CN110386593A - The method that the induction of amorphous precursor body synthesizes spherical boron nitride (BN) nano-powder - Google Patents
The method that the induction of amorphous precursor body synthesizes spherical boron nitride (BN) nano-powder Download PDFInfo
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- CN110386593A CN110386593A CN201910597510.4A CN201910597510A CN110386593A CN 110386593 A CN110386593 A CN 110386593A CN 201910597510 A CN201910597510 A CN 201910597510A CN 110386593 A CN110386593 A CN 110386593A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
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- 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
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
A kind of method that the induction of amorphous precursor body synthesizes spherical boron nitride (BN) nano-powder, belongs to field of inorganic nonmetallic material.Preparation method includes four raw material mixing, precursor preparation, high temperature pyrolysis, impurity treatment steps.Raw material containing B and the raw material containing N are mixed, heating stirring is added in ethanol solution to moisture evaporating completely；Again by mixed raw material through heat preservation 120-360 minutes of 200~550 DEG C of Muffle furnace, grinding obtains precursor last high temperature pyrolysis of the granularity less than 200 mesh；In a nitrogen atmosphere, precursor powder is warming up to 800~1450 DEG C, and keeps the temperature 120~360 minutes, furnace cooling is washed in ethanol solution after obtaining white powder, and centrifugal treating removes impurity, and drying obtains spherical BN nano-powder.The spherical BN nano raw material that the present invention prepares has the structural advantages such as pattern is uniform, with high purity, size is controllable；With performance advantages such as wear-resisting, corrosion-resistant, high temperature resistant, outstanding heating conduction, insulation performances；And preparation process is simple, at low cost, high yield rate, can be used for industrialized production.
Description
Technical field
The invention belongs to inorganic non-metallic materials science, nano structural material field, the spherical BN for being related to a kind of high yield is received
Rice raw powder's production technology.
Technical background
For hexagonal boron nitride (h-BN) due to its excellent physical and chemical properties, including low-density, low-friction coefficient is excellent
Corrosion resistance, high-termal conductivity, chemical durability and inoxidizability etc. cause the extensive concern of people.Therefore, it is in smelting
Gold, environment, aerospace, the fields such as health care have important application.However, sintering character difference significantly limits h-BN's
Using.The microscopic appearance of flat crystal is presented currently, being mostly used in and preparing the powder materials of BN ceramics.Due to laminated structure
Anisotropy make ceramic be also easy to produce hole, it is difficult to it is fine and close, even if in (> 2000 DEG C) of high temperature sintering and pressure auxiliary
Under the conditions of be still difficult to obtain fine and close ceramic.Therefore, it is proposed that preparing spherical BN crystal as BN ceramic powder original
The new approaches of material, spherical BN powder can increase the bulk density of ceramic body, improve the densified sintering product of BN ceramics；Simultaneously will
Diameter of particle is limited in nanoscale, increases the activity of raw material, alleviates BN ceramic and is difficult to the problem of being sintered.
Currently, the method for industrially preparing BN mainly has CRN method, borax-urea (ammonium chloride) method, chemistry
Vapour deposition process (CVD) etc., and sheet-like morphology is presented in the BN crystal of these methods preparation, mainly since BN crystal has easily
In the characteristic along (00l) crystal face preferred growth.Therefore, spherical BN crystal most where the shoe pinches are prepared to be to inhibit the preferred growth of BN
Characteristic, and then control its direction of growth.However, previous preparation thinking does not carry out relevant design, but it is flat in two dimension
The enough growing spaces of BN crystal are left on the direction of face for, so that BN crystal is easier to grow into laminated structure.Theoretically, if energy
Control the location of growing point BN, so that it may further control its direction of growth.Therefore, it is proposed that Research Thinking are as follows: pass through
Inhibit B, N atomic bonding on an atomic scale, inhibits BN in the preferred growth of (00l) crystal face, to control it to lamellar growth
Trend, and then induce BN to spherical morphology develop.
Summary of the invention
In view of boron oxide shows the sticking molten state of tool under lower temperature (≤1200 DEG C).The present invention proposes one
That is, at a lower temperature N atom is introduced into B-O structure by the novel amorphous precursor body revulsion of kind, utilize sticky amorphous liquid phase
Coating function limit the preferential growth of BN, induction BN crystal develops to spherical-like morphology.
Following target may be implemented through the invention: (1) realizing the mass production of High Purity Spherical BN nano-powder；(2)
Realize that the controllable metaplasia of BN nano-powder appearance and size produces；(3) whole preparation process method is simple, low in cost, is suitable for work
Industry metaplasia produces.
The technical scheme is that being obtained by adjusting the parameters such as material rate and reaction temperature, time with amorphous
The presoma of structure.And spherical BN nano-powder is prepared using the amorphous precursor body high temperature pyrolysis.It mainly include raw material mixing, preceding
Drive body preparation, high temperature pyrolysis and impurity treatment, the specific steps are as follows:
(1) raw material mixes: B and N molar ratio mixes each raw material from 1:2 to 1:20 in molar ratio, and the aqueous solution of ethyl alcohol is added
In, it is stirred evenly in 80~120 DEG C, and stir always to moisture evaporating completely.
