CN107235729B - High-purity SiC pressure-sensitive ceramic - Google Patents

High-purity SiC pressure-sensitive ceramic Download PDF

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CN107235729B
CN107235729B CN201710355530.1A CN201710355530A CN107235729B CN 107235729 B CN107235729 B CN 107235729B CN 201710355530 A CN201710355530 A CN 201710355530A CN 107235729 B CN107235729 B CN 107235729B
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sensitive ceramic
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CN107235729A (en
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陈健
黄政仁
朱云洲
刘学建
陈忠明
姚秀敏
刘岩
袁明
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Shanghai Institute of Ceramics of CAS
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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • H01—ELECTRIC ELEMENTS
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    • H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
    • H01C7/105—Varistor cores
    • H01C7/118—Carbide, e.g. SiC type
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Abstract

The invention relates to a high-purity SiC voltage-sensitive ceramic, wherein the density of the SiC voltage-sensitive ceramic is 3.21 +/-0.01 gcm‑3And the voltammetry characteristic is kept unchanged within 20-100 ℃, and the preparation method of the SiC pressure sensitive ceramic comprises the following steps: placing SiC powder at the bottom of a graphite crucible body, and controlling the porosity of the powder to be 50-70%; heating to 1200-1400 ℃ in vacuum to remove impurities adsorbed by the SiC powder; introducing inert atmosphere, continuously heating to 2100-2300 ℃, and controlling the pressure to be 103～105Pa, controlling the temperature gradient along the height direction of the graphite crucible to be 2.5-4 ℃/cm, preserving the heat for 30-120 minutes, and growing the SiC pressure-sensitive ceramic on the inner surface of the top cover of the graphite crucible by adopting a physical vapor transport method.

