve the processing efficiency; in addition, the auxiliary materials may also include coloring agent, antiseptic, aromatic, etc.
Silica particles are also a commonly used abrasive, and silica sol is a hydrated dispersion of nano-scale silica particles in water or a solvent, and since silica sol has high adhesion and high temperature resistance, and good wear resistance, polishing and filling properties, abrasive polishing agents composed of silica particles and silica sol are now widely used for planarization and polishing of surfaces of various materials, such as ultra-precision polishing and polishing of various chips in the electronic industry.
Examples of fine polishing in which an abrasive polishing agent consisting of silica particles and silica sol, or only silica sol, is applied to a variety of materials can be found in various patent applications, such as:
the invention patent application, namely a sapphire polishing solution and a preparation method thereof (application number: 201810235033.2), is used for polishing sapphire, the invention patent application, namely a CMP polishing composition suitable for gallium nitride materials (application number: 201610601993.7), can be applied to polishing gallium nitride, and the invention patent application, namely a polishing solution for quartz optical glass processing (application number: 201610783260.X), is applied to polishing ultrathin semiconductor wafers and the like.
Also, there are several patented technologies for preparing silica sol used in the field of fine polishing, for example:
the invention patent with application number 201410505702.5, namely a preparation method of silica sol, discloses a method for preparing silica sol by adopting fumed silica; the preparation of the silica sol is carried out by taking organosilane as a raw material in the invention patent preparation method of alkali-resistant ultra-pure silica sol with metal impurity content less than 1PPM (application number: 200710019366.3), the invention patent colloidal sol and a preparation method thereof (application number: 201480034350.8) and the invention patent silica sol and a preparation method thereof (application number: 200780027760. X); the invention relates to a water-soluble polymer coated special-shaped silica sol, a preparation method and application thereof (application number: 201611157145.8), which is prepared by a silica powder raw material alkalization process; the invention relates to a processing method of silica sol (application number: 201410505730). the silica sol is prepared by carrying out resin exchange on common silica sol and adding organic substances for modification.
It can be found from examination of the above patent documents that although the prior art has conducted corresponding studies on the application of silica sol to the field of ultra-precision grinding and polishing, and various methods are provided for the preparation of silica sol for ultra-precision grinding and polishing, there is only a limited research on how to improve the grinding and polishing efficiency and ensure the grinding and polishing quality in the process of using silica sol for grinding and polishing, however, as a grinding and polishing agent, the grinding and polishing efficiency and the grinding and polishing quality are two equally important problems, and both should be considered in practical application.
The grinding and polishing efficiency and the grinding and polishing quality are related to the hardness and the morphology of the abrasive particles of the grinding and polishing agent, the internal structure of the grinding and polishing agent and the like, and are directly related to the applicability and the practicability of the grinding and polishing agent.
Although, for example, in the invention patent "polydisperse large-particle-size silica sol and its preparation method" (application No. 201610382474.6) and the invention patent "preparation method of a silicon controlled sol having a particle size" (application No. 201610157738.8), it is proposed to increase the polishing efficiency by adding a seed crystal to the silica sol to increase the hardness or size of the silica sol particles, however, in these methods, the added seed crystal is usually monodisperse spherical silica sol seed crystal with the particle diameter of 20-30 nm, and the seed crystal particles are tiny and inevitably have the characteristics of sol, namely, the hydrated thin film layer formed on the surface of the particles is thicker, so that the final grinding polishing agent has low hardness, low grinding and polishing efficiency and poor effect, therefore, the grinding and polishing silica sol provided by the prior art cannot meet the requirement of ultra-precision grinding and polishing, and has become one of the bottlenecks affecting the use of silica sol as an ultra-precision grinding and polishing material.
Although the invention patent application 'production method of high-hardness silica sol for grinding and polishing' (application number: 202010837634.8) provides a high-hardness silica sol for grinding and polishing which can obtain the high-hardness silica sol for grinding and polishing with different grinding crystal grain sizes and different grinding crystal appearances by adding grinding material seed crystals with different grain sizes and different appearances, thereby satisfying the grinding and polishing requirements of different devices and different materials and improving the grinding and polishing efficiency, the preparation process is more complicated and has an improved place, and the product has the defects of more grinding crystal edges and corners and unsatisfactory grinding and polishing effect.
Disclosure of Invention
In order to overcome the defects in the prior art, the embodiment of the invention provides a preparation method of a silicon dioxide grinding polishing agent, aiming at:
the method provided by the invention is used for preparing and producing the silicon dioxide grinding and polishing agent which has the passivated polygon corners and loose silicon dioxide crystal particles on the surface, is used for super-precision grinding and polishing of processing materials, improves the grinding and polishing efficiency, improves the grinding and polishing quality, meets the production requirements, simplifies the production flow of the grinding and polishing agent, improves the production efficiency, and obtains corresponding economic benefits while obtaining better social benefits.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing a silicon dioxide grinding and polishing agent comprises the following steps:
the preparation method comprises the steps of preparing abrasive crystal seeds, preparing high-purity saturated silica sol solution, preparing abrasive crystal nuclei with loose silica crystal particles deposited, and preparing an abrasive crystal nucleus mixed emulsion wrapped by the silica sol layer;
the preparation steps of the abrasive grain seed crystal comprise:
putting rod-shaped or irregular multi-edge abrasive powder into a high-frequency ultrasonic grinding device, adding water, carrying out wet ultrafine grinding, and washing and filtering to obtain abrasive seed crystal initial particles with required particle sizes;
placing the abrasive seed crystal initial particles in a high-pressure kettle, adding pure water, adding concentrated ammonia water serving as a catalyst, stirring and heating to ensure that the abrasive seed crystal initial particles are dissolved in the pure water dissolved with ammonium ions at the edges, realizing the shape reformation of the abrasive seed crystal initial particles, and obtaining a mixture of abrasive seed crystals with passivated surface edges and corners and an ammonia water solution;
washing, filtering and drying the mixture of the abrasive seed crystal and the ammonia water solution to obtain the abrasive seed crystal;
the preparation method of the high-purity saturated silica sol solution comprises the following steps:
adding high-purity simple substance silicon powder and pure water into a high-pressure kettle, adding concentrated ammonia water as a catalyst, heating and stirring to enable the high-purity simple substance silicon powder to react with water under the catalysis of the concentrated ammonia water to generate hydrated silicic acid, and continuing heating and stirring to enable the hydrated silicic acid to gradually polymerize under the alkaline water quality condition formed by the concentrated ammonia water to obtain alkaline silicon dioxide initial sol;
aging and removing ammonia from the initial silica sol to obtain neutral silica sol;
introducing a gas isolation lubricant into the neutral silica sol to dissolve gas into silica sol particles and among the particles in the neutral silica sol so as to reduce the polymerization force among the silica sol particles, and heating and concentrating to obtain a high-purity saturated silica sol solution;
the preparation steps of the abrasive material crystal nucleus deposited with the loose silicon dioxide crystal particles comprise:
adding a certain amount of the abrasive seed crystals into the high-purity saturated silica sol solution to form a seed crystal silica sol mixed solution, introducing the gas isolation lubricant into the seed crystal silica sol mixed solution to keep the mixed solution in a boiling state, heating and stirring the mixed solution, gradually concentrating the seed crystal silica sol mixed solution, and depositing part of silica sol particles in the seed crystal silica sol mixed solution on the abrasive seed crystals to form a loose silica crystal layer to obtain a crystal mixed solution;
aging the crystallization mixed solution, washing with water, filtering, removing water and concentrating to obtain an abrasive crystal nucleus deposited with loose silicon dioxide crystal particles;
the preparation method of the abrasive crystal nucleus mixed emulsion wrapped with the silica sol layer comprises the following steps:
mixing the abrasive crystal nucleus with pure water and concentrated ammonia water in a high-pressure kettle, heating and stirring to partially dissolve loose silicon dioxide crystal particles on the surface of the abrasive crystal nucleus to form silica sol, then decompressing and deaminating, adding a dispersing agent and a surfactant, stirring uniformly, and cooling to obtain the abrasive crystal nucleus mixed emulsion wrapped with the silica sol layer, namely the grinding and polishing agent.