(2) precursor preparation: mixed raw material is put into Muffle furnace and is heated to 200~550 DEG C of heat preservation 120-360 points
Room temperature is naturally cooled to after clock, products therefrom is ground with mortar, obtains BxCyNzOkHlPrecursor powder.
(3) high temperature pyrolysis: moving to alumina crucible for obtained precursor powder, be then placed in vertical tubular furnace, leads to
Enter nitrogen, stove is then warming up to 800~1450 DEG C and keeps the temperature 120~360 minutes, reaction product is naturally cooled to furnace later
Room temperature.
(4) impurity treatment: reaction product is impregnated in ethanol solution after taking out, and is centrifuged 3~5 times to remove remnants
Reactant.
The amorphous precursor body revulsion that the present invention uses is a kind of easy to operate, low in cost, environmentally protective, and is easy to criticize
Measure the preparation method of production.On the basis of the theory, we pass through control raw material and ratio, reaction time, reaction temperature etc.
Technological parameter controls BxCyNzOkHlThe Nomenclature Composition and Structure of Complexes of presoma further controls reaction temperature when presoma pyrolysis, anti-
Between seasonable, the technological parameters such as reaction atmosphere, so that it may realize the control to product purity, pattern, size etc., realize spherical nitridation
The industrialized production of boron nano-powder.
The beneficial effects of the present invention are: (1) can on the basis of guaranteeing BN purity, by controlling multiple affecting parameters,
The controllable spherical BN nano-powder of appearance and size (diameter is 10~200nm, with a thickness of 20~50nm) is prepared, thus realization pair
The regulation of the performances such as material luminescence generated by light, thermally conductive, ceramic consistency；(2) low raw-material cost of the invention used, preparation
Method is simple, equipment requirement is low, yield is big, is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is preparation method process flow chart of the invention；
Fig. 2 is the XRD diagram of presoma and BN product that the embodiment of the present invention is prepared；
Fig. 3 is the SEM figure of the spherical BN nano material of the different-shape being prepared of the embodiment of the present invention and size, respectively
Flat plate-like BN, cellular BN for ellipsoid BN, 50-200nm of spherical BN, 50nm of spherical BN, 20nm of partial size 10nm receive
Rice material.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Embodiment 1
Using boric acid and urea mol ratio 1:1 as raw material, 90 DEG C of stirrings are complete to moisture in the aqueous solution (30vol%) of ethyl alcohol
Pervaporation.The mixed raw material is kept the temperature 240 minutes through 200 DEG C of Muffle furnace in air atmosphere and obtains the B of amorphousxCyNzOkHlBefore
Body is driven, presoma is ground to less than 200 mesh, is warming up to 1100 DEG C of heat preservation sintering in 240 minutes synthesis BN materials in a nitrogen atmosphere
Material.Its pattern is that evenly dispersed nanometer is spherical, and average grain diameter is about 20nm.
Embodiment 2
Using boron oxide and urea mol ratio 1:2 as raw material, stirred to moisture for 90 DEG C in the aqueous solution (30vol%) of ethyl alcohol
Evaporating completely.The mixed raw material is obtained into B after 200 DEG C of Muffle furnace keep the temperature 240 minutes in air atmospherexCyNzOkHlForerunner
Presoma is ground to less than 200 mesh by body, is warming up to 1100 DEG C of heat preservation sintering in 240 minutes synthesis BN materials in a nitrogen atmosphere.
Its pattern is that evenly dispersed nanometer is spherical, and average grain diameter is about 20nm.
Embodiment 3
Using boric acid and biuret molar ratio 1:5 as raw material, stirred to moisture for 90 DEG C in the aqueous solution (30vol%) of ethyl alcohol
Evaporating completely.The mixed raw material is obtained into B after 200 DEG C of Muffle furnace keep the temperature 240 minutes in air atmospherexCyNzOkHlForerunner
Presoma is ground to less than 200 mesh by body, is warming up to 1100 DEG C of heat preservation sintering in 240 minutes synthesis BN materials in a nitrogen atmosphere.
Its pattern is the BN nano material of porous flake.
Embodiment 4
Using boron oxide and melamine molar ratio 1:1 as raw material, stirred extremely for 90 DEG C in the aqueous solution (30vol%) of ethyl alcohol
Moisture evaporating completely.The mixed raw material is obtained into B after 400 DEG C of heat preservation 4h of Muffle furnace in air atmospherexCyNzOkHlForerunner
Presoma is ground to less than 200 mesh by body, is warming up to 1000 DEG C of heat preservation sintering in 120 minutes synthesis BN materials in a nitrogen atmosphere.
Its pattern is that uniform nanometer is spherical, and average grain diameter is about 20nm.
