CN109293369A - A kind of preparation method of the boron nitride ceramics of low oxygen content - Google Patents
A kind of preparation method of the boron nitride ceramics of low oxygen content Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the boron nitride ceramics of low oxygen content, hot pressed sintering is carried out again after boron nitride powder is heat-treated under atmosphere, the volatilization that nitrogen promotes boron oxide is passed through during hot pressed sintering, so that the boron nitride ceramics of low oxygen content be made, oxygen content is lower than 0.1wt%.This method simple process, performance are stablized, and production cost is low.
Description
Technical field
The invention belongs to ceramic manufacturing fields, and in particular to a kind of preparation method of the boron nitride ceramics of low oxygen content.
Background technique
With the high speed development of great power LED technology, the aluminium nitride substrate of high heat conductance becomes indispensable in LED production
A kind of few raw material.In the sintering process of aluminium nitride ceramics, due to sintering temperature height, and very to the oxygen content in atmosphere
Sensitivity does load bearing board using heating element of tungsten and metal tungsten product, though can avoid the pollution of oxygen, tungsten product price is high, and density is big,
It is inconvenient, carbon-graphite heater is currently mainly used, graphite felt makees vacuum/inspiration sintering furnace of thermal insulation material, uses boron nitride
Crucible is as setting material.However, since the residual quantity of oxygen in general business boron nitride powder is about between 0.5-1.5wt%,
Oxygen residual is basically unchanged in ceramics after hot pressed sintering.Remaining oxygen can be volatilized release in the form of boron oxide under high temperature, be passed through
When boron nitride ceramics crucible sintering the tape casting prepares aluminium nitride or silicon nitride board, curtain coating plate is often mounted in boron nitride box
In son, prolongs slab since a crucible box cannot fill too many laminar flow, in order to improve efficiency, need to do in boron nitride crucible box
It is high at 20-30 millimeters, it is then stacked in sintering furnace, in such a stove, there are many boron nitride crucible box quantity, boron nitride
Residual oxygen in crucible evaporates during sintered aluminum nitride or silicon nitride board to be polluted, and product can be seriously affected
The performances such as thermal conductivity.Therefore the hot pressed boron product of hypoxemia amount is needed to meet the requirements production requirement.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of the boron nitride ceramics of low oxygen content, using hot pressed sintering skill
Art, by the regulation of atmosphere in the pretreatment and sintering process to boron nitride powder, the oxygen substantially reduced in boron nitride ceramics contains
Amount, sintered boron nitride oxygen content are lower than 0.1wt%.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of preparation method of the boron nitride ceramics of low oxygen content, comprising the following steps:
(1) powder pre-processes: hexagonal boron nitride powder being carried out ball milling dispersion, the powder after ball milling is sieved and is dried；
(2) it powder pre-burning: is placed in boron nitride crucible after the powder after drying is smashed to pieces, then boron nitride crucible is placed in atmosphere
Pre-burning is heated in sintering furnace, oxygen content is less than 0.1wt% in the powder after pre-burning；
(3) powder secondary ball milling: the powder after pre-burning is subjected to secondary ball milling dispersion, the powder after secondary ball milling is sieved and is done
It is dry；
(4) it is burnt into: the powder after secondary ball milling being sintered in hot pressing furnace, obtains the boron nitride ceramics of hypoxemia amount.
Further, hexagonal boron nitride powder is pure boron nitride powder in step (1), and average grain diameter is less than 5 μm.
Further, the ball-milling medium in step (1) and step (3) is alcohol, and Ball-milling Time is 4 ~ for 24 hours.
Further, drying temperature is 80 DEG C in step (1) and step (3), and drying time is 2 ~ for 24 hours.
Further, boron nitride crucible purity is greater than 99% in step (2), and powder piling height in boron nitride crucible is small
In 3mm.
Further, atmosphere employed in step (2) is one of vacuum, nitrogen, inert gas, heats pre-burning temperature
Degree is 1500 ~ 2200 °C, and the time is 1 ~ 12h.
Further, the mistake sieve size in step (3) is less than 200 mesh.
Further, the sintering processing in step (4) is hot pressed sintering, and sintering temperature is 1800-2200 °C, sintering time
For 2-12h, application pressure is 20-100MPa.
Further, the sintering atmosphere in step (4) is vacuum, is filled with nitrogen after temperature rises to 1200 °C, until
Sintering terminates.
Further, the density of sintered boron nitride ceramics is 1.6-2.1g/cm in step (4)3, bending strength 8-
30MPa, oxygen content are lower than 0.1wt%.
