CN105693261A - ZrB2-SiC-Cf ultra-high temperature ceramic composite material and preparation method thereof - Google Patents

ZrB2-SiC-Cf ultra-high temperature ceramic composite material and preparation method thereof Download PDF

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CN105693261A
CN105693261A CN201610015369.9A CN201610015369A CN105693261A CN 105693261 A CN105693261 A CN 105693261A CN 201610015369 A CN201610015369 A CN 201610015369A CN 105693261 A CN105693261 A CN 105693261A
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zrb
ceramic composite
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temperature ceramic
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胡平
桂凯旋
张幸红
方成
徐建国
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Harbin Institute of Technology
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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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    • C04B35/58078—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on zirconium or hafnium borides
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract

The invention discloses a ZrB2-SiC-Cf ultra-high temperature ceramic composite material and a preparation method thereof, belongs to the field of ultra-high temperature ceramic materials, and aims at overcoming the intrinsic brittleness of ZrB2-based ultra-high temperature ceramics.The composite material is prepared from, by volume, 30%-60% of ZrB2 powder with the particle size ranging from 100 nm to 200 nm, 15%-30% of SiC powder with the particle size ranging from 100 nm to 500 nm and 20%-50% of carbon fibers.The method comprises the steps that 1, the ZrB2 powder, the SiC powder and the carbon fibers are added into absolute ethyl alcohol for ultrasonic cleaning; 2, ball milling and drying are conducted; 3, grinding and sieving are conducted, the mixture is put into a graphite die, hot-pressure sintering is conducted at the temperature of 1,400-1,500 DEG C and pressure of 20-40 MPa, cooling is conducted to reach the room temperature, and the ZrB2-SiC-Cf ultra-high temperature ceramic composite material is obtained.The ZrB2-SiC-Cf ultra-high temperature ceramic composite material and the preparation method thereof have the advantages that the sintering temperature is low, the fiber damage is small, and the failure strain of the composite material is high; the sintering temperature ranges from 1,400 DEG C to 1,500 DEG C; the ultra-high temperature ceramic composite material can be applied to the fields of ultra-high temperature thermal-protection structure materials and the like.

Description

A kind of ZrB2-SiC-Cf ultrahigh temperature ceramic composite and preparation method thereof
Technical field
The invention belongs to ultrahigh temperature ceramic composite field；It is specifically related to a kind of ZrB2-SiC-CfUltrahigh temperature ceramic composite and preparation method thereof。
Background technology
Superhigh temperature ceramics mainly includes the boride of some magnesium-yttrium-transition metals, carbide and nitride (such as ZrB2、HfB2, TaC, HfC, ZrC, HfN etc.), their fusing point, all more than 3000 DEG C, is the very potential superhigh temperature thermal protection struc ture material of one。In these superhigh temperature ceramics, ZrB2Based ultra-high temperature pottery becomes one very promising non-ablative type superhigh temperature heat insulation material because having higher thermal conductivity, moderate thermal coefficient of expansion and good antioxidation ablation property, can be used for the crucial hot-end component of reentry vehicle, the nose cone of endoatmosphere hypersonic aircraft, leading edge and engine chamber, aspects such as promoting high-speed aircraft aeroperformance, control ability, flight efficiency will be had revolutionary contribution。But, the intrinsic fragility of such material limits its engineer applied at present。For this problem, domestic and international research worker takes accomplished in many ways ZrB2Based ultra-high temperature pottery toughness reinforcing, such as yttria stabilizator, soft mutually toughness reinforcing, crystal whisker toughened and fiber reinforced。These methods, while improve ZrB to a certain extent2The fracture toughness of based ultra-high temperature pottery, but such material still shows brittle fracture in fracture process, it is impossible to meet the demand of engineer applied。Wherein, carbon fiber is with a wide range of applications in toughness reinforcing superhigh temperature ceramics。But, carbon fiber-reinforced ultrahigh temperature ceramic composite generally requires and is sintered at very high temperatures, carbon fiber is made to be easy at high temperature react the degeneration of the damage causing its structure and performance with superhigh temperature ceramics matrix, thus greatly reducing the toughening effect of fiber。