Embodiment 5
Using boric acid and urea mol ratio 2:3 as raw material, 90 DEG C of stirrings are complete to moisture in the aqueous solution (30vol%) of ethyl alcohol
Pervaporation.The mixed raw material is obtained into the B of amorphous after 200 DEG C of Muffle furnace heat preservation 2h in air atmospherexCyNzOkHlForerunner
Presoma is ground to less than 200 mesh by body, is warming up to 1000 DEG C of heat preservation sintering in 240 minutes synthesis BN materials in a nitrogen atmosphere.
Its pattern is that nanometer is spherical, and average grain diameter is about 10nm.
Embodiment 6
Using boric acid and urea mol ratio 1:2 as raw material, 90 DEG C of stirrings are complete to moisture in the aqueous solution (30vol%) of ethyl alcohol
Pervaporation.The mixed raw material is obtained into B after 200 DEG C of heat preservation 4h of Muffle furnace in air atmospherexCyNzOkHlPresoma, will before
It drives body to be ground to less than 200 mesh, is warming up to 1250 DEG C of heat preservation sintering in 240 minutes synthesis BN nano materials in a nitrogen atmosphere.Its
Pattern is equally distributed ellipsoid, and average grain diameter is about 50nm.
Embodiment 7
Using boric acid and cyanuric acid molar ratio 2:1 as raw material, stirred to water for 90 DEG C in the aqueous solution (30vol%) of ethyl alcohol
Divide evaporating completely.The mixed raw material is obtained into B after 400 DEG C of heat preservation 4h of Muffle furnace in air atmospherexCyNzOkHlPresoma,
Presoma is ground to less than 200 mesh, 1450 DEG C of heat preservation sintering in 240 minutes is warming up in a nitrogen atmosphere and synthesizes BN nanometers of materials
Material.Its pattern is the oblate spheroid shape of similar plate-like, and average grain diameter is 50~200nm, 30~60nm of thickness.
Claims (6)
1. a kind of method that the induction of amorphous precursor body synthesizes spherical boron nitride (BN) nano-powder, it is characterised in that specific synthesis step
It is rapid as follows:
(1) raw material mix: by B and N raw material be added ethyl alcohol aqueous solution in, stirred evenly in 80~120 DEG C, and stir always to
Moisture evaporating completely；
(2) precursor preparation: mixed raw material is put into Muffle furnace heat, keep the temperature, after naturally cool to room temperature, gained produces
Object is ground with mortar, obtains BxCyNzOkHlPrecursor powder；
(3) high temperature pyrolysis: obtained precursor powder is moved into alumina crucible, is then placed in vertical tubular furnace, is passed through nitrogen
Gas, then by reaction product after stove heating, heat preservation with furnace cooled to room temperature；
(4) impurity treatment: reaction product is impregnated in ethanol solution after taking out, and is centrifuged 3~5 times to remove the anti-of remnants
Answer object.
2. the method that amorphous precursor body induction according to claim 1 synthesizes spherical boron nitride (BN) nano-powder, special
Sign is mixing method described in step (1) for material by wet type mixing, and the molar ratio of B raw material and N raw material is 1:2~1:20.
3. the method that amorphous precursor body induction according to claim 1 synthesizes spherical boron nitride (BN) nano-powder, special
Sign is in Muffle furnace that heating temperature is 200~550 DEG C, soaking time 120-360 minutes；The presoma is amorphous knot
Structure, granularity is less than 200 mesh after grinding.
4. the method that amorphous precursor body induction according to claim 1 synthesizes spherical boron nitride (BN) nano-powder, special
Sign is that step (3) pyrolysis temperature is 800~1450 DEG C, and soaking time 120~360 minutes, reaction product was after pyrolysis
Powder, based on spherical nanometer BN, diameter is 3nm~200nm.
5. the preparation method of spherical BN nano-powder according to right 1-4, it is characterised in that the raw material containing B is boron
One or more of acid, boron oxide.
6. the preparation method of spherical BN nano-powder according to right 1-4, it is characterised in that the raw material containing N is urine
One or more of element, biuret, cyanuric acid or melamine.
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Cited By (3)
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| CN111377418A (en) * | 2020-03-23 | 2020-07-07 | 河北工业大学 | Synthesis method of porous hexagonal boron nitride |
| CN111777047A (en) * | 2020-07-13 | 2020-10-16 | 丹东市化工研究所有限责任公司 | Preparation method of nano-submicron sphere-like boron nitride |
| CN113753866A (en) * | 2021-08-03 | 2021-12-07 | 湖南大学 | Hexagonal boron nitride nanocrystal and solid phase preparation method thereof |
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|---|---|---|---|---|
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| CN111777047A (en) * | 2020-07-13 | 2020-10-16 | 丹东市化工研究所有限责任公司 | Preparation method of nano-submicron sphere-like boron nitride |
| CN113753866A (en) * | 2021-08-03 | 2021-12-07 | 湖南大学 | Hexagonal boron nitride nanocrystal and solid phase preparation method thereof |
| CN113753866B (en) * | 2021-08-03 | 2023-02-07 | 湖南大学 | Hexagonal boron nitride nanocrystal and solid phase preparation method thereof |
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