CN106278284A - A kind of method utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material - Google Patents
A kind of method utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material Download PDFInfo
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Abstract
The present invention relates to a kind of method utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material, belong to insulant preparation field.Boron nitride preparation process is first by BN original washing powder body and additive and sintering aid mixing granulation；Then mixed powder is loaded in ring-shaped graphite mould, carry out substep hot pressed sintering；Boron nitride ceramic material is obtained after sintering.In the method, the technique of hot pressed sintering includes that cryogenic vacuum keeps step, middle temperature nitrogen pressure holding step and high temperature inert atmosphere pressure holding step step by step；By this technique, gaseous impurity can be effectively facilitated and discharge, improve consistency and the intensity of boron nitride ceramic material.
Description
Technical field
A kind of method utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material of the present invention, belongs to insulation material
Material preparation field.
Background technology
Boron nitride is commonly called as white graphite, characteristic to graphite is similar and quality is pure white, there are two kinds of crystal formations: six sides with cube, logical
Often in hexagonal structure.Under the high temperature specific condition with supertension, hexagonal structure crystal formation can be converted into cubic.Wherein six side
Boron nitride range is extensive, and its powder can be as excellent lubricant and releasing agent, and pottery can be used as melting evaporated metal
Crucible, boat, liquid metal conveying pipe, rocket nozzles, high power device base, semiconductor element doped source, and various
High temperature (high pressure, high frequency) insulating radiation parts.
The preparation method of hexagonal boron nitride includes cold-press method and pressure sintering, the ceramic density that wherein prepared by pressure sintering at present
The advantages such as height, intensity are high, mature production technology are used widely.As 103626498A discloses a kind of boron nitride ceramics spray
Mouth, adds carborundum, zirconium oxide and other additives in boron nitride, thus improves the service life of boron nitride ceramics；
103922773A discloses a kind of thin strap continuous casting boron nitride pottery, adds aluminium nitride powder, magnalium in hexagonal boron nitride
Spinelle, other additives such as mullite, improve the thermal shock resistance of boron nitride ceramics and reduce thermal conductivity；104193341A
Disclose the preparation method of a kind of hexagonal boron nitride pottery, first use cold moudling, the most in air atmosphere and nitrogen gas
Carry out pressureless sintering under atmosphere to prepare, thus improve the heat conductivity of boron nitride ceramics, reduce production cost.
In conventional boron nitride preparation method, graphite jig is used to carry out blank forming, owing to relating to pressure and temperature
Higher, graphite jig is susceptible to problems of crack, has a strong impact on the preparation efficiency of material.
Summary of the invention
The present invention is by providing the novel graphite mould of a kind of boron nitride, to improve the preparation of boron nitride ceramic material
Efficiency.
A kind of method utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material, the method includes following step
Rapid:
(1) by containing additive and the BN original washing powder body mixing granulation wishing burning agent；
(2) mixed powder is loaded in ring-shaped graphite mould, carry out substep hot pressed sintering；
(3) boron nitride ceramic material is obtained after sintering；
In this invention, ring-shaped graphite mould includes internal ring and outer shroud, and between internal ring and outer shroud, gap is 5 ~ 20mm.
Preferably, the technique of hot pressed sintering includes that low temperature keeps step, middle temperature pressure holding step and high temperature pressure holding step；Low
Temperature keeps step to be 500 ~ 800 DEG C, and temperature retention time is 0.5 ~ 2 hour；Middle temperature pressure holding step is 1000 ~ 1500 DEG C, pressure 15 ~
20MPa, the dwell time is 0.5 ~ 2 hour；High temperature pressure holding step is 1600 ~ 1900 DEG C, pressure 16 ~ 25MPa, the dwell time is 1 ~
3 hours；
In the method, low temperature is carried out under vacuo, and middle temperature is carried out in a nitrogen atmosphere, and high temperature is carried out under an inert atmosphere.
In the method, preferred additive includes the one in CaO, SiC, Si3N4, ZrO2, Al2O3, Y2O3 or many
Kind, sintering aid includes B2O3.
More preferably, additive level is 15 ~ 30wt.%, and sintering aid content is 5 ~ 10wt.%, and surplus is BN powder body.
The present invention focuses on multistep pressurize technique, wherein at cold stage, under vacuum atmosphere, and volatile gas
Discharge, at middle thermophase, by heating, be conducive to the gaseous impurity of difficulty volatilization to discharge, thus ensure that final boron nitride ceramics
The purity of material, consistency and intensity.
Composition in the present invention, in addition to main constituent BN, also includes a certain amount of additive and sintering aid.
Combine between the powder body during wherein sintering aid is conducive to sintering process.
In additive, yittrium oxide is classic ceramic material stabilizer, yittrium oxide and the boron nitride in material, zirconium oxide
And carborundum all has sufficiently stable affinity, yittrium oxide mixes and makes ceramic material of the present invention more have excellent resisting
Thermal shock performance, improves bending strength and the fracture toughness of material.
Al2O3 has the strongest cohesive force and resistance to spallation, and the liquid phase that Al2O3 is at high temperature formed can bond effectively
BN.The oxide on Al2O3 Yu SiC surface at high temperature reacts formation aluminosilicate liquid phase, promotes that the sintering of SiC pottery causes
Densification.At high temperature, Al2O3 Yu ZrO2 can produce co-melting phenomenon, improves the uniformity of sintered density.SiC with Si3N4 is the most favourable
Raising in intensity.
In the present invention, graphite jig be annular, ring mould relative to square dies, uniform force in all directions.Graphite
There is certain gap between outer shroud and outer shroud, make internal ring on the basis of high-temperature expansion, it is ensured that the contact between inner and outer ring is tight,
Thus avoid the raising of the problem of Cracking of graphite jig, beneficially production efficiency.
