CN106882771A - A kind of method of hexagonal boron nitride regrowth - Google Patents
A kind of method of hexagonal boron nitride regrowth Download PDFInfo
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- CN106882771A CN106882771A CN201510938857.2A CN201510938857A CN106882771A CN 106882771 A CN106882771 A CN 106882771A CN 201510938857 A CN201510938857 A CN 201510938857A CN 106882771 A CN106882771 A CN 106882771A
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- boron nitride
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- regrowth
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a kind of method of hexagonal boron nitride regrowth.Using high-temperature vacuum furnace as synthesis device, the boron nitride of particle diameter grows as raw material under 1500-2200 DEG C of vacuum condition using in difference, and particle diameter increases boron nitride after the reaction, is hexagonal structure, realizes the regrowth of boron nitride.Load in graphite crucible after boron nitride is compacted, load in high temperature furnace, inert gas or application of vacuum are passed through to stove interior circulation, be to slowly warm up to temperature, after reaction 4-24h, material in cooling stove obtains regrowth hexagonal boron nitride.The beneficial effects of the invention are as follows：Hexagonal boron nitride particle diameter is improved using high-temperature vacuum furnace, solves the problems, such as that boron nitride aborning fix by particle diameter, disclosure satisfy that demand of the different field to boron nitride particle diameter.
Description
Technical field
The method of hexagonal boron nitride regrowth is made as synthesis device with high-temperature vacuum furnace the invention discloses a kind of.
Background technology
Hexagonal boron nitride because its crystal formation is similar with graphite and white powder is referred to as white graphite, in the condition of superhigh temperature
Under (2800 DEG C) still show good performance, be a kind of new inorganic material, with preferable application prospect, at present
It was found that application field include that releasing agent, high-temperature lubricant, composite ceramic material additive, synthesizing cubic boron nitride, atom are anti-
Answer structural material, aircraft, spout of rocket engine of heap etc..With the continuous expansion of boron nitride material application field and demand
Amount constantly expands, and high-quality, many particle diameters, polymorphous synthetic route turn into the direction of scientific and technical personnel's research.At present, six sides are synthesized
The method of boron nitride is high-temperature synthesis, and product cut size is more fixed, and limits its application in different field.
The invention provides using high-temperature vacuum furnace as synthesis device, in 1500-2200 DEG C, vacuum or inert gas conditions
Lower growth, the method for making hexagonal boron nitride regrowth, the hexagonal boron nitride particle diameter for obtaining increases obvious.
The content of the invention
Solved the above problems it is an object of the invention to provide a kind of method of hexagonal boron nitride regrowth, by high temperature bar
Under part and under vacuum or inert gas reaction atmosphere, regrow the particle diameter of hexagonal boron nitride, different size hexagonal boron nitride
Particle diameter improve at least 10%.
The technical scheme is that：
A kind of method of hexagonal boron nitride regrowth, using high-temperature vacuum furnace as consersion unit, be with hexagonal boron nitride
Raw material, loads in graphite crucible after hexagonal boron nitride is compacted, and loads in high-temperature vacuum furnace, and inert gas is passed through to stove interior circulation
Or application of vacuum, 1500-2200 DEG C, after insulation 4-24h is warming up to 50-200 DEG C of speed per hour, material in cooling stove is obtained
To the hexagonal structure hexagonal boron nitride of the uniform particle diameter of regrowth.
Another heating mode is：First 3 hours, in-furnace temperature at the uniform velocity rose to 800 DEG C, and 3-6 hours, in-furnace temperature was at the uniform velocity
1400 DEG C are risen to, 1500-1700 DEG C is at the uniform velocity risen within 6-7 hours, 1700-1900 DEG C is at the uniform velocity risen within 7-8 hours, 8-9 hours at the uniform velocity
1900-2100 DEG C is risen to, 2100-2200 DEG C is at the uniform velocity risen within 9-10 hours, continues to be incubated 4-24 hours.
Described hexagonal boron nitride is the boron nitride with laminated structure, hexagonal structure.
