CN108483414B - Low-temperature synthesis diamond boron nitride powder based on molten salt growth method and preparation method thereof - Google Patents
Low-temperature synthesis diamond boron nitride powder based on molten salt growth method 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
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Abstract
The invention relates to a low-temperature synthesized diamond boron nitride powder based on a molten salt growth method and a preparation method thereof. The technical scheme is as follows: mixing 15-20 wt% of boron source, 35-40 wt% of ammonium chloride, 18-21 wt% of sodium chloride and 22-27 wt% of potassium chloride to obtain a mixture. Under the condition of nitrogen atmosphere, firstly heating the mixture to 280-300 ℃ at the speed of 1.5-2 ℃/min, then heating to 700-900 ℃ at the speed of 3-5 ℃/min, preserving heat for 3-4 h, and naturally cooling to obtain a reaction product. And soaking the reaction product in distilled water for 1-2 h, washing with distilled water for 2-3 times, and drying at 100-110 ℃ to obtain the rhombus boron nitride powder synthesized at low temperature based on a molten salt method. The invention has the characteristics of low cost, low synthesis temperature, simple production process and short period; the rhombus boron nitride powder prepared by the method based on the molten salt growth method and synthesized at low temperature has high purity and good crystal growth.
Description
Technical Field
The invention belongs to the technical field of boron nitride powder. In particular to diamond-shaped boron nitride powder synthesized at low temperature based on a molten salt growth method and a preparation method thereof.
Background
Boron Nitride (BN) is a novel ceramic material with excellent properties and great development potential, and is widely used in the fields of metallurgy, machinery, electronics, nuclear energy, aerospace and the like due to its low dielectric constant, microwave penetration, good electrical insulation, low thermal expansion, wide band gap, high temperature lubricity, high temperature stability and the like. Hexagonal boron nitride (h-BN) similar to a graphite laminated structure, cubic boron nitride (c-BN) similar to a diamond sphalerite structure, close-packed hexagonal boron nitride (w-BN) similar to a hexagonal diamond wurtzite structure and rhombohedral boron nitride (r-BN) similar to a three-phase graphite structure, turbostratic boron nitride (t-BN) of a laminated structure and amorphous boron nitride are common.
the methods for preparing boron nitride that have been reported so far mainly relate to the preparation of h-BN and c-BN. Hu et al (J.Q.Hu, Q.Y.Lu, K.B.Tang, et al. Synthesis and Characterization of Nanocristalline Boron Nitride [ J.Q.Hu]Journal of Solid State Chemistry, 1999, 148:325-The temperature is kept for 2h and 22MPa under the pressure of KBH4-NH4Cl reacts to synthesize h-BN and c-BN mixed nano boron nitride powder, but the yield of BN is not high and is only 70 percent, and the reaction is needed under high pressure. L.X.Lin et al (L.X.Lin, Y.ZHEN, et al.face synthesis of hexagonal boron nitride fibers and flowers [ J.]Materials Letters, 2007, 61:1735-4And NH4The method comprises the steps of reacting Cl raw materials in a water system at 120 ℃ for 48 hours to synthesize a precursor and an intermediate of boron nitride, heating the precursor and the intermediate to 1250 ℃ in a nitrogen atmosphere, and preserving heat for 10 hours to prepare the h-BN fiber with the diameter of 1-2 mu m. M.T.Zheng et al (M.T.Zheng, Y.L.Gu, Z.L.xu, et al.Synthesis and characterization of boron nitride nanoparticles [ J.]Materials Letters, 2007, 61:1943-4And NH4Cl as main raw material, CoCl2·6H2O is a catalyst. Adding CoCl2·6H2Heating O at 500 deg.C for 4h, and reacting with KBH4And NH4And mixing with Cl. The mixture is heated to 600 ℃ in an autoclave with the pressure of about 30MPa and is kept warm for 12 hours, so that the h-BN nano-rod with the diameter of 60-150 nm and the length of several micrometers is successfully prepared, but the method needs to react in a high-pressure environment, and the heat preservation time is too long.
The synthesis of r-BN in the preparation of boron nitride is commonly carried out by Chemical Vapor Deposition (CVD) methods, for example, M.Chubarov et al, with triethylboron and ammonia as precursors and chemical vapor deposition, at 1500 ℃ and 70mba pressure, to produce r-BN (M.Chubarov, H.Pedersen, H) on sapphire substrates.et al.On the effect of silicon in CVD of sp2hybridized boron nitride thin films[J]crystengcomm, 2013, 15: 455-. Then, an AlN buffer layer is formed by in-situ nitridation before BN growth, and the temperature is 1200-1500 ℃ with H2r-BN (M.Chubarov, H.Pedersen, H) is produced as a carrier gas at low pressure (typically 100mbar or less).et al.Boron nitride:A new photonic material[J]Physica B Condensed Matter, 2014, 439: 29-34). However, the chemical vapor deposition method mostly needs higher reaction temperature, certain pressure or in a specific explosive atmosphere, and the purity of the synthesized r-BN is not high.
