CN102351208A - Method for rapidly producing boron nitride by using intermediate frequency carbon tube furnace - Google Patents

Method for rapidly producing boron nitride by using intermediate frequency carbon tube furnace Download PDF

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CN102351208A
CN102351208A CN2011101901444A CN201110190144A CN102351208A CN 102351208 A CN102351208 A CN 102351208A CN 2011101901444 A CN2011101901444 A CN 2011101901444A CN 201110190144 A CN201110190144 A CN 201110190144A CN 102351208 A CN102351208 A CN 102351208A
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boron nitride
intermediate frequency
tube furnace
carbon tube
frequency carbon
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谷云乐
张来平
葛春晓
常吉生
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Wuhan Institute of Technology
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Abstract

The invention relates to a preparation method of hexagonal boron nitride powder, which comprises the following steps of: with an intermediate frequency carbon tube furnace as production equipment, adding materials comprising melamine and boric acid into a high speed mixer according to molar ratio and evenly mixing to obtain a mixture; filling the mixture into a graphite boat of the intermediate frequency carbon tube furnace; under a nitrogen atmosphere at 1600 to 2000 DEG C, continuously pushing boats into the intermediate frequency carbon tube furnace to realize rapid and continuous production of hexagonal boron nitride with high purity; and crushing to prepare boron nitride powder. The method has the beneficial effects that: (1) the demanded temperature of reaction can be reached by rapidly heating, heating evenness is realized, the capabilities of effectively improving reaction synthetic efficiency and shortening production cycle are achieved; and because the technology for preparing the hexagonal boron nitride powder only comprises the processes of raw material mixing, reacting and product crushing, the advantages of simple operation, low energy consumption, high yield, low cost, good product quality and suitability for scale production are realized; and (2) the product purity is increased, the purity of the produced hexagonal boron nitride is higher than 97wt%, and the hexagonal boron nitride can be used for industrial application without further purification.

