CN109650355A - A kind of method of low temperature preparation hexagonal boron nitride - Google Patents
A kind of method of low temperature preparation hexagonal boron nitride Download PDFInfo
- Publication number
- CN109650355A CN109650355A CN201710681166.8A CN201710681166A CN109650355A CN 109650355 A CN109650355 A CN 109650355A CN 201710681166 A CN201710681166 A CN 201710681166A CN 109650355 A CN109650355 A CN 109650355A
- Authority
- CN
- China
- Prior art keywords
- boron nitride
- low temperature
- hexagonal boron
- urea
- borax
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
A kind of method of low temperature preparation hexagonal boron nitride belongs to field of inorganic nonmetallic material.Specific steps are as follows: boric acid and urea are mixed in a certain ratio first, a small amount of borax is added and makees cosolvent.It is put into crucible after ball milling, 900 DEG C of heat preservation a period of times is warming up in nitrogen atmosphere, then be warming up to 1200~1400 DEG C of progress secondary heat treatments.The boron nitride powder of purity is high, better crystallinity degree, sheet is obtained after washing.The method is at low cost, simple process, is particularly suitable for large-scale production.
Description
Technical field
The invention belongs to the preparation fields of inorganic non-metallic powder, and in particular to a kind of side of low temperature preparation hexagonal boron nitride
Method.
Background technique
Boron nitride (BN) be it is a kind of have excellent performance and the new ceramic material for the potentiality that grow a lot, at present to boron nitride
Research is concentrated mainly on hexagonal phase and cubic phase.Hexagonal boron nitride can generally turn under high temperature (1800 DEG C), high pressure (>=5GPa)
Become cubic boron nitride, cubic boron nitride has the structure of similar diamond, and it is novel fire resistant that hardness, which is only second to diamond,
Superhard material is generally used for production drill bit, grinding tool, high temperature abrasive material and polishing agent etc..Hexagonal boron nitride has thermal coefficient high, swollen
Swollen coefficient is low, corrosion-resistant, good thermal shock, the advantages that good insulating, high temperature lubricating is good, processing performance is good, nontoxic, general to use
Make the structural wood of the additive of the polymer such as plastic resin, the release agent of metal forming, the lubricant of metal wire-drawing, reactor
Material, aluminum evaporation container material, the spout of aircraft engine, high-temp thermal couple protective casing and filler used for cosmetic etc..
The preparation method of hexagonal boron nitride mainly has borax-urea (ammonium chloride) method, hydrothermal synthesis method, borax-melamine
Amine method, chemical vapour deposition technique, high-frequency plasma method etc..The wherein sample of chemical vapor deposition and the preparation of high frequency plasma method
Crystallinity is high, with high purity, but equipment and expensive starting materials, it is difficult to realize large-scale production.Industrial production hexagonal boron nitride is most
It is borax-urea (ammonium chloride) method, it is this method simple process, at low cost, but boron nitride content is not high, low yield, and is tied
The high boron nitride of brilliant degree generally requires 1700 DEG C or more, increases cost.
Summary of the invention
The present invention is to overcome above-mentioned deficiency, using boric acid and urea as major ingredient after further investigation reaction mechanism, is added a small amount of
The well-developed boron nitride powder of purity is high, better crystallinity degree, sheet can be obtained as cosolvent, at 1400 DEG C of highest or less in borax
Body.The technical solution adopted by the present invention is that:
(1) Methods For Purification for recrystallizing technical grade borax and urea, it is pure to reach analysis；
(2) 400 DEG C of heat preservation 0.5h of above-mentioned borax are carried out dehydrating, dewatered borax and urea are dried；
(3) by the weighing by a certain percentage of boric acid and urea, a small amount of borax is added and makees cosolvent, be put into ball mill and be sufficiently mixed
It is even；
(4) above-mentioned mixed raw material is packed into crucible, be put into high temperature furnace, 900 DEG C of heat preservations one are warming up in nitrogen atmosphere
It is warming up to 1200~1400 DEG C of progress secondary heat treatments again after the section time；
(5) washing purification will be carried out after the above-mentioned boron nitride powder grinding being prepared.
Further, the mass ratio of boric acid described in step (3) and urea be 1:(0.75~1.45), borax account for boric acid and
The 0~15% of urea gross mass, hybrid mode are dry-mixed.
