CN114890393B - Low-temperature preparation method of BN microsphere - Google Patents

Low-temperature preparation method of BN microsphere Download PDF

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CN114890393B
CN114890393B CN202210296958.4A CN202210296958A CN114890393B CN 114890393 B CN114890393 B CN 114890393B CN 202210296958 A CN202210296958 A CN 202210296958A CN 114890393 B CN114890393 B CN 114890393B
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CN114890393A (en
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王兵
王应德
李威
邵长伟
王小宙
韩成
龙鑫
杜贻昂
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National University of Defense Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary 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
    • C01B21/064Binary 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
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    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention discloses a low-temperature preparation method of BN microspheres, which comprises the steps of preparing a homogeneous solution with mass concentration of 0.1-0.5 g/ml in a solvent by taking trichloroborazine as a raw material; and (3) carrying out solvothermal treatment on the homogeneous solution for 1-12 h at the temperature of 120-220 ℃, naturally placing or quenching to room temperature, and centrifuging to obtain BN microspheres. The preparation method provided by the invention has the advantages of simple process, no need of adding any additive, low cost, high yield of over 99.6 percent, high purity of the prepared BN microsphere, uniform morphology and small dispersity.

Description

一种BN微球的低温制备方法A kind of low-temperature preparation method of BN microsphere

技术领域technical field

本发明涉及有机合成技术领域,尤其是一种BN微球的低温制备方法。The invention relates to the technical field of organic synthesis, in particular to a low-temperature preparation method of BN microspheres.

背景技术Background technique

氮化硼(BN)陶瓷具有高热导率、高稳定性,能在900℃以下的氧化气氛中和2800℃以上的惰性气氛中使用,BN粉体作为加热容器内衬,可大幅降低烧成温度同时显著提高容器的致密性和柔韧性。BN还具有电绝缘性、低介电性、自润滑性、屏蔽性及高的化学稳定性等独特的物理化学性质,BN及其复合材料是优良的耐高温透波、耐腐蚀抗辐射及高频高压绝缘散热材料。Boron nitride (BN) ceramics has high thermal conductivity and high stability, and can be used in an oxidizing atmosphere below 900°C and an inert atmosphere above 2800°C. BN powder can be used as a lining of a heating vessel, which can greatly reduce the firing temperature At the same time, the compactness and flexibility of the container are significantly improved. BN also has unique physical and chemical properties such as electrical insulation, low dielectric, self-lubricating, shielding and high chemical stability. BN and its composite materials are excellent high temperature resistance, wave penetration, corrosion resistance, radiation resistance and high High frequency and high voltage insulation and heat dissipation materials.

目前,BN粉体的制备方法主要有硼砂合成法、尿素法、卤化物合成法,这些合成方法得到的BN粉体形貌不可控,合成温度均在1000℃以上,合成成本高、纯度低、工艺复杂。At present, the preparation methods of BN powder mainly include borax synthesis method, urea method, and halide synthesis method. The shape of BN powder obtained by these synthesis methods is uncontrollable, and the synthesis temperature is above 1000 ° C. The synthesis cost is high and the purity is low. The process is complicated.

发明内容Contents of the invention

本发明提供一种BN微球的低温制备方法,用于克服现有技术中合成成本高、工艺复杂等缺陷。The invention provides a low-temperature preparation method of BN microspheres, which is used to overcome the defects of high synthesis cost and complicated process in the prior art.

为实现上述目的,本发明提出一种BN微球的低温制备方法,包括以下步骤:In order to achieve the above object, the present invention proposes a low-temperature preparation method of BN microspheres, comprising the following steps:

S1:在无水无氧条件下,将三氯环硼氮烷(TCB)溶解在有机溶剂中配成0.1~0.5g/ml的均质溶液;S1: Under anhydrous and oxygen-free conditions, dissolve trichloroborazine (TCB) in an organic solvent to prepare a homogeneous solution of 0.1-0.5 g/ml;

S2:在无水无氧条件下,将所述均质溶液置于反应釜中,密封好后进行溶剂热反应,所述溶剂热反应的温度为120~220℃、时间为1~12h;S2: Under anhydrous and oxygen-free conditions, place the homogeneous solution in a reaction kettle, seal it well, and perform a solvothermal reaction. The temperature of the solvothermal reaction is 120-220° C., and the time is 1-12 hours;

S3:反应结束后自然或者淬冷至室温,得到BN微球。S3: Naturally or quenched to room temperature after the reaction to obtain BN microspheres.

