CN103172382A - Preparation method of ultra-temperature oxidative damage resistant zirconium diboride-silicon carbide ceramic base composite material - Google Patents
Preparation method of ultra-temperature oxidative damage resistant zirconium diboride-silicon carbide ceramic base composite material Download PDFInfo
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- CN103172382A CN103172382A CN2013101402676A CN201310140267A CN103172382A CN 103172382 A CN103172382 A CN 103172382A CN 2013101402676 A CN2013101402676 A CN 2013101402676A CN 201310140267 A CN201310140267 A CN 201310140267A CN 103172382 A CN103172382 A CN 103172382A
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Abstract
The invention relates to a preparation method of an ultra-temperature oxidative damage resistant zirconium diboride-silicon carbide ceramic base composite material, and relates to a preparation method of an ultra-temperature oxidative damage resistant ceramic base composite material. The preparation method aims to solve the problem of poor oxide layer stability of the traditional zirconium diboride-silicon carbide ceramic base composite material at a superhigh temperature (more than 1700 DEG C). The preparation method comprises the following steps of: 1, preparing the zirconium diboride-silicon carbide ceramic base composite material; and 2, carrying out oxidization inhibition processing to obtain the superhigh temperature oxidative damage resistant zirconium diboride-silicon carbide ceramic base composite material. The preparation method disclosed by the invention can be used for preparing the superhigh temperature oxidative damage resistant zirconium diboride-silicon carbide ceramic base composite material.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic matric composite of anti-ultra high temp oxidative damage.
Background technology
The development of hypersonic flight technology has proposed harsh requirement to thermally protective materials.ZrB
2ceramic matric composite has high fusing point, higher thermal conductance and specific conductivity, excellent resist chemical performance, relatively low density, moderate price.Excellent over-all properties can be competent at the extreme Aerodynamic Heating environment of the key positions such as hypersonic aircraft termination, nose of wing, meet the strict demand of aircraft to the thermal protection system structural integrity, be a kind of very promising non-ablative-type protective coating structured material simultaneously.
Pure ZrB
2the stupalith oxidation generates ZrO
2and B
2o
3, the glassy phase of generation covers the material surface matrix that suppressed the oxygen diffusing protection, has improved the antioxidant property of material.But when temperature during higher than 120O ° of C, the B of generation
2o
3glassy phase volatilizees in a large number and loses the provide protection to matrix, and the rate of oxidation of material is accelerated, and during to 1800 ° of C, the material complete oxidation lost efficacy.For the antioxidant property that improves this material adds second-phase SiC.SiC adds the sintering characteristic that not only can improve material, and inhibiting grain growth has also significantly improved the antioxidant property of material.The SiO that the SiC oxidation generates
2with B
2o
3form borosilicate, suppressed B
2o
2volatilization, there is good mobility and wettability covering material surface simultaneously, make surface imperfection up, effectively protected material.Yet work as temperature higher than 1600 ° of C, the SiC active oxidation glassy phase that material surface generates simultaneously volatilizees in a large number, sharply escaping gas has destroyed the integrity of surface oxide layer, accelerate the oxidising process of material, greatly limited the long service of zirconium diboride-carbon/silicon carbide ceramic matrix composite under ultra high temp (>1700 ° of C).
Summary of the invention
The present invention will solve existing zirconium diboride-carbon/silicon carbide ceramic matrix composite to have the problem of the poor stability of zone of oxidation under ultra high temp (>1700 ° of C), and a kind of preparation method of zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage is provided.
The preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of a kind of anti-ultra high temp oxidative damage of the present invention, carry out according to the following steps:
One, prepare zirconium diboride-carbon/silicon carbide ceramic matrix composite: take by weight the zirconium diboride powder of 70 ~ 90 parts and the silicon carbide powder of 30 ~ 10 parts, and zirconium diboride powder and silicon carbide powder are carried out to wet ball-milling, obtain slip, then by the gained slip, by rotatory evaporator, in temperature, it is under ° C condition of 50 ° of C ~ 90 dry 1 hour ~ 4 hours, mixed powder after being dried, finally by the mixed powder after the oven dry obtained under vacuum or inert gas atmosphere at 1700 ° of C ~ l90O ° of C temperature hot pressed sintering, hot pressing pressure is 3OMPa, soaking time is 20 minutes ~ 60 minutes, after naturally cooling to room temperature, take out, obtain zirconium diboride-carbon/silicon carbide ceramic matrix composite,
Two, oxidation suppresses to process: zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1 is placed in oxidation and suppresses treatment unit, be filled with pure oxygen or air, the control gas flow is lmL/min ~ 500mL/min, then suppressing the under meter for the treatment of unit and vacuum pump by oxidation, to control the gaseous tension that oxidation suppresses in the treatment unit reaction chamber be lPa ~ l0000Pa, the electromagnetic induction heating device that finally utilizes oxidation to suppress treatment unit is heated to 1400 ° of C ~ 1700 ° C by zirconium diboride-carbon/silicon carbide ceramic matrix composite, then be incubated, soaking time is 1 minute ~ 180 minutes, obtain the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage.
The particle diameter of the zirconium diboride powder described in step 1 of the present invention is less than 10 microns; The particle diameter of the silicon carbide powder described in step 1 is less than 10 microns.
Advantage of the present invention: one, under 1700 ° of C ~ 200O ° of C of ultra high temp, under identical oxidizing condition and in identical oxidization time, zirconium diboride-the carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage prepared by the present invention is compared with zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by existing method, oxidated layer thickness has reduced 15% ~ 40%, the mass area ratio velocity of variation has reduced by 20% ~ 45%, the rate of oxidation of material is slow, and antioxidant property is good, two, the present invention is by ZrB
2-SiC ceramic matric composite is placed in oxidation and suppresses treatment unit, pre-treatment under the high-temperature low-pressure environment, at the prefabricated one deck porous zirconia of material surface layer, due to the chemical potential gradient existed, the zirconium white skeleton of this complications can effectively reduce the oxygen partial pressure at basal body interface place, and inhibited oxidation atmosphere spreads to material internal, and the zirconium white skeleton can provide support, guarantee the hot strength of zone of oxidation, in this external dynamic oxidation process, this generated in-situ porous zirconia can play the effect of thermal barrier coating because of its lower thermal conductivity, reduce the thermograde of body material, three, the present invention is with ZrB
2-SiC ceramic matric composite is applied as background under ultra high temp (>1700 ° of C), has proposed a kind of simple ZrB that effectively improves
2the method of the anti-ultra high temp oxidative damage of-SiC ceramic matric composite, prefabricated porous zirconia skeleton microstructure is evenly regular, with body material, is combined reliably, when improving the material antioxidant property, does not affect other performances of material, four, oxidation inhibition treatment unit of the present invention can be realized the experimental state under differing temps (room temperature ~ 2000 ° C), different pressures (lPa ~ l00000Pa), differential responses atmosphere, zirconium diboride-the carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage that five, prepared by the present invention can be under ultra high temp (1700 ° of C ~ 2000 ° C) long service.
The accompanying drawing explanation
A kind of oxidation that Fig. 1 is embodiment four suppresses the structural representation for the treatment of unit;
Fig. 2 is the zirconia surface skeleton Cross Section Morphology figure of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage of test one preparation.
Embodiment
Embodiment one: the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of a kind of anti-ultra high temp oxidative damage of present embodiment, carry out according to the following steps:
One, prepare zirconium diboride-carbon/silicon carbide ceramic matrix composite: take by weight the zirconium diboride powder of 70 ~ 90 parts and the silicon carbide powder of 30 ~ 10 parts, and zirconium diboride powder and silicon carbide powder are carried out to wet ball-milling, obtain slip, then by the gained slip, by rotatory evaporator, in temperature, it is under ° C condition of 50 ° of C ~ 90 dry 1 hour ~ 4 hours, mixed powder after being dried, finally by the mixed powder after the oven dry obtained under vacuum or inert gas atmosphere at 1700 ° of C ~ l90O ° of C temperature hot pressed sintering, hot pressing pressure is 3OMPa, soaking time is 20 minutes ~ 60 minutes, after naturally cooling to room temperature, take out, obtain zirconium diboride-carbon/silicon carbide ceramic matrix composite,
Two, oxidation suppresses to process: zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1 is placed in oxidation and suppresses treatment unit, be filled with pure oxygen or air, the control gas flow is lmL/min ~ 500mL/min, then suppressing the under meter 1 for the treatment of unit and vacuum pump 10 by oxidation, to control the gaseous tension that oxidations suppress in the treatment unit reaction chambers be lPa ~ l0000Pa, the electromagnetic induction heating device that finally utilizes oxidation to suppress treatment unit is heated to 1400 ° of C ~ 1700 ° C by zirconium diboride-carbon/silicon carbide ceramic matrix composite, then be incubated, soaking time is 1 minute ~ 180 minutes, obtain the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage.
