CN116444277A - Preparation method of oversized silicon nitride ceramic ball for oversized bearing - Google Patents
Preparation method of oversized silicon nitride ceramic ball for oversized bearing Download PDFInfo
- Publication number
- CN116444277A CN116444277A CN202210015042.7A CN202210015042A CN116444277A CN 116444277 A CN116444277 A CN 116444277A CN 202210015042 A CN202210015042 A CN 202210015042A CN 116444277 A CN116444277 A CN 116444277A
- Authority
- CN
- China
- Prior art keywords
- oversized
- ball
- silicon nitride
- nitride ceramic
- sintering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 55
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 45
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000000843 powder Substances 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000005469 granulation Methods 0.000 claims abstract description 14
- 230000003179 granulation Effects 0.000 claims abstract description 14
- 239000007921 spray Substances 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 8
- 210000001161 mammalian embryo Anatomy 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 13
- 238000005229 chemical vapour deposition Methods 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- 238000009966 trimming Methods 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 8
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 7
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 5
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 abstract description 7
- 238000003825 pressing Methods 0.000 abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000006104 solid solution Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000003863 physical function Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3856—Carbonitrides, e.g. titanium carbonitride, zirconium carbonitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
- C04B2235/445—Fluoride containing anions, e.g. fluosilicate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a preparation method of an oversized silicon nitride ceramic ball for an oversized bearing. The method is carried out by weighing 6wt% MgSiN 2 ‑YbF 3 、94wt％β‑Si 3 N 4 Premixing the powder to achieve the aim of uniform mixing; ball milling the obtained materials with absolute ethyl alcohol as a medium for evenly mixing for 15-20 h, wherein the ball milling speed is 90-120 rpm, and drying for 4-5 h at 65-75 ℃ through a rotary evaporator; atomizing the obtained material by closed spray granulation to obtain the product with particle diameter of 50-100 μm and apparent density of 0.85g/cm 3 ～0.90g/cm 3 Is a uniform powder material; placing the powder into ball grinding tool, pre-pressing under 40-45 MPa to obtain ceramic ball green body, and mixingCutting off redundant parts of the green embryo to repair the green embryo; carrying out cold isostatic pressing forming on the green embryo under the condition of 280-300 MPa; the obtained blank ball is placed into a pneumatic sintering furnace for sintering treatment, and sintered for 1-2 h at 1850-2000 ℃ and the nitrogen pressure is 9-12 MPa, so that the large-size silicon nitride ceramic ball is prepared.
Description
Technical Field
The invention relates to the technical field of preparation of silicon nitride ceramic balls, in particular to a preparation method of an oversized silicon nitride ceramic ball for an oversized bearing.
Background
The silicon nitride has higher hardness and strength as a ceramic structure, good corrosion resistance and oxidation resistance, small high-temperature-resistant density and small expansion coefficient, and is suitable for being used as a key structural material with high fatigue life and high precision requirement. Silicon nitride has brittleness, and due to the limitation of a sintering process, the quality of a large-size silicon nitride ceramic structure product is unstable, and the problems of deformation, uneven density and the like are easy to occur. And the performances of the ceramic balls of the domestic silicon nitride ceramic balls and the imported silicon nitride ceramic balls are different to a certain extent, so that a more mature sintering method of the silicon nitride substrate is necessary to be provided to solve the problems.
Disclosure of Invention
The invention aims to provide a preparation method of oversized silicon nitride ceramic balls for oversized bearings, which aims to solve the problems of easy deformation, non-compactness and the like of the existing oversized silicon nitride ceramic balls in the domestic market in the sintering process.