Further, crucible described in step (4) is silicon nitride, boron nitride, aluminium nitride and applies in boron nitride coating crucible
One kind, 900 DEG C of soaking times are 0.5~2h, and secondary treatment soaking time is 1~5h.
Further, washing reagent described in step (5) is dehydrated alcohol.
Detailed description of the invention
Fig. 1 is the SEM figure for the non-ball milling of boron nitride powder being prepared using technique of the invention.
Fig. 2 is the XRD diagram for the boron nitride powder being prepared using technique of the invention.
Specific embodiment
Embodiment 1
By after purification, dehydration, drying boric acid and urea 1:0.9 in mass ratio weigh, add boric acid and urea gross mass 8%
Borax as cosolvent, after ball mill it is dry-mixed uniformly.The raw material mixed is fitted into silicon nitride crucible, in high temperature furnace
First 900 DEG C of heat preservations 0.5h, rear 1350 DEG C of heat preservations 2h.With dehydrated alcohol washes clean after the powder grinding being prepared, obtain brilliant
It is mutually the platelet boron nitride powder of 100%-BN, better crystallinity degree, purity is high.
Embodiment 2
By after purification, dehydration, drying boric acid and urea 1:1.45 in mass ratio weigh, add boric acid and urea gross mass
10% borax is dry-mixed uniform after ball mill as cosolvent.The raw material mixed is fitted into silicon nitride crucible, in high temperature
First 900 DEG C of heat preservations 1h, rear 1350 DEG C of heat preservations 2h in furnace.With dehydrated alcohol washes clean after the powder grinding being prepared, obtain
Crystal phase is the platelet boron nitride powder of 100%-BN, better crystallinity degree, purity is high.
Claims (6)
1. a kind of method of low temperature preparation hexagonal boron nitride, which is characterized in that including following key step:
(1) Methods For Purification for recrystallizing technical grade borax and urea, it is pure to reach analysis；
(2) 400 DEG C of heat preservation 0.5h of above-mentioned borax are carried out dehydrating, dewatered borax and urea are dried；
(3) by the weighing by a certain percentage of boric acid and urea, a small amount of borax is added and makees cosolvent, be put into ball mill and be sufficiently mixed
It is even；
(4) above-mentioned mixed raw material is packed into crucible, be put into high temperature furnace, 900 DEG C of heat preservations one are warming up in nitrogen atmosphere
It is warming up to 1200~1400 DEG C of progress secondary heat treatments again after the section time；
(5) washing purification will be carried out after the above-mentioned boron nitride powder grinding being prepared.
2. a kind of method of low temperature preparation hexagonal boron nitride described in accordance with the claim 1, which is characterized in that institute in step (3)
The mass ratio for stating boric acid and urea is 1:(0.75~1.45), borax accounts for the 0~15% of boric acid and urea gross mass.
3. a kind of method of low temperature preparation hexagonal boron nitride described in accordance with the claim 1, which is characterized in that institute in step (3)
It is dry-mixed for stating hybrid mode.
4. a kind of method of low temperature preparation hexagonal boron nitride described in accordance with the claim 1, which is characterized in that institute in step (4)
Stating crucible is one of silicon nitride, boron nitride, aluminium nitride and painting boron nitride coating crucible.
5. a kind of method of low temperature preparation hexagonal boron nitride described in accordance with the claim 1, which is characterized in that step (4) is described
