CN110218958B - A kind of method for preparing silicon carbide nanowire reinforced titanium matrix composite material at low temperature - Google Patents

Abstract

Translated fromChinese

本发明公开了一种低温制备碳化硅纳米线增强钛基复合材料的方法，该方法将无水乙醇、正硅酸乙酯、蒸馏水和盐酸溶液混匀后加入石墨粉得包覆二氧化硅溶胶的石墨粉，经碳热还原反应得碳化硅纳米线，然后将碳化硅纳米线超声后分散后加入钛粉保温搅匀，经干燥得碳化硅纳米线与钛粉的混合粉末，再进行放电等离子热压烧结，得碳化硅纳米线增强钛基复合材料。本发明在低温、高压下进行放电等离子热压烧结，避免了高温环境中碳化硅纳米线与钛反应生成碳化物及硅化物，保证了碳化硅纳米线的强韧化效应；同时，碳化硅纳米线与钛基紧密结合，形成多尺度增韧结构，提高了碳化硅纳米线的强韧化效应，提高了碳化硅纳米线增强钛基复合材料的力学性能。

The invention discloses a method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature. In the method, anhydrous ethanol, ethyl orthosilicate, distilled water and hydrochloric acid solution are mixed uniformly, and graphite powder is added to obtain a coated silica sol The graphite powder is obtained by carbothermic reduction reaction to obtain silicon carbide nanowires. Then, the silicon carbide nanowires are ultrasonically dispersed, and then titanium powder is added for heat preservation and stirring. After drying, the mixed powder of silicon carbide nanowires and titanium powder is obtained, and then the discharge plasma is carried out. Hot pressing and sintering to obtain a silicon carbide nanowire reinforced titanium matrix composite material. The invention conducts discharge plasma hot pressing sintering under low temperature and high pressure, avoids the formation of carbides and silicides from the reaction between silicon carbide nanowires and titanium in a high temperature environment, and ensures the strengthening and toughening effect of silicon carbide nanowires; The wires are closely combined with the titanium matrix to form a multi-scale toughening structure, which improves the toughening effect of the silicon carbide nanowires and improves the mechanical properties of the silicon carbide nanowires reinforced titanium matrix composites.

Description

Translated fromChinese

一种低温制备碳化硅纳米线增强钛基复合材料的方法A kind of method for preparing silicon carbide nanowire reinforced titanium matrix composite material at low temperature

技术领域technical field

本发明属于材料制备技术领域，具体涉及一种低温制备碳化硅纳米线增强钛基复合材料的方法。The invention belongs to the technical field of material preparation, in particular to a method for preparing a silicon carbide nanowire reinforced titanium-based composite material at a low temperature.

背景技术Background technique

钛及钛合金作为性能优异的轻量化结构材料，拥有较高的比强度、比刚度及良好的加工性、耐蚀性与耐高温性能，在航天航空、船舶汽车、兵器工程、医疗器械和化工能源等众多领域的应用前景广阔。但钛及钛合金耐磨性差、硬度较低等弱点阻碍其在工程中的应用。为满足高新科技飞速发展伴随的种种需求，急需研发新型钛合金复合材料以满足航空航天事业发展的需求。As lightweight structural materials with excellent performance, titanium and titanium alloys have high specific strength, specific stiffness and good processability, corrosion resistance and high temperature resistance. It has broad application prospects in many fields such as energy. However, the weak wear resistance and low hardness of titanium and titanium alloys hinder their application in engineering. In order to meet the various needs accompanied by the rapid development of high-tech, it is urgent to develop new titanium alloy composite materials to meet the needs of the development of the aerospace industry.

碳化硅纳米线具有高强度、高模量、耐热、耐磨等优异性能，已成功应用于增强和改性陶瓷基，金属基和树脂基复合材料并且显示较好的增韧效果。利用热压烧结工艺制备碳化硅纳米线增强钛基复合材料过程中，由于高温环境下(热压烧结工艺的温度通常为1200℃～1400℃)钛的活性比较高，碳化硅纳米线易于钛发生反应，生成碳化物及硅化物，失去碳化硅纳米线的固有的结构特征，从而导致碳化硅纳米线的强韧化效应减弱。Silicon carbide nanowires have excellent properties such as high strength, high modulus, heat resistance, wear resistance, etc., and have been successfully used to strengthen and modify ceramic matrix, metal matrix and resin matrix composite materials and show good toughening effect. In the process of preparing silicon carbide nanowires reinforced titanium matrix composites by hot pressing sintering process, due to the high activity of titanium in high temperature environment (the temperature of hot pressing sintering process is usually 1200℃～1400℃), silicon carbide nanowires are prone to titanium generation. After the reaction, carbides and silicides are formed, and the inherent structural characteristics of the silicon carbide nanowires are lost, thereby reducing the strengthening and toughening effect of the silicon carbide nanowires.

发明内容SUMMARY OF THE INVENTION

本发明所要解决的技术问题在于针对上述现有技术的不足，提供一种低温制备碳化硅纳米线增强钛基复合材料的方法。该方法将碳化硅纳米线与钛粉混匀后，在低温、高压的条件下进行放电等离子热压烧结制备碳化硅纳米线增强钛基复合材料，避免了常规热烧结过程的高温环境中碳化硅纳米线与钛反应生成碳化物及硅化物，保证了碳化硅纳米线的强韧化效应；同时，碳化硅纳米线与钛基紧密结合，形成多尺度增韧结构，提高了碳化硅纳米线的强韧化效应，提高了碳化硅纳米线增强钛基复合材料的力学性能。The technical problem to be solved by the present invention is to provide a method for preparing a silicon carbide nanowire reinforced titanium-based composite material at a low temperature in view of the deficiencies of the above-mentioned prior art. In the method, after mixing silicon carbide nanowires and titanium powder, spark plasma hot pressing is performed under low temperature and high pressure conditions to prepare silicon carbide nanowires reinforced titanium matrix composite material, which avoids the high temperature environment of silicon carbide in the conventional thermal sintering process. The nanowires react with titanium to form carbides and silicides, which ensure the toughening effect of the silicon carbide nanowires; at the same time, the silicon carbide nanowires are closely combined with the titanium base to form a multi-scale toughening structure, which improves the toughness of the silicon carbide nanowires. The toughening effect improves the mechanical properties of silicon carbide nanowires reinforced titanium matrix composites.

