CN105645987B - A kind of method of electric field-assisted low temperature Fast Sintering porous ceramics - Google Patents
A kind of method of electric field-assisted low temperature Fast Sintering porous ceramics Download PDFInfo
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Abstract
Description
技术领域technical field
本发明属于多孔陶瓷材料制备技术领域，具体涉及一种电场辅助低温快速烧结多孔陶瓷的方法。The invention belongs to the technical field of porous ceramic material preparation, and in particular relates to a method for electric field-assisted low-temperature rapid sintering of porous ceramics.
背景技术Background technique
多孔陶瓷材料是指在成型与烧结过程中形成大量孔洞的无机非金属材料。多孔陶瓷含有很多相互连接紧密的气孔，按照孔的结构可以分为闭气孔型、开气孔型和贯通气孔型三大类。多孔陶瓷具有热导率低、气孔率高、高温稳定性好、物理化学稳定性等优异性能，已经普遍应用于能源化工、过滤分离、催化剂载体、隔热保温和航空航天等领域。Porous ceramic materials refer to inorganic non-metallic materials that form a large number of pores during the molding and sintering process. Porous ceramics contain many pores that are closely connected to each other. According to the structure of the pores, they can be divided into three categories: closed pores, open pores and through pores. Porous ceramics have excellent properties such as low thermal conductivity, high porosity, good high temperature stability, and physical and chemical stability.
多孔陶瓷的应用是以高气孔率为基础的，当提高陶瓷的气孔率时，可获得优异的多孔性能，但是强度的降低会限制它的应用。因此，在高强度和高气孔率之间如何选择来保证陶瓷的性能，将很大程度上影响着多孔陶瓷的应用。常用的方法有很多，比如改变生坯的制备工艺，调节陶瓷颗粒的尺寸和孔径的大小等方法，如在专利CN103588482A中公布了一种通过发泡法注凝工艺制备高气孔率及高强度钇硅氧多孔陶瓷的方法，最后在1500℃～1550℃下进行1.5～2.5小时的高温反应烧结；在专利CN104130004A中公布了一种高强度块状多孔氧化铝纳米陶瓷的制备方法，成型后的坯体在800℃～1000℃下保温2小时烧结。在专利US19884777153A中公开了一种通过控制孔的微观结构制备多孔陶瓷的方法，通过调节孔径大小和孔的分布，在1300℃～1500℃下烧结成型，能提高陶瓷的强度。以上提及的高强度或高气孔率的多孔陶瓷制备方法，有一个共同的特点，即高温长时间烧结多孔陶瓷。The application of porous ceramics is based on high porosity. When the porosity of ceramics is increased, excellent porous performance can be obtained, but the reduction of strength will limit its application. Therefore, how to choose between high strength and high porosity to ensure the performance of ceramics will greatly affect the application of porous ceramics. There are many commonly used methods, such as changing the preparation process of the green body, adjusting the size of the ceramic particles and the size of the aperture, etc., such as the patent CN103588482A, which discloses a method of preparing high-porosity and high-strength yttrium by foaming and pouring technology. The method of silicon-oxygen porous ceramics, and finally high-temperature reaction sintering at 1500 ° C to 1550 ° C for 1.5 to 2.5 hours; in the patent CN104130004A, a preparation method of high-strength block porous alumina nano-ceramics is disclosed. The body is sintered at 800°C to 1000°C for 2 hours. Patent US19884777153A discloses a method of preparing porous ceramics by controlling the microstructure of pores. By adjusting the pore size and distribution of pores, sintering at 1300°C to 1500°C can improve the strength of ceramics. The above-mentioned preparation methods of high-strength or high-porosity porous ceramics have a common feature, that is, sintering porous ceramics at high temperature for a long time.
然而，陶瓷的烧结是一个持续的致密化过程，在传统的烧结方法中，烧结温度越高，烧结时间越长，其致密化程度越大，机械性能越好，但是会面临一个严峻的问题，即降低气孔率，影响多孔陶瓷的性能。如何控制陶瓷的烧结过程，降低烧结温度，大大缩短烧结时间，实现低温快速烧结，获得高强度高气孔率的多孔陶瓷，这在拓展多孔陶瓷的应用领域方面显得尤为重要。However, the sintering of ceramics is a continuous densification process. In the traditional sintering method, the higher the sintering temperature and the longer the sintering time, the greater the degree of densification and the better the mechanical properties, but it will face a serious problem, That is to reduce the porosity and affect the performance of porous ceramics. How to control the sintering process of ceramics, reduce the sintering temperature, greatly shorten the sintering time, realize low-temperature rapid sintering, and obtain porous ceramics with high strength and high porosity is particularly important in expanding the application field of porous ceramics.
