CN108483414A - One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof - Google Patents
One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof Download PDFInfo
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- 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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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The present invention relates to one kind synthesizing rhombohedral boron nitride powder and preparation method thereof based on molten-salt growth method low temperature.Its technical solution is：The potassium chloride of the boron source of 15~20wt%, the ammonium chloride of 35~40wt%, the sodium chloride of 18~21wt% and 22~27wt% are mixed, mixture is obtained.Under the conditions of nitrogen atmosphere, the mixture is first warming up to 280~300 DEG C with the rate of 1.5~2 DEG C/min, then 700~900 DEG C are warming up to the rate of 3~5 DEG C/min, keeps the temperature 3~4h, natural cooling obtains reaction product.The reaction product is impregnated into 1~2h in distilled water, then is washed with distilled water 2~3 times, is then dried under the conditions of 100~110 DEG C and synthesizes rhombohedral boron nitride powder to get based on molten-salt growth method low temperature.The present invention has the characteristics that at low cost, synthesis temperature is low, simple production process and period are short；It is good based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder purity height and crystal development to be prepared with this method.
Description
Technical field
The invention belongs to boron nitride powder technical fields.Rhombohedral boron nitride is synthesized based on molten-salt growth method low temperature more particularly to one kind
Powder and preparation method thereof.
Background technology
Boron nitride (BN) be it is a kind of have excellent performance and the new ceramic material for the potentiality that grow a lot, since it has low Jie
Electric constant, can microwave penetration, good electrical insulating property, low thermal expansion, broad-band gap, high temperature lubricating and high-temperature stability etc., quilt
It is widely used in the fields such as metallurgy, machinery, electronics, nuclear energy, aerospace.It common are six side's nitrogen of similar graphite laminate structure
Change boron (h-BN), the cubic boron nitride (c-BN) of similar diamond zincblende lattce structure, similar to lonsdaleite wurtzite structure
The rhombohedral boron nitride (r-BN) of close heap hexagonal boron nitride (w-BN) and tripartite's phase graphite-structure, the rapid layer boron nitride of layer structure
(t-BN) and unsetting boron nitride.
The method for preparing boron nitride reported at present relates generally to the preparation of h-BN and c-BN.J.Q.Hu et al.
(J.Q.Hu, Q.Y.Lu, K.B.Tang, et al.Synthesis and Characterization of
Nanocrystalline Boron Nitride [J] .Journal of Solid State Chemistry, 1999,148:
It 325-328.) uses autoclave and in nitrogen atmosphere, is kept the temperature at 650 DEG C under the pressure of 2h and 22MPa by KBH4-NH4Cl is anti-
It answers, synthesizes h-BN and c-BN mixing nano boron nitride powders, but the yield of BN is not high, only 70%, and need in condition of high voltage
Lower reaction.L.X.Lin et al. (L.X.Lin, Y.Zheng, Y.Zheng, et al.Facile synthesis of
Hexagonal boron nitride fibers and flowers [J] .Materials Letters, 2007,61:1735-
1737.) by KBH4And NH4Cl raw materials reaction 48h in the aqueous systems that temperature is 120 DEG C synthesizes presoma and the centre of boron nitride
Then presoma and intermediate are heated to 1250 DEG C and keep the temperature 10h by body in a nitrogen atmosphere, prepare a diameter of 1~2 μm
H-BN fibers, this method flow is more complex, and synthesis temperature is high and soaking time is long.M.T.Zheng et al. (M.T.Zheng,
Y.L.Gu, Z.L.Xu, et al.Synthesis and characterization of boron nitride nanoropes
[J] .Materials Letters, 2007,61:1943-1945.) with KBH4And NH4Cl is as primary raw material, CoCl2·6H2O
For catalyst.By CoCl2·6H2O heats 4h at 500 DEG C, then with KBH4And NH4Cl is mixed.It is about in pressure by mixture
It is heated to 600 DEG C of heat preservation 12h in 30MPa autoclaves, is successfully prepared a diameter of 60~150nm, length up to several microns
H-BN nanometer rods, but this method needs react under hyperbaric environment, and soaking time is long.
To preparing the synthesis of the r-BN in boron nitride frequently with chemical vapour deposition technique (CVD), for example, M.Chubarov etc.
People using boron triethyl and ammonia as presoma and using chemical vapor deposition method, under 1500 DEG C and 70mba of pressure,
R-BN (M.Chubarov, H.Pedersen, H. are generated in Sapphire Substrateet al.On the effect of
silicon in CVD of sp2Hybridized boron nitride thin films [J] .Crystengcomm,
2013,15:455-458.).AlN buffer layers are then formed by nitridation in situ using before BN growths, 1200~1500
DEG C with H2R-BN (M.Chubarov, H.Pedersen, H. are generated under low pressure (usual 100mbar or lower) as carrier gaset al.Boron nitride:A new photonic material[J].Physica B Condensed
Matter, 2014,439:29-34.).But chemical vapour deposition technique is used, needs higher reaction temperature, certain pressure mostly
By force or in specific explosive atmosphere, and the r-BN purity synthesized is not high.