The invention provides a preparation method of an oversized silicon nitride ceramic ball for an oversized bearing, which comprises the following steps:
step one, weighing 6 weight percent MgSiN 2 -YbF 3 、94wt％β-Si 3 N 4 Premixing the powder to achieve the aim of uniform mixing;
step two, absolute ethyl alcohol is used as a medium, the materials obtained in the step one are ball-milled and evenly mixed for 15-20 h, the ball milling speed is 90-120 r/min, and the materials are dried for 4-5 h at 65-75 ℃ through a rotary evaporator;
step three, atomizing the material obtained in the step two by closed spray granulation to obtain the material with the particle size of 50-100 microns and the bulk density of 0.85g/cm 3 ～0.90g/cm 3 Is a uniform powder material;
step four, placing the powder into a ball grinding tool for prepressing under 40-45 MPa to prepare ceramic ball blanks, and trimming the blanks by cutting off redundant parts;
step five, performing cold isostatic pressing molding on the green embryo under the condition of 280-300 MPa;
step six, placing the blank ball obtained in the step five into a pneumatic sintering furnace for sintering treatment, and sintering for 1-2 h at 1850-2000 ℃ with the nitrogen pressure of 9-12 MPa.
In the second step, absolute ethyl alcohol is used as a medium, the materials obtained in the first step are ball-milled and uniformly mixed for 18 hours, the ball milling speed is 100 revolutions per minute, and the materials are dried for 4.5 hours at 70 ℃ through a rotary evaporator.
Further, in the third step, the material obtained in the second step is atomized through closed spray granulation to obtain the material with the particle size of 80 microns and the bulk density of 0.88g/cm 3 Is a uniform powder of (a).
In the fourth step, the powder is placed into a ball grinding tool to be pre-pressed under 42MPa, a ceramic ball green body is manufactured, and redundant parts of the green body are cut off for shaping.
In the fifth step, the green body is subjected to cold isostatic pressing under 290 MPa.
In the sixth step, the blank ball obtained in the fifth step is put into a pneumatic sintering furnace to be sintered, and the blank ball is sintered for 1.5 hours at the temperature of 1900 ℃ and the nitrogen pressure is 10MPa.
Further, the method further comprises the following steps: and step seven, depositing a silicon carbide layer on the surface of the silicon nitride ceramic ball obtained in the step six by adopting chemical vapor deposition.
In the seventh step, the silicon nitride ceramic balls are added into a reactor, and methyl trichlorosilane, argon and hydrogen are introduced into the reactor to react for 4 to 6 hours at the temperature of 1200 to 1500 ℃.
In the seventh step, the silicon nitride ceramic balls are added into a reactor, and methyltrichlorosilane, argon and hydrogen are introduced into the reactor to react for 5 hours at the temperature of 1300 ℃.
In the sixth step, when the blank ball obtained in the fifth step is placed into a gas pressure sintering furnace to perform sintering treatment, the sintering aid is one or more of yttrium oxide, magnesium oxide, aluminum oxide and tungsten carbide.
The invention has the following beneficial effects: the invention provides oversized silicon nitride for an oversized bearingCeramic balls are prepared by weighing 6wt% MgSiN 2 -YbF 3 、94wt％β-Si 3 N 4 Premixing the powder to achieve the aim of uniform mixing; ball milling the obtained materials with absolute ethyl alcohol as a medium for evenly mixing for 15-20 h, wherein the ball milling speed is 90-120 rpm, and drying for 4-5 h at 65-75 ℃ through a rotary evaporator; atomizing the obtained material by closed spray granulation to obtain the product with particle diameter of 50-100 μm and apparent density of 0.85g/cm 3 ～0.90g/cm 3 Is a uniform powder material; placing the powder into a ball grinding tool for prepressing under 40-45 MPa to prepare ceramic ball blanks, and trimming the blanks by cutting off redundant parts; carrying out cold isostatic pressing forming on the green embryo under the condition of 280-300 MPa; the obtained blank ball is placed into a pneumatic sintering furnace for sintering treatment, and sintered for 1-2 h at 1850-2000 ℃ and the nitrogen pressure is 9-12 MPa, so that the large-size silicon nitride ceramic ball is prepared.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for preparing oversized silicon nitride ceramic balls for oversized bearings.
Detailed Description
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The invention will be described in detail below with reference to the drawings in connection with embodiments. It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
Referring to fig. 1, an embodiment of the invention provides a method for preparing oversized silicon nitride ceramic balls for oversized bearings, which includes the following steps:
step one, weighing 6 weight percent MgSiN 2 -YbF 3 、94wt％β-Si 3 N 4 The powder is premixed to achieve the purpose of uniform mixing.