Bao et al (K.Bao, F.Y.Yu, L.Shi, et al. Synthesis of high purity crystalline rare boron BN ternary crystalline nano-plate a continuous soluble state reaction [ J.Bao]Journal of Solid State Chemistry, 2009, 182: 925-931) by Solid phase reaction and in an autoclave from NaNH2And B2O3The temperature is kept for 6h at 600 ℃ to prepare the high-crystallization r-BN triangular nanosheet, but the method needs to react for a long time under the high-pressure condition. Ye et al (L.F.Ye, F.Liang, L.ZHao, et al, catalysis in synthesis of rhodo-blast nitride in sodium chloride salt [ J.]Na was used in Ceramics International, 2016, 42:11626-2B4O7Mg is used as a main raw material, NaCl is used as molten salt, and r-BN powder is prepared under the conditions of heat preservation for 3 hours at the temperature of 1000 ℃ and nitrogen atmosphere. However, the synthesized r-BN contains h-BN, and the purity of the r-BN is not high.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a method for preparing diamond-shaped boron nitride powder based on a molten salt method and having low cost, low synthesis temperature, simple production process and short period.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
Step one, mixing 15-20 wt% of boron source, 35-40 wt% of ammonium chloride, 18-21 wt% of sodium chloride and 22-27 wt% of potassium chloride to obtain a mixture.
and secondly, under the condition of a nitrogen atmosphere, heating the mixture to 280-300 ℃ at the speed of 1.5-2 ℃/min, heating to 700-900 ℃ at the speed of 3-5 ℃/min, preserving heat for 3-4 h, and naturally cooling to obtain a reaction product.
And step three, soaking the reaction product in distilled water for 1-2 hours, washing with distilled water for 2-3 times, and drying at 100-110 ℃ to obtain the rhombus boron nitride powder synthesized at low temperature based on the molten salt method.
The boron source is potassium borohydride or sodium borohydride, and the purity is more than or equal to 97.0 wt%; the granularity of the boron source is less than or equal to 0.1 mm.
The purity of the ammonium chloride is more than or equal to 99.5 wt%; the granularity of the ammonium chloride is less than or equal to 0.1 mm.
The purity of the sodium chloride is more than or equal to 99.5 wt%; the granularity of the sodium chloride is less than or equal to 0.1 mm.
The purity of the potassium chloride is more than or equal to 99.5 wt%; the granularity of the potassium chloride is less than or equal to 0.1 mm.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
According to the method, potassium borohydride or sodium borohydride is used as a boron source, ammonium chloride is used as a nitrogen source, sodium chloride and potassium chloride are used as molten salts, heat preservation is carried out for 3-4 hours under the conditions of nitrogen atmosphere and low temperature of 700-900 ℃, reaction products are obtained, then distilled water is used for washing, and drying is carried out, so that the rhombus boron nitride powder synthesized at low temperature based on the molten salt method is obtained, and therefore the method is low in synthesis temperature, short in period and simple in process. The potassium borohydride or sodium borohydride, ammonium chloride, sodium chloride and potassium chloride used in the invention can be purchased in the market, and has low price and low production cost.
The raw materials used in the method are all easy to dissolve in water, the reaction product can be cleaned by water, and the obtained diamond boron nitride powder synthesized at low temperature based on a molten salt method has high purity; the method adopts the molten salt method to synthesize the diamond-shaped boron nitride powder based on the molten salt method at low temperature, the eutectic point of the sodium chloride and the potassium chloride molten salt is 657 ℃, a liquid phase environment can be generated at 657 ℃, the reaction rate is improved, the reaction conditions are reduced, the powder obtained by the molten salt method has the advantages of uniform structure, uniform product appearance, good crystal development, the length of about 200-300 nm and the thickness of about 40-70 nm.
According to the invention, the temperature of the mixture is raised to 280-300 ℃ at a speed of 1.5-2 ℃/min, so that ammonium chloride and potassium borohydride (or sodium borohydride) can generate relatively stable substances, and the volatilization loss of ammonium chloride in the subsequent heating process can be remarkably reduced.
