CN100999412A - Sialon quasi monodimension nanometer material and its preparation method - Google Patents
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- 239000000843 powder Substances 0.000 claims abstract description 44
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
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- 241000209456 Plumbago Species 0.000 claims 9
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims 9
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 9
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- 229910002804 graphite Inorganic materials 0.000 abstract description 30
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract description 23
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Abstract
本发明涉及一种Sialon准一维纳米材料，它的原料由以下组分按照重量百分比组成：含氢硅油37％～55％、乙二胺43％～60％，Al粉2％～10％；其制备方法包括以下步骤：a.按照重量百分比取含氢硅油、乙二胺、Al粉，混合，在反应釜中进行反应，反应温度控制在0～100℃的条件下不断搅拌8～12小时，反应形成Si－Al－O－N－C聚合物；b.将上一步骤所得产物置于石墨坩埚中，石墨坩埚放入气氛压力烧结炉中，通入氮气，炉内氮气压力控制在0.5～1.5MPa，控制温度在1200～1500℃的条件下保温2～3小时，在石墨坩埚中结晶形成Sialon准一维纳米材料。其介电性能优异，机械强度高，耐高温性能和导热性好，制备工艺简单、制作成本低，产率高，结晶均匀性好。The invention relates to a Sialon quasi-one-dimensional nanomaterial. Its raw materials are composed of the following components according to weight percentage: 37%-55% of hydrogen-containing silicone oil, 43%-60% of ethylenediamine, and 2%-10% of Al powder; Its preparation method includes the following steps: a. Take hydrogen-containing silicone oil, ethylenediamine, and Al powder according to the weight percentage, mix them, and carry out the reaction in a reaction kettle. The reaction temperature is controlled at 0-100 ° C and continuously stirred for 8-12 hours , react to form Si-Al-O-N-C polymer; b. Place the product obtained in the previous step in a graphite crucible, put the graphite crucible into an atmosphere pressure sintering furnace, feed nitrogen, and control the nitrogen pressure in the furnace at 0.5 ～1.5MPa, control the temperature at 1200～1500°C for 2～3 hours, and crystallize in a graphite crucible to form a Sialon quasi-one-dimensional nanomaterial. It has excellent dielectric properties, high mechanical strength, high temperature resistance and thermal conductivity, simple preparation process, low production cost, high yield and good crystallization uniformity.
Description
技术领域technical field
本发明涉及一种纳米材料及其制备方法，具体地说是一种Sialon准一维纳米材料及其制备方法。The invention relates to a nano material and a preparation method thereof, in particular to a Sialon quasi-one-dimensional nano material and a preparation method thereof.
背景技术Background technique
纳米科学技术被认为是21世纪头等重要的科学技术。纳米科学与技术将改变几乎每一种人造物质的特性，材料性能的重大改进以及制造方式重大变化，将在新世纪引起一场新的工业革命。1991年Iijima发现了纳米碳管，其独特的结构特性与理化性能在世界范围内掀起了研究热潮。之后，人们制备出了MoS2、WS2、BN、GaN纳米管和Si、Ag、CdTe、GaN纳米线等新的一维纳米材料，发展了一系列新的一维纳米材料的制备方法。由于一维纳米材料具有特殊的传输特性，光学特性以及表面效应，使得一维纳米材料在场效应晶体管、单电子晶体管、二极管、场发射、逻辑电路、激光器、传感器方面有广泛的应用。一维纳米材料可以根据其空心或实心以及形貌不同可以分为以下几类：纳米管、纳米棒或纳米线、纳米带、纳米同轴电缆以及纳米核壳结构。Nanotechnology is considered to be the most important science and technology in the 21st century. Nanoscience and technology will change the properties of almost every man-made substance, and major improvements in material performance and major changes in manufacturing methods will cause a new industrial revolution in the new century. In 1991, Iijima discovered carbon nanotubes, and its unique structural characteristics and physical and chemical properties set off a research boom around the world. Afterwards, new one-dimensional nanomaterials such as MoS 2 , WS 2 , BN, GaN nanotubes and Si, Ag, CdTe, GaN nanowires were prepared, and a series of new preparation methods for one-dimensional nanomaterials were developed. Due to the special transmission characteristics, optical properties and surface effects of one-dimensional nanomaterials, one-dimensional nanomaterials are widely used in field-effect transistors, single-electron transistors, diodes, field emission, logic circuits, lasers, and sensors. One-dimensional nanomaterials can be divided into the following categories according to their hollow or solid shape and different shapes: nanotubes, nanorods or nanowires, nanobelts, nanocoaxial cables, and nanocore-shell structures.