K.Bao et al. (K.Bao, F.Y.Yu, L.Shi, et al.Synthesis of highly crystalline
rhombohedral BN triangular nanoplates via a convenient solid state reaction
[J] .Journal of Solid State Chemistry, 2009,182:925-931.) by solid phase reaction and in autoclave
In, by NaNH2And B2O36h is kept the temperature under the conditions of 600 DEG C, prepares highly crystalline r-BN triangles nanometer sheet, but this method needs
The long period is reacted under high pressure.L.F.Ye et al. (L.F.Ye, F.Liang, L.Zhao, et al.Catalyzed
synthesis of rhombohedral boron nitride in sodium chloride molten salt[J]
.Ceramics International, 2016,42:11626-11633.) use Na2B4O7With Mg as primary raw material, NaCl
As fused salt, is kept the temperature at 1000 DEG C and prepare r-BN powder under 3h and nitrogen atmosphere.But contain h-BN in the r-BN of synthesis, r-BN is pure
Degree is not high.
Invention content
The present invention is directed to overcome prior art defect, it is therefore an objective to which offer one kind is at low cost, synthesis temperature is low, production technology is simple
The single and period is short based on molten-salt growth method low temperature synthesis rhombohedral boron nitride raw powder's production technology, with this method preparation based on fused salt
Method low temperature synthesizes rhombohedral boron nitride powder purity height and crystal development is good.
To achieve the above object, the technical solution adopted in the present invention is：
Step 1: by the boron source of 15~20wt%, the ammonium chloride of 35~40wt%, the sodium chloride of 18~21wt% and 22~
The potassium chloride of 27wt% mixes, and obtains mixture.
Step 2: under the conditions of nitrogen atmosphere, the mixture is first warming up to 280 with the rate of 1.5~2 DEG C/min~
300 DEG C, then 700~900 DEG C are warming up to the rate of 3~5 DEG C/min, 3~4h is kept the temperature, natural cooling obtains reaction product.
Step 3: the reaction product is impregnated 1~2h in distilled water, then be washed with distilled water 2~3 times, then in
It is dried under the conditions of 100~110 DEG C and synthesizes rhombohedral boron nitride powder to get based on molten-salt growth method low temperature.
The boron source is potassium borohydride or is sodium borohydride, purity >=97.0wt%；Granularity≤0.1mm of the boron source.
Purity >=99.5wt% of the ammonium chloride；Granularity≤0.1mm of the ammonium chloride.
Purity >=99.5wt% of the sodium chloride；Granularity≤0.1mm of sodium chloride.
Purity >=99.5wt% of the potassium chloride；Granularity≤0.1mm of potassium chloride.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art：
The present invention is using potassium borohydride or sodium borohydride as boron source, using ammonium chloride as nitrogen source, with sodium chloride and potassium chloride
As fused salt, 3~4h is kept the temperature under nitrogen atmosphere and 700~900 DEG C of cryogenic conditions, obtains reaction product, then with distillation
Water washing, drying synthesizes rhombohedral boron nitride powder to get based on molten-salt growth method low temperature, therefore synthesis temperature is low, the period is short, technique is simple
It is single.Potassium borohydride or sodium borohydride, ammonium chloride, sodium chloride and potassium chloride raw material used in the present invention are commercially available, cheap, raw
It produces at low cost.
The raw materials used in the present invention is soluble easily in water, can wash by water reaction product, and acquisition is synthesized based on molten-salt growth method low temperature
Rhombohedral boron nitride powder purity is high；The present invention is synthesized using molten-salt growth method and synthesizes rhombohedral boron nitride based on molten-salt growth method low temperature at low temperature
Powder can generate liquid phase environment because the eutectic point of sodium chloride and potassium chloride fused salt is 657 DEG C under the conditions of 657 DEG C, improve reaction
Rate and reduction reaction condition, and it is uniform using the powder structure that molten-salt growth method obtains, and product pattern is uniform, and crystal development is good,
Length is about 200~300nm, and thickness is about 40~70nm.
The mixture is warming up to 280~300 DEG C by the present invention with the rate of 1.5~2 DEG C/min, makes ammonium chloride and boron hydrogen
Relatively stable substance can be generated by changing potassium (or sodium borohydride), can substantially reduce volatilization of the ammonium chloride in subsequent temperature-rise period
Loss.