The particle diameter of the zirconium diboride powder described in the present embodiment step 1 is less than 10 microns; The particle diameter of the silicon carbide powder described in step 1 is less than 10 microns.
Under 1700 ° of C ~ 2000 ° C of ultra high temp, under identical oxidizing condition and in identical oxidization time, zirconium diboride-the carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage prepared by present embodiment is compared with zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by existing method, oxidated layer thickness has reduced 15% ~ 40%, the mass area ratio velocity of variation has reduced by 20% ~ 45%, the rate of oxidation of material is slow, and antioxidant property is good.
Present embodiment is by ZrB
2-SiC ceramic matric composite is placed in oxidation and suppresses treatment unit, pre-treatment under the high-temperature low-pressure environment, at the prefabricated one deck porous zirconia of material surface layer, due to the chemical potential gradient existed, the zirconium white skeleton of this complications can effectively reduce the oxygen partial pressure at basal body interface place, and inhibited oxidation atmosphere spreads to material internal, and the zirconium white skeleton can provide support, guarantee the hot strength of zone of oxidation, in this external dynamic oxidation process, this generated in-situ porous zirconia can play the effect of thermal barrier coating because of its lower thermal conductivity, reduce the thermograde of body material.
Present embodiment is with ZrB
2-SiC ceramic matric composite is applied as background under ultra high temp (>1700 ° of C), has proposed a kind of simple ZrB that effectively improves
2the method of the anti-ultra high temp oxidative damage of-SiC ceramic matric composite, prefabricated porous zirconia skeleton microstructure is evenly regular, with body material, is combined reliably, when improving the material antioxidant property, does not affect other performances of material.
The oxidation of present embodiment suppresses treatment unit can realize the experimental state under differing temps (room temperature ~ 2000 ° C), different pressures (lPa ~ l00000Pa), differential responses atmosphere.
Zirconium diboride-the carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage prepared by present embodiment can be under ultra high temp (1700 ° of C ~ 2000 ° C) long service.
Embodiment two: present embodiment is different from embodiment one: the particle diameter of the zirconium diboride powder described in step 1 is less than 10 microns; The particle diameter of the silicon carbide powder described in step 1 is less than 10 microns.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two: the rare gas element described in step 1 is argon gas.Other is identical with embodiment one or two.
Embodiment four: in conjunction with Fig. 1, present embodiment is different from one of embodiment one to three: the oxidation described in step 2 suppresses treatment unit and comprises under meter 1, optical pyrometer 2, Calcium Fluoride (Fluorspan) glass 3, top cover 4, silica tube 5, zirconium white support 6, bottom 7, electromagnetic induction heating coil 8, tensimeter 9 and vacuum pump 10; Described under meter 1 is communicated with the inlet mouth of top cover 4, described Calcium Fluoride (Fluorspan) glass 3 is embedded in top cover 4 light can be appeared from silica tube 5 inside, top cover 4 is sealedly connected on the upper end of silica tube 5, bottom 7 is sealedly connected on the bottom of silica tube 5, zirconium white support 6 be arranged on silica tube 5 inner and with the silica tube outside surface at zirconium white support 6 top end opposite position places on be provided with electromagnetic induction heating coil 8, described vacuum pump 10 is communicated with the air outlet of bottom 7 by tensimeter 9.
The oxidation of present embodiment suppresses the principle of work for the treatment of unit: by under meter 1, tensimeter 10 and vacuum pump 11, come conditioned reaction gas flow and gaseous tension; Top cover 4, silica tube 5 and bottom 7 have formed the main body of enclosed reaction chamber jointly; Sample, for the experiment detected materials, provides support by 7 pairs of experiment materials of zirconium white support; Electromagnetic induction heating coil 8 and corresponding device are heating system, can realize being rapidly heated of material; Optical pyrometer 2 and Calcium Fluoride (Fluorspan) glass 3 are temp measuring systems, and optical pyrometer 2 is measured the specimen surface temperature by Calcium Fluoride (Fluorspan) glass 3.Above-mentioned each device connects in certain sequence and operates can realize different atmosphere, gaseous tension and temperature of reaction, to meet the demand of the zirconium diboride-carbon/silicon carbide ceramic matrix composite for preparing anti-ultra high temp oxidative damage.