Therefore, the sintering temperature of ultrahigh temperature ceramic composite is reduced, it is suppressed that carbon fiber, at the performance degradation of sintering process, becomes the key problem preparing carbon fiber-reinforced ultrahigh temperature ceramic composite。Research shows, the sintering temperature of ceramic material is closely related with the size of original powder body, and the reduction of diameter of particle can increase its surface energy, improves the sintering activity of powder body, reduces the sintering temperature of powder body。
Adopt nanometer ZrB2Powder body substitutes micron ZrB2Powder body prepares ZrB2-SiC-CfUltrahigh temperature ceramic composite is expected to reduce the sintering temperature of such material, it is suppressed that the structural damage of carbon fiber and performance degradation, gives full play to the toughening effect of carbon fiber。But, the reunion of powder body can be caused again when diameter of particle is reduced to nanoscale, and along with its reunion degree of reduction of diameter of particle is more serious。The reunion of powder body make it occur in sintering process aggregate preferentially sinters and the phenomenon of crystal grain fast growth, hinder the low temperature densification of powder body and cause the inhomogeneities of sintered body microstructure。It addition, ZrB2The oxygen impurities of powder surface can suppress the densification behavior in its sintering process, and along with the Surface Oxygen impurity reducing its powder body of diameter of particle is more many。Accordingly, it would be desirable to select the ZrB of appropriate particle size2Powder body is alleviated the reunion of nano-powder and is reduced the Surface Oxygen impurity of powder body simultaneously, promotes ZrB2The low temperature densification of based ultra-high temperature ceramic composite。
Summary of the invention
It is contemplated that overcome ZrB2The intrinsic fragility of based ultra-high temperature pottery, and provide a kind of ZrB2-SiC-CfUltrahigh temperature ceramic composite and preparation method thereof。The present invention adopts nanometer ZrB2Powder body carries out low temperature hot-press sintering and prepares carbon fiber-reinforced ZrB2The method of-SiC ultrahigh temperature ceramic composite, has that sintering temperature is low, fibre damage is little, a composite failure strain high。
For solving above-mentioned technical problem, ZrB in the present invention2-SiC-CfUltrahigh temperature ceramic composite by volume mark is by 30%～60%ZrB2Powder body, 15%～30%SiC powder body and what 20%～50% carbon fiber was made, wherein, described ZrB2Diameter of particle is (100～200) nm, and described SiC diameter of particle is (100～500) nm。
A kind of ZrB in the present invention2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, by ZrB2Powder body, SiC powder body and carbon fiber join in dehydrated alcohol, carry out ultrasonic cleaning；
Step 2, it is subsequently poured in politef ball grinder and carries out ball milling 8～24h, then vacuum rotating dries and obtains powder body A；Step 3, by the powder body A obtained in step 2 grind sieve, load graphite jig, utilize vacuum sintering funace temperature be (1400～1500) DEG C, pressure carry out hot pressed sintering (1～3) h under (20～40) MPa, it is subsequently cooled to room temperature, obtains ZrB2-SiC-CfUltrahigh temperature ceramic composite。
In step 2, abrading-ball adopts WC ball, and rotational speed of ball-mill is (200～250) r/min。
Utilizing Rotary Evaporators to carry out vacuum rotating in step 2 to dry, rotating speed is (30～50) r/min, and baking temperature is (70～90) DEG C。
Nanometer ZrB that the present invention adopts mean diameter to be 100～200nm2Powder body prepares carbon fiber-reinforced ZrB at low temperatures2-SiC ultrahigh temperature ceramic composite, the present invention is used to prepare the sintering temperature (1400～1500 DEG C) of superhigh temperature ceramics significantly lower than the sintering temperature (1900～2000 DEG C) preparing superhigh temperature ceramics by traditional micropowder, it is suppressed that the structural damage of fiber。The composite consistency obtained reaches 80.4～91.6%, and critical crack size and failure strain all increase along with the increase of fiber content。When fiber volume fraction is 50%, the critical crack size of composite and failure strain respectively reach 169.3 μm and 0.32%, and composite shows the feature of non-brittle fracture when fiber volume fraction reaches more than 40%。