Therefore, the present invention has the characteristics that at low cost, synthesis temperature is low, simple production process and period are short；Use this method
What is prepared is good based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder purity height and crystal development.
Description of the drawings
Fig. 1 is a kind of XRD diagram synthesizing rhombohedral boron nitride powder based on molten-salt growth method low temperature prepared by the present invention；
Fig. 2 is the SEM figures shown in FIG. 1 that rhombohedral boron nitride powder is synthesized based on molten-salt growth method low temperature.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection domain
System.
In present embodiment：
Purity >=97.0wt% of the boron source；Granularity≤0.1mm of the boron source.
Purity >=99.5wt% of the ammonium chloride；Granularity≤0.1mm of the ammonium chloride.
Purity >=99.5wt% of the sodium chloride；Granularity≤0.1mm of sodium chloride.
Purity >=99.5wt% of the potassium chloride；Granularity≤0.1mm of potassium chloride.
It is repeated no more in embodiment.
Embodiment 1
One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof.Preparation method described in the present embodiment
It is：
Step 1: by the boron source of 17~20wt%, the ammonium chloride of 35~38wt%, the sodium chloride of 19~20wt% and 23~
The potassium chloride of 26wt% mixes, and obtains mixture.
Step 2: under the conditions of nitrogen atmosphere, the mixture is first warming up to 280 with the rate of 1.5~2 DEG C/min~
300 DEG C, then 700~800 DEG C are warming up to the rate of 3~4 DEG C/min, 3~4h is kept the temperature, natural cooling obtains reaction product.
Step 3: the reaction product is impregnated 1~2h in distilled water, then be washed with distilled water 2~3 times, then in
It is dried under the conditions of 100~110 DEG C and synthesizes rhombohedral boron nitride powder to get based on molten-salt growth method low temperature.
Boron source described in the present embodiment is potassium borohydride.
Embodiment 2
One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof.The present embodiment is boron hydrogen except boron source
Change outside sodium, remaining is the same as embodiment 1.
Embodiment 3
One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof.Preparation method described in the present embodiment
It is：
Step 1: by the boron source of 16~19wt%, the ammonium chloride of 36~39wt%, the sodium chloride of 20~21wt% and 22~
The potassium chloride of 25wt% mixes, and obtains mixture.
Step 2: under the conditions of nitrogen atmosphere, the mixture is first warming up to 280 with the rate of 1.5~2 DEG C/min~
300 DEG C, then 800~900 DEG C are warming up to the rate of 3.5~4.5 DEG C/min, 3~4h is kept the temperature, natural cooling obtains reaction production
Object.
Step 3: the reaction product is impregnated 1~2h in distilled water, then be washed with distilled water 2~3 times, then in
It is dried under the conditions of 100~110 DEG C and synthesizes rhombohedral boron nitride powder to get based on molten-salt growth method low temperature.
Boron source described in the present embodiment is sodium borohydride.
Embodiment 4
One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof.The present embodiment is boron hydrogen except boron source
Change outside potassium, remaining is the same as embodiment 3.
Embodiment 5
One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof.Preparation method described in the present embodiment
It is：
Step 1: by the boron source of 15~18wt%, the ammonium chloride of 37~40wt%, the sodium chloride of 18~19wt% and 24~
The potassium chloride of 27wt% mixes, and obtains mixture.
Step 2: under the conditions of nitrogen atmosphere, the mixture is first warming up to 280 with the rate of 1.5~2 DEG C/min~
300 DEG C, then 750~850 DEG C are warming up to the rate of 4~5 DEG C/min, 3~4h is kept the temperature, natural cooling obtains reaction product.
Step 3: the reaction product is impregnated 1~2h in distilled water, then be washed with distilled water 2~3 times, then in
It is dried under the conditions of 100~110 DEG C and synthesizes rhombohedral boron nitride powder to get based on molten-salt growth method low temperature.
Boron source described in the present embodiment is potassium borohydride.
Embodiment 6
One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof.The present embodiment is boron hydrogen except boron source
Change outside sodium, remaining is the same as embodiment 5.
Present embodiment has following good effect compared with prior art：
Present embodiment is using potassium borohydride or sodium borohydride as boron source, using ammonium chloride as nitrogen source, with sodium chloride
With potassium chloride as fused salt, 3~4h is kept the temperature under nitrogen atmosphere and 700~900 DEG C of cryogenic conditions, obtains reaction product, with
After be washed with distilled water, drying to get based on molten-salt growth method low temperature synthesize rhombohedral boron nitride powder, therefore synthesis temperature is low, the period is short,
It is simple for process.Potassium borohydride or sodium borohydride, ammonium chloride, sodium chloride and the cities potassium chloride raw material Jun Ke used in present embodiment
Purchase, it is cheap, production cost is low.