The oxidation of present embodiment suppresses treatment unit can realize the experimental state under differing temps (room temperature ~ 2000 ° C), different pressures (lPa-l00000Pa), differential responses atmosphere.
Embodiment five: present embodiment is different from one of embodiment one to four: controlling gas flow in step 2 is 5mL/min ~ 500mL/min.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: suppressing by oxidation the gaseous tension that the under meter 1 for the treatment of unit and vacuum pump 10 control in the oxidation suppressing device reaction chambers in step 2 is 100Pa ~ 5000Pa.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: the electromagnetic induction heating device that utilizes oxidation to suppress treatment unit in step 2 is heated to 150O ° of C ~ 1700 ° C by zirconium diboride-carbon/silicon carbide ceramic matrix composite.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven: in step 2, soaking time is 20 minutes ~ 60 minutes.Other is identical with one of embodiment one to seven.
Adopt following verification experimental verification effect of the present invention:
Test one: in conjunction with Fig. 1, a kind of preparation method of zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage, carry out according to the following steps:
One, prepare zirconium diboride-carbon/silicon carbide ceramic matrix composite: 240g zirconium diboride powder and 60g silicon carbide powder are carried out to wet ball-milling; obtain slip; then by the gained slip, by rotatory evaporator, in temperature, it is under 70 ° of C conditions dry 4 hours; mixed powder after being dried; finally by the mixed powder after the oven dry obtained under argon gas atmosphere at 1800 ° of C temperature hot pressed sintering; hot pressing pressure is 3OMPa; soaking time is 60 minutes; take out after naturally cooling to room temperature, obtain zirconium diboride-carbon/silicon carbide ceramic matrix composite;
Two, oxidation suppresses to process: by diameter, be that 20mm and thickness are 3mm zirconium diboride-carbon/silicon carbide ceramic matrix composite, be placed in oxidation and suppress treatment unit, be filled with pure oxygen, the control gas flow is 50mL/min, then suppressing the under meter for the treatment of unit and vacuum pump by oxidation, to control the gaseous tension that oxidation suppresses in the treatment unit reaction chamber be lOPa, the electromagnetic induction heating device that finally utilizes oxidation to suppress treatment unit is heated to 1400 ° of C by zirconium diboride-carbon/silicon carbide ceramic matrix composite, then be incubated, soaking time is 20 minutes, obtain the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage.
Respectively by the oxidation 30 minutes in 1700 ° of C air of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage of this test preparation and zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, material section after oxidation is passed through to sem observation, take pictures, measure respectively the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage of this test preparation and the oxidated layer thickness of zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, the velocity of variation that simultaneously utilizes electronic balance unit of measure area to improve quality, as shown in table 1.
Adopt the zirconium diboride-carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage of this test of sem observation preparation, as shown in Figure 2, Fig. 2 is the zirconium white skeleton Cross Section Morphology figure of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage of this test preparation, prefabricated porous zirconia skeleton microstructure is evenly regular as shown in Figure 2, with body material, is combined reliably.
Test two: in conjunction with Fig. 1, a kind of preparation method of zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage, carry out according to the following steps:
One, prepare zirconium diboride-carbon/silicon carbide ceramic matrix composite: 270g zirconium diboride powder and 30g silicon carbide powder are carried out to wet ball-milling; obtain slip; then by the gained slip, by rotatory evaporator, in temperature, it is under 75 ° of C conditions dry 3.5 hours; mixed powder after being dried; finally by the mixed powder after the oven dry obtained under argon gas atmosphere at 190O ° of C temperature hot pressed sintering; hot pressing pressure is 3OMPa; soaking time is 30 minutes; take out after naturally cooling to room temperature, obtain zirconium diboride-carbon/silicon carbide ceramic matrix composite;
Two, oxidation suppresses to process: by diameter, be that 2Omm and thickness are that 3mm zirconium diboride-carbon/silicon carbide ceramic matrix composite is placed in oxidation inhibition treatment unit, be filled with air, the control gas flow is 300mL/min, then suppressing the under meter for the treatment of unit and vacuum pump by oxidation, to control the gaseous tension that oxidation suppresses in the treatment unit reaction chamber be 10OOPa, the electromagnetic induction heating device that finally utilizes oxidation to suppress treatment unit is heated to 150O ° of C by zirconium diboride-carbon/silicon carbide ceramic matrix composite, then be incubated, soaking time is 30 minutes, obtain the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage.
Respectively by the oxidation 30 minutes in 1800 ° of C air of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage of this test preparation and zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, material section after oxidation is passed through to sem observation, take pictures, measure respectively the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage of this test preparation and the oxidated layer thickness of zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, the velocity of variation that simultaneously utilizes electronic balance unit of measure area to improve quality, as shown in table 1.
Test three: in conjunction with Fig. 1, a kind of preparation method of zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage, carry out according to the following steps:
One, prepare zirconium diboride-carbon/silicon carbide ceramic matrix composite: 270g zirconium diboride powder and 30g silicon carbide powder are carried out to wet ball-milling; obtain slip; then by the gained slip, by rotatory evaporator, in temperature, it is under 80 ° of C conditions dry 2 hours; mixed powder after being dried; finally by the mixed powder after the oven dry obtained under argon gas atmosphere at 190O ° of C temperature hot pressed sintering; hot pressing pressure is 3OMPa; soaking time is 30 minutes; take out after naturally cooling to room temperature, obtain zirconium diboride-carbon/silicon carbide ceramic matrix composite;
Two, oxidation suppresses to process: by diameter, be that 2Omm and thickness are 3mm zirconium diboride-carbon/silicon carbide ceramic matrix composite, be placed in oxidation and suppress treatment unit, be filled with air, the control gas flow is 10OmL/min, then suppressing the under meter for the treatment of unit and vacuum pump by oxidation, to control the gaseous tension that oxidation suppresses in the treatment unit reaction chamber be 1OOPa, the electromagnetic induction heating device that finally utilizes oxidation to suppress treatment unit is heated to 150O ° of C by zirconium diboride-carbon/silicon carbide ceramic matrix composite, then be incubated, soaking time is 30 minutes, obtain the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage.
Respectively by the oxidation 30 minutes in 1800 ° of C air of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage of this test preparation and zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, material section after oxidation is passed through to sem observation, take pictures, measure respectively the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage of this test preparation and the oxidated layer thickness of zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, the velocity of variation that simultaneously utilizes electronic balance unit of measure area to improve quality, as shown in table 1.
Test four: in conjunction with Fig. 1, a kind of preparation method of zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage, carry out according to the following steps:
One, prepare zirconium diboride-carbon/silicon carbide ceramic matrix composite: 270g zirconium diboride powder and 30g silicon carbide powder are carried out to wet ball-milling; obtain slip; then by the gained slip, by rotatory evaporator, in temperature, it is under 90 ° of C conditions dry 1 hour; mixed powder after being dried; finally by the mixed powder after the oven dry obtained under argon gas atmosphere at 190O ° of C temperature hot pressed sintering; hot pressing pressure is 3OMPa; soaking time is 30 minutes; take out after naturally cooling to room temperature, obtain zirconium diboride-carbon/silicon carbide ceramic matrix composite;
Two, oxidation suppresses to process: by diameter, be that 2Omm and thickness are that 3mm zirconium diboride-carbon/silicon carbide ceramic matrix composite is placed in oxidation inhibition treatment unit, be filled with air, the control gas flow is 100mL/min, then suppressing the under meter for the treatment of unit and vacuum pump by oxidation, to control the gaseous tension that oxidation suppresses in the treatment unit reaction chamber be 100Pa, the electromagnetic induction heating device that finally utilizes oxidation to suppress treatment unit is heated to 1600 ° of C by zirconium diboride-carbon/silicon carbide ceramic matrix composite, then be incubated, soaking time is 30 minutes, obtain the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage.
Respectively by the oxidation 10 minutes in 1950 ° of C air of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage of this test preparation and zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, material section after oxidation is passed through to sem observation, take pictures, measure respectively the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage of this test preparation and the oxidated layer thickness of zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, the velocity of variation that simultaneously utilizes electronic balance unit of measure area to improve quality, add shown in table 1.
Test five: in conjunction with Fig. 1, a kind of preparation method of zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage, carry out according to the following steps:
One, prepare zirconium diboride-carbon/silicon carbide ceramic matrix composite: 270g zirconium diboride powder and 30g silicon carbide powder are carried out to wet ball-milling; obtain slip; then by the gained slip, by rotatory evaporator, in temperature, it is under 70 ° of C conditions dry 4 hours; mixed powder after being dried; finally by the mixed powder after the oven dry obtained under argon gas atmosphere at 190O ° of C temperature hot pressed sintering; hot pressing pressure is 3OMPa; soaking time is 30 minutes; take out after naturally cooling to room temperature, obtain zirconium diboride-carbon/silicon carbide ceramic matrix composite;
Two, oxidation suppresses to process: by diameter, be that 2Omm and thickness are that 3mm zirconium diboride-carbon/silicon carbide ceramic matrix composite is placed in oxidation inhibition treatment unit, be filled with air, the control gas flow is 200mL/min, then suppressing the under meter for the treatment of unit and vacuum pump by oxidation, to control the gaseous tension that oxidation suppresses in the treatment unit reaction chamber be 5OOPa, the electromagnetic induction heating device that finally utilizes oxidation to suppress treatment unit is heated to 1650 ° of C by zirconium diboride-carbon/silicon carbide ceramic matrix composite, then be incubated, soaking time is 60 minutes, obtain the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage.
Respectively by the oxidation 30 minutes in 1850 ° of C air of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage of this test preparation and zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, material section after oxidation is passed through to sem observation, take pictures, measure respectively the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage of this test preparation and the oxidated layer thickness of zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, the velocity of variation that simultaneously utilizes electronic balance unit of measure area to improve quality, as shown in table 1.
Test six: in conjunction with Fig. 1, a kind of preparation method of zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage, carry out according to the following steps:
One, prepare zirconium diboride-carbon/silicon carbide ceramic matrix composite: 270g zirconium diboride powder and 30g silicon carbide powder are carried out to wet ball-milling; obtain slip; then by the gained slip, by rotatory evaporator, in temperature, it is under 70 ° of C conditions dry 4 hours; mixed powder after being dried; finally by the mixed powder after the oven dry obtained under argon gas atmosphere at 190O ° of C temperature hot pressed sintering; hot pressing pressure is 3OMPa; soaking time is 30 minutes; take out after naturally cooling to room temperature, obtain zirconium diboride-carbon/silicon carbide ceramic matrix composite;
Two, oxidation suppresses to process: by diameter, be that 2Omm and thickness are that 3mm zirconium diboride-carbon/silicon carbide ceramic matrix composite is placed in oxidation inhibition treatment unit, be filled with air, the control gas flow is 500mL/min, then suppressing the under meter for the treatment of unit and vacuum pump by oxidation, to control the gaseous tension that oxidation suppresses in the treatment unit reaction chamber be 50OOPa, the electromagnetic induction heating device that finally utilizes oxidation to suppress treatment unit is heated to 1700 ° of C by zirconium diboride-carbon/silicon carbide ceramic matrix composite, then be incubated, soaking time is 40 minutes, obtain the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage.
Respectively by the oxidation 15 minutes in 190O ° of C air of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage of this test preparation and zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, material section after oxidation is passed through to sem observation, take pictures, measure respectively the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage of this test preparation and the oxidated layer thickness of zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1, the velocity of variation that simultaneously utilizes electronic balance unit of measure area to improve quality, as shown in table 1.
Table 1
As shown in Table 1; zirconium diboride-the carbon/silicon carbide ceramic matrix composite of the anti-ultra high temp oxidative damage prepared by method of the present invention and not oxidised press down zirconium diboride-carbon/silicon carbide ceramic matrix that silks processes again full material compare; oxidated layer thickness has reduced 15%～40%, and the mass area ratio velocity of variation is grand low by 20%～45%; Under identical oxidizing condition and in identical oxidization time, the oxidated layer thickness of the compound village of the zirconium diboride-carbon/silicon carbide ceramic matrix of the anti-ultra high temp oxidative damage that adopts method of the present invention to prepare material is thin, the mass area ratio velocity of variation is little, and the rate of oxidation of material is slow, and antioxidant property is good.
Claims (8)
1. the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of an anti-ultra high temp oxidative damage is characterized in that the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage carries out according to the following steps:
One, prepare zirconium diboride-carbon/silicon carbide ceramic matrix composite: take by weight the zirconium diboride powder of 70 ~ 90 parts and the silicon carbide powder of 30 ~ 10 parts, and zirconium diboride powder and silicon carbide powder are carried out to wet ball-milling, obtain slip, then by the gained slip, by rotatory evaporator, in temperature, it is under ° C condition of 50 ° of C ~ 90 dry 1 hour ~ 4 hours, mixed powder after being dried, finally by the mixed powder after the oven dry obtained under vacuum or inert gas atmosphere at 1700 ° of C ~ l900 ° of C temperature hot pressed sintering, hot pressing pressure is 3OMPa, soaking time is 20 minutes ~ 60 minutes, after naturally cooling to room temperature, take out, obtain zirconium diboride-carbon/silicon carbide ceramic matrix composite,
Two, oxidation suppresses to process: zirconium diboride-carbon/silicon carbide ceramic matrix composite prepared by step 1 is placed in oxidation and suppresses treatment unit, be filled with pure oxygen or air, the control gas flow is lmL/min ~ 500mL/min, then suppressing the under meter (1) for the treatment of unit and vacuum pump (10) by oxidation, to control the gaseous tension that oxidation suppresses in the treatment unit reaction chamber be lPa ~ 10000Pa, the electromagnetic induction heating device that finally utilizes oxidation to suppress treatment unit is heated to 1400 ° of C-1700 ° of C by zirconium diboride-carbon/silicon carbide ceramic matrix composite, then be incubated, soaking time is 1 minute ~ 180 minutes, obtain the zirconium diboride-carbon/silicon carbide ceramic matrix composite of anti-ultra high temp oxidative damage.
2. the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of a kind of anti-ultra high temp oxidative damage according to claim 1, is characterized in that the particle diameter of the zirconium diboride powder described in step 1 is less than 10 microns; The particle diameter of the silicon carbide powder described in step 1 is less than 10 microns.
3. the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of a kind of anti-ultra high temp oxidative damage according to claim 1, is characterized in that the rare gas element described in step 1 is argon gas.
4. the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of a kind of anti-ultra high temp oxidative damage according to claim 1, is characterized in that the oxidation described in step 2 suppresses treatment unit and comprises under meter (1), optical pyrometer (2), Calcium Fluoride (Fluorspan) glass (3), top cover (4), silica tube (5), zirconium white support (6), bottom (7), electromagnetic induction heating coil (8), tensimeter (9) and vacuum pump (10); described under meter (1) is communicated with the inlet mouth of top cover (4), described Calcium Fluoride (Fluorspan) glass (3) is embedded in top cover (4) light can be appeared from silica tube (5) inside, top cover (4) is sealedly connected on the upper end of silica tube (5), bottom (7) is sealedly connected on the bottom of silica tube (5), zirconium white support (6) be arranged on silica tube (5) inner and with the silica tube outside surface at zirconium white support (6) top end opposite position place on be provided with electromagnetic induction heating coil (8), described vacuum pump (10) is communicated with the air outlet of bottom (7) by tensimeter (9).
5. the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of a kind of anti-ultra high temp oxidative damage according to claim 1, is characterized in that controlling gas flow in step 2 is 5mL/min ~ 500mL/min.
6. the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of a kind of anti-ultra high temp oxidative damage according to claim 1, is characterized in that in step 2 suppressing the under meter (1) for the treatment of unit and gaseous tension that vacuum pump (10) is controlled in the oxidation suppressing device reaction chamber is 100Pa ~ 5000Pa by oxidation.
7. the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of a kind of anti-ultra high temp oxidative damage according to claim 1, is characterized in that in step 2 that the electromagnetic induction heating device that utilizes oxidation to suppress treatment unit is heated to 1500 ° of C ~ 1700 ° C by zirconium diboride-carbon/silicon carbide ceramic matrix composite.
8. the preparation method of the zirconium diboride-carbon/silicon carbide ceramic matrix composite of a kind of anti-ultra high temp oxidative damage according to claim 1, is characterized in that in step 2, soaking time is 20 minutes ~ 60 minutes.
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