Therefore, the invention has the characteristics of low cost, low synthesis temperature, simple production process and short period; the rhombus boron nitride powder prepared by the method based on the molten salt growth method and synthesized at low temperature has high purity and good crystal growth.
Drawings
FIG. 1 is an XRD (X-ray diffraction) diagram of diamond-shaped boron nitride powder prepared by the invention and synthesized at low temperature based on a molten salt method;
FIG. 2 is an SEM image of the diamond-shaped boron nitride powder synthesized at low temperature based on the molten salt method shown in FIG. 1.
Detailed Description
The invention is further described with reference to the following figures and detailed description, without limiting its scope.
In this embodiment:
the purity of the boron source is more than or equal to 97.0 wt%; the granularity of the boron source is less than or equal to 0.1 mm.
The purity of the ammonium chloride is more than or equal to 99.5 wt%; the granularity of the ammonium chloride is less than or equal to 0.1 mm.
The purity of the sodium chloride is more than or equal to 99.5 wt%; the granularity of the sodium chloride is less than or equal to 0.1 mm.
The purity of the potassium chloride is more than or equal to 99.5 wt%; the granularity of the potassium chloride is less than or equal to 0.1 mm.
The detailed description is omitted in the embodiments.
Example 1
a low-temperature synthesized diamond boron nitride powder based on a molten salt growth method and a preparation method thereof. The preparation method in this example is:
Step one, mixing 17-20 wt% of boron source, 35-38 wt% of ammonium chloride, 19-20 wt% of sodium chloride and 23-26 wt% of potassium chloride to obtain a mixture.
and secondly, under the condition of a nitrogen atmosphere, heating the mixture to 280-300 ℃ at the speed of 1.5-2 ℃/min, heating to 700-800 ℃ at the speed of 3-4 ℃/min, preserving heat for 3-4 h, and naturally cooling to obtain a reaction product.
And step three, soaking the reaction product in distilled water for 1-2 hours, washing with distilled water for 2-3 times, and drying at 100-110 ℃ to obtain the rhombus boron nitride powder synthesized at low temperature based on the molten salt method.
In this embodiment, the boron source is potassium borohydride.
Example 2
A low-temperature synthesized diamond boron nitride powder based on a molten salt growth method and a preparation method thereof. This example is the same as example 1 except that the boron source is sodium borohydride.
Example 3
A low-temperature synthesized diamond boron nitride powder based on a molten salt growth method and a preparation method thereof. The preparation method in this example is:
Step one, mixing 16-19 wt% of boron source, 36-39 wt% of ammonium chloride, 20-21 wt% of sodium chloride and 22-25 wt% of potassium chloride to obtain a mixture.
And secondly, under the condition of a nitrogen atmosphere, heating the mixture to 280-300 ℃ at the speed of 1.5-2 ℃/min, heating to 800-900 ℃ at the speed of 3.5-4.5 ℃/min, preserving the heat for 3-4 h, and naturally cooling to obtain a reaction product.
And step three, soaking the reaction product in distilled water for 1-2 hours, washing with distilled water for 2-3 times, and drying at 100-110 ℃ to obtain the rhombus boron nitride powder synthesized at low temperature based on the molten salt method.
In this embodiment, the boron source is sodium borohydride.
Example 4
A low-temperature synthesized diamond boron nitride powder based on a molten salt growth method and a preparation method thereof. This example is the same as example 3 except that the boron source is potassium borohydride.
Example 5
A low-temperature synthesized diamond boron nitride powder based on a molten salt growth method and a preparation method thereof. The preparation method in this example is:
Step one, mixing 15-18 wt% of boron source, 37-40 wt% of ammonium chloride, 18-19 wt% of sodium chloride and 24-27 wt% of potassium chloride to obtain a mixture.
And secondly, under the condition of a nitrogen atmosphere, heating the mixture to 280-300 ℃ at the speed of 1.5-2 ℃/min, heating to 750-850 ℃ at the speed of 4-5 ℃/min, preserving heat for 3-4 h, and naturally cooling to obtain a reaction product.
And step three, soaking the reaction product in distilled water for 1-2 hours, washing with distilled water for 2-3 times, and drying at 100-110 ℃ to obtain the rhombus boron nitride powder synthesized at low temperature based on the molten salt method.
in this embodiment, the boron source is potassium borohydride.
Example 6
A low-temperature synthesized diamond boron nitride powder based on a molten salt growth method and a preparation method thereof. This example is the same as example 5 except that the boron source is sodium borohydride.
