CN109987943A - A kind of preparation method of beta-silicon nitride powder - Google Patents

A kind of preparation method of beta-silicon nitride powder Download PDF

Info

Publication number
CN109987943A
CN109987943A CN201910268491.0A CN201910268491A CN109987943A CN 109987943 A CN109987943 A CN 109987943A CN 201910268491 A CN201910268491 A CN 201910268491A CN 109987943 A CN109987943 A CN 109987943A
Authority
CN
China
Prior art keywords
powder
ball
alcohol
silicon
silicon nitride
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
Application number
CN201910268491.0A
Other languages
Chinese (zh)
Inventor
杨德安
高春兰
张宝强
郭靖栋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin University
Original Assignee
Tianjin University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Tianjin University filed Critical Tianjin University
Priority to CN201910268491.0A priority Critical patent/CN109987943A/en
Publication of CN109987943A publication Critical patent/CN109987943A/en
Pending legal-status Critical Current

Links

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
    • C04B35/591—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 obtained by reaction sintering
    • 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
    • C04B35/626—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
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

The present invention relates to a kind of preparation methods of beta-silicon nitride powder, will adulterate TiO2The silicon powder of powder carries out ball milling, adds silicon nitride abrading-ball and alcohol；It is put into ball mill and carries out ball milling, then the TiO after ball milling2Silicon powder filtered, remove the alcohol in removing silicon powder；Powder after suction filtration is dried in a vacuum drying oven, removes remaining alcohol；Sample after above-mentioned vacuum drying is ground up, sieved, evengranular powder is obtained；By the doping TiO after above-mentioned grinding2Silicon powder be put into high temperature process furnances, vacuumize, be passed through nitrogen and hydrogen mixture, rise to 800 DEG C to be less than or equal to 4 DEG C/min, then rise to 1300-1400 DEG C to be less than or equal to 2 DEG C/min, and keep the temperature 2-4h；Obtain beta-silicon nitride powder.The present invention is low, at low cost with nitriding temperature, the nitridation period is short；β-Si in prepared powder3N4It is mutually up to 64wt%, partial size is small and part is corynebacterium.

