CN114380611B - Method for manufacturing reaction sintering silicon carbide ceramic grinding disc - Google Patents
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Abstract
The invention discloses a method for manufacturing a reaction sintering silicon carbide ceramic grinding disc, which comprises the following specific steps: preparing granulation powder, adding a toughening material, dipping a carbon fiber woven body, preforming a grinding disc blank, processing the grinding disc blank, sintering the grinding disc blank, and processing the grinding disc. The grinding disc prepared by the method has good toughness, high radial strength and good reliability; the method has the advantages of simple process, low production cost and high production efficiency, and is suitable for industrially preparing the high-performance silicon carbide ceramic grinding disc.
Description
Technical Field
The invention relates to the technical field of silicon carbide ceramic grinding materials, in particular to a method for manufacturing a reaction sintering silicon carbide ceramic grinding disc.
Background
The grinding process is a common process for finishing a processing surface by utilizing the relative motion of a grinding tool (grinding disc/sheet) and a workpiece under a certain pressure, and the grinding process also needs to select abrasive particles with proper types and particle sizes to improve the processing efficiency and ensure the processing quality. The grinding process can be used for processing various metal and non-metal materials, and has wide application in the fields of precious stones, ceramics, mobile phones, wafers and the like.
The grinding disc is an important key component of grinding processing equipment. When the grinding disc rotates, the grinding particles are driven by the grinding disc to flexibly grind or polish the workpiece, and the grinding particles can also generate a grinding effect on the grinding disc when grinding the workpiece, namely, the grinding disc is worn and consumed. Therefore, the material and performance of the grinding disc have great influence on the grinding efficiency and quality. In addition to a high geometric accuracy of the working surface, the grinding disks should satisfy the following requirements: 1) The structure is reasonable, and the rigidity, the precision retentivity and the wear resistance are good; 2) The material has proper hardness, and the uniformity and the consistency of the hardness in the surface are good; 3) The grinding disc has uniform and compact tissue and no defects of impurities, foreign matters, air holes, cracks and the like; 4) The machined surface is provided with proper groove arrangement, so that the chip removal and containing performance is good, and the heat dissipation performance is good.
The materials of the prior common grinding disc mainly comprise copper, tin, stainless steel, cast iron, resin and the like, and the application occasions of the grinding discs made of different materials are different. The copper disc is mainly used for fine grinding of workpieces such as sapphire and the like; tin plates are also used mainly for refining, such as for example of ceramic products; stainless steel discs are commonly used for the fine grinding of metal products; the iron plate is mainly used for rough grinding, such as rough grinding of iron and alloy steel products.
Chips are the key in modern high-tech field, and wafers made by cutting, grinding and polishing ingots are the basis for preparing chips. For example, in the semiconductor industry, a polishing disk made of cast iron or carbon steel is commonly used, but the cast iron or carbon steel has relatively low hardness and rigidity, poor oxidation resistance and corrosion resistance, and poor wear resistance, and thus has a short service life. And the coefficient of thermal expansion is large, the thermal conductivity is low, and the flatness and parallelism of the silicon wafer are difficult to ensure due to abrasion and thermal deformation of the grinding disc during the process of processing the silicon wafer, particularly during high-speed grinding or polishing. With the increasing popularity of the third generation semiconductor silicon carbide single crystal, it has been difficult for conventional metal abrasive disks to meet their requirements for high speed grinding or polishing due to the higher hardness of the silicon carbide single crystal.
The silicon carbide ceramic has the advantages of high hardness, wear resistance, corrosion resistance, high rigidity, high thermal conductivity, small thermal expansion coefficient, good chemical stability and the like, so that the silicon carbide ceramic becomes an ideal material for high-speed precision grinding and polishing grinding discs of wafers, sapphire panels, solar silicon wafers, electronic ceramics and the like. However, silicon carbide ceramics have poor toughness, and when they are used as polishing disks for high-speed polishing, the centrifugal force exceeds the tensile strength thereof, which may cause damage to the polishing disks.
Therefore, the problem to be solved is to improve the toughness of the silicon carbide ceramic grinding disk.
Reaction sintering is a common preparation method of silicon carbide ceramics, and the silicon carbide is generated by in-situ reaction of molten silicon infiltrated into a green body and existing carbon in the green body, and the silicon carbide micro powder in the green body is combined to prepare the compact silicon carbide ceramics. However, the direct reaction of the molten silicon with the carbon fibers results in a decrease in the performance of the carbon fibers and a decrease in the reinforcing and toughening effects of the carbon fibers.