The engineer applied of the carbon fiber-reinforced ultrahigh temperature ceramic composite of the present invention is limited by fibre structure damage and the performance degradation that carbon fiber and ultra-high temperature ceramic powder cause in high temperature recombination process。The sintering temperature reducing carbon fiber-reinforced ultrahigh temperature ceramic composite can effectively suppress fibre damage, improves the reliability of composite。The surface of powder body can be the important driving force in sintering process, and the particle diameter reducing powder body can promote its sintering activity, promotes the low temperature densification of powder body。But the reduction of particle diameter can cause the reunion of powder body and the increase of powder surface oxygen impurities, it is suppressed that the low temperature densification of powder body。The powder body adopting appropriate particle size scope can effectively be alleviated the reunion of nano-powder and reduce its Surface Oxygen impurity, reduces the sintering temperature of superhigh temperature ceramics, it is achieved the low-temperature sintering of carbon fiber-reinforced ultrahigh temperature ceramic composite。
The ultrahigh temperature ceramic composite of the present invention can be applicable to the fields such as superhigh temperature thermal protection struc ture material。
Accompanying drawing explanation
Fig. 1 is the carbon fiber-reinforced ultrahigh temperature ceramic composite fracture apperance of detailed description of the invention three；Fig. 2 is the stress-strain diagram of the ultrahigh temperature ceramic composite of detailed description of the invention two to five。
Detailed description of the invention
Technical solution of the present invention is not limited to and the detailed description of the invention of act set forth below, also includes the combination in any between each detailed description of the invention。
Detailed description of the invention one: a kind of ZrB in present embodiment2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, it is the ZrB of 150nm by mean diameter2Powder body, mean diameter are the SiC powder body of 200nm and carbon fiber joins in dehydrated alcohol (volume of dehydrated alcohol is about powder body and long-pending 30 times of total fiber), carry out ultrasonic cleaning about 30 minutes；Wherein ZrB2Volume fraction be 60%, the volume fraction of SiC is 20%, and the volume fraction of carbon fiber is 20%；
Step 2, being subsequently poured in politef ball grinder and carry out ball milling 10h, abrading-ball adopts WC ball。Rotational speed of ball-mill is 220r/min, and recycling Rotary Evaporators is 35r/min, temperature at rotating speed is that under 80 DEG C of conditions, vacuum rotating dries, and obtains powder body A；
Step 3, the powder body A obtained is ground sieve in step 2, load graphite jig, utilize vacuum sintering funace temperature be 1400 DEG C, pressure for carrying out hot pressed sintering 2h under 30MPa, be subsequently cooled to room temperature, obtain ZrB2-SiC-CfUltrahigh temperature ceramic composite。
The ZrB that present embodiment method obtains2-SiC-CfUltrahigh temperature ceramic composite consistency is 90.2%, and critical crack size is 58.9 μm, and failure strain reaches 0.11%, and fibre damage is effectively suppressed。
Detailed description of the invention two: a kind of ZrB in present embodiment2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, it is the ZrB of 150nm by mean diameter2Powder body, mean diameter are the SiC powder body of 500nm and carbon fiber joins in dehydrated alcohol (volume of dehydrated alcohol is about powder body and long-pending 30 times of total fiber), carry out ultrasonic cleaning about 30 minutes；Wherein ZrB2Volume fraction be 60%, the volume fraction of SiC is 20%, and the volume fraction of carbon fiber is 20%；
Step 2, being subsequently poured in politef ball grinder and carry out ball milling 10h, abrading-ball adopts WC ball。Rotational speed of ball-mill is 220r/min, and recycling Rotary Evaporators is 35r/min, temperature at rotating speed is that under 80 DEG C of conditions, vacuum rotating dries, and obtains powder body A；
Step 3, the powder body A obtained is ground sieve in step 2, load graphite jig, utilize vacuum sintering funace temperature be 1450 DEG C, pressure for carrying out hot pressed sintering 2h under 30MPa, be subsequently cooled to room temperature, obtain ZrB2-SiC-CfUltrahigh temperature ceramic composite。
The ZrB that present embodiment method obtains2-SiC-CfUltrahigh temperature ceramic composite consistency is 91.6%, and critical crack size is 56.40 μm, and failure strain reaches 0.10%, and fibre damage is effectively suppressed。