Description

A kind of preparation method of beta-silicon nitride powder
Technical field
The present invention relates to technical field of ceramic material, specifically a kind of beta-silicon nitride powder (β-Si3N4) preparation method.
Background technique
The development of science and technology proposes more harsh requirement, silicon nitride (Si to the performance of material3N4) ceramic with excellent machine Tool, physical and chemical properties are provided simultaneously with high theoretical thermal conductivity (reaching as high as 400W/ (m*K)), can be applied to various industry Field, while being also a kind of Electronic Packaging ceramic substrate alternative materials of great potential.Prepare the silicon nitride ceramic of high quality Body is the basis for preparing high-performance silicon nitride ceramics, and the powder quality prepared using distinct methods is different.Common nitridation There are two types of silicon powders, and one is α-Si3N4, one is β-Si3N4。β-Si3N4Thermal conductivity is high, is suitable for baseplate material, but prepare β-Si3N4Temperature be higher than 1400 DEG C, high preparation temperature causes β-Si3N4The increase of powder cost limits β-Si3N4 Powder application.Prepare β-Si3N4The problem of ceramic powder maximum is how to prepare at a lower temperature.
Si3N4There are many kinds of raw powder's production technologies, wherein direct nitridation method simple process, and cost is relatively low, is industrially prepared A kind of conventional method of beta-silicon nitride powder, but this preparation method period is long, low efficiency is unfavorable for producing.Therefore seek height Efficiency, economy and the β-Si that can manufacture high quality3N4Powder is of great significance.
Summary of the invention
The purpose of the present invention is to provide a kind of β-Si3N4Raw powder's production technology, provide it is a kind of based on direct nitridation method, A kind of low, at low cost, the nitridation period is short, process is simple and yield the is high method of nitriding temperature.
To achieve the above object, the invention provides the following technical scheme:
A kind of β-Si3N4Raw powder's production technology comprising following steps:
1) 2.5-8wt%TiO will, be adulterated2The silicon powder of powder carries out ball milling, and the powder after ball milling is respectively put into silicon nitride In ball grinder, add silicon nitride abrading-ball and alcohol, wherein powder: abrading-ball: alcohol quality ratio is 1:(3-5): 1.5；It is put into ball milling Ball milling, revolving speed 300-400r/min, Ball-milling Time 2-4h are carried out in machine；
2), by the doping TiO after above-mentioned ball milling2Silicon powder filtered, remove the alcohol in removing silicon powder；It later, will be above-mentioned Powder after suction filtration is dried in a vacuum drying oven, removes remaining alcohol, and 50-75 DEG C of temperature, drying time 2-4h； Sample after above-mentioned vacuum drying is subjected to ground 50-80 mesh, obtains evengranular powder；
3), by the doping TiO after above-mentioned grinding2Powder be put into high temperature process furnances, vacuumize 4-6 times, be passed through nitrogen hydrogen Gaseous mixture rises to 800 DEG C to be less than or equal to 4 DEG C/min, then rises to 1300-1400 DEG C to be less than or equal to 2 DEG C/min, and keep the temperature 2- 4h；Obtain beta-silicon nitride powder.
The particle size of micron silicon powder used in the step (1) is 1-20 μm, and purity is more than or equal to 99.9%.
Powder in the step (1): abrading-ball: alcohol quality ratio is 1:(3-5): 1.5.
Sample in the step (2) after vacuum drying carries out ground 50-80 mesh.
TiO used2Powder purity is that analysis is pure.
Purity of alcohol used is that analysis is pure.
Step is nitrogen and hydrogen mixture in (3) in the step (1): nitrogen 92-95%, hydrogen 5-8%.
The phase composition for preparing material of the invention is principal crystalline phase β-Si3N4With a small amount of α-Si3N4, wherein microscopic appearance be Corynebacterium and a small amount of particle and fiber.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention uses TiO2Powder is catalyst, in 1300-1400 DEG C of nitridation completely.So present invention reduces nitrogen Change temperature, shorten nitridation time and yield is high.
2, the present invention utilizes TiO2Powder is catalyst, is catalyzed the nitridation of silicon powder, obtain graininess and corynebacterium when Huang, And β-Si3N4Content is up to 64wt%.
3, the present invention introduces a small amount of TiO during the reaction2Powder, product purity are high.
4, the raw materials used in the present invention is from a wealth of sources and cheap, and operating procedure is simple, is easy to control, and production cost is low, With very big industrialization prospect.
Detailed description of the invention
Fig. 1 (a): the XRD spectra after silicon powder nitrogenizes 2h at 1300 DEG C in embodiment 1.
Fig. 1 (b): the XRD spectra after silicon powder nitrogenizes 2h at 1350 DEG C in example 2.
Fig. 1 (c): the XRD spectra after silicon powder nitrogenizes 2h at 1400 DEG C in embodiment 3.
Fig. 1 (d): the XRD spectra after silicon powder nitrogenizes 4h at 1400 DEG C in example 4.
Fig. 2 (a): the SEM picture after silicon powder nitrogenizes 2h at 1300 DEG C in embodiment 1.
Fig. 2 (b): the SEM picture after silicon powder nitrogenizes 2h at 1350 DEG C in example 2.
Fig. 2 (c): the SEM picture after silicon powder nitrogenizes 2h at 1400 DEG C in embodiment 3.
Fig. 2 (d): the SEM picture after silicon powder nitrogenizes 4h at 1400 DEG C in example 4.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and detailed description.
It is first that raw material Unify legislation involved in present embodiment is as follows to avoid repeating, not superfluous in embodiment It states:
For the silicon powder particle having a size of 1-20 μm, purity is more than or equal to 99.9%.The TiO2Powder purity is that analysis is pure. The purity of alcohol is that analysis is pure.The nitrogen and hydrogen mixture: nitrogen 92-95%, hydrogen 5-8%.