为解决上述技术问题，本发明采用的技术方案是：一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，该方法包括以下步骤：In order to solve the above-mentioned technical problems, the technical solution adopted in the present invention is: a method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature, characterized in that the method comprises the following steps:

步骤一、将无水乙醇和正硅酸乙酯混合后搅拌均匀，然后加入蒸馏水和盐酸溶液并搅拌均匀，得到二氧化硅溶胶；所述无水乙醇、正硅酸乙酯、蒸馏水和盐酸溶液中盐酸的摩尔比为(3～5)：(0.5～2)：(3～8)：(0.1～0.5)；Step 1. After mixing absolute ethanol and tetraethyl silicate, stir evenly, then add distilled water and hydrochloric acid solution and stir evenly to obtain silica sol; in the absolute ethanol, ethyl orthosilicate, distilled water and hydrochloric acid solution The molar ratio of hydrochloric acid is (3-5): (0.5-2): (3-8): (0.1-0.5);

步骤二、将粒度为60目～150目的石墨粉加入到步骤一中得到的二氧化硅溶胶中搅拌均匀，然后放置于烘箱中，在温度为100℃的条件下干燥12h～24h，得到包覆二氧化硅溶胶的石墨粉；Step 2: Add graphite powder with a particle size of 60 mesh to 150 mesh into the silica sol obtained in step 1 and stir evenly, then place it in an oven, and dry it at a temperature of 100 ° C for 12 h to 24 h to obtain a coating Graphite powder of silica sol;

步骤三、将步骤二中得到的包覆二氧化硅溶胶的石墨粉放置于高温管式炉中进行碳热还原反应，然后经超声清洗和离心，去掉上清液，得到的沉淀物为碳化硅纳米线；所述碳热还原反应的具体过程为：在氩气保护气氛条件下，以5℃/min～10℃/min的速率升温至1400℃～1700℃后保温1h～3h；Step 3: Place the silica sol-coated graphite powder obtained in Step 2 in a high-temperature tubular furnace to carry out a carbothermic reduction reaction, then ultrasonically clean and centrifuge to remove the supernatant, and the obtained precipitate is silicon carbide. Nanowires; the specific process of the carbothermal reduction reaction is as follows: under the condition of an argon protective atmosphere, the temperature is raised to 1400°C to 1700°C at a rate of 5°C/min to 10°C/min, and then kept for 1h to 3h;

步骤四、将步骤三中得到的碳化硅纳米线加入到无水乙醇中超声60min～120min，然后加入钛粉并在60℃～80℃的水浴锅保温条件下机械搅拌均匀，再经干燥得到碳化硅纳米线与钛粉的混合粉末；Step 4. Add the silicon carbide nanowires obtained in step 3 into absolute ethanol for 60min-120min, then add titanium powder and stir mechanically evenly under the heat preservation condition of a water bath at 60°C to 80°C, and then dry to obtain carbonization Mixed powder of silicon nanowires and titanium powder;

步骤五、将步骤四中得到的碳化硅纳米线与钛粉的混合粉末装入模具中，然后放置于放电等离子热压烧结炉中进行放电等离子热压烧结，经冷却后得到碳化硅纳米线增强钛基复合材料；所述放电等离子热压烧结的工艺参数为：真空度1.0×10^-3Pa～3.0×10^-3Pa，温度600℃～900℃，压力40MPa～180MPa，保温时间5min～10min。Step 5. Put the mixed powder of silicon carbide nanowires and titanium powder obtained in step 4 into a mold, and then place it in a discharge plasma hot pressing sintering furnace for discharge plasma hot pressing sintering, and obtain silicon carbide nanowires after cooling. Titanium matrix composite material; the process parameters of the spark plasma hot pressing sintering are: vacuum degree 1.0 × 10^-3 Pa ~ 3.0 × 10^-3 Pa, temperature 600 ℃ ~ 900 ℃, pressure 40MPa ~ 180MPa, holding time 5min ~ 10min .

本发明首先采用溶胶凝胶碳热还原反应法制备碳化硅纳米线，然后将碳化硅纳米线与钛粉混匀后进行放电等离子热压烧结，在温度600℃～900℃、压力40MPa～180MPa的低温高压的条件下制备碳化硅纳米线增强钛基复合材料，避免了常规热烧结过程的高温环境中碳化硅纳米线与钛反应生成碳化物及硅化物而失去碳化硅纳米线的固有的结构特征，导致碳化硅纳米线的强韧化效应减弱，同时，该低温高压条件下碳化硅纳米线与钛基紧密结合，形成多尺度增韧结构，提高了碳化硅纳米线的强韧化效应，提高了碳化硅纳米线增强钛基复合材料的力学性能。In the present invention, silicon carbide nanowires are first prepared by a sol-gel carbothermic reduction reaction method, and then the silicon carbide nanowires and titanium powder are mixed uniformly and then sintered by discharge plasma hot pressing. The preparation of silicon carbide nanowires reinforced titanium-based composite materials under the condition of low temperature and high pressure avoids the reaction of silicon carbide nanowires with titanium in the high temperature environment of the conventional thermal sintering process to form carbides and silicides and lose the inherent structural characteristics of silicon carbide nanowires , resulting in the weakening of the toughening effect of silicon carbide nanowires. At the same time, under the condition of low temperature and high pressure, the silicon carbide nanowires are closely combined with the titanium base to form a multi-scale toughening structure, which improves the toughening effect of silicon carbide nanowires. Mechanical properties of silicon carbide nanowires reinforced titanium matrix composites.

上述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤一中所述盐酸溶液的质量浓度为37％。上述盐酸溶液浓度为常用的使用浓度，配制方便。The above-mentioned method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature is characterized in that the mass concentration of the hydrochloric acid solution in step 1 is 37%. The concentration of the above-mentioned hydrochloric acid solution is the commonly used concentration, and the preparation is convenient.

上述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤二中所述粒度为60目～150目的石墨粉与二氧化硅溶胶的质量比为1:5，所述搅拌均匀的时间为20min～60min。上述石墨粉二氧化硅溶胶的质量比及对应的搅拌时间促进了石墨粉均匀地包裹在二氧化硅溶胶周围，有利于得到尺寸均匀的碳化硅纳米线。The above-mentioned method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature is characterized in that the mass ratio of graphite powder with particle size of 60 meshes to 150 meshes and silica sol in step 2 is 1:5, so The time for the uniform stirring is 20 min to 60 min. The above-mentioned mass ratio of the graphite powder to the silica sol and the corresponding stirring time promotes the graphite powder to be evenly wrapped around the silica sol, which is beneficial to obtain silicon carbide nanowires with uniform size.

上述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤三中所述超声清洗和离心的次数均为两次，所述离心采用的转速为8000r/min～10000r/min。上述超声清洗和离心的次数及离心转速有利于碳热还原反应体系中杂质的去除，从而得到表面无杂质的碳化硅纳米线。The above-mentioned method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature is characterized in that the times of ultrasonic cleaning and centrifugation in step 3 are both twice, and the rotational speed used in the centrifugation is 8000r/min～10000r /min. The above-mentioned times of ultrasonic cleaning and centrifugation and the centrifugal speed are beneficial to the removal of impurities in the carbothermic reduction reaction system, thereby obtaining silicon carbide nanowires with no impurities on the surface.

