CN115448729A - BN-ZrO 2 Microwave sintering method of-SiC complex phase ceramic - Google Patents
BN-ZrO 2 Microwave sintering method of-SiC complex phase ceramic Download PDFInfo
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Abstract
The invention discloses BN-ZrO 2 A microwave sintering method of-SiC complex phase ceramic, belonging to the field of ceramic microwave sintering. The microwave sintering method comprises the following steps: 1) Mixing boron nitride powder, zirconia powder and silicon carbide powder, performing ball milling, and sieving to obtain mixed powder; 2) Mixing the mixed powder and the sintering aid, performing dry pressing preforming, and performing cold isostatic pressing preforming on a blank body subjected to dry pressing preforming to obtain a green body; 3) Microwave heating the green body to prepare BN-ZrO 2 -SiC complex phase ceramics. The method is characterized in that the densification of the ceramic can be effectively promoted by utilizing the microwave plasma effect and the electric field-driven atomic diffusion mechanism in the microwave heating process, the zirconium diboride generated in situ has excellent performance and uniform distribution, and the ceramic can be greatly improvedProperties of the porcelain article.
Description
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to BN-ZrO 2 A microwave sintering method of-SiC complex phase ceramics.
Background
The thin strip continuous casting production technology is a revolutionary short process flow in the field of industrial production of steel strips. The thin strip continuous casting technology is adopted, so that the production process is greatly simplified, the production period is shortened, and the equipment investment is reduced. Compared with the traditional process, the method can reduce the engineering investment by 75-90 percent, reduce the production cost by 20-30 percent, improve the yield, save energy, reduce consumption, reduce environmental pollution and reduce harmful gases (such as CO) 2 、NO x 、SO 2 ) 70 to 90 percent of the discharge amount and the like. The side sealing technology is one of the most critical technologies in the twin-roll thin strip continuous casting technology, is a key factor influencing the quality and the process stability of a cast strip in the thin strip continuous casting process, and finally determines whether the thin strip continuous casting technology can be applied to industrial production on a large scale. The side seal is a leakage-proof device added at two ends of the casting rolls for forming a liquid metal molten pool between the two casting rolls, and plays roles of restraining metal liquid, promoting thin strip forming, ensuring thin strip edge quality and the like.
The solid side sealing technology is the most mature side sealing technology which is closest to actual production at present, and is vigorously researched and developed by various industry strong countries in the world. The device of the core in the solid side seal is a side seal plate prepared from an inorganic non-metallic material, the research key of the solid side seal technology lies in the material of the side seal plate, the material of the side seal plate is required to have good thermal shock resistance, excellent high-temperature mechanical property, good molten steel erosion resistance and heat insulation performance, and the side seal plate is required to have proper wear resistance so as to ensure good dynamic sealing performance between the side seal plate and a crystallization roller. Therefore, the research of the side sealing plate plays an important role in promoting the thin strip steel continuous casting process.
BN-ZrO 2 the-SiC complex phase ceramic takes h-BN as a matrix and zirconium oxide and silicon carbide as mechanical reinforcing phases, has the performances of high wear resistance, good erosion resistance, good thermal shock resistance and the like, and is widely applied as a side sealing plate for thin strip continuous casting. At present, BN-ZrO 2 The densification of the-SiC complex phase ceramic mainly depends on high-temperature hot-pressing sintering, the high-temperature hot-pressing period is long, the efficiency is low, the energy consumption is high, and a hot-pressing die is expensive and easy to damage, so a new sintering mode needs to be explored.
Disclosure of Invention
The invention aims to provide BN-ZrO 2 Microwave sintering method of-SiC complex phase ceramic, capable of realizing BN-ZrO under non-pressure condition 2 The densification of the-SiC complex phase ceramic solves the problems of long period, low efficiency, high energy consumption and expensive and easily damaged hot-pressing die in the high-temperature hot-pressing sintering process of the traditional high-temperature hot-pressing sintering process.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides BN-ZrO 2 The microwave sintering method of the-SiC complex phase ceramic comprises the following steps:
1) Mixing boron nitride powder, zirconia powder and silicon carbide powder, performing ball milling, and sieving to obtain mixed powder;
2) Mixing the mixed powder and the sintering aid, performing dry pressing preforming, and performing cold isostatic pressing preforming on a blank body subjected to dry pressing preforming to obtain a green body;
3) Microwave heating the green body to prepare BN-ZrO 2 -SiC complex phase ceramics.