Inert gas is passed through to consersion unit circulation or to consersion unit application of vacuum, described inert gas is helium,
Argon gas, neon, vacuum degree control is being not more than -0.1MPa during application of vacuum.
Beneficial effects of the present invention：
1) the big particle diameter hexagonal boron nitride that the regrowth process of hexagonal boron nitride of the present invention is obtained, product content is high, crystal formation
Good, uniform particle sizes solve the limitation that current product cut size is used different field；
2) in building-up process, using the simple process of a step high―temperature nuclei, the regrowth of hexagonal boron nitride is realized；
3) the hexagonal boron nitride impurity content by high―temperature nuclei is small, without other treatment are carried out, reduces the life of product
Produce cost.
4) reaction condition of the present invention is simple gentle controllable, is suitable for industrialized production.
Brief description of the drawings
Fig. 1 is the size distribution of the specific embodiment of the invention 1 and cumulative chart.
Fig. 2 is the size distribution of the specific embodiment of the invention 2 and cumulative chart.
Fig. 3 is the size distribution of the specific embodiment of the invention 3 and cumulative chart.
Fig. 4 is the size distribution of the specific embodiment of the invention 4 and cumulative chart.
Fig. 5 is the size distribution of the specific embodiment of the invention 5 and cumulative chart.
Specific embodiment
The present invention is expanded on further below by embodiment, but embodiment will not be limited the invention.In the present invention
The technological parameter enumerated of technical scheme bound value, the interval product that can realize application claims.
Embodiment 1
It is during 1.1 microns of hexagonal boron nitrides add graphite crucibles, to be put into high-temperature vacuum furnace after compacting by 20 kilograms of particle diameters,
Bell is covered tightly, with vacuum pumped furnace air, is replaced to argon gas is passed through in stove, kept argon gas circulation to be passed through in stove afterwards and protected
Shield, opening heating makes in-furnace temperature be slowly increased to 1500 DEG C, and programming rate is first 3 hours, and in-furnace temperature at the uniform velocity rises to 800 DEG C,
3-6 hours, in-furnace temperature at the uniform velocity rose to 1400 DEG C, at the uniform velocity rose within 6-6.5 hours 1500 DEG C, and constant temperature is after 5 hours, close heating,
Material in cooling stove, after being cooled to room temperature, obtains white puff boron nitride powder, and product cut size is risen to by 1.1 microns
2.33 microns.
Product test
Tester is shown in Fig. 1, table 6 for laser fineness gage result.
Table 1 is size distribution and the content accumulation of embodiment 1.
| Particle diameter μm | 0.11 | 0.21 | 0.40 | 0.76 | 1.44 | 2.75 | 5.23 | 9.96 | 18.95 | 36.07 |
| Content % | 0.12 | 4.81 | 15.14 | 30.03 | 42.84 | 52.58 | 63.82 | 79.64 | 96.70 | 100 |
Embodiment 2
It is during 4.8 microns of hexagonal boron nitrides add graphite crucibles, to be put into high-temperature vacuum furnace after compacting by 22 kilograms of particle diameters,
Bell is covered tightly, with vacuum pumped furnace air, is replaced to argon gas is passed through in stove, kept argon gas circulation to be passed through in stove afterwards and protected
Shield, opening heating makes in-furnace temperature be slowly increased to 1650 DEG C, and programming rate is first 3 hours, and in-furnace temperature at the uniform velocity rises to 800 DEG C,
3-6 hours, in-furnace temperature at the uniform velocity rose to 1400 DEG C, at the uniform velocity rose within 6-7 hours 1650 DEG C, and constant temperature is after 18 hours, closed heating, cold
But material in stove, after being cooled to room temperature, obtains white puff boron nitride powder, and it is micro- that product cut size rises to 8.9 by 4.8 microns
Rice.
Product test
Tester is shown in Fig. 2, table 6 for laser fineness gage result.
