CN108997020A - A kind of high-performance zirconium boride ceramic and its preparation method and application - Google Patents
A kind of high-performance zirconium boride ceramic and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to technical field of semiconductor, a kind of high-performance zirconium boride ceramic and its preparation method and application is disclosed, the zirconium boride ceramic is with ZrB2Powder is raw material, MgO-Re2O3Mixed powder is sintering aid, adds Si3N4It is mixed after whisker or AlN whisker, obtains ZrB2‑Si3N4(AlN) whisker-MgO-Re2O3Mixed powder, then the mixed powder is sieved, 1450~1550 DEG C of sintering under an inert atmosphere, heat preservation is made after being forced into 25~35MPa.This method has the advantages that simple process, sintering temperature are low etc., and the zirconium boride ceramic partial size of preparation is thinner, forms the long bar-like grains in part, consistency and bending strength with higher, with the rodlike ZrB of duration2The formation of crystal grain improves ZrB2The toughness of ceramics, can be used in the fields such as aerospace, weapons, the energy, machinery.
Description
Technical field
The invention belongs to superhigh temperature ceramic material technical field, more particularly, to a kind of high-performance zirconium boride ceramic and
Preparation method and application.
Background technique
Superhigh temperature ceramics generally refer to transition metal carbide, boride, nitride and its phase that fusing point is greater than 3000 DEG C
The complex phase ceramic answered, such as ZrB2、TiB2、TaB2, ZrC, TiC, HfC etc..Superhigh temperature ceramics and its composite material have high-melting-point,
The excellent properties such as high conductivity, high thermal conductivity.It has a wide range of applications in fields such as aerospace, the energy, machinery, wherein
ZrB2Superhigh temperature ceramics receive the highest attention of researcher.
Due to zirconium boride (ZrB2) there is high-vapor-pressure and low diffusion coefficient, and its powder surface includes oxygen impurities, such as
ZrO2、B2O3Deng, it is more difficult to realize sintering densification.For general hot pressed sintering temperature at 1800 DEG C or more, sintering temperature is higher, at
This is also higher.Sintering temperature excessively high simultaneously leads to ZrB2The fast growth of partial size, and some crystal grain meeting abnormal growth causes
Crackle generates, this is to ZrB2The mechanical property of ceramics has adverse effect.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, a kind of high-performance ZrB is provided2Ceramics.
Another object of the present invention is to provide above-mentioned high-performance ZrB2The preparation method of ceramics.
A further object of the present invention is to provide above-mentioned high-performance ZrB2The application of ceramics.
The purpose of the present invention is realized by following technical proposals:
A kind of high-performance zirconium boride ceramic, the zirconium boride ceramic are with ZrB2Powder is raw material, MgO-Re2O3Mixed powder
Body is sintering aid, adds Si3N4It is mixed after whisker or AlN whisker, obtains ZrB2-Si3N4(AlN) whisker-MgO-Re2O3It is mixed
Powder is closed, then the mixed powder is sieved, 1450~1550 DEG C of sintering, keep the temperature after being forced into 25~35MPa under an inert atmosphere
It is made.
Preferably, the MgO-Re2O3Middle Re=Y, La, Ce, Pr, Nd, Pm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or
Lu。
Preferably, the ZrB2: Si3N4Whisker or AlN whisker: MgO-Re2O3Volume ratio be (75~95): (0~
20): 5.
It is further preferable that the MgO:Re2O3Volume ratio be 2:3.
Preferably, the heating rate of the sintering is 5~20 DEG C/min, and the time of the heat preservation is 0.5~2h.
Preferably, the inert atmosphere is argon gas.
Preferably, the ZrB2The purity of powder be 98~100%, 0.5 μm of partial size <；The MgO-Re2O3Mixed powder
Purity be 98~100%.
The preparation method of the high-performance zirconium boride ceramic, comprises the following specific steps that:
S1. by ZrB2Powder, Si3N4Whisker or AlN whisker, MgO-Re2O3Sintering aid is mixed after ingredient, dry
Close uniform ZrB2-Si3N4(AlN) whisker-MgO-Re2O3Mixed powder；
S2. by ZrB in step S12-Si3N4(AlN) whisker-MgO-Re2O3Mixed powder sieving, pours into hot pressing furnace graphite mo(u)ld
In tool, 1450~1550 DEG C are warming up to the rate of 5~20 DEG C/min in an inert atmosphere, is kept the temperature after being pressurized to 25~35MPa
High-performance zirconium boride ceramic is made in 0.5~2h, release while heat preservation terminates.
Preferably, ZrB described in step S12: Si3N4(AlN) whisker: MgO:Re2O3Volume ratio be 85:10:2:3.
Preferably, rate described in step S2 is 10 DEG C/min, and the temperature of the heating is 1500 DEG C, the heat preservation when
Between be 1h, the pressure of the pressurization is 30MPa.
Application of the high-performance zirconium boride ceramic in aerospace, weapons, the energy and machinery field.