Beneficial effects of the present invention:
(1) present invention uses hot pressing and sintering technique, by the regulation of atmosphere in the pretreatment and sintering process to boron nitride powder,
The oxygen content of powder after pretreatment is reduced to 0.1wt% hereinafter, and guaranteeing the oxygen of the boron nitride ceramics in subsequent sintering process
Content is less than 0.1wt%；
(2) boron nitride ceramics of the method for the present invention preparation is with good performance, density 1.6-2.1g/cm3, bending strength is
8-30MPa。
(3) the method for the present invention process is simple, easily controllable, and good process repeatability, cost is relatively low.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, the present invention will be further described for following instance, but
It is not used to limit the scope of the present invention.
Embodiment 1
(1) hexagonal boron nitride powder that average grain diameter is 2 μm is subjected to ball milling dispersion, ball-milling medium is alcohol, and Ball-milling Time is
12 hours.It is 12 hours dry under 80 °C in an oven after powder sieving after ball milling.
(2) it is placed in boron nitride crucible after smashing the powder after drying to pieces, the piling height of powder is 2mm.By crucible
It is placed in atmosphere sintering furnace and is heated to 1800 °C, keep the temperature 10 hours, pre-burning atmosphere is vacuum atmosphere.
(3) powder of pre-burning is subjected to secondary ball milling, ball-milling medium is alcohol, and Ball-milling Time is 12 hours;Secondary ball
Powder after mill is 12 hours dry under 80 °C in an oven after 230 mesh sieves.
(4) powder after secondary ball milling is sintered in hot pressing furnace, sintering temperature is 2100 °C, sintering time 4
Hour, application pressure is 30MPa.First furnace body is vacuumized before heating, is heated to being passed through flowing pure nitrogen gas at 1200 °C, until
Sintering terminates.
(5) sintered boron nitride ceramics surface is ground off into 0.2mm, measuring its density is 1.76g/cm3, bending strength is
12MPa, oxygen content 0.096wt%.
Embodiment 2
(1) hexagonal boron nitride powder that average grain diameter is 0.5 μm is subjected to ball milling dispersion, ball-milling medium is alcohol, Ball-milling Time
It is 8 hours.It is 8 hours dry under 80 °C in an oven after powder sieving after ball milling.
(2) it is placed in boron nitride crucible after smashing the powder after drying to pieces, the piling height of powder is 3mm.By crucible
It is placed in atmosphere sintering furnace and is heated to 2000 °C, keep the temperature 10 hours, pre-burning atmosphere is nitrogen atmosphere.
(3) powder of pre-burning is subjected to secondary ball milling, ball-milling medium is alcohol, and Ball-milling Time is 8 hours.Secondary ball milling
Powder afterwards is 8 hours dry under 80 °C in an oven after 230 mesh sieves；
(4) powder after secondary ball milling is sintered in hot pressing furnace, sintering temperature is 2200 °C, and sintering time is 12 small
When, application pressure is 80MPa.First furnace body is vacuumized before heating, is heated to being passed through flowing pure nitrogen gas at 1200 °C, until burning
Junction beam.
(5) sintered boron nitride ceramics surface is ground off into 0.2mm, measuring its density is 1.94g/cm3, bending strength is
23MPa, oxygen content 0.077wt%.
Comparative example 1
(1) hexagonal boron nitride powder that average grain diameter is 2 μm is subjected to ball milling dispersion, ball-milling medium is alcohol, and Ball-milling Time is
12 hours.It is 12 hours dry under 80 °C in an oven after powder sieving after ball milling.
(2) powder after drying is placed in boron nitride crucible after smashing to pieces, and the piling height of powder is 2mm.Crucible is put
It is placed in atmosphere sintering furnace and is heated to 1300 °C, keep the temperature 10 hours, pre-burning atmosphere is vacuum atmosphere.
(3) powder of pre-burning is subjected to secondary ball milling, ball-milling medium is alcohol, and Ball-milling Time is 12 hours;Secondary ball
Powder after mill is 12 hours dry under 80 °C in an oven after 230 mesh sieves.
(4) powder after secondary ball milling is sintered in hot pressing furnace, sintering temperature is 1700 °C, sintering time 4
Hour, application pressure is 30MPa.First furnace body is vacuumized before heating, is heated to being passed through flowing pure nitrogen gas at 1200 °C, until
Sintering terminates.
(5) sintered boron nitride ceramics surface is ground off into 0.2mm, measuring its density is 1.41g/cm3, bending strength is
6MPa, oxygen content 0.617wt%.