Description

A kind of method of utilizing the quick production boron nitride of intermediate frequency carbon tube furnace
Technical field
The present invention relates to field of ceramic material preparation, the concrete preparation method who relates to a kind of hexagonal boron nitride powder.
Background technology
Boron nitride is a kind of novel inorganic materials, it mainly contain six sides, cube and oblique three kinds of crystal formations in side, with regard to use range, hexagonal boron nitride is used the most extensive.Hexagonal boron nitride has excellent high-temperature oxidation resistance, chemical stability, excellent lubricity, high heat conductance, good neutron absorptive character and good wave penetrate capability etc.; Can be widely used in high-tech areas [1 such as machinery, metallurgy, electronics, aerospace; 2], therefore shown great attention to by scientific circles and industry member always.
Hexagonal boron nitride after being synthesized out in 1842, and the synthesis method that has developed at present is tens kinds [3] nearly, mainly comprise borax-urea (ammonium chloride) method, hydrothermal synthesis method, chemical vapor deposition (CVD) method etc.There are [4] such as up-to-date synthesis method of report such as Hao to adopt H before this 3BO 3, white phosphorus and NaN 3For raw material has synthesized the hexagonal nanometer boron nitride micro mist with hydrothermal method under 300 ℃ of conditions; Dong Shouyi [5] etc. are solvent with benzene or xylenes, under 250 ℃, use Li 3N and BBr 3It is brilliant to have synthesized spherical hexagonal nano.The boron nitride powder granularity of hydrothermal synthesis method preparation is little, but productive rate is very low, is not suitable for suitability for industrialized production.Tang Chengchun employing CVD methods such as [6] selects suitable boron source at NH 3Synthesized hexagonal nanometer boron nitride microsphere under the atmosphere, its purity and sphericity are very high, but need accurately control reaction conditions in the preparation process.What industrial production hexagonal boron nitride employing at present was more is borax-urea (ammonium chloride) method, promptly does main boron source with boric acid, boric anhydride, borax etc., and urea, trimeric cyanamide etc. is done nitrogenous source, at NH 3Or N 2Synthetic hexagonal boron nitride in the atmosphere.For example, Hu Wanying [7] forms intermediates at 200～600 ℃ of following pre-reaction 2～3h earlier with borax, ammonium chloride, then at 700～1000 ℃ NH 3React 4～10h under the atmosphere and form high purity BN powder, obviously reduce but glass mutual-assistance output occurs in the reaction, and the aftertreatment difficulty.[8] such as happy red will earlier at 900 ℃ of following vacuum heat-preserving 30min, obtain purity and are 95.6% hexagonal boron nitride with boric acid, borax and urea then after being incubated 2.5h under 1300 ℃ of nitrogen.Also have report to prepare boron nitride powder with boric acid and trimeric cyanamide before this, for example, Qiu Tai etc. [9] are after raw material adopts ball mill mixing or heating for dissolving legal system to be equipped with presoma with boric acid and trimeric cyanamide, and under 1700 ℃ of nitrogen atmospheres, insulation 3h makes boron nitride particle; Ni Kun etc. [10] prepare presoma with boric acid and trimeric cyanamide, add crystallization auxiliary, and behind insulation 2～12h under 800～2000 ℃, pickling is purified and obtained the macrocrystalline hexagonal boron nitride powder.These methods are owing to the restriction on the building-up reactions equipment, and the general reaction times is long partially, and the production cycle is long partially, can not continuous production.
Reference
[1] Ge Lei, poplar is built, Qiu Tai. preparing method's progress [J] of hexagonal boron nitride. and electronic component and material, 2008,27 (6): 22-29.
[2]Robert T.P.，Chaitanya K.N..Synthetic routes to boron nitride[J].Chem.Rev.，1990，90(1)：73-91.
[3]Guo Shengguan，Lu Bo，Wang Jisen，Ning Hongta，Xu Qingxin.Study of application and synthesis of boron nitride[J].Shandong Machinery，2004，6：16-19.
[4]Yu Meiyan，Li Kai，Hao Xiaopeng，Lai Zefeng，Wang Qilong，Cui Deliang，Some key factors affecting the hydrothermal synthesis of boron nitride crystals[J].Journal of Synthetic Crystals，2004，33(3)：328-331.
[5] Dong Shouyi, Hao Xiaopeng .GaP such as Yu Meiyan are nanocrystalline to the thing phase of the synthetic boron nitride of solvent thermal and the influence [J] of microcosmic appearance. functional materials, 2004,6 (35): 695-697.
[6] Tang Chengchun, Ding Xiaoxia, Gao Jianming etc. a kind of hexagonal nanometer boron nitride microsphere and synthesis method and application [P] .CN1931719A.
[7] Hu Wanying. synthesize the novel process [J] of hexagonal boron nitride continuously. modern technologies pottery, 2002,23 (2): 35-36
[8] find pleasure in red will, Tian Guishan, it is beautiful to record, and opens and walks slowly like a woman. and utilize the vacuum nitriding stove to prepare hexagonal boron nitride powder technical study and sign [J]. silicate is circulated a notice of, and 2010,29 (2): 444-449.
[9] high honour, Qiu Tai, Shen Chunying. boric acid and trimeric cyanamide precursor legal system are equipped with the research of hexagonal boron nitride. Chinese silicate association academic nd Annual Meeting summary collection [C] in 2003, Beijing in 2003
[10] Ni Kun, Song Mingzhi, eschscholtzia, Zhou Xiaodong. production method of macrocrystalline hexagonal boron nitride [P] .CN101891165A
[11] Chinese Academy of Sciences Shanghai silicate chemistry and engineering institute compile. ceramic analysis [M]. and Shanghai, the 1976.199. of the Shanghai People's Press
[12]R.Arenal，A.Ferrari，S.Reich，et al.Raman Spectroscopy of Single-Wall Boron Nitride Nanotubes[J].Nano Lett.，2006，6：1812～1816.
[13]C.Zhi，Y.Bando，C.C.Tang，D.Golberg，Immobilization of proteins on boron nitride nanotubes[J].J.Am.Chem.Soc.2005，127：17144-17145.
[14]R.S.Wagner，W.C.Ellis，Vapor-liquid-solid mechanism of single crystal growth[J].Appl.Phys.Lett.1964，4：89-90.
Summary of the invention:
Problem to be solved by this invention is the deficiency of above-mentioned prior art and the preparation method of a kind of " continuously push boat type intermediate frequency carbon tube furnace " the quick synthesis of high purity hexagonal boron nitride of method powder of proposing; Preparation technology only comprises raw materials mix, reaction and product crushing process; Simple to operate; Energy expenditure is low; Productive rate is high; Cost is low, and quality product is good, is fit to large-scale production.
The solution that the present invention adopts is: a kind of method of utilizing the quick production boron nitride of intermediate frequency carbon tube furnace is a production unit with the intermediate frequency carbon tube furnace, and material trimeric cyanamide and boric acid are pressed a mole proportioning C 3N 6H 6: H 3BO 3After mixing in=1: 1.25～3.5 adding high speed mixers; Pack in the graphite boat of intermediate frequency carbon tube furnace; Be loaded with 1～15kg material in each graphite boat; Under 1600～2000 ℃ of temperature of reaction and nitrogen atmosphere; Whenever in the intermediate frequency carbon tube furnace, push away boat continuously at a distance from 10～40min; Can realize rapid Continuous production high purity hexagonal boron nitride, obtain boron nitride powder through pulverizing again.
Press such scheme, described intermediate frequency carbon tube furnace, its cavity are horizontal circle shaped reaction cavity, and frequency is 300～1000HZ.
Press such scheme, the quality of material trimeric cyanamide and boric acid is 2～12kg in described each graphite boat, and in the intermediate frequency carbon tube furnace, pushing away boat pitch time continuously is 15～25min.
Press such scheme, the mole proportioning of described trimeric cyanamide and boric acid is C 3N 6H 6: H 3BO 3=1: 1.75～3.0, described trimeric cyanamide and boric acid are 100～300 order pressed powders, purity>=99.5wt%.
Press such scheme, said nitrogen atmosphere flow velocity is 2～10L/min, and nitrogen inlet is arranged on the graphite boat exit end of intermediate frequency carbon tube furnace, so that nitrogen feeds.
Press such scheme, the temperature of said reaction is 1800～1950 ℃, and hexagonal boron nitride powder crystallization that obtains and purity are best, and purity＞97wt.%, grain diameter are 0.5～10 μ m.
The reaction equation that exists in the synthetic hexagonal boron nitride powder process of " push boat type intermediate frequency carbon tube furnace continuously " method that the present invention relates to is following:
2C 3N 6H 6+4H 3BO 3＝B 4N 3O 2H+4H 2NCN+2CO 2+NH 3+6H 2O (1)
B 4N 3O 2H+3/2N 2+2H 2O＝4BN+5/2H 2+2NO 2 (2)
B 4N 3O 2H＝8BN+2B 2O 3+NH 3 (3)
B 2O 3+2NH 3＝2BN+3H 2O (4)
In experimentation, C at first 3N 6H 6And H 3BO 3Reaction at high temperature generates the intermediate product B of boracic, nitrogen 4N 3O 2H discharges a large amount of gas H simultaneously 2NCN, CO 2, NH 3And water vapour (formula 1).Most of intermediate product B 4N 3O 2H is at N 2The atmosphere effect forms BN down, and has been accompanied by H 2And NO 2Gas release (formula 2).Simultaneously, few part B 4N 3O 2H at high temperature directly resolves into BN, B 2O 3And NH 3(formula 3), newly-generated B 2O 3Again and NH 3Effect generate down BN (formula 4).Discharge a large amount of gas in the whole reaction system, gas evolution can play the effect of isolating product particle, avoids the grained sintered and reunion of hexagonal boron nitride.
Beneficial effect of the present invention is: (1) the present invention adopts the intermediate frequency carbon tube furnace to be rapidly heated and reaches and reacts needed temperature, homogeneous heating, and help effectively improving the reaction combined coefficient, shorten the production cycle.The present invention prepares the hexagonal boron nitride powder craft and only comprises raw materials mix, reaction and product crushing process, and simple to operate, energy expenditure is low, and productive rate is high, and cost is low, and quality product is good, is fit to large-scale production; (2) the present invention adopts nitrogen atmosphere that required nitrogenous source in the reaction process can be provided effectively apace, improves reaction efficiency, and helps reducing oxygen level in the product.Nitrogen inlet is arranged on the graphite boat exit end, avoids product by exhaust emission, improve product purity, the hexagonal boron nitride purity＞97wt% that is produced need not to be further purified and just can drop into the industry use.
Description of drawings
Fig. 1 is an intermediate frequency carbon tube furnace structure diagram of producing hexagonal boron nitride;
Fig. 2 is the XRD spectra of the hexagonal boron nitride sample of embodiment 1;
Fig. 3 is the Raman spectrogram of the hexagonal boron nitride sample of embodiment 1;
Fig. 4 is the FTIR spectrogram of the hexagonal boron nitride sample of embodiment 1;
Fig. 5 is the SEM photo of the hexagonal boron nitride sample of embodiment 1.
Embodiment
Further introduce the present invention through embodiment below, but embodiment can not be construed as limiting the invention.
Embodiment 1
Take by weighing 226kg trimeric cyanamide and 250kg boric acid (mole proportioning C 3N 6H 6: H 3BO 3=1: 2.25) add mix in the high speed mixer after; The graphite boat of each the intermediate frequency carbon tube furnace 8.5kg mixture of packing into; The adjusting nitrogen flow rate is 5L/min; After graphite boat being pushed the reaction cavity of 1850 ℃ of intermediate frequency carbon tube furnaces; Trimeric cyanamide and boric acid fully react, and whenever in the intermediate frequency carbon tube furnace, advance boat and go out boat at a distance from 20min and carry out continuously, can make white hexagonal boron nitride continuously; Obtaining boron nitride powder product 98.6kg after the pulverizing altogether, is that its productive rate of base of calculation is up to 98.54% with boric acid.