Furthermore, the abrasive powder is any one or more of crystalline silica powder, crystal powder, remelted crystal powder and crystalline quartz powder, and the average particle size of the initial particles of the abrasive seed crystals is 0.5-5 microns.
Further, the gas isolation lubricant is one or more of olefin, alkane, alkaline gas and inert gas.
Further, the olefin is ethylene, the alkane is methane or propane, the alkaline gas is methylamine, and the inert gas is nitrogen or argon.
Further:
the concentrated ammonia water is ammonia water with the mass percentage concentration of ammonia of 25-28%;
the dispersing agent is one or more of sodium hexametaphosphate, sodium polyacrylate or sodium citrate, and the surfactant is an anionic surfactant or a nonionic surfactant.
Further, the dosage of the abrasive seed crystal is 0.5-15% of the total mass of the grinding and polishing agent.
Furthermore, the mass percentage concentration of silicon dioxide in the high-purity saturated silica sol solution is 10-50%, the purity of the silicon dioxide is more than 99.999%, and the average particle size of silica sol particles is 2-40 nm.
Further, in the step of preparing the abrasive seed crystal, the ultrasonic frequency of the high-frequency ultrasonic grinding device is 15-30 MHz.
Further, in the step of preparing the high-purity saturated silica sol solution and the step of preparing the abrasive crystal nucleus deposited with the loose silica crystal particles, the pressure of the introduced gas isolation lubricant is 1-4 MPa.
Further:
stirring speed of the stirring is 200-1000 r/min, and heating temperature of the heating is controlled to be 120-180 ℃;
in the preparation step of the abrasive seed crystal, the preparation step of the high-purity saturated silica sol solution and the preparation step of the abrasive crystal nucleus mixed emulsion wrapped by the silica sol layer, the working pressure of the high-pressure autoclave is kept between 2 and 6 MPa.
Compared with the prior art, the invention has the beneficial effects and remarkable progresses that:
1) the invention provides a preparation method of a silicon dioxide grinding and polishing agent, which comprises the steps of preparing abrasive crystal seeds, preparing high-purity saturated silica sol solution, preparing abrasive crystal nuclei deposited with loose silicon dioxide crystal particles, and preparing an abrasive crystal nucleus mixed emulsion wrapped with a silica sol layer, wherein the steps can be used for preparing the silicon dioxide grinding and polishing agent which has passivated polygon corners, has the high-hardness abrasive crystal nuclei with the loose silicon dioxide crystal particles on the surface and is wrapped with the silica sol layer on the abrasive crystal nuclei;
2) the silicon dioxide grinding and polishing agent prepared by the preparation method of the silicon dioxide grinding and polishing agent has the advantages that the grinding material crystal nucleus is provided with the high-hardness grinding material crystal seeds with passivated multi-edge angles, and the surface of the grinding material crystal seeds is provided with loose silicon dioxide crystal particles, so that the grinding and polishing agent for a workpiece can be efficiently finished at different levels by using the high-hardness grinding material crystal seeds and the loose silicon dioxide crystal particles with softer hardness, compared with the grinding and polishing agent consisting of silica sol particles or monodisperse spherical silica sol crystal seeds with the particle size of 20-30 nm, the grinding and polishing effect of the silicon dioxide grinding and polishing agent crystal seeds can be greatly improved, and the grinding material crystal seeds are passivated at the edge angles, so that the silicon dioxide grinding and polishing agent has efficient grinding and polishing performance, is not easy to scratch the surface of the workpiece, influences the grinding and polishing quality of the workpiece, or influences further fine polishing, meanwhile, as the surface of the abrasive crystal nucleus is wrapped with the hydrated film layer formed by the silica sol, on one hand, the abrasive crystal nucleus in the grinding polishing agent can be effectively dispersed and ground, so that the abrasive crystal nucleus can efficiently and uniformly play a grinding and polishing role, and on the other hand, the lubricating property and the filling property of the sol can be utilized to make up for the damage caused by rigid friction formed when high-hardness abrasive crystal seeds and loose silica crystal particles with softer hardness grind and polish a workpiece, so that the grinding and polishing quality is improved, the requirements of special ultra-precision grinding and polishing are met, and the requirements of social related manufacturing industries are met;
3) the preparation method of the silicon dioxide grinding and polishing agent provided by the invention creatively adopts a series of combined preparation processes, which comprises the steps of passivating the edges and corners of abrasive seed crystals under an alkaline condition, forming silicon dioxide crystal particles with hardness lower than that of the abrasive seed crystals by depositing high-purity saturated silica sol solution on the abrasive seed crystals, and forming a silica sol layer on the prepared abrasive crystal nuclei with loose silicon dioxide crystal particles deposited by hydrating under the alkaline condition, so that the grinding and polishing agent with a multiple structure and multiple abrasive hardness combined into a whole is formed, and the production requirements can be met on the basis of meeting the requirements of high-efficiency grinding and polishing and ensuring the grinding and polishing quality;
4) the silicon dioxide grinding polishing agent prepared by the preparation method of the silicon dioxide grinding polishing agent provided by the invention has the advantages of good dispersibility and stability, difficulty in coagulation, easiness in storage and capability of obtaining excellent use effect;
5) the preparation method of the silicon dioxide grinding polishing agent provided by the invention has the advantages of unique and stable process, strong operability, no pollution to the environment in the production process, energy conservation and environmental protection, provides positive social benefits, and can obtain better economic benefits for enterprises, thereby having great popularization and application values.