Present embodiment is prepared as shown in the picture based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder, and Fig. 1 is
A kind of XRD diagram synthesizing rhombohedral boron nitride powder based on molten-salt growth method low temperature prepared by embodiment 1；Fig. 2 is shown in FIG. 1 based on molten
Salt method low temperature synthesizes the SEM figures of rhombohedral boron nitride powder.It will be seen from figure 1 that made product purity is high；As can be seen from Figure 2
Product pattern is uniform, and crystal development is good, and length is about 200~300nm, and thickness is about 40~70nm.
Present embodiment is raw materials used soluble easily in water, can wash by water reaction product, is conducive to obtain high-purity
Based on molten-salt growth method low temperature synthesize rhombohedral boron nitride powder；Present embodiment is synthesized at low temperature using molten-salt growth method based on molten
Salt method low temperature synthesizes rhombohedral boron nitride powder, can be in 657 DEG C of conditions because the eutectic point of sodium chloride and potassium chloride fused salt is 657 DEG C
Lower generation liquid phase environment improves reaction rate and reduces reaction condition, and uniform using the powder structure that molten-salt growth method obtains.
The mixture is warming up to 280~300 DEG C by present embodiment with the rate of 1.5~2 DEG C/min, makes chlorination
Ammonium and potassium borohydride (or sodium borohydride) can generate relatively stable substance, can substantially reduce ammonium chloride in subsequent temperature-rise period
In volatilization loss.
Therefore, present embodiment has the characteristics that at low cost, synthesis temperature is low, simple production process and period are short；
It is good based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder purity height and crystal development to be prepared with this method.
Claims (6)
1. one kind synthesizing rhombohedral boron nitride raw powder's production technology based on molten-salt growth method low temperature, it is characterised in that the preparation method
It is：
Step 1: by the boron source of 15~20wt%, the ammonium chloride of 35~40wt%, the sodium chloride of 18~21wt% and 22~
The potassium chloride of 27wt% mixes, and obtains mixture；
Step 2: under the conditions of nitrogen atmosphere, the mixture is first warming up to 280~300 with the rate of 1.5~2 DEG C/min
DEG C, then 700~900 DEG C are warming up to the rate of 3~5 DEG C/min, 3~4h is kept the temperature, natural cooling obtains reaction product；
Step 3: the reaction product is impregnated 1~2h in distilled water, then be washed with distilled water 2~3 times, then in 100~
It is dried under the conditions of 110 DEG C and synthesizes rhombohedral boron nitride powder to get based on molten-salt growth method low temperature.
2. being based on molten-salt growth method low temperature according to claim 1 synthesizes rhombohedral boron nitride raw powder's production technology, it is characterised in that
The boron source is potassium borohydride or is sodium borohydride, purity >=97.0wt%；Granularity≤0.1mm of the boron source.
3. being based on molten-salt growth method low temperature according to claim 1 synthesizes rhombohedral boron nitride raw powder's production technology, it is characterised in that
Purity >=99.5wt% of the ammonium chloride；Granularity≤0.1mm of the ammonium chloride.
4. being based on molten-salt growth method low temperature according to claim 1 synthesizes rhombohedral boron nitride raw powder's production technology, it is characterised in that
Purity >=99.5wt% of the sodium chloride；Granularity≤0.1mm of sodium chloride.
5. being based on molten-salt growth method low temperature according to claim 1 synthesizes rhombohedral boron nitride raw powder's production technology, it is characterised in that
Purity >=99.5wt% of the potassium chloride；Granularity≤0.1mm of potassium chloride.
6. one kind synthesizing rhombohedral boron nitride powder based on molten-salt growth method low temperature, it is characterised in that described to synthesize water chestnut based on molten-salt growth method low temperature
Shape boron nitride powder is according to the system for synthesizing rhombohedral boron nitride powder described in any one of right 1~5 based on molten-salt growth method low temperature
Rhombohedral boron nitride powder is synthesized based on molten-salt growth method low temperature prepared by Preparation Method.
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| CN109503174A (en) * | 2018-11-29 | 2019-03-22 | 盐城师范学院 | A kind of preparation method of ultra-thin cubic boron nitride film |
| CN114132904A (en) * | 2021-12-06 | 2022-03-04 | 湖南大学 | High oil absorption whitening hexagonal boron nitride porous microspheres for cosmetics |
| CN114836205A (en) * | 2022-03-18 | 2022-08-02 | 武汉科技大学 | Rare earth doped boron nitride nano powder and preparation method thereof |
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