Si in the present invention3N4Whisker or AlN whisker are as additive, due to Si3N4There is good remove with AlN itself
Oxygen effect can remove ZrB2The oxygen on surface, to inhibit ZrB2The fast growth of crystal grain, while promoting ZrB2Ceramics are in low temperature
Densified sintering product, the ZrB of preparation2Ceramic partial size is thinner, intensity with higher.In addition, Si3N4It can promote rodlike ZrB with AlN2
The formation of crystal grain, improves ZrB2The toughness of ceramics. MgO-Re2O3As liquid-phase sintering auxiliary agent, it can also promote ZrB2With
Si3N4(AlN) powder is fine and close.
Compared with prior art, the invention has the following advantages:
1. the present invention passes through addition Si3N4Whisker or AlN whisker, promote rodlike ZrB2The formation of crystal grain, with MgO-Re2O3
For sintering aid, due to Si3N4Whisker or AlN whisker have deaerating effect, improve ceramic performance.
2. the ZrB that the present invention is sintered preparation at low temperature2Ceramic partial size is thinner, and consistency with higher and bending resistance are strong
Degree, the formation with the rodlike ZrB2 crystal grain of duration improve ZrB2The toughness of ceramics.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
1. preparation:
(1) with ZrB2Powder (purity 99%, 0.3 μm of partial size) is raw material, with Si3N4Whisker is the addition for improving ceramic performance
Agent, with MgO-Yb2O3(purity 99%, 0.5 μm of partial size) is sintering aid, by ZrB2:Si3N4Whisker: MgO:Yb2O3Volume ratio
Ingredient is carried out for 85:10:2:3.Using ethyl alcohol as solvent, ZrB2Ball is ball-milling medium, with revolving speed 100r/ on planetary ball mill
Min ball milling mixing 8h obtains ZrB after mixing, dry2-Si3N4Whisker-MgO-Yb2O3Mixed powder；
(2) by ZrB2-Si3N4Whisker-MgO-Yb2O3Mixed powder sieving, then by the powder after sieving in hot pressing furnace,
1500 DEG C are warming up to the rate of 10 DEG C/min, keeps the temperature 1h, 30MPa is pressurized to before heat preservation, release while heat preservation terminates is whole
A process atmosphere is 1atm argon gas, and ZrB is made2Ceramics.
2. performance test: above-mentioned obtained ZrB2The relative density of ceramics is about 98%, hardness 26GPa, and bending resistance is strong
Degree is 980MPa, fracture toughness 9.5MPam1/2。
Embodiment 2
1. preparation:
(1) with ZrB2Powder (purity 99%, 0.3 μm of partial size) is raw material, is the addition for improving ceramic performance with AlN whisker
Agent, with MgO-Yb2O3(purity 99%, 0.5 μm of partial size) is sintering aid, by ZrB2: AlN whisker: MgO:Yb2O3Volume ratio
Ingredient is carried out for 85:10:2:3.Using ethyl alcohol as solvent, ZrB2Ball is ball-milling medium, with revolving speed 100r/ on planetary ball mill
Min ball milling mixing 8h obtains ZrB after mixing, dry2- AlN whisker-MgO-Yb2O3Mixed powder；
(2) by uniformly mixed ZrB2- AlN whisker-MgO-Yb2O3Mixed powder sieving, then exists the powder after sieving
In hot pressing furnace, 1500 DEG C are warming up to the rate of 10 DEG C/min, 1h is kept the temperature, is pressurized to 30MPa before heat preservation, keeps the temperature the same of end
When release, whole process atmosphere be 1atm argon gas, be made ZrB2Ceramics.
2. performance test: above-mentioned obtained ZrB2The relative density of ceramics is about 98%, hardness 25GPa, and bending resistance is strong
Degree is 950MPa, fracture toughness 9.3MPam1/2。
Embodiment 3
1. preparation:
(1) with ZrB2Powder (purity 99%, 0.3 μm of partial size) is raw material, with Si3N4Whisker is the addition for improving ceramic performance
Agent, with MgO-Y2O3(purity 99%, 0.5 μm of partial size) is sintering aid, by ZrB2:Si3N4Whisker: MgO:Yb2O3Volume ratio
Ingredient is carried out for 75:20:2:3.Using ethyl alcohol as solvent, ZrB2Ball is ball-milling medium, with revolving speed 100r/ on planetary ball mill
Min ball milling mixing 8h obtains ZrB after mixing, dry2-Si3N4Pleasantly surprised Xu-MgO-Y2O3Mixed powder；
(2) by uniformly mixed ZrB2-Si3N4Whisker-MgO-Y2O3Mixed powder sieving, then exists the powder after sieving
In hot pressing furnace, 1500 DEG C are warming up to the rate of 20 DEG C/min, 2h is kept the temperature, is pressurized to 25MPa before heat preservation, keeps the temperature the same of end
When release, whole process atmosphere be 1atm argon gas, be made ZrB2Ceramics.