And step two, taking absolute ethyl alcohol as a medium, ball-milling the material obtained in the step one, uniformly mixing for 15-20 h, wherein the ball-milling speed is 90-120 r/min, and drying for 4-5 h at 65-75 ℃ through a rotary evaporator.
Step three, atomizing the material obtained in the step two by closed spray granulation to obtain the material with the particle size of 50-100 microns and the bulk density of 0.85g/cm 3 ～0.90g/cm 3 Is a uniform powder of (a).
Specifically, closed spray granulation refers to a granulation method in which slurry or solution is sprayed into a granulation tower, and the slurry or solution is dried and agglomerated under the action of spray hot air, so as to obtain spherical granules. The process is widely used to produce catalysts of various particle sizes or other particles of desired particle size. The method is suitable for experiments and small-scale production, and has the advantages of good precision of the particle balls and uniform particles.
And fourthly, placing the powder into a ball grinding tool for prepressing under 40-45 MPa to prepare ceramic ball blanks, and trimming the blanks after cutting off redundant parts.
And fifthly, carrying out cold isostatic pressing molding on the green embryo under the condition of 280-300 MPa.
Specifically, the cold isostatic pressing is a molding process in which a rubber film filled with powder is placed in a closed container, the same pressure is applied to the rubber film by an oil pump, and a compact green body is prepared under the action of high pressure.
Step six, placing the blank ball obtained in the step five into a pneumatic sintering furnace for sintering treatment, and sintering for 1-2 h at 1850-2000 ℃ with the nitrogen pressure of 9-12 MPa.
Specifically, the sintering aid is one or more of yttrium oxide, magnesium oxide, aluminum oxide and tungsten carbide. When the sintering aid is capable of forming a solid solution with the sinter, the lattice will be distorted and activated. The sintering temperature can be reduced, which increases the diffusion and sintering rate, which is particularly strong for the formation of vacancy or interstitial solid solutions. Thus, for a high temperature oxide sintering process in which the diffusion mechanism is controlled, a sintering aid is selected that has a similar radius to the cation of the sinter but a different electricity price to form an absent solid solution; or the selection of smaller radius cations to form interstitial solid solutions will generally aid sintering. Some oxides undergo a crystal form transformation during sintering with a large volume effect, which makes sintering densification difficult and easily causes cracking of the green body. In this case, sintering can be promoted by selecting an appropriate sintering aid for suppression. The mechanism is that a certain amount of CaO and MgO are added during the sintering of ZrO 2. At around 1200 ℃, the stable monoclinic ZrO2 turns into tetragonal ZrOz with a volume shrinkage of about 10%, deteriorating the stability of the article. Ca2+ (or Mg2+) with low cost ratio of Zr4+ is introduced, so that a cubic stable solid solution of Zr1-xCaxO2 can be formed. This both prevents cracking of the article and increases the concentration of vacancies in the crystal to accelerate sintering. The crystal grain growth in the later sintering stage plays an important role in sintering densification. However, if the secondary recrystallization or intermittent grain growth is too fast, the grain coarsening and the grain boundary widening cause the occurrence of the densification phenomenon and affect the microstructure of the product. At this time, the densification process may be promoted by adding a sintering aid that can suppress abnormal growth of crystal grains. The addition of small amounts of MgO to Al2O3, as mentioned above, for example, has this effect. At this time, magnesia-alumina spinel formed by MgO and Al2O3 is distributed among Al2O3 grains, and thus grain growth is suppressed and elimination of pores is promoted, so that it is possible to obtain a sufficiently dense transparent alumina polycrystal. If a proper liquid phase exists during sintering, the particle rearrangement and mass transfer process is often greatly promoted. Another mechanism of action of the sintering aid is that a liquid phase can be generated at lower temperatures to facilitate sintering. The presence of a liquid phase may be a lower melting point of the sintering aid itself; multiple eutectic mixtures with sinter are also possible. For example, a small amount CaO, srO, ti02 is added to BeO; the former is to add a small amount of V205 or CuO, etc. to MgO; when mixed sintering aids such as CaO and TiO2, mnO and TiO2, siO2 and CaO are added into Al2O3, the two functions are combined, so that the sintering can be more effectively accelerated.