上述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤三中得到的碳化硅纳米线的直径为50nm～200nm。上述尺寸的碳化硅纳米线比表面积大，强度高，且可在钛粉中形成均匀分散。The above-mentioned method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature is characterized in that the diameter of the silicon carbide nanowire obtained in step 3 is 50 nm to 200 nm. The silicon carbide nanowires of the above-mentioned size have large specific surface area, high strength, and can be uniformly dispersed in the titanium powder.

上述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤四中所述钛粉的粒度为15μm～45μm。上述粒度的钛粉粒度合适，有利于分散。The above-mentioned method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature is characterized in that the particle size of the titanium powder in step 4 is 15 μm˜45 μm. The titanium powder with the above-mentioned particle size has a suitable particle size and is favorable for dispersion.

上述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤四中所述机械搅拌均匀的时间为6h～12h。上述机械搅拌均匀的时间促进了钛粉与碳化硅纳米线充分混合均匀。The above-mentioned method for preparing a silicon carbide nanowire reinforced titanium-based composite material at a low temperature is characterized in that the time for uniform mechanical stirring in step 4 is 6 h to 12 h. The above-mentioned time for uniform mechanical stirring promotes the uniform mixing of the titanium powder and the silicon carbide nanowires.

上述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤四中所述干燥的温度为80℃～100℃，时间为8h～12h。该干燥参数可快速干燥得到碳化硅纳米线与钛粉的混合粉末。The above-mentioned method for preparing a silicon carbide nanowire reinforced titanium-based composite material at a low temperature is characterized in that the drying temperature in step 4 is 80°C to 100°C, and the time is 8h to 12h. The drying parameters can quickly dry to obtain a mixed powder of silicon carbide nanowires and titanium powder.

上述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤五中所述模具的直径为30mm～60mm。采用上述模具有利于放电等离子热压烧结过程中电流快速通过模具并加热，实现快速升温。The above-mentioned method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature is characterized in that the diameter of the mold in step 5 is 30mm-60mm. The use of the above-mentioned mold is beneficial to the rapid passing of the current through the mold and heating during the spark plasma hot pressing sintering process, so as to achieve rapid temperature rise.

上述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤五中所述碳化硅纳米线增强钛基复合材料中碳化硅纳米线的质量分数为0.01％～10％。上述质量分数的碳化硅纳米线可均匀分散在钛基中，有效提高了钛基复合材料的力学性能。The above-mentioned method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature is characterized in that the mass fraction of silicon carbide nanowires in the silicon carbide nanowire-reinforced titanium-based composite material in step 5 is 0.01% to 10% . The above-mentioned mass fraction of silicon carbide nanowires can be uniformly dispersed in the titanium matrix, which effectively improves the mechanical properties of the titanium matrix composite material.

本发明与现有技术相比具有以下优点：Compared with the prior art, the present invention has the following advantages:

1、本发明将碳化硅纳米线与钛粉混匀后，在低温、高压的条件下进行放电等离子热压烧结，制备碳化硅纳米线增强钛基复合材料，避免了常规热烧结过程的高温环境中碳化硅纳米线与钛反应生成碳化物及硅化物，保证了碳化硅纳米线的强韧化效应，提高了碳化硅纳米线增强钛基复合材料的力学性能。1. In the present invention, after mixing silicon carbide nanowires and titanium powder, discharge plasma hot-pressing sintering is performed under the conditions of low temperature and high pressure to prepare silicon carbide nanowires reinforced titanium-based composite material, which avoids the high temperature environment of conventional thermal sintering process. The medium silicon carbide nanowires react with titanium to form carbides and silicides, which ensures the toughening effect of the silicon carbide nanowires and improves the mechanical properties of the silicon carbide nanowires reinforced titanium-based composite material.

2、本发明采用低温高压的放电等离子热压烧结条件，使碳化硅纳米线与钛基紧密结合，形成多尺度增韧结构，提高了碳化硅纳米线的强韧化效应，提高了碳化硅纳米线增强钛基复合材料的力学性能。2. The present invention adopts the low temperature and high pressure discharge plasma hot pressing sintering conditions, so that the silicon carbide nanowires and the titanium base are closely combined to form a multi-scale toughening structure, which improves the toughening effect of the silicon carbide nanowires and improves the silicon carbide nanowires. Mechanical properties of wire-reinforced titanium matrix composites.

3、本发明采用溶胶凝胶碳热还原反应法制备碳化硅纳米线，然后利用超声分散设备快速将所制备的碳化硅纳米线在乙醇溶液中均匀分散，保证了碳化硅纳米线在复合材料中均匀分布。3. The present invention adopts the sol-gel carbothermic reduction reaction method to prepare silicon carbide nanowires, and then uses ultrasonic dispersing equipment to quickly and uniformly disperse the prepared silicon carbide nanowires in an ethanol solution, ensuring that the silicon carbide nanowires are in the composite material. Evenly distributed.

4、本发明将钛粉加入到碳化硅纳米线分散液中，采用机械搅拌的方式在保温条件下混合均匀，降低了制备过程对碳化硅纳米线的损伤，进一步保证了碳化硅纳米线的强韧化效应。4. In the present invention, titanium powder is added into the dispersion liquid of silicon carbide nanowires, and the method of mechanical stirring is used to mix uniformly under the condition of heat preservation, which reduces the damage to the silicon carbide nanowires during the preparation process, and further ensures the strength of the silicon carbide nanowires. toughening effect.

5、与未强化的钛基材料相比，本发明制备的碳化硅纳米线增强钛基复合材料的压缩屈服强度提高了107.7％～136.8％。5. Compared with the unreinforced titanium-based material, the compressive yield strength of the silicon carbide nanowire-reinforced titanium-based composite material prepared by the present invention is increased by 107.7% to 136.8%.

下面通过附图和实施例对本发明的技术方案作进一步的详细描述。The technical solutions of the present invention will be further described in detail below through the accompanying drawings and embodiments.

附图说明Description of drawings

图1是本发明的工艺流程图。Fig. 1 is a process flow diagram of the present invention.

图2是本发明实施例1制备的碳化硅纳米线的SEM图(5000×)。FIG. 2 is a SEM image (5000×) of silicon carbide nanowires prepared in Example 1 of the present invention.

图3是本发明实施例1制备的碳化硅纳米线的SEM图(20000×)。3 is a SEM image (20000×) of the silicon carbide nanowires prepared in Example 1 of the present invention.

图4是本发明实施例1制备的碳化硅纳米线增强钛基复合材料的断口FE-SEM图(50000×)。FIG. 4 is a fracture FE-SEM image (50000×) of the silicon carbide nanowire reinforced titanium matrix composite material prepared in Example 1 of the present invention.

图5是本发明对比例1制备的钛基材料的断口SEM图(5000×)。FIG. 5 is a SEM image (5000×) of the fracture surface of the titanium-based material prepared in Comparative Example 1 of the present invention.

