CN110511034A - A kind of high yield ceramics and its preparation method and application - Google Patents

A kind of high yield ceramics and its preparation method and application Download PDF

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Publication number
CN110511034A
CN110511034A CN201910717528.3A CN201910717528A CN110511034A CN 110511034 A CN110511034 A CN 110511034A CN 201910717528 A CN201910717528 A CN 201910717528A CN 110511034 A CN110511034 A CN 110511034A
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China
Prior art keywords
ceramics
high yield
preparation
presoma
yield
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CN201910717528.3A
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Chinese (zh)
Inventor
詹创添
吴利翔
牛文彬
朱林林
郭伟明
林华泰
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Guangdong University of Technology
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Guangdong University of Technology
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Priority to CN201910717528.3A priority Critical patent/CN110511034A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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 carbides or oxycarbides
    • C04B35/565Shaped 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 carbides or oxycarbides based on silicon carbide
    • C04B35/571Shaped 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 carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention belongs to ceramic forerunner technical field, a kind of high yield ceramics and its preparation method and application are disclosed, the method is suppressed after presoma raw material to be pulverized to sieving, and 300~800 DEG C of heat treatment, obtains modified presoma under protective atmosphere;Modified presoma is carried out again to suppress after pulverizing sieving again, is cracked for 800~1200 DEG C under vacuum or protective atmosphere, obtains the ceramics of high yield.The ceramics of high yield and high-quality have been made in the present invention, and the yield of the high yield ceramics is 80~99%;The partial size of the ceramics is 0.01~10 μm.The high yield ceramics can be applicable to increasing material manufacturing, aerospace with or the fields such as nuclear energy.