Disclosure of Invention
In view of the above, the present invention provides a method for manufacturing a high-toughness reaction-sintered silicon carbide ceramic grinding disk, which solves the problems of poor reliability and easy radial cracking of the grinding disk caused by poor toughness of silicon carbide ceramic.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for manufacturing a reaction sintering silicon carbide ceramic grinding disc comprises the steps of preparing a grinding disc by using a raw material comprising a matrix material and a toughening material; the matrix material comprises, by mass, 100 parts of silicon carbide micro powder, 5-15 parts of carbon powder, 5-15 parts of adhesive, 0.5-3 parts of surfactant and 0.5-2 parts of dispersant; the toughening material is carbon fiber and a carbon fiber woven body, and the addition amount of the carbon fiber is 0-15% of the total amount of the matrix material;
the manufacturing method specifically comprises the following steps:
(1) Preparation of granulated powder
Weighing the matrix material according to the proportion, adding deionized water, and performing ball milling for 8-20 hours to obtain silicon carbide ceramic slurry; then, carrying out spray granulation on the silicon carbide ceramic slurry to obtain granulated powder; the water content of the granulated powder is 0.5-1.2%, and the mass ratio of the granulated powder with the granularity of 60-180 meshes is more than 95%;
(2) Adding toughening material
Adding short carbon fibers into the granulated powder, and mixing by using a vibrating screen;
(3) Impregnation treatment of carbon fiber woven body
Weaving carbon fibers into a carbon fiber woven body with a two-dimensional mesh structure, wherein the length and the width of meshes of the carbon fiber woven body are respectively 3-50mm and 3-50mm; then dipping the carbon fiber bundles in the mixed slurry to ensure that the surface of the carbon fiber bundles is fully distributed with the mixed slurry, wherein the mixed slurry is prepared by mixing nano carbon powder, nano silicon powder, a binder, a dispersing agent and deionized water by wet ball milling for 8-20 hours;
then placing the carbon fiber woven body in a vacuum drying oven, placing the carbon fiber woven body for 5-20h at the temperature of 25-35 ℃, and then heating to 60-80 ℃ for drying for 10-30h to dry the carbon fiber woven body; soaking the dried carbon fiber woven body in the mixed slurry again, and repeating the steps for multiple times to ensure that the surface of the dried carbon fiber woven body is uniformly coated with a layer of silicon powder and carbon powder; preserving the heat of the dried impregnated carbon fiber woven body for 1-6 hours at 1430-1600 ℃ in a vacuum furnace; silicon powder and carbon powder on the surface of the carbon fiber woven fabric are subjected to in-situ reaction to form silicon carbide and a silicon carbide protective layer of the carbon fiber, so that the performance of the carbon fiber is prevented from being reduced during subsequent siliconizing treatment.
The carbon fiber woven body is subjected to dipping treatment, so that the interface bonding strength of the carbon fiber and the silicon carbide ceramic matrix can be improved, and the carbon fiber can be protected from being corroded by molten silicon; the radial strength of the silicon carbide ceramic can be obviously improved by the mesh design of the carbon fibers, and because the meshes are too small, granulated powder is not easy to enter a woven body, so that the silicon carbide ceramic matrix is easy to layer; the mesh size is too large, and the toughening effect is not obvious;
(4) Preforming of abrasive disk blanks
Laying a layer of silicon carbide granulation powder added with short carbon fibers in a mould, compacting and flattening the silicon carbide granulation powder on a vibration platform, laying a soaked carbon fiber woven body, laying a layer of silicon carbide granulation powder added with short carbon fibers, and vertically tamping the carbon fiber woven body by using a blunt metal rod, wherein the tip diameter of the metal rod is smaller than the mesh size of the carbon fiber woven body; part of the short carbon fibers are distributed in the vertical direction by up and down ramming, so that the toughness of the silicon carbide ceramic is improved, and the powder laying density is improved; the laying thickness of the granulation powder and the carbon fiber braided body can be adjusted according to the thickness of the grinding disc;
molding the mold after vibrating compaction and flattening to obtain a preformed blank of the grinding disc, performing cold isostatic pressing on the preformed blank after packaging and vacuumizing, wherein the pressure of the cold isostatic pressing is 60-150MPa, the pressure maintaining time is 5-30min, and the green density of the blank of the grinding disc is controlled to be 1.80-2.10g/cm 3 ；
(5) Machining of abrasive disk blanks
Drying the grinding disc blank formed by cold isostatic pressing at 80-150 ℃ for 8-20 hours; then turning to obtain a flat surface and required appearance and size, and machining a groove with required shape and size on the working surface according to the requirement;
(6) Sintering of abrasive disk blanks
Placing the processed grinding disc blank in a vacuum sintering furnace, paving metal silicon particles below and on the side surface of the grinding disc, smearing a thin layer of boron nitride slurry on a groove on the working surface of the grinding disc to prevent the groove from being damaged by the silicon particles, wherein the silicon consumption is 0.8-2.0 times of the mass of the grinding disc blank, and preserving heat at 1450-1800 ℃ for 1-8 hours to prepare a grinding disc sintered body;
(7) Manufacture of abrasive discs
And grinding, lapping and polishing the sintered body of the lapping disc to obtain the silicon carbide ceramic lapping disc with required specification, shape, size and flatness.
Preferably, the carbon fiber woven body and the chopped carbon fibers are high-strength carbon fibers, and the tensile strength of the high-strength carbon fibers is not less than 2500MPa; wherein the length of the chopped carbon fiber is 3-10mm, and the diameter of the tow is less than 500 mu m; the diameter of the carbon fiber braided body tows is less than 2000 mu m.