图6是本发明对比例2制备的碳化硅纳米线增强钛基复合材料的断口SEM图(5000×)。6 is a fracture SEM image (5000×) of the silicon carbide nanowire reinforced titanium-based composite material prepared in Comparative Example 2 of the present invention.

具体实施方式Detailed ways

如图1所示，本发明制备碳化硅纳米线增强钛基复合材料的具体过程为：将二氧化硅溶胶和石墨粉混合搅拌后，得到包覆二氧化硅溶胶的石墨粉，然后经碳热还原反应得到碳化硅纳米线，将碳化硅纳米线与钛粉混匀后进行放电等离子热压烧结，得到碳化硅纳米线增强钛基复合材料。As shown in Figure 1, the specific process of preparing the silicon carbide nanowire reinforced titanium-based composite material in the present invention is as follows: after mixing and stirring the silica sol and the graphite powder, the graphite powder coated with the silica sol is obtained, and then the carbon-heated graphite powder is obtained. The silicon carbide nanowires are obtained by the reduction reaction, and the silicon carbide nanowires and the titanium powder are mixed uniformly, and then discharge plasma hot pressing is performed to obtain the silicon carbide nanowires reinforced titanium-based composite material.

实施例1Example 1

本实施例包括以下步骤：This embodiment includes the following steps:

步骤一、将无水乙醇和正硅酸乙酯混合后搅拌均匀，然后加入蒸馏水和质量浓度为37％的盐酸溶液并搅拌均匀，得到二氧化硅溶胶；所述无水乙醇、正硅酸乙酯、蒸馏水和盐酸溶液中盐酸的摩尔比为3：0.5：3：0.1；Step 1: Mix the absolute ethanol and ethyl orthosilicate and stir evenly, then add distilled water and a hydrochloric acid solution with a mass concentration of 37% and stir evenly to obtain a silica sol; the absolute ethanol, ethyl orthosilicate , the molar ratio of hydrochloric acid in distilled water and hydrochloric acid solution is 3:0.5:3:0.1;

步骤二、将粒度为60目～150目的石墨粉加入到步骤一中得到的二氧化硅溶胶中搅拌20min，然后放置于烘箱中，在温度为100℃的条件下干燥12h，得到包覆二氧化硅溶胶的石墨粉；所述粒度为60目～150目的石墨粉与二氧化硅溶胶的质量比为1:5；Step 2: Add graphite powder with a particle size of 60 mesh to 150 mesh into the silica sol obtained in step 1 and stir for 20 minutes, then place in an oven, and dry for 12 hours at a temperature of 100 ° C to obtain coated dioxide The graphite powder of silica sol; the mass ratio of the graphite powder with the particle size of 60 mesh to 150 mesh and the silica sol is 1:5;

步骤三、将步骤二中得到的包覆二氧化硅溶胶的石墨粉放置于高温管式炉中进行碳热还原反应，然后依次经一次超声清洗、一次离心、二次超声清洗和二次离心，去掉二次离心的上清液，得到的沉淀物为碳化硅纳米线；所示一次离心和二次离心采用的转速均为8000r/min；所述碳热还原反应的具体过程为：在氩气保护气氛条件下，以5℃/min的速率升温至1400℃后保温1h；所述碳化硅纳米线的直径为50nm；Step 3, placing the silica sol-coated graphite powder obtained in step 2 in a high-temperature tubular furnace to carry out a carbothermic reduction reaction, and then performing an ultrasonic cleaning, a centrifugation, a second ultrasonic cleaning and a second centrifugation successively, Remove the supernatant of the second centrifugation, and the obtained precipitate is silicon carbide nanowires; the rotation speed used for the first centrifugation and the second centrifugation is both 8000r/min; the specific process of the carbothermal reduction reaction is: in argon gas Under protective atmosphere conditions, the temperature was raised to 1400°C at a rate of 5°C/min, and then kept for 1 h; the diameter of the silicon carbide nanowires was 50 nm;

步骤四、将0.01g步骤三中得到的碳化硅纳米线加入到100g无水乙醇中超声60min，然后加入100g粒度为15μm～45μm的钛粉并在60℃的水浴锅保温条件下机械搅拌均匀6h，再在温度为80℃的条件下干燥8h，得到碳化硅纳米线与钛粉的混合粉末；Step 4. Add 0.01 g of the silicon carbide nanowires obtained in step 3 into 100 g of absolute ethanol and ultrasonically for 60 min, then add 100 g of titanium powder with a particle size of 15 μm to 45 μm, and mechanically stir uniformly for 6 h under the thermal insulation condition of a water bath at 60° C. , and then dried at a temperature of 80 °C for 8 h to obtain a mixed powder of silicon carbide nanowires and titanium powder;

步骤五、将步骤四中得到的碳化硅纳米线与钛粉的混合粉末装入模具中，然后放置于放电等离子热压烧结炉中进行放电等离子热压烧结，经冷却后得到碳化硅纳米线增强钛基复合材料；所述模具的直径为30mm；所述放电等离子热压烧结的工艺参数为：真空度1.0×10^-3Pa，温度600℃，压力180MPa，保温时间5min。Step 5. Put the mixed powder of silicon carbide nanowires and titanium powder obtained in step 4 into a mold, and then place it in a discharge plasma hot pressing sintering furnace for discharge plasma hot pressing sintering, and obtain silicon carbide nanowires after cooling. Titanium-based composite material; the diameter of the mold is 30mm; the process parameters of the spark plasma hot pressing sintering are: vacuum degree 1.0×10^-3 Pa, temperature 600°C, pressure 180MPa, and holding time 5min.

图2是本实施例制备的碳化硅纳米线的SEM图(5000×)，图3是本实施例制备的碳化硅纳米线的SEM图(20000×)，从图2和图3可以看出，本实施例制备的碳化硅纳米线未发生团聚现象。Fig. 2 is the SEM image (5000×) of the silicon carbide nanowires prepared in this embodiment, and Fig. 3 is the SEM image (20000×) of the silicon carbide nanowires prepared in this embodiment. It can be seen from Figs. 2 and 3 that, The silicon carbide nanowires prepared in this example did not agglomerate.

图4是本实施例制备的碳化硅纳米线增强钛基复合材料的断口FE-SEM图(50000×)，从图4可以看出，本实施例的碳化硅纳米线增强钛基复合材料断裂过程中，碳化硅纳米线从钛基体中拔出，延长了裂纹扩展的路线，有利于提高碳化硅纳米线增强钛基复合材料的力学性能。Fig. 4 is a fracture FE-SEM image (50000×) of the silicon carbide nanowire reinforced titanium matrix composite material prepared in this embodiment. It can be seen from Fig. 4 that the fracture process of the silicon carbide nanowire reinforced titanium matrix composite material in this embodiment is In the process, the silicon carbide nanowires are pulled out from the titanium matrix, which prolongs the route of crack propagation, which is beneficial to improve the mechanical properties of silicon carbide nanowires reinforced titanium matrix composites.