为实现上述目的,本发明还提出一种BN微球,由上述所述低温制备方法制备得到;所述BN微球为实心微球,纯度大于99%,微球直径分布在1~5μm。To achieve the above object, the present invention also proposes a BN microsphere, which is prepared by the above-mentioned low-temperature preparation method; the BN microsphere is a solid microsphere with a purity greater than 99%, and the diameter of the microsphere is distributed in the range of 1-5 μm.

为实现上述目的,本发明还提出一种BN微球的应用,将上述所述低温制备方法制备得到的BN微球或者上述所述BN微球应用于耐火、润滑、热屏蔽和反应堆结构材料中。In order to achieve the above object, the present invention also proposes an application of BN microspheres, the BN microspheres prepared by the above-mentioned low-temperature preparation method or the above-mentioned BN microspheres are applied to refractory, lubrication, heat shielding and reactor structural materials .

与现有技术相比,本发明的有益效果有:Compared with prior art, the beneficial effect of the present invention has:

本发明提供的BN微球的低温制备方法以三氯环硼氮烷为原料,将该三氯环硼氮烷配成0.1~0.5g/ml的均质溶液,再将该均质溶液置于反应釜中进行溶剂热反应,溶剂热反应过程中由于加热会使反应釜具有一定的压力,在压力的作用下可促使溶剂热反应的正向进行,显著降低了反应所需的温度,从而降低成本。本发明提供的制备方法工艺简单,不需要添加任何添加剂,成本低,产率在99%以上,制备得到的BN微球纯度高(≧99.6%),形貌均一、分散度小。The low-temperature preparation method of BN microspheres provided by the present invention uses trichloroborazine as a raw material, prepares the trichloroborazine into a homogeneous solution of 0.1 to 0.5 g/ml, and then places the homogeneous solution in The solvothermal reaction is carried out in the reaction kettle. During the solvothermal reaction process, the reaction kettle will have a certain pressure due to heating. cost. The preparation method provided by the invention has simple process, does not need to add any additives, has low cost, and the yield is over 99%. The prepared BN microspheres have high purity (≧99.6%), uniform appearance and small dispersion.

附图说明Description of drawings

为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图示出的结构获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. For those skilled in the art, other drawings can also be obtained according to the structures shown in these drawings without creative effort.

图1是实施例4制备的BN实心微球SEM照片;Fig. 1 is the BN solid microsphere SEM photograph that embodiment 4 prepares;

图2为实施例4制备的BN实心微球红外光谱图。Fig. 2 is the infrared spectrogram of the BN solid microsphere prepared in Example 4.

本发明目的的实现、功能特点及优点将结合实施例,参照附图做进一步说明。The realization of the purpose of the present invention, functional characteristics and advantages will be further described in conjunction with the embodiments and with reference to the accompanying drawings.

具体实施方式Detailed ways

下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of the present invention.

另外,本发明各个实施例之间的技术方案可以相互结合,但是必须是以本领域普通技术人员能够实现为基础,当技术方案的结合出现相互矛盾或无法实现时应当认为这种技术方案的结合不存在,也不在本发明要求的保护范围之内。In addition, the technical solutions of the various embodiments of the present invention can be combined with each other, but it must be based on the realization of those skilled in the art. When the combination of technical solutions is contradictory or cannot be realized, it should be considered as a combination of technical solutions. Does not exist, nor is it within the scope of protection required by the present invention.

无特殊说明,所使用的药品/试剂均为市售。Unless otherwise specified, the drugs/reagents used were all commercially available.

本发明提出一种BN微球的低温制备方法,包括以下步骤:The present invention proposes a low-temperature preparation method of BN microspheres, comprising the following steps:

S1:在无水无氧条件下,将三氯环硼氮烷溶解在有机溶剂中配成0.1~0.5g/ml的均质溶液;S1: Under anhydrous and oxygen-free conditions, dissolve trichloroborazine in an organic solvent to prepare a homogeneous solution of 0.1-0.5 g/ml;

S2:在无水无氧条件下,将所述均质溶液置于反应釜中,密封好后进行溶剂热反应,所述溶剂热反应的温度为120~220℃、时间为1~12h;S2: Under anhydrous and oxygen-free conditions, place the homogeneous solution in a reaction kettle, seal it well, and perform a solvothermal reaction. The temperature of the solvothermal reaction is 120-220° C., and the time is 1-12 hours;

S3:反应结束后自然或者淬冷至室温,得到BN微球。S3: Naturally or quenched to room temperature after the reaction to obtain BN microspheres.

