CN105399426A - Preparation method of boron nitride ceramic - Google Patents
Preparation method of boron nitride ceramic Download PDFInfo
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- CN105399426A CN105399426A CN201510785500.5A CN201510785500A CN105399426A CN 105399426 A CN105399426 A CN 105399426A CN 201510785500 A CN201510785500 A CN 201510785500A CN 105399426 A CN105399426 A CN 105399426A
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Abstract
The invention discloses a preparation method of boron nitride ceramic. The method comprises the following three steps: preparing raw boron nitride powder; mixing rare earth oxides and carrying out hot-pressing sintering. The method is simple, feasible and applicable to industrial production; the strength of the boron nitride ceramic can be significantly improved; and the application range is expanded.
Description
Technical field
The present invention relates to boron nitride ceramics production technical field, particularly a kind of preparation method of boron nitride ceramics.
Background technology
Boron nitride is commonly called as white graphite, characteristic and graphite-phase like and quality is pure white, there are two kinds of crystal formations: six sides with cube, be hexagonal structure usually.Under the special conditions of high temperature and ultra-high voltage, hexagonal structure crystal formation can be converted into cubic.Wherein hexagonal boron nitride use range is extensive, its powder can be used as excellent lubricant and releasing agent, and pottery can be used as crucible, boat, liquid metal transfer lime, the rocket nozzles of melting evaporated metal, high power device base, semiconductor element doped source, and various high temperature (high pressure, high frequency) insulating radiation parts.
The preparation method of current hexagonal boron nitride comprises cold press process and pressure sintering, and wherein the ceramic density prepared of pressure sintering is high, intensity is high, and the advantages such as mature production technology are used widely.As CN103626498A discloses a kind of boron nitride ceramics nozzle, in boron nitride, add silicon carbide, zirconium white and other additives, thus improve the work-ing life of boron nitride ceramics; CN103922773A discloses a kind of thin strap continuous casting boron nitride pottery, adds aluminium nitride powder, magnesium-aluminium spinel, other additives such as mullite in hexagonal boron nitride, improves the heat-shock resistance of boron nitride ceramics and reduces thermal conductivity; CN104193341A discloses a kind of preparation method of hexagonal boron nitride pottery, first adopts coldmoulding, then in air atmosphere and carry out pressureless sintering to prepare under nitrogen atmosphere, thus improves the thermal conductivity of boron nitride ceramics, reduces production cost.
The pressure sintering of current routine is prepared in the technique of boron nitride, relates to the shaping of base substrate, heating, and the links of pressurization, long flow path, complex process.Above-mentioned pressureless sintering mode, the ceramic density of preparation is low, is difficult to meet industrial applications, needs to be optimized proportioning raw materials and the preparation technology of boron nitride, thus improves density and the intensity of final pottery.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of boron nitride ceramics, simple, be applicable to suitability for industrialized production, the intensity of final boron nitride ceramics can be significantly improved, widened its use range.
The technical solution adopted for the present invention to solve the technical problems is:
A preparation method for boron nitride ceramics, comprises the following steps:
(1) preparation of the former powder of boron nitride: obtain the former powder of boron nitride after boron nitride powder and additive being mixed;
(2) mixed rare-earth oxide: put into ball mill ball milling after being mixed with oxide nano rare earth by boron nitride raw powder, ball milling terminates post-drying and obtains hot pressing powder;
(3) hot pressed sintering: hot pressing powder is put into graphite jig hot-forming, obtain boron nitride ceramic material after cooling, described hot-forming temperature is 1600-1900 DEG C, and pressure is 20-25MPa.
The preparation of the former powder of boron nitride: boron nitride powder can be boron simple substance nitriding, vapor phase process, existing boron nitride powder prepared by the methods such as boron oxide nitriding.The boron nitride powder prepared is aided with a certain amount of additive to obtain raw material powder required in the present invention, because pure boron nitride powder is difficult to sintering, therefore the present invention adds additive and carrys out acceleration of sintering, wherein boron oxide can improve density and the intensity of boron nitride, and adds moisture resistance and thermal conductivity that calcium oxide and boron oxide can also improve boron nitride prod.
Ball milling is selected to mix boron nitride raw powder and oxide nano rare earth hybrid mode in the present invention, to ensure the stable and even of whole process.