Detailed description of the invention three: a kind of ZrB in present embodiment2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, it is the ZrB of 150nm by mean diameter2Powder body, mean diameter are the SiC powder body of 500nm and carbon fiber joins in dehydrated alcohol (volume of dehydrated alcohol is about powder body and long-pending 30 times of total fiber), carry out ultrasonic cleaning about 30 minutes；Wherein ZrB2Volume fraction be 50%, the volume fraction of SiC is 20%, and the volume fraction of carbon fiber is 30%；
Step 2, being subsequently poured in politef ball grinder and carry out ball milling 10h, abrading-ball adopts WC ball。Rotational speed of ball-mill is 220r/min, and recycling Rotary Evaporators is 35r/min, temperature at rotating speed is that under 80 DEG C of conditions, vacuum rotating dries, and obtains powder body A；
Step 3, the powder body A obtained is ground sieve in step 2, load graphite jig, utilize vacuum sintering funace temperature be 1450 DEG C, pressure for carrying out hot pressed sintering 2h under 30MPa, be subsequently cooled to room temperature, obtain ZrB2-SiC-CfUltrahigh temperature ceramic composite。
The ZrB that present embodiment method obtains2-SiC-CfUltrahigh temperature ceramic composite consistency is 90.5%, and critical crack size is 98.10 μm, and failure strain reaches 0.20%, and fibre damage is effectively suppressed。
The ZrB that present embodiment method obtains2-SiC-CfThe fracture apperance of ultrahigh temperature ceramic composite, as it is shown in figure 1, the carbon fiber structural after sintering as shown in Figure 1 is complete, damages little, and the ZrB that present embodiment method obtains2-SiC-CfUltrahigh temperature ceramic composite occurs in that obvious spike protein gene effect in fracture process。
Detailed description of the invention four: a kind of ZrB in present embodiment2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, it is the ZrB of 150nm by mean diameter2Powder body, mean diameter are the SiC powder body of 500nm and carbon fiber joins in dehydrated alcohol (volume of dehydrated alcohol is about powder body and long-pending 30 times of total fiber), carry out ultrasonic cleaning about 30 minutes；Wherein ZrB2Volume fraction be 40%, the volume fraction of SiC is 20%, and the volume fraction of carbon fiber is 40%；
Step 2, being subsequently poured in politef ball grinder and carry out ball milling 10h, abrading-ball adopts WC ball。Rotational speed of ball-mill is 220r/min, and recycling Rotary Evaporators is 35r/min, temperature at rotating speed is that under 80 DEG C of conditions, vacuum rotating dries, and obtains powder body A；
Step 3, the powder body A obtained is ground sieve in step 2, load graphite jig, utilize vacuum sintering funace temperature be 1450 DEG C, pressure for carrying out hot pressed sintering 2h under 30MPa, be subsequently cooled to room temperature, obtain ZrB2-SiC-CfUltrahigh temperature ceramic composite。
The ZrB obtained in present embodiment method2-SiC-CfUltrahigh temperature ceramic composite consistency is 85.7%, and critical crack size is 118.70 μm, and failure strain reaches 0.22%, and fibre damage is effectively suppressed, and composite material exhibits goes out the feature of non-brittle fracture。
Detailed description of the invention five: a kind of ZrB in present embodiment2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, it is the ZrB of 150nm by mean diameter2Powder body, mean diameter are the SiC powder body of 500nm and carbon fiber joins in dehydrated alcohol (volume of dehydrated alcohol is about powder body and long-pending 30 times of total fiber), carry out ultrasonic cleaning about 30 minutes；Wherein ZrB2Volume fraction be 30%, the volume fraction of SiC is 20%, and the volume fraction of carbon fiber is 50%；
Step 2, being subsequently poured in politef ball grinder and carry out ball milling 10h, abrading-ball adopts WC ball。Rotational speed of ball-mill is 220r/min, and recycling Rotary Evaporators is 35r/min, temperature at rotating speed is that under 80 DEG C of conditions, vacuum rotating dries, and obtains powder body A；
Step 3, the powder body A obtained is ground sieve in step 2, load graphite jig, utilize vacuum sintering funace temperature be 1450 DEG C, pressure for carrying out hot pressed sintering 2h under 30MPa, be subsequently cooled to room temperature, obtain ZrB2-SiC-CfUltrahigh temperature ceramic composite。
The ZrB that present embodiment method obtains2-SiC-CfUltrahigh temperature ceramic composite consistency is 80.4%, and critical crack size is 169.30 μm, and failure strain reaches 0.32%, and fibre damage is effectively suppressed, and composite material exhibits goes out the feature of non-brittle fracture。