优选地,所述溶剂热反应的温度为200℃、时间为6h。Preferably, the temperature of the solvothermal reaction is 200° C. and the time is 6 h.

优选地,所述有机溶剂为甲苯、二甲苯、二氯苯和正戊烷中的至少一种。Preferably, the organic solvent is at least one of toluene, xylene, dichlorobenzene and n-pentane.

优选地,所述溶剂热反应釜中均质溶液体积占比不超过3/4。Preferably, the volume ratio of the homogeneous solution in the solvothermal reactor does not exceed 3/4.

优选地,所述均质溶液的浓度为0.1g/ml;所述溶剂热反应的温度为220℃、时间为1h。Preferably, the concentration of the homogeneous solution is 0.1 g/ml; the temperature of the solvothermal reaction is 220° C. and the time is 1 h.

优选地,所述均质溶液的浓度为0.3g/ml;所述溶剂热反应的温度为200℃、时间为6h。Preferably, the concentration of the homogeneous solution is 0.3 g/ml; the temperature of the solvothermal reaction is 200° C. and the time is 6 h.

优选地,所述均质溶液的浓度为0.5g/ml;所述溶剂热反应的温度为220℃、时间为1h。Preferably, the concentration of the homogeneous solution is 0.5 g/ml; the temperature of the solvothermal reaction is 220° C. and the time is 1 h.

优选地,所述均质溶液的浓度为0.5g/ml;所述溶剂热反应的温度为200℃、时间为6h。Preferably, the concentration of the homogeneous solution is 0.5 g/ml; the temperature of the solvothermal reaction is 200° C. and the time is 6 h.

本发明还提出一种BN微球,由上述所述低温制备方法制备得到;所述BN微球为实心微球,纯度大于99%,微球直径分布在1~5μm。The present invention also proposes a BN microsphere, which is prepared by the above-mentioned low-temperature preparation method; the BN microsphere is a solid microsphere with a purity greater than 99%, and the diameter of the microsphere is distributed in the range of 1-5 μm.

本发明还提出一种BN微球的应用,将上述所述低温制备方法制备得到的BN微球或者上述所述BN微球应用于耐火、润滑、热屏蔽和反应堆结构材料等领域中。The present invention also proposes an application of BN microspheres. The BN microspheres prepared by the above-mentioned low-temperature preparation method or the above-mentioned BN microspheres are applied to the fields of refractory, lubrication, heat shielding, and reactor structural materials.

实施例1Example 1

本实施例提供一种BN微球的低温制备方法,包括以下步骤:This embodiment provides a low-temperature preparation method of BN microspheres, comprising the following steps:

S1:在无水无氧条件下,将三氯环硼氮烷溶解在有机溶剂中配成0.1g/ml的均质溶液;S1: Under anhydrous and oxygen-free conditions, dissolve trichloroborazine in an organic solvent to prepare a 0.1g/ml homogeneous solution;

S2:在无水无氧条件下,将所述均质溶液置于200mL反应釜中,密封好后进行溶剂热反应,溶剂热反应的温度为220℃、时间为1h;S2: Under anhydrous and oxygen-free conditions, put the homogeneous solution in a 200mL reaction kettle, seal it well, and conduct a solvothermal reaction. The temperature of the solvothermal reaction is 220°C and the time is 1h;

S3:反应结束后自然或者淬冷至室温,得到BN实心微球。S3: Naturally or quenched to room temperature after the reaction to obtain BN solid microspheres.

实施例2Example 2

本实施例提供一种BN微球的低温制备方法,与实施例1相比,均质溶液浓度为0.5g/ml,其他过程同实施例1。This example provides a low-temperature preparation method of BN microspheres. Compared with Example 1, the concentration of the homogeneous solution is 0.5 g/ml, and other processes are the same as Example 1.

实施例3Example 3

本实施例提供一种BN微球的低温制备方法,与实施例1相比,均质溶液浓度为0.3g/ml,其他过程同实施例1。This example provides a low-temperature preparation method of BN microspheres. Compared with Example 1, the concentration of the homogeneous solution is 0.3 g/ml, and other processes are the same as Example 1.