Preferably, the silicon carbide micro powder is prepared from D 50 Silicon carbide micropowder of 3 to 10 μm, D 50 15-30 μm of silicon carbide micropowder and D 50 Silicon carbide micro powder with the particle size of 40-60 mu m is prepared by the following raw materials in percentage by mass (3-8): (2-4): 1 in proportion.
Preferably, the binder is a phenolic resin, polyvinyl alcohol or carboxymethyl cellulose.
Preferably, the surfactant is stearic acid or fatty glyceride; the dispersant is tetramethyl ammonium hydroxide or polyacrylic acid.
Preferably, D of the carbon powder 50 Less than 200nm.
Preferably, the molar ratio of the nano carbon powder to the nano silicon powder in the step (3) is 1:1.05-1.25 percent, the addition amount of the binder is 2-10 percent of the total mass of the nano carbon powder and the nano silicon powder, the addition amount of the dispersant is 0.5-3 percent of the total mass of the nano carbon powder and the nano silicon powder, and the ratio of the deionized water to the total mass of the nano carbon powder and the nano silicon powder is 1.0-2.0:1; wherein D of the nano carbon powder and the nano silicon powder 50 Are not more than 100nm.
Preferably, the dispersant in step (3) is polyvinylpyrrolidone or tetramethylammonium hydroxide.
Preferably, the binder in step (3) is polyvinyl alcohol or carboxymethyl cellulose.
The beneficial effects of the invention are:
according to the invention, the silicon carbide ceramic is toughened through the high-strength two-dimensional carbon fiber braided body, so that the toughness and reliability of the silicon carbide ceramic grinding disc are improved; the nano silicon powder and the nano carbon powder coated on the carbon fiber braided body tows are subjected to in-situ reaction by an impregnation method to generate the silicon carbide, so that the interface bonding strength of the carbon fibers and the silicon carbide ceramic matrix is improved, and the toughening effect of the grinding disc is enhanced.
By adding the short carbon fibers and adopting a vertical up-down tamping mode, the short carbon fibers are vertical to the two-dimensional carbon fiber woven body, and the toughening effect in the vertical direction is achieved.
The vibrating platform is adopted to stamp and pave to become technology to combine mould pressing pre-compaction shaping, cold isostatic pressing shaping technology preparation abrasive disc unburned bricks, can improve unburned bricks homogeneity, improve unburned bricks density, intensity, the unburned bricks processing of being convenient for, and guarantee the homogeneity, the uniformity of final product.
The invention adopts a fine-bundle two-dimensional carbon fiber braided body and combines the short carbon fibers which are vertically distributed, and simultaneously enhances the strength and the toughness of the silicon carbide ceramic in the horizontal and vertical directions.
According to the invention, silicon powder and carbon powder on the surface of the carbon fiber woven fabric are subjected to in-situ reaction by adopting reactive sintering to form silicon carbide, so that a silicon carbide protective layer of the carbon fiber is formed, and the performance of the carbon fiber is prevented from being reduced during subsequent siliconizing treatment.
Compared with the method for preparing the carbon fiber reinforced and toughened silicon carbide ceramic material by adopting the three-dimensional carbon fiber woven body as the matrix skeleton and utilizing the melting infiltration process and the chemical vapor infiltration process, the method has the advantages of simple process, low production cost and high production efficiency, and is suitable for industrially preparing the high-performance silicon carbide ceramic grinding disc.
Detailed Description
The invention is further described below using examples.
Example 1
A method for manufacturing a reaction sintering silicon carbide ceramic grinding disc comprises the following steps:
(1) Preparation of granulated powder
Weighing the matrix materials according to the proportion: d 50 50 parts of 3 mu m silicon carbide micro powder, D 50 15 mu m silicon carbide micro powder 35 parts, D 50 15 portions of silicon carbide micro powder with the particle size of 40 mu m and carbon powder5 parts of phenolic resin, 5 parts of stearic acid, 0.5 part of tetramethyl ammonium hydroxide and 0.5 part of tetramethyl ammonium hydroxide.
And then adding the weighed matrix material into 90 parts of deionized water, and carrying out ball milling in a roller ball mill for 8 hours to obtain the silicon carbide ceramic slurry.
Spraying and granulating the silicon carbide ceramic slurry by using a centrifugal spray tower to obtain granulated powder; the water content of the granulated powder is measured to be 0.6 percent, and the mass ratio of the granulated powder between 60 and 180 mesh standard sieves is 96.6 percent.
(2) Adding toughening material
Weighing 100 parts of granulated powder, adding 3 parts of chopped carbon fibers with the length of 3mm and the tow diameter of 100 mu m, and uniformly mixing by using a vibrating screen.
(3) Impregnation treatment of carbon fiber woven body
100 parts of nano carbon powder, 250 parts of nano silicon powder, 18 parts of polyvinyl alcohol and 3.5 parts of polyvinylpyrrolidone, 450 parts of deionized water is added, and the mixture is ball-milled for 14 hours in a roller ball mill to prepare the mixture slurry of the nano silicon powder and the nano carbon powder.