The ZrB that detailed description of the invention two to five method obtains2-SiC-CfThe stress-strain diagram of ultrahigh temperature ceramic composite as in figure 2 it is shown, as shown in Figure 2, ZrB2-SiC-CfThe failure strain of ultrahigh temperature ceramic composite composite increases along with the increase of fiber volume fraction, and composite shows the feature of non-brittle fracture when fiber volume fraction is more than 40%。
Detailed description of the invention six: a kind of ZrB in present embodiment2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, it is the ZrB of 200nm by mean diameter2Powder body, mean diameter are the SiC powder body of 100nm and carbon fiber joins in dehydrated alcohol (volume of dehydrated alcohol is about powder body and long-pending 30 times of total fiber), carry out ultrasonic cleaning about 30 minutes；Wherein ZrB2Volume fraction be 50%, the volume fraction of SiC is 20%, and the volume fraction of carbon fiber is 30%；
Step 2, being subsequently poured in politef ball grinder and carry out ball milling 10h, abrading-ball adopts WC ball。Rotational speed of ball-mill is 220r/min, and recycling Rotary Evaporators is 35r/min, temperature at rotating speed is that under 80 DEG C of conditions, vacuum rotating dries, and obtains powder body A；
Step 3, the powder body A obtained is ground sieve in step 2, load graphite jig, utilize vacuum sintering funace temperature be 1500 DEG C, pressure for carrying out hot pressed sintering 1h under 30MPa, be subsequently cooled to room temperature, obtain ZrB2-SiC-CfUltrahigh temperature ceramic composite。
The ZrB that present embodiment method obtains2-SiC-CfUltrahigh temperature ceramic composite consistency is 91.5%, and critical crack size is 97.54 μm, and failure strain reaches 0.21%, and fibre damage is effectively suppressed。
Detailed description of the invention seven: a kind of ZrB in present embodiment2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, it is the ZrB of 200nm by mean diameter2Powder body, mean diameter are the SiC powder body of 3500nm and carbon fiber joins in dehydrated alcohol (volume of dehydrated alcohol is about powder body and long-pending 30 times of total fiber), carry out ultrasonic cleaning about 30 minutes；Wherein ZrB2Volume fraction be 60%, the volume fraction of SiC is 15%, and the volume fraction of carbon fiber is 25%；
Step 2, being subsequently poured in politef ball grinder and carry out ball milling 10h, abrading-ball adopts WC ball。Rotational speed of ball-mill is 220r/min, and recycling Rotary Evaporators is 35r/min, temperature at rotating speed is that under 80 DEG C of conditions, vacuum rotating dries, and obtains powder body A；
Step 3, the powder body A obtained is ground sieve in step 2, load graphite jig, utilize vacuum sintering funace temperature be 1500 DEG C, pressure for carrying out hot pressed sintering 3h under 30MPa, be subsequently cooled to room temperature, obtain ZrB2-SiC-CfUltrahigh temperature ceramic composite。
The ZrB that present embodiment method obtains2-SiC-CfUltrahigh temperature ceramic composite consistency is 90.8%, and critical crack size is 71.4 μm, and failure strain reaches 0.14%, and fibre damage is effectively suppressed。
Detailed description of the invention eight: a kind of ZrB in present embodiment2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, it is the ZrB of 200nm by mean diameter2Powder body, mean diameter are the SiC powder body of 500nm and carbon fiber joins in dehydrated alcohol (volume of dehydrated alcohol is about powder body and long-pending 30 times of total fiber), carry out ultrasonic cleaning about 30 minutes；Wherein ZrB2Volume fraction be 40%, the volume fraction of SiC is 30%, and the volume fraction of carbon fiber is 30%；
Step 2, being subsequently poured in politef ball grinder and carry out ball milling 10h, abrading-ball adopts WC ball。Rotational speed of ball-mill is 220r/min, and recycling Rotary Evaporators is 35r/min, temperature at rotating speed is that under 80 DEG C of conditions, vacuum rotating dries, and obtains powder body A；
Step 3, the powder body A obtained is ground sieve in step 2, load graphite jig, utilize vacuum sintering funace temperature be 1450 DEG C, pressure for carrying out hot pressed sintering 3h under 30MPa, be subsequently cooled to room temperature, obtain ZrB2-SiC-CfUltrahigh temperature ceramic composite。
The ZrB that present embodiment method obtains2-SiC-CfUltrahigh temperature ceramic composite consistency is 91.3%, and critical crack size is 99.6 μm, and failure strain reaches 0.21%, and fibre damage is effectively suppressed。

Claims (10)