实施例4Example 4

本实施例提供一种BN微球的低温制备方法,包括以下步骤:This embodiment provides a low-temperature preparation method of BN microspheres, comprising the following steps:

S1:在无水无氧条件下,将三氯环硼氮烷溶解在有机溶剂中配成0.3g/ml的均质溶液;S1: Under anhydrous and oxygen-free conditions, dissolve trichloroborazine in an organic solvent to prepare a 0.3g/ml homogeneous solution;

S2:在无水无氧条件下,将所述均质溶液置于200mL反应釜中,密封好后进行溶剂热反应,溶剂热反应的温度为200℃、时间为6h;S2: Under anhydrous and oxygen-free conditions, put the homogeneous solution in a 200mL reactor, seal it well, and perform solvothermal reaction, the temperature of the solvothermal reaction is 200°C, and the time is 6h;

S3:反应结束后自然或者淬冷至室温,得到BN实心微球。S3: Naturally or quenched to room temperature after the reaction to obtain BN solid microspheres.

本实施例制备得到的BN实心微球SEM照片如图1所示,由图可知,所制备的BN微球直径在2±0.5μm范围内。The SEM photo of the BN solid microspheres prepared in this example is shown in Figure 1 , and it can be seen from the figure that the diameter of the prepared BN microspheres is within the range of 2±0.5 μm.

本实施例制备得到的BN实心微球红外光谱图如图2所示,由图可知,所制备的BN红外光谱与商业BN的红外光谱基本一致。The infrared spectrum of the BN solid microspheres prepared in this example is shown in Figure 2. It can be seen from the figure that the infrared spectrum of the prepared BN is basically consistent with that of commercial BN.

实施例5Example 5

本实施例提供一种BN微球的低温制备方法,与实施例4相比,均质溶液浓度为0.5g/ml,其他过程同实施例4。This example provides a low-temperature preparation method of BN microspheres. Compared with Example 4, the concentration of the homogeneous solution is 0.5 g/ml, and other processes are the same as Example 4.

实施例6Example 6

本实施例提供一种BN微球的低温制备方法,与实施例4相比,均质溶液浓度为0.1g/ml,其他过程同实施例4。This example provides a low-temperature preparation method of BN microspheres. Compared with Example 4, the concentration of the homogeneous solution is 0.1 g/ml, and other processes are the same as Example 4.

实施例7Example 7

本实施例提供一种BN微球的低温制备方法,与实施例4相比,溶剂热反应的温度为120℃、时间为12h,其他过程同实施例4。This example provides a low-temperature preparation method of BN microspheres. Compared with Example 4, the temperature of the solvothermal reaction is 120° C. and the time is 12 hours, and other processes are the same as Example 4.

实施例8Example 8

本实施例提供一种BN微球的低温制备方法,与实施例4相比,溶剂热反应的温度为150℃、时间为10h,其他过程同实施例4。This example provides a low-temperature preparation method of BN microspheres. Compared with Example 4, the temperature of the solvothermal reaction is 150° C. and the time is 10 h, and other processes are the same as Example 4.

实施例9Example 9

本实施例提供一种BN微球的低温制备方法,与实施例4相比,溶剂热反应的温度为180℃、时间为10h,其他过程同实施例4。This example provides a low-temperature preparation method of BN microspheres. Compared with Example 4, the temperature of the solvothermal reaction is 180° C. and the time is 10 h, and other processes are the same as Example 4.

通过实施例1~9可知,均质溶液浓度将影响最终BN微球的产量,随着均质溶液浓度增大,最终产量呈上升趋势。溶剂热反应的温度和时间则直接影响BN微球的成核速率及生长速率从而控制这微球的直径、质量。From Examples 1 to 9, it can be known that the concentration of the homogeneous solution will affect the final yield of BN microspheres, and the final yield tends to increase as the concentration of the homogeneous solution increases. The temperature and time of the solvothermal reaction directly affect the nucleation rate and growth rate of BN microspheres, thereby controlling the diameter and quality of the microspheres.

以上所述仅为本发明的优选实施例,并非因此限制本发明的专利范围,凡是在本发明的发明构思下,利用本发明说明书及附图内容所作的等效结构变换,或直接/间接运用在其他相关的技术领域均包括在本发明的专利保护范围内。The above is only a preferred embodiment of the present invention, and does not therefore limit the patent scope of the present invention. Under the inventive concept of the present invention, the equivalent structural transformation made by using the description of the present invention and the contents of the accompanying drawings, or direct/indirect use All other relevant technical fields are included in the patent protection scope of the present invention.