Drawings
To more clearly illustrate the technical solution of the present invention, the drawings required for the embodiment of the present invention will be briefly described below.
Obviously:
the drawings in the following description are only part of the embodiments of the present invention, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without creative efforts, but the other drawings also belong to the drawings required to be used by the embodiments of the present invention.
FIG. 1 is a Scanning Electron Microscope (SEM) electron micrograph of abrasive particles of a silicon dioxide abrasive polishing agent provided by an embodiment of the invention;
fig. 2 is a schematic structural view of an abrasive crystal nucleus wrapped with a silica sol layer of a silicon dioxide polishing agent according to an embodiment of the present invention.
In the figure:
10-abrasive seed crystal, 20-silicon dioxide crystal particle and 30-silica sol layer.
Detailed Description
In order to make the objects, technical solutions, advantages and significant progress of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings provided in the embodiments of the present invention, and it is obvious that all of the described embodiments are only some embodiments of the present invention, but not all embodiments;
all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that:
the terms "first," "second," and the like in the description and claims of the present invention and in the drawings of embodiments of the present invention, are used for distinguishing between different objects and not for describing a particular order;
furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not limited to the listed steps or elements, but may alternatively include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
It is to be understood that:
in the description of the embodiments of the present invention, some basic operation terms commonly used in the art, for example, "heating", "stirring", "mixing", "dissolving", "washing", "filtering", and "drying", etc., are used, and it should be understood that these terms are used in a broad sense, and may be performed by various conventional apparatuses and instruments in the art, or may be performed by the latest apparatuses, such as program control operation, unmanned automatic operation, etc., unless otherwise specifically limited, and those skilled in the art can understand the specific meaning of the above terms in the present invention according to specific situations and use specific operation methods to achieve the operation purpose.
It should also be noted that:
the following embodiments may be combined with each other, and the same or similar concepts or processes may not be described in detail in some embodiments;
further, the raw materials, equipment and facilities mentioned in the following specific examples are commercially available.
The technical means of the present invention will be described in detail below with specific examples.
Examples
The preparation method of the silicon dioxide polishing agent provided in this embodiment specifically includes:
the method comprises the following steps of preparing abrasive crystal seeds, preparing high-purity saturated silica sol solution, preparing abrasive crystal nuclei deposited with loose silica crystal particles, and preparing an abrasive crystal nucleus mixed emulsion wrapped with a silica sol layer, wherein:
the preparation method of the abrasive grain seed comprises the following steps:
putting rod-shaped or irregular multi-edge abrasive powder into a high-frequency ultrasonic grinding device, adding water, carrying out wet ultrafine grinding, and washing and filtering to obtain abrasive seed crystal initial particles with required particle sizes;
placing the initial abrasive seed crystal particles in a high-pressure kettle, adding pure water, adding concentrated ammonia water serving as a catalyst, stirring and heating to ensure that the initial abrasive seed crystal particles are dissolved in the pure water dissolved with ammonium ions at the edges, realizing the shape reformation of the initial abrasive seed crystal particles, and obtaining a mixture of the abrasive seed crystals with passivated surface edges and corners and an ammonia water solution;
washing, filtering and drying a mixture of the abrasive seed crystal and an ammonia water solution to obtain the abrasive seed crystal;
the preparation method of the high-purity saturated silica sol solution comprises the following steps:
adding high-purity simple substance silicon powder and pure water into a high-pressure kettle, adding concentrated ammonia water as a catalyst, heating and stirring to enable the high-purity simple substance silicon powder to react with water under the catalysis of the concentrated ammonia water to generate hydrated silicic acid, and continuing heating and stirring to enable the hydrated silicic acid to gradually polymerize under the alkaline water quality condition formed by the concentrated ammonia water to obtain alkaline silicon dioxide initial sol;
aging and removing ammonia from the initial silica sol to obtain neutral silica sol;
introducing a gas isolation lubricant into the neutral silica sol to dissolve gas into silica sol particles and among the particles in the neutral silica sol so as to reduce the polymerization force among the silica sol particles, and heating and concentrating to obtain a high-purity saturated silica sol solution;
the preparation of abrasive nuclei on which the crystalline particles of loose silica are deposited comprises the following steps:
adding a certain amount of abrasive seed crystals into high-purity saturated silica sol liquid to form seed crystal silica sol mixed liquid, introducing a gas isolation lubricant into the seed crystal silica sol mixed liquid to keep the mixed liquid in a boiling state, heating and stirring, gradually concentrating the seed crystal silica sol mixed liquid, and depositing part of silica sol particles in the seed crystal silica sol mixed liquid on the abrasive seed crystals to form a loose silica crystal layer to obtain crystal mixed liquid;
aging the crystallization mixed solution, washing with water, filtering, removing water and concentrating to obtain an abrasive crystal nucleus deposited with loose silicon dioxide crystal particles;
the preparation method of the abrasive crystal nucleus mixed emulsion wrapped with the silica sol layer comprises the following steps:
mixing the abrasive crystal nucleus with pure water and concentrated ammonia water in a high-pressure kettle, heating and stirring to partially dissolve loose silicon dioxide crystal particles on the surface of the abrasive crystal nucleus to form silica sol, then decompressing and deaminating, adding a dispersing agent and a surfactant, stirring uniformly, and cooling to obtain the abrasive crystal nucleus mixed emulsion wrapped with the silica sol layer, namely the grinding and polishing agent.
In this embodiment:
the abrasive powder can be any one or more of crystalline silicon dioxide powder, crystal powder, remelted crystal powder and crystalline quartz powder;
the average particle size of the abrasive seed crystal initial particles can be selected within the range of 0.5-5 microns according to the requirements of grinding and polishing, wherein the silicon dioxide grinding and polishing agent prepared from the large-particle abrasive seed crystal initial particles is suitable for carrying out high-efficiency grinding operation on a workpiece, and the silicon dioxide grinding and polishing agent prepared from the small-particle abrasive seed crystal initial particles is suitable for carrying out fine polishing operation on the workpiece.