1. a ZrB2-SiC-CfUltrahigh temperature ceramic composite, it is characterised in that ZrB2-SiC-CfUltrahigh temperature ceramic composite by volume mark is by 30%～60%ZrB2Powder body, 15%～30%SiC powder body and what 20%～50% carbon fiber was made, wherein, described ZrB2Diameter of particle is (100～200) nm, and described SiC diameter of particle is (100～500) nm。
2. a kind of ZrB according to claim 12-SiC-CfUltrahigh temperature ceramic composite, it is characterised in that ZrB2-SiC-CfUltrahigh temperature ceramic composite by volume mark is by 60%ZrB2Powder body, 20%SiC powder body and what 20% carbon fiber was made。
3. a kind of ZrB according to claim 12-SiC-CfUltrahigh temperature ceramic composite, it is characterised in that ZrB2-SiC-CfUltrahigh temperature ceramic composite by volume mark is by 50%ZrB2Powder body, 20%SiC powder body and what 30% carbon fiber was made。
4. a kind of ZrB according to claim 12-SiC-CfUltrahigh temperature ceramic composite, it is characterised in that ZrB2-SiC-CfUltrahigh temperature ceramic composite by volume mark is by 40%ZrB2Powder body, 20%SiC powder body and what 40% carbon fiber was made。
5. a kind of ZrB according to claim 12-SiC-CfUltrahigh temperature ceramic composite, it is characterised in that ZrB2-SiC-CfUltrahigh temperature ceramic composite by volume mark is by 30%ZrB2Powder body, 20%SiC powder body and what 50% carbon fiber was made。
6. a kind of ZrB according to claim 12-SiC-CfUltrahigh temperature ceramic composite, it is characterised in that ZrB2-SiC-CfUltrahigh temperature ceramic composite by volume mark is by 40%ZrB2Powder body, 30%SiC powder body and what 30% carbon fiber was made。
7. a kind of ZrB according to claim 12-SiC-CfUltrahigh temperature ceramic composite, it is characterised in that described ZrB2Diameter of particle is 150nm；Described SiC diameter of particle is 200nm。
8. a kind of ZrB as described in any one in claim 1-72-SiC-CfThe preparation method of ultrahigh temperature ceramic composite, it is characterised in that a kind of ZrB2-SiC-CfThe preparation method of ultrahigh temperature ceramic composite carries out in the steps below:
Step one, by ZrB2Powder body, SiC powder body and carbon fiber join in dehydrated alcohol, carry out ultrasonic cleaning；
Step 2, it is subsequently poured in politef ball grinder and carries out ball milling 8～24h, then vacuum rotating dries and obtains powder body A；
Step 3, by the powder body A obtained in step 2 grind sieve, load graphite jig, utilize vacuum sintering funace temperature be (1400～1500) DEG C, pressure carry out hot pressed sintering (1～3) h under (20～40) MPa, it is subsequently cooled to room temperature, obtains ZrB2-SiC-CfUltrahigh temperature ceramic composite。
9. a kind of ZrB according to claim 82-SiC-CfThe preparation method of ultrahigh temperature ceramic composite, it is characterised in that in step 2, abrading-ball adopts WC ball, and rotational speed of ball-mill is (200～250) r/min。
10. a kind of ZrB according to claim 82-SiC-CfThe preparation method of ultrahigh temperature ceramic composite, it is characterised in that utilize Rotary Evaporators to carry out vacuum rotating in step 2 and dry, rotating speed is (30～50) r/min, and baking temperature is (70～90) DEG C。
CN201610015369.9A 2016-01-11 2016-01-11 ZrB2-SiC-Cf ultra-high temperature ceramic composite material and preparation method thereof Pending CN105693261A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106866151A (en) * 2017-03-09 2017-06-20 哈尔滨工业大学 A kind of method that slurry injection technique prepares carbon fiber-reinforced zirconium boride composite material of silicon carbide
CN110304932A (en) * 2019-08-11 2019-10-08 西南石油大学 One kind having HfB2The preparation method of the Cf/SiC composite material at interface

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006240957A (en) * 2005-03-07 2006-09-14 Showa Denko Kk Conductive silicon carbide ceramic and its manufacturing method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006240957A (en) * 2005-03-07 2006-09-14 Showa Denko Kk Conductive silicon carbide ceramic and its manufacturing method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈亚西: ""ZrB2-Cf陶瓷基复合材料的力学性能及氧化性研究"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106866151A (en) * 2017-03-09 2017-06-20 哈尔滨工业大学 A kind of method that slurry injection technique prepares carbon fiber-reinforced zirconium boride composite material of silicon carbide
CN110304932A (en) * 2019-08-11 2019-10-08 西南石油大学 One kind having HfB2The preparation method of the Cf/SiC composite material at interface
CN110304932B (en) * 2019-08-11 2021-11-02 西南石油大学 Preparation method of Cf/SiC composite material with HfB2 interface

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