Placing a two-dimensional mesh-shaped carbon fiber woven body with a tow diameter of 100 mu m and a mesh length and a mesh width of 20mm and 20mm respectively in mixed slurry for dipping for 8min, wherein the carbon fiber woven body can shake in the slurry in the dipping process, so that the surface of the carbon fiber woven body is fully covered with nano silicon powder and nano carbon powder.
Then placing the carbon fiber woven body in a vacuum drying oven, placing the carbon fiber woven body for 20 hours at 25 ℃, and then heating to 80 ℃ for drying for 10 hours to dry the carbon fiber woven body; and then, putting the dried carbon fiber woven body into the mixed slurry again for dipping, and repeating the steps of dipping and drying for 3 times to uniformly coat a layer of nano silicon powder and nano carbon powder on the surface of the dried carbon fiber woven body.
And then preserving the dried impregnated carbon fiber woven body in a vacuum furnace at the temperature of 1430 ℃ for 6 hours to enable silicon powder and carbon powder on the surface of the carbon fiber woven body to react in situ to form silicon carbide and form a silicon carbide protective layer of the carbon fiber.
(4) Preforming of abrasive disk blanks
Firstly paving a layer of silicon carbide granulation powder containing short carbon fibers with the thickness of 40mm in a stainless steel mould with the inner diameter of 600mm on a vibration platform, then paving a soaked carbon fiber woven body, vertically tamping up and down in a mesh of the carbon fiber woven body by using a blunt metal rod with the tip diameter of 5mm, vibrating and flattening, paving a layer of silicon carbide granulation powder added with the short carbon fibers with the thickness of 20mm, paving a soaked carbon fiber woven body, vertically tamping up and down in the mesh of the woven body by using a blunt metal rod with the tip diameter of 5mm, vibrating and flattening; laying a layer of silicon carbide granulation powder with the thickness of 20mm and added with short carbon fibers, laying the impregnated carbon fiber braided body, vertically tamping the carbon fiber braided body up and down in the mesh of the braided body by using a blunt metal rod with the tip diameter of 5mm, and vibrating and compacting and flattening; then a layer of silicon carbide granulation powder mixed with short carbon fibers and having a thickness of 40mm is paved, a blunt metal rod with the tip diameter of 5mm is used for vertically ramming up and down in meshes of the braided body, and the braided body is vibrated to compact and level.
And performing compression molding on the mold after the vibration compaction and the flattening to obtain a preformed blank of the grinding disc, and performing cold isostatic pressing on the preformed blank after packaging and vacuumizing, wherein the pressure of the cold isostatic pressing is 60MPa, and the pressure maintaining time is 30min.
(5) Machining of abrasive disk blanks
Drying the grinding disc blank formed by cold isostatic pressing at 80 ℃ for 20 hours; and then turning to obtain a cylinder with an outer diameter of 580mm, a thickness of 70mm and two planar upper and lower surfaces. A series of concentric circular grooves are machined in one plane of the cylinder, the depth of each groove is 3mm, the width of each groove is 1.5mm, and the distance between the grooves is 10mm.
(6) Sintering of abrasive disk blanks
Placing the processed grinding disc blank in a vacuum sintering furnace, paving metal silicon particles below and on the side surface of the grinding disc, wherein the silicon consumption is 1.2 times of the mass of the grinding disc blank, smearing a thin layer of boron nitride slurry on the groove of the working surface of the grinding disc to prevent the silicon particles from forming on the groove to damage the groove structure, and preserving heat at 1450 ℃ for 8 hours to obtain the grinding disc sintered body.
(7) Manufacture of abrasive discs
And grinding, lapping and polishing the grinding disc sintered body to obtain the silicon carbide ceramic grinding disc with required specification, shape, size and flatness.
Through detection, the obtained silicon carbide ceramic grinding disc has the relative density of 99.3 percent, the Vickers microhardness of 24.6GPa, the three-point bending strength of 626.1MPa and the fracture toughness of 8.5 MPa-m 1/2 。
Example 2
A method for manufacturing a reaction sintering silicon carbide ceramic grinding disc comprises the following steps:
(1) Preparation of granulated powder
Weighing the matrix materials according to the proportion: d 50 58 parts of 6.5 mu m silicon carbide micro powder and D 50 30 portions of silicon carbide micro powder with the particle size of 25 mu m, D 50 12 parts of 45-micron silicon carbide micro powder, 10 parts of carbon powder, 6 parts of phenolic resin, 0.8 part of stearic acid and 0.6 part of tetramethyl ammonium hydroxide.
And then adding the weighed matrix material into 120 parts of deionized water, and carrying out ball milling in a roller ball mill for 12 hours to obtain silicon carbide ceramic slurry.
Then, carrying out spray granulation on the silicon carbide ceramic slurry by using a centrifugal spray tower to obtain granulated powder; the water content of the granulated powder is measured to be 0.7 percent, and the mass ratio of the granulated powder between 60 and 180 mesh standard sieves is 96.0 percent.