Intermediate frequency carbon tube furnace structure diagram of the present invention such as accompanying drawing 1; Mainly comprise carbon pipe 2, body of heater coil 3 and graphite boat 4; Its cavity is a horizontal circle shaped reaction cavity; Frequency is 300～1000HZ; Reaction atmosphere nitrogen inlet 1 is arranged on graphite boat exit end 8 places of intermediate frequency carbon tube furnace; Waste gas outlet 5 is arranged on the graphite boat exit end 7 of intermediate frequency carbon tube furnace, as scheming direction for pushing away boat direction 6.
Hexagonal boron nitride samples obtained X-ray diffraction (XRD) analysis using XD-5A X-ray powder diffractometer (30kV, 20mA,
Figure BDA0000074467620000041
), 2θ at 20 ~ 80 ° range, current 30mA, voltage 30kV.Infrared spectrogram (FTIR) is with Nicolet-6700 type infrared spectrometer, and the KBr pressed powder is used in sample preparation.Raman spectrogram (Raman) is with Nicolet-DXR type Raman spectrometer, and excitation light source is the Nd:YAG laser apparatus, excitation wavelength 532nm.Observe pattern with the scanning electronic microscope (SEM) of JSM-5510LV model, method for making sample is directly to adopt the product powder distribution on the double faced adhesive tape and be bonded on the sample copper platform and observe behind the metal spraying.Adopt neutralization titration to measure the nitrogen content [11] of synthetic hexagonal boron nitride.
Accompanying drawing 2 is XRD spectra of hexagonal boron nitride sample.From the XRD patterns can be seen in all of the diffraction peaks at d values 3.3532,2.1831,2.0732,1.8233,1.6705,
Figure BDA0000074467620000042
Office, corresponding to the hexagonal boron nitride (002), (100), (101), (102 ), (004), (110) crystal face.By each crystal face d value of XRD, calculating the product lattice constant is a=0.2515nm, c=0.6789nm, and with the a=0.2504nm of standard card JCPDS 73-2095 report, c=0.6661nm conforms to basically, proves that the product that makes is a hexagonal boron nitride.Do not occur other impurity characteristics diffraction peaks in addition, showing does not have other crystalline impurity in the product.
Accompanying drawing 3 is Raman spectrograms of hexagonal boron nitride sample.Be positioned at 1354cm -1The absorption peak of wavelength is corresponding to the cancellated E2g in plane vibration of hexagonal boron nitride pattern [12].The characteristic peak that does not occur other in the collection of illustrative plates, showing does not have uncombined carbon and carbon compound in the product.
Accompanying drawing 4 is that the hexagonal boron nitride sample is at 500～4000cm -1FTIR spectrogram in the wavelength region.Be positioned at 813cm -1And 1374cm -1The outer TO vibration of face of the corresponding B-N key of absorption peak difference at wavelength around place and the in plane vibration pattern [13,14] of B-N-B key.At 3416cm -1Near the absorption band peak be because after the sample surfaces partial hydrolysis due to the O-H key.The TTIR collection of illustrative plates is not observed the absorption band peak of other impurity, illustrates that product purity is very high.
Accompanying drawing 5 is SEM photos of hexagonal boron nitride sample, has shown product pattern and size.Scale length is represented 1 μ m in the photo.Visible by photo, the boron nitride particle that is obtained in the form of sheets, the particle dia scope is 0.5～5 μ m, mean thickness is about 250nm.
The nitrogen content that adopts neutralization titration to measure synthetic hexagonal boron nitride product is 55.71wt.%, and can calculate boron nitride purity is 98.73wt.%.
Embodiment 2
Change feed molar proportioning among the embodiment 1, take by weighing 275kg trimeric cyanamide and 250kg boric acid (mole proportioning C 3N 6H 6: H 3BO 3=1: 1.85), other synthesis technologic parameter and embodiment 1 remain unchanged, and obtain boron nitride powder product 97.3kg altogether, are that its productive rate of base of calculation is up to 97.21% with boric acid.Product is through XRD, Raman, FTIR, sem analysis are indicated as the high purity hexagonal boron nitride, particle in the form of sheets, the particle dia scope is 2～10 μ m, mean thickness is about 350nm.The nitrogen content that adopts neutralization titration to measure synthetic hexagonal boron nitride product is 54.97wt.%, and can calculate boron nitride purity is 97.45wt.%.
Embodiment 3
Change 1950 ℃ of temperature of reaction (intermediate frequency carbon tube furnace temperature) among the embodiment 1, other synthesis technologic parameter and embodiment 1 remain unchanged, and obtain boron nitride powder product 98.1kg altogether, are that its productive rate of base of calculation is up to 98.21% with boric acid.Product is through XRD, Raman, FTIR, sem analysis are indicated as the high purity hexagonal boron nitride, particle in the form of sheets, the particle dia scope is 0.5～5 μ m, mean thickness is about 300nm.The nitrogen content that adopts neutralization titration to measure synthetic hexagonal boron nitride product is 55.26wt.%, and can calculate boron nitride purity is 97.93wt.%.
Embodiment 4
Take by weighing 275kg trimeric cyanamide and 250kg boric acid (mole proportioning C 3N 6H 6: H 3BO 3=1: 1.85) add mix in the high speed mixer after; Each graphite boat 12kg mixture of packing into; The adjusting nitrogen flow rate is 6L/min; After graphite boat being pushed the reaction cavity of 1850 ℃ of intermediate frequency carbon tube furnaces; Trimeric cyanamide and boric acid fully react, and whenever in the intermediate frequency carbon tube furnace, advance boat and go out boat at a distance from 30min and carry out continuously, can make white hexagonal boron nitride powder continuously; Obtaining boron nitride powder product 97.3kg after the pulverizing altogether, is that its productive rate of base of calculation is up to 97.42% with boric acid.Product is through XRD, Raman, FTIR, sem analysis are indicated as the high purity hexagonal boron nitride, particle in the form of sheets, the particle dia scope is 1～10 μ m, mean thickness is about 300nm.The nitrogen content that adopts neutralization titration to measure synthetic hexagonal boron nitride product is 54.80wt.%, and can calculate boron nitride purity is 97.14wt.%.