我们知道Sialon陶瓷材料具有高强、高硬、高韧性、耐磨损、耐腐蚀、抗氧化、抗热震、低热膨胀、自润滑、导热性好、电绝缘等一系列优良性能，在航空、航天、电子、冶金、机械、石油、化工、能源、交通、电器等领域获得了广泛的应用，是一类重要的结构材料、高温材料和介电绝缘材料。目前与Sialon结构类似的准一维氮化硅纳米材料的合成方法主要有：(1)碳纳米管限域生长法：以碳纳米管为膜板，以硅的氧化物或卤化物为硅源，在大量的氮化气氛中合成Si3N4纳米线，此方法需要先合成碳纳米管，工艺较复杂；(2)电弧放电法、激光烧蚀法：以电弧放电或激光烧蚀技术在高温下合成Si3N4纳米线，此方法的不足是产率低，杂质较多；(3)化学气相沉积(CVD)法：此法一般是以硅粉、氧化硅粉或含硅卤素在高温或等离子体环境中形成硅蒸汽与氮化气氛发生反应，在一定的冷却基板通过杂质形核按VLS机制生长氮化硅纳米材料，此法产率较低，也存在一定的杂质；(4)水热合成法；(5)碳热还原法。此外，还有中国专利2004100441585公布了一种用有机聚合物制备的Si-Al-O-N-C陶瓷材料及其制备方法。We know that Sialon ceramic materials have a series of excellent properties such as high strength, high hardness, high toughness, wear resistance, corrosion resistance, oxidation resistance, thermal shock resistance, low thermal expansion, self-lubrication, good thermal conductivity, and electrical insulation. It has been widely used in fields such as electronics, metallurgy, machinery, petroleum, chemical industry, energy, transportation, electrical appliances, etc. It is an important class of structural materials, high-temperature materials and dielectric insulation materials. At present, the synthesis methods of quasi-one-dimensional silicon nitride nanomaterials similar to Sialon structure mainly include: (1) carbon nanotube confinement growth method: carbon nanotubes are used as membrane plates, and silicon oxides or halides are used as silicon sources , synthesize Si 3 N 4 nanowires in a large amount of nitriding atmosphere. This method needs to synthesize carbon nanotubes first, and the process is more complicated; (2) arc discharge method and laser ablation method: arc discharge or laser ablation technology is used in Si 3 N 4 nanowires are synthesized at high temperature. The disadvantages of this method are low yield and more impurities; (3) chemical vapor deposition (CVD) method: this method is generally based on silicon powder, silicon oxide powder or silicon-containing halogen Silicon vapor formed in a high temperature or plasma environment reacts with the nitriding atmosphere, and silicon nitride nanomaterials are grown on a certain cooling substrate through the nucleation of impurities according to the VLS mechanism. This method has a low yield and certain impurities; (4 ) Hydrothermal synthesis method; (5) Carbothermal reduction method. In addition, Chinese patent 2004100441585 discloses a Si-Al-ONC ceramic material prepared from an organic polymer and a preparation method thereof.
发明内容Contents of the invention
本发明所要解决的技术问题是克服上述现有技术的不足，提供一种介电性能优异，机械强度高，耐高温性能和导热性好，制备工艺简单、制作成本低，产率高，结晶均匀性好的Sialon准一维纳米材料及其制备方法。The technical problem to be solved by the present invention is to overcome the deficiencies of the above-mentioned prior art, and to provide a product with excellent dielectric properties, high mechanical strength, high temperature resistance and thermal conductivity, simple preparation process, low production cost, high yield and uniform crystallization. A Sialon quasi-one-dimensional nanomaterial with good properties and a preparation method thereof.