Preferably, the boron nitride powder, the zirconia powder and the silicon carbide powder are all micro-nano-scale; the mass ratio of the boron nitride powder, the zirconia powder and the silicon carbide powder is 40-80: 20 to 40:5 to 20.
Preferably, the ball milling conditions in the step 1) are that the ball-to-material ratio is 0.5 to 1 to 2:1, the rotating speed is 100 to 300r/min, and the mixing time is 60 to 120min.
Preferably, the sintering aid in the step 2) is Al 2 O 3 And Y 2 O 3 Mixture of (1), al 2 O 3 And Y 2 O 3 The mass ratio of (A) to (B) is 0.5-2: 1, the addition amount is 1-5% of the mass of the mixed powder.
Preferably, the pressure of the dry-pressing preforming in the step 2) is 50-80 MPa, and the pressure maintaining time is 1-3 min; the pressure of the cold isostatic pressing preforming is 150-300 MPa, and the pressure maintaining time is 30-60 s.
Preferably, the frequency of the microwave heating is 2.45GHz or 9.15GHz, and the output power is 2-15 KW.
Preferably, the microwave heating conditions in step 3) are as follows: when the temperature is less than or equal to 600 ℃, the power is increased by 1KW every 5-10 min; when the temperature is higher than 600 ℃, adjusting the heating rate to 10-20 ℃/min, heating to 1200-1600 ℃, and preserving the heat for 10-60 min.
Preferably, the green body is placed in a heat-insulating structure for microwave heating; after the green body is placed into the heat-insulating structure, the calcined alumina powder covers the green body, and the graphite covers the alumina powder.
Preferably, the heat preservation structure consists of a multi-layer structure, and the heat preservation structure sequentially comprises an alumina hollow sphere layer, a light mullite sheet layer, a polycrystalline mullite fiber cotton layer, a light mullite sheet layer and an alumina sagger layer from inside to outside.
Another object of the present invention is to provide BN-ZrO prepared by the microwave sintering method 2 ZrB generated in situ in-SiC complex phase ceramic 2 And (3) powder.
Compared with the prior art, the invention has the following beneficial effects:
microwave heating of BN-ZrO 2 In the process of the SiC complex phase ceramic, the high-temperature conductivity of the silicon carbide and the zirconium oxide is increased, the local electric field is enhanced, the microwave plasma is induced, the product is rapidly heated, the sintering temperature can be effectively reduced, and an electric field drives an atomic diffusion mechanism, so that the densification process of the ceramic can be effectively promoted, and the densification of the complex phase ceramic under the non-pressure condition is realized; in addition, in the microwave sintering process, zirconium diboride powder is generated in situ and used as a reinforcing phase, so that the performance of the ceramic product can be obviously improved, and the uniformity of the dispersion of the zirconium diboride powder in the ceramic product can be obviously improved by adopting a microwave in-situ introduction mode.
Drawings
FIG. 1 is an XRD pattern of a sintered sample of example 1;
FIG. 2 is an SEM photograph of a sintered sample of example 1.
Detailed Description
The invention provides BN-ZrO 2 The microwave sintering method of the-SiC complex phase ceramic comprises the following steps:
1) Mixing boron nitride powder, zirconia powder and silicon carbide powder, performing ball milling, and sieving to obtain mixed powder;
2) Mixing the mixed powder and the sintering aid, performing dry pressing preforming, and performing cold isostatic pressing preforming on a blank body subjected to dry pressing preforming to obtain a green body;
3) Microwave heating the green body to prepare BN-ZrO 2 -SiC complex phase ceramics.
In the invention, the boron nitride powder, the zirconia powder and the silicon carbide powder are all in micro-nanometer level; the mass ratio of the boron nitride powder, the zirconia powder and the silicon carbide powder is preferably 40 to 80:20 to 40:5 to 20, more preferably 45 to 75:25 to 35:5 to 15, more preferably 50 to 60:25 to 30:10 to 15.
In the present invention, the ball milling conditions in step 1) are that the ball-to-feed ratio is preferably 0.5 to 2:1, more preferably 0.8 to 1.5, and even more preferably 1:1 to 1.2; the ball milling rotating speed is preferably 100-300 r/min, more preferably 150-250 r/min, and more preferably 180-220 r/min; the mixing time is preferably 60 to 120min, more preferably 70 to 110min, and still more preferably 80 to 100min.