Claims (6)

1. a method of utilizing the quick production boron nitride of intermediate frequency carbon tube furnace is characterized in that with the intermediate frequency carbon tube furnace be production unit, and material trimeric cyanamide and boric acid are pressed a mole proportioning C 3N 6H 6: H 3BO 3After mixing in=1: 1.25～3.5 adding high speed mixers; Pack in the graphite boat of intermediate frequency carbon tube furnace; Be loaded with 1～15kg material in each graphite boat; Under 1600～2000 ℃ of temperature of reaction and nitrogen atmosphere; Whenever in the intermediate frequency carbon tube furnace, push away boat continuously at a distance from 10～40min; Can realize rapid Continuous production high purity hexagonal boron nitride, obtain boron nitride powder through pulverizing again.
2. the method for utilizing the quick production boron nitride of intermediate frequency carbon tube furnace according to claim 1 is characterized in that described intermediate frequency carbon tube furnace, and its cavity is a horizontal circle shaped reaction cavity, and frequency is 300～1000HZ.
3. the method for utilizing the quick production boron nitride of intermediate frequency carbon tube furnace according to claim 1 and 2; It is characterized in that the quality of material trimeric cyanamide and boric acid is 2～12kg in described each graphite boat, in the intermediate frequency carbon tube furnace, pushing away boat pitch time continuously is 15～25min.
4. the method for utilizing the quick production boron nitride of intermediate frequency carbon tube furnace according to claim 1, the mole proportioning that it is characterized in that described trimeric cyanamide and boric acid is C 3N 6H 6: H 3BO 3=1: 1.75～3.0, described trimeric cyanamide and boric acid are 100～300 order pressed powders, purity>=99.5wt%.
5. the method for utilizing the quick production boron nitride of intermediate frequency carbon tube furnace according to claim 1 is characterized in that said nitrogen atmosphere flow velocity is 2～10L/min, and nitrogen inlet is arranged on the graphite boat exit end of intermediate frequency carbon tube furnace.
6. the method for utilizing the quick production boron nitride of intermediate frequency carbon tube furnace according to claim 1, the temperature that it is characterized in that said reaction is 1800～1950 ℃.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104528669A (en) * 2014-12-03 2015-04-22 营口天元化工研究所股份有限公司 Synthesis method for hexagonal boron nitride
CN106414311A (en) * 2013-11-27 2017-02-15 北伊利诺斯大学董事会 Boron nitride and method of producing boron nitride
CN108239784A (en) * 2018-03-23 2018-07-03 韶关保绿环保科技股份有限公司 Zone melting furnace system
CN109336128A (en) * 2018-12-25 2019-02-15 董克胜 A kind of process producing 99%-99.99% high-purity pure boron
CN109809374A (en) * 2019-01-16 2019-05-28 武汉工程大学 A kind of push boat type semi-continuous process boron nitride nano-tube prepares furnace and its application method
CN115850885A (en) * 2023-02-16 2023-03-28 河北恒源线缆有限公司 Overhead cable with corrosion-resistant shell and preparation method thereof