本发明解决上述技术问题采用的技术方案是：The technical solution adopted by the present invention to solve the problems of the technologies described above is:
一种Sialon准一维纳米材料，其特征在于它的原料由以下组分按照重量百分比组成：含氢硅油37％～55％、乙二胺43％～60％，Al粉2％～10％；所述的Sialon准一维纳米材料制备方法包括以下步骤：a.按照重量百分比取含氢硅油37％～55％、乙二胺43％～60％，Al粉2％～10％，将含氢硅油、乙二胺和Al粉混合，在反应釜中进行反应，反应温度控制在0～100℃的条件下不断搅拌8～12小时，反应形成Si-Al-O-N-C聚合物；b.将上一步骤所得产物置于石墨坩埚中，石墨坩埚放入气氛压力烧结炉中，通入氮气，炉内氮气压力控制在0.5～1.5MPa，控制温度在1200～1500℃的条件下保温2～3小时，在石墨坩埚中结晶形成Sialon准一维纳米材料。A Sialon quasi-one-dimensional nanomaterial is characterized in that its raw materials are composed of the following components according to weight percentage: 37% to 55% of hydrogen-containing silicone oil, 43% to 60% of ethylenediamine, and 2% to 10% of Al powder; The preparation method of the described Sialon quasi-one-dimensional nanomaterial comprises the following steps: a. Take 37%-55% of hydrogen-containing silicone oil, 43%-60% of ethylenediamine, and 2%-10% of Al powder according to the weight percentage; Silicone oil, ethylenediamine and Al powder are mixed and reacted in a reactor. The reaction temperature is controlled at 0-100°C and stirred continuously for 8-12 hours to form a Si-Al-O-N-C polymer; b. The product obtained in the step is placed in a graphite crucible, the graphite crucible is placed in an atmosphere pressure sintering furnace, nitrogen gas is introduced, the nitrogen pressure in the furnace is controlled at 0.5-1.5 MPa, and the temperature is controlled at 1200-1500 ° C for 2-3 hours. Crystallization in graphite crucibles to form Sialon quasi-one-dimensional nanomaterials.
本发明Sialon准一维纳米材料的制备方法，其特征在于在步骤a、b之间还包括a`步骤：其将a步骤所得产物在管式气氛保护炉中，在温度200～1000℃之间，通入氮气，氮气流量200～400ml/min，升温速率控制在1～10℃/min的条件下反应8～12小时，对Si-Al-O-N-C有机聚合物进行裂解，得到Si-Al-O-N-C粉末。The preparation method of the Sialon quasi-one-dimensional nanomaterial of the present invention is characterized in that it also includes a step between steps a and b: it puts the product obtained in step a in a tubular atmosphere protection furnace at a temperature between 200 and 1000 ° C. , feed nitrogen, the nitrogen flow rate is 200-400ml/min, and the heating rate is controlled at 1-10°C/min to react for 8-12 hours to crack the Si-Al-O-N-C organic polymer to obtain Si-Al-O-N-C powder.
本发明Sialon准一维纳米材料包括Sialon纳米线和Sialon纳米带。Sialon纳米线直径在50～150nm，长度达数百μm，Sialon纳米带宽度在50～500nm，厚度在10～100nm，长度达数百μm，为100～1000μm。本发明使用聚合物制备Sialon准一维纳米材料介电性能优异，机械强度高，耐高温性能和导热性好，制备工艺简单、制作成本低，产率高，结晶均匀性好The Sialon quasi-one-dimensional nanometer material of the present invention includes Sialon nanowires and Sialon nanobelts. Sialon nanowires have a diameter of 50-150nm and a length of hundreds of μm; Sialon nanoribbons have a width of 50-500nm, a thickness of 10-100nm, and a length of hundreds of μm, which is 100-1000μm. The invention uses the polymer to prepare the Sialon quasi-one-dimensional nanomaterial with excellent dielectric properties, high mechanical strength, good high temperature resistance and thermal conductivity, simple preparation process, low production cost, high yield and good crystallization uniformity
本发明的特点是：其一，本方法引入了使用含有还原性胺基的先驱体粉末在高压反应炉中制备纳米材料这一关键环节；其二，该工艺不使用催化剂，可大量制备纯净纳米材料，原材料使用工业用含氢硅油、乙二胺和铝粉，成本低；其三，可以通过控制反应温度、反应时间和气体分压来实现纳米材料的成分、尺寸和结构的调控。其应用廉价的有机含氢硅油聚合物先驱体在气氛气压烧结炉中制备。The characteristics of the present invention are: firstly, the method introduces the key step of preparing nanomaterials in a high-pressure reaction furnace using precursor powders containing reducing amine groups; secondly, the process does not use catalysts and can prepare a large amount of pure nano Materials, raw materials use industrial hydrogen-containing silicone oil, ethylenediamine and aluminum powder, and the cost is low; third, the composition, size and structure of nanomaterials can be adjusted by controlling the reaction temperature, reaction time and gas partial pressure. It uses cheap organic hydrogen-containing silicone oil polymer precursors to prepare in an atmosphere pressure sintering furnace.