Description

High-purity SiC pressure-sensitive ceramic
Technical Field
The invention relates to a high-density high-purity SiC ceramic pressure-sensitive ceramic and a preparation method thereof, belonging to the field of SiC ceramics.
Background
The varistor ceramic material is a semiconductor ceramic material which has nonlinear volt-ampere characteristics at a certain temperature and a certain voltage range and the resistance of which is sharply reduced along with the increase of voltage. According to the nonlinear volt-ampere characteristic, a nonlinear resistor, namely a piezoresistor, can be made of the semiconductor ceramic material. The piezoresistor has wide application, and can be used for spark suppression, overvoltage protection, lightning rod preparation, voltage stabilization and the like. Because the piezoresistor plays an important role in protecting equipment safety and ensuring normal and stable operation of the equipment, the piezoresistor is widely applied to the fields of aviation, aerospace, post and telecommunications, railways, automobiles, household appliances and the like, and numerous scholars at home and abroad also carry out extensive and deep research on piezoresistor ceramic materials. Although the ZnO piezoresistor is widely used, the SiC piezoresistor has the advantages that the performance is slightly inferior to the corresponding performance of a ZnO resistor element in the field of demagnetization speed, the SiC piezoresistor has obvious advantages in various integrated comprehensive performances such as reliable operation of the element, compact structure, small volume, large capacity, good timeliness, and the element can independently realize better current sharing and energy sharing characteristics, and the chemical stability and physical characteristics of the SiC ceramic such as corrosion resistance, irradiation resistance, thermal conductivity and the like are superior to those of the ZnO ceramic material. At present, only a few foreign companies such as M & I and the like produce SiC voltage-sensitive ceramic materials internationally, and demagnetization resistors used in a plurality of domestic large hydropower stations are all products from the M & I company, such as famous three gorges hydropower stations, two beaches hydropower stations and the like.
At present, the SiC ceramic can be dense only by adding a sintering aid, the most common SiC ceramics are solid phase sintered SiC ceramics added with a B-C system and liquid phase sintered SiC ceramics added with aluminum oxide and yttrium oxide, but the SiC ceramics added with the sintering aid has certain influence on the performance due to the existence of a grain boundary phase, and the stability of the electrical performance is difficult to ensure.
Disclosure of Invention
In order to solve the problems, the invention provides SiC voltage-sensitive ceramic. The density of the SiC voltage-sensitive ceramic is 3.21 +/-0.01 gcm-3And the voltammetry characteristic is kept unchanged within 20-100 ℃, and the preparation method of the SiC pressure sensitive ceramic comprises the following steps:
placing SiC powder at the bottom of a graphite crucible body, and controlling the porosity of the powder to be 50-70%;
heating to 1200-1400 ℃ in vacuum to remove impurities adsorbed by the SiC powder;
introducing inert atmosphere, continuously heating to 2100-2300 ℃, and controlling the pressure to be 103～105Pa, controlling the temperature gradient along the height direction of the graphite crucible to be 2.5-4 ℃/cm, preserving the heat for 30-60 minutes, and growing the SiC pressure-sensitive ceramic on the inner surface of the top cover of the graphite crucible by adopting a physical vapor transport method.
The invention adopts a PVT (physical vapor transport) method to prepare the high-density SiC voltage-sensitive ceramic. The PVT method (as shown in fig. 1) mainly consists in: a certain amount of SiC powder is put at the bottom of the graphite crucible, the graphite crucible is heated under a certain air pressure condition, so that the internal temperature field of the graphite crucible reaches a certain requirement (2100-2300 ℃), the powder at the bottom of the graphite crucible is decomposed at high temperature to generate gas components for crystal growth, and finally the gas components are conveyed to the top surface of the crucible under the action of temperature gradient and are deposited to grow to obtain SiC ceramic. When crystals grow in the SiC ceramic, the temperature in the crucible is gradually reduced from powder to polycrystal to form a certain temperature gradient, and due to the existence of the temperature gradient, the concentration of gas molecules in the crucible from a source to a seed crystal is different, namely the concentration gradient is determined by the temperature gradient. The temperature gradient and the small fluctuation of the concentration gradient are one of the main causes of defect formation, and when the temperature and the concentration of the polycrystal are different, the grown crystal generates defects such as micropipes, dislocations, inclusions and the like. The distance between the polycrystal and the powder is reduced, the SiC polycrystal grows under the condition of approaching the equilibrium state, the probability of temperature and concentration gradient fluctuation can be reduced, and the quality of the SiC ceramic is improved. The SiC ceramic obtained by the method has high purity, the density is close to the theoretical density of SiC crystals, and the intrinsic physical and chemical properties of SiC are maintained.
Preferably, the inert atmosphere is at least one of Ar gas and He gas.
Preferably, the particle size of the SiC powder is 0.1 to 1 μm.
Preferably, the purity of the SiC powder is 99.9 wt%.
Preferably, the vacuum degree of the vacuum is less than or equal to 10-3Pa。
The high-density high-purity SiC voltage-sensitive resistor ceramic material prepared by the invention has lower voltage-sensitive voltage, better voltage-resistant stability along with the change of temperature, constant volt-ampere characteristic in a certain temperature range and 1mAcm of current density-2Voltage dependent voltage U1mAIs more than or equal to 0.6Vmm-1The nonlinear coefficient is more than or equal to 2, and the method can be used in the field of high-temperature microelectronics.
Drawings
FIG. 1 is a schematic diagram of preparing high-purity high-density SiC ceramic by a PVT method;
FIG. 2 is a photograph of the microstructure of a highly dense and highly pure SiC ceramic obtained by the PVT method;
FIG. 3 is a voltage-current characteristic curve of high-purity SiC voltage-sensitive ceramic under different temperatures.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
The invention prepares the high-density high-purity SiC pressure-sensitive ceramic by a PVT method, wherein the purity of SiC powder is up to 99.9 percent, and the density of the SiC ceramic is 3.21 +/-0.01 gcm-3The relative density is close to 100 percent, the volt-ampere characteristic is kept unchanged within 20-100 ℃, and the current density is 1mAcm-2Voltage dependent voltage U1mA≥0.6Vmm-1The nonlinear coefficient is more than or equal to 2.
The following is an exemplary description of the preparation method of the SiC pressure sensitive ceramic provided by the present invention, as shown in fig. 1.