Compared with the prior art, the specific implementation mode has the following positive effects:
according to the specific embodiment, potassium borohydride or sodium borohydride is used as a boron source, ammonium chloride is used as a nitrogen source, sodium chloride and potassium chloride are used as molten salts, the temperature is kept for 3-4 hours under the condition of nitrogen atmosphere and low temperature of 700-900 ℃, reaction products are obtained, then distilled water is used for washing, and drying is carried out, so that the rhombus boron nitride powder synthesized at low temperature based on the molten salt method is obtained, and therefore the synthesis temperature is low, the period is short, and the process is simple. The potassium borohydride or sodium borohydride, ammonium chloride, sodium chloride and potassium chloride used in the specific embodiment can be purchased in the market, and have low price and low production cost.
The diamond-shaped boron nitride powder prepared by the embodiment and synthesized at a low temperature based on the molten salt method is shown in the attached drawing, and fig. 1 is an XRD (X-ray diffraction) diagram of the diamond-shaped boron nitride powder prepared in example 1 and synthesized at a low temperature based on the molten salt method; FIG. 2 is an SEM image of the diamond-shaped boron nitride powder synthesized at low temperature based on the molten salt method shown in FIG. 1. As can be seen from FIG. 1, the product obtained has high purity; as can be seen from FIG. 2, the product has uniform morphology, good crystal growth, a length of about 200-300 nm, and a thickness of about 40-70 nm.
The raw materials used in the specific embodiment are all easy to dissolve in water, and the reaction product can be cleaned by water, so that the high-purity diamond boron nitride powder synthesized at low temperature based on a molten salt method can be obtained; the method adopts a molten salt method to synthesize diamond-shaped boron nitride powder at low temperature based on the molten salt method, and because the eutectic point of sodium chloride and potassium chloride molten salt is 657 ℃, a liquid phase environment can be generated at 657 ℃, the reaction rate is improved, the reaction conditions are reduced, and the powder obtained by the molten salt method has a uniform structure.
According to the specific embodiment, the temperature of the mixture is increased to 280-300 ℃ at the speed of 1.5-2 ℃/min, so that ammonium chloride and potassium borohydride (or sodium borohydride) can generate stable substances, and the volatilization loss of ammonium chloride in the subsequent temperature increasing process can be obviously reduced.
Therefore, the specific implementation mode has the characteristics of low cost, low synthesis temperature, simple production process and short period; the rhombus boron nitride powder prepared by the method based on the molten salt growth method and synthesized at low temperature has high purity and good crystal growth.
Claims (5)
1. A preparation method for synthesizing diamond-shaped boron nitride powder at low temperature based on a molten salt growth method is characterized by comprising the following steps:
Step one, mixing 15-20 wt% of boron source, 35-40 wt% of ammonium chloride, 18-21 wt% of sodium chloride and 22-27 wt% of potassium chloride to obtain a mixture;
Step two, under the condition of nitrogen atmosphere, firstly heating the mixture to 280-300 ℃ at the speed of 1.5-2 ℃/min, then heating to 700-900 ℃ at the speed of 3-5 ℃/min, preserving heat for 3-4 h, and naturally cooling to obtain a reaction product;
Soaking the reaction product in distilled water for 1-2 h, washing with distilled water for 2-3 times, and drying at 100-110 ℃ to obtain the rhombus boron nitride powder synthesized at low temperature based on the molten salt method;
The boron source is potassium borohydride or sodium borohydride, and the purity is more than or equal to 97.0 wt%; the granularity of the boron source is less than or equal to 0.1 mm.
2. The method for preparing diamond-shaped boron nitride powder based on molten salt growth by low-temperature synthesis according to claim 1, wherein the purity of ammonium chloride is more than or equal to 99.5 wt%; the granularity of the ammonium chloride is less than or equal to 0.1 mm.
3. The preparation method for synthesizing diamond-shaped boron nitride powder at low temperature based on the molten salt growth method according to claim 1, wherein the purity of the sodium chloride is more than or equal to 99.5 wt%; the granularity of the sodium chloride is less than or equal to 0.1 mm.
4. The preparation method for synthesizing diamond-shaped boron nitride powder at low temperature based on the molten salt growth method according to claim 1, wherein the purity of the potassium chloride is more than or equal to 99.5 wt%; the granularity of the potassium chloride is less than or equal to 0.1 mm.
5. the diamond-shaped boron nitride powder synthesized at low temperature based on the molten salt method is characterized by being prepared by the preparation method for synthesizing the diamond-shaped boron nitride powder at low temperature based on the molten salt method according to any one of claims 1 to 4.
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