Key of the present invention is the use of oxide nano rare earth, adds Y in traditional method
2o
3deng rare earth oxide, because granularity is comparatively large, and chemical combination difficulty between boron nitride material, be difficult to play obvious performance boost, and the oxide material of Nano grade, owing to having nanoscale, can be good at playing the effect improving intensity.Adding of these rare-earth nano oxides, to improving the sintered density of boron nitride and intensity is very effective, in the present invention, the content of oxide nano rare earth is 0.5 ~ 3%, cross and do not have tough effect at least, and addition is too much, boron nitride ceramics temperature tolerance can be caused to reduce, affect final use.
It is very crucial that step of the present invention (3) controls hot pressing temperature and pressure, hot pressing temperature and hypotony, is difficult to the boron nitride ceramic material that formation is final.
As preferably, boron nitride powder, additive and oxide nano rare earth three summation are 100%, and concrete proportioning is as follows: additive 0.3-4.1%, oxide nano rare earth 0.5-3%, boron nitride powder surplus.
As preferably, described additive is selected from one or more in boron oxide, silicon nitride, aluminium nitride, calcium oxide, zirconium white, silicon carbide.
As preferably, described oxide nano rare earth is selected from one or more in cerium oxide, lanthanum trioxide, yttrium oxide, Praseodymium trioxide, Neodymium trioxide.The present invention selects above-mentioned specific rare-earth nano oxide, can significantly improve sintered density and the intensity of boron nitride.
As preferably, in step (2), the parameter of ball milling is: material: water: the mass ratio of ball is 1:1:3-5, and Ball-milling Time is 3-10 hour.
As preferably, hot-formingly in step (3) to carry out in a nitrogen atmosphere.Adopt nitrogen atmosphere very favourable to keeping the stability of final boron nitride block.
As preferably, the particle diameter of described oxide nano rare earth is 10-80nm.Controlling the particle diameter of oxide nano rare earth is 10-80nm, and chemical combination is easy like this and between boron nitride material, can be good at the effect playing raising intensity and density.
The invention has the beneficial effects as follows: simple, be applicable to suitability for industrialized production, the intensity of final boron nitride ceramics can be significantly improved, widened its use range.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the ordinary method of this area.
Embodiment:
A preparation method for boron nitride ceramics, comprises the following steps:
(1) preparation of the former powder of boron nitride: obtain the former powder of boron nitride after boron nitride powder and additive being mixed.
(2) mixed rare-earth oxide: put into ball mill ball milling by after boron nitride raw powder and oxide nano rare earth (particle diameter 10-80nm), the material of ball milling: water: the mass ratio of ball is 1:1:3-5, Ball-milling Time is 3-10 hour, and ball milling terminates post-drying and obtains hot pressing powder.
(3) hot pressed sintering: hot-forming under hot pressing powder is put into graphite jig nitrogen atmosphere, obtains boron nitride ceramic material after cooling.
The concrete proportioning of composition of boron nitride ceramics and hot compression parameters are in table 1.
Composition prepared by table 1 boron nitride ceramics and hot pressing parameters
As can be seen from Table 1, by adding oxide nano rare earth, the intensity of final boron nitride ceramics can be significantly improved.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (7)
1. a preparation method for boron nitride ceramics, is characterized in that, comprises the following steps:
(1) preparation of the former powder of boron nitride: obtain the former powder of boron nitride after boron nitride powder and additive being mixed;
(2) mixed rare-earth oxide: put into ball mill ball milling after being mixed with oxide nano rare earth by boron nitride raw powder, ball milling terminates post-drying and obtains hot pressing powder;
(3) hot pressed sintering: hot pressing powder is put into graphite jig hot-forming, obtain boron nitride ceramic material after cooling, described hot-forming temperature is 1600-1900 DEG C, and pressure is 20-25MPa.
2. preparation method according to claim 1, is characterized in that: boron nitride powder, additive and oxide nano rare earth three summation are 100%, and concrete proportioning is as follows: additive 0.3-4.1%, oxide nano rare earth 0.5-3%, boron nitride powder surplus.
3. preparation method according to claim 1 and 2, is characterized in that: described additive is selected from one or more in boron oxide, silicon nitride, aluminium nitride, calcium oxide, zirconium white, silicon carbide.
4. preparation method according to claim 1 and 2, is characterized in that: described oxide nano rare earth is selected from one or more in cerium oxide, lanthanum trioxide, yttrium oxide, Praseodymium trioxide, Neodymium trioxide.
5. preparation method according to claim 1 and 2, is characterized in that: in step (2), the parameter of ball milling is: material: water: the mass ratio of ball is 1:1:3-5, and Ball-milling Time is 3-10 hour.
6. preparation method according to claim 1 and 2, is characterized in that: hot-formingly in step (3) carry out in a nitrogen atmosphere.