(2) Adding toughening material
Weighing 100 parts of granulating powder, adding 5 parts of chopped carbon fibers with the length of 5mm and the strand diameter of 120 mu m, and uniformly mixing by using a vibrating screen.
(3) Impregnation treatment of carbon fiber woven body
100 parts of nano carbon powder, 270 parts of nano silicon powder, 20 parts of polyvinyl alcohol and 3.5 parts of polyvinylpyrrolidone, adding 500 parts of deionized water, and ball-milling for 15 hours in a roller ball mill to prepare the mixture slurry of the nano silicon powder and the nano carbon powder.
Placing a two-dimensional mesh-shaped carbon fiber woven body with a tow diameter of 500 mu m and a mesh length and a mesh width of 3mm and 3mm respectively in mixed slurry for soaking for 5min, wherein the carbon fiber woven body can shake in the slurry in the soaking process, so that the surface of the carbon fiber woven body is fully covered with nano silicon powder and nano carbon powder.
Then placing the carbon fiber woven body in a vacuum drying box, placing the carbon fiber woven body for 10 hours at the temperature of 30 ℃, and then heating the carbon fiber woven body to 70 ℃ for drying for 20 hours to dry the carbon fiber woven body; and then, putting the dried carbon fiber woven body into the mixed slurry again for dipping, and repeating the steps of dipping and drying for 3 times to uniformly coat a layer of nano silicon powder and nano carbon powder on the surface of the dried carbon fiber woven body. And then preserving the dried impregnated carbon fiber woven body in a vacuum furnace at 1500 ℃ for 4 hours to enable silicon powder and carbon powder on the surface of the carbon fiber woven body to react in situ to form silicon carbide and form a silicon carbide protective layer of the carbon fiber.
(4) Preforming of abrasive disk blanks
Firstly paving a layer of silicon carbide granulation powder containing short carbon fibers with the thickness of 40mm in a stainless steel mould with the inner diameter of 600mm on a vibration platform, then paving a soaked carbon fiber woven body, vertically tamping up and down in a mesh of the carbon fiber woven body by using a blunt metal rod with the tip diameter of 5mm, vibrating and flattening, paving a layer of silicon carbide granulation powder added with the short carbon fibers with the thickness of 20mm, paving a soaked carbon fiber woven body, vertically tamping up and down in the mesh of the woven body by using a blunt metal rod with the tip diameter of 5mm, vibrating and flattening; paving a layer of silicon carbide granulation powder which is 20mm thick and added with the short carbon fibers, paving the impregnated carbon fiber woven body, vertically tamping the carbon fiber woven body up and down in meshes of the woven body by using a blunt metal rod with the tip diameter of 5mm, and vibrating and compacting and leveling; then, a layer of silicon carbide granulation powder mixed with the short carbon fibers and having a thickness of 40mm is paved, a blunt metal rod with a tip diameter of 5mm is used for vertically tamping up and down in meshes of the woven body, and the woven body is vibrated to compact and flatten.
And performing compression molding on the mold after the vibration compaction and the flattening to obtain a preformed blank of the grinding disc, and performing cold isostatic pressing on the preformed blank after packaging and vacuumizing, wherein the pressure of the cold isostatic pressing is 80MPa, and the pressure maintaining time is 6min.
(5) Machining of abrasive disk blanks
Drying the grinding disc blank formed by cold isostatic pressing for 10 hours at the temperature of 100 ℃; and then turning to obtain a cylinder with an outer diameter of 580mm, a thickness of 70mm and two planar upper and lower surfaces. A plurality of rows of concentric circular grooves are machined in one plane of the cylinder, the depth of each groove is 3mm, the width of each groove is 1.5mm, and the distance between the grooves is 10mm.
(6) Sintering of abrasive disk blanks
Placing the processed grinding disc blank in a vacuum sintering furnace, spreading metal silicon particles below and on the side surface of the grinding disc, wherein the silicon consumption is 1.2 times of the mass of the grinding disc blank, coating a thin layer of boron nitride slurry on the groove of the working surface of the grinding disc to prevent the silicon particles formed on the groove from damaging the groove structure, and preserving heat at 1600 ℃ for 4 hours to obtain the grinding disc sintered body.
(7) Manufacture of abrasive discs
And grinding, lapping and polishing the sintered body of the lapping disc to obtain the silicon carbide ceramic lapping disc with required specification, shape, size and flatness.
Through detection, the obtained silicon carbide ceramic grinding disc is 99.4 percent, the Vickers microhardness is 24.5GPa, the three-point bending strength is 629.8MPa, and the fracture toughness is 8.5 MPa.m 1/2 。
Example 3
A method for manufacturing a reaction sintering silicon carbide ceramic grinding disc comprises the following steps:
(1) Preparation of granulated powder
Weighing the matrix materials according to the proportion: d 50 60 parts of 10 mu m silicon carbide micro powder and D 50 30 parts of 30 mu m silicon carbide micro powder and D 50 10 parts of 60-micron silicon carbide micro powder, 15 parts of carbon powder, 15 parts of polyvinyl alcohol, 3 parts of fatty glyceride and 2 parts of polyacrylic acid.