本发明Sialon准一维纳米材料介电性能优异，机械强度高，耐高温性能和导热性好，制备工艺简单、制作成本低，产率高，结晶均匀性好。The Sialon quasi-one-dimensional nanometer material of the invention has excellent dielectric properties, high mechanical strength, good high temperature resistance and thermal conductivity, simple preparation process, low production cost, high yield and good crystallization uniformity.
附图说明Description of drawings
下面结合实施例对本发明做进一步说明。The present invention will be further described below in conjunction with embodiment.
本发明一种Sialon准一维纳米材料，它的原料由以下组分按照重量百分比组成：含氢硅油37％～55％、乙二胺43％～60％，Al粉2％～10％。The invention discloses a Sialon quasi-one-dimensional nanometer material. Its raw materials are composed of the following components according to weight percentage: 37%-55% of hydrogen-containing silicone oil, 43%-60% of ethylenediamine, and 2%-10% of Al powder.
上述Sialon准一维纳米材料制备方法包括以下步骤：a.按照重量百分比取含氢硅油37％～55％、乙二胺43％～60％，Al粉2％～10％，将含氢硅油、乙二胺和Al粉混合，在反应釜中进行反应，反应温度控制在0～100℃的条件下不断搅拌8～12小时，反应形成Si-Al-O-N-C聚合物；b.将上一步骤所得产物置于石墨坩埚中，石墨坩埚放入气氛压力烧结炉中，通入氮气，炉内氮气压力控制在0.5～1.5MPa，控制温度在1200～1500℃的条件下保温2～3小时，在石墨坩埚中结晶形成Sialon准一维纳米材料。The preparation method of the above-mentioned Sialon quasi-one-dimensional nanomaterial comprises the following steps: a. Take 37% to 55% of hydrogen-containing silicone oil, 43% to 60% of ethylenediamine, and 2% to 10% of Al powder according to weight percentage, and mix hydrogen-containing silicone oil, Ethylenediamine and Al powder are mixed and reacted in a reactor. The reaction temperature is controlled at 0-100°C and continuously stirred for 8-12 hours to form a Si-Al-O-N-C polymer; b. The product is placed in a graphite crucible, the graphite crucible is placed in an atmosphere pressure sintering furnace, nitrogen is introduced, the nitrogen pressure in the furnace is controlled at 0.5-1.5MPa, and the temperature is controlled at 1200-1500°C for 2-3 hours. Sialon quasi-one-dimensional nanomaterials are formed by crystallization in a crucible.