In the present invention, in the sieving process, the sieve is preferably 60 mesh, 70 mesh or 80 mesh.
In the invention, the sintering agent in the step 2) is Al 2 O 3 And Y 2 O 3 Mixture of (2), al 2 O 3 And Y 2 O 3 The mass ratio of (a) is preferably 0.5 to 2:1, more preferably 0.8 to 1.5, and still more preferably 1:1; the amount of addition is preferably 1 to 5%, more preferably 2 to 4%, and still more preferably 3% of the mass of the mixed powder.
In the present invention, the pressure of the dry-pressing preforming in step 2) is preferably 50 to 80MPa, more preferably 55 to 75MPa, and still more preferably 60 to 70MPa; the pressure maintaining time is preferably 1 to 3min, more preferably 1.5 to 2.5min, and still more preferably 2 to 2.5min; the pressure of the cold isostatic pressing preforming is preferably 150 to 300MPa, more preferably 180 to 270MPa, and more preferably 200 to 250MPa; the dwell time is preferably 30 to 60 seconds, more preferably 35 to 55 seconds, and still more preferably 40 to 50 seconds.
In the present invention, the frequency of the microwave heating is preferably 2.45GHz or 9.15GHz; the output power is preferably 2 to 15KW, more preferably 4 to 12KW, and still more preferably 5 to 10KW.
In the present invention, the microwave heating conditions in step 3) are as follows:
when the temperature is less than or equal to 600 ℃, the power is increased by 1KW every 5min;
when the temperature is higher than 600 ℃, adjusting the heating rate, preferably 10-20 ℃/min, more preferably 12-18 ℃/min, and more preferably 14-16 ℃/min; preferably, the temperature is increased to 1200-1600 ℃, more preferably 1300-1550 ℃, and even more preferably 1400-1500 ℃; the heat preservation is preferably 10 to 60min, more preferably 20 to 50min, and still more preferably 30 to 40min.
In the invention, a green body is placed in a heat insulation structure, and is placed in a microwave resonant cavity together with the heat insulation structure for microwave heating, a microwave source is started, the input power is intermittently adjusted from low to high, the reflected power is recorded, and the temperature change is recorded at the temperature of over 600 ℃.
In the invention, after a green body is placed in a heat preservation structure, calcined alumina powder covers the green body, and graphite covers the alumina powder; in the microwave heating process, the graphite reacts with air inside the heat-insulating structure to generate carbon monoxide, so that the inside of the heat-insulating structure is in carbon-containing reducing atmosphere.
According to the invention, the heat insulation structure is composed of a plurality of layers, wherein the innermost layer is an alumina hollow sphere sheet serving as a heat insulation layer, the mullite sheet serving as a heat insulation layer is provided with a mullite cover plate with a round hole at the upper part, alumina hollow sphere bricks are padded at the lower part to form a sample bin together, the next outer layer is a polycrystalline mullite fiber cotton serving as a heat insulation layer, the outermost layer is a quadrilateral structure surrounded by lightweight mullite sheets, and the lightweight mullite sheets are placed in an alumina sagger together to form a microwave sintering device.
In the invention, the microwave resonant cavity can adopt a conventional structure, and the uniform distribution of the microwave field intensity in the resonant cavity is ensured through the distribution of the positions of the magnetrons; the top of the cavity is provided with an exhaust device and a probing hole for inserting a far infrared radiation thermometer; the infrared thermometer monitors the temperature of the sample in the resonant cavity in real time, and the measured temperature range is 600-1800 ℃.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
1) Adding 30g of boron nitride powder, 15g of zirconia powder and 5g of silicon carbide powder into a ball milling tank, ball milling by using a planetary ball mill, wherein the ball-to-material ratio is 2:1, the rotating speed is 300r/min, the mixing time is 60min, and the ball-milled powder passes through a 60-mesh screen to obtain mixed powder;
2) Weighing 5g of mixed powder into a mortar, and adding Al 2 O 3 And Y 2 O 3 The mass ratio is 1:1, 0.25g of sintering aid, uniformly stirring, pouring into a mold, and performing dry pressing for 2min, wherein the pressing pressure is 70MPa;
3) Pressing the preformed blank by using a cold isostatic press to obtain a disc-shaped blank body, wherein the pressing pressure is 250MPa, and the pressure is maintained for 30s;
4) Placing the green body in a heat insulation structure, placing the green body and the heat insulation structure together in a microwave resonant cavity, starting a microwave source, setting the frequency of microwave heating to be 2.45GHz, intermittently adjusting the input power from low to high, and uniformly increasing the input power by 1KW every 10 minutes at the temperature of below 600 ℃; and after the measured temperature is displayed at 600 ℃, increasing the input power according to the heating rate, keeping the heating rate at 10-20 ℃/min, keeping the temperature for 30min when the temperature rises to 1400 ℃, recording the reflected power and the temperature change in the sintering process, and closing the microwave source to obtain the material.
