CN113185302A - Large-size silicon nitride ceramic ball for wind power generation and preparation method and application thereof - Google Patents
Large-size silicon nitride ceramic ball for wind power generation and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a large-size silicon nitride ceramic ball for wind power generation and a preparation method and application thereof, and relates to the technical field of wind power generation. According to the invention, the silicon nitride ceramic ball is prepared by adopting hot-pressing sintering, the hot-pressing sintering method has the effect of mechanical pressurization at high temperature, the sintering driving force can be improved, and the densification is promoted, so that the content of the required sintering aid is low, the oxynitride liquid phase formed by the reaction of the sintering aid and the surface substance of particles during sintering is less, and the glass phase left between grain boundaries after sintering is less, thereby being beneficial to improving the fatigue life of the silicon nitride ceramic ball; the prepared silicon nitride ceramic ball has uniform density, high hardness, strong fracture toughness, good batch stability, simple and efficient generation process and low cost, and can avoid the problems of deformation, cracking and the like.
Description
Technical Field
The invention relates to the technical field of wind power generation, in particular to a large-size silicon nitride ceramic ball for wind power generation and a preparation method and application thereof.
Background
In recent years, wind power has received increasing attention worldwide as one of clean, pollution-free renewable energy sources. With the transformation and upgrading of the energy structure in China, the development and construction scale of wind power is larger, the installed capacity of the wind power generator is increased year by year, and the continuous and safe operation of the wind power generator provides a solid guarantee for the transformation of the energy structure. The rolling bearing is one of key components of a transmission device of a wind turbine generator, generally works in severe environments such as low speed, heavy load and gust, the running state of the rolling bearing directly influences the safe and stable running of the wind turbine generator, the rolling bearing breaks down to generate great influence on the running state of the whole rotating machine and even the whole fan, and the whole wind turbine generator is stopped in serious conditions.
With the successive investment of domestic high-power grid-connected wind driven generators and the vigorous development of aerospace industry, silicon nitride ceramic bearing balls have strong market demands at home and abroad. The silicon nitride ceramic ball has excellent performances of light weight, self-lubrication, high elastic modulus, corrosion resistance, insulation, no magnetism, thermal shock resistance, oxidation resistance and the like, and the mechanical property below 900 ℃ is almost unchanged, so the silicon nitride ceramic ball is widely applied to the field of high-speed, high-precision and long-life bearings of aviation and aerospace engines, wind driven generators and the like. The bearing adopting silicon nitride (phi is more than or equal to 30mm) as the material of the rolling body has the characteristics of light weight, low friction loss, strong dry running capability and the like, and can effectively prolong the service life of the wind turbine generator.
At present, a series of problems exist in the preparation process of large-size silicon nitride ceramic balls (phi 30-101.6 mm), the forming difficulty is high, the formed biscuit balls need manual ball repair, the density gradient of the ball blanks is not uniform, and therefore the problems of deformation, cracking and the like easily occur in the sintering process, the preparation cost of the large-size silicon nitride ceramic balls is high, and the batch stability is poor. Therefore, the development of a production process suitable for large-size silicon nitride ceramic balls is realized, and the efficient batch preparation of the silicon nitride ceramic balls is of great significance for accelerating the localization process of key components of the high-power grid-connected wind power generator.
Disclosure of Invention
The invention aims to provide a large-size silicon nitride ceramic ball for wind power generation and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a large-size silicon nitride ceramic ball for wind power generation, which comprises the following steps:
mixing silicon nitride, a sintering aid and an organic solvent, and performing ball milling and mixing to obtain mixed slurry; the mass percent of the silicon nitride is 95-99%, and the mass percent of the sintering aid is 1-5% based on 100% of the total mass of the silicon nitride and the sintering aid;
carrying out spray granulation on the mixed slurry to obtain spray granulation powder;
placing the spray granulation powder in a spherical sintering mold, and performing hot-pressing sintering to obtain a ceramic blank ball;
finely processing the ceramic blank ball to obtain a large-size silicon nitride ceramic ball for wind power generation;
the diameter of the large-size silicon nitride ceramic ball for wind power generation is 30-101.6 mm.
