CN105198445A - Boron nitride multi-phase ceramic side sealing plate and preparation method thereof - Google Patents
Boron nitride multi-phase ceramic side sealing plate and preparation method thereof Download PDFInfo
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- CN105198445A CN105198445A CN201510689621.XA CN201510689621A CN105198445A CN 105198445 A CN105198445 A CN 105198445A CN 201510689621 A CN201510689621 A CN 201510689621A CN 105198445 A CN105198445 A CN 105198445A
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Abstract
The invention discloses a boron nitride multi-phase ceramic side sealing plate and a preparation method thereof and relates to a multi-phase ceramic side sealing plate and a preparation method thereof. The invention aims at solving the technical problem that the high-temperature anti-bending strength and thermal creep resistance of a boron nitride multi-phase ceramic material are reduced for a reason that the added low-melting-point phase is remained. The boron nitride multi-phase ceramic side sealing plate consists of boron nitride, electric-melting zirconia, silicon carbide and additives. The preparation method comprises the following steps: 1) weighing raw materials; 2) preparing composite powder, 3) placing the composite powder in a mold, increasing temperature and decreasing the temperature to room temperature to obtain the boron nitride multi-phase ceramic side sealing plate. The compactness of the boron nitride multi-phase ceramic side sealing plate prepared by adopting the method disclosed by the invention can reach more than 97 percent, the comprehensive mechanical performance is excellent, the anti-bending strength can reach 350MPa, and no obvious softening phenomenon occurs during high-temperature mechanical performance testing. The invention belongs to the field of preparation of ceramic side sealing plates.
Description
Technical field
The present invention relates to a kind of complex phase ceramic side seal board and preparation method thereof.
Background technology
Twin-roll thin strip continuous casting technology is a kind of novel Thin Strip Steel production technique, as the cutting edge technology in development of iron & steel industry direction, can without production processes such as continuous casting, heating and hot rollings, be directly the strip base of 1 ~ 5mm by the aquatic output thickness of liquid steel, complete all processes from liquid metal to solid-state strip at short notice.In addition, in acquisition property, there is unique advantage, the minimizing production ways of high performance steel can be realized, obtain the extensive attention of world steel circle, but still need constantly to improve to realize suitability for industrialized production as early as possible.
Side seal board is the leakage-proof part added at crystallization roll two ends, plays constraint metal liquid, promotes that strip is shaping, ensures the effects such as strip edge quality.But the working condition requirement of crystallization roll is comparatively complicated, comparatively harsh requirement is all proposed to the mechanical property of side seal board material and physicochemical property stability, the requirements such as thermal shock resistance, anti-molten steel erosion performance, high temperature resistant friction and wear behavior and high temperature dimensional stability need be possessed simultaneously, cause traditional refractory materials can not meet the working condition requirement of side seal board, need the appearance of novel refractory badly.
Hexagonal boron nitride stupalith, there is high-temperature self-lubrication effect, thermal expansivity is low, thermal conductivity is high, thermal shock resistance is good, stability at elevated temperature is good, good and molten metal such as not to infiltrate at the advantage to coagulative separability, be a member important in advanced ceramics material family, the key project such as Metal smelting and high temperature friction and wear field can be widely used in.But boron nitride has the physical propertys such as the strong and self-diffusion coefficient of high-melting-point, covalent linkage is low, and easily forms card room structure in sintering process, is also difficult to be destroyed even if apply external force.Adopt general conventional hot-press sintering process, at 1800 ~ 2000 DEG C, by its densified sintering product, need could add the preparation cost of boron nitride ceramic material under the high temperature hot pressing condition of 20 ~ 40MPa, hinder the widespread use of boron nitride material at engineering field.
Although interpolation low melting point is on good terms effectively promote boron nitride diphase ceramic material sintering densification, a large amount of residual of low melting point phase can cause thermomechanical property to be subject to a significant impact, obvious reduction high-temperature bending strength and heat creep resistance energy.In addition, the dissolving diffusion of low melting point in opposite directions in molten steel, not only reduces the anti-molten steel erosion performance of boron nitride complex phase ceramic, reduces its work-ing life and safety in utilization, also can pollute molten steel, affect quality product.Therefore, how to select effective sintering aid and technology of preparing, be the engineering challenge needing solution badly always.Therefore, Study and Development goes out the reasonable and corresponding technology of preparing of component composition, thus the side seal board material preparing military service excellent performance has great importance to the development of strip continuous casting technology and large rule suitability for industrialized production.
Summary of the invention
The present invention adds the low melting point residual technical problem reducing boron nitride diphase ceramic material high-temperature bending strength and heat creep resistance energy mutually to solve, and provides a kind of boron nitride complex phase ceramic side seal board and preparation method thereof.
Boron nitride complex phase ceramic side seal board is made up of the additive of the boron nitride of 65 parts ~ 85 parts, the electric-melting zirconia of 15 parts ~ 35 parts, the silicon carbide of 5 parts ~ 15 parts and 5 parts ~ 10 parts by weight; Described additive is MAX phase.
Described MAX phase is Nb
2alC, Zr
2alC, V
2alC, Ti
2snC, Zr
2snC, Ti
2alN, Ti
3alC
2or Nb
4alC
3.
Described MAX phase is Ti
3al (C
0.5, N
0.5)
2, (Nb, Zr)
2alC, (Ti, V)
2alC, (Ti, Nb)
2alC, (Ti, Cr)
2alC, (Ti, Ta)
2alC, (V, Nb)
2alC, (V, Ta)
2alC, (V, Cr)
2alC or (Ti, Hf)
2inC.
Described MAX phase is Nb
2alC-Zr
2alC, Zr
2alC-Zr
2snC or (Nb, Zr)
2alC-(V, Ta)
2alC.
The preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, the additive of the boron nitride of 65 parts ~ 85 parts, the electric-melting zirconia of 15 parts ~ 35 parts, the silicon carbide of 5 parts ~ 15 parts and 5 parts ~ 10 parts is taken by weight;
Two, add in dispersion medium by boron nitride, electric-melting zirconia, silicon carbide and additive, wet ball grinding, after 10 ~ 48 hours, carries out dry 10h ~ 48h at 70 DEG C ~ 150 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 5 DEG C/min ~ 25 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1200 DEG C ~ 1400 DEG C time, be forced into 20MPa ~ 40MPa, then be warming up to 1400 DEG C ~ 1800 DEG C; heat-insulation pressure keeping 0.5 ~ 5h; again with 5 DEG C/min ~ 25 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
Dispersion medium described in step 2 is alcohol, dehydrated alcohol or ethanol mass concentration are the aqueous ethanolic solution of 55% ~ 95%.
Boron nitride-base complex phase ceramic side seal material hot pressed sintering preparation method proposed by the invention, the favourable sintering temperature reducing boron nitride complex phase ceramic, suppress the granular size of thing phase that generates and skewness and the defect such as pore and local organization segregation, prepared material grains is tiny, has excellent comprehensive mechanical property.In addition, in preparation process, do not add the sintering aid of low melting point, improve the high-temperature service performance of boron nitride-base complex phase ceramic side seal material.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.3, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, depth of erosion is less than 700 μm, and properties meets side seal board service condition usability.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment boron nitride complex phase ceramic side seal board is made up of the additive of the boron nitride of 65 parts ~ 85 parts, the electric-melting zirconia of 15 parts ~ 35 parts, the silicon carbide of 5 parts ~ 15 parts and 5 parts ~ 10 parts by weight; Described additive is MAX phase
Described MAX phase is Nb
2alC, Zr
2alC, V
2alC, Ti
2snC, Zr
2snC, Ti
2alN, Ti
3alC
2or Nb
4alC
3.
Embodiment two: present embodiment and one of embodiment one or two are Ti unlike described MAX phase
3al (C
0.5, N
0.5)
2, (Nb, Zr)
2alC, (Ti, V)
2alC, (Ti, Nb)
2alC, (Ti, Cr)
2alC, (Ti, Ta)
2alC, (V, Nb)
2alC, (V, Ta)
2alC, (V, Cr)
2alC or (Ti, Hf)
2inC.Other is identical with embodiment one.
Embodiment three: present embodiment and one of embodiment one to two are Nb unlike described MAX phase
2alC-Zr
2alC, Zr
2alC-Zr
2snC or (Nb, Zr)
2alC-(V, Ta)
2alC.Other is identical with one of embodiment one to two.
Embodiment four: the preparation method of the boron nitride complex phase ceramic side seal board described in embodiment one carries out according to following steps:
One, take the additive of the boron nitride of 65 parts ~ 85 parts, the electric-melting zirconia of 15 parts ~ 35 parts, the silicon carbide of 5 parts ~ 15 parts and 5 parts ~ 10 parts by weight, additive is MAX phase is Nb
2alC, Zr
2alC, V
2alC, Ti
2snC, Zr
2snC, Ti
2alN, Ti
3alC
2or Nb
4alC
3;
Two, add in dispersion medium by boron nitride, electric-melting zirconia, silicon carbide and additive, wet ball grinding, after 10 ~ 48 hours, carries out dry 10h ~ 48h at 70 DEG C ~ 150 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 5 DEG C/min ~ 25 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1200 DEG C ~ 1400 DEG C time, be forced into 20MPa ~ 40MPa, then be warming up to 1400 DEG C ~ 1800 DEG C; heat-insulation pressure keeping 0.5 ~ 5h; again with 5 DEG C/min ~ 25 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
Embodiment five: present embodiment and embodiment four are dehydrated alcohol or ethanol mass concentration unlike the dispersion medium described in step 2 is the aqueous ethanolic solution of 55% ~ 95%.Other is identical with embodiment four.
Embodiment six: present embodiment and one of embodiment four to five are Ti unlike the MAX phase described in step one
3al (C
0.5, N
0.5)
2, (Nb, Zr)
2alC, (Ti, V)
2alC, (Ti, Nb)
2alC, (Ti, Cr)
2alC, (Ti, Ta)
2alC, (V, Nb)
2alC, (V, Ta)
2alC, (V, Cr)
2alC or (Ti, Hf)
2inC.Other is identical with one of embodiment four to five.
Embodiment seven: present embodiment and one of embodiment four to six are Nb unlike the MAX phase described in step one
2alC-Zr
2alC, Zr
2alC-Zr
2snC or (Nb, Zr)
2alC-(V, Ta)
2alC.Other is identical with one of embodiment four to six.
Embodiment eight: one of present embodiment and embodiment four to seven unlike in step 3 with 15 DEG C/min temperature rise rate, rise to 1500 DEG C, and apply the pressure of 30MPa, heat-insulation pressure keeping 3h.Other is identical with one of embodiment four to seven.
Adopt following experimental verification effect of the present invention:
Experiment one: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, the Nb of the boron nitride of 65 parts, the electric-melting zirconia of 15 parts, the silicon carbide of 10 parts and 10 parts is taken by weight
2alC;
Two, by boron nitride, electric-melting zirconia, silicon carbide and Nb
2alC adds in alcohol dispersion medium, and wet ball grinding, after 10 hours, carries out dry 10h at 80 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 10 DEG C/min temperature rise rate; start to apply pressure at 800 DEG C, 1200 DEG C time, be forced into 30MPa, and be warming up to 1600 DEG C; heat-insulation pressure keeping 1 hour under 1600 DEG C of temperature condition; room temperature is cooled to the rate of temperature fall of 15 ~ 20 DEG C/min, and simultaneously unloading pressure, obtain boron nitride complex phase ceramic side seal board.The density of prepared boron nitride complex phase ceramic side seal board can reach more than 97%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 350MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.26, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 700 μm, properties meets side seal board service condition usability.
Experiment two: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, the Ti of the boron nitride of 75 parts, the electric-melting zirconia of 10 parts, the silicon carbide of 10 parts and 5 parts is taken by weight
2alC;
Two, by boron nitride, electric-melting zirconia, silicon carbide and Ti
2alC adds in alcohol dispersion medium, and wet ball grinding, after 20 hours, carries out dry 20h at 90 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 15 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1400 DEG C time, be forced into 30MPa, then be warming up to 1700 DEG C; heat-insulation pressure keeping 1h; again with 8 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
The density of prepared boron nitride-base ceramic side seal board material can reach more than 97%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 300MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.3, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 700 μm, properties meets side seal board service condition usability.
Experiment three: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, the Ti of the boron nitride of 75 parts, the electric-melting zirconia of 10 parts, the silicon carbide of 10 parts and 5 parts is taken by weight
3alC
2;
Two, by boron nitride, electric-melting zirconia, silicon carbide and Ti
3alC
2add in alcohol dispersion medium, wet ball grinding, after 20 hours, carries out dry 20h at 90 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 15 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1400 DEG C time, be forced into 30MPa, then be warming up to 1700 DEG C; heat-insulation pressure keeping 1h; again with 8 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
The density of prepared boron nitride-base ceramic side seal board material can reach more than 97%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 320MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.28, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 700 μm, properties meets side seal board service condition usability.
Experiment four: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, the Nb of the boron nitride of 75 parts, the electric-melting zirconia of 10 parts, the silicon carbide of 10 parts and 5 parts is taken by weight
4alC
3;
Two, by boron nitride, electric-melting zirconia, silicon carbide and Nb
4alC
3add in alcohol dispersion medium, wet ball grinding, after 20 hours, carries out dry 20h at 90 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 15 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1400 DEG C time, be forced into 30MPa, then be warming up to 1700 DEG C; heat-insulation pressure keeping 1h; again with 8 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
The density of prepared boron nitride-base ceramic side seal board material can reach more than 97%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 340MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.26, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 700 μm, properties meets side seal board service condition usability.
Experiment five: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, take by weight the boron nitride of 75 parts, the electric-melting zirconia of 10 parts, the silicon carbide of 10 parts and 5 parts (Ti, Hf)
2inC;
Two, by boron nitride, electric-melting zirconia, silicon carbide and (Ti, Hf)
2inC adds in alcohol dispersion medium, and wet ball grinding, after 20 hours, carries out dry 20h at 90 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 15 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1400 DEG C time, be forced into 30MPa, then be warming up to 1700 DEG C; heat-insulation pressure keeping 1h; again with 8 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
The density of prepared boron nitride-base ceramic side seal board material can reach more than 97%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 350MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.25, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 650 μm, properties meets side seal board service condition usability.
Experiment six: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, take by weight the boron nitride of 75 parts, the electric-melting zirconia of 15 parts, the silicon carbide of 5 parts and 5 parts (Ti, Nb)
2alC;
Two, by boron nitride, electric-melting zirconia, silicon carbide and (Ti, Nb)
2alC adds in alcohol dispersion medium, and wet ball grinding, after 20 hours, carries out dry 20h at 90 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 15 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1400 DEG C time, be forced into 30MPa, then be warming up to 1700 DEG C; heat-insulation pressure keeping 1h; again with 8 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
The density of prepared boron nitride-base ceramic side seal board material can reach more than 97%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 350MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.3, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 600 μm, properties meets side seal board service condition usability.
Experiment seven: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, take by weight the boron nitride of 75 parts, the electric-melting zirconia of 10 parts, the silicon carbide of 10 parts and 5 parts (Ti, Cr)
2alC;
Two, by boron nitride, electric-melting zirconia, silicon carbide and (Ti, Cr)
2alC adds in alcohol dispersion medium, and wet ball grinding, after 20 hours, carries out dry 20h at 90 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 15 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1400 DEG C time, be forced into 30MPa, then be warming up to 1600 DEG C; heat-insulation pressure keeping 1h; again with 8 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
The density of prepared boron nitride-base ceramic side seal board material can reach more than 97%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 330MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.3, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 580 μm, properties meets side seal board service condition usability.
Experiment eight: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, the Nb of the boron nitride of 65 parts, the electric-melting zirconia of 25 parts, the silicon carbide of 5 parts and 5 parts is taken by weight
2alC-Zr
2alC;
Two, by boron nitride, electric-melting zirconia, silicon carbide and Nb
2alC-Zr
2alC adds in alcohol dispersion medium, and wet ball grinding, after 48 hours, carries out dry 40h at 150 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 15 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1400 DEG C time, be forced into 40MPa, then be warming up to 1500 DEG C; heat-insulation pressure keeping 1h; again with 15 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
The density of prepared boron nitride complex phase ceramic side seal board can reach more than 97%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 380MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.3, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 620 μm, properties meets side seal board service condition usability.
Experiment nine: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, the Zr of the boron nitride of 65 parts, the electric-melting zirconia of 20 parts, the silicon carbide of 5 parts and 10 parts is taken by weight
2alC-Zr
2snC;
Two, by boron nitride, electric-melting zirconia, silicon carbide and Zr
2alC-Zr
2snC adds in dispersion medium, and wet ball grinding, after 30 hours, carries out dry 20h at 100 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 9 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1400 DEG C time, be forced into 30MPa, then be warming up to 1600 DEG C; heat-insulation pressure keeping 1h; again with 15 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
The density of prepared boron nitride complex phase ceramic side seal board can reach more than 98%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 400MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.After the thermal shock of 1000 DEG C of thermal shock temperature difference, crackle is not had to produce at side seal board, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.26, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 650 μm, properties meets side seal board service condition usability.
Experiment ten: the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, take by weight the boron nitride of 65 parts, the electric-melting zirconia of 20 parts, the silicon carbide of 5 parts and 10 parts (Nb, Zr)
2alC-(V, Ta)
2alC;
Two, by boron nitride, electric-melting zirconia, silicon carbide and (Nb, Zr)
2alC-(V, Ta)
2alC adds in alcohol dispersion medium, and wet ball grinding, after 48 hours, carries out dry 40h at 150 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 20 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1400 DEG C time, be forced into 30MPa, then be warming up to 1600 DEG C; heat-insulation pressure keeping 1h; again with 20 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
The density of prepared boron nitride complex phase ceramic side seal board can reach more than 97%, makes to have excellent comprehensive mechanical property, and its bending strength can reach 350MPa, does not occur obvious ruckbildung in mechanical behavior under high temperature test.Side seal board does not have crackle to produce after the thermal shock of 1000 DEG C of thermal shock temperature difference, phenomenon of rupture is there is not 20 times through 800 DEG C of thermal shock temperature difference heat circulation thermal shocks, with crystallization roll, there is good frictional wear consistency, mutual frictional coefficient is less than 0.3, there is good anti-molten steel erosion performance, under 1600 DEG C of eating conditions, corrode 40 minutes depth of erosion and be less than 550 μm, properties meets side seal board service condition usability.
Claims (10)
1. boron nitride complex phase ceramic side seal board, is characterized in that boron nitride complex phase ceramic side seal board is made up of the additive of the boron nitride of 65 parts ~ 85 parts, the electric-melting zirconia of 15 parts ~ 35 parts, the silicon carbide of 5 parts ~ 15 parts and 5 parts ~ 10 parts by weight; Described additive is MAX phase.
2. boron nitride complex phase ceramic side seal board according to claim 1, is characterized in that described MAX phase is for Nb
2alC, Zr
2alC, V
2alC, Ti
2snC, Zr
2snC, Ti
2alN, Ti
3alC
2or Nb
4alC
3.
3. boron nitride complex phase ceramic side seal board according to claim 1, is characterized in that described MAX phase is for Ti
3al (C
0.5, N
0.5)
2, (Nb, Zr)
2alC, (Ti, V)
2alC, (Ti, Nb)
2alC, (Ti, Cr)
2alC, (Ti, Ta)
2alC, (V, Nb)
2alC, (V, Ta)
2alC, (V, Cr)
2alC or (Ti, Hf)
2inC.
4. boron nitride complex phase ceramic side seal board according to claim 1, is characterized in that described MAX phase is for Nb
2alC-Zr
2alC, Zr
2alC-Zr
2snC or (Nb, Zr)
2alC-(V, Ta)
2alC.
5. the preparation method of boron nitride complex phase ceramic side seal board, is characterized in that the preparation method of boron nitride complex phase ceramic side seal board carries out according to following steps:
One, the additive of the boron nitride of 65 parts ~ 85 parts, the electric-melting zirconia of 15 parts ~ 35 parts, the silicon carbide of 5 parts ~ 15 parts and 5 parts ~ 10 parts is taken by weight;
Two, add in dispersion medium by boron nitride, electric-melting zirconia, silicon carbide and additive, wet ball grinding, after 10 ~ 48 hours, carries out dry 10h ~ 48h at 70 DEG C ~ 150 DEG C, crosses 200 mesh sieves, obtains the composite powder mixed;
Three, composite powder is put into mould; under the condition of vacuum or inert atmosphere protection; with 5 DEG C/min ~ 25 DEG C/min temperature rise rate; be warming up to 800 DEG C to start to apply pressure, 1200 DEG C ~ 1400 DEG C time, be forced into 20MPa ~ 40MPa, then be warming up to 1400 DEG C ~ 1800 DEG C; heat-insulation pressure keeping 0.5 ~ 5h; again with 5 DEG C/min ~ 25 DEG C/min rate of temperature fall, be down to room temperature, obtain boron nitride complex phase ceramic side seal board.
6. the preparation method of boron nitride complex phase ceramic side seal board according to claim 5, is characterized in that the dispersion medium described in step 2 is alcohol, dehydrated alcohol or ethanol mass concentration is the aqueous ethanolic solution of 55% ~ 95%.
7. the preparation method of boron nitride complex phase ceramic side seal board according to claim 5 or 6, is characterized in that the MAX phase described in step one is for Nb
2alC, Zr
2alC, V
2alC, Ti
2snC, Zr
2snC, Ti
2alN, Ti
3alC
2or Nb
4alC
3.
8. the preparation method of boron nitride complex phase ceramic side seal board according to claim 5 or 6, is characterized in that the MAX phase described in step one is for Ti
3al (C
0.5, N
0.5)
2, (Nb, Zr)
2alC, (Ti, V)
2alC, (Ti, Nb)
2alC, (Ti, Cr)
2alC, (Ti, Ta)
2alC, (V, Nb)
2alC, (V, Ta)
2alC, (V, Cr)
2alC or (Ti, Hf)
2inC.
9. the preparation method of boron nitride complex phase ceramic side seal board according to claim 5 or 6, is characterized in that the MAX phase described in step one is for Nb
2alC-Zr
2alC, Zr
2alC-Zr
2snC or (Nb, Zr)
2alC-(V, Ta)
2alC.
10. the preparation method of boron nitride complex phase ceramic side seal board according to claim 5 or 6, to is characterized in that in step 3, with 15 DEG C/min temperature rise rate, rising to 1500 DEG C, and applying the pressure of 30MPa, heat-insulation pressure keeping 3h.
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