Description

A kind of high yield ceramics and its preparation method and application
Technical field
The invention belongs to ceramic forerunner technical fields, more particularly, to a kind of high yield ceramics and preparation method thereof And application.
Background technique
Structural ceramics generally all has the good characteristics such as high-strength, high hard, high temperature resistant, corrosion-resistant and anti-neutron irradiation, is The critical material of the departments such as automobile, machinery, metallurgy and aerospace exploitation new technology.However, ceramic material is because of its brittleness, greatly The preparation of Complex Different Shape part is limited, ceramics can be prepared in ceramic forerunner after Pintsch process, therefore presoma can be used to Increasing material manufacturing molding is directly carried out, then carries out anisotropic part required for cracking-being sintered acquisition, equally, presoma can also be used as It is connected between a kind of connecting material progress is ceramic.
However, all there is its low yield when using presoma in increasing material manufacturing or connection area more than either The problem of, for increasing material manufacturing, yield is too low to will cause subsequent cracking-biggish volume contraction of sintering generation, to influence ruler Very little precision and mechanical property;For connection area, it is easy because yield is too low so that connection procedure center tap generates larger sky Gap influences switching performance.In order to solve problem above, the method for being badly in need of seeking to improve precursor ceramic yield, current research It is concentrated mainly on from synthesis presoma, to improve the yield of presoma;However, these preparation methods condition is excessively harsh, no It is easy to industrial application, excessively limits to.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, a kind of preparation method of high yield ceramics is provided.It should Method is directly modified the presoma of low-yield, to improve its ceramic yield, the method has easy to operate, can advise greatly Mould uses, and fundamentally solves the problems, such as presoma low yield.
Another object of the present invention is to provide the high yield ceramics of above method preparation.
A further object of the present invention is to provide the applications of above-mentioned high yield ceramics.
The purpose of the present invention is realized by following technical proposals:
A kind of preparation method of high yield ceramics, comprises the following specific steps that:
S1. it is suppressed after presoma raw material being pulverized sieving, 300~800 DEG C of heat treatment, obtains under protective atmosphere Modified presoma;
S2., suppressed after modified presoma to be carried out to pulverizing sieving again, under vacuum or protective atmosphere 800~1200 DEG C into Row cracking obtains high yield ceramics.
Preferably, precursor material described in step S1 is Polycarbosilane or polysilazane, the pottery of the precursor material Porcelain yield is 10~50%.
Preferably, the time of heat treatment described in step S1 is 0.5~2h.
Preferably, the time of cracking described in step S2 is 0.5~2h.
Preferably, yield ceramic described in step S2 is 80~99%.
Preferably, oxygen content ceramic described in step S2 is 0.01~0.2wt%;The partial size of particle is in the ceramics 0.01~10 μm.
Preferably, protective atmosphere described in step S1 and S2 is nitrogen or argon gas.
A kind of high yield ceramics, the high yield ceramics are made by the method.
Preferably, the yield of the high yield ceramics is 80~99%;The partial size of particle is 0.01~10 μ in the ceramics m。
Application of the high yield ceramics in increasing material manufacturing, aerospace or nuclear energy field.
Compared with prior art, the invention has the following advantages:
1. ceramics of the invention are using low-yield ceramic forerunner as raw material, by Cold pretreatment early period, at heat Reason carries out strand adjustment, significantly improves strand presoma yield adjusted, then pretreated ceramic forerunner is passed through Cracking processing, is remarkably improved the yield of ceramic particle.
2. the present invention by being directly modified to low-yield presoma, largely improves the yield of presoma, should Method is simple, can scale use, it is at low cost.
3. the ceramic particle purity of present invention cracking preparation is higher, size tunable.
Detailed description of the invention
Fig. 1 is the thermogravimetric analysis figure of the modified presoma of embodiment 1.
Fig. 2 is the XRD diagram of the SiC ceramic presoma of embodiment 1.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention. Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
1. being pressed into Φ after Polycarbosilane is pulverized sieving using Polycarbosilane as presoma raw material (yield 40%) 20mm high 10mm sample, is put into tube furnace in a nitrogen atmosphere, carries out heat treatment 1h at 500 DEG C, obtains modified presoma;
2. modified presoma is carried out again after pulverizing sieving, identical dimensioned blocks are pressed into, are carried out in tube furnace 1200 DEG C of heat preservation 1h cracking, cracking atmosphere are nitrogen, and SiC ceramic is made.
Thermogravimetric analysis is carried out to the modified presoma of gained in step 1, as shown in Figure 1, yield is from original 40% at this time It is increased to 89%;The XRD of SiC ceramic is obtained after cracking as shown in Fig. 2, the object of SiC ceramic is mutually SiC, oxygen content 0.05%, Partial size is 5 μm.
Embodiment 2
The polysilazane for being 20% using yield is precursor material, after carrying out 300 DEG C of heat preservation 0.5h heat treatment, yield at this time It is increased to 80%, is continued after 800 DEG C of progress 0.5h cracking, Si is made3N4Ceramics.Gained Si3N4Ceramics oxygen content be 0.1%, diameter of particle is 0.02 μm.
Embodiment 3
The Polycarbosilane for being 30% using yield is precursor material, and after carrying out 700 DEG C of heat preservation 2h heat treatments, yield is mentioned at this time Height continues after 1000 DEG C of progress 0.5h cracking to 95%, and SiC ceramic is made.The object for obtaining SiC ceramic is mutually SiC, oxygen content It is 0.05%, diameter of particle is 0.1 μm.
Embodiment 4
The polysilazane for being 50% using yield is precursor material, after carrying out 600 DEG C of heat preservation 0.5h heat treatment, yield at this time It is increased to 85%, is continued after 900 DEG C of progress 0.5h cracking, SiC ceramic is made.The object for obtaining SiC ceramic is mutually SiC, and oxygen contains Amount is 0.01%, and diameter of particle is 0.05 μm.
Embodiment 5
The polysilazane for being 10% using yield is precursor material, after carrying out 500 DEG C of heat preservation 0.5h heat treatment, yield at this time It is increased to 80%, is continued after 1200 DEG C of progress 0.5h cracking, SiC ceramic is made.The object for obtaining SiC ceramic is mutually SiC, and oxygen contains Amount is 0.1%, and diameter of particle is 0.02 μm.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (10)