Claims (7)

1.一种BN微球的低温制备方法,其特征在于,包括以下步骤:1. a low-temperature preparation method of BN microspheres, characterized in that, comprises the following steps: S1:在无水无氧条件下,将三氯环硼氮烷溶解在有机溶剂中配成0.1~0.5g/mL的均质溶液;所述有机溶剂为甲苯、二甲苯、二氯苯和正戊烷中的至少一种;S1: Under anhydrous and oxygen-free conditions, dissolve trichloroborazine in an organic solvent to form a homogeneous solution of 0.1~0.5g/mL; the organic solvent is toluene, xylene, dichlorobenzene and n-pentyl at least one of alkanes; S2:在无水无氧条件下,将所述均质溶液置于反应釜中,密封好后进行溶剂热反应,所述溶剂热反应的温度为120~220℃、时间为1~12h;S2: Under anhydrous and oxygen-free conditions, place the homogeneous solution in a reaction kettle, seal it, and perform a solvothermal reaction. The temperature of the solvothermal reaction is 120-220° C., and the time is 1-12 hours; S3:反应结束后自然或者淬冷至室温,得到BN微球;所述BN微球为实心微球,纯度大于99%,微球直径分布在1~5µm。S3: Naturally or quenching to room temperature after the reaction to obtain BN microspheres; the BN microspheres are solid microspheres with a purity greater than 99%, and the diameter of the microspheres is distributed between 1 and 5 μm. 2.如权利要求1所述的低温制备方法,其特征在于,所述溶剂热反应的温度为200℃、时间为6h。2. The low-temperature preparation method according to claim 1, wherein the temperature of the solvothermal reaction is 200°C and the time is 6h. 3.如权利要求1所述的低温制备方法,其特征在于,所述溶剂热反应釜中均质溶液体积占比不超过3/4。3. The low-temperature preparation method according to claim 1, wherein the volume ratio of the homogeneous solution in the solvothermal reactor is no more than 3/4. 4.如权利要求1所述的低温制备方法,其特征在于,所述均质溶液的浓度为0.1g/mL;所述溶剂热反应的温度为220℃、时间为1h。4 . The low-temperature preparation method according to claim 1 , wherein the concentration of the homogeneous solution is 0.1 g/mL; the temperature of the solvothermal reaction is 220° C. and the time is 1 h. 5.如权利要求1所述的低温制备方法,其特征在于,所述均质溶液的浓度为0.3g/mL;所述溶剂热反应的温度为200℃、时间为6h。5 . The low-temperature preparation method according to claim 1 , wherein the concentration of the homogeneous solution is 0.3 g/mL; the temperature of the solvothermal reaction is 200° C. and the time is 6 h. 6.如权利要求1所述的低温制备方法,其特征在于,所述均质溶液的浓度为0.5g/mL;所述溶剂热反应的温度为220℃、时间为1h。6 . The low-temperature preparation method according to claim 1 , wherein the concentration of the homogeneous solution is 0.5 g/mL; the temperature of the solvothermal reaction is 220° C. and the time is 1 h. 7.如权利要求1所述的低温制备方法,其特征在于,所述均质溶液的浓度为0.5g/mL;所述溶剂热反应的温度为200℃、时间为6h。7 . The low-temperature preparation method according to claim 1 , wherein the concentration of the homogeneous solution is 0.5 g/mL; the temperature of the solvothermal reaction is 200° C. and the time is 6 h.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0162137A2 (en) * 1984-05-21 1985-11-27 Toshiba Tungaloy Co. Ltd. Method for preparing boron nitride
EP0544570A1 (en) * 1991-11-28 1993-06-02 Elf Atochem S.A. Process for the preparation of boron nitride and the obtaind boron nitride
CN103395752A (en) * 2013-08-09 2013-11-20 哈尔滨工业大学(威海) Preparation method for boron nitride micron solid ball
CN106348262A (en) * 2016-11-24 2017-01-25 陕西聚洁瀚化工有限公司 Preparation method of BN (boron nitride)

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0162137A2 (en) * 1984-05-21 1985-11-27 Toshiba Tungaloy Co. Ltd. Method for preparing boron nitride
EP0544570A1 (en) * 1991-11-28 1993-06-02 Elf Atochem S.A. Process for the preparation of boron nitride and the obtaind boron nitride
CN103395752A (en) * 2013-08-09 2013-11-20 哈尔滨工业大学(威海) Preparation method for boron nitride micron solid ball
CN106348262A (en) * 2016-11-24 2017-01-25 陕西聚洁瀚化工有限公司 Preparation method of BN (boron nitride)

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