Placing SiC powder in a graphite crucible body, covering a graphite crucible top cover, placing the graphite crucible top cover in a growth furnace, and heating to 1200-1400 ℃ in vacuum to remove impurities adsorbed by the SiC powder. The SiC powder can also be placed in a crucible (graphite crucible) and compacted before, and the porosity can be kept between 50 and 70 percent. The vacuum degree of the vacuum is less than or equal to 10-3Pa. As an example, SiC powder is put at the bottom of a graphite crucible of a medium-frequency induction high-temperature sintering furnace, and the porosity of the powder after compaction is 50-70%. The furnace is vacuumized, and the vacuum degree is controlled to be 10-3Heating graphite crucible to 1200 deg.C below Pa, and removing impurities adsorbed by SiC powder at high temperatureAnd (4) quality. The SiC powder with the average particle size of 0.1-1 micron is selected as the raw material, and the purity of the powder is more than 99.9%.
And after removing impurities, introducing inert atmosphere, and continuously heating to 2100-2300 ℃ so that the bottom and/or the lower part of the graphite crucible body is/are positioned in the heating zone to ensure that the temperature of the bottom of the graphite crucible body is higher than that of the top cover of the graphite crucible, and growing the SiC pressure sensitive ceramic by adopting a physical vapor transport method. The temperature gradient in the height direction of the graphite crucible is controlled to be 2.5-4.0 ℃/mm, namely, the temperature gradient from the top cover of the graphite crucible to the bottom of the graphite crucible body can be 2.5-4 ℃/cm. In the SiC pressure sensitive ceramic growth process, the growth time can be 30-120 minutes. The inert atmosphere may be at least one of Ar gas and He gas. The inert atmosphere may have a pressure of 103～105Pa. As an example, high-purity Ar gas is introduced, and the gas pressure is controlled to be 103～105Pa, the temperature of the furnace is raised to 2200 ℃, and the temperature gradient in the height direction of the crucible is controlled to be 2.5-4.0 ℃/mm.
The preparation method of the high-density high-purity SiC pressure-sensitive ceramic comprises the following steps: high-purity SiC powder is used as a raw material. The raw materials are placed at the bottom of a graphite crucible of a medium-frequency induction high-temperature sintering furnace, and the porosity is 50-70%. And vacuumizing the furnace, heating the graphite crucible to a certain temperature of 1200 ℃, and removing impurities adsorbed by the SiC powder at a high temperature. Introducing high-purity Ar gas, and controlling the gas pressure within a certain range (the gas pressure is 10)3-105Pa), the temperature of the furnace is raised to 2200 ℃, and the temperature gradient in the height direction of the crucible is controlled to be 2.5-4.0 ℃/mm. The particle size of the SiC powder is 0.1-1 mu m. The purity of the SiC powder is 99.9 wt%. The vacuum degree is less than or equal to 10-3Pa。
The density of the SiC ceramic prepared by the invention is 3.21 +/-0.01 gcm-3The relative density approaches 100%. Voltage-dependent voltage U with constant voltage-current characteristics at different temperatures1mA(Current Density 1mAcm-2)≥0.6Vmm-1The nonlinear coefficient is more than or equal to 2. The prepared SiC voltage-sensitive ceramic has lower voltage-sensitive voltage and better stability, and can be used in the field of high-temperature microelectronics.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
Selecting high-purity SiC powder with the average particle size of 0.5 micron and the purity of 99.9 percent, putting the SiC powder at the bottom of a graphite crucible of a medium-frequency induction graphite furnace, wherein the porosity of the powder is 0.6; the furnace is vacuumized, and the vacuum degree is controlled to be 10-3Heating the graphite crucible to 1200 ℃ below Pa, and removing impurities adsorbed by the SiC powder at high temperature; introducing high-purity Ar gas, and controlling the gas pressure at 103Pa, heating the furnace to 2200 ℃, and controlling the temperature gradient of the height of the furnace at 2.5 ℃/mm; the heat preservation time is 30min, and SiC ceramic is obtained, wherein the density of the SiC ceramic is 3.21g/cm3The microstructure is shown in FIG. 2, and the grain size of the SiC ceramic is shown in FIG. 2. Processing the obtained SiC ceramic into a wafer with the thickness of 10mm phi and the thickness of 2mm, grinding two ends of the wafer, uniformly coating silver paste electrodes on the two ends of the wafer, then, preserving the temperature of the wafer in a muffle furnace at 750 ℃ for 30min, and testing the volt-ampere characteristics of the obtained SiC ceramic wafer at different temperatures by a Keithley2450 multi-channel testing system (as shown in figure 3), wherein the voltage-dependent voltage U of the wafer is1mA＝1.6Vmm-1the nonlinear coefficient α remains unchanged at 2.34.
Example 2
Selecting high-purity SiC powder with the average particle size of 0.5 micron and the purity of 99.9 percent, putting the SiC powder at the bottom of a graphite crucible of a medium-frequency induction graphite furnace, wherein the porosity of the powder is 0.6; the furnace is vacuumized, and the vacuum degree is controlled to be 10-3Heating the graphite crucible to 1200 ℃ below Pa, and removing impurities adsorbed by the SiC powder at high temperature; introducing high-purity Ar gas, and controlling the gas pressure at 103Pa, heating the furnace to 2200 ℃, and controlling the temperature gradient of the height of the furnace at 3 DEG CPer mm; the heat preservation time is 30min, and SiC ceramic is obtained, wherein the density of the SiC ceramic is 3.20g/cm3. Processing the obtained SiC ceramic into a wafer with the thickness of 10mm phi and the thickness of 2mm, grinding two ends of the wafer, uniformly coating silver paste electrodes on the two ends of the wafer, then, preserving the temperature of the wafer in a muffle furnace at 750 ℃ for 30min, and testing the volt-ampere characteristics of the obtained SiC ceramic wafer at different temperatures by a Keithley2450 multi-channel testing system, wherein the voltage-dependent voltage U of the wafer is1mA＝1.55Vmm-1the nonlinear coefficient α remains unchanged at 2.20.
Example 3
Selecting high-purity SiC powder with the average particle size of 0.5 micron and the purity of 99.9 percent, putting the SiC powder at the bottom of a graphite crucible of a medium-frequency induction graphite furnace, wherein the porosity of the powder is 0.6; the furnace is vacuumized, and the vacuum degree is controlled to be 10-3Heating the graphite crucible to 1200 ℃ below Pa, and removing impurities adsorbed by the SiC powder at high temperature; introducing high-purity Ar gas, and controlling the gas pressure at 103Pa, heating the furnace to 2300 ℃, and controlling the temperature gradient of the height of the furnace at 2.5 ℃/mm; the heat preservation time is 120min, and SiC ceramic is obtained, wherein the density of the SiC ceramic is 3.21g/cm3. Processing the obtained SiC ceramic into a wafer with the thickness of 10mm phi and the thickness of 2mm, grinding two ends of the wafer, uniformly coating silver paste electrodes on the two ends of the wafer, then, preserving the temperature of the wafer in a muffle furnace at 750 ℃ for 30min, and testing the volt-ampere characteristics of the obtained SiC ceramic wafer at different temperatures by a Keithley2450 multi-channel testing system, wherein the voltage-dependent voltage U of the wafer is1mA＝0.6Vmm-1the nonlinear coefficient α remains unchanged at 3.21.