900 DEG C of soaking times are 0.5~2h, and secondary heat treatment soaking time is 1~5h.
6. a kind of method of low temperature preparation hexagonal boron nitride described in accordance with the claim 1, which is characterized in that step (5) is described
Washing reagent is dehydrated alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710681166.8A CN109650355A (en) | 2017-10-11 | 2017-10-11 | A kind of method of low temperature preparation hexagonal boron nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710681166.8A CN109650355A (en) | 2017-10-11 | 2017-10-11 | A kind of method of low temperature preparation hexagonal boron nitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109650355A true CN109650355A (en) | 2019-04-19 |
Family
ID=66108201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710681166.8A Pending CN109650355A (en) | 2017-10-11 | 2017-10-11 | A kind of method of low temperature preparation hexagonal boron nitride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109650355A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919431A (en) * | 2021-02-07 | 2021-06-08 | 辽东学院 | High-yield and high-crystallinity hexagonal boron nitride nanosheet and preparation method thereof |
| CN113337910A (en) * | 2021-06-25 | 2021-09-03 | 南通强生石墨烯科技有限公司 | White graphene moisture-absorbing sweat-releasing cool polyamide staple fiber and preparation method thereof |
| CN113851255A (en) * | 2021-09-08 | 2021-12-28 | 常州精瓷仪器科技有限公司 | High-insulation easy-rheological thermocouple boron nitride-based filling material and filling method |
| CN115259111A (en) * | 2022-05-09 | 2022-11-01 | 上海交通大学 | Preparation method of boron nitride nanotube |
| CN115520841A (en) * | 2022-08-30 | 2022-12-27 | 山东工业陶瓷研究设计院有限公司 | Spherical boron nitride powder and in-situ synthesis preparation method thereof |
-
2017
- 2017-10-11 CN CN201710681166.8A patent/CN109650355A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919431A (en) * | 2021-02-07 | 2021-06-08 | 辽东学院 | High-yield and high-crystallinity hexagonal boron nitride nanosheet and preparation method thereof |
| CN113337910A (en) * | 2021-06-25 | 2021-09-03 | 南通强生石墨烯科技有限公司 | White graphene moisture-absorbing sweat-releasing cool polyamide staple fiber and preparation method thereof |
| CN113851255A (en) * | 2021-09-08 | 2021-12-28 | 常州精瓷仪器科技有限公司 | High-insulation easy-rheological thermocouple boron nitride-based filling material and filling method |
| CN115259111A (en) * | 2022-05-09 | 2022-11-01 | 上海交通大学 | Preparation method of boron nitride nanotube |
| CN115520841A (en) * | 2022-08-30 | 2022-12-27 | 山东工业陶瓷研究设计院有限公司 | Spherical boron nitride powder and in-situ synthesis preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109650355A (en) | A kind of method of low temperature preparation hexagonal boron nitride | |
| CN102173396B (en) | Production method of high-content alpha-crystal form silicon nitride powders | |
| CN102173397B (en) | Production method of high-content silicon nitride (Si3N4) powder | |
| CN101891165A (en) | Production method of macrocrystalline hexagonal boron nitride | |
| CN101372325A (en) | Carbon nitride polyporous material and use thereof for hydrogen storage | |
| JP2010042963A (en) | Manufacture method of hexagonal boron nitride | |
| CN106006584A (en) | Preparation method of hexagonal boron nitride powder | |
| CN107673766A (en) | A kind of structural ceramics high purity silicon nitride raw powder's production technology | |
| CN103318855A (en) | Preparation method of chromium nitride | |
| CN102400067A (en) | Method for reinforcing spinel whisker-enhanced aluminum-based composite material compactly | |
| CN105541339B (en) | A kind of preparation method of no bonding agent glomerocryst boron nitride complex | |
| CN103272527A (en) | High temperature and high pressure direct synthesis method of cubic boron nitride in titanium nitride plated coating | |
| CN104499053A (en) | Method for preparing silicon nitride crystal whisker | |
| CN107954723B (en) | Preparation method of alpha-phase silicon nitride powder | |
| CN109663543A (en) | A kind of direct Synthesis boron skin nitrogen core polycrystalline diamond preparation method | |
| US20120063983A1 (en) | Method for Synthesis of Boron Nitride Nanopowder | |
| Efremov et al. | The analysis of thermal stability of detonation nanodiamond | |
| CN104528672A (en) | Preparation method of alpha-silicon nitride | |
| Lee et al. | Hexagonal plate‐like ternary carbide particulates synthesized by a carbothermal reduction process: processing parameters and synthesis mechanism | |
| CN105253864B (en) | A kind of preparation method of beta-silicon nitride powder | |
| CN105712305A (en) | New silicon nitride powder synthesis method | |
| Zhao et al. | Preparation and characterisation of boron nitride whiskers | |
| CN110255512A (en) | A kind of preparation method of cubic boron nitride | |
| CN107522178A (en) | A kind of method for preparing boron nitride nano-tube | |
| JPS62100404A (en) | Production of pulverous hexagonal boron nitride having high purity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190419 |