2. performance test: above-mentioned obtained ZrB2The relative density of ceramics is about 96%, hardness 25GPa, and bending resistance is strong
Degree is 900MPa, fracture toughness 9.0MPam1/2。
Embodiment 4
1. preparation:
(1) with ZrB2Powder (purity 99%, 0.3 μm of partial size) is raw material, with Si3N4Whisker is the addition for improving ceramic performance
Agent, with MgO-Lu2O3(purity 99%, 0.5 μm of partial size) is sintering aid, by ZrB2:Si3N4Whisker: MgO:Lu2O3Volume point
Number is than being that 85:10:2:3 carries out ingredient.Using ethyl alcohol as solvent, ZrB2Ball is ball-milling medium, with revolving speed on planetary ball mill
100r/min ball milling mixing 8h obtains ZrB after mixing, dry2-Si3N4Whisker-MgO-Lu2O3Mixed powder；
(2) by uniformly mixed ZrB2-Si3N4Whisker-MgO-Lu2O3Mixed powder sieving, then by the powder after sieving
In hot pressing furnace, 1550 DEG C are warming up to the rate of 5 DEG C/min, 0.5h is kept the temperature, is pressurized to 35MPa before heat preservation, heat preservation terminates
While release, whole process atmosphere be 1atm argon gas, be made ZrB2Ceramics.
2. performance test: above-mentioned obtained ZrB2The relative density of ceramics is about 96%, hardness 24GPa, and bending resistance is strong
Degree is 880MPa, fracture toughness 8.5MPam1/2。
Embodiment 5
1. preparation:
(1) with ZrB2Powder (purity 99%, 0.3 μm of partial size) is raw material, is the addition for improving ceramic performance with AlN whisker
Agent, with MgO-Yb2O3(purity 99%, 0.5 μm of partial size) is sintering aid, by ZrB2: AlN whisker: MgO:Yb2O3Volume ratio
Ingredient is carried out for 80:15:2:3.Using ethyl alcohol as solvent, ZrB2Ball is ball-milling medium, with revolving speed 100r/ on planetary ball mill
Min ball milling mixing 8h obtains ZrB after mixing, dry2- AlN whisker-MgO-Yb2O3Mixed powder；
(2) by uniformly mixed ZrB2- AlN whisker-MgO-Yb2O3Mixed powder sieving, then exists the powder after sieving
In hot pressing furnace, 1500 DEG C are warming up to the rate of 10 DEG C/min, 1h is kept the temperature, is pressurized to 30MPa before heat preservation, keeps the temperature the same of end
When release, whole process atmosphere be 1atm argon gas, be made ZrB2Ceramics.
2. performance test: above-mentioned obtained ZrB2The relative density of ceramics is about 96%, hardness 24.5GPa, bending resistance
Intensity is 890MPa, fracture toughness 8.6MPam1/2。
Embodiment 6
1. preparation:
(1) with ZrB2Powder (purity 99%, 0.3 μm of partial size) is raw material, with Si3N4Whisker is the addition for improving ceramic performance
Agent, with MgO-Yb2O3(purity 99%, 0.5 μm of partial size) is sintering aid, by ZrB2:Si3N4Whisker: MgO:Yb2O3Volume ratio
Ingredient is carried out for 90:5:2:3.Using ethyl alcohol as solvent, ZrB2Ball is ball-milling medium, with revolving speed 100r/min on planetary ball mill
Ball milling mixing 8h obtains ZrB after mixing, dry2-Si3N4Whisker-MgO-Yb2O3Mixed powder；
(2) by uniformly mixed ZrB2-Si3N4Whisker-MgO-Yb2O3Mixed powder sieving, then by the powder after sieving
In hot pressing furnace, 1500 DEG C are warming up to the rate of 10 DEG C/min, 1h is kept the temperature, is pressurized to 30MPa before heat preservation, keeps the temperature end
Release simultaneously, whole process atmosphere are 1atm argon gas, and ZrB is made2Ceramics.
2. performance test: above-mentioned obtained ZrB2The relative density of ceramics is about 98%, hardness 25.5GPa, bending resistance
Intensity is 940MPa, fracture toughness 9.2MPam1/2。
Embodiment 7
1. preparation:
(1) with ZrB2Powder (purity 99%, 0.3 μm of partial size) is raw material, is the addition for improving ceramic performance with AlN whisker
Agent, with MgO-Yb2O3(purity 99%, 0.5 μm of partial size) is sintering aid, by ZrB2: AlN whisker: MgO:Yb2O3Volume ratio
Ingredient is carried out for 90:5:2:3.Using ethyl alcohol as solvent, ZrB2Ball is ball-milling medium, with revolving speed 100r/min on planetary ball mill
Ball milling mixing 8h obtains ZrB after mixing, dry2- AlN whisker-MgO-Yb2O3Mixed powder；
(2) by uniformly mixed ZrB2- AlN whisker-MgO-Yb2O3Mixed powder sieving, then exists the powder after sieving
In hot pressing furnace, 1450 DEG C are warming up to the rate of 10 