And step seven, depositing a silicon carbide layer on the surface of the silicon nitride ceramic ball obtained in the step six by adopting chemical vapor deposition.
Specifically, chemical vapor deposition mainly uses one or more vapor compounds or simple substances containing thin film elements to perform chemical reaction on the surface of a substrate to generate a thin film. Chemical vapor deposition is a new technology developed over the last decades to produce inorganic materials. Chemical vapor deposition has been widely used to purify materials, develop new crystals, deposit various single crystal, polycrystalline or glassy inorganic thin film materials. These materials may be oxides, sulfides, nitrides, carbides, binary or multi-element inter-compounds in groups III-V, II-IV, IV-VI, and their physical functions may be precisely controlled by vapor phase doping deposition processes. In the seventh step, the silicon nitride ceramic balls are added into a reactor, and methyl trichlorosilane, argon and hydrogen are introduced into the reactor to react for 4 to 6 hours at the temperature of 1200 to 1500 ℃.
The method for preparing the oversized silicon nitride ceramic ball for the oversized bearing of the present invention is described below by means of several specific examples.
Example 1
Weighing 6wt% MgSiN 2 -YbF 3 、94wt％β-Si 3 N 4 The powder is premixed to achieve the purpose of uniform mixing. And (3) taking absolute ethyl alcohol as a medium, ball-milling the obtained materials, uniformly mixing for 18 hours, wherein the ball-milling speed is 100 revolutions per minute, and drying for 4.5 hours at 70 ℃ through a rotary evaporator. Atomizing the obtained material by closed spray granulation to obtain the product with the particle diameter of 80 microns and the apparent density of 0.88g/cm 3 Is a uniform powder of (a). And (3) placing the powder into a ball grinding tool for 42MPa pre-pressing to prepare ceramic ball blanks, and cutting off redundant parts of the blanks for trimming. The green body was cold isostatic pressed under 290 MPa. And (3) putting the obtained blank balls into a pneumatic sintering furnace for sintering treatment, wherein the sintering auxiliary agents are yttrium oxide and magnesium oxide, and sintering is carried out for 1.5 hours at the temperature of 1900 ℃ and the nitrogen pressure is 10MPa. Depositing a silicon carbide layer on the surface of the silicon nitride ceramic ball by adopting chemical vapor deposition: nitrogen is added toAdding silicon carbide ceramic balls into a reactor, introducing methyltrichlorosilane, argon and hydrogen into the reactor, and reacting for 5 hours at the temperature of 1300 ℃.
Example two
Weighing 6wt% MgSiN 2 -YbF 3 、94wt％β-Si 3 N 4 The powder is premixed to achieve the purpose of uniform mixing. And (3) taking absolute ethyl alcohol as a medium, ball-milling the obtained materials, uniformly mixing for 15 hours, wherein the ball-milling speed is 90 revolutions per minute, and drying for 4 hours at 65 ℃ through a rotary evaporator. Atomizing the obtained material by closed spray granulation to obtain the product with the particle diameter of 50 microns and the apparent density of 0.85g/cm 3 Is a uniform powder of (a). And (3) placing the powder into a ball grinding tool for prepressing under 40MPa to prepare ceramic ball blanks, and cutting off redundant parts of the blanks for trimming. The green body was cold isostatic pressed under 280 MPa. The obtained blank ball is put into a gas pressure sintering furnace for sintering treatment, wherein the sintering auxiliary agent is alumina and tungsten carbide, and the blank ball is sintered for 1h at 1850 ℃ and the nitrogen pressure is 9MPa. Depositing a silicon carbide layer on the surface of the silicon nitride ceramic ball by adopting chemical vapor deposition: adding silicon nitride ceramic balls into a reactor, introducing methyltrichlorosilane, argon and hydrogen into the reactor, and reacting for 4 hours at the temperature of 1200 ℃.