The invention will be further described with reference to the accompanying drawings and detailed description.
Embodiment 1
1), by TiO2Raw material is weighed with Si powder 2.5:97.5 in mass ratio, 2.5wt%TiO will be adulterated2The silicon powder of powder into Powder after ball milling is respectively put into silicon nitride ball grinding jar by row ball milling, adds silicon nitride abrading-ball and alcohol, wherein powder: mill Ball: alcohol quality ratio is 1:3:1.5.It is put into ball mill and carries out ball milling, revolving speed 300r/min, Ball-milling Time 4h.
2), by the doping 2.5wt%TiO after above-mentioned ball milling2Silicon powder filtered, remove the alcohol in removing silicon powder；Later, Powder after above-mentioned suction filtration is dried in a vacuum drying oven, removes remaining alcohol, temperature 50 C, drying time 4h.Sample after above-mentioned vacuum drying is subjected to ground 80 mesh, obtains evengranular powder；
3), by the doping 2.5wt%TiO after above-mentioned grinding2Powder be put into high temperature process furnances, vacuumize 4 times, be passed through Nitrogen and hydrogen mixture rises to 800 DEG C with 4 DEG C/min, then rises to 1300 DEG C with 2 DEG C/min, and keep the temperature 2h.Obtain silicon nitride powder Body.Its XRD diagram such as Fig. 1 (a), SEM figure such as Fig. 2 (a).
Embodiment 2
1), by TiO2Raw material is weighed with Si powder 5:95 in mass ratio, 5wt%TiO will be adulterated2The silicon powder of powder carries out ball milling, Powder after ball milling is respectively put into silicon nitride ball grinding jar, adds silicon nitride abrading-ball and alcohol, wherein powder: abrading-ball: alcohol Mass ratio is 1:5:1.5.It is put into ball mill and carries out ball milling, revolving speed 400r/min, Ball-milling Time 2h.
2), by the doping 5wt%TiO after above-mentioned ball milling2Silicon powder filtered, remove the alcohol in removing silicon powder；Later, will Powder after above-mentioned suction filtration is dried in a vacuum drying oven, removes remaining alcohol, temperature 50 C, drying time 4h. Sample after above-mentioned vacuum drying is subjected to ground 75 mesh, obtains evengranular powder；
3), by the doping 5wt%TiO after above-mentioned grinding2Powder be put into high temperature process furnances, vacuumize 6 times, be passed through nitrogen Hydrogen gaseous mixture rises to 800 DEG C with 4 DEG C/min, then rises to 1350 DEG C with 2 DEG C/min, and keep the temperature 2h.Obtain beta-silicon nitride powder. Its XRD diagram such as Fig. 1 (b), SEM figure such as Fig. 2 (b).
Embodiment 3
1), by TiO2Raw material is weighed with Si powder 2.5:97.5 in mass ratio, 2.5wt%TiO will be adulterated2The silicon powder of powder into Powder after ball milling is respectively put into silicon nitride ball grinding jar by row ball milling, adds silicon nitride abrading-ball and alcohol, wherein powder: mill Ball: alcohol quality ratio is 1:4:1.5.It is put into ball mill and carries out ball milling, revolving speed 400r/min, Ball-milling Time 4h.
2), by the doping 2.5wt%TiO after above-mentioned ball milling2Silicon powder filtered, remove the alcohol in removing silicon powder；Later, Powder after above-mentioned suction filtration is dried in a vacuum drying oven, removes remaining alcohol, 75 DEG C of temperature, drying time 4h.Sample after above-mentioned vacuum drying is subjected to ground 80 mesh, obtains evengranular powder；
3), by the doping 2.5wt%TiO after above-mentioned grinding2Powder be put into high temperature process furnances, vacuumize 5 times, be passed through Nitrogen and hydrogen mixture rises to 800 DEG C with 3 DEG C/min, then rises to 1400 DEG C with 2 DEG C/min, and keep the temperature 2h.Obtain silicon nitride powder Body.Its XRD diagram such as Fig. 1 (c), SEM figure such as Fig. 2 (c).
Embodiment 4
1), by TiO2Raw material is weighed with Si powder 8:92 in mass ratio, 8wt%TiO will be adulterated2The silicon powder of powder carries out ball milling, Powder after ball milling is respectively put into silicon nitride ball grinding jar, adds silicon nitride abrading-ball and alcohol, wherein powder: abrading-ball: alcohol Mass ratio is 1:4:1.5.It is put into ball mill and carries out ball milling, revolving speed 400r/min, Ball-milling Time 4h.
2), by the doping 8wt%TiO after above-mentioned ball milling2Silicon powder filtered, remove the alcohol in removing silicon powder；Later, will Powder after above-mentioned suction filtration is dried in a vacuum drying oven, removes remaining alcohol, and 75 DEG C of temperature, drying time 4h. Sample after above-mentioned vacuum drying is subjected to ground 50 mesh, obtains evengranular powder；
3), by the doping 8wt%TiO after above-mentioned grinding2Powder be put into high temperature process furnances, vacuumize 6 times, be passed through nitrogen Hydrogen gaseous mixture rises to 800 DEG C with 4 DEG C/min, then rises to 1400 DEG C with 2 DEG C/min, and keep the temperature 4h.Obtain beta-silicon nitride powder. Its XRD diagram such as Fig. 1 (d), SEM figure such as Fig. 2 (d).
A kind of preparation method for beta-silicon nitride powder that the present invention is disclosed and proposed, those skilled in the art can pass through reference Present disclosure, the appropriate links such as condition route that change are realized, are preferably implemented although method and technology of preparing of the invention has passed through Example is described, related technical personnel obviously can not depart from the content of present invention, in spirit and scope to as described herein Methods and techniques route is modified or reconfigures, to realize final technology of preparing.In particular, it should be pointed out that Suo Youxiang Similar replacement and change is apparent to those skilled in the art, they are considered as being included in essence of the invention In mind, range and content.

Claims (7)

1. a kind of preparation method of beta-silicon nitride powder, it is characterized in that the following steps are included:
1) 2.5-8wt%TiO will, be adulterated2The silicon powder of powder carries out ball milling, and the powder after ball milling is respectively put into silicon nitride ball milling In tank, add silicon nitride abrading-ball and alcohol, wherein powder: abrading-ball: alcohol quality ratio is 1:(3-5): 1.5；It is put into ball mill Carry out ball milling, revolving speed 300-400r/min, Ball-milling Time 2-4h；
2), by the doping TiO after above-mentioned ball milling2Silicon powder filtered, remove the alcohol in removing silicon powder；Later, it was filtered above-mentioned Powder afterwards is dried in a vacuum drying oven, removes remaining alcohol, and 50-75 DEG C of temperature, drying time 2-4h；It will be above-mentioned Sample after vacuum drying carries out ground 50-80 mesh, obtains evengranular powder；
3), by the doping TiO after above-mentioned grinding2Powder be put into high temperature process furnances, vacuumize 4-6 times, be passed through nitrogen hydrogen mixing Gas rises to 800 DEG C to be less than or equal to 4 DEG C/min, then rises to 1300-1400 DEG C to be less than or equal to 2 DEG C/min, and keep the temperature 2-4h； Obtain beta-silicon nitride powder.
2. the method as described in claim 1, the particle size of micron silicon powder used in characterization step (1) is 1-20 μm, Purity is more than or equal to 99.9%.
3. the method as described in claim 1, powder in characterization step (1): abrading-ball: alcohol quality ratio is 1:(3-5): 1.5.
4. the method as described in claim 1, the sample after the middle vacuum drying of characterization step (2) carries out ground 50-80 mesh Sieve.
5. the method as described in claim 1, it is characterized in that TiO used2Powder purity is that analysis is pure.
6. the method as described in claim 1, feature step purity of alcohol used is that analysis is pure.
7. the method as described in claim 1, step is nitrogen and hydrogen mixture in (3) in characterization step (1): nitrogen 92-95%, Hydrogen 5-8%.
CN201910268491.0A 2019-04-04 2019-04-04 A kind of preparation method of beta-silicon nitride powder Pending CN109987943A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910268491.0A CN109987943A (en) 2019-04-04 2019-04-04 A kind of preparation method of beta-silicon nitride powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910268491.0A CN109987943A (en) 2019-04-04 2019-04-04 A kind of preparation method of beta-silicon nitride powder

Publications (1)

Publication Number Publication Date
CN109987943A true CN109987943A (en) 2019-07-09

Family

ID=67132376

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910268491.0A Pending CN109987943A (en) 2019-04-04 2019-04-04 A kind of preparation method of beta-silicon nitride powder

Country Status (1)

Country Link
CN (1) CN109987943A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1657404A (en) * 2004-02-18 2005-08-24 中国科学院理化技术研究所 Method for synthesizing silicon nitride powder by atmospheric pressure combustion
CN102503434A (en) * 2011-09-30 2012-06-20 中国科学院理化技术研究所 Method for synthesizing silicon nitride powder by nitriding silicon powder under conditions of medium temperature and micro positive pressure
CN105541341A (en) * 2016-01-12 2016-05-04 河北高富氮化硅材料有限公司 Method for preparing high-compactness silicon nitride ceramic by adding composite additives
CN107673766A (en) * 2016-08-02 2018-02-09 河北高富氮化硅材料有限公司 A kind of structural ceramics high purity silicon nitride raw powder's production technology
CN108383532A (en) * 2018-05-28 2018-08-10 江苏东浦精细陶瓷科技股份有限公司 A kind of dense silicon nitride ceramic material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1657404A (en) * 2004-02-18 2005-08-24 中国科学院理化技术研究所 Method for synthesizing silicon nitride powder by atmospheric pressure combustion
CN102503434A (en) * 2011-09-30 2012-06-20 中国科学院理化技术研究所 Method for synthesizing silicon nitride powder by nitriding silicon powder under conditions of medium temperature and micro positive pressure
CN105541341A (en) * 2016-01-12 2016-05-04 河北高富氮化硅材料有限公司 Method for preparing high-compactness silicon nitride ceramic by adding composite additives
CN107673766A (en) * 2016-08-02 2018-02-09 河北高富氮化硅材料有限公司 A kind of structural ceramics high purity silicon nitride raw powder's production technology
CN108383532A (en) * 2018-05-28 2018-08-10 江苏东浦精细陶瓷科技股份有限公司 A kind of dense silicon nitride ceramic material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
WEIMING GUO等: "Effect of TiO2 additives on nitridation of Si powders", 《MATERIALS LETTERS》 *

Similar Documents

Publication Publication Date Title
US9534316B2 (en) Silicon carbide powder and method for manufacturing the same
CN103360077B (en) Silicon nitride crucible and preparation method thereof
CN103601498A (en) Preparation method of Ti3AlC2 ceramic powder
CN101428771A (en) Method for producing A1Npowder with microwave carbon thermoreduction cooling-down catalysis calcination
CN102807370A (en) Method for rapidly preparing AlON ceramic powder by means of carbon thermal reduction
CN104150911B (en) A kind of method of microwave-assisted quickly synthesis in low temperature nano-silicon nitride-silicon carbide composite powder body
CN109437919B (en) Method for preparing aluminum nitride ceramic powder based on urea/melamine nitrogen source
CN104499053A (en) Method for preparing silicon nitride crystal whisker
CN106565246A (en) Aluminum nitride/yttrium nitride composite powder preparation method
CN107758634A (en) A kind of method based on the clay standby high-purity α phase silicon nitride powders of silicon caused by crystal silicon solar batteries
US20130129599A1 (en) Silicon carbide and method for manufacturing the same
CN109987943A (en) A kind of preparation method of beta-silicon nitride powder
CN104446496A (en) Preparation method of AlON powder and transparent ceramics prepared from AlON powder
CN101698611A (en) Method for preparing silicon nitride powder with saw dust
CN109650896B (en) Synthesis method of LiAlON transparent ceramic powder
US10384941B2 (en) Method for producing spherical silicon nitride powder
CN116332183A (en) Method for producing silicon carbide powder, silicon carbide powder and application thereof
CN104233454A (en) Method for effectively synthesizing monocrystal hexagonal boron nitride structure by substitution reaction
CN109970035A (en) A kind of α-siliconnitride raw powder's production technology
US9416012B2 (en) Method of fabricating silicon carbide powder
JPH02258677A (en) Sic powder, preparation thereof and use thereof
CN102897726B (en) Method for preparing Si3N4 nanometer wire
CN114790107B (en) SiO preparation at low temperature by using polycrystalline silicon cutting waste 2 -Si 3 N 4 Method for compounding ceramic
CN114716252B (en) Preparation method of easy-sintering high-purity silicon nitride powder
KR20130020490A (en) Silicon carbide and method for manufacturing the same

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