Preferably, the silicon nitride has a particle size distribution in which the cumulative volume fraction of the particle size distribution is 50% and the cumulative volume fraction corresponds to the particle size D501.5 μm, in which silicon nitride, α -Si3N4The content is 95%, and the purity of the silicon nitride is 99.9%.
Preferably, the sintering aid comprises one or more of magnesium oxide, aluminum oxide, yttrium oxide, zirconium oxide, lanthanum oxide, cerium oxide and neodymium oxide.
Preferably, the rotation speed of the ball milling and mixing is 100-400 r/min, and the time is 6-24 h.
Preferably, the inlet temperature of a spray granulation tower for spray granulation is 190-200 ℃, the aperture of a spray sheet is 0.7-0.9 mm, and the particle size of spray granulation powder is 50-100 mu m.
Preferably, the sintering temperature of the hot-pressing sintering is room temperature to 1850 ℃, the sintering pressure is 15 to 25MPa, and the total sintering time is 7 to 11 hours; the temperature rise rate in the sintering process is 1-15 ℃/min.
Preferably, the procedure of hot press sintering comprises: the first stage is as follows: heating the mixture from room temperature to 900 ℃ for 80-120 min; and a second stage: heating from 900 ℃ to 1200 ℃ for 60-100 min; and a third stage: heating from 1200 ℃ to 1500 ℃ for 120-150 min; a fourth stage: preserving heat for 30-60 min at 1500 ℃; the fifth stage: heating from 1500 ℃ to 1700 ℃, wherein the time is 80-100 min; the sixth stage: heating from 1700 ℃ to 1850 ℃ for 60-100 min.
Preferably, the finishing comprises coarse grinding, fine grinding, finish grinding, lapping and ultra lapping which are carried out in sequence.
The invention provides a large-size silicon nitride ceramic ball for wind power generation, which is prepared by the preparation method in the technical scheme.
The invention provides application of the large-size silicon nitride ceramic ball for wind power generation in a wind power generator bearing.
The invention provides a preparation method of a large-size silicon nitride ceramic ball for wind power generation, which comprises the following steps: mixing silicon nitride, a sintering aid and an organic solvent, and performing ball milling and mixing to obtain mixed slurry; the mass percent of the silicon nitride is 95-99%, and the mass percent of the sintering aid is 1-5% based on 100% of the total mass of the silicon nitride and the sintering aid; carrying out spray granulation on the mixed slurry to obtain spray granulation powder; placing the spray granulation powder in a spherical sintering mold, and performing hot-pressing sintering to obtain a ceramic blank ball; finely processing the ceramic blank ball to obtain a large-size silicon nitride ceramic ball for wind power generation; the diameter of the large-size silicon nitride ceramic ball for wind power generation is 30-101.6 mm. The silicon nitride ceramic ball is prepared by hot-pressing sintering, the hot-pressing sintering method has the effect of mechanical pressurization at high temperature, the sintering driving force can be improved, and densification is promoted, so that the content of the required sintering aid is low, the oxynitride liquid phase formed by the reaction of the sintering aid and a particle surface substance during sintering is less, and the glass phase left between grain boundaries after sintering is less, so that the grain boundary phase and the glass phase of the obtained silicon nitride ceramic material are less, the purity of the silicon nitride ceramic ball is high, and the fatigue life and the reliability of the wind power generation bearing can be effectively improved.
The invention utilizes spray granulation to prevent the components in the mixed slurry from agglomerating, settling and layering, and obtains spray granulation powder with regular particle appearance, uniform particle size distribution, good fluidity and proper apparent density by controlling the volatilization rate of the solvent on the surface of the particles, thereby improving the performance of a powder filling mould and improving the density and uniformity of a biscuit.
The invention uses the spray granulation powder for hot-pressing sintering, does not need a forming agent, can improve the powder fluidity and the mold filling density, simultaneously can avoid the step of removing the forming agent after the ceramic ball is formed, saves the process time, reduces the impurity content of the ceramic ball, and further improves the mechanical property of the ceramic ball.
The spherical sintering mold is used, the bottleneck that the traditional mold for hot-pressing sintering is simple in shape and only can be used for preparing products with simple shapes can be overcome, the spherical silicon nitride material is obtained by direct sintering, the silicon nitride ball obtained by processing cylindrical silicon nitride is avoided, the mechanical nonuniformity of the girdle band is reduced, and the density uniformity of the silicon nitride ceramic ball is promoted.