7. preparation method according to claim 1 and 2, is characterized in that: the particle diameter of described oxide nano rare earth is 10-80nm.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278283A (en) * | 2016-08-04 | 2017-01-04 | 长兴鑫宇耐火材料有限公司 | A kind of step sintering prepares the method for boron nitride ceramic material |
| CN106278284A (en) * | 2016-08-04 | 2017-01-04 | 长兴鑫宇耐火材料有限公司 | A kind of method utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material |
| CN106588027A (en) * | 2016-12-10 | 2017-04-26 | 包头稀土研究院 | Method for manufacturing high-density boron nitride ceramic |
| CN107459355A (en) * | 2017-08-02 | 2017-12-12 | 武汉钢铁有限公司 | A kind of thin-belt casting rolling industrial ceramic material and preparation method thereof |
| CN110430972A (en) * | 2017-02-10 | 2019-11-08 | 圣戈本陶瓷及塑料股份有限公司 | Boron nitride with controlled oxidation boron level |
| CN111410539A (en) * | 2020-03-03 | 2020-07-14 | 哈尔滨工业大学 | Y-Al-Si-O multi-element glass phase reinforced hexagonal boron nitride-based multiphase ceramic and preparation method thereof |
| CN112011182A (en) * | 2020-08-13 | 2020-12-01 | 乳源东阳光氟树脂有限公司 | Polyimide film and preparation method thereof |
| CN112521159A (en) * | 2020-03-20 | 2021-03-19 | 山东晶亿新材料有限公司 | Boron nitride composite ceramic and preparation method and application thereof |
| TWI737739B (en) * | 2016-05-31 | 2021-09-01 | 日商電化股份有限公司 | BN sintered body with excellent corrosion resistance and its manufacturing method |
| CN114315372A (en) * | 2020-09-30 | 2022-04-12 | 山东硅纳新材料科技有限公司 | Preparation process of high-strength h-BN ceramic |
| CN117142863A (en) * | 2023-10-31 | 2023-12-01 | 山东鹏程陶瓷新材料科技有限公司 | Boron nitride ceramic setter plate and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI737739B (en) * | 2016-05-31 | 2021-09-01 | 日商電化股份有限公司 | BN sintered body with excellent corrosion resistance and its manufacturing method |
| CN106278284A (en) * | 2016-08-04 | 2017-01-04 | 长兴鑫宇耐火材料有限公司 | A kind of method utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material |
| CN106278283A (en) * | 2016-08-04 | 2017-01-04 | 长兴鑫宇耐火材料有限公司 | A kind of step sintering prepares the method for boron nitride ceramic material |
| CN106588027A (en) * | 2016-12-10 | 2017-04-26 | 包头稀土研究院 | Method for manufacturing high-density boron nitride ceramic |
| CN110430972A (en) * | 2017-02-10 | 2019-11-08 | 圣戈本陶瓷及塑料股份有限公司 | Boron nitride with controlled oxidation boron level |
| CN107459355A (en) * | 2017-08-02 | 2017-12-12 | 武汉钢铁有限公司 | A kind of thin-belt casting rolling industrial ceramic material and preparation method thereof |
| CN107459355B (en) * | 2017-08-02 | 2020-05-26 | 武汉钢铁有限公司 | Industrial ceramic material for casting and rolling thin strip and preparation method thereof |
| CN111410539A (en) * | 2020-03-03 | 2020-07-14 | 哈尔滨工业大学 | Y-Al-Si-O multi-element glass phase reinforced hexagonal boron nitride-based multiphase ceramic and preparation method thereof |
| CN111410539B (en) * | 2020-03-03 | 2023-02-21 | 哈尔滨工业大学 | Y-Al-Si-O multi-element glass phase reinforced hexagonal boron nitride-based multiphase ceramic |
| CN112521159A (en) * | 2020-03-20 | 2021-03-19 | 山东晶亿新材料有限公司 | Boron nitride composite ceramic and preparation method and application thereof |
| CN112011182A (en) * | 2020-08-13 | 2020-12-01 | 乳源东阳光氟树脂有限公司 | Polyimide film and preparation method thereof |
| CN114315372A (en) * | 2020-09-30 | 2022-04-12 | 山东硅纳新材料科技有限公司 | Preparation process of high-strength h-BN ceramic |
| CN117142863A (en) * | 2023-10-31 | 2023-12-01 | 山东鹏程陶瓷新材料科技有限公司 | Boron nitride ceramic setter plate and preparation method thereof |
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Application publication date: 20160316 |