1. a kind of preparation method of high yield ceramics, which is characterized in that comprise the following specific steps that:
S1. it is suppressed after presoma raw material being pulverized sieving, 300~800 DEG C of heat treatment, is modified under protective atmosphere Presoma;
S2. modified presoma is carried out suppressing after pulverizing sieving again, is split for 800~1200 DEG C under vacuum or protective atmosphere Solution obtains high yield ceramics.
2. the preparation method of high yield ceramics according to claim 1, which is characterized in that presoma described in step S1 is former Material is Polycarbosilane or polysilazane, and the ceramic yield of the precursor material is 10~50%.
3. the preparation method of high yield ceramics according to claim 1, which is characterized in that heat treatment described in step S1 Time is 0.5~2h.
4. the preparation method of high yield ceramics according to claim 1, which is characterized in that cracking described in step S2 when Between be 0.5~2h.
5. the preparation method of high yield ceramics according to claim 1, which is characterized in that ceramic production described in step S2 Rate is 80~99%.
6. the preparation method of high yield ceramics according to claim 1, which is characterized in that ceramic oxygen described in step S2 Content is 0.01~0.2wt%;The partial size of particle is 0.01~10 μm in the ceramics.
7. the preparation method of high yield ceramics according to claim 1, which is characterized in that protected described in step S1 and S2 Atmosphere is nitrogen or argon gas.
8. a kind of high yield ceramics, which is characterized in that the high yield ceramics are by the described in any item methods of claim 1-7 It is made.
9. high yield according to claim 8 ceramics, which is characterized in that the yield of the high yield ceramics for 80~ 99%;The partial size of particle is 0.01~10 μm in the ceramics.
10. application of the high yield ceramics described in claim 8 or 9 in increasing material manufacturing, aerospace or nuclear energy field.
CN201910717528.3A 2019-08-05 2019-08-05 A kind of high yield ceramics and its preparation method and application Pending CN110511034A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112759410A (en) * 2021-01-06 2021-05-07 中广核研究院有限公司 Silicon carbide ceramic connection method and silicon carbide cladding
CN113979784A (en) * 2020-11-23 2022-01-28 航天特种材料及工艺技术研究所 High-density ceramic matrix composite and preparation method thereof

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CN101215156A (en) * 2008-01-18 2008-07-09 天津大学 Silicon-oxygen-carbon ceramic products and preparing method thereof
CN101348370A (en) * 2008-09-11 2009-01-21 中国人民解放军国防科学技术大学 Precursor solution of carbide ceramic, carbide ceramic and preparation thereof
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CN109576821A (en) * 2019-01-28 2019-04-05 江西嘉捷信达新材料科技有限公司 High ceramic yield Polycarbosilane presoma and its preparation method and application

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CN101215154A (en) * 2008-01-18 2008-07-09 天津大学 Carbon content controllable silicon-containing ceramic and preparing method thereof
CN101215156A (en) * 2008-01-18 2008-07-09 天津大学 Silicon-oxygen-carbon ceramic products and preparing method thereof
CN101348370A (en) * 2008-09-11 2009-01-21 中国人民解放军国防科学技术大学 Precursor solution of carbide ceramic, carbide ceramic and preparation thereof
CN102660030A (en) * 2012-05-14 2012-09-12 浙江理工大学 Preparation method of Si-C-N ceramic precursor
CN104177621A (en) * 2014-08-14 2014-12-03 中国科学院化学研究所 Novel liquid polycarbosilane as well as preparation method and application thereof
CN104291791A (en) * 2014-09-24 2015-01-21 西安交通大学 Preparation method of amorphous SiOC ceramic powder
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113979784A (en) * 2020-11-23 2022-01-28 航天特种材料及工艺技术研究所 High-density ceramic matrix composite and preparation method thereof
CN112759410A (en) * 2021-01-06 2021-05-07 中广核研究院有限公司 Silicon carbide ceramic connection method and silicon carbide cladding

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Application publication date: 20191129