Furthermore, in the present embodiment:
the gas isolation lubricant is one or more of olefin, alkane, alkaline gas and inert gas, specifically, the olefin can adopt ethylene, the alkane can adopt methane or propane, the alkaline gas can adopt methylamine, and the inert gas can adopt nitrogen or argon;
the concentrated ammonia water is ammonia water with the mass percent concentration of 25-28% of ammonia;
the dispersant is one or more of sodium hexametaphosphate, sodium polyacrylate or sodium citrate;
the surfactant may be an anionic surfactant or a nonionic surfactant.
In addition, in the present embodiment:
the dosage of the abrasive seed crystal can be selected from 0.5-15% of the total mass of the grinding and polishing agent; wherein:
the consumption of the abrasive seed crystal is large, and the prepared silicon dioxide grinding polishing agent has high hardness and strong cutting force, is suitable for cutting and grinding the surface of a workpiece, and has the characteristics of quick cutting and high efficiency;
the dosage of the abrasive seed crystal is small, and the prepared silicon dioxide grinding polishing agent has low hardness, weak cutting force and good polishing effect, and is suitable for fine polishing processing of the surface of a workpiece.
Meanwhile, in the embodiment, the mass percentage concentration of the silicon dioxide in the high-purity saturated silica sol solution should be controlled within the range of 10-50%, the purity of the silicon dioxide should be greater than 99.999%, and the average particle size of the silica sol particles is controlled within the range of 2-40 nm, so that the sufficient concentration and purity of the silica sol particles are ensured, a loose silica crystal layer can be effectively crystallized and deposited on the abrasive seed crystal within a certain time, and the uniform size, ordered stacking and proper hardness of the crystal particles of the silica crystal layer are ensured, thereby generating better cutting and polishing capabilities.
Furthermore, in the present embodiment:
when the abrasive crystal seeds are prepared, the ultrasonic frequency of the high-frequency ultrasonic grinding device is controlled within the range of 15-30 MHz, so that a better grinding effect is obtained;
in the preparation of the high-purity saturated silica sol solution and the preparation process of the abrasive crystal nucleus deposited with loose silica crystal particles, the pressure of the introduced gas isolation lubricant is controlled to be 1-4 MPa, so that the gas isolation lubricant can be fully dissolved into the mixture liquid undergoing hydration or crystallization to play the isolation and lubrication functions of the gas isolation lubricant, the agglomeration and large-scale aggregation of the silica sol particles are prevented, the silica sol particles are uniformly dispersed, and the high-purity saturated silica sol solution which is uniformly and stably dispersed or the silica crystal particle layer which is uniformly distributed and has basically consistent deposition thickness is obtained.
In addition, in the present embodiment:
the stirring speed can be controlled between 200 and 1000 revolutions per minute according to the specific conditions in each preparation step, and the heating temperature is controlled between 120 and 180 ℃;
in the preparation step of the abrasive seed crystal, the preparation step of the high-purity saturated silica sol solution and the preparation step of the abrasive crystal nucleus mixed emulsion wrapped with the silica sol layer, the working pressure of the autoclave is kept between 2 and 6 MPa.
From the above description, it can be seen that:
firstly, the preparation method of the silica grinding and polishing agent provided by the embodiment includes a preparation step of an abrasive seed crystal, a preparation step of a high-purity saturated silica sol solution, a preparation step of an abrasive crystal nucleus on which loose silica crystal particles are deposited, and a preparation step of an abrasive crystal nucleus mixed emulsion coated with a silica sol layer, and through these steps, the silica grinding and polishing agent which has a passivated polygonal corner, has a high-hardness abrasive crystal nucleus with the loose silica crystal particles on the surface thereof, and is coated with the silica sol layer on the abrasive crystal nucleus can be prepared;
secondly, the silicon dioxide grinding and polishing agent prepared by the preparation method of the silicon dioxide grinding and polishing agent provided by the embodiment has the advantages that the grinding material crystal nucleus is provided with the high-hardness grinding material crystal seeds with passivated multi-edge angles, and the surface of the grinding material crystal seeds is provided with loose silicon dioxide crystal particles, so that the grinding and polishing agent for the workpiece can be efficiently finished at different levels by utilizing the high-hardness grinding material crystal seeds and the loose silicon dioxide crystal particles with softer hardness, compared with the grinding and polishing agent consisting of only silica sol particles or monodisperse spherical silicon dioxide sol crystal seeds with the particle size of 20-30 nm, the grinding and polishing effect can be greatly improved, and the grinding material crystal seeds are passivated at the edge angles, so that the grinding and polishing agent has efficient grinding and polishing performance, is not easy to scratch the surface of the workpiece, influences the grinding and polishing quality of the workpiece, or influences further fine polishing, meanwhile, as the surface of the abrasive crystal nucleus is wrapped with the hydrated film layer formed by the silica sol, on one hand, the abrasive crystal nucleus in the grinding polishing agent can be effectively dispersed and ground, so that the abrasive crystal nucleus can efficiently and uniformly play a grinding and polishing role, and on the other hand, the lubricating property and the filling property of the sol can be utilized to make up for the damage caused by rigid friction formed when high-hardness abrasive crystal seeds and loose silica crystal particles with softer hardness grind and polish a workpiece, so that the grinding and polishing quality is improved, the requirements of special ultra-precision grinding and polishing are met, and the requirements of social related manufacturing industries are met;
thirdly, the preparation method of the silicon dioxide grinding and polishing agent provided by the embodiment creatively adopts a series of combined preparation processes, including passivating the edges and corners of the abrasive seed crystal under an alkaline condition, forming silicon dioxide crystal particles with hardness lower than that of the abrasive seed crystal by depositing high-purity saturated silica sol solution on the abrasive seed crystal, and forming a silica sol layer on the prepared abrasive crystal nucleus with loose silicon dioxide crystal particles deposited thereon by hydration under the alkaline condition, so as to form the grinding and polishing agent with multiple structures and multiple abrasive hardness combinations, which can meet the production requirements on the basis of meeting the requirements of high-efficiency grinding and polishing and guaranteeing the grinding and polishing quality;
in addition, the silicon dioxide grinding polishing agent prepared by the preparation method of the silicon dioxide grinding polishing agent provided by the embodiment has good dispersibility and stability, is not easy to coagulate, is easy to store, and can obtain excellent use effect;
moreover, the preparation method of the silicon dioxide grinding polishing agent provided by the embodiment has the advantages of unique and stable process, strong operability, no pollution to the environment in the production process, energy conservation and environmental protection, provides positive social benefits, and can obtain better economic benefits for enterprises, thereby having great popularization and application values.
To further help understanding the technical solutions provided by the embodiments of the present invention, and the specific operation processes and effects obtained by the embodiments of the present invention, further description is made below by using specific examples.