对比例1Comparative Example 1

本对比例包括以下步骤：This comparative example includes the following steps:

步骤一、将100g粒度为15μm～45μm的钛粉在温度为80℃的条件下干燥8h；Step 1, drying 100 g of titanium powder with a particle size of 15 μm to 45 μm at a temperature of 80° C. for 8 hours;

步骤五、将步骤一中经干燥后的钛粉装入直径为30mm的模具中，然后放置于放电等离子热压烧结炉中进行放电等离子热压烧结，经冷却后得到钛基复合材料；所述放电等离子热压烧结的工艺参数为：真空度1.0×10^-3Pa，温度600℃，压力180MPa，保温时间5min。Step 5: Put the titanium powder dried in step 1 into a mold with a diameter of 30 mm, and then place it in a discharge plasma hot pressing sintering furnace for discharge plasma hot pressing sintering, and obtain a titanium-based composite material after cooling; The process parameters of spark plasma hot pressing sintering are: vacuum degree 1.0×10^-3 Pa, temperature 600°C, pressure 180MPa, and holding time 5min.

图5是本对比例制备的钛基材料的断口SEM图(5000×)，从图5可以看出，本对比例制备的钛基材料中没有碳化硅纳米线的存在。FIG. 5 is a fracture SEM image (5000×) of the titanium-based material prepared in this comparative example. It can be seen from FIG. 5 that there is no silicon carbide nanowire in the titanium-based material prepared in this comparative example.

对比例2Comparative Example 2

本对比例包括以下步骤：This comparative example includes the following steps:

步骤一、将无水乙醇和正硅酸乙酯混合后搅拌均匀，然后加入蒸馏水和质量浓度为37％的盐酸溶液并搅拌均匀，得到二氧化硅溶胶；所述无水乙醇、正硅酸乙酯、蒸馏水和盐酸溶液中盐酸的摩尔比为3：0.5：3：0.1；Step 1: Mix the absolute ethanol and ethyl orthosilicate and stir evenly, then add distilled water and a hydrochloric acid solution with a mass concentration of 37% and stir evenly to obtain a silica sol; the absolute ethanol, ethyl orthosilicate , the molar ratio of hydrochloric acid in distilled water and hydrochloric acid solution is 3:0.5:3:0.1;

步骤二、将粒度为60目～150目的石墨粉加入到步骤一中得到的二氧化硅溶胶中搅拌20min，然后放置于烘箱中，在温度为100℃的条件下干燥12h，得到包覆二氧化硅溶胶的石墨粉；所述粒度为60目～150目的石墨粉与二氧化硅溶胶的质量比为1:5；Step 2: Add graphite powder with a particle size of 60 mesh to 150 mesh into the silica sol obtained in step 1 and stir for 20 minutes, then place in an oven, and dry for 12 hours at a temperature of 100 ° C to obtain coated dioxide The graphite powder of silica sol; the mass ratio of the graphite powder with the particle size of 60 mesh to 150 mesh and the silica sol is 1:5;

步骤三、将步骤二中得到的包覆二氧化硅溶胶的石墨粉放置于高温管式炉中进行碳热还原反应，然后依次经一次超声清洗、一次离心、二次超声清洗和二次离心，去掉二次离心的上清液，得到的沉淀物为碳化硅纳米线；所示一次离心和二次离心采用的转速均为8000r/min；所述碳热还原反应的具体过程为：在氩气保护气氛条件下，以5℃/min的速率升温至1400℃后保温1h；所述碳化硅纳米线的直径为50nm；Step 3, placing the silica sol-coated graphite powder obtained in step 2 in a high-temperature tubular furnace to carry out a carbothermic reduction reaction, and then performing an ultrasonic cleaning, a centrifugation, a second ultrasonic cleaning and a second centrifugation successively, Remove the supernatant of the second centrifugation, and the obtained precipitate is silicon carbide nanowires; the rotation speed used for the first centrifugation and the second centrifugation is both 8000r/min; the specific process of the carbothermal reduction reaction is: in argon gas Under protective atmosphere conditions, the temperature was raised to 1400°C at a rate of 5°C/min, and then kept for 1 h; the diameter of the silicon carbide nanowires was 50 nm;

步骤四、将0.01g步骤三中得到的碳化硅纳米线加入到100g无水乙醇中超声60min，然后加入100g粒度为15μm～45μm的钛粉并在60℃的水浴锅保温条件下机械搅拌均匀6h，再在温度为80℃的条件下干燥8h，得到碳化硅纳米线与钛粉的混合粉末；Step 4. Add 0.01 g of the silicon carbide nanowires obtained in step 3 into 100 g of absolute ethanol and ultrasonically for 60 min, then add 100 g of titanium powder with a particle size of 15 μm to 45 μm, and mechanically stir uniformly for 6 h under the thermal insulation condition of a water bath at 60° C. , and then dried at a temperature of 80 °C for 8 h to obtain a mixed powder of silicon carbide nanowires and titanium powder;

步骤五、将步骤四中得到的碳化硅纳米线与钛粉的混合粉末装入模具中，然后放置于放电等离子热压烧结炉中进行放电等离子热压烧结，经冷却后得到碳化硅纳米线增强钛基复合材料；所述模具的直径为30mm；所述放电等离子热压烧结的工艺参数为：真空度1.0×10^-3Pa，温度1200℃，压力40MPa，保温时间5min。Step 5. Put the mixed powder of silicon carbide nanowires and titanium powder obtained in step 4 into a mold, and then place it in a discharge plasma hot pressing sintering furnace for discharge plasma hot pressing sintering, and obtain silicon carbide nanowires after cooling. Titanium-based composite material; the diameter of the mold is 30mm; the process parameters of the spark plasma hot pressing sintering are: vacuum degree 1.0×10^-3 Pa, temperature 1200°C, pressure 40MPa, and holding time 5min.

图6是本对比例制备的碳化硅纳米线增强钛基复合材料的断口SEM图(5000×)，从图6可以看出本对比例制备的碳化硅纳米线增强钛基复合材料中的碳化硅纳米线在高温烧结条件下完全失去了原有的特征形貌。Fig. 6 is the fracture SEM image (5000×) of the silicon carbide nanowire reinforced titanium matrix composite material prepared by this comparative example. It can be seen from Fig. 6 that the silicon carbide in the silicon carbide nanowire reinforced titanium matrix composite material prepared by this comparative example is The nanowires completely lost their original characteristic morphology under high temperature sintering conditions.