Accompanying drawing explanation
The hot pressed sintering schematic diagram of Fig. 1 boron nitride, wherein 1 is seaming chuck, and 2 is graphite jig, and 3 is push-down head, and 4 is final
The boron nitride ceramics base substrate of molding.
Fig. 2 is graphite jig schematic diagram.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Preparing boron nitride-base powder body, wherein additive is SiC, and content is 20wt.%, and sintering aid is B2O3, and content is 8wt.%, nitrogen
Change boron is surplus, several powder body mix homogeneously.
Mixed powder is loaded in graphite jig, carries out hot pressed sintering.
In hot pressed sintering step, low temperature keeps step to be 600 DEG C, and temperature retention time is 1.5 hours；Middle temperature pressure holding step is
1300 DEG C, pressure 18MPa, the dwell time is 2 hours；High temperature pressure holding step is 1800 DEG C, pressure 20MPa, and the dwell time is 2 little
Time.
Material after being completed by sintering takes out, and obtains boron nitride ceramic material.
Embodiment 2
Preparing boron nitride-base powder body, wherein additive is Si4N3, and content is 20wt.%, and sintering aid is B2O3, and content is 8wt.%,
Boron nitride is surplus, several powder body mix homogeneously.
Mixed powder is loaded in graphite jig, carries out hot pressed sintering.
In hot pressed sintering step, low temperature keeps step to be 800 DEG C, and temperature retention time is 1.5 hours；Middle temperature pressure holding step is
1200 DEG C, pressure 20MPa, the dwell time is 2 hours；High temperature pressure holding step is 1900 DEG C, pressure 18MPa, and the dwell time is 1.5
Hour.
Material after being completed by sintering takes out, and obtains boron nitride ceramic material.
Embodiment 3
Preparing boron nitride-base powder body, wherein additive is CaO, and content is 18wt.%, and sintering aid is B2O3, and content is 8wt.%, nitrogen
Change boron is surplus, several powder body mix homogeneously.
Mixed powder is loaded in graphite jig, carries out hot pressed sintering.
In hot pressed sintering step, low temperature keeps step to be 700 DEG C, and temperature retention time is 1.5 hours；Middle temperature pressure holding step is
1500 DEG C, pressure 18MPa, the dwell time is 2 hours；High temperature pressure holding step is 1900 DEG C, pressure 20MPa, and the dwell time is 1.2
Hour.
Material after being completed by sintering takes out, and obtains boron nitride ceramic material.
Embodiment 4
Preparing boron nitride-base powder body, wherein additive is SiC+Y2O3, and content is respectively 5wt.% and 12wt.%, and sintering aid is
B2O3, content is 8wt.%, and boron nitride is surplus, several powder body mix homogeneously.
Mixed powder is loaded in graphite jig, carries out hot pressed sintering.
In hot pressed sintering step, low temperature keeps step to be 700 DEG C, and temperature retention time is 1.5 hours；Middle temperature pressure holding step is
1400 DEG C, pressure 18MPa, the dwell time is 1.5 hours；High temperature pressure holding step is 1600 DEG C, pressure 20MPa, and the dwell time is 2
Hour.
Material after being completed by sintering takes out, and obtains boron nitride ceramic material.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for those skilled in the art
For Yuan, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any amendment of being made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (4)
1. one kind utilizes the method that ring-shaped graphite mould step sintering prepares boron nitride ceramic material, it is characterised in that described side
Method comprises the following steps:
(1) by containing additive and the BN original washing powder body mixing granulation wishing burning agent；
(2) mixed powder is loaded in ring-shaped graphite mould, carry out substep hot pressed sintering；
(3) boron nitride ceramic material is obtained after sintering；
Described ring-shaped graphite mould includes internal ring and outer shroud, and between internal ring and outer shroud, gap is 5 ~ 20mm.
2. a kind of side utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material as claimed in claim 1
Method, it is characterised in that the technique of described substep hot pressed sintering includes that low temperature keeps step, middle temperature pressure holding step and high temperature pressurize
Step；
Described low temperature keeps step to be 500 ~ 800 DEG C, and temperature retention time is 0.5 ~ 2 hour；
Described middle temperature pressure holding step is 1000 ~ 1500 DEG C, pressure 15 ~ 20MPa, and the dwell time is 0.5 ~ 2 hour；
Described high temperature pressure holding step is 1600 ~ 1900 DEG C, pressure 16 ~ 25MPa, and the dwell time is 1 ~ 3 hour；
In described preparation method, low temperature is carried out under vacuo, and middle temperature is carried out in a nitrogen atmosphere, and high temperature enters under an inert atmosphere
OK.
3. a kind of side utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material as claimed in claim 1
Method, it is characterised in that described additive includes one or more in CaO, SiC, Si3N4, ZrO2, Al2O3, Y2O3, helps burning
Agent is B2O3.
4. a kind of side utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material as claimed in claim 3
Method, it is characterised in that described additive level is 15 ~ 30wt.%, sintering aid content is 5 ~ 10wt.%.
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Cited By (3)
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|---|---|---|---|---|
| CN106938932A (en) * | 2017-03-14 | 2017-07-11 | 南京云启金锐新材料有限公司 | High-purity high-strength degree zirconium oxide silicon nitride composite ceramics and preparation method thereof |
| CN109824368A (en) * | 2018-12-14 | 2019-05-31 | 安泰天龙钨钼科技有限公司 | A kind of method and apparatus of low energy consumption hot pressing production boron nitride-base 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 |
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| CN106938932A (en) * | 2017-03-14 | 2017-07-11 | 南京云启金锐新材料有限公司 | High-purity high-strength degree zirconium oxide silicon nitride composite ceramics and preparation method thereof |
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| 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 |
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