Putting 100 g of rod-shaped crystalline silica powder into a high-frequency ultrasonic grinding device, adding 200 g of water to enable the crystalline silica powder to be pasty, then carrying out wet-process superfine grinding for 2 minutes, wherein the ultrasonic frequency of the high-frequency ultrasonic grinding device is set from low to high by adopting a gradient method, the lowest frequency is 150MHz, the highest frequency is 30MHz, and then, obtaining abrasive seed crystal initial particles with the average particle size of 5 micrometers through water washing and filtering;
putting 50 g of abrasive seed crystal initial particles into an autoclave, adding 150 g of pure water, adding 50 g of concentrated ammonia water with the mass percentage concentration of ammonia being 25% as a catalyst, stirring and heating, wherein the stirring speed and the heating temperature are set by adopting a gradient rising method, the stirring speed is set to be 200-1000 r/min, the heating temperature is controlled to be 120-180 ℃, the pressure in the autoclave is maintained to be 2-6 MPa, the abrasive seed crystal initial particles are dissolved in the pure water dissolved with ammonium ions, the shape reforming of the abrasive seed crystal initial particles is realized, a mixture of abrasive seed crystals with passivated surface edges and an ammonia water solution is obtained, and the mixture of the abrasive seed crystals and the ammonia water solution is washed, filtered and dried to obtain the abrasive seed crystals;
adding 10 g of high-purity elemental silicon powder and 150 g of pure water into an autoclave, adding 50 g of concentrated ammonia water with the mass percent concentration of ammonia being 25% as a catalyst, heating and stirring to enable the high-purity elemental silicon powder to react with water under the catalysis of the concentrated ammonia water to generate hydrated silicic acid, wherein the stirring speed and the heating temperature are set by adopting a gradient rising method, the stirring speed is set to be 200-1000 r/min, the heating temperature is controlled to be 120-180 ℃, and the pressure in the autoclave is maintained to be 2-6 MPa;
continuously heating and stirring to ensure that hydrated silicic acid is gradually polymerized under the alkaline water quality condition formed by strong ammonia water to obtain an alkaline silicon dioxide initial sol, wherein the stirring speed and the heating temperature are set by adopting a gradient reduction method, the stirring speed is finally maintained at 200 r/min, the heating temperature is maintained at 120 ℃, and the pressure in the high-pressure kettle is maintained between 2 and 6 MPa;
aging the initial silica sol for 8 hours, and then removing ammonia under reduced pressure to obtain neutral silica sol;
introducing a gas isolation lubricant formed by mixing 30% of ethylene and 70% of methylamine into neutral silica sol to dissolve gas in silica sol particles and among the particles in the neutral silica sol so as to reduce the polymerization force among the silica sol particles, and heating and concentrating to obtain a high-purity saturated silica sol solution with the silica mass percentage concentration of 50%, the silica purity of more than 99.999% and the average particle size of the silica sol particles of 20-40 nm;
adding 30 g of abrasive seed crystal into the high-purity saturated silica sol solution to form a seed crystal silica sol mixed solution, introducing a gas isolation lubricant consisting of 30% of ethylene and 70% of methylamine into the seed crystal silica sol mixed solution to keep the mixed solution in a boiling state, heating and stirring, gradually concentrating the seed crystal silica sol mixed solution, and depositing part of silica sol particles in the seed crystal silica sol mixed solution on the abrasive seed crystal to form a loose silica crystal layer to obtain a crystal mixed solution, wherein the stirring speed is kept at 200 revolutions per minute, the heating temperature is kept at 120 ℃, and the pressure in the autoclave is kept between 2 and 6 MPa;
aging the crystallization mixed solution for 8 hours, then washing with water, filtering, and then removing water and concentrating to obtain the abrasive material crystal nucleus deposited with loose silicon dioxide crystal particles;
mixing the abrasive crystal nucleus with 150 g of pure water and 50 g of 25% concentrated ammonia water in percentage by mass in an autoclave, heating and stirring to partially melt loose silica crystal particles on the surface of the abrasive crystal nucleus to form silica sol with the thickness of 40-80 nm, wherein the stirring speed and the heating temperature are set by adopting a gradient rising method, the stirring speed is set to be 200-1000 rpm, the heating temperature is controlled to be 120-180 ℃, and the pressure in the autoclave is maintained to be 2-6 MPa;
then, reducing pressure and removing ammonia, adding 0.1 g of sodium hexametaphosphate as a dispersing agent and 0.3 g of anionic polyacrylamide as a surfactant, uniformly stirring, and cooling to obtain an abrasive crystal nucleus mixed emulsion coated with a silica sol layer, namely a silicon dioxide grinding and polishing agent sample 1#。
The silicon dioxide grinding and polishing agent obtained in the case has larger abrasive seed crystal particles, thicker silicon dioxide sol particle crystallization deposition and thinner silicon sol layer, so the silicon dioxide grinding and polishing agent has higher hardness and better cutting force, is suitable for efficiently grinding workpieces, and can be mainly used as a grinding agent.
Case 2
The operation process and control conditions of this case are basically the same as those of case 1, except that the specifications and varieties of the raw materials are different, and the control conditions are slightly adjusted, and hereinafter, only the differences between this case and case 1 will be described, and the rest of the same operation process and control conditions will not be described again.
The abrasive powder used in the case is remelted crystal powder, the wet-process ultrafine grinding time is 3 minutes, and the average particle size of the obtained abrasive seed crystal initial particles is 3.5 microns;
the gas isolation lubricant adopts mixed gas which comprises 50 percent of ethylene gas, 25 percent of propane gas and 25 percent of nitrogen gas in volume percentage;
the mass percentage concentration of silicon dioxide in the obtained high-purity saturated silica sol solution is 40%, the purity of the silicon dioxide is more than 99.999%, and the average particle size of silica sol particles is 20-40 nm;
the thickness of silica sol formed on the surface of the abrasive crystal nucleus is 40-80 nm, the dispersing agent is 0.2 g of sodium polyacrylate, the surfactant is 0.3 g of anionic surfactant alkyl sulfonate, and the obtained silicon dioxide grinding and polishing agent is sample 2#。
The silicon dioxide grinding polishing agent obtained in the case still has larger abrasive seed crystal particles, thicker silicon dioxide sol particle crystallization deposition and thinner silicon sol layer, so that the hardness is higher, the cutting force is better, the silicon dioxide grinding polishing agent is suitable for efficiently grinding workpieces, and the silicon dioxide grinding polishing agent can be mainly used as an abrasive.