The silicon nitride ceramic ball prepared by the method has the advantages of good batch stability, simple and efficient generation process, low cost and capability of avoiding the problems of deformation, cracking and the like. The results of the examples show that the large-size silicon nitride ceramic balls for wind power generation prepared by the invention have uniform density, the strength of 1240-1310 MPa and the fracture toughness of more than 9 MPa-m1/2Ra is more than or equal to 0.006 and less than or equal to 0.010 in surface roughness, the spherical error is 0.2-0.4, and all performance indexes meet the requirements of GB/T308.2-2010/ISO 3290-2: 2008 "rolling bearing bead part 2: the standard requirement of G20 grade of the standard requirement of silicon nitride ceramic micro-beads.
Drawings
Fig. 1 is a TEM image of the silicon nitride ceramic balls prepared in example 1.
Detailed Description
The invention provides a preparation method of a large-size silicon nitride ceramic ball for wind power generation, which comprises the following steps:
mixing silicon nitride, a sintering aid and an organic solvent, and performing ball milling and mixing to obtain mixed slurry; the mass percent of the silicon nitride is 95-99%, and the mass percent of the sintering aid is 1-5% based on 100% of the total mass of the silicon nitride and the sintering aid;
carrying out spray granulation on the mixed slurry to obtain spray granulation powder;
placing the spray granulation powder in a spherical sintering mold, and performing hot-pressing sintering to obtain a ceramic blank ball;
finely processing the ceramic blank ball to obtain a large-size silicon nitride ceramic ball for wind power generation;
the diameter of the large-size silicon nitride ceramic ball for wind power generation is 30-101.6 mm.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
According to the invention, silicon nitride, a sintering aid and an organic solvent are mixed, and ball milling and mixing are carried out to obtain mixed slurry. In the present invention, the particle size distribution of the silicon nitride corresponds to a particle size D at a cumulative volume fraction of 50%501.5 μm, in which silicon nitride, α -Si3N4The content is preferably 95%, and the purity of the silicon nitride is preferably 99.9%.
In the present invention, the sintering aid preferably includes one or more of magnesium oxide, aluminum oxide, yttrium oxide, zirconium oxide, lanthanum oxide, cerium oxide, and neodymium oxide; when the sintering aids are preferably selected from the above-mentioned sintering aids, the proportion of the sintering aids of different types is not particularly limited, and the sintering aids can be prepared in any proportion.
In the invention, the total mass of the silicon nitride and the sintering aid is 100%, the mass percent of the silicon nitride is 95-99%, preferably 96-98%, and the mass percent of the sintering aid is 1-5%, preferably 2-4%.
In the present invention, the organic solvent is preferably absolute ethanol; the mass ratio of the organic solvent to the total mass of the silicon nitride and the sintering aid is preferably 2: 1.
In the invention, the grinding medium used for ball milling and mixing is preferably silicon nitride balls; the mass ratio of the silicon nitride ceramic balls to the total mass of the silicon nitride and the sintering aid is preferably 2: 1.
In the present invention, the ball-milling mixing is preferably performed in a ball mill or a stirring mill; the specification of the silicon nitride ball and the specific specification of the ball mill or the stirring mill are not specially limited, and the corresponding equipment well known in the field can be used.
In the invention, the rotation speed of the ball milling mixing is preferably 100-400 r/min, more preferably 200-300 r/min, and the time is preferably 6-24 h, more preferably 10-20 h.
After the mixed slurry is obtained, the mixed slurry is subjected to spray granulation to obtain spray granulation powder. In the invention, the spray granulation is preferably carried out in a spray granulation tower, the inlet temperature of the spray granulation tower for the spray granulation is preferably 190-200 ℃, more preferably 195 ℃, the pore diameter of a spray piece is preferably 0.7-0.9 mm, more preferably 0.8mm, and the particle diameter of the spray granulation powder is preferably 50-100 μm. In the present invention, the specification of the spray granulation tower is not particularly limited, and a spray granulation tower known in the art and capable of satisfying the above conditions may be selected.