或上述Sialon准一维纳米材料制备方法包括以下步骤：a.按照重量百分比取含氢硅油37％～55％、乙二胺43％～60％，Al粉2％～10％，将含氢硅油、乙二胺和Al粉混合，在反应釜中进行反应，反应温度控制在0～100℃的条件下不断搅拌8～12小时，反应形成Si-Al-O-N-C聚合物；a.将聚合物在管式气氛保护炉中，在温度200～1000℃之间，通入氮气，氮气流量200～400ml/min，升温速率控制在1～10℃/min的条件下反应8～12小时，对Si-Al-O-N-C有机聚合物进行裂解，得到Si-Al-O-N-C粉末；b.所制备的Si-Al-O-N-C粉末置于石墨坩埚中，石墨坩埚放入气氛气压烧结炉中，通入氮气，炉内氮气压力控制在0.5～1.5MPa，控制温度在1200～1500℃的条件下保温2～3小时，在石墨坩埚中结晶形成Sialon准一维纳米结构。Or the preparation method of the above-mentioned Sialon quasi-one-dimensional nanomaterial comprises the following steps: a. Take 37% to 55% of hydrogen-containing silicone oil, 43% to 60% of ethylenediamine, and 2% to 10% of Al powder according to the percentage by weight; , ethylenediamine and Al powder are mixed, reacted in a reactor, and the reaction temperature is controlled at 0-100 ° C and continuously stirred for 8-12 hours to form a Si-Al-O-N-C polymer; a. In the tube-type atmosphere protection furnace, the temperature is between 200-1000 °C, nitrogen gas is introduced, the nitrogen flow rate is 200-400ml/min, and the heating rate is controlled at 1-10 °C/min for 8-12 hours. The Al-O-N-C organic polymer is cracked to obtain Si-Al-O-N-C powder; b. The prepared Si-Al-O-N-C powder is placed in a graphite crucible, and the graphite crucible is placed in an atmosphere pressure sintering furnace, and nitrogen is introduced into the furnace. The nitrogen pressure is controlled at 0.5-1.5MPa, the temperature is controlled at 1200-1500°C for 2-3 hours, and the Sialon quasi-one-dimensional nanostructure is formed by crystallization in a graphite crucible.
实施例1：Example 1:
Sialon准一维纳米材料，它的原料由以下组分按照重量百分比组成：含氢硅油55％、乙二胺43％，Al粉2％。Sialon准一维纳米材料的制备方法，a.将含氢硅油198ml、乙二胺155ml和Al粉6克混合，在反应釜中进行反应，反应温度控制在0～100℃，使用溶剂为四氢呋喃500ml和正己烷250ml，在常温下不断搅拌8～12小时，反应形成Si-Al-O-N-C聚合物；a.将聚合物在管式气氛保护炉中对Si-Al-O-N-C有机聚合物进行裂解，通入氮气，氮气流量为200～400ml/min，温度工艺为在室温～750℃的温度范围内，升温速度为5℃/min，在750℃保温1小时，在750～1000℃的温度范围内，升温速度为5℃/min，在1000℃保温1小时，得到Si-Al-O-N-C粉末；b.将所制备的Si-Al-O-N-C粉末置于石墨坩埚中，石墨坩埚放入气氛压力压烧结炉中，通入氮气压力为1.2Mpa，控制温度在1400℃的条件下保温2小时，在石墨坩埚中结晶形成厚度为40nm.，宽度为200nm，长数百μm的Sialon纳米带。The Sialon quasi-one-dimensional nanomaterial is composed of the following components according to weight percentage: 55% hydrogen-containing silicone oil, 43% ethylenediamine, and 2% Al powder. The preparation method of Sialon quasi-one-dimensional nanomaterials, a. Mix 198ml of hydrogen-containing silicone oil, 155ml of ethylenediamine and 6 grams of Al powder, and react in a reaction kettle. The reaction temperature is controlled at 0-100°C, and the solvent used is 500ml of tetrahydrofuran. and n-hexane 250ml, stirring continuously at room temperature for 8 to 12 hours, reacting to form Si-Al-O-N-C polymer; Inject nitrogen, the nitrogen flow rate is 200-400ml/min, the temperature process is within the temperature range of room temperature to 750°C, the heating rate is 5°C/min, and the temperature is kept at 750°C for 1 hour, and within the temperature range of 750-1000°C, The heating rate is 5°C/min, and the temperature is kept at 1000°C for 1 hour to obtain Si-Al-O-N-C powder; b. Put the prepared Si-Al-O-N-C powder in a graphite crucible, and put the graphite crucible into an atmosphere pressure sintering furnace In the process, the nitrogen pressure is 1.2Mpa, and the temperature is controlled at 1400°C for 2 hours. Sialon nanobelts with a thickness of 40nm., a width of 200nm, and a length of hundreds of μm are crystallized in a graphite crucible.
