WO2023197682A1 - 一种高效制备氮化硼纳米片的方法 - Google Patents

一种高效制备氮化硼纳米片的方法 Download PDF

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WO2023197682A1
WO2023197682A1 PCT/CN2022/142028 CN2022142028W WO2023197682A1 WO 2023197682 A1 WO2023197682 A1 WO 2023197682A1 CN 2022142028 W CN2022142028 W CN 2022142028W WO 2023197682 A1 WO2023197682 A1 WO 2023197682A1
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boron nitride
nanosheets
nitride nanosheets
cleaning
reaction
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PCT/CN2022/142028
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French (fr)
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毕见强
梁关东
王绍印
殷壮壮
孙国勋
王伟礼
尚蒙蒙
梁延杰
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山东大学
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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
    • C01B21/0646—Preparation by pyrolysis of boron and nitrogen containing compounds
    • 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
    • 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
    • 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
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • 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

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  • the invention belongs to the technical field of inorganic non-metallic materials, and specifically relates to a preparation method of boron nitride nanosheets.
  • the purpose of the present invention is to provide an efficient preparation method of boron nitride nanosheets.
  • the present invention uses zinc borate nanosheets as the boron source, and at the same time, the zinc borate nanosheets are also used as the substrate template for the reaction, and ammonia gas is used as the nitrogen source to prepare boron nitride nanosheets through high-temperature nitridation reaction.
  • the boron element in the zinc borate nanosheets near the melting point continuously diffuses to the surface to react with ammonia gas, depositing a layer of boron nitride nanosheets on the surface of the zinc borate nanosheets, leaving zinc oxide in the inner layer, and then passes through Ultrasonic pickling with concentrated hydrochloric acid washes away the zinc oxide to obtain pure boron nitride nanosheets.
  • the above preparation method has the advantages of stability, reliability, simple operation, low equipment cost, easy availability of raw materials, and high yield.
  • the first aspect of the present invention provides a method for preparing boron nitride nanosheets.
  • the preparation method includes using zinc borate nanosheets as a boron source and performing a high-temperature heating reaction in an ammonia atmosphere to obtain the nitride. Boron nanosheets.
  • zinc borate nanosheets serve as a model agent and boron source at the same time, providing a sheet template for the deposition of boron nitride.
  • the present invention provides a preparation method of zinc borate nanosheets, which is prepared by heating zinc nitrate and sodium borate. The preparation method is as follows: respectively heating the aqueous solutions of zinc nitrate and sodium borate to 65-75°C, and mixing the two solutions. Prepared by heating in a water bath at 65-75°C for 18-24 hours.
  • the concentration of the zinc nitrate solution is 0.1-0.3 mol/L.
  • the concentration of the sodium borate solution is 0.05-0.15 mol/L.
  • the reaction product is washed and dried to obtain the zinc borate nanosheets.
  • the drying temperature is 55-65°C and the drying time is 8-12 hours.
  • the specific method for high-temperature heating of the boron source and ammonia is as follows: place the boron source in a tube furnace, introduce ammonia gas to perform a high-temperature reaction, the reaction temperature is 800-1100°C, and the heating rate is 8-1100°C. 12°C/min, holding time is 2 ⁇ 4h.
  • the flow rate of the ammonia gas is 65-75 sccm; further, it is 68-72 sccm, and a specific example is 71.9 sccm.
  • the steps of cleaning and drying the product are also included; the cleaning is carried out with an acid solution, and the acid solution is hydrochloric acid, nitric acid or sulfuric acid solution.
  • the pickling uses a hydrochloric acid solution for ultrasonic cleaning, the hydrochloric acid concentration is 2 to 5 mol/L, and the ultrasonic cleaning time is 3 to 5 hours.
  • the above-mentioned ultrasonic cleaning also includes a water washing step.
  • the water washing uses deionized water for centrifugal cleaning.
  • the number of cleaning times can be adjusted according to the cleaning effect, such as 3 to 5 times.