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CN2218916Y (en) * 1994-12-28 1996-01-31 中国科学院金属研究所 Intermediate frequency induction furnace for preparing crucible product for pyrolyzing boron nitride
CN101891165A (en) * 2010-07-15 2010-11-24 丹东市化工研究所有限责任公司 Production method of macrocrystalline hexagonal boron nitride

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Publication number Priority date Publication date Assignee Title
CN2218916Y (en) * 1994-12-28 1996-01-31 中国科学院金属研究所 Intermediate frequency induction furnace for preparing crucible product for pyrolyzing boron nitride
CN101891165A (en) * 2010-07-15 2010-11-24 丹东市化工研究所有限责任公司 Production method of macrocrystalline hexagonal boron nitride

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106414311A (en) * 2013-11-27 2017-02-15 北伊利诺斯大学董事会 Boron nitride and method of producing boron nitride
CN104528669A (en) * 2014-12-03 2015-04-22 营口天元化工研究所股份有限公司 Synthesis method for hexagonal boron nitride
CN108239784A (en) * 2018-03-23 2018-07-03 韶关保绿环保科技股份有限公司 Zone melting furnace system
CN109336128A (en) * 2018-12-25 2019-02-15 董克胜 A kind of process producing 99%-99.99% high-purity pure boron
CN109809374A (en) * 2019-01-16 2019-05-28 武汉工程大学 A kind of push boat type semi-continuous process boron nitride nano-tube prepares furnace and its application method
CN109809374B (en) * 2019-01-16 2022-07-19 武汉工程大学 Push boat type semi-continuous boron nitride nanotube preparation furnace and use method thereof
CN115850885A (en) * 2023-02-16 2023-03-28 河北恒源线缆有限公司 Overhead cable with corrosion-resistant shell and preparation method thereof
CN115850885B (en) * 2023-02-16 2023-04-25 河北恒源线缆有限公司 Overhead cable with corrosion-resistant shell and preparation method thereof

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