纳米带与其他的一维纳米材料结构上存在较大区别，其截面不同于纳米管和纳米线那样接近圆型，而是呈现窄长方形，其厚度可达几到几十纳米，宽度达几十到几百纳米，而长度可达几毫米。纳米带作为一种新颖的一维纳米结构，具有结晶完好、无缺陷等优点。导体纳米带是用于研究电子输运中限域效应的较好的模型，半导体纳米带可以作为纳米传感器的核心部分。Sialon纳米带具有其他纳米带不具备的独特性能和应用前景，比如非常高的机械强度和耐高温性能，可用于纳米复合材料增强方面；由于Sialon优异的介电性能、导热性和机械强度Sialon纳米带可用于构筑单纳米电子器件的电路基板及其电介质，以及用于超级电容器的绝缘材料等。可见Sialon纳米带可能成为未来构筑纳米元器件不可缺少的重要材料之一。There is a big difference in structure between nanobelts and other one-dimensional nanomaterials. Its cross-section is different from that of nanotubes and nanowires, which is close to a circle, but a narrow rectangle, with a thickness of several to tens of nanometers and a width of tens of nanometers to hundreds of nanometers, and up to several millimeters in length. As a novel one-dimensional nanostructure, nanobelts have the advantages of perfect crystallization and no defects. Conductive nanoribbons are a better model for studying confinement effects in electron transport, and semiconducting nanoribbons can be used as the core part of nanosensors. Sialon nanobelts have unique properties and application prospects that other nanobelts do not have, such as very high mechanical strength and high temperature resistance, which can be used in the reinforcement of nanocomposites; due to Sialon's excellent dielectric properties, thermal conductivity and mechanical strength Sialon nano Tape can be used to build circuit substrates and dielectrics for single-nanometer electronic devices, as well as insulating materials for supercapacitors. It can be seen that Sialon nanoribbons may become one of the indispensable and important materials for the construction of nano-components in the future.
实施例2：Example 2:
一种Sialon准一维纳米材料及其的制备方法，它的原料由以下组分按照重量百分比组成：含氢硅油37％、乙二胺60％，Al粉3％。步骤为：a.将含氢硅油169ml、乙二胺274ml和Al粉15克混合，在反应釜中进行反应，反应温度控制在0～100℃，使用溶剂为四氢呋喃500ml和正己烷250ml，在常温下不断搅拌8～12小时，反应形成Si-Al-O-N-C聚合物。其他步骤和工艺条件与具体实施例1相同。在石墨坩埚中结晶形成厚度为50nm，，宽度为300nm，长数百μm的Sialon纳米带。A Sialon quasi-one-dimensional nanometer material and its preparation method. Its raw materials are composed of the following components according to weight percentage: 37% of hydrogen-containing silicone oil, 60% of ethylenediamine, and 3% of Al powder. The steps are: a. Mix 169ml of hydrogen-containing silicone oil, 274ml of ethylenediamine and 15g of Al powder, and react in a reaction kettle. The reaction temperature is controlled at 0-100°C. Under constant stirring for 8 to 12 hours, the reaction forms Si-Al-O-N-C polymer. Other steps and processing condition are identical with specific embodiment 1. Sialon nanobelts with a thickness of 50nm, a width of 300nm, and a length of hundreds of μm were formed by crystallization in a graphite crucible.
实施例3：Example 3:
一种Sialon准一维纳米材料及其的制备方法，它的原料由以下组分按照重量百分比组成：含氢硅油45％、乙二胺45％，Al粉10％。步骤为：a.将含氢硅油68ml、乙二胺70ml和Al粉15克混合，在反应釜中进行反应，反应温度控制在0～100℃，使用溶剂为四氢呋喃500ml和正己烷250ml，在常温下不断搅拌8～12小时，反应形成Si-Al-O-N-C聚合物；b.将上一步骤所得产物置于石墨坩埚中，石墨坩埚放入气氛压力烧结炉中，通入氮气，炉内氮气压力控制在1.5MPa，控制温度在1200℃的条件下保温3小时，在石墨坩埚中结晶形成Sialon准一维纳米材料，为厚度为80nm，，宽度为4000nm，长数百μm的Sialon纳米带。A Sialon quasi-one-dimensional nanometer material and its preparation method. Its raw materials are composed of the following components according to weight percentage: 45% of hydrogen-containing silicone oil, 45% of ethylenediamine, and 10% of Al powder. The steps are: a. Mix 68ml of hydrogen-containing silicone oil, 70ml of ethylenediamine and 15g of Al powder, and react in a reaction kettle. The reaction temperature is controlled at 0-100°C. Under constant stirring for 8 to 12 hours, the reaction forms a Si-Al-O-N-C polymer; b. The product obtained in the previous step is placed in a graphite crucible, and the graphite crucible is placed in an atmosphere pressure sintering furnace, and nitrogen gas is introduced, and the nitrogen pressure in the furnace Controlled at 1.5MPa, controlled temperature at 1200°C for 3 hours, and crystallized in a graphite crucible to form Sialon quasi-one-dimensional nanomaterials, which are Sialon nanobelts with a thickness of 80nm, a width of 4000nm, and a length of several hundred μm.