  • the thickness of boron nitride nanosheets prepared by the above method is between 5-14nm, and the lateral size can be controlled from nanometer to micrometer, which has the advantage of being mass-produced; in addition, the single-time output of the above preparation method can reach At the gram level, the size of zinc borate nanosheets can be controlled by controlling the reaction time of the precursor; in addition, the size and thickness of boron nitride nanosheets can be controlled by controlling parameters such as the temperature and reaction time of ammonia nitridation.
  • the boron nitride nanosheets can be controlled by controlling the lateral size of the zinc borate nanosheets. size; in addition, the quality and thickness of boron nitride nanosheets are also closely related to the temperature, time and other parameters of the ammonia nitridation reaction, so the quality and thickness of the prepared boron nitride nanosheets can be further controlled by adjusting the ammonia nitridation parameters. thickness.
  • the preparation method of boron nitride nanosheets provided by the present invention can realize the preparation of boron nitride nanosheets in large quantities. Compared with mechanical stripping, vapor deposition and other methods, it significantly improves the yield of a single reaction and effectively meets the needs of boron nitride nanosheets. practical application.
  • the raw materials used in the above preparation method are easy to obtain and low in cost, and the production equipment is relatively simple and easy to operate, making it easy to realize industrial scale-up production.
  • the present invention uses thinner zinc borate nanosheets as the boron source and base template to realize the controllable preparation of boron nitride nanosheets with lateral dimensions from nanometer to micrometer, and can nitride the nanosheets according to the purpose of use. The lateral dimensions of boron nanosheets are adjusted.
  • Figure 1 is a scanning electron microscope photo of the flaky zinc borate precursor nanosheets prepared by the water bath reaction for 24 hours in Examples 1 to 3 of the present invention and the water bath reaction for 18 hours in Example 4. It can be clearly seen that the size of the zinc borate nanosheets is smaller after the reaction for 18 hours. Much smaller than the zinc borate nanosheets that reacted for 24 h;
  • Figure 1A shows the preparation of precursor nanosheets after 24 hours of reaction, with a magnification of 20,000 times;
  • Figure 1B shows the preparation of precursor nanosheets after 18 hours of reaction, with a magnification of 20,000 times
  • Figure 2 is a scanning electron microscope photograph of boron nitride nanosheets prepared in Examples 1 to 4 of the present invention. From Figures 2A, 2B and 2C of Examples 1 to 3, it can be seen that the ammonia nitriding temperature increases from 800°C At 1000°C, the surface of the boron nitride nanosheets prepared becomes smooth and the size also increases.
  • the boron nitride nanosheets prepared at 800°C have a lower reaction temperature and the boron source diffuses slowly during the reaction, resulting in the prepared nitrogen There are many crumb-like nanosheets in the boron nitride nanosheets, and the quality is poor; while the boron nitride nanosheets prepared at 900°C and 1000°C are of better quality, with smooth surfaces and lateral dimensions in the micron range; Figure 2D can be seen in the water bath reaction After nitriding zinc borate nanosheets as a boron source at 900°C for 18 hours, the lateral size of the boron nitride nanosheets obtained is very small, and the size is nanoscale.
  • magnification of Figures 2A, 2B, and 2C is 10,000 times;
  • Figure 3 is a magnified scanning electron microscope image of a single boron nitride nanosheet prepared in Example 2 of the present invention
  • magnification is 30,000 times.
  • Figure 4 is an AFM spectrum of boron nitride nanosheets prepared in Example 3 of the present invention.
  • Figure 5 is an XRD pattern of boron nitride nanosheets prepared in Examples 1 to 3 of the present invention.
  • the mixed powder obtained from the zinc borate nanosheets is reacted with ammonia gas at a high temperature in a tube furnace.
  • the heating rate is 10°C/min
  • the reaction temperature is 900°C
  • the holding time is 3h.
  • the ammonia gas The flow rate is 71.9sccm;
  • the mixed powder obtained from the zinc borate nanosheets is reacted with ammonia gas at a high temperature in a tube furnace.
  • the heating rate is 10°C/min
  • the reaction temperature is 1000°C
  • the holding time is 3h.