XRD of the sintered material is shown in figure 1, and SEM of the sintered zirconium diboride powder is shown in figure 2.
Example 2
1) Adding 30g of boron nitride powder, 15g of zirconia powder and 5g of silicon carbide powder into a ball milling tank, ball milling by using a planetary ball mill, wherein the ball-to-material ratio is 2:1, the rotating speed is 300r/min, the mixing time is 60min, and the ball-milled powder passes through a 60-mesh screen to obtain mixed powder;
2) Weighing 5g of mixed powder into a mortar, and adding Al 2 O 3 And Y 2 O 3 The mass ratio is 1:1, 0.25g of sintering aid, uniformly stirring, pouring into a mold, and performing dry pressing for 2min, wherein the pressing pressure is 70MPa;
3) Pressing the preformed blank by using a cold isostatic press to obtain a disc-shaped blank body, wherein the pressing pressure is 250MPa, and the pressure is maintained for 30s;
4) Placing the green body in a heat insulation structure, placing the green body and the heat insulation structure together in a microwave resonant cavity, starting a microwave source, setting the frequency of microwave heating to be 2.45GHz, intermittently adjusting the input power from low to high, and uniformly increasing the input power by 1KW at intervals of 5 minutes below 600 ℃; and after the measured temperature is displayed at 600 ℃, the input power is increased according to the heating rate, the heating rate is maintained at 10-20 ℃/min, the temperature is kept for 40min when the temperature rises to 1550 ℃, the reflected power and the temperature change are recorded in the sintering process, and the microwave source is closed, so that the microwave sintering furnace is obtained.
Example 3
1) Adding 40g of boron nitride powder, 20g of zirconia powder and 5g of silicon carbide powder into a ball milling tank, and ball milling by using a planetary ball mill, wherein the ball-material ratio is 0.5;
2) Weighing 10g of mixed powder into a mortar, and adding Al 2 O 3 And Y 2 O 3 The mass ratio is 0.5:1, 0.1g of sintering aid, uniformly stirring, pouring into a mould, and performing dry pressing preforming under the pressing pressure of 50MPa for 1min;
3) Pressing the preformed blank by using a cold isostatic press to obtain a disc-shaped blank body, wherein the pressing pressure is 150MPa, and the pressure is maintained for 30s;
4) Placing the green body in a heat insulation structure, placing the green body and the heat insulation structure together in a microwave resonant cavity, starting a microwave source, setting the frequency of microwave heating to be 2.45GHz, intermittently adjusting the input power from low to high, and uniformly increasing the input power by 1KW at intervals of 5 minutes below 600 ℃; and after the measured temperature is displayed at 600 ℃, increasing the input power according to the heating rate, keeping the heating rate at 10-20 ℃/min, keeping the temperature for 10min when the temperature rises to 1400 ℃, recording the reflected power and the temperature change in the sintering process, and closing the microwave source to obtain the material.