发明内容Contents of the invention
要解决的技术问题technical problem to be solved
为了避免现有技术的不足之处，本发明提出一种电场辅助低温快速烧结多孔陶瓷的方法，采用的方法是电场辅助烧结，根据不同材质的多孔陶瓷坯体，可选择不同的电场条件。解决的技术问题是如何低温快速烧结多孔陶瓷并使其具有较高强度和较高气孔率。In order to avoid the deficiencies of the prior art, the present invention proposes a method for electric field-assisted low-temperature rapid sintering of porous ceramics. The method adopted is electric field-assisted sintering, and different electric field conditions can be selected according to the porous ceramic bodies of different materials. The technical problem solved is how to quickly sinter porous ceramics at low temperature and make them have higher strength and higher porosity.
技术方案Technical solutions
一种电场辅助低温快速烧结多孔陶瓷的方法，其特征在于步骤如下：A method for electric field-assisted low-temperature rapid sintering of porous ceramics, characterized in that the steps are as follows:
步骤1：将含有气孔的陶瓷坯体加热到临界温度；所述临界温度为在施加电场强度的条件下恰好发生快速烧结的温度；Step 1: heating the ceramic green body containing pores to a critical temperature; the critical temperature is the temperature at which rapid sintering occurs under the condition of an applied electric field strength;
步骤2：对陶瓷坯体施加一个电流形成临界电场，并且持续≥10s，小于20min的时间完成多孔陶瓷的烧结；所述临界电场是能发生快速烧结的电场强度。Step 2: Apply a current to the ceramic body to form a critical electric field, and last for ≥10s, less than 20 minutes to complete the sintering of the porous ceramic; the critical electric field is the electric field strength that can cause rapid sintering.
所述含有气孔的陶瓷坯体的气孔率为70％～90％。The porosity of the ceramic body containing pores is 70%-90%.
所述临界温度T为：300℃≤T≤1200℃。The critical temperature T is: 300°C≤T≤1200°C.
所述电场强度E为：5V/cm≤E≤500V/cm。The electric field strength E is: 5V/cm≤E≤500V/cm.
所述施加电流密度J为：5mA/mm2≤J≤1A/mm2。The applied current density J is: 5mA/mm 2 ≤J≤1A/mm 2 .
有益效果Beneficial effect
本发明提出的一种电场辅助低温快速烧结多孔陶瓷的方法，将多孔陶瓷坯体升温至合适的温度，然后加上合适的电场强度，可实现陶瓷的快速烧结。可以根据不同的多孔陶瓷材料选择不同的电场强度条件。电场能激发物质的传输过程，提高粒子活度和扩散迁移速率，使陶瓷颗粒迅速烧结，能有效的降低烧结温度和烧结时间。这种电场辅助低温快速烧结的方法能获得高强度和高气孔率的多孔陶瓷。The invention proposes a method for electric-field-assisted low-temperature rapid sintering of porous ceramics. The porous ceramic body is heated to a suitable temperature, and then a suitable electric field is applied to realize rapid sintering of the ceramics. Different electric field strength conditions can be selected according to different porous ceramic materials. The electric field can stimulate the material transport process, increase the particle activity and diffusion migration rate, make the ceramic particles sinter rapidly, and effectively reduce the sintering temperature and sintering time. This electric field-assisted low-temperature rapid sintering method can obtain porous ceramics with high strength and high porosity.
本发明中，由于(1)在外电场的作用下，电场的焦耳热和质量传输效应，提高了粒子活度和扩散迁移速率，加快了反应进程，提高了反应速度。(2)临界电场恰好能激发物质的传输过程，使陶瓷颗粒迅速烧结，但又不会因电场强度过高导致粒子的扩散速率过快。该方法在保证多孔陶瓷气孔率的前提下，能有效地提高其强度，适用于氧化锆、氧化铝及其复合材料等离子化合物材料。In the present invention, due to (1) under the action of an external electric field, the Joule heat and mass transport effect of the electric field improve the particle activity and diffusion migration rate, accelerate the reaction process, and increase the reaction speed. (2) The critical electric field can just excite the transport process of the material, so that the ceramic particles can be sintered rapidly, but the diffusion rate of the particles will not be too fast due to the high electric field strength. The method can effectively improve the strength of the porous ceramics under the premise of ensuring the porosity of the porous ceramics, and is suitable for plasma compound materials such as zirconia, alumina and their composite materials.
附图说明Description of drawings
图1为实例1所制备的氧化锆多孔陶瓷截面高倍显微照片；Fig. 1 is the high power photomicrograph of the zirconia porous ceramic section prepared by example 1;
图2为实例2所制备的氧化锆多孔陶瓷截面高倍显微照片；Fig. 2 is the high power photomicrograph of the zirconia porous ceramic section prepared by example 2;
图3为实例3所制备的氧化锆多孔陶瓷截面高倍显微照片；Fig. 3 is the high magnification photomicrograph of the zirconia porous ceramic section prepared by example 3;
图4为实例4所制备的氧化锆多孔陶瓷截面高倍显微照片；Fig. 4 is the high magnification photomicrograph of the zirconia porous ceramic section prepared by example 4;
图5为实例5所制备的氧化锆多孔陶瓷截面高倍显微照片。Fig. 5 is a high-magnification photomicrograph of the cross-section of the zirconia porous ceramic prepared in Example 5.