将图4、图5和图6进行比较，采用碳化硅纳米线作为增强相可制备得到钛基复合材料，且采用放电等离子烧结工艺进行低温高压烧结，使得碳化硅纳米线原有的特征形貌得到较好的保存，从而对钛基复合材料的力学性能起到更好地增强作用；而采用常规真空热压烧结工艺进行高温低压烧结，由于烧结温度过高，基体中钛的活性比较高，碳化硅纳米线易于钛发生反应，生成碳化物及硅化物，失去碳化硅纳米线的固有的结构特征，从而导致碳化硅纳米线的增强作用减弱。Comparing Figure 4, Figure 5 and Figure 6, the titanium-based composite material can be prepared by using silicon carbide nanowires as the reinforcing phase, and the spark plasma sintering process is used for low temperature and high pressure sintering, so that the original characteristic morphology of silicon carbide nanowires can be obtained. It can be well preserved, so as to better enhance the mechanical properties of titanium matrix composites; while the conventional vacuum hot pressing sintering process is used for high temperature and low pressure sintering, due to the high sintering temperature, the activity of titanium in the matrix is relatively high, Silicon carbide nanowires are prone to react with titanium to form carbides and silicides, and lose the inherent structural characteristics of silicon carbide nanowires, thereby weakening the reinforcing effect of silicon carbide nanowires.

实施例2Example 2

本实施例包括以下步骤：This embodiment includes the following steps:

步骤一、将无水乙醇和正硅酸乙酯混合后搅拌均匀，然后加入蒸馏水和质量浓度为37％的盐酸溶液并搅拌均匀，得到二氧化硅溶胶；所述无水乙醇、正硅酸乙酯、蒸馏水和盐酸溶液中盐酸的摩尔比为5：2：8：0.5；Step 1: Mix the absolute ethanol and ethyl orthosilicate and stir evenly, then add distilled water and a hydrochloric acid solution with a mass concentration of 37% and stir evenly to obtain a silica sol; the absolute ethanol, ethyl orthosilicate , the molar ratio of hydrochloric acid in distilled water and hydrochloric acid solution is 5:2:8:0.5;

步骤二、将粒度为60目～150目的石墨粉加入到步骤一中得到的二氧化硅溶胶中搅拌60min，然后放置于烘箱中，在温度为100℃的条件下干燥24h，得到包覆二氧化硅溶胶的石墨粉；所述粒度为60目～150目的石墨粉与二氧化硅溶胶的质量比为1:5；Step 2: Add graphite powder with a particle size of 60 mesh to 150 mesh into the silica sol obtained in step 1 and stir for 60 minutes, then place in an oven, and dry for 24 hours at a temperature of 100 ° C to obtain coated dioxide The graphite powder of silica sol; the mass ratio of the graphite powder with the particle size of 60 mesh to 150 mesh and the silica sol is 1:5;

步骤三、将步骤二中得到的包覆二氧化硅溶胶的石墨粉放置于高温管式炉中进行碳热还原反应，然后依次经一次超声清洗、一次离心、二次超声清洗和二次离心，去掉二次离心的上清液，得到的沉淀物为碳化硅纳米线；所示一次离心和二次离心采用的转速均为10000r/min；所述碳热还原反应的具体过程为：在氩气保护气氛条件下，以10℃/min的速率升温至1700℃后保温3h；所述碳化硅纳米线的直径为200nm；Step 3, placing the silica sol-coated graphite powder obtained in step 2 in a high-temperature tubular furnace to carry out a carbothermic reduction reaction, and then performing an ultrasonic cleaning, a centrifugation, a second ultrasonic cleaning and a second centrifugation successively, Remove the supernatant of the second centrifugation, and the obtained precipitate is silicon carbide nanowires; the rotation speed used for the first centrifugation and the second centrifugation are both 10000r/min; the specific process of the carbothermal reduction reaction is: in argon gas Under the condition of protective atmosphere, the temperature was raised to 1700°C at a rate of 10°C/min and then kept for 3h; the diameter of the silicon carbide nanowires was 200nm;

步骤四、将10g步骤三中得到的碳化硅纳米线加入到100g无水乙醇中超声120min，然后加入90g粒度为15μm～45μm的钛粉并在80℃的水浴锅保温条件下机械搅拌均匀12h，再在温度为100℃的条件下干燥12h，得到碳化硅纳米线与钛粉的混合粉末；Step 4. Add 10 g of the silicon carbide nanowires obtained in step 3 to 100 g of absolute ethanol and ultrasonically for 120 min, then add 90 g of titanium powder with a particle size of 15 μm to 45 μm, and stir mechanically for 12 h under the condition of water bath insulation at 80 ° C. and then dried at a temperature of 100 °C for 12 hours to obtain a mixed powder of silicon carbide nanowires and titanium powder;

步骤五、将步骤四中得到的碳化硅纳米线与钛粉的混合粉末装入模具中，然后放置于放电等离子热压烧结炉中进行放电等离子热压烧结，经冷却后得到碳化硅纳米线增强钛基复合材料；所述模具的直径为60mm；所述放电等离子热压烧结的工艺参数为：真空度3.0×10^-3Pa，温度900℃，压力40MPa，保温时间10min。Step 5. Put the mixed powder of silicon carbide nanowires and titanium powder obtained in step 4 into a mold, and then place it in a discharge plasma hot pressing sintering furnace for discharge plasma hot pressing sintering, and obtain silicon carbide nanowires after cooling. Titanium matrix composite material; the diameter of the mold is 60mm; the process parameters of the spark plasma hot pressing sintering are: vacuum degree 3.0×10^-3 Pa, temperature 900°C, pressure 40MPa, holding time 10min.

实施例3Example 3

本实施例包括以下步骤：This embodiment includes the following steps:

步骤一、将无水乙醇和正硅酸乙酯混合后搅拌均匀，然后加入蒸馏水和质量浓度为37％的盐酸溶液并搅拌均匀，得到二氧化硅溶胶；所述无水乙醇、正硅酸乙酯、蒸馏水和盐酸溶液中盐酸的摩尔比为4：1.5：6：0.3；Step 1: Mix the absolute ethanol and ethyl orthosilicate and stir evenly, then add distilled water and a hydrochloric acid solution with a mass concentration of 37% and stir evenly to obtain a silica sol; the absolute ethanol, ethyl orthosilicate , the molar ratio of hydrochloric acid in distilled water and hydrochloric acid solution is 4:1.5:6:0.3;

步骤二、将粒度为60目～150目的石墨粉加入到步骤一中得到的二氧化硅溶胶中搅拌40min，然后放置于烘箱中，在温度为100℃的条件下干燥20h，得到包覆二氧化硅溶胶的石墨粉；所述粒度为60目～150目的石墨粉与二氧化硅溶胶的质量比为1:5；Step 2: Add graphite powder with a particle size of 60 mesh to 150 mesh into the silica sol obtained in step 1 and stir for 40 minutes, then place in an oven, and dry for 20 hours at a temperature of 100 ° C to obtain coated dioxide The graphite powder of silica sol; the mass ratio of the graphite powder with the particle size of 60 mesh to 150 mesh and the silica sol is 1:5;