实施例4：Example 4:
一种Sialon准一维纳米材料及其的制备方法，写明它的原料由以下组分按照重量百分比组成：含氢硅油49％、乙二胺49％，Al粉2％。a步骤为：将含氢硅油104ml、乙二胺102ml和Al粉5克混合，在反应釜中进行反应，反应温度控制在0～100℃，使用溶剂为四氢呋喃500ml和正己烷250ml，在常温下不断搅拌8～12小时，反应形成Si-Al-O-N-C聚合物；b.将上一步骤所得产物置于石墨坩埚中，石墨坩埚放入气氛压力烧结炉中，通入氮气，炉内氮气压力控制在0.8MPa，控制温度在1500℃的条件下保温2小时，在石墨坩埚中结晶形成Sialon准一维纳米材料，得到厚度为30nm，，宽度为150nm，长数百μm的Sialon纳米带。A Sialon quasi-one-dimensional nanomaterial and its preparation method, which state that its raw materials are composed of the following components according to weight percentage: 49% of hydrogen-containing silicone oil, 49% of ethylenediamine, and 2% of Al powder. Step a is: mix 104ml of hydrogen-containing silicone oil, 102ml of ethylenediamine and 5 grams of Al powder, and react in a reaction kettle. Stir continuously for 8 to 12 hours, and react to form Si-Al-O-N-C polymer; b. Place the product obtained in the previous step in a graphite crucible, put the graphite crucible into an atmosphere pressure sintering furnace, feed nitrogen, and control the nitrogen pressure in the furnace At 0.8MPa, the temperature is controlled at 1500°C for 2 hours, and the Sialon quasi-one-dimensional nanomaterial is crystallized in a graphite crucible to obtain a Sialon nanoribbon with a thickness of 30nm, a width of 150nm, and a length of several hundred μm.
实施例5：Example 5:
一种Sialon准一维纳米材料及其的制备方法，它的原料由以下组分按照重量百分比组成：含氢硅油55％、乙二胺43％，Al粉2％。本实施例与具体实施1的步骤a、a`相同，b步骤为：将所制备的Si-Al-O-N-C粉末置于石墨坩埚中，石墨坩埚放入气氛压力压烧结炉中，通入氮气压力为1.2Mpa，控制温度在1350℃的条件下保温2小时。在石墨坩埚中结晶形成得到厚度为50nm，，宽度为4000nm，长数百μm的Sialon纳米带。A Sialon quasi-one-dimensional nanometer material and its preparation method. Its raw materials are composed of the following components according to weight percentage: 55% of hydrogen-containing silicone oil, 43% of ethylenediamine, and 2% of Al powder. This embodiment is the same as the steps a and a` of the specific implementation 1, and the step b is: place the prepared Si-Al-O-N-C powder in a graphite crucible, put the graphite crucible into an atmosphere pressure sintering furnace, and pass nitrogen pressure The temperature is 1.2Mpa, and the temperature is controlled at 1350°C for 2 hours. Sialon nanoribbons with a thickness of 50nm, a width of 4000nm, and a length of hundreds of μm were obtained by crystallization in a graphite crucible.