The invention utilizes spray granulation to prevent the components in the mixed slurry from agglomerating, settling and layering, and controls the volatilization rate of the solvent on the surface of the particles by controlling the inlet temperature of a spray granulation tower and the aperture of a spray piece, thereby obtaining the spray granulation powder with regular particle appearance, uniform particle size distribution, good fluidity and proper apparent density, further improving the performance of a powder filling mould and improving the density and uniformity of a biscuit.
After the spray granulation powder is obtained, the spray granulation powder is placed in a spherical sintering mold for hot-pressing sintering to obtain the ceramic blank ball. The spherical sintering mold is not particularly limited in the present invention, and the cylindrical sintering mold may be processed into the spherical sintering mold according to a method well known in the art. The spherical sintering mold is used, the bottleneck that the traditional mold for hot-pressing sintering is simple in shape and only can be used for preparing products with simple shapes can be overcome, the spherical silicon nitride material is obtained by direct sintering, the silicon nitride ball obtained by processing cylindrical silicon nitride is avoided, the mechanical nonuniformity of the girdle band is reduced, and the density uniformity of the silicon nitride ceramic ball is promoted.
In the invention, the hot-pressing sintering is preferably carried out under the protection of nitrogen under normal pressure. In the invention, the sintering temperature of the hot-pressing sintering is preferably room temperature to 1850 ℃, the sintering pressure is preferably 15 to 25MPa, more preferably 18 to 22MPa, and the total sintering time is preferably 7 to 11 hours, more preferably 8 to 9 hours; the heating rate in the sintering process is preferably 1-15 ℃/min, and more preferably 5-12 ℃/min.
In the present invention, the procedure of the hot press sintering preferably includes: the first stage is as follows: heating the mixture from room temperature to 900 ℃ for 80-120 min; and a second stage: heating from 900 ℃ to 1200 ℃ for 60-100 min; and a third stage: heating from 1200 ℃ to 1500 ℃ for 120-150 min; a fourth stage: preserving heat for 30-60 min at 1500 ℃; the fifth stage: heating from 1500 ℃ to 1700 ℃, wherein the time is 80-100 min; the sixth stage: heating from 1700 ℃ to 1850 ℃ for 60-100 min.
In the present invention, the procedure of the hot press sintering more preferably includes: the first stage is as follows: heating to 900 deg.C from room temperature for 90 min; and a second stage: heating from 900 deg.C to 1200 deg.C for 60 min; and a third stage: heating from 1200 ℃ to 1500 ℃ for 130 min; a fourth stage: preserving heat for 50min at 1500 ℃; the fifth stage: heating from 1500 deg.C to 1700 deg.C for 90 min; the sixth stage: heating from 1700 deg.C to 1850 deg.C for 80 min.
In the present invention, the hot press sintering is preferably performed in a hot press sintering furnace, and the hot press sintering furnace is not particularly limited in the present invention, and any hot press sintering furnace known in the art that can satisfy the above conditions may be used.
Because of the difficult sintering property of silicon nitride ceramics, the common process adopts liquid phase sintering, a sintering aid is added to improve the sintering driving force and promote densification, the sintering aid reacts with certain parts of the particle surface layer to form an oxynitride liquid phase during high-temperature sintering, and the liquid phase can leave a glass phase between grain boundaries after sintering, so that the fatigue life of ceramic balls can be reduced. According to the invention, the silicon nitride ceramic ball is prepared by hot-pressing sintering, the sintering driving force is improved by utilizing the mechanical pressurization effect of the hot-pressing sintering, and the densification is promoted, so that the content of the required sintering aid is low, the oxynitride liquid phase formed by the reaction of the sintering aid and the particle surface substance during sintering is less, and the glass phase left between grain boundaries after sintering is less, thereby being beneficial to improving the fatigue life of the silicon nitride ceramic ball.
After the ceramic blank ball is obtained, the ceramic blank ball is subjected to finish machining to obtain a large-size silicon nitride ceramic ball for wind power generation; the diameter of the large-size silicon nitride ceramic ball for wind power generation is 30-101.6 mm. In the present invention, the finish machining preferably includes rough grinding, fine grinding, finish grinding, lapping and ultra lapping which are performed in this order. In the invention, the pressure applied between the upper grinding plate and the lower grinding plate for rough grinding is preferably (1-5) × 10KN, more preferably (2-4) × 10 KN; the rotating speed of the lower grinding disc used for coarse grinding is preferably 5-50 r/min, and more preferably 15-35 r/min.