步骤三、将步骤二中得到的包覆二氧化硅溶胶的石墨粉放置于高温管式炉中进行碳热还原反应，然后依次经一次超声清洗、一次离心、二次超声清洗和二次离心，去掉二次离心的上清液，得到的沉淀物为碳化硅纳米线；所示一次离心和二次离心采用的转速均为9000r/min；所述碳热还原反应的具体过程为：在氩气保护气氛条件下，以9℃/min的速率升温至1500℃后保温2h；所述碳化硅纳米线的直径为100nm；Step 3, placing the silica sol-coated graphite powder obtained in step 2 in a high-temperature tubular furnace to carry out a carbothermic reduction reaction, and then performing an ultrasonic cleaning, a centrifugation, a second ultrasonic cleaning and a second centrifugation successively, Remove the supernatant of the second centrifugation, and the obtained precipitate is silicon carbide nanowires; the rotational speed used for the first centrifugation and the second centrifugation are both 9000 r/min; the specific process of the carbothermal reduction reaction is: in argon gas Under the condition of protective atmosphere, the temperature was raised to 1500°C at a rate of 9°C/min and then kept for 2h; the diameter of the silicon carbide nanowires was 100nm;

步骤四、将0.3g步骤三中得到的碳化硅纳米线加入到100g无水乙醇中超声80min，然后加入100g粒度为15μm～45μm的钛粉并在70℃的水浴锅保温条件下机械搅拌均匀10h，再在温度为90℃的条件下干燥10h，得到碳化硅纳米线与钛粉的混合粉末；Step 4. Add 0.3 g of the silicon carbide nanowires obtained in step 3 to 100 g of absolute ethanol and ultrasonically for 80 min, then add 100 g of titanium powder with a particle size of 15 μm to 45 μm and stir mechanically for 10 h under the condition of a water bath at 70 ° C. , and then dried at a temperature of 90 °C for 10 h to obtain a mixed powder of silicon carbide nanowires and titanium powder;

步骤五、将步骤四中得到的碳化硅纳米线与钛粉的混合粉末装入模具中，然后放置于放电等离子热压烧结炉中进行放电等离子热压烧结，经冷却后得到碳化硅纳米线增强钛基复合材料；所述模具的直径为50mm；所述放电等离子热压烧结的工艺参数为：真空度2.0×10^-3Pa，温度700℃，压力60MPa，保温时间6min。Step 5. Put the mixed powder of silicon carbide nanowires and titanium powder obtained in step 4 into a mold, and then place it in a discharge plasma hot pressing sintering furnace for discharge plasma hot pressing sintering, and obtain silicon carbide nanowires after cooling. Titanium-based composite material; the diameter of the mold is 50mm; the process parameters of the spark plasma hot pressing sintering are: vacuum degree 2.0×10^-3 Pa, temperature 700°C, pressure 60MPa, and holding time 6min.

将本发明实施例1～实施例3、对比例2制备的碳化硅纳米线增强钛基复合材料和对比例1制备的钛基材料进行力学性能测试，以压缩屈服强度作为测试标准，结果如下表1所示。The mechanical properties of the silicon carbide nanowire-reinforced titanium-based composite materials prepared in Examples 1 to 3 of the present invention and Comparative Example 2 and the titanium-based materials prepared in Comparative Example 1 were tested, and the compressive yield strength was used as the test standard. The results are as follows 1 shown.

表1实施例1～实施例3、对比例2制备的碳化硅纳米线增强钛基复合材料和对比例1制备的钛基材料Table 1 Silicon carbide nanowire-reinforced titanium-based composite materials prepared in Examples 1 to 3 and Comparative Example 2 and titanium-based materials prepared in Comparative Example 1

从表1可知，本发明实施例1～实施例3制备的碳化硅纳米线增强钛基复合材料的压缩屈服强度均高于对比例1制备的钛基材料、对比例2制备的碳化硅纳米线增强钛基复合材料的压缩屈服强度；在相同的制备工艺条件下，实施例1采用低温烧结制备的碳化硅纳米线增强钛基复合材料的压缩屈服强度高于对比例2采用高温烧结制备的碳化硅纳米线增强钛基复合材料的压缩屈服强度，说明在低温、高压的条件下进行放电等离子热压烧结避免了常规热烧结过程的高温环境中碳化硅纳米线与钛反应生成碳化物及硅化物，保证了碳化硅纳米线的强韧化效应，提高了碳化硅纳米线增强钛基复合材料的力学性能；在相同的放电等离子热压烧结参数条件下，实施例1采用碳化硅纳米线作为增强相制备的钛基复合材料的压缩屈服强度高于对比例1未采用碳化硅纳米线制备的钛基材料的压缩屈服强度，说明放电等离子热压烧结作用下，碳化硅纳米线与钛基紧密结合，形成多尺度增韧结构，提高了碳化硅纳米线的强韧化效应，提高了碳化硅纳米线增强钛基复合材料的力学性能。It can be seen from Table 1 that the compressive yield strengths of the silicon carbide nanowire-reinforced titanium-based composite materials prepared in Examples 1 to 3 of the present invention are all higher than those of the titanium-based materials prepared in Comparative Example 1 and the silicon carbide nanowires prepared in Comparative Example 2. Enhanced compressive yield strength of titanium matrix composites; under the same preparation process conditions, the compressive yield strength of silicon carbide nanowires reinforced titanium matrix composites prepared by low-temperature sintering in Example 1 is higher than that of carbonized carbides prepared by high-temperature sintering in Comparative Example 2 The compressive yield strength of silicon nanowires reinforced titanium matrix composites indicates that spark plasma hot pressing sintering at low temperature and high pressure avoids the formation of carbides and silicides from silicon carbide nanowires and titanium in the high temperature environment of the conventional thermal sintering process. , to ensure the toughening effect of silicon carbide nanowires and improve the mechanical properties of silicon carbide nanowires reinforced titanium matrix composites; under the same spark plasma hot pressing sintering parameters, Example 1 uses silicon carbide nanowires as reinforcement The compressive yield strength of the titanium-based composite material prepared by phase preparation is higher than that of the titanium-based material prepared without silicon carbide nanowires in Comparative Example 1, indicating that under the action of spark plasma hot-pressing sintering, the silicon carbide nanowires are closely combined with the titanium matrix. , forming a multi-scale toughening structure, improving the toughening effect of silicon carbide nanowires, and improving the mechanical properties of silicon carbide nanowires reinforced titanium matrix composites.

以上所述，仅是本发明的较佳实施例，并非对本发明作任何限制。凡是根据发明技术实质对以上实施例所作的任何简单修改、变更以及等效变化，均仍属于本发明技术方案的保护范围内。The above descriptions are only preferred embodiments of the present invention, and do not limit the present invention in any way. Any simple modifications, changes and equivalent changes made to the above embodiments according to the technical essence of the invention still fall within the protection scope of the technical solutions of the present invention.