Table 2 is size distribution and the content accumulation of embodiment 2.
| Particle diameter μm | 0.1 | 0.2 | 0.4 | 0.9 | 2 | 4 | 7 | 15 | 30 | 62 |
| Content % | 0 | 2.08 | 7.94 | 17.15 | 22.75 | 30.42 | 42.26 | 70.18 | 95.48 | 100 |
Embodiment 3
It is during 9 microns of hexagonal boron nitrides add graphite crucibles, to be put into high-temperature vacuum furnace after compacting by 22 kilograms of particle diameters, covers
Tight bell, with vacuum pumped furnace air, replaces to argon gas is passed through in stove, keeps argon gas circulation to be passed through in stove afterwards and is protected
Shield, opening heating makes in-furnace temperature be slowly increased to 1750 DEG C, and programming rate is first 3 hours, and in-furnace temperature at the uniform velocity rises to 800 DEG C,
3-6 hours, in-furnace temperature at the uniform velocity rose to 1400 DEG C, at the uniform velocity rises within 6-7 hours 1500-1700 DEG C, at the uniform velocity rises within 6-7.5 hours
1750 DEG C, constant temperature closes heating, cools down material in stove after 7 hours, after being cooled to room temperature, obtains white puff boron nitride powder
End, product cut size rises to 14.82 microns by 9 microns.
Product test
Tester is shown in Fig. 3, table 6 for laser fineness gage result.
Table 3 is size distribution and the content accumulation of embodiment 3.
| Particle diameter μm | 0.1 | 0.2 | 0.5 | 1 | 2 | 4 | 9 | 19 | 41 | 85 |
| Content % | 0 | 1.74 | 8.51 | 13.88 | 16.57 | 21.05 | 34.04 | 60.62 | 94.47 | 100 |
Embodiment 4
It is during 21.5 microns of hexagonal boron nitrides add graphite crucibles, high-temperature vacuum furnace to be put into after compacting by 20 kilograms of particle diameters
In, bell is covered tightly, vavuum pump is opened, after vacuum reaches -0.1MPa in stove, opening heating is slowly increased to in-furnace temperature
1750 DEG C, programming rate is first 3 hours, and in-furnace temperature at the uniform velocity rises to 800 DEG C, and 3-6 hours, in-furnace temperature at the uniform velocity rose to 1400
DEG C, 1750 DEG C are at the uniform velocity risen within 6-7 hours, constant temperature closes heating, cools down material in stove after 6 hours, after being cooled to room temperature, obtains
To white puff boron nitride powder, product cut size rises to 29.49 microns by 21.5 microns.
Product test
Tester is shown in Fig. 4, table 6 for laser fineness gage result.
Table 4 is size distribution and the content accumulation of embodiment 4.
| Particle diameter μm | 0.3 | 0.6 | 1 | 2 | 4 | 7 | 14 | 26 | 50 | 95 |
| Content % | 0.03 | 0.75 | 1.52 | 2.07 | 3.39 | 6.35 | 16.82 | 42.25 | 84.73 | 100 |
Embodiment 5
It is during 27 microns of hexagonal boron nitrides add graphite crucibles, to be put into high-temperature vacuum furnace after compacting by 20 kilograms of particle diameters,
Bell is covered tightly, vavuum pump is opened, after vacuum reaches -0.1MPa in stove, opening heating makes in-furnace temperature be slowly increased to 2100
DEG C, programming rate is first 3 hours, and in-furnace temperature at the uniform velocity rises to 800 DEG C, and 3-6 hours, in-furnace temperature at the uniform velocity rose to 1400 DEG C, 6-7
Hour at the uniform velocity rises to 1500-1700 DEG C, at the uniform velocity rises within 7-8 hours 1850 DEG C, and constant temperature closes heating, cools down thing in stove after 6 hours
Material, after being cooled to room temperature, obtains white puff boron nitride powder, and product cut size rises to 35.45 microns by 27 microns.
Product test
Tester is shown in Fig. 5, table 6 for laser fineness gage result.