  • the ammonia gas The flow rate is 71.9sccm;
  • the mixed powder obtained from the zinc borate nanosheets is reacted with ammonia gas at a high temperature in a tube furnace.
  • the heating rate is 10°C/min
  • the reaction temperature is 900°C
  • the holding time is 3h.
  • the ammonia gas The flow rate is 71.9sccm;

Abstract

本发明涉及一种氮化硼纳米片的制备方法，属于无机非金属材料技术领域。本发明首先合成纳米片状的硼酸锌为前驱体硼源以及基底模版，氨气做为氮源，在较低温度下制备了形貌良好，具有微米级横向尺寸的氮化硼纳米片；同时，因为纳米片状的硼酸锌前驱体采用一步沉淀法制备，产量大，操作简单，使得此方法制备氮化硼纳米片具有尺寸可调、产量大、可量产的优势，为氮化硼纳米片的大量应用提供了基础。

Description

一种高效制备氮化硼纳米片的方法
本发明要求于2022年4月11日提交中国专利局、申请号为202210374129.3、发明名称为“一种高效制备氮化硼纳米片的方法”的中国专利申请的优先权，其全部内容通过引用结合在本发明中。
技术领域
本发明属于无机非金属材料技术领域，具体涉及一种氮化硼纳米片的制备方法。
背景技术
该背景技术部分公开内容并不必然被视为现有技术。
2004年，Geim和Novoselov制备出了稳定存在的石墨烯(graphene)材料，并证明了石墨烯具有独特而又优异的性质，由此科学界掀起了石墨烯材料的研究热潮。随着研究的不断深入，与其具有相似结构的其它二维层状材料不断增多，氮化硼纳米片由于在石墨烯类似优异性能的基础上，具有其独特的电绝缘和抗高温氧化性质，引起了广泛的关注。
目前，人们对于氮化硼纳米片的相关性质已经有了比较深入的了解，并且采用了各种方法制备出了氮化硼纳米片，对于氮化硼纳米片的应用也有了进一步的研究。但是，由于现有的制备方法主要通过“自上而下”的剥离六方氮化硼获得氮化硼纳米片。但由于六方氮化硼层间结合力相对石墨较强，难以被剥离，导致产量较低。若使用非常强的机械力剥离六方氮化硼，虽然产量得到了提高，不可避免的导致所制备的氮化硼纳米片的质量大打折扣，存在较多的晶体缺陷，对氮化 硼纳米片后期的应用产生限制。其他制备方法，例如现阶段“自下而上”的化学气相沉积法制备出的氮化硼纳米片同样存在产量低、价格较高的问题，这也限制了氮化硼纳米片在很多领域的进一步应用。因此，开发一种更加高效稳定的制备氮化硼纳米片的工艺方法，仍是本领域研究的重点和难点。
发明内容
基于上述技术背景，本发明目的在于提供一种氮化硼纳米片的高效制备方法。为了实现上述技术目的，本发明以硼酸锌纳米片为硼源，同时硼酸锌纳米片也做为反应的基底模版，氨气做为氮源，通过高温氮化反应，制备氮化硼纳米片。反应过程中处于熔点温度附近的硼酸锌纳米片中的硼元素不断向表面扩散与氨气进行反应，在硼酸锌纳米片表面沉积一层氮化硼纳米片，内层留下氧化锌，然后通过浓盐酸超声酸洗将氧化锌洗掉，得到纯的氮化硼纳米片。上述方式制备方法具有稳定可靠、操作简单、设备成本较低、原料易得、可产量的优势。
基于上述技术效果，本发明第一方面，提供一种氮化硼纳米片的制备方法，所述制备方法包括以硼酸锌纳米片作为硼源，在氨气氛围下高温加热反应得到所述氮化硼纳米片。