Claims (9)

Translated fromChinese

1.一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，该方法包括以下步骤：1. a method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature, is characterized in that, the method comprises the following steps:步骤一、将无水乙醇和正硅酸乙酯混合后搅拌均匀，然后加入蒸馏水和盐酸溶液并搅拌均匀，得到二氧化硅溶胶；所述无水乙醇、正硅酸乙酯、蒸馏水和盐酸溶液中盐酸的摩尔比为(3～5)：(0.5～2)：(3～8)：(0.1～0.5)；所述盐酸溶液的质量浓度为37％；Step 1. After mixing absolute ethanol and tetraethyl silicate, stir evenly, then add distilled water and hydrochloric acid solution and stir evenly to obtain silica sol; in the absolute ethanol, ethyl orthosilicate, distilled water and hydrochloric acid solution The molar ratio of hydrochloric acid is (3-5): (0.5-2): (3-8): (0.1-0.5); the mass concentration of the hydrochloric acid solution is 37%;步骤二、将粒度为60目～150目的石墨粉加入到步骤一中得到的二氧化硅溶胶中搅拌均匀，然后放置于烘箱中，在温度为100℃的条件下干燥12h～24h，得到包覆二氧化硅溶胶的石墨粉；Step 2: Add graphite powder with a particle size of 60 mesh to 150 mesh into the silica sol obtained in step 1 and stir evenly, then place it in an oven, and dry it at a temperature of 100 ° C for 12 h to 24 h to obtain a coating Graphite powder of silica sol;步骤三、将步骤二中得到的包覆二氧化硅溶胶的石墨粉放置于高温管式炉中进行碳热还原反应，然后经超声清洗和离心，去掉上清液，得到的沉淀物为碳化硅纳米线；所述碳热还原反应的具体过程为：在氩气保护气氛条件下，以5℃/min～10℃/min的速率升温至1400℃～1700℃后保温1h～3h；Step 3: Place the silica sol-coated graphite powder obtained in Step 2 in a high-temperature tubular furnace to carry out a carbothermic reduction reaction, then ultrasonically clean and centrifuge to remove the supernatant, and the obtained precipitate is silicon carbide. Nanowires; the specific process of the carbothermal reduction reaction is as follows: under the condition of an argon protective atmosphere, the temperature is raised to 1400°C to 1700°C at a rate of 5°C/min to 10°C/min, and then kept for 1h to 3h;步骤四、将步骤三中得到的碳化硅纳米线加入到无水乙醇中超声60min～120min，然后加入钛粉并在60℃～80℃的水浴锅保温条件下机械搅拌均匀，再经干燥得到碳化硅纳米线与钛粉的混合粉末；Step 4. Add the silicon carbide nanowires obtained in step 3 into absolute ethanol for 60min-120min, then add titanium powder and stir mechanically evenly under the heat preservation condition of a water bath at 60°C to 80°C, and then dry to obtain carbonization Mixed powder of silicon nanowires and titanium powder;步骤五、将步骤四中得到的碳化硅纳米线与钛粉的混合粉末装入模具中，然后放置于放电等离子热压烧结炉中进行放电等离子热压烧结，经冷却后得到碳化硅纳米线增强钛基复合材料；所述放电等离子热压烧结的工艺参数为：真空度1.0×10^-3Pa～3.0×10^-3Pa，温度600℃～900℃，压力40MPa～180MPa，保温时间5min～10min。Step 5. Put the mixed powder of silicon carbide nanowires and titanium powder obtained in step 4 into a mold, and then place it in a discharge plasma hot pressing sintering furnace for discharge plasma hot pressing sintering, and obtain silicon carbide nanowires after cooling. Titanium matrix composite material; the process parameters of the spark plasma hot pressing sintering are: vacuum degree 1.0 × 10^-3 Pa ~ 3.0 × 10^-3 Pa, temperature 600 ℃ ~ 900 ℃, pressure 40MPa ~ 180MPa, holding time 5min ~ 10min .2.根据权利要求1所述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤二中所述粒度为60目～150目的石墨粉与二氧化硅溶胶的质量比为1:5，所述搅拌均匀的时间为20min～60min。2. a kind of method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature according to claim 1, is characterized in that, the particle size described in step 2 is the quality of 60-mesh-150-mesh graphite powder and silica sol The ratio is 1:5, and the time for the uniform stirring is 20min-60min.3.根据权利要求1所述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤三中所述超声清洗和离心的次数均为两次，所述离心采用的转速为8000r/min～10000r/min。3. a kind of method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature according to claim 1, is characterized in that, the times of ultrasonic cleaning and centrifugation described in step 3 are both twice, the centrifugation adopts The rotating speed is 8000r/min～10000r/min.4.根据权利要求1所述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤三中得到的碳化硅纳米线的直径为50nm～200nm。4 . The method for preparing silicon carbide nanowire reinforced titanium-based composite material at low temperature according to claim 1 , wherein the silicon carbide nanowire obtained in step 3 has a diameter of 50 nm to 200 nm. 5 .5.根据权利要求1所述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤四中所述钛粉的粒度为15μm～45μm。5 . The method for preparing a silicon carbide nanowire reinforced titanium-based composite material at low temperature according to claim 1 , wherein the particle size of the titanium powder in step 4 is 15 μm˜45 μm. 6 .6.根据权利要求1所述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤四中所述机械搅拌均匀的时间为6h～12h。6 . The method for preparing a silicon carbide nanowire reinforced titanium-based composite material at a low temperature according to claim 1 , wherein the time for uniform mechanical stirring in step 4 is 6 h to 12 h. 7 .7.根据权利要求1所述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤四中所述干燥的温度为80℃～100℃，时间为8h～12h。7 . The method for preparing a silicon carbide nanowire reinforced titanium-based composite material at a low temperature according to claim 1 , wherein the drying temperature in step 4 is 80° C. to 100° C. and the time is 8 h to 12 h. 8 .8.根据权利要求1所述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤五中所述模具的直径为30mm～60mm。8 . The method for preparing a silicon carbide nanowire reinforced titanium-based composite material at low temperature according to claim 1 , wherein the diameter of the mold in step 5 is 30 mm to 60 mm. 9 .9.根据权利要求1所述的一种低温制备碳化硅纳米线增强钛基复合材料的方法，其特征在于，步骤五中所述碳化硅纳米线增强钛基复合材料中碳化硅纳米线的质量分数为0.01％～10％。9 . The method for preparing a silicon carbide nanowire reinforced titanium-based composite material at a low temperature according to claim 1 , wherein the quality of the silicon carbide nanowires in the silicon carbide nanowire-reinforced titanium-based composite material described in step 5 is the quality of the silicon carbide nanowires. 10 . The fraction is 0.01% to 10%.

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