Example 4
1) Adding 40g of boron nitride powder, 20g of zirconia powder and 10g of silicon carbide powder into a ball milling tank, ball milling by using a planetary ball mill, wherein the ball-to-material ratio is 2:1, the rotating speed is 300r/min, the mixing time is 120min, and the ball-milled powder passes through a 80-mesh screen to obtain mixed powder;
2) Weighing 10g of mixed powder into a mortar, and adding Al 2 O 3 And Y 2 O 3 The mass ratio of (A) to (B) is 2:1, 0.5g of sintering aid, uniformly stirring, pouring into a mold, and performing dry pressing for preforming, wherein the pressing pressure is 80MPa, and the pressure maintaining time is 3min;
3) Pressing the preformed blank by using a cold isostatic press to obtain a disc-shaped blank body, wherein the pressing pressure is 300MPa, and the pressure is maintained for 60s;
4) Placing the green body in a heat insulation structure, placing the green body and the heat insulation structure together in a microwave resonant cavity, starting a microwave source, setting the frequency of microwave heating to be 9.15GHz, intermittently adjusting the input power from low to high, and uniformly increasing the input power by 1KW every 10 minutes at the temperature of below 600 ℃; and after the measured temperature is displayed at 600 ℃, improving the input power according to the heating rate, keeping the heating rate at 10-20 ℃/min, improving the input power, keeping the temperature for 60min after the temperature rises to 1600 ℃, recording the reflected power and the temperature change in the sintering process, and closing the microwave source to obtain the microwave sintering material.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. BN-ZrO 2 The microwave sintering method of the-SiC complex phase ceramic is characterized by comprising the following steps of:
1) Mixing boron nitride powder, zirconia powder and silicon carbide powder, performing ball milling, and then sieving to obtain mixed powder;
2) Mixing the mixed powder and the sintering aid, performing dry pressing preforming, and performing cold isostatic pressing preforming on a blank body subjected to dry pressing preforming to obtain a green body;
3) Microwave heating the green body to prepare BN-ZrO 2 -SiC complex phase ceramics.
2. The BN-ZrO of claim 1 2 The microwave sintering method of the-SiC complex phase ceramic is characterized in that the boron nitride powder, the zirconia powder and the silicon carbide powder are all micro-nano-scale; the mass ratio of the boron nitride powder, the zirconia powder and the silicon carbide powder is 40-80: 20 to 40:5 to 20.
3. The BN-ZrO of claim 1 or 2 2 The microwave sintering method of the-SiC complex phase ceramic is characterized in that the ball milling condition in the step 1) is that the ball-to-material ratio is 0.5.
4. B according to claim 3N-ZrO 2 The microwave sintering method of the-SiC complex phase ceramic is characterized by comprising the following steps: the sintering aid in the step 2) is Al 2 O 3 And Y 2 O 3 Mixture of (1), al 2 O 3 And Y 2 O 3 The mass ratio of (A) to (B) is 0.5-2: 1, the addition amount is 1-5% of the mass of the mixed powder.
5. The BN-ZrO of claim 1, 2 or 4 2 The microwave sintering method of the-SiC complex phase ceramic is characterized in that the pressure of the dry pressing preforming in the step 2) is 50-80 MPa, and the pressure maintaining time is 1-3 min; the pressure of the cold isostatic pressing preforming is 150-300 MPa, and the pressure maintaining time is 30-60 s.
6. The BN-ZrO of claim 5 2 The microwave sintering method of the-SiC complex phase ceramic is characterized in that the frequency of microwave heating is 2.45GHz or 9.15GHz, and the output power is 2-15 KW.
7. The BN-ZrO of claim 6 2 The microwave sintering method of the-SiC complex phase ceramic is characterized in that the microwave heating conditions in the step 3) are as follows: when the temperature is less than or equal to 600 ℃, the power is increased by 1KW every 5-10 min; when the temperature is higher than 600 ℃, adjusting the heating rate to 10-20 ℃/min, heating to 1200-1600 ℃, and preserving the heat for 10-60 min.
8. The BN-ZrO of claim 6 or 7 2 The microwave sintering method of the-SiC composite ceramic is characterized in that a green body is placed in a heat insulation structure to be subjected to microwave heating; after the green body is placed into the heat-insulating structure, the calcined alumina powder covers the green body, and the graphite covers the alumina powder.
9. The BN-ZrO of claim 8 2 The microwave sintering method of the-SiC complex phase ceramic is characterized in that the heat preservation structure consists of a multilayer structure, and comprises an alumina hollow sphere layer, a light mullite sheet layer, a polycrystalline mullite fiber cotton layer and light mullite in sequence from inside to outsideA sheet layer and an alumina sagger layer.
10. BN-ZrO produced by the microwave sintering method according to any one of claims 1 to 9 2 -SiC complex phase ceramic in which ZrB is generated in situ 2 And (3) powder.
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