CN112898029A - Preparation method of silicon nitride substrate raw material - Google Patents
Preparation method of silicon nitride substrate raw material Download PDFInfo
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- CN112898029A CN112898029A CN202110131933.4A CN202110131933A CN112898029A CN 112898029 A CN112898029 A CN 112898029A CN 202110131933 A CN202110131933 A CN 202110131933A CN 112898029 A CN112898029 A CN 112898029A
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- 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
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- 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
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Abstract
The invention discloses a preparation method of a silicon nitride substrate raw material. The invention provides a preparation method of a silicon nitride substrate raw material. The silicon nitride raw powder and the additive are fully fused, and the fused powder is combusted by utilizing an atmosphere pressure sintering method, so that the additive is released in the atmosphere pressure sintering process, and the silicon nitride substrate prepared by the silicon nitride substrate raw material can meet the process requirements of overlarge size, ultrathin thickness, high heat conductivity and the like and simultaneously ensure the mechanical property.
Description
Technical Field
The invention relates to the technical field of preparation of silicon nitride substrate raw materials, in particular to a preparation method of a silicon nitride substrate raw material.
Background
Silicon nitride is an important structural ceramic material, has high hardness, self lubricating property and wear resistance, and is an atomic crystal; is resistant to oxidation at high temperature. It can resist cold and hot impact, and can be heated to above 1000 deg.C in air, and can be rapidly cooled and then rapidly heated, and can not be broken. At present, only a few colleges and scientific research institutions are engaged in related research and development and technical attack of silicon nitride substrate raw materials in China, and the silicon nitride powder on the existing domestic market is difficult to have qualitative breakthrough in the aspects of improving the compactness and the purity. Therefore, it is necessary to provide a method for preparing a raw material for a silicon nitride substrate to solve the above problems.
Disclosure of Invention
The invention aims to provide a method for preparing a silicon nitride substrate raw material, which aims to solve the problem that the compactness and purity of silicon nitride powder on the existing domestic market need to be improved.
The invention provides a preparation method of a silicon nitride substrate raw material, which comprises the following steps:
step one, adding an additive into silicon nitride raw powder, wherein the additive is a rare earth additive;
step two, fully fusing the silicon nitride raw powder and the additive;
and step three, burning the fused powder by utilizing an atmosphere pressure sintering process to release the additive in the atmosphere pressure sintering process.
Further, the third step further includes: the highest combustion reaction temperature of a Si-N system is controlled by adopting a gas-phase enhanced temperature control activation method, and the reaction activation energy is reduced by adopting chemical excitation and mechanical activation means.
Further, the third step further includes: the powder block is sucked and swept by utilizing the induced air negative pressure of the dust removal system and the cyclone separator according to the powder particle size design of the silicon nitride powder, the bridging is eliminated, and the compactness is improved.
Further, in the first step, the rare earth additive is one or more of yttrium fluoride, lanthanum trifluoride, anhydrous ytterbium fluoride, europium fluoride, samarium trifluoride, cerium trifluoride, or neodymium fluoride.
Further, in the step one, the method further comprises: adding metal oxide into the silicon nitride raw powder, wherein the metal oxide is one or more of aluminum oxide, magnesium oxide, zirconium oxide or titanium oxide.
Further, in the step one, the method further comprises: and adding a binder into the silicon nitride raw powder, wherein the binder is polyvinyl alcohol, polyvinyl butyral, polyethylene glycol or phenolic resin.
Further, in the step one, the method further comprises: and adding a dispersing agent into the silicon nitride raw powder, wherein the dispersing agent is ammonium polyacrylate.
Further, in the step one, the method further comprises: and adding a defoaming agent into the silicon nitride raw powder, wherein the defoaming agent is tributyl phosphate.
The invention has the following beneficial effects:
the invention provides a preparation method of a silicon nitride substrate raw material. The silicon nitride raw powder and the additive are fully fused, and the fused powder is combusted by utilizing an atmosphere pressure sintering method, so that the additive is released in the atmosphere pressure sintering process, and the silicon nitride substrate prepared by the silicon nitride substrate raw material can meet the process requirements of overlarge size, ultrathin thickness, high heat conductivity and the like and simultaneously ensure the mechanical property.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings 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 it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a flow chart of a method for preparing a silicon nitride substrate raw material according to the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings. It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. 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, a method for preparing a silicon nitride substrate raw material according to an embodiment of the present invention includes the following steps:
step one, adding an additive into the silicon nitride raw powder, wherein the additive is a rare earth additive.
In this embodiment, in the first step, the rare earth additive is one or more of yttrium fluoride, lanthanum trifluoride, anhydrous ytterbium fluoride, europium fluoride, samarium trifluoride, cerium trifluoride, or neodymium fluoride. Yttrium fluoride is a chemical substance and is off-white powder or crystal at normal temperature. Lanthanum trifluoride is a white face-centered cubic crystal, is almost insoluble in water, but can be dissolved in alcohol, and the dissolution rule is the same as that of rare earth chloride. Europium fluoride is gray powder and has stable chemical property; it is insoluble in water and soluble in acid. The europium fluoride micro-nano rod can be prepared by synthesizing a compound containing fluorine ions and an oxide containing europium ions by a hydrothermal method under an alkaline condition. Cerium trifluoride is commonly used as a high-purity chemical and a coating material, and is insoluble in water under standard conditions. The neodymium fluoride is white and slightly purplish red powder, is insoluble in water, hydrochloric acid, nitric acid and sulfuric acid, can be dissolved in perchloric acid, has hygroscopicity in air and is relatively stable.
Rare earth additives such as yttrium fluoride, lanthanum trifluoride, anhydrous ytterbium fluoride, europium fluoride, samarium trifluoride, cerium trifluoride or neodymium fluoride are used as sintering aids, so that oxygen in the aids can be prevented from entering silicon nitride lattices, and the influence of lattice oxygen on the thermal conductivity of silicon nitride ceramics is reduced. The prepared silicon nitride ceramic not only has higher thermal conductivity, but also has the advantages of high mechanical strength, water resistance, oxidation resistance and the like, and becomes a material with great potential in the field of electronic packaging.
In the first step, the method may further include: adding metal oxide into the silicon nitride raw powder, wherein the metal oxide is one or more of aluminum oxide, magnesium oxide, zirconium oxide or titanium oxide. The metal oxide is used as a sintering aid, the sintering aid forms a liquid phase with a trace amount of silicon dioxide on the surface of silicon nitride when the temperature of the eutectic point of the metal oxide is exceeded, particles are rearranged in the liquid phase to realize close packing, the liquid phase is converted into a glass phase after cooling and is left in a sintered body, and only a silicon nitride phase exists in the sintered body.
In the first step, the method may further include: and adding a binder into the silicon nitride raw powder, wherein the binder is polyvinyl alcohol, polyvinyl butyral, polyethylene glycol or phenolic resin. Polyvinyl alcohol is an organic compound, is a white flaky, flocculent or powdery solid in appearance, and is odorless. Is soluble in water, slightly soluble in dimethyl sulfoxide, and insoluble in gasoline, kerosene, vegetable oil, benzene, toluene, dichloroethane, carbon tetrachloride, acetone, ethyl acetate, methanol, ethylene glycol, etc. Polyvinyl alcohol is an important chemical raw material, and is used for manufacturing polyvinyl acetal, gasoline-resistant pipelines, vinylon, fabric treating agents, emulsifiers, paper coatings, adhesives, glue and the like. Polyvinyl butyral is the product of the acid catalyzed condensation of polyvinyl alcohol with butyraldehyde. PVB molecules contain longer branched chains, so that the PVB has good flexibility, low glass transition temperature and high tensile strength and impact strength; PVB has excellent transparency, good solubility, good light resistance, water resistance, heat resistance, cold resistance and film forming property; the functional group contained in it can be used for saponification reaction of phthalidyl, acetification reaction of phthalidyl, sulfonation reaction of phthalidyl and other various reactions; has high adhesion with materials such as glass, metal (especially aluminum), and the like. Therefore, the resin is widely applied to the fields of manufacturing laminated safety glass, adhesives, ceramic stained paper, aluminum foil paper, electrical equipment materials, glass fiber reinforced plastic products, fabric treating agents and the like, and becomes an indispensable synthetic resin material. Polyethylene glycol is a high molecular polymer, has no irritation, slightly bitter taste, good water solubility, and good compatibility with many organic components. Has excellent lubricity, moisture retention, dispersibility and bonding agent, can be used as an antistatic agent, a softening agent and the like, and has extremely wide application in the industries of cosmetics, pharmacy, chemical fiber, rubber, plastics, papermaking, paint, electroplating, pesticides, metal processing, food processing and the like. Phenolic resin, also called bakelite, is colorless or yellowish brown transparent, and is usually sold in the market with a colorant in red, yellow, black, green, brown, blue and other colors, in the form of granules or powder. The corrosion inhibitor is resistant to weak acid and weak base, can be decomposed when meeting strong acid, and can be corroded when meeting strong base. Insoluble in water, and soluble in organic solvents such as acetone and alcohol. Obtained by condensation polymerization of phenol formaldehyde or derivatives thereof.
In the first step, the method may further include: and adding a dispersing agent into the silicon nitride raw powder, wherein the dispersing agent is ammonium polyacrylate. And adding a defoaming agent into the silicon nitride raw powder, wherein the defoaming agent is tributyl phosphate. The ammonium polyacrylate is used as special ceramic dispersant, and the solid is white powder dissolved in water. The solution is colorless or yellowish liquid with pungent odor. Tributyl phosphate is colorless to light yellow transparent liquid, decomposes at boiling point temperature, dissolves in most organic solvents and hydrocarbons, is insoluble or slightly soluble in glycerol, hexanediol and amines, has ester universality, and hydrolyzes under alkaline conditions. Dry hydrogen chloride is introduced at room temperature to produce chlorobutane. Reacting with benzene in the presence of boron trifluoride to produce sec-butylbenzene and 1, 4-di-sec-butylbenzene. Treatment with aniline and dilute sodium hydroxide solution produces dibutylaniline.
And step two, fully fusing the silicon nitride raw powder and the additive.
Specifically, the raw materials can be selected according to the following weight parts: 80 parts of silicon nitride raw powder, 10 parts of metal oxide, 4 parts of rare earth oxide, 1 part of binder, 0.5 part of dispersant and 0.1 part of defoamer, and the raw materials can be stirred, mixed and uniformly mixed.
And step three, burning the fused powder by utilizing an atmosphere pressure sintering process to release the additive in the atmosphere pressure sintering process.
The thickness of the silicon nitride substrate is required to be 0.24-0.32 mm, the thermal conductivity is more than or equal to 90, and additives which can be achieved in the atmosphere pressure sintering process need to be prepared in the raw material formula.
In this embodiment, the third step may further include:
the highest combustion reaction temperature of a Si-N system is controlled by adopting a gas-phase enhanced temperature control activation method, and the reaction activation energy is reduced by adopting chemical excitation and mechanical activation means, so that the powder reaction activity is improved, the reaction kinetics is promoted, and the low-cost silicon nitride powder is synthesized by combustion.
In this embodiment, the third step may further include:
the powder block is sucked and swept by utilizing the induced air negative pressure of the dust removal system and the cyclone separator according to the powder particle size design of the silicon nitride powder, the bridging is eliminated, and the compactness is improved. The cyclone separator is a device for separating a gas-solid system or a liquid-solid system, and the working principle is that solid particles or liquid drops with larger inertial centrifugal force are thrown to an outer wall surface to be separated by virtue of the rotating motion caused by tangential introduction of airflow. The cyclone separator has the main characteristics of simple structure, high operation flexibility, high efficiency, convenient management and maintenance and low price, is used for collecting dust with the diameter of more than 5-10 mu m, is widely applied to the pharmaceutical industry, is particularly suitable for being used as an internal separation device of a fluidized bed reactor or a pre-separator under the conditions of coarse dust particles, high dust concentration and high temperature and high pressure, and is separation equipment with wide industrial application.
Meanwhile, the purity of the silicon nitride powder is ensured by adopting closed operation and replacing manual operation with equipment, so that the impurity content of the silicon nitride powder is improved from PPm level to PPb level, and the particle size distribution of the powder is narrowed, thereby achieving the optimal state of meeting performance requirements and practical application.
In conclusion, the preparation method of the silicon nitride substrate raw material provided by the embodiment of the invention realizes that the product reaches the international advanced level, and meanwhile, the product output can be realized by using domestic equipment, and the low-cost large-scale production can be realized, the average cost is 30-40% lower than the international advanced level, and the method completely replaces the foreign import.
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 according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those illustrated or otherwise described herein.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for preparing a silicon nitride substrate raw material is characterized by comprising the following steps:
step one, adding an additive into silicon nitride raw powder, wherein the additive is a rare earth additive;
step two, fully fusing the silicon nitride raw powder and the additive;
and step three, burning the fused powder by utilizing an atmosphere pressure sintering process to release the additive in the atmosphere pressure sintering process.
2. The method of claim 1, wherein the third step further comprises:
the highest combustion reaction temperature of a Si-N system is controlled by adopting a gas-phase enhanced temperature control activation method, and the reaction activation energy is reduced by adopting chemical excitation and mechanical activation means.
3. The method of claim 1, wherein the third step further comprises:
the powder block is sucked and swept by utilizing the induced air negative pressure of the dust removal system and the cyclone separator according to the powder particle size design of the silicon nitride powder, the bridging is eliminated, and the compactness is improved.
4. The method of claim 1, wherein in the first step, the rare earth additive is one or more of yttrium fluoride, lanthanum trifluoride, ytterbium fluoride anhydrous, europium fluoride, samarium trifluoride, cerium trifluoride, or neodymium fluoride.
5. The method for preparing a silicon nitride substrate raw material according to claim 1, wherein the first step further comprises: adding metal oxide into the silicon nitride raw powder, wherein the metal oxide is one or more of aluminum oxide, magnesium oxide, zirconium oxide or titanium oxide.
6. The method for preparing a silicon nitride substrate raw material according to claim 1, wherein the first step further comprises: and adding a binder into the silicon nitride raw powder, wherein the binder is polyvinyl alcohol, polyvinyl butyral, polyethylene glycol or phenolic resin.
7. The method for preparing a silicon nitride substrate raw material according to claim 1, wherein the first step further comprises: and adding a dispersing agent into the silicon nitride raw powder, wherein the dispersing agent is ammonium polyacrylate.
8. The method for preparing a silicon nitride substrate raw material according to claim 1, wherein the first step further comprises: and adding a defoaming agent into the silicon nitride raw powder, wherein the defoaming agent is tributyl phosphate.
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2021
- 2021-01-30 CN CN202110131933.4A patent/CN112898029A/en active Pending
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| US20120196125A1 (en) * | 2011-01-27 | 2012-08-02 | Korea Institute Of Machinery & Materials | Method of manufacturing pre-sintered si-mixture granule for porous sintered reaction-bonded silicon nitride, porous pre-sintered granule manufactured by the method, and method of manufacturing porous sintered reaction-bonded silicon nitride |
| CN105669209A (en) * | 2015-12-30 | 2016-06-15 | 刘操 | Silicon nitride ceramic material, and preparation method and application thereof |
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| KR20170135105A (en) * | 2016-05-30 | 2017-12-08 | 한국세라믹기술원 | Manufacturing method of sheet-type silicon nitride subststrate |
| CN108409336A (en) * | 2018-05-28 | 2018-08-17 | 江苏东浦精细陶瓷科技股份有限公司 | Silicon nitride ceramics and preparation method thereof |
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| CN111170745A (en) * | 2020-01-09 | 2020-05-19 | 北京科技大学 | Preparation method of high-thermal-conductivity silicon nitride substrate |
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