上述制备方法中，硼酸锌纳米片同时充当模型剂及硼源，为了氮化硼的沉积提供片状模板。本发明进一步的，提供了一种硼酸锌纳米片的制备方式，采用硝酸锌及硼酸钠加热制备，制备方式如下：分别加热硝酸锌及硼酸钠的水溶液至65～75℃，将两溶液混合后在65～75℃水浴加热18～24h制备得到。
进一步的，所述硝酸锌溶液的浓度为0.1～0.3mol/L。
进一步的，所述硼酸钠溶液的浓度为0.05～0.15mol/L。
上述水浴反应结束后，将反应产物清洗并干燥得到所述硼酸锌纳米片，所述干燥温度55～65℃，干燥时间为8～12h。
优选的，所述硼源与氨气高温加热的具体方式如下：将硼源置于管式炉中，通入氨气进行高温反应，所述反应温度为800～1100℃，升温速率为8～12℃/min，保温时间为2～4h。
进一步的，所述氨气的流量为65～75sccm；更进一步的，为68～72sccm，具体的实例如71.9sccm。
优选的，所述高温加热完成后还包括对产物进行清洗、干燥的步骤；所述清洗采用酸液进行清洗，所述酸液为盐酸、硝酸或硫酸溶液。
进一步的，所述酸洗采用盐酸溶液进行超声清洗，所述盐酸浓度为2～5mol/L，所述超声清洗的时间为3～5h。
上述超声清洗后还包括水洗步骤，所述水洗采用去离子水进行离心清洗，清洗次数可以依据清洗的效果进行调整，如3～5次，清洗完成后在55～65℃下干燥8～12h得到所述氮化硼纳米片。
经验证，上述方式制备的氮化硼纳米片厚度为5-14nm之间，横向尺寸可实现纳米级到微米级的调控制备，具有可量产的优势；另外，上述制备方法单次产量可达克级，可通过控制前驱体的反应时间来控制硼酸锌纳米片的大小；另外，可控制氨气氮化的温度、反应时间等参数的方式对氮化硼纳米片的尺寸、厚度进行调控。经实施例验证，硼酸锌纳米片的尺寸随水浴反应时间的延长逐渐增大，又因为硼酸锌纳米片作为基底模版，所以可以通过控制硼酸锌纳米 片的横向尺寸来控制氮化硼纳米片的尺寸；另外，氮化硼纳米片的质量和厚度也与氨气氮化反应的温度、时间等参数息息相关，所以可通过调控氨气氮化参数进一步调控所制备的氮化硼纳米片的质量和厚度。
以上一个或多个技术方案的有益效果是：
1、本发明提供的氮化硼纳米片制备方法，能够实现氮化硼纳米片的大量制备，相比机械剥离、气相沉积等方式显著提高了单次反应的产量，有效满足氮化硼纳米片的实际应用。
2、上述制备方法中所采用的原料易得、成本低，并且生产设备相对简单，操作方便，容易实现工业上的扩大化生产。
3、另外，本发明以厚度较薄的硼酸锌纳米片做为硼源和基底模版，实现了纳米级到微米级横向尺寸的氮化硼纳米片的可控制备，可依据使用目的对氮化硼纳米片的横向尺寸进行调整。
附图说明
构成本发明的一部分的说明书附图用来提供对本发明的进一步理解，本发明的示意性实施例及其说明用于解释本发明，并不构成对本发明的不当限定。
图1为本发明实施例1～3中水域反应24h和实施例4水浴反应18h所制备的片状硼酸锌前驱体纳米片的扫描电镜照片，可以明显看出反应18h硼酸锌纳米片的尺寸要远小于反应24h的硼酸锌纳米片；
其中，图1A为反应24h制备前驱体纳米片，其放大倍数为20000倍；
图1B为反应18h制备前驱体纳米片，其放大倍数为20000倍；
图2为本发明实施例1～4制备的氮化硼纳米片的扫描电镜照片，从实施例1～3的图2A、2B、2C中可以看出随氨气氮化温度从800℃升高到1000℃，所制备的氮化硼纳米片表面趋于光滑，尺寸也有所增加；其中800℃的氮化硼纳米片因为反应温度较低，反应过程中硼源扩散较慢，导致制备的氮化硼纳米片存在许多碎屑状纳米片，质量较差；而900℃和1000℃制备的氮化硼纳米片质量较好，表面光滑，横向尺寸在微米级；图2D可以看出以水浴反应18h的硼酸锌纳米片作为硼源900℃氮化后，获得的氮化硼纳米片横向尺寸非常小，尺寸为纳米级。
其中，图2A、2B、2C的放大倍数为10000倍；
图2D放大倍数为25000倍。
图3为本发明实施例2制备的氮化硼纳米片的单片扫描电镜放大图像；
其中，放大倍数为30000倍。
图4为本发明实施例3制备的氮化硼纳米片的AFM图谱。
图5为本发明实施例1～3制备的氮化硼纳米片的XRD图谱。
具体实施方式
应该指出，以下详细说明都是例示性的，旨在对本发明提供进一步的说明。除非另有指明，本文使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。
需要注意的是，这里所使用的术语仅是为了描述具体实施方式， 而非意图限制根据本发明的示例性实施方式。如在这里所使用的，除非上下文另外明确指出，否则单数形式也意图包括复数形式，此外，还应当理解的是，当在本说明书中使用术语“包含”和/或“包括”时，其指明存在特征、步骤、操作、器件、组件和/或它们的组合。
为了使得本领域技术人员能够更加清楚地了解本发明的技术方案，以下将结合具体的实施例详细说明本发明的技术方案。
实施例1：
(1)称取0.02mol六水合硝酸锌和0.01mol十水合硼酸钠分别加入到两个装有100mL去离子水的烧杯中，在恒温搅拌水浴锅中搅拌30分钟，并加热到70℃，至六水合硝酸锌和十水合硼酸钠完全溶解；
(2)将上述六水合硝酸锌溶液匀速倒入搅拌的十水合硼酸钠溶液中，70℃下反应24h；
(3)将水浴反应后的产物离心清洗3次后60℃干燥10h以上，收集获得硼酸锌纳米片；
(4)将得到的硼酸锌纳米片在管式炉中与氨气进行高温反应，升温速率为10℃/min，反应温度为800℃，保温时间为3h，反应过程中氨气的流量为71.9sccm；
(5)将高温反应后产物加入到浓度为2mol/L的盐酸溶液中超声酸洗4h；
(6)将超声酸洗后的悬浊液使用去离子水离心清洗3次后60℃干燥10h以上，收集得到氮化硼纳米片。
实施例2：
(1)称取0.02mol六水合硝酸锌和0.01mol十水合硼酸钠分别加入到两个装有100mL去离子水的烧杯中，在恒温搅拌水浴锅中搅拌30分钟，并加热到70℃，至六水合硝酸锌和十水合硼酸钠完全溶解；
(2)将上述六水合硝酸锌溶液匀速倒入搅拌的十水合硼酸钠溶液中，70℃下反应24h；
(3)将水浴反应后的产物离心清洗3次后60℃干燥10h以上，收集获得硼酸锌纳米片；
(4)将得到的硼酸锌纳米片得到的混合粉末在管式炉中与氨气进行高温反应，升温速率为10℃/min，反应温度为900℃，保温时间为3h，反应过程中氨气的流量为71.9sccm；
(5)将高温反应后产物加入到浓度为2mol/L的盐酸溶液中超声酸洗4h；
(6)将超声酸洗后的悬浊液使用去离子水离心清洗3次后60℃干燥10h以上，收集得到氮化硼纳米片。
实施例3：
(1)称取0.02mol六水合硝酸锌和0.01mol十水合硼酸钠分别加入到两个装有100mL去离子水的烧杯中，在恒温搅拌水浴锅中搅拌30分钟，并加热到70℃，至六水合硝酸锌和十水合硼酸钠完全溶解；
(2)将上述六水合硝酸锌溶液匀速倒入搅拌的十水合硼酸钠溶液中，70℃下反应24h；
(3)将水浴反应后的产物离心清洗3次后60℃干燥10h以上，收集获得硼酸锌纳米片；
(4)将得到的硼酸锌纳米片得到的混合粉末在管式炉中与氨气进行高温反应，升温速率为10℃/min，反应温度为1000℃，保温时间为3h，反应过程中氨气的流量为71.9sccm；
(5)将高温反应后产物加入到浓度为2mol/L的盐酸溶液中超声酸洗4h；
(6)将超声酸洗后的悬浊液使用去离子水离心清洗3次后60℃干燥10h以上，收集得到氮化硼纳米片。
实施例4：
(1)称取0.02mol六水合硝酸锌和0.01mol十水合硼酸钠分别加入到两个装有100mL去离子水的烧杯中，在恒温搅拌水浴锅中搅拌30分钟，并加热到70℃，至六水合硝酸锌和十水合硼酸钠完全溶解；
(2)将上述六水合硝酸锌溶液匀速倒入搅拌的十水合硼酸钠溶液中，70℃下反应18h；
(3)将水浴反应后的产物离心清洗3次后60℃干燥10h以上，收集获得硼酸锌纳米片；
(4)将得到的硼酸锌纳米片得到的混合粉末在管式炉中与氨气进行高温反应，升温速率为10℃/min，反应温度为900℃，保温时间为3h，反应过程中氨气的流量为71.9sccm；
(5)将高温反应后产物加入到浓度为2mol/L的盐酸溶液中超声酸洗4h；
(6)将超声酸洗后的悬浊液使用去离子水离心清洗3次后60℃干燥10h以上，收集得到氮化硼纳米片。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

  1. 一种氮化硼纳米片的制备方法，其特征在于，所述制备方法以硼酸锌纳米片作为硼源，在氨气氛围下高温加热得到所述氮化硼纳米片。
  2. 如权利要求1所述氮化硼纳米片的制备方法，其特征在于，所述硼酸锌纳米片的制备方式如下：分别加热硝酸锌及硼酸钠的水溶液至65～75℃，将两溶液混合后在65～75℃水浴加热18～24h制备得到。
  3. 如权利要求2所述氮化硼纳米片的制备方法，其特征在于，所述硝酸锌溶液的浓度为0.1～0.3mol/L；
    或，所述硼酸钠溶液的浓度为0.05～0.15mol/L。
  4. 如权利要求2所述氮化硼纳米片的制备方法，其特征在于，所述水浴反应结束后，将反应产物清洗并干燥得到所述硼酸锌纳米片，所述干燥温度55～65℃，干燥时间为8～12h。
  5. 如权利要求1所述氮化硼纳米片的制备方法，其特征在于，所述硼源为不同反应条件下所制备的硼酸锌纳米片，硼酸锌纳米片同时作为制备氮化硼纳米片的基底模版。
  6. 如权利要求1所述氮化硼纳米片的制备方法，其特征在于，所述硼源与氨气高温加热的具体方式如下：将硼源置于管式炉中，通入氨气进行高温反应，所述反应温度为800～1100℃，升温速率为8～12℃/min，保温时间为2～4h。
  7. 如权利要求6所述氮化硼纳米片的制备方法，其特征在于，所述氨气的流量为70～140sccm；进一步的，为70～72sccm，具体的，为71.9sccm。
  8. 如权利要求6所述氮化硼纳米片的制备方法，其特征在于，所述高温加热完成后还包括对产物进行清洗、干燥的步骤；所述清洗采用酸液进行清洗，所述酸液为盐酸、硝酸或硫酸溶液。
  9. 如权利要求8所述氮化硼纳米片的制备方法，其特征在于，所述酸洗采用盐酸溶液进行超声清洗，所述盐酸浓度为1.5～2.5mol/L，所述超声清洗的时间为3～5h。
  10. 如权利要求9所述氮化硼纳米片的制备方法，其特征在于，所述超声清洗后还包括水洗步骤，所述水洗采用去离子水进行离心清洗，清洗次数可以依据清洗的效果进行调整，如3～5次，清洗完成后在60～80℃下干燥8～12h得到所述氮化硼纳米片。
PCT/CN2022/142028 2022-04-11 2022-12-26 一种高效制备氮化硼纳米片的方法 WO2023197682A1 (zh)

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