And then adding the weighed matrix material into 150 parts of deionized water, and carrying out ball milling in a roller ball mill for 20 hours to obtain silicon carbide ceramic slurry.
Spraying and granulating the silicon carbide ceramic slurry by using a centrifugal spray tower to obtain granulated powder; the water content of the granulated powder is measured to be 1.2 percent, and the mass ratio of the granulated powder between 60 and 180 mesh standard sieves is 96.2 percent.
(2) Adding toughening material
Weighing 100 parts of granulated powder, adding 4 parts of chopped carbon fibers with the length of 10mm and the tow diameter of 200 mu m, and uniformly mixing by using a vibrating screen.
(3) Impregnation treatment of carbon fiber woven body
100 parts of nano carbon powder, 270 parts of nano silicon powder, 20 parts of polyvinyl alcohol and 3.5 parts of polyvinylpyrrolidone, adding 500 parts of deionized water, and performing ball milling in a roller ball mill for 15 hours to prepare mixture slurry of the nano silicon powder and the nano carbon powder.
Placing a two-dimensional mesh-shaped carbon fiber woven body with a tow diameter of 1000 mu m and mesh openings of which the length and width are 50mm and 50mm respectively into mixed slurry for soaking for 5min, wherein the carbon fiber woven body can shake in the slurry in the soaking process, so that the surface of the carbon fiber woven body is fully covered with nano silicon powder and nano carbon powder.
Then placing the carbon fiber woven body in a vacuum drying oven, placing the carbon fiber woven body for 5 hours at 35 ℃, and then heating to 80 ℃ for drying for 10 hours to dry the carbon fiber woven body; and then, putting the dried carbon fiber woven body into the mixed slurry again for dipping, and repeating the steps of dipping and drying for 3 times to uniformly coat a layer of nano silicon powder and nano carbon powder on the surface of the dried carbon fiber woven body. And then preserving the dried impregnated carbon fiber woven body in a vacuum furnace at 1600 ℃ for 2 hours to enable silicon powder and carbon powder on the surface of the carbon fiber woven body to react in situ to form silicon carbide and form a silicon carbide protective layer of the carbon fiber.
(4) Preforming of abrasive disk blanks
Firstly paving a layer of silicon carbide granulation powder containing short carbon fibers with the thickness of 40mm in a stainless steel mould with the inner diameter of 600mm on a vibration platform, then paving a soaked carbon fiber woven body, vertically tamping up and down in the meshes of the carbon fiber woven body by using a blunt metal rod with the tip diameter of 5mm, vibrating and leveling, paving a layer of silicon carbide granulation powder with the thickness of 20mm and added with the short carbon fibers, paving the soaked carbon fiber woven body, vertically tamping up and down in the meshes of the woven body by using a blunt metal rod with the tip diameter of 5mm, vibrating and leveling; laying a layer of silicon carbide granulation powder with the thickness of 20mm and added with short carbon fibers, laying the impregnated carbon fiber braided body, vertically tamping the carbon fiber braided body up and down in the mesh of the braided body by using a blunt metal rod with the tip diameter of 5mm, and vibrating and compacting and flattening; then, a layer of silicon carbide granulation powder mixed with the short carbon fibers and having a thickness of 40mm is paved, a blunt metal rod with a tip diameter of 5mm is used for vertically tamping up and down in meshes of the woven body, and the woven body is vibrated to compact and flatten.
And performing compression molding on the mold after the vibration compaction and the flattening to obtain a preformed blank of the grinding disc, and performing cold isostatic pressing on the preformed blank after packaging and vacuumizing, wherein the pressure of the cold isostatic pressing is 150MPa, and the pressure maintaining time is 5min.
(5) Machining of abrasive disk blanks
Drying the grinding disc blank formed by cold isostatic pressing at 150 ℃ for 8 hours; and then turning to obtain a cylinder with an outer diameter of 580mm, a thickness of 70mm and two planar upper and lower surfaces. A plurality of rows of concentric circular grooves are machined in one plane of the cylinder, the depth of each groove is 3mm, the width of each groove is 1.5mm, and the distance between the grooves is 10mm.
(6) Sintering of abrasive disk blanks
Placing the processed grinding disc blank in a vacuum sintering furnace, spreading metal silicon particles below and on the side surface of the grinding disc, wherein the silicon consumption is 1.2 times of the mass of the grinding disc blank, coating a thin layer of boron nitride slurry on the groove of the working surface of the grinding disc to prevent the silicon particles formed on the groove from damaging the groove structure, and preserving heat at 1800 ℃ for 2 hours to obtain the grinding disc sintered body.
(7) Manufacture of abrasive discs
And grinding, lapping and polishing the sintered body of the lapping disc to obtain the silicon carbide ceramic lapping disc with required specification, shape, size and flatness.