具体实施方式Detailed ways
现结合实施例、附图对本发明作进一步描述：Now in conjunction with embodiment, accompanying drawing, the present invention will be further described:
实施例1Example 1
1)将气孔率为70％～90％的多孔陶瓷坯体以5℃/min的升温速率加热至1000℃；1) heating the porous ceramic body with a porosity of 70% to 90% to 1000°C at a heating rate of 5°C/min;
2)给已经加热至1000℃的多孔陶瓷坯体加上电场强度5V/cm，当电源供给状态从恒压态跳转成恒流态时，调节电流密度为80mA/mm2，计时10s后跳转至降温程序，以5℃/min降至室温，即得到气孔率为80％，压缩强度为9MPa的氧化锆多孔陶瓷。2) Add an electric field strength of 5V/cm to the porous ceramic body that has been heated to 1000°C. When the power supply state jumps from a constant voltage state to a constant current state, adjust the current density to 80mA/mm 2 and jump after 10s Switch to the cooling program and cool down to room temperature at 5° C./min to obtain a zirconia porous ceramic with a porosity of 80% and a compressive strength of 9 MPa.
实施例2Example 2
1)将气孔率为70％～90％的多孔陶瓷坯体以5℃/min的升温速率升至1000℃；1) Raise the porous ceramic body with a porosity of 70% to 90% to 1000°C at a heating rate of 5°C/min;
2)给已经加热至1000℃的多孔陶瓷坯体加上电场强度5V/cm，当电源供给状态从恒压态跳转成恒流态时，调节电流密度为80mA/mm2，计时30s后跳转至降温程序，以5℃/min降至室温，即得到气孔率为79％，压缩强度为9.5MPa的氧化锆多孔陶瓷。2) Add an electric field strength of 5V/cm to the porous ceramic body that has been heated to 1000°C. When the power supply state jumps from a constant voltage state to a constant current state, adjust the current density to 80mA/mm 2 , and jump after 30s Turn to the cooling program and cool down to room temperature at 5° C./min to obtain a zirconia porous ceramic with a porosity of 79% and a compressive strength of 9.5 MPa.
实施例3Example 3
1)将气孔率为70％～90％的多孔陶瓷坯体以5℃/min的升温速率升至950℃；1) Raise the porous ceramic body with a porosity of 70% to 90% to 950°C at a heating rate of 5°C/min;
2)给已经加热至950℃的多孔陶瓷坯体加上电场强度200V/cm，当电源供给状态从恒压态跳转成恒流态时，调节电流密度为500mA/mm2，计时30s后跳转至降温程序，以5℃/min降至室温，即得到气孔率为85％，压缩强度为7MPa的氧化锆多孔陶瓷。2) Apply an electric field strength of 200V/cm to the porous ceramic body that has been heated to 950°C. When the power supply state jumps from a constant voltage state to a constant current state, adjust the current density to 500mA/mm 2 and jump after 30s Turn to the cooling program and cool down to room temperature at 5° C./min to obtain a porous zirconia ceramic with a porosity of 85% and a compressive strength of 7 MPa.
实施例4Example 4
1)将气孔率为70％～90％的多孔陶瓷坯体以5℃/min的升温速率升至900℃；1) raising the porous ceramic body with a porosity of 70% to 90% to 900°C at a heating rate of 5°C/min;
2)给已经加热至900℃的多孔陶瓷坯体加上电场强度300V/cm，当电源供给状态从恒压态跳转成恒流态时，调节电流密度为200mA/mm2，计时30s后跳转至降温程序，以5℃/min降至室温，即得到气孔率为78％，压缩强度为12MPa的氧化锆多孔陶瓷。2) Apply an electric field strength of 300V/cm to the porous ceramic body that has been heated to 900°C. When the power supply state jumps from a constant voltage state to a constant current state, adjust the current density to 200mA/mm 2 and jump after 30s Switch to the cooling program and cool down to room temperature at 5° C./min to obtain a zirconia porous ceramic with a porosity of 78% and a compressive strength of 12 MPa.
实施例5Example 5
1)将气孔率为70％～90％的多孔陶瓷坯体以5℃/min的升温速率升至850℃；1) Raise the porous ceramic body with a porosity of 70% to 90% to 850°C at a heating rate of 5°C/min;
2)给已经加热至850℃的多孔陶瓷坯体加上电场强度500V/cm，当电源供给状态从恒压态跳转成恒流态时，调节电流密度为5mA/mm2，计时30s后跳转至降温程序，以5℃/min降至室温，即得到气孔率为75％，压缩强度为15MPa的氧化锆多孔陶瓷。2) Apply an electric field strength of 500V/cm to the porous ceramic body that has been heated to 850°C. When the power supply state jumps from a constant voltage state to a constant current state, adjust the current density to 5mA/mm 2 and jump after 30s Switch to the cooling program and cool down to room temperature at 5° C./min to obtain a zirconia porous ceramic with a porosity of 75% and a compressive strength of 15 MPa.
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