实施例6：Embodiment 6:
一种Sialon准一维纳米材料及其的制备方法，它的原料由以下组分按照重量百分比组成：含氢硅油55％、乙二胺43％，Al粉2％。本实施例与具体实施1的步骤a、a`相同，不同的是，b步骤为：将所制备的Si-Al-O-N-C粉末置于石墨坩埚中，石墨坩埚放入气氛压力压烧结炉中，通入氮气压力为1.2Mpa，控制温度在1300℃的条件下保温2小时。在石墨坩埚中结晶形成直径为90nm，长数百μm的Sialon纳米线。A Sialon quasi-one-dimensional nanometer material and its preparation method. Its raw materials are composed of the following components according to weight percentage: 55% of hydrogen-containing silicone oil, 43% of ethylenediamine, and 2% of Al powder. This embodiment is the same as steps a and a` of the specific implementation 1, the difference is that the step b is as follows: the prepared Si-Al-O-N-C powder is placed in a graphite crucible, and the graphite crucible is placed in an atmosphere pressure sintering furnace, The nitrogen pressure is 1.2Mpa, and the temperature is controlled at 1300°C for 2 hours. Crystallized in a graphite crucible to form Sialon nanowires with a diameter of 90 nm and a length of several hundred μm.
实施例7Example 7
Sialon准一维纳米材料，它的原料由以下组分按照重量百分比组成：含氢硅油45％、乙二胺48％、Al粉7％。Sialon准一维纳米材料的制备方法，a.将含氢硅油96ml、乙二胺103ml和Al粉15克混合，在反应釜中进行反应，反应温度控制在0～100℃，使用溶剂为四氢呋喃500ml和正己烷250ml，在常温下不断搅拌8～12小时，反应形成Si-Al-O-N-C聚合物；a.将聚合物在管式气氛保护炉中对Si-Al-O-N-C有机聚合物进行裂解，通入氮气，氮气流量为200～400ml/min，温度工艺为在室温～750℃的温度范围内，升温速度为5℃/min，在750℃保温1小时，在750～1000℃的温度范围内，升温速度为5℃/min，在1000℃保温1小时，得到Si-Al-O-N-C粉末；b.将所制备的Si-Al-O-N-C粉末置于石墨坩埚中，石墨坩埚放入气氛压力压烧结炉中，通入氮气压力为1.2Mpa，控制温度在1400℃的条件下保温2小时，在石墨坩埚中结晶形成厚度为50nm，，宽度为280nm，长数百μm的Sialon纳米带。The Sialon quasi-one-dimensional nanomaterial is composed of the following components according to weight percentage: 45% hydrogen-containing silicone oil, 48% ethylenediamine, and 7% Al powder. The preparation method of Sialon quasi-one-dimensional nanomaterials, a. Mix 96ml of hydrogen-containing silicone oil, 103ml of ethylenediamine and 15g of Al powder, and react in a reaction kettle. The reaction temperature is controlled at 0-100°C, and the solvent used is 500ml of tetrahydrofuran. and n-hexane 250ml, stirring continuously at room temperature for 8 to 12 hours, reacting to form Si-Al-O-N-C polymer; Inject nitrogen, the nitrogen flow rate is 200-400ml/min, the temperature process is within the temperature range of room temperature to 750°C, the heating rate is 5°C/min, and the temperature is kept at 750°C for 1 hour, and within the temperature range of 750-1000°C, The heating rate is 5°C/min, and the temperature is kept at 1000°C for 1 hour to obtain Si-Al-O-N-C powder; b. Put the prepared Si-Al-O-N-C powder in a graphite crucible, and put the graphite crucible into an atmosphere pressure sintering furnace In the process, the nitrogen pressure was 1.2Mpa, the temperature was controlled at 1400°C for 2 hours, and the Sialon nanoribbons with a thickness of 50nm, a width of 280nm, and a length of hundreds of μm were crystallized in a graphite crucible.
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| CN101570919B (en) * | 2009-06-05 | 2010-09-01 | 哈尔滨工业大学（威海） | Sialon nano non-woven fabric and preparation method thereof |
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| JP2704332B2 (en) * | 1991-10-11 | 1998-01-26 | 株式会社ノリタケカンパニーリミテド | Carbon fiber reinforced silicon nitride nanocomposite and method for producing the same |
| JP3081842B1 (en) * | 1999-07-13 | 2000-08-28 | ファインセラミックス技術研究組合 | α-sialon particles |
| CN1266078C (en) * | 2004-12-22 | 2006-07-26 | 哈尔滨工业大学 | SiALONC ceramic with hydrogen silicone oil and Al powder and production thereof |
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| CN102924088A (en) * | 2012-11-27 | 2013-02-13 | 哈尔滨工业大学（威海） | Sialon bicrystal nanoribbon and method for preparing same |
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