Through detection, the obtained silicon carbide ceramic grinding disc has the relative density of 99.3 percent, the Vickers microhardness of 24.3GPa, the three-point bending strength of 631.1MPa and the fracture toughness of 8.6 MPa.m 1/2 。
Comparative example 1:
a method for manufacturing a reaction sintering silicon carbide ceramic grinding disc comprises the following steps:
technical solution reference is made to example 1.
The difference is that:
removing the dipping treatment of the carbon fiber woven body in the step (3); and (5) simultaneously removing the pre-forming of the grinding disc blank in the step (4) and laying a carbon fiber braided body layer.
The rest of the procedure was the same as in example 1.
Through detection, the obtained silicon carbide ceramic grinding disc has the relative density of 99.7 percent, the Vickers microhardness of 25.4GPa, the three-point bending strength of 390.6MPa and the fracture toughness of 4.1MPa.m 1/2 。
Comparative example 2:
a method for manufacturing a reaction sintering silicon carbide ceramic grinding disc comprises the following steps:
technical solution reference is made to example 1.
The difference is that:
removing the short carbon fiber added in the step (2); in the step (4), a blunt metal rod is not used for vertically ramming up and down in meshes of the braided body.
The rest is the same as in example 1.
Through detection, the obtained silicon carbide ceramic grinding disc has the relative density of 99.5 percent, the Vickers microhardness of 25.0GPa, the three-point bending strength of 570.2MPa and the fracture toughness of 7.7MPa.m 1/2 。
Comparative example 3:
a method for manufacturing a reaction sintering silicon carbide ceramic grinding disc comprises the following steps:
technical solution reference is made to example 1.
The difference is that: the dipping treatment of the carbon fiber braided body in the step (3) is removed.
The rest is the same as in example 1.
Through detection, the obtained silicon carbide ceramic grinding disc has the relative density of 99.3 percent, the Vickers microhardness of 25.1GPa, the three-point bending strength of 530.2MPa and the fracture toughness of 6.1MPa.m 1/2 。
Comparative example 4:
a method for manufacturing a reaction sintering silicon carbide ceramic grinding disc comprises the following steps:
technical solution reference is made to example 1.
The difference is that: the carbon fiber woven body is changed into carbon fiber cloth almost without meshes.
The rest is the same as in example 1.
The obtained silicon carbide ceramic grinding disc has poor bonding strength between the ceramic matrix and the carbon fiber cloth, and the ceramic matrix and the carbon fiber cloth are easy to delaminate and peel.
And (4) analyzing results:
1. compared with the comparative example 1, the embodiment 1-3 shows that the two-dimensional carbon fiber braided body can achieve remarkable reinforcing and toughening effects.
2. Compared with the comparative example 2, the embodiment 1-3 shows that the technical scheme of the invention introduces the chopped carbon fibers, and vertically tamps the chopped carbon fibers up and down in the meshes of the braided body by using the blunt metal rod to vertically distribute part of the chopped carbon fibers, thereby achieving the effects of strengthening and toughening.
3. Compared with the comparative example 3, the embodiment 1-3 shows that the technical scheme of the invention has the advantages that the nano silicon component and the nano carbon powder are coated on the carbon fiber braided body tows and react in situ to generate the silicon carbide, so that the carbon fibers can be protected from being corroded by molten silicon, the strength of the carbon fibers cannot be reduced, the interface bonding strength of the carbon fibers and a silicon carbide ceramic matrix is improved, and the reinforcing and toughening effects are better played.
4. Compared with the comparative example 4, the embodiment 1-3 shows that the technical scheme of the invention utilizes the carbon fiber woven body with meshes to toughen, is beneficial to the combination of the silicon carbide ceramic matrix and the reinforced carbon fibers, avoids layering, and thus better plays a role in strengthening and toughening.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The manufacturing method of the reaction sintering silicon carbide ceramic grinding disc is characterized in that raw materials for preparing the grinding disc comprise a matrix material and a toughening material; the matrix material comprises, by mass, 100 parts of silicon carbide micro powder, 5-15 parts of carbon powder, 5-15 parts of adhesive, 0.5-3 parts of surfactant and 0.5-2 parts of dispersant; the toughening material is a chopped carbon fiber and carbon fiber woven body, and the addition amount of the carbon fiber is 0-15% of the total amount of the matrix material;
the manufacturing method specifically comprises the following steps:
(1) Preparation of granulated powder
Weighing the matrix material according to the proportion, adding deionized water, wherein the using amount of the deionized water is 0.9-1.5 times of the mass of the silicon carbide micro powder, and then carrying out ball milling for 8-20 hours to prepare silicon carbide ceramic slurry; then, carrying out spray granulation on the silicon carbide ceramic slurry to obtain granulated powder; the water content of the granulated powder is 0.5-1.2%, and the mass ratio of the granulated powder with the granularity of 60-180 meshes is more than 95%;
(2) Adding toughening material
Adding short carbon fibers into the granulated powder, and mixing by using a vibrating screen; wherein the length of the chopped carbon fiber is 3-10mm, and the diameter of the tow is less than 500 mu m;
(3) Impregnation treatment of carbon fiber woven body
Weaving carbon fibers into a carbon fiber woven body with a two-dimensional mesh structure, wherein the value range of the length and the width of meshes is 3-50mm, and the diameter of tows of the carbon fiber woven body is less than 2000 mu m; then dipping the carbon fiber bundles in the mixed slurry to ensure that the surface of the carbon fiber bundles is fully distributed with the mixed slurry, wherein the mixed slurry is obtained by mixing nano carbon powder, nano silicon powder, a bonding agent, a dispersing agent and deionized water through wet ball milling for 8-20 hours; the molar ratio of the nano carbon powder to the nano silicon powder is 1:1.05-1.25 percent, the addition of the adhesive is 2-10 percent of the total mass of the nano carbon powder and the nano silicon powder, the addition of the dispersant is 0.5-3 percent of the total mass of the nano carbon powder and the nano silicon powder, and the ratio of the deionized water to the total mass of the nano carbon powder and the nano silicon powder is 1.0-2.0:1; wherein D of the nano carbon powder and the nano silicon powder 50 Are not more than 100nm;
then placing the carbon fiber woven body in a vacuum drying oven, placing the carbon fiber woven body for 5-20h at the temperature of 25-35 ℃, and then heating to 60-80 ℃ for drying for 10-30h to dry the carbon fiber woven body; soaking the dried carbon fiber woven body in the mixed slurry again, and repeating the steps for multiple times to uniformly coat a layer of mixed slurry on the surface of the dried carbon fiber woven body; preserving the heat of the dried impregnated carbon fiber woven body in a vacuum furnace at 1430-1600 ℃ for 1-6 hours;
(4) Preforming of abrasive disk blanks
Laying a layer of silicon carbide granulation powder added with short carbon fibers in a mould, compacting and flattening the silicon carbide granulation powder on a vibration platform, laying a soaked carbon fiber woven body, laying a layer of silicon carbide granulation powder added with short carbon fibers, and vertically tamping the carbon fiber woven body by using a blunt metal rod, wherein the tip diameter of the metal rod is smaller than the mesh size of the carbon fiber woven body;
molding the mold after vibrating compaction and flattening to obtain a preformed blank of the grinding disc, performing cold isostatic pressing on the preformed blank after packaging and vacuumizing, wherein the pressure of the cold isostatic pressing is 60-150MPa, the pressure maintaining time is 5-30min, and the green density of the blank of the grinding disc is controlled to be 1.80-2.10g/cm 3 ；
(5) Machining of abrasive disk blanks
Drying the grinding disc blank formed by cold isostatic pressing at 80-150 ℃ for 8-20 hours; then turning to obtain a flat surface and required appearance and size, and machining a groove with required shape and size on the working surface according to the requirement;
(6) Sintering of abrasive disk blanks
Placing the processed grinding disc blank in a vacuum sintering furnace, paving metal silicon particles below and on the side surface of the grinding disc, smearing a thin layer of boron nitride slurry on a groove on the working surface of the grinding disc to prevent the groove from being damaged by the silicon particles, wherein the silicon consumption is 0.8-2.0 times of the mass of the grinding disc blank, and preserving heat at 1450-1800 ℃ for 1-8 hours to prepare a grinding disc sintered body;
(7) Manufacture of abrasive discs
And grinding, lapping and polishing the sintered body of the lapping disc to obtain the silicon carbide ceramic lapping disc with required specification, shape, size and flatness.
2. The method for manufacturing the reaction-sintered silicon carbide ceramic grinding disk according to claim 1, wherein the carbon fiber woven body and the chopped carbon fibers are high-strength carbon fibers having a tensile strength of not less than 2500MPa.
3. The method for manufacturing the reaction-sintered silicon carbide ceramic grinding disk according to claim 1, wherein the silicon carbide micro powder is prepared from D 50 Silicon carbide micropowder of 3 to 10 μm, D 50 15-30 μm of silicon carbide micropowder and D 50 Silicon carbide micro powder with the particle size of 40-60 mu m is prepared by the following raw materials in percentage by mass (3-8): (2-4): 1, and mixing the components in a ratio of 1.
4. The method of claim 1, wherein the binder is phenolic resin, polyvinyl alcohol, or carboxymethyl cellulose.
5. The method for manufacturing the reaction-sintered silicon carbide ceramic grinding disk according to claim 1, wherein the surfactant is stearic acid or fatty glyceride; the dispersant is tetramethyl ammonium hydroxide or polyacrylic acid.
6. The method for manufacturing a reaction-sintered silicon carbide ceramic grinding disk according to claim 1, wherein D is the amount of the carbon powder 50 Less than 200nm.
7. The method for manufacturing a reaction-sintered silicon carbide ceramic grinding disk according to claim 1, wherein the dispersant in the step (3) is polyvinylpyrrolidone or tetramethylammonium hydroxide.
8. The method for manufacturing a reaction-sintered silicon carbide ceramic abrasive disk according to claim 1, wherein the binder in the step (3) is polyvinyl alcohol or carboxymethyl cellulose.
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