Claims (3)

1. The SiC voltage-sensitive ceramic is characterized in that the density of the SiC voltage-sensitive ceramic is 3.21 +/-0.01 gcm-3And the voltammetry characteristic is kept unchanged within 20-100 ℃, and the preparation method of the SiC pressure sensitive ceramic comprises the following steps:
placing SiC powder at the bottom of a graphite crucible body, controlling the porosity of the powder to be 50-70%, wherein the particle size of the SiC powder is 0.1-1 mu m, and the purity of the SiC powder is more than or equal to 99.9 wt%;
heating to 1200-1400 ℃ in vacuum to remove impurities adsorbed by the SiC powder;
let in inert gasContinuously raising the temperature to 2100-2200 ℃ under the atmosphere of sexual atmosphere, and controlling the pressure to be 103～105Pa, controlling the temperature gradient along the height direction of the graphite crucible to be 2.5-4 ℃/cm, preserving the heat for 30-120 minutes, and growing the SiC pressure-sensitive ceramic on the inner surface of the top cover of the graphite crucible by adopting a physical vapor transport method;
the SiC voltage-sensitive ceramic has a current density of 1mAcm-2Voltage dependent voltage U1mA≥1.55Vmm-1The nonlinear coefficient is more than or equal to 2.
2. The SiC pressure sensitive ceramic of claim 1, wherein the inert atmosphere is at least one of Ar gas and He gas.
3. The SiC voltage-sensitive ceramic of claim 1 or 2, wherein the vacuum degree of the vacuum is less than or equal to 10-3Pa。
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CN105565813A (en) * 2015-12-22 2016-05-11 中国科学院上海硅酸盐研究所 Silicon carbide low-voltage-sensitive ceramic and solid-phase sintering preparation method thereof
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