Table 5 is size distribution and the content accumulation of embodiment 5.
| Particle diameter μm | 0.4 | 0.7 | 1 | 2 | 4 | 8 | 16 | 30 | 56 | 105 |
| Content % | 0.06 | 0.52 | 0.8 | 0.92 | 1.68 | 4.42 | 13.91 | 39.17 | 82 | 100 |
The experimental result table of comparisons of table 6
| Embodiment | Boron nitride content % | ||
| Embodiment 1 | 99.2 | 0.4 | 2.33 |
| Embodiment 2 | 99.7 | 0.2 | 8.9 |
| Embodiment 3 | 99.5 | 0.3 | 14.82 |
| Embodiment 4 | 99.4 | 0.3 | 29.49 |
| Embodiment 5 | 99.1 | 0.5 | 35.45 |
Claims (5)
1. a kind of method of hexagonal boron nitride regrowth, it is characterised in that using high-temperature vacuum furnace as consersion unit, with six sides
Boron nitride is raw material, and hexagonal boron nitride compacting is placed in high-temperature vacuum furnace, and inert gas is passed through to high-temperature vacuum furnace interior circulation
Or application of vacuum, it is warming up to 1500-2200 DEG C with 50-200 DEG C of speed per hour；After insulation 4-24h, material in cooling stove is obtained
To the hexagonal structure hexagonal boron nitride of the uniform particle diameter of regrowth.
2. a kind of method of hexagonal boron nitride regrowth, it is characterised in that using high-temperature vacuum furnace as consersion unit, with six sides
Boron nitride is raw material, and hexagonal boron nitride compacting is placed in high-temperature vacuum furnace, and inert gas is passed through to high-temperature vacuum furnace interior circulation
Or application of vacuum, heating mode：First 3 hours, in-furnace temperature at the uniform velocity rose to 800 DEG C, and 3-6 hours, in-furnace temperature at the uniform velocity rose to
1400 DEG C, 1500-1700 DEG C is at the uniform velocity risen within 6-7 hours, at the uniform velocity rise within 7-8 hours 1700-1900 DEG C, at the uniform velocity risen within 8-9 hours
1900-2100 DEG C, at the uniform velocity rise to 2100-2200 DEG C within 9-10 hours；After insulation 4-24h, material in cooling stove obtains regrowth
The hexagonal structure hexagonal boron nitride of uniform particle diameter.
3. method according to claim 1 and 2, it is characterised in that be passed through inert gas or to anti-to consersion unit circulation
Answer equipment vacuum to process, described inert gas is helium, argon gas, neon, during application of vacuum vacuum degree control being not more than-
0.1MPa。
4. method according to claim 1 and 2, it is characterised in that described hexagonal boron nitride is with laminated structure, six
The boron nitride of prismatic crystal type.
5. method according to claim 3, it is characterised in that described hexagonal boron nitride is with laminated structure, six sides
The boron nitride of crystal formation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2018104260A (en) * | 2016-12-28 | 2018-07-05 | 昭和電工株式会社 | Hexagonal boron nitride powder, method for producing the same, resin composition and resin sheet |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61168570A (en) * | 1985-01-18 | 1986-07-30 | 川崎製鉄株式会社 | Boron nitride sintered body and manufacture |
| JPS62100403A (en) * | 1985-10-28 | 1987-05-09 | Kawasaki Steel Corp | Production of fine powder of hexagonal boron nitride having high purity |
| JP2010037123A (en) * | 2008-08-04 | 2010-02-18 | Kaneka Corp | Method for producing hexagonal boron nitride |
-
2015
- 2015-12-15 CN CN201510938857.2A patent/CN106882771A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61168570A (en) * | 1985-01-18 | 1986-07-30 | 川崎製鉄株式会社 | Boron nitride sintered body and manufacture |
| JPS62100403A (en) * | 1985-10-28 | 1987-05-09 | Kawasaki Steel Corp | Production of fine powder of hexagonal boron nitride having high purity |
| JP2010037123A (en) * | 2008-08-04 | 2010-02-18 | Kaneka Corp | Method for producing hexagonal boron nitride |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2018104260A (en) * | 2016-12-28 | 2018-07-05 | 昭和電工株式会社 | Hexagonal boron nitride powder, method for producing the same, resin composition and resin sheet |
| US11305993B2 (en) | 2016-12-28 | 2022-04-19 | Showa Denko K.K. | Hexagonal boron nitride powder, method for producing same, resin composition and resin sheet |
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Application publication date: 20170623 |