In the invention, the pressure applied between the upper grinding plate and the lower grinding plate for fine grinding is preferably (1-5) × 10KN, more preferably (2-4) × 10 KN; the rotating speed of the lower grinding disc used for fine grinding is preferably 5-50 r/min, and more preferably 15-30 r/min.
In the present invention, the pressure applied between the upper grinding plate and the lower grinding plate for refining is preferably (0.5 to 3) × 10KN, more preferably (1 to 2) × 10 KN; the rotating speed of the lower grinding disc for fine grinding is preferably 5-25 r/min, and more preferably 10-20 r/min.
In the invention, the pressure applied between the upper grinding plate and the lower grinding plate for lapping is preferably (1.0-1.2) × 10 KN; the rotating speed of the lower grinding disc is preferably 5-25 r/min, and more preferably 10-20 r/min.
In the invention, the pressure applied between the upper grinding plate and the lower grinding plate for ultra-finishing is preferably (0.5-3) × 10 KN; the rotating speed of the lower grinding disc for ultra-precision grinding is preferably 5-25 r/min, and more preferably 10-20 r/min.
The components of the device for coarse grinding, fine grinding and ultra-fine grinding are not particularly limited, and corresponding devices well known in the art can be selected.
The invention provides a large-size silicon nitride ceramic ball for wind power generation, which is prepared by the preparation method in the technical scheme. The strength of the large-size silicon nitride ceramic ball for wind power generation prepared by the invention is 1240-1310 MPa, and the fracture toughness is more than 9 MPa.m1/2Ra is more than or equal to 0.006 and less than or equal to 0.010 in surface roughness, the spherical error is 0.2-0.4, and all performance indexes meet the requirements of GB/T308.2-2010/ISO 3290-2: 2008 "rolling bearing bead part 2: the standard requirement of G20 grade of the standard requirement of silicon nitride ceramic micro-beads.
The invention provides application of the large-size silicon nitride ceramic ball for wind power generation in a wind power generator bearing. The method of the present invention is not particularly limited, and the method may be applied according to a method known in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
In the following examples, the particle size distribution of the silicon nitride used corresponds to a particle size D at a cumulative volume fraction of 50%501.5 μm, in which silicon nitride, α -Si3N4The content is 95%, and the purity of the silicon nitride is 99.9%; based on the total mass of the silicon nitride and the sintering aid as 100 percent.
Example 1
Putting a sintering aid (0.5 percent of magnesium oxide and 0.5 percent of yttrium oxide), 99 percent of silicon nitride, absolute ethyl alcohol (the weight is 2 times of the total weight of the sintering aid and the silicon nitride powder) and silicon nitride balls (the weight is 2 times of the total weight of the sintering aid and the silicon nitride powder) into a ball mill for mixing for 24 hours at the rotating speed of 400r/min to obtain mixed slurry;
carrying out spray granulation on the mixed slurry through a spray granulation tower, wherein the inlet temperature of the spray granulation tower is 200 ℃, the aperture of a spray sheet is 0.7mm, and spray granulation powder with the particle size of 50-100 mu m is obtained;
filling the spray granulation powder
The spherical sintering mould is placed in a hot-pressing sintering furnace, nitrogen is adopted for normal pressure protection in the sintering process, the temperature is increased from room temperature to 900 ℃, and the time is 90 min; and a second stage: heating from 900 deg.C to 1200 deg.C for 60 min; and a third stage: heating from 1200 deg.C to 1500 deg.C for 120 min; a fourth stage: preserving heat for 30min at 1500 ℃; the fifth stage: heating from 1500 deg.C to 1700 deg.C for 80 min; the sixth stage: heating from 1700 ℃ to 1850 ℃ for 60min, wherein the total sintering time is 440min and the sintering pressure is 25 MPa;
the ceramic blank ball is subjected to coarse grinding, fine grinding and ultra-fine grinding in sequence, wherein the pressure applied between an upper grinding plate and a lower grinding plate in the coarse grinding process is 5.0 multiplied by 10KN, and the rotating speed of a lower grinding disc is 50 r/min; in the fine grinding procedure, the pressure applied between the upper grinding plate and the lower grinding plate is 5.0 multiplied by 10KN, and the rotating speed of the lower grinding plate is 40 r/min; the pressure applied between the upper grinding plate and the lower grinding plate in the fine grinding procedure is 3.0 multiplied by 10KN, and the rotating speed of the lower grinding disc is 25 r/min; in the lapping procedure, the pressure applied between the upper grinding plate and the lower grinding plate is 1.2 multiplied by 10KN, and the rotating speed of the lower grinding plate is 15 r/min; the pressure applied between the upper and lower grinding plates in the ultra-fine grinding process is 0.8 × 10KN, and the rotation speed of the lower grinding disc is 10r/min to obtain
And (5) obtaining a silicon nitride ceramic ball finished product.