Example III
Weighing 6wt% MgSiN 2 -YbF 3 、94wt％β-Si 3 N 4 The powder is premixed to achieve the purpose of uniform mixing. And (3) taking absolute ethyl alcohol as a medium, ball-milling the obtained materials, uniformly mixing for 20 hours, wherein the ball-milling speed is 120 r/min, and drying for 5 hours at 75 ℃ through a rotary evaporator. Atomizing the obtained material by closed spray granulation to obtain the product with the particle diameter of 100 micrometers and the apparent density of 0.9g/cm 3 Is a uniform powder of (a). Placing the powder into a ball grinding tool for 45MPa pre-pressing to prepare ceramic ball blanks, and cutting off redundant parts of the blanks for trimming. The green body was cold isostatic pressed under 300 MPa. And (3) putting the obtained blank balls into a pneumatic sintering furnace for sintering treatment, wherein sintering aids are yttrium oxide, magnesium oxide, aluminum oxide and tungsten carbide, and sintering for 2 hours at 2000 ℃ under the nitrogen pressure of 12MPa. Depositing a silicon carbide layer on the surface of the silicon nitride ceramic ball by adopting chemical vapor deposition: silicon nitride ceramicsBall was added to the reactor, and methyltrichlorosilane, argon and hydrogen were introduced into the reactor and reacted at 1500 ℃ for 6h.
From the above examples, the invention provides a method for preparing oversized silicon nitride ceramic balls for oversized bearings by weighing 6wt% of MgSiN 2 -YbF 3 、94wt％β-Si 3 N 4 Premixing the powder to achieve the aim of uniform mixing; ball milling the obtained materials with absolute ethyl alcohol as a medium for evenly mixing for 15-20 h, wherein the ball milling speed is 90-120 rpm, and drying for 4-5 h at 65-75 ℃ through a rotary evaporator; atomizing the obtained material by closed spray granulation to obtain the product with particle diameter of 50-100 μm and apparent density of 0.85g/cm 3 ～0.90g/cm 3 Is a uniform powder material; placing the powder into a ball grinding tool for prepressing under 40-45 MPa to prepare ceramic ball blanks, and trimming the blanks by cutting off redundant parts; carrying out cold isostatic pressing forming on the green embryo under the condition of 280-300 MPa; the obtained blank ball is placed into a pneumatic sintering furnace for sintering treatment, and sintered for 1-2 h at 1850-2000 ℃ and the nitrogen pressure is 9-12 MPa, so that the large-size silicon nitride ceramic ball is prepared.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
It should be noted that the terms "first," "second," and the like in the description and claims of the present application and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that embodiments of the present application described herein may be capable of being practiced otherwise than as specifically illustrated and described herein.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the oversized silicon nitride ceramic ball for the oversized bearing is characterized by comprising the following steps of:
step one, weighing 6 weight percent MgSiN 2 -YbF 3 、94wt％β-Si 3 N 4 Premixing the powder to achieve the aim of uniform mixing;
step two, absolute ethyl alcohol is used as a medium, the materials obtained in the step one are ball-milled and evenly mixed for 15-20 h, the ball milling speed is 90-120 r/min, and the materials are dried for 4-5 h at 65-75 ℃ through a rotary evaporator;
step three, atomizing the material obtained in the step two by closed spray granulation to obtain the material with the particle size of 50-100 microns and the bulk density of 0.85g/cm 3 ～0.90g/cm 3 Is a uniform powder material;
step four, placing the powder into a ball grinding tool for prepressing under 40-45 MPa to prepare ceramic ball blanks, and trimming the blanks by cutting off redundant parts;
step five, performing cold isostatic pressing molding on the green embryo under the condition of 280-300 MPa;
step six, placing the blank ball obtained in the step five into a pneumatic sintering furnace for sintering treatment, and sintering for 1-2 h at 1850-2000 ℃ with the nitrogen pressure of 9-12 MPa.
2. The method for preparing the oversized silicon nitride ceramic ball for the oversized bearing, which is disclosed in claim 1, is characterized in that in the second step, absolute ethyl alcohol is used as a medium, the materials obtained in the first step are ball-milled and mixed for 18 hours, the ball-milling speed is 100 revolutions per minute, and the materials are dried for 4.5 hours at 70 ℃ through a rotary evaporator.
3. The method for preparing oversized silicon nitride ceramic balls for oversized bearings according to claim 1, wherein in the third step, the material obtained in the second step is atomized by closed spray granulation to obtain the ceramic balls with a particle size of 80 microns and a bulk density of 0.88g/cm 3 Is a uniform powder of (a).
4. The method for manufacturing oversized silicon nitride ceramic balls for oversized bearings according to claim 1, wherein in the fourth step, powder is placed in a ball grinder to be pre-pressed under 42MPa, a ceramic ball green body is manufactured, and the redundant parts of the green body are cut off for trimming.
5. The method for producing oversized silicon nitride ceramic balls for oversized bearings according to claim 1, wherein in the fifth step, the green body is cold isostatic pressed under 290 MPa.
6. The method for preparing oversized silicon nitride ceramic balls for oversized bearings according to claim 1, wherein in the sixth step, the blank balls obtained in the fifth step are put into a gas pressure sintering furnace to be sintered, and sintered for 1.5 hours at 1900 ℃ under a nitrogen pressure of 10MPa.
7. The method for preparing oversized silicon nitride ceramic balls for oversized bearings according to claim 1, further comprising:
and step seven, depositing a silicon carbide layer on the surface of the silicon nitride ceramic ball obtained in the step six by adopting chemical vapor deposition.
8. The method for preparing oversized silicon nitride ceramic balls for oversized bearings according to claim 7, wherein in the seventh step, silicon nitride ceramic balls are added into a reactor, methyltrichlorosilane, argon and hydrogen are introduced into the reactor, and the reaction is carried out for 4 to 6 hours at a temperature of 1200 to 1500 ℃.
9. The method for preparing oversized silicon nitride ceramic balls for oversized bearings according to claim 8, wherein in the seventh step, silicon nitride ceramic balls are added into a reactor, methyltrichlorosilane, argon and hydrogen are introduced into the reactor, and the reaction is carried out for 5 hours at 1300 ℃.
10. The method for preparing oversized silicon nitride ceramic balls for oversized bearings according to claim 1, wherein in the sixth step, when the blank balls obtained in the fifth step are put into a gas pressure sintering furnace for sintering treatment, the sintering aid is one or more of yttrium oxide, magnesium oxide, aluminum oxide and tungsten carbide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210015042.7A CN116444277A (en) | 2022-01-07 | 2022-01-07 | Preparation method of oversized silicon nitride ceramic ball for oversized bearing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210015042.7A CN116444277A (en) | 2022-01-07 | 2022-01-07 | Preparation method of oversized silicon nitride ceramic ball for oversized bearing |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116444277A true CN116444277A (en) | 2023-07-18 |
Family
ID=87118872
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210015042.7A Pending CN116444277A (en) | 2022-01-07 | 2022-01-07 | Preparation method of oversized silicon nitride ceramic ball for oversized bearing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116444277A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05294729A (en) * | 1992-04-16 | 1993-11-09 | Ube Ind Ltd | Silicon nitride-based spherical sintered compact and tis production |
| CN101100388A (en) * | 2007-07-17 | 2008-01-09 | 清华大学 | High heat conductivity silicon nitride ceramics material and preparation method thereof |
| CN106518089A (en) * | 2016-11-25 | 2017-03-22 | 中国工程物理研究院材料研究所 | Preparation method of high performance large size silicon nitride ceramic material |
| CN107399974A (en) * | 2016-05-22 | 2017-11-28 | 河北高富氮化硅材料有限公司 | A kind of method added fluoride and prepare high heat conduction silicon nitride ceramics |
| US20180237347A1 (en) * | 2015-08-17 | 2018-08-23 | Korea Advanced Institute Of Science And Technology | Silicon nitride sintered body with high thermal conductivity and method for manufacturing same |
| CN111533561A (en) * | 2020-07-06 | 2020-08-14 | 佛山华骏特瓷科技有限公司 | Silicon nitride-based ceramic ball and preparation method and application thereof |
| CN111548163A (en) * | 2020-05-18 | 2020-08-18 | 北京中材人工晶体研究院有限公司 | Method for preparing silicon nitride ceramic balls for large-size wind power generation |
-
2022
- 2022-01-07 CN CN202210015042.7A patent/CN116444277A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05294729A (en) * | 1992-04-16 | 1993-11-09 | Ube Ind Ltd | Silicon nitride-based spherical sintered compact and tis production |
| CN101100388A (en) * | 2007-07-17 | 2008-01-09 | 清华大学 | High heat conductivity silicon nitride ceramics material and preparation method thereof |
| US20180237347A1 (en) * | 2015-08-17 | 2018-08-23 | Korea Advanced Institute Of Science And Technology | Silicon nitride sintered body with high thermal conductivity and method for manufacturing same |
| CN107399974A (en) * | 2016-05-22 | 2017-11-28 | 河北高富氮化硅材料有限公司 | A kind of method added fluoride and prepare high heat conduction silicon nitride ceramics |
| CN106518089A (en) * | 2016-11-25 | 2017-03-22 | 中国工程物理研究院材料研究所 | Preparation method of high performance large size silicon nitride ceramic material |
| CN111548163A (en) * | 2020-05-18 | 2020-08-18 | 北京中材人工晶体研究院有限公司 | Method for preparing silicon nitride ceramic balls for large-size wind power generation |
| CN111533561A (en) * | 2020-07-06 | 2020-08-14 | 佛山华骏特瓷科技有限公司 | Silicon nitride-based ceramic ball and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2404021C2 (en) | Polycrystalline abrasive materials and method of their fabrication | |
| KR101161337B1 (en) | Bonded abrasive article and method of making | |
| JP2024500914A (en) | High thermal conductivity silicon nitride ceramic insulating board and method for manufacturing the same | |
| WO2003004437A1 (en) | Translucent rare earth oxide sintered article and method for production thereof | |
| JPH07277814A (en) | Alumina-based ceramic sintered compact | |
| JP2013507526A (en) | Tin oxide ceramic sputtering target and method for producing the same | |
| RU2402507C2 (en) | Ceramic material and preparation method thereof | |
| JPS61266359A (en) | Silicon nitride sintered body and manufacture | |
| CN113548891B (en) | Two-phase cobalt tantalate ceramic block and preparation method thereof | |
| KR102011586B1 (en) | Polycrystalline abrasive structure | |
| CN116444277A (en) | Preparation method of oversized silicon nitride ceramic ball for oversized bearing | |
| EP0121518A1 (en) | Making hot pressed silicon nitride by use of low density reaction bonded body. | |
| US7648675B2 (en) | Reaction sintered zirconium carbide/tungsten composite bodies and a method for producing the same | |
| CN115259853A (en) | High-entropy fluorite oxide target material and preparation method thereof | |
| CN114835473A (en) | Alumina ceramic and preparation method thereof | |
| CN106631173A (en) | C/C composite material SiC-Y2Hf2O7 compound coating and preparation method thereof | |
| CN103288455A (en) | Method for producing composite ceramic from cubic boron nitride | |
| CN115710130A (en) | Ceramic composition, silicon nitride ceramic material and preparation method thereof, and preparation method of silicon nitride ceramic product | |
| JP2000128625A (en) | Aluminous ceramic sintered compact and its production | |
| KR102002347B1 (en) | Zr-based composite ceramic material, its manufacturing method and shell ornament | |
| CN108997000A (en) | A kind of high-temperature crucible and its manufacturing method | |
| CN112978684B (en) | Intra-crystalline porous high-performance skutterudite thermoelectric material and preparation method thereof | |
| CN116217270B (en) | Production process of diamond film coated dielectric ball with surface of zirconia ball | |
| KR102318672B1 (en) | Cubic boron nitride particle and manufacturing method thereof | |
| JPS60186470A (en) | Manufacture of silicon nitride sintered body |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |