CN100588637C - The in-situ reaction preparation method of zirconium diboride base composite phase ceramic - Google Patents
The in-situ reaction preparation method of zirconium diboride base composite phase ceramic Download PDFInfo
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Abstract
The present invention relates to zirconium diboride (ZrB
2) in-situ reaction preparation method of base complex phase ceramic.The present invention is a raw material with common micron order commercial powder cheaply, mixes the back and adopts discharge plasma sintering method to carry out Fast Sintering, and sintering range is 1300～1500 ℃; The temperature rise rate scope is 80～200 ℃/min; The sintering pressure scope is 10～100MPa; Soaking time is 0～30min.The present invention utilizes the high reactivity of raw material reaction heat release and the synthetic newly-generated phase that obtains of reaction, prepares fine and close ZrB at a lower temperature
2Base complex phase ceramic; The material that obtains has the complex phase of two-phase or two-phase and forms structure, and each phase content can be regulated by changing the starting raw material proportioning; The material fine microstructure for preparing, tiny by reacting synthetic each phase crystal grain that obtains, second phase or the third phase of generation are evenly distributed on ZrB
2Form three-dimensional network between the particle, suppress ZrB
2Growing up of crystal grain need not to add other sintering agents, sintering efficient height.
Description
Technical field
The present invention relates to zirconium diboride (ZrB
2) in-situ reaction preparation method of base complex phase ceramic, comprise zirconium diboride-zirconium carbide-silicon carbide (ZrB
2-ZrC-SiC), zirconium diboride-zirconium carbide-molybdenum disilicide (ZrB
2-ZrC-MoSi
2), zirconium diboride-titanium boride-zirconium carbide (ZrB
2-TiB
2-ZrC) zirconium diboride-zirconium nitride-silicon carbide (ZrB
2-ZrN-SiC), zirconium diboride-zirconium carbide (ZrB
2-ZrC), zirconium diboride-silicon carbide (ZrB
2-SiC) the in-situ reaction preparation method of complex phase ceramic.Belong to non-oxidized substance complex phase ceramic field.
Background technology
Ultrahigh-temperature pottery (UHTC) material has hot strength and high-temperature oxidation resistance, flight in the time of can adapting to superelevation velocity of sound length, atmospheric layer reenter, stride extreme environments such as aerial flight and rocket propulsion system, can be used for various key positions or parts such as aircraft nose cone, the leading edge of a wing, numbers of hot-side engine.The ultrahigh-temperature pottery is mainly the polynary composite ultra-high temperature stupalith system of being made up of high-melting-point boride, carbide and oxide compound.The transition metal compounds of group, ZrB
2, HfB
2, TaB
2, TiB
2, TiC, TaC, fusing points such as ZrC and HfC are about 3000 ℃, and the good thermo-chemical stability of these compounds makes them can descend the candidate material of use as extreme environment.ZrB wherein
2Have also simultaneously that electrical and thermal conductivity is good, characteristics such as heat-shock resistance, resistance to chemical corrosion and density are relatively low, become the emphasis of ultrahigh-temperature ceramic research.Consider that from practical application single boride ceramics can't satisfy desired physics, chemistry and structure properties under ultra-high temperature condition simultaneously.Selecting different materials to carry out reasonable combination from the material design angle is the approach that addresses this problem.
Give full play to ZrB
2The performance of base complex phase ceramic material, obtain high performance superhigh temperature ceramic material, guarantee the mechanical behavior under high temperature and the high-temperature oxidation resistance of material, not only need its composition is designed, also need to control, go out densification, be evenly distributed and sintered compact that crystal grain is tiny mutually by certain prepared to its preparation.So the preparation science of superhigh temperature ceramic material has become important research project.The research focus mainly concentrates on oxidation-resistance (by additive, as carbide, silicide etc.), highly malleablized structure design (improve hot strength and toughness, can utilize particle or fiber reinforcement), preparation technology (how reducing sintering temperature) at present.
ZrB
2Complex phase ceramic is generally prepared by direct mixing method, and F.Monteverde is at ZrB
2In directly sneak into MoSi
2(International Journal of Applied Ceramic Technology, 3,32,2006), superfine (Applied Physics, 82A, 329,2006) the grade in an imperial examination two-phase obtains sintered compact by hot-press method then, and people such as Diletta Sciti utilize fine powder, at ZrB
2The middle MoSi that adds
2Carry out normal pressure-sintered (Journal of Materials Research, 20,922,2005).But picture ZrB
2, TiB
2, non-oxide ceramicses such as SiC, ZrC self-diffusion coefficient very little, even hot pressed sintering also is difficult to obtain fine and close sintered compact, the intensity of material, erosion resistance etc. are difficult to reach service requirements.Add a small amount of metal and can significantly improve sintering character, as F.Monteverde (Journal of the European CeramicSociety, 22,279,2002) as Ni) introduce shown in the content.But these metal additives can remain in the crystal boundary place of pottery, thereby reduce the mechanical behavior under high temperature and the corrosion resistance of material.Utilize the method for reaction hot-pressing to prepare ZrB in relatively low temperature under need not the situation of sintering aid
2-SiC complex phase ceramic, open shown in the flat P2002-249378 and G.J.Zhang (Journal of the AmericanCeramic Society as the spy, 83,2330,2000) carry in the text, and it is tiny than primary particle to obtain each phase particle size, but still needs at high temperature to be incubated for a long time (60min) for the sintered compact that obtains densification, preparation cycle is longer, and is incubated the maintenance that is unfavorable for reacting the thin crystalline substance that obtains for a long time.Utilize discharge plasma sintering method, as Kyoung Hun Kim, at ZrB
2In directly sneak into ZrC, obtain sintered compact (Materials Characterization, 50,31,2003) by discharge plasma sintering method then, need not sintering aid, when reducing sintering temperature, prepare complex phase ceramic fast, and ZrB
2, the ZrC particle compares with initial powder and changes not quite, but still needs 1800 ℃ high temperature for reaching 97% relative density sintering temperature.
Summary of the invention
The object of the present invention is to provide a kind of ZrB
2The in-situ reaction preparation method of base complex phase ceramic.Utilize this method cost low, less energy consumption, technology is simple, preparation cycle is short, and utilize this method can obtain the purity height, be evenly distributed mutually, crystal grain is tiny, the ZrB of good mechanical performance
2The base composite diphase material.
The present invention realizes with combining of discharge plasma sintering advantage with reaction sintering, prepares ZrB at a lower temperature fast
2Base complex phase ceramic.The prepared material of the present invention has binary or the above phase composite structure of binary, and complicated phase composite can improve phase composite and the microstructural stability of complex phase ceramic under ultra-high temperature condition to a certain extent; Each interphase interface is pure, helps the mechanical behavior under high temperature and the oxidation-resistance of material; Second phase or third phase that reaction generates are evenly distributed on ZrB
2Around the particle or inside can fine inhibition ZrB
2Particulate is grown up; Sintering time is short, helps thin brilliant formation; Electric current increases the controllability of electro-conductive material preparation directly by sample.
Specifically, the present invention adopts and selects commercial Zr, ZrSi
2, B
4C, BN, Mo, Si and Ti powder are raw material.The design raw material is formed proportioning, utilizes reaction formula:
2Zr+B
4C+Si＝2ZrB
2+SiC (1)
3Zr+B
4C＝2ZrB
2+ZrC (2)
(2+x)Zr+B
4C+(1-x)Si＝2ZrB
2+xZrC+(1-x)SiC 0＜x＜1 (3)
(3-x)Zr+B
4C+xTi＝(2-x)ZrB
2+ZrC+xTiB
2 0＜x＜0.6 (4)
3Zr+B
4C+xSi+xC＝2ZrB
2+ZrC+xSiC 0＜x＜1.6 (5)
3Zr+B
4C+2xSi+xMo＝2ZrB
2+ZrC+xMoSi
2 0＜x＜0.8 (6)
(2+3x)Zr+B
4C+2xBN+Si＝(2+x)ZrB
2+2xZrN+SiC 0＜x＜2.4 (7)
xZr+ZrSi
2+0.5(1+x)B
4C＝(1+x)ZrB
2+2SiC+0.5(x-3)C 3＜x (8)
Obtaining phase composite by SPS original position rapid reaction sintering is ZrB
2-SiC, ZrB
2-ZrC, ZrB
2-ZrC-SiC, ZrB
2-ZrC-MoSi
2, ZrB
2-ZrC-TiB
2, ZrB
2The composite diphase material of-ZrN-SiC.Utilize the stock yard exothermic heat of reaction can reduce sintering temperature, utilize that the synthetic high reactivity that obtains of reaction is newly-generated to can be used to promote ZrB mutually
2Base complex phase ceramic densification under lower temperature; Characteristics such as, sintering time fast in conjunction with discharge plasma sintering (SPS) technology heat-up rate is short, electric field activating effect and pulsed current shock effect can prepare uniform microstructure, matrix material that crystal grain is tiny; In the reaction process new thing generate mutually and in this course from purification effect, can obtain purified composite diphase material interface.And utilize generated in-situ second phase, as SiC, ZrC, MoSi
2Deng being evenly distributed on ZrB
2Form three-dimensional network between the particle, can suppress ZrB
2Growing up of crystal grain.Complicated phase composite and purified material interface can improve phase composite and the microstructural stability of complex phase ceramic under ultra-high temperature condition to a certain extent, provide possibility for this class material can use under ultrahigh-temperature.By reaction in obtain second mutually or the content of third phase regulate by changing the starting raw material proportioning.
Method feature provided by the invention is at first to design raw material and forms proportioning, utilize the three-dimensional blender machine to carry out batch mixing then, carry out SPS reaction in sintering at last, main by control SPS sintering process parameter, comprise sintering temperature, pressure, temperature rise rate, soaking time etc.Following each step is specifically arranged:
1, the selection of material powder and preparation
With commercially available commercial Zr, ZrSi
2, B
4C, BN, Mo, Si and Ti powder are raw material.B used in the present invention
4C, BN are the powder less than 5 microns, other raw materials Zr, ZrSi
2, Mo, Ti and Si be 300 orders (≤48 μ m) powders, wherein the largest particle particle diameter is about 50 μ m.Various raw material powders are made into mixed powder according to a certain ratio, add dehydrated alcohol and are made into slurry, utilize the three-dimensional blender machine to carry out batch mixing.The wet mixing time is 10～30 hours, and drying is put into the three-dimensional blender machine at last once more and carried out 0.5～2 hour dried mixing, and obtains the raw material mixed powder.
2, discharge plasma quick in situ reaction sintering
The gained powder packed into to be positioned in the heating chamber of discharging plasma sintering equipment behind the graphite jig, carries out discharge plasma sintering after vacuumizing.In preparation process, need strict control process parameters, comprise sintering temperature, pressure, temperature rise rate, soaking time etc.Wherein, temperature rise rate is regulated by changing the discharge plasma pulsed current.Sintering range is 1300～1500 ℃; The temperature rise rate scope is 80～200 ℃/min; The sintering pressure scope is 10～100MPa; Soaking time is 0～30min.
In sum, the invention is characterized in: adopt micron order common commercial raw material, use slightly and also can obtain to have the binary or the polybasic composite diphase material at fine microstructure and pure interface than the raw material of low-purity; Technology is simple, the cycle is short, energy consumption is low, and reaction is synthetic once to be finished with sintering; Microstructure is controlled, and electric current has increased the controllability to the conducting sample preparation directly by sample in the sintering process.
The invention provides a kind of SPS of utilization quick in situ reaction sintering and prepare ZrB
2The method of base complex phase ceramic.Adopt common commercial powder, with the control microstructure, prepare that particle is tiny, phase composition is evenly distributed, mechanical property and the good material of electroconductibility by the quick densifying reaction sintering.Workability, the reliability of products of material are greatly improved.And this method preparation cycle is short, energy consumption is low, environmental friendliness, and production cost significantly reduces, thereby has good industrial prospect.
Description of drawings
Fig. 1 is the X-ray diffractogram of embodiment 1;
Fig. 2 is the backscattered electron photo of the material polished surface of embodiment 1;
Fig. 3 is the scanning electron microscope (SEM) of the material sintered compact fracture of embodiment 1;
Fig. 4 is the X-ray diffractogram of embodiment 5;
Fig. 5 is each first vegetarian noodles distribution situation in the material of embodiment 5, and wherein: (a) is the backscattered electron photo of material polished surface among the figure, (b), (c), (d), (e) represent the distribution situation of B, Mo, C, Zr element respectively.
Embodiment
The present invention will describe in detail with the following examples, but the present invention is not limited by the following examples.
Embodiment 1
For preparation consists of ZrB
2The composite diphase material of-SiC 25% volume content at first carries out proportion design, and reaction equation is as follows:
2Zr+B
4C+Si＝2ZrB
2+SiC ①
Prepare burden according to design result, with commercial materials Zr, B
4C and Si powder mix, and are medium wet mixing 10～30 hours with dehydrated alcohol, obtain uniform slurry, this slurry is done after the thorough drying in baking oven once more mixed 0.5～2 hour, obtain the raw material mixed powder at last.Taking by weighing the powder that mixes packs into to be placed in the discharging plasma sintering equipment (SPS) behind the graphite jig and carries out sintering.
The SPS preparation process is carried out under vacuum condition, and sintering temperature is 1450 ℃, 80～150 ℃/min of temperature rise rate, and soaking time is 0～30min, the plus-pressure 10～100MPa of holding stage institute.The sample Vickers' hardness is 17～19GPa, and fracture toughness property is 3.5～4.5MPam
1/2
Embodiment 2
For the preparation phase composite is ZrB
2The composite diphase material of-ZrC 30% volume content at first carries out proportion design, and reaction equation is as follows:
3Zr+B
4C＝2ZrB
2+ZrC ②
Prepare burden according to design result, with commercial materials Zr and B
4The C powder mixes, and is medium wet mixing 10～30 hours with dehydrated alcohol, obtains uniform slurry, this slurry is done after the thorough drying in baking oven once more mixed 0.5～2 hour, obtains the raw material mixed powder at last.Taking by weighing the powder that mixes packs into to be placed in the discharging plasma sintering equipment (SPS) behind the graphite jig and carries out sintering.
The SPS preparation process is carried out under vacuum condition, and sintering temperature is 1500 ℃, 80～150 ℃/min of temperature rise rate, and soaking time is 0～30min, the plus-pressure 10～100MPa of holding stage institute.The sample Vickers' hardness is 17.0～19.0GPa, and fracture toughness property is 2.5～3.5MPam
1/2
Embodiment 3
For the preparation phase composite is ZrB
2-ZrC-TiB
2Composite diphase material, at first carry out proportion design, reaction equation is as follows:
(3-x)Zr+B
4C+xTi＝(2-x)ZrB
2+ZrC+xTiB
2 0＜x＜0.6 ④
With x=0.5 is example, promptly prepares each phase volume ratio V of material
ZrB2: V
ZrC: V
TiB2=54: 31: 15.Prepare burden according to design result, with commercial materials Zr, B
4C and Ti powder mix, and are medium wet mixing 10～30 hours with dehydrated alcohol, obtain uniform slurry, this slurry is done after the thorough drying in baking oven once more mixed 0.5～2 hour, obtain the raw material mixed powder at last.Taking by weighing the powder that mixes packs into to be placed in the discharging plasma sintering equipment (SPS) behind the graphite jig and carries out sintering.
The SPS preparation process is carried out under vacuum condition, and sintering temperature is 1380 ℃, 80～150 ℃/min of temperature rise rate, and soaking time is 3～12min, the plus-pressure 20～65MPa of holding stage institute.The sample Vickers' hardness is 16.5～19.0GPa, and fracture toughness property is 4.0～5.5MPam
1/2
Embodiment 4
For the preparation phase composite is ZrB
2The composite diphase material of-ZrC-SiC at first carries out proportion design, and reaction equation is as follows:
(2+x)Zr+B
4C+(1-x)Si＝2ZrB
2+xZrC+(1-x)SiC 0＜x＜1 ③
3Zr+B
4C+ySi+yC＝2ZrB
2+ZrC+ySiC 0＜y＜1.6 ⑤
Utilize above-mentioned two reaction equations all can obtain phase composite and be ZrB
2The composite diphase material of-ZrC-SiC is with 3Zr+B
4C+ySi+yC, y=0.46 are example, promptly prepare each phase volume ratio V of material
ZrB2: V
ZrC: V
SiC=63: 27: 10.Prepare burden according to design result, with commercial materials Zr, B
4C, Si and C powder mix, and are medium wet mixing 10～30 hours with dehydrated alcohol, obtain uniform slurry, this slurry is done after the thorough drying in baking oven once more mixed 0.5～2 hour, obtain the raw material mixed powder at last.Taking by weighing the powder that mixes packs into to be placed in the discharging plasma sintering equipment (SPS) behind the graphite jig and carries out sintering.
The SPS preparation process is carried out under vacuum condition, and sintering temperature is 1450 ℃, 80～150 ℃/min of temperature rise rate, and soaking time is 0～30min, the plus-pressure 10～100MPa of holding stage institute.The sample Vickers' hardness is 16.5～19.0GPa, and fracture toughness property is 3.0～4.5MPam
1/2
For the preparation phase composite is ZrB
2-ZrC-MoSi
2Composite diphase material, at first carry out proportion design, reaction equation is as follows:
3Zr+B
4C+2xSi+xMo＝2ZrB
2+ZrC+xMoSi
2 0＜x＜0.8 ⑥
With x=0.5 is example, promptly prepares each phase volume ratio V of material
ZrB2: V
ZrC: V
MoSi2=57: 25: 18.Prepare burden according to design result, with commercial materials Zr, B
4C, Si and Mo powder mix, and are medium wet mixing 10～30 hours with dehydrated alcohol, obtain uniform slurry, this slurry is done after the thorough drying in baking oven once more mixed 0.5～2 hour, obtain the raw material mixed powder at last.Taking by weighing the powder that mixes packs into to be placed in the discharging plasma sintering equipment (SPS) behind the graphite jig and carries out sintering.
The SPS preparation process is carried out under vacuum condition, and sintering temperature is 1380 ℃, 80～150 ℃/min of temperature rise rate, and soaking time is 0～30min, the plus-pressure 10～100MPa of holding stage institute.The sample Vickers' hardness is 15.5～17.0GPa, and fracture toughness property is 4.0～5.5MPam
1/2
Embodiment 6
For the preparation phase composite is ZrB
2The composite diphase material of-ZrN-SiC at first carries out proportion design, and reaction equation is as follows:
(2+3x)Zr+B
4C+2xBN+Si＝(2+x)ZrB
2+2xZrN+SiC?0＜x＜2.4 ⑦
With x=0.09 is example, promptly prepares each phase volume ratio V of material
ZrB2: V
ZrN: V
SiC=72: 5: 23.Prepare burden according to design result, with commercial materials Zr, B
4C, BN and Si powder mix, and are medium wet mixing 10～30 hours with dehydrated alcohol, obtain uniform slurry, this slurry is done after the thorough drying in baking oven once more mixed 0.5～2 hour, obtain the raw material mixed powder at last.Taking by weighing the powder that mixes packs into to be placed in the discharging plasma sintering equipment (SPS) behind the graphite jig and carries out sintering.
The SPS preparation process is carried out under vacuum condition, and sintering temperature is 1400 ℃, 80～150 ℃/min of temperature rise rate, and soaking time is 0～30min, the plus-pressure 10～100MPa of holding stage institute.The sample Vickers' hardness is 15.5～17.0GPa, and fracture toughness property is 4.0～5.0MPam
1/2
Embodiment 7
For the preparation phase composite is ZrB
2The composite diphase material of-SiC at first carries out proportion design, and reaction equation is as follows:
xZr+ZrSi
2+0.5(1+x)B
4C＝(1+x)ZrB
2+2SiC+0.5(x-3)C 3＜x ⑧
With x=4 is example, promptly prepares each phase volume ratio V of material
ZrB2: V
SiC: V
C=77: 21: 2.Prepare burden according to design result, with commercial materials Zr, ZrSi
2, B
4C and C powder mix, and are medium wet mixing 10～30 hours with dehydrated alcohol, obtain uniform slurry, this slurry is done after the thorough drying in baking oven once more mixed 0.5～2 hour, obtain the raw material mixed powder at last.Taking by weighing the powder that mixes packs into to be placed in the discharging plasma sintering equipment (SPS) behind the graphite jig and carries out sintering.
The SPS preparation process is carried out under vacuum condition, and sintering temperature is 1450 ℃, 80～150 ℃/min of temperature rise rate, and soaking time is 3～12min, the plus-pressure 20～65MPa of holding stage institute.The sample Vickers' hardness is 17～19GPa, and fracture toughness property is 3.5～4.5MPam
1/2
Claims (5)
1, ZrB
2The preparation method of the reaction in of base complex phase ceramic, it is characterized in that the material powder that mixes being placed in the graphite jig by generating two-phase or triphasic complex phase ceramic reaction formula, utilize discharge plasma sintering method reaction sintering under vacuum condition, processing step is:
(1) combination treatment of raw material: various raw material powders are made into mixed powder by required proportioning, add dehydrated alcohol and are made into slurry, utilize mixer to carry out batch mixing, and mixing time is 10～30 hours;
(2) slurry drying behind the ball milling obtains powder, puts into mixer once more and carries out doing in 0.5～2 hour mixed;
(3) reaction in Fast Sintering: the gained powder packed into to be positioned in the heating chamber of discharging plasma sintering equipment behind the graphite jig, carries out discharge plasma sintering after vacuumizing, and sintering range is 1300～1500 ℃; The temperature rise rate scope is 80～200 ℃/min; The sintering pressure scope is 10～100MPa; Soaking time is 0～30min;
The reaction formula of described generation two-phase or triphasic complex phase ceramic reaction in is any in following 8 kinds:
2Zr+B
4C+Si＝2ZrB
2+SiC (1)
3Zr+B
4C＝2ZrB
2+ZrC (2)
(2+x)Zr+B
4C+(1-x)Si＝2ZrB
2+xZrC+(1-x)SiC 0＜x＜1 (3)
(3-x)Zr+B
4C+xTi＝(2-x)ZrB
2+ZrC+xTiB
2 0＜x＜0.6 (4)
3Zr+B
4C+xSi+xC＝2ZrB
2+ZrC+xSiC 0＜x＜1.6 (5)
3Zr+B
4C+2xSi+xMo＝2ZrB
2+ZrC+xMoSi
2 0＜x＜0.8 (6)
(2+3x)Zr+B
4C+2xBN+Si＝(2+x)ZrB
2+2xZrN+SiC 0＜x＜2.4 (7)
xZr+ZrSi
2+0.5(1+x)B
4C＝(1+x)ZrB
2+2SiC+0.5(x-3)C 3＜x (8)
2, by the described ZrB of claim 1
2The preparation method of the reaction in of base complex phase ceramic is characterized in that the raw material that uses is common commercial Zr, ZrSi
2, B
4C, BN, Mo, Si and Ti powder, wherein B
4C or BN are the powder less than 5 microns, Zr, ZrSi
2, Mo, Ti or Si be particle diameter≤48 μ m powders.
3, by the described ZrB of claim 1
2The preparation method of the reaction in of base complex phase ceramic is characterized in that each phase content of being obtained by reaction in can regulate by changing the starting raw material proportioning.
4, by claim 1,2 or 3 any described ZrB
2The preparation method of the reaction in of base complex phase ceramic is characterized in that second phase or the third phase that generate are evenly distributed on ZrB
2Form three-dimensional network between the particle, suppress principal crystalline phase ZrB
2Growing up of crystal grain.
5, by the described ZrB of claim 1
2The preparation method of the reaction in of base complex phase ceramic is characterized in that temperature rise rate regulates by changing the discharge plasma pulsed current.
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Citations (1)
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| JP2002249378A (en) * | 2001-02-22 | 2002-09-06 | National Institute Of Advanced Industrial & Technology | Reaction synthesis of high strength zorconium diboride- silicon carbide composite |
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