Example 2
Putting a sintering aid (0.5 percent of magnesium oxide and 0.5 percent of aluminum oxide), 99 percent of silicon nitride, absolute ethyl alcohol (the weight is 2 times of the total weight of the sintering aid and the silicon nitride powder) and silicon nitride balls (the weight is 2 times of the total weight of the sintering aid and the silicon nitride powder) into a ball mill for mixing for 24 hours at the rotating speed of 100r/min to obtain mixed slurry;
carrying out spray granulation on the mixed slurry through a spray granulation tower, wherein the inlet temperature of the spray granulation tower is 190 ℃, the aperture of a spray sheet is 0.9mm, and spray granulation powder with the particle size of 50-100 mu m is obtained;
filling the spray granulation powder
The spherical sintering mould is placed in a hot-pressing sintering furnace, nitrogen is adopted for normal pressure protection in the sintering process, the temperature is increased from room temperature to 900 ℃, and the time is 90 min; and a second stage: heating from 900 deg.C to 1200 deg.C for 60 min; and a third stage: heating from 1200 deg.C to 1500 deg.C for 120 min; a fourth stage: preserving heat for 60min at 1500 ℃; the fifth stage: heating from 1500 deg.C to 1700 deg.C for 80 min; the sixth stage: heating from 1700 ℃ to 1850 ℃, wherein the time is 100min, the sintering pressure is 20MPa, and the total sintering time is 510min, so as to obtain a ceramic blank ball;
the ceramic blank ball is subjected to coarse grinding, fine grinding and ultra-fine grinding in sequence, wherein the pressure applied between an upper grinding plate and a lower grinding plate in the coarse grinding process is 4.0 multiplied by 10KN, and the rotating speed of a lower grinding disc is 40 r/min; in the fine grinding procedure, the pressure applied between the upper grinding plate and the lower grinding plate is 4.0 multiplied by 10KN, and the rotating speed of the lower grinding plate is 30 r/min; the pressure applied between the upper grinding plate and the lower grinding plate in the fine grinding procedure is 2.5 multiplied by 10KN, and the rotating speed of the lower grinding disc is 25 r/min; in the lapping procedure, the pressure applied between the upper grinding plate and the lower grinding plate is 1.1 multiplied by 10KN, and the rotating speed of the lower grinding plate is 15 r/min; the pressure applied between the upper and lower grinding plates in the ultra-fine grinding process is 0.7 × 10KN, and the rotation speed of the lower grinding disc is 10r/min to obtain
And (5) obtaining a silicon nitride ceramic ball finished product.