The operation process and control conditions of this case are basically the same as those of case 1, except that the specifications and varieties of the raw materials are different, and the control conditions are slightly adjusted, and hereinafter, only the differences between this case and case 1 will be described, and the rest of the same operation process and control conditions will not be described again.
The grinding material powder used in the method is crystal powder, the wet ultrafine grinding time is 4 minutes, and the average particle size of the obtained grinding material seed crystal initial particles is 1-2 microns;
the mass percent concentration of ammonia of the strong ammonia water used as the catalyst is 26 percent, and the gas isolation lubricant adopts mixed gas which comprises 20 percent of methane gas, 20 percent of methylamine gas, 40 percent of ethylene gas and 20 percent of propane gas in volume percent respectively;
the mass percentage concentration of silicon dioxide in the obtained high-purity saturated silica sol solution is 30%, the purity of the silicon dioxide is more than 99.999%, and the average particle size of silica sol particles is 40-110 nm;
the thickness of silica sol formed on the surface of the abrasive crystal nucleus is 100-200 nm, the dispersing agent is 0.2 g of sodium citrate, the surfactant is 0.1 g of anionic surfactant alkyl sulfonate and 0.1 g of nonionic surfactant fatty alcohol-polyoxyethylene ether, and the obtained silica grinding and polishing agent is sample 3#。
The silicon dioxide grinding and polishing agent obtained by the method has moderate abrasive seed crystal particle size, and moderate silicon dioxide sol particle crystallization deposition and thickness of a silicon sol layer, so that the cutting force is moderate, and the silicon dioxide grinding and polishing agent can be used for grinding and polishing workpieces.
The operation process and control conditions of this case are basically the same as those of case 1, except that the specifications and varieties of the raw materials are different, and the control conditions are slightly adjusted, and hereinafter, only the differences between this case and case 1 will be described, and the rest of the same operation process and control conditions will not be described again.
The grinding material powder used in the method is a mixture of crystal quartz powder and crystal powder, the wet-process ultrafine grinding time is 4 minutes, and the average particle size of the obtained grinding material seed crystal initial particles is 1-2 microns;
the gas isolation lubricant adopts mixed gas composed of 30% of methylamine gas, 30% of propane and 40% of nitrogen gas in volume percentage;
the mass percentage concentration of silicon dioxide in the obtained high-purity saturated silica sol solution is 20%, the purity of the silicon dioxide is more than 99.999%, and the average particle size of silica sol particles is 40-110 nm;
the thickness of silica sol formed on the surface of the abrasive crystal nucleus is 100-200 nm, the dispersing agents are 0.1 g of sodium hexametaphosphate and 0.1 g of sodium citrate, the surfactant is 0.3 g of nonionic surfactant alkylphenol polyoxyethylene ether, and the obtained silica grinding polishing agent is sample 4#。
The silicon dioxide grinding polishing agent obtained in the case has smaller particles of the grinding material crystal seeds, thinner silicon dioxide sol particle crystallization deposition and thicker silicon sol layer, so that the hardness is lower, the polishing performance is better, and the silicon dioxide grinding polishing agent is suitable for finely polishing workpieces and is mainly used as a polishing agent.
Case 5
The operation process and control conditions of this case are basically the same as those of case 1, except that the specifications and varieties of the raw materials are different, and the control conditions are slightly adjusted, and hereinafter, only the differences between this case and case 1 will be described, and the rest of the same operation process and control conditions will not be described again.
The grinding material powder used in the method is crystal quartz powder, the wet-process ultrafine grinding time is 5 minutes, and the average particle size of the obtained grinding material seed crystal initial particles is 0.5-1 micron;
the gas isolation lubricant adopts mixed gas which comprises 50 percent of methylamine gas and 50 percent of argon gas by volume percentage;
the mass percentage concentration of silicon dioxide in the obtained high-purity saturated silica sol solution is 10%, the purity of the silicon dioxide is more than 99.999%, and the average particle size of silica sol particles is 90-130 nm;
the thickness of silica sol formed on the surface of the abrasive crystal nucleus is 180-260 nm, the dispersing agents are 0.05 g of sodium hexametaphosphate, 0.0.5 g of sodium polyacrylate and 0.05 g of sodium citrate or 0.3 g of nonionic surfactant alkylolamide, and the obtained silicon dioxide grinding and polishing agent is sample 5#。
The silicon dioxide grinding and polishing agent obtained in the case has low hardness and better polishing performance due to the tiny particles of the grinding material crystal seeds, moderate crystallization and deposition of silicon dioxide sol particles and thicker silicon sol layer, and is suitable for finely polishing workpieces and mainly used as the polishing agent.
Effects of the embodiment
In order to further illustrate that the silicon dioxide grinding and polishing agent which is prepared by the preparation method of the silicon dioxide grinding and polishing agent provided by the embodiment of the invention and has the passivated polygonal corners and the high-hardness abrasive crystal nuclei with loose silicon dioxide crystal particles on the surfaces, and the abrasive crystal nuclei are wrapped by the silica sol layer to be used as the dispersant and the lubricant of the abrasive crystal nuclei, is used for ultra-precision grinding and polishing of processing materials, can improve the grinding and polishing efficiency and the grinding and polishing quality, and meets the production requirements, and the effects of the silicon dioxide grinding and polishing agent are explained through related tests and detections.
1. Product detection
Fig. 1 is a Scanning Electron Microscope (SEM) electron micrograph of abrasive particles of a silicon dioxide polishing slurry according to an embodiment of the present invention, and fig. 2 is a schematic structural view of abrasive nuclei coated with a silica sol layer of a silicon dioxide polishing slurry according to an embodiment of the present invention:
the silicon dioxide grinding and polishing agent prepared by the preparation method of the silicon dioxide grinding and polishing agent provided by the invention has the advantages that the abrasive particles have the abrasive seed crystal 10 with high hardness, the silicon dioxide crystal particles 20 with relatively small hardness and looseness are deposited on the surface of the abrasive seed crystal 10, the abrasive seed crystal 10 and the silicon dioxide crystal particles 20 form the abrasive crystal nucleus in the silicon dioxide grinding and polishing agent prepared by the preparation method of the silicon dioxide grinding and polishing agent provided by the invention, and the outer layer of the abrasive crystal nucleus is wrapped by the silica sol layer 30 which can be used as the self-dispersing agent and the lubricating agent of the abrasive crystal nucleus.
Table 1 shows the silicon dioxide polishing abrasives 1 prepared in examples 1 to 5#～5#The appearance characteristics of (a) and the characteristics of the abrasive seed crystal thereof; wherein:
the appearance of the sample was checked by visual inspection;
the average grain diameter of the abrasive seed crystal, the average grain size of the silica sol grain and the average thickness of the silica sol layer are obtained by scanning and calculating through a scanning electron microscope.
TABLE 1
As can be seen from table 1:
in the preparation method provided in this embodiment, first, the cutting ability of the prepared silica polishing slurry can be determined by selecting different specification types of abrasive seed crystals, because the cutting ability of the polishing slurry is mainly determined by the hardness of the abrasive seed crystals and the particle size of the abrasive seed crystals, and the cutting ability is a main index of the polishing efficiency of the polishing slurry;
secondly, the average particle size of the silica sol particles with certain grinding and polishing capacity can also be adjusted by adjusting the mass percentage concentration of the silica in the high-purity saturated silica sol solution, the smaller the silica sol particles are, the weaker the grinding and polishing capacity is, however, the tighter the silica particles formed by deposition and crystallization of the silica sol particles are, the higher the hardness is, and the stronger the cutting capacity is, so that the silica crystal particles with different cutting capacities can be obtained by adjusting the mass percentage concentration of the silica in the high-purity saturated silica sol solution and controlling the deposition and crystallization conditions and time of the silica sol particles;
controlling the rehydration condition and time of the silicon dioxide crystal particles to obtain a silica sol layer with different thicknesses wrapped outside the abrasive crystal nucleus;
although the silica sol layer also has certain cutting capacity, the cutting capacity of the silica sol layer is generally weaker and is more suitable for being used as a polishing agent on the surface of a workpiece, and the adhesiveness and the lubricity of the silica sol layer can play good lubricating, cooling and filling effects during grinding and polishing, so that the requirements of special ultra-precision grinding and polishing can be met.
Therefore, as can be seen from table 1, when the method provided by the present invention is used to prepare the silica polishing slurry, the polishing performance of the polishing slurry can be adjusted as required to meet the production requirements.
2. Grinding and polishing effect test
2.1) test method and detection indexes:
on the same polishing machine, different grinding polishing agents are respectively adopted to grind or polish workpieces made of the same material, the removal rate of the workpieces on the surface within the same time is mainly considered in the grinding process, and the removal rate and the scratch rate of the workpieces on the surface within the same time are mainly considered in the polishing process, wherein:
the removal rate is: within a certain time, the surface of the plane object is ground to the thickness of the plane object ground by the grinding and polishing agent;
the scratch rate is as follows: the number of scratches and pits which appear after the grinding and polishing of the grinding and polishing agent in unit area, wherein the scratches are scratches with a certain depth on the surface of the ground object.
2.2) detection method and detection instrument:
the scratch and the pit on the surface of the planar object are observed and detected by a wafer appearance detector;
the removal rate was measured using a three-dimensional profile gauge.
2.3.1) grinding test:
grinding a sample: 304 stainless steel plates and 4 inch sapphire plates;
test abrasives: the polishing agent 1 for polishing silicon dioxide provided in examples 1 to 5 of the present invention#～5#；
Comparison with abrasives: naerceae 2329plus (A) is a silica sol grinding agent with the average particle size of silica sol particles of 90-115 nanometers sold in the market.
Table 2 shows the thickness of the surface of the polished sample removed in 10 minutes after polishing the stainless steel sheet and the 4 inch sapphire sheet of the polished sample 304 with the test abrasive and the comparative abrasive.
TABLE 2
As can be seen from table 2:
the polishing agent 1 for polishing silicon dioxide provided in examples 1 to 5 of the present invention#～5#The removal rate of the 304 stainless steel sheet and the 4 inch sapphire sheet in the same time is far greater than that of the grinding polishing agent of the famous brand in the market world, that is, the silicon dioxide grinding polishing agent provided by the embodiment of the invention can greatly improve the grinding and polishing efficiency, meet the production requirement, improve the practicability, has good applicability and has great popularization and utilization values.
2.3.2) polishing test:
polishing the sample: 6 inches of silicon wafer;
test polishing agent: the polishing agent 1 for polishing silicon dioxide provided in examples 1 to 5 of the present invention#～5#；
Comparative polishing agent:
nano Kernel 2360(B), a commercially available ready-to-use polishing solution specially used for polishing silicon wafers, wherein silica sol particles of the ready-to-use polishing solution are in multimodal particle size distribution, and the average particle size is 60 nanometers;
dow 6504(C), a commercially available polishing solution having an average silica sol particle size of 70 to 80nm, and containing a strong base component.
Table 3 shows the thickness of the surface of the ground sample removed in 10 minutes and the scratch on the surface of the ground sample, which were obtained after polishing 6 inches of silicon wafers of the polished sample with the test polishing agent and the comparative polishing agent.
TABLE 3
As can be seen from table 3:
first, the polishing agent 1 for polishing silicon dioxide provided in examples 1 to 5 of the present embodiment#～5#In 1#～5#The removal rate of 6 inches of silicon wafer in the same time is far greater than or equal to that of the grinding polishing agent sold under the brand name in the world, namely, the silicon dioxide grinding polishing agent 1 provided by the embodiment of the invention is utilized#～5#The efficiency of grinding and polishing can be greatly improved, although 1#Higher than B and C, but 3#The scratch rate of the steel is equivalent to C; furthermore, 4#、5#The removal rate of the polishing slurry is not only greater than C but also much greater than B, and the scratch rate is slightly inferior to B and better than C, so that the silicon dioxide polishing slurry prepared by the preparation method of the silicon dioxide polishing slurry provided by the embodiment can improve the polishing efficiency, and 1#～3#The insufficient scratch rate performance of the sample can be realized by adopting 4#、5#Correcting the sample after performing middle polishing and fine polishing;
secondly, the comparative polishing agent C is prepared by adding KOH and H on the basis of silica sol2O2Organic chemical composition such as improve the chemical corrosivity, thereby corrode the silicon chip and soften and then improve polishing effect, however, this kind of polishing solution (abrasive material) corrodes the board seriously, simultaneously, need use a large amount of water in the course of lapping, cause the waste of water resource, moreover, the pollution and the environmental protection injury of the chemical composition of interpolation to water are very big, and the silicon dioxide that this embodiment provided grinds the polishing agent and does not add the chemical corrosion composition, carry out pure physical mechanical polishing and can reach and exceed the like abrasive material among the prior art, the effect is extremely showing, can provide huge help to the grinding of this trade, the polishing operation.
In summary, it can be seen that:
the preparation method of the silicon dioxide grinding and polishing agent provided by the embodiment of the invention has the advantages of unique and stable process and strong operability, can produce grinding and polishing products meeting various requirements and social requirements, does not cause pollution to the environment in the production process, is energy-saving and environment-friendly, provides positive social benefits, and can obtain better economic benefits for enterprises, thereby having great popularization and application values.
During the description of the above description:
the description of the terms "present embodiment," "present invention embodiment," "illustrated at … …," "further," and the like, means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention;
in this specification, the schematic representations of the terms used above are not necessarily for the same embodiment or example, and the particular features, structures, materials, or characteristics described, etc., may be combined or brought together in any suitable manner in any one or more embodiments or examples;
furthermore, those of ordinary skill in the art may combine or combine features of different embodiments or examples and features of different embodiments or examples described in this specification without undue conflict.
Finally, it should be noted that:
although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made on the technical solutions described in the foregoing embodiments, or some or all of the technical features of the embodiments can be equivalently replaced, and the corresponding technical solutions do not depart from the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing a silicon dioxide grinding and polishing agent is characterized by comprising the following steps:
the preparation method comprises the steps of preparing abrasive crystal seeds, preparing high-purity saturated silica sol solution, preparing abrasive crystal nuclei with loose silica crystal particles deposited, and preparing an abrasive crystal nucleus mixed emulsion wrapped by the silica sol layer;
the preparation steps of the abrasive grain seed crystal comprise:
putting rod-shaped or irregular multi-edge abrasive powder into a high-frequency ultrasonic grinding device, adding water, carrying out wet ultrafine grinding, and washing and filtering to obtain abrasive seed crystal initial particles with required particle sizes;
placing the abrasive seed crystal initial particles in a high-pressure kettle, adding pure water, adding concentrated ammonia water serving as a catalyst, stirring and heating to ensure that the abrasive seed crystal initial particles are dissolved in the pure water dissolved with ammonium ions at the edges, realizing the shape reformation of the abrasive seed crystal initial particles, and obtaining a mixture of abrasive seed crystals with passivated surface edges and corners and an ammonia water solution;
washing, filtering and drying the mixture of the abrasive seed crystal and the ammonia water solution to obtain the abrasive seed crystal;
the preparation method of the high-purity saturated silica sol solution comprises the following steps:
adding high-purity simple substance silicon powder and pure water into a high-pressure kettle, adding concentrated ammonia water as a catalyst, heating and stirring to enable the high-purity simple substance silicon powder to react with water under the catalysis of the concentrated ammonia water to generate hydrated silicic acid, and continuing heating and stirring to enable the hydrated silicic acid to gradually polymerize under the alkaline water quality condition formed by the concentrated ammonia water to obtain alkaline silicon dioxide initial sol;
aging and removing ammonia from the initial silica sol to obtain neutral silica sol;
introducing a gas isolation lubricant into the neutral silica sol to dissolve gas into silica sol particles and among the particles in the neutral silica sol so as to reduce the polymerization force among the silica sol particles, and heating and concentrating to obtain a high-purity saturated silica sol solution;
the preparation steps of the abrasive material crystal nucleus deposited with the loose silicon dioxide crystal particles comprise:
adding a certain amount of the abrasive seed crystals into the high-purity saturated silica sol solution to form a seed crystal silica sol mixed solution, introducing the gas isolation lubricant into the seed crystal silica sol mixed solution to keep the mixed solution in a boiling state, heating and stirring the mixed solution, gradually concentrating the seed crystal silica sol mixed solution, and depositing part of silica sol particles in the seed crystal silica sol mixed solution on the abrasive seed crystals to form a loose silica crystal layer to obtain a crystal mixed solution;
aging the crystallization mixed solution, washing with water, filtering, removing water and concentrating to obtain an abrasive crystal nucleus deposited with loose silicon dioxide crystal particles;
the preparation method of the abrasive crystal nucleus mixed emulsion wrapped with the silica sol layer comprises the following steps:
mixing the abrasive crystal nucleus with pure water and concentrated ammonia water in a high-pressure kettle, heating and stirring to partially dissolve loose silicon dioxide crystal particles on the surface of the abrasive crystal nucleus to form silica sol, then decompressing and deaminating, adding a dispersing agent and a surfactant, stirring uniformly, and cooling to obtain the abrasive crystal nucleus mixed emulsion wrapped with the silica sol layer, namely the grinding and polishing agent.
2. The method of making a silica abrasive polishing slurry of claim 1 wherein:
the abrasive powder is any one or more of crystalline silica powder, crystal powder, remelted crystal powder and crystalline quartz powder, and the average particle size of the initial particles of the abrasive seed crystals is 0.5-5 microns.
3. The method of making a silica abrasive polishing slurry of claim 1 wherein: the gas isolation lubricant is one or more of olefin, alkane, alkaline gas and inert gas.
4. The method of making a silica abrasive polishing slurry of claim 3 wherein:
the olefin is ethylene, the alkane is methane or propane, the alkaline gas is methylamine, and the inert gas is nitrogen or argon.
5. The method of making a silica abrasive polishing slurry of claim 1 wherein:
the concentrated ammonia water is ammonia water with the mass percentage concentration of 25-28% of ammonia, the dispersing agent is one or more of sodium hexametaphosphate, sodium polyacrylate or sodium citrate, and the surfactant is an anionic surfactant or a nonionic surfactant.
6. The method of making a silica abrasive polishing slurry of claim 1 wherein: the dosage of the abrasive seed crystal is 0.5-15% of the total mass of the grinding and polishing agent.
7. The method of making a silica abrasive polishing slurry of claim 1 wherein:
the mass percentage concentration of silicon dioxide in the high-purity saturated silica sol solution is 10-50%, the purity of the silicon dioxide is more than 99.999%, and the average particle size of silica sol particles is 2-40 nm.
8. The method of making a silica abrasive polishing slurry of claim 1 wherein: in the step of preparing the abrasive seed crystal, the ultrasonic frequency of the high-frequency ultrasonic grinding device is 15-30 MHz.
9. The method of making a silica abrasive polishing slurry of claim 1 wherein:
and in the preparation step of the high-purity saturated silica sol solution and the preparation step of the abrasive crystal nucleus deposited with the loose silica crystal particles, the pressure of the introduced gas isolation lubricant is 1-4 MPa.
10. The method of making a silica abrasive polishing slurry of claim 1 wherein:
stirring speed of the stirring is 200-1000 r/min, and heating temperature of the heating is controlled to be 120-180 ℃;
in the preparation step of the abrasive seed crystal, the preparation step of the high-purity saturated silica sol solution and the preparation step of the abrasive crystal nucleus mixed emulsion wrapped by the silica sol layer, the working pressure of the high-pressure autoclave is kept between 2 and 6 MPa.
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