By embodiment 1 and comparative example 1 it is found that when the temperature of burn-in process and sintering process is lower than institute's limiting temperature of the present invention
When, the oxygen content of boron nitride ceramics obtained is much higher than 0.1%, and mechanical property is also relatively poor.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (10)
1. a kind of preparation method of the boron nitride ceramics of low oxygen content, it is characterised in that: the described method comprises the following steps:
(1) powder pre-processes: hexagonal boron nitride powder being carried out ball milling dispersion, the powder after ball milling is sieved and is dried；
(2) it powder pre-burning: is placed in boron nitride crucible after the powder after drying is smashed to pieces, then boron nitride crucible is placed in atmosphere
Pre-burning is heated in sintering furnace to 1500-2200 °C, keeps the temperature 1-12 hours, oxygen content is less than 0.1wt% in the powder after pre-burning；
(3) powder secondary ball milling: the powder after pre-burning is subjected to secondary ball milling dispersion, the powder after secondary ball milling is sieved and is done
It is dry；
(4) it is burnt into: the powder after secondary ball milling is sintered in hot pressing furnace, sintering temperature is 1800-2200 °C, when sintering
Between be 2-12 hour, application pressure be 20-100MPa, obtain the boron nitride ceramics of low oxygen content.
2. a kind of preparation method of the boron nitride ceramics of low oxygen content according to claim 1, it is characterised in that: step
(1) hexagonal boron nitride powder is pure boron nitride powder in, and average grain diameter is less than 5 μm.
3. a kind of preparation method of the boron nitride ceramics of low oxygen content according to claim 1, it is characterised in that: step
(1) and the ball-milling medium in step (3) is alcohol, and Ball-milling Time is 4 ~ for 24 hours.
4. a kind of preparation method of the boron nitride ceramics of low oxygen content according to claim 1, it is characterised in that: step
(1) and in step (3) drying temperature is 80 DEG C, and drying time is 2 ~ for 24 hours.
5. a kind of preparation method of the boron nitride ceramics of low oxygen content according to claim 1, it is characterised in that: step
(2) boron nitride crucible purity is greater than 99% in, and powder piling height in boron nitride crucible is less than 3mm.
6. a kind of preparation method of the boron nitride ceramics of low oxygen content according to claim 1, it is characterised in that: step
(2) atmosphere employed in is one of vacuum, nitrogen, inert gas, and heating calcined temperature is 1500 ~ 2200 °C, the time
For 1 ~ 12h.
7. a kind of preparation method of the boron nitride ceramics of low oxygen content according to claim 1, it is characterised in that: step
(3) the mistake sieve size in is less than 200 mesh.
8. a kind of preparation method of the boron nitride ceramics of low oxygen content according to claim 1, it is characterised in that: step
(4) sintering processing in is hot pressed sintering, and sintering temperature is 1800-2200 °C, sintering time 2-12h, and application pressure is 20-
100MPa。
9. a kind of preparation method of the boron nitride ceramics of low oxygen content according to claim 1, it is characterised in that: step
(4) sintering atmosphere in is vacuum, is filled with nitrogen after temperature rises to 1200 °C, until terminating.
10. a kind of preparation method of the boron nitride ceramics of low oxygen content according to claim 1, it is characterised in that: step
(4) density of sintered boron nitride ceramics is 1.6-2.1g/cm in3, bending strength 8-30MPa, oxygen content is lower than
0.1wt%。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4289503A (en) * | 1979-06-11 | 1981-09-15 | General Electric Company | Polycrystalline cubic boron nitride abrasive and process for preparing same in the absence of catalyst |
| CN1582265A (en) * | 2001-11-02 | 2005-02-16 | 通用电气公司 | Low oxygen cubic boron nitride and its production |
| CN103626498A (en) * | 2013-12-13 | 2014-03-12 | 山东鹏程特种陶瓷有限公司 | Boron nitride based ceramic nozzle and preparation method thereof |
-
2018
- 2018-10-24 CN CN201811246908.5A patent/CN109293369A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4289503A (en) * | 1979-06-11 | 1981-09-15 | General Electric Company | Polycrystalline cubic boron nitride abrasive and process for preparing same in the absence of catalyst |
| CN1582265A (en) * | 2001-11-02 | 2005-02-16 | 通用电气公司 | Low oxygen cubic boron nitride and its production |
| CN103626498A (en) * | 2013-12-13 | 2014-03-12 | 山东鹏程特种陶瓷有限公司 | Boron nitride based ceramic nozzle and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 裴立宅: "《高技术陶瓷材料》", 30 June 2015 * |
| 陈广乐，彭珍珍，范仕刚，刘允超: "热压烧结高纯hBN陶瓷材料及其致密性研究", 《硅酸盐通报》 * |
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