Example 3
Putting a sintering aid (2% of magnesium oxide, 2% of aluminum oxide and 1% of zirconium oxide) and 95% of silicon nitride, absolute ethyl alcohol (the weight is 2 times of the total weight of the sintering aid and the silicon nitride powder) and silicon nitride balls (the weight is 2 times of the total weight of the sintering aid and the silicon nitride powder) into a ball mill for mixing for 24 hours at the rotating speed of 400r/min to obtain mixed slurry;
carrying out spray granulation on the mixed slurry through a spray granulation tower, wherein the inlet temperature of the spray granulation tower is 200 ℃, the aperture of a spray sheet is 0.9mm, and spray granulation powder with the particle size of 50-100 mu m is obtained;
filling the spray granulation powder
The spherical sintering mould is placed in a hot-pressing sintering furnace, nitrogen is adopted for normal pressure protection in the sintering process, the temperature is increased from room temperature to 900 ℃, and the time is 90 min; and a second stage: heating from 900 deg.C to 1200 deg.C for 80 min; and a third stage: heating from 1200 ℃ to 1500 ℃ for 130 min; a fourth stage: preserving heat for 50min at 1500 ℃; the fifth stage: heating from 1500 deg.C to 1700 deg.C for 80 min; the sixth stage: heating from 1700 ℃ to 1850 ℃ for 90min, wherein the total sintering time is 520min and the sintering pressure is 18 MPa;
the ceramic blank ball is subjected to coarse grinding, fine grinding and ultra-fine grinding in sequence, wherein the pressure applied between an upper grinding plate and a lower grinding plate in the coarse grinding process is 4.0 multiplied by 10KN, and the rotating speed of a lower grinding disc is 40 r/min; in the fine grinding procedure, the pressure applied between the upper grinding plate and the lower grinding plate is 4.0 multiplied by 10KN, and the rotating speed of the lower grinding plate is 30 r/min; the pressure applied between the upper grinding plate and the lower grinding plate in the fine grinding procedure is 2.0 multiplied by 10KN, and the rotating speed of the lower grinding disc is 20 r/min; in the lapping procedure, the pressure applied between the upper grinding plate and the lower grinding plate is 1.0 multiplied by 10KN, and the rotating speed of the lower grinding plate is 15 r/min; the pressure applied between the upper and lower grinding plates in the ultra-fine grinding process is 0.6 × 10KN, and the rotation speed of the lower grinding disc is 10r/min to obtain
And (5) obtaining a silicon nitride ceramic ball finished product.
Example 4
Putting a sintering aid (1% of magnesium oxide, 2.5% of aluminum oxide and 1.5% of neodymium oxide), 95% of silicon nitride, absolute ethyl alcohol (the weight is 2 times of the total weight of the sintering aid and the silicon nitride powder) and silicon nitride balls (the weight is 2 times of the total weight of the sintering aid and the silicon nitride powder) into a ball mill for mixing for 24 hours at the rotating speed of 200r/min to obtain mixed slurry;
carrying out spray granulation on the mixed slurry through a spray granulation tower, wherein the inlet temperature of the spray granulation tower is 190 ℃, the aperture of a spray sheet is 0.9mm, and spray granulation powder with the particle size of 50-100 mu m is obtained;
filling the spray granulation powder
The spherical sintering mould is placed in a hot-pressing sintering furnace, nitrogen is adopted for normal pressure protection in the sintering process, the temperature is increased from room temperature to 900 ℃, and the time is 90 min; and a second stage: heating from 900 deg.C to 1200 deg.C for 80 min; and a third stage: heating from 1200 deg.C to 1500 deg.C for 150 min; a fourth stage: preserving heat for 40min at 1500 ℃; the fifth stage: heating from 1500 deg.C to 1700 deg.C for 80 min; the sixth stage: heating from 1700 ℃ to 1850 ℃ for 60min, wherein the total sintering time is 500min and the sintering pressure is 18 MPa;
the ceramic blank ball is subjected to coarse grinding, fine grinding and ultra-fine grinding in sequence, wherein the pressure applied between an upper grinding plate and a lower grinding plate in the coarse grinding process is 3.0 multiplied by 10KN, and the rotating speed of a lower grinding disc is 40 r/min; in the fine grinding procedure, the pressure applied between the upper grinding plate and the lower grinding plate is 3.0 multiplied by 10KN, and the rotating speed of the lower grinding plate is 30 r/min; the pressure applied between the upper grinding plate and the lower grinding plate in the fine grinding procedure is 2.0 multiplied by 10KN, and the rotating speed of the lower grinding disc is 20 r/min; in the lapping procedure, the pressure applied between the upper grinding plate and the lower grinding plate is 1.0 multiplied by 10KN, and the rotating speed of the lower grinding plate is 15 r/min; the pressure applied between the upper and lower grinding plates in the ultra-fine grinding process is 0.6 × 10KN, and the rotation speed of the lower grinding disc is 10r/min to obtain
And (5) obtaining a silicon nitride ceramic ball finished product.
Comparative example 1
Chinese patent (publication No. CN111548163A) carries out system selection through nano modification and particle grading, silicon nitride ceramic balls for large-size wind power generation are prepared through air pressure sintering and hot isostatic pressing sintering, and the hardness of the silicon nitride ceramic balls prepared by the schemes of examples 1-4 is 1465kg/mm2The bending strength is about 800MPa and can not reach the I-grade material standard in F2094-2018 a.
Performance testing
1) TEM tests were performed on the silicon nitride ceramic balls prepared in example 1, and the results are shown in fig. 1; as can be seen from FIG. 1, the silicon nitride ceramic material prepared by the present invention has a small amount of grain boundary phase and glass phase, and the purity of the silicon nitride ceramic balls is high.
2) The silicon nitride ceramic balls prepared in examples 1 to 4 were subjected to performance tests, wherein the density was tested according to the method described in GB/T25995-:
TABLE 1 results of performance tests on silicon nitride ceramic balls prepared in examples 1 to 4
As can be seen from Table 1, the large-size silicon nitride ceramic balls prepared by the method have uniform density, high hardness, strong fracture toughness, good batch stability and the like, and can avoid the problems of deformation, cracking and the like; meanwhile, the performance indexes of the prepared silicon nitride ceramic ball finished product all meet the requirements of GB/T308.2-2010/ISO 3290-2: 2008 "rolling bearing bead part 2: silicon nitride ceramic beads "standard requirements grade G20 (see table 2).
TABLE 2G 20 Standard requirements
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of large-size silicon nitride ceramic balls for wind power generation is characterized by comprising the following steps:
mixing silicon nitride, a sintering aid and an organic solvent, and performing ball milling and mixing to obtain mixed slurry; the mass percent of the silicon nitride is 95-99%, and the mass percent of the sintering aid is 1-5% based on 100% of the total mass of the silicon nitride and the sintering aid;
carrying out spray granulation on the mixed slurry to obtain spray granulation powder;
placing the spray granulation powder in a spherical sintering mold, and performing hot-pressing sintering to obtain a ceramic blank ball;
finely processing the ceramic blank ball to obtain a large-size silicon nitride ceramic ball for wind power generation;
the diameter of the large-size silicon nitride ceramic ball for wind power generation is 30-101.6 mm.
2. The method according to claim 1, wherein the silicon nitride has a particle size distribution in which the cumulative volume fraction of the particle size D is 50% of the particle size D501.5 μm, in which silicon nitride, α -Si3N4The content is 95%, and the purity of the silicon nitride is 99.9%.
3. The method of claim 1, wherein the sintering aid comprises one or more of magnesium oxide, aluminum oxide, yttrium oxide, zirconium oxide, lanthanum oxide, cerium oxide, and neodymium oxide.
4. The preparation method of claim 1, wherein the rotation speed of the ball milling and mixing is 100-400 r/min, and the time is 6-24 h.
5. The method according to claim 1, wherein the inlet temperature of a spray granulation tower used for spray granulation is 190 to 200 ℃, the pore diameter of a spray sheet is 0.7 to 0.9mm, and the particle diameter of the spray granulated powder is 50 to 100 μm.
6. The preparation method according to claim 1, wherein the sintering temperature of the hot-press sintering is room temperature to 1850 ℃, the sintering pressure is 15 to 25MPa, and the total sintering time is 7 to 11 h; the temperature rise rate in the sintering process is 1-15 ℃/min.
7. The production method according to claim 1 or 6, wherein the procedure of the hot press sintering includes: the first stage is as follows: heating the mixture from room temperature to 900 ℃ for 80-120 min; and a second stage: heating from 900 ℃ to 1200 ℃ for 60-100 min; and a third stage: heating from 1200 ℃ to 1500 ℃ for 120-150 min; a fourth stage: preserving heat for 30-60 min at 1500 ℃; the fifth stage: heating from 1500 ℃ to 1700 ℃, wherein the time is 80-100 min; the sixth stage: heating from 1700 ℃ to 1850 ℃ for 60-100 min.
8. The production method according to claim 1, wherein the finishing comprises rough grinding, fine grinding, finish grinding, lapping and ultra lapping which are performed in this order.
9. The large-size silicon nitride ceramic balls for wind power generation prepared by the preparation method of any one of claims 1 to 8.
10. Use of the large-sized silicon nitride ceramic balls for wind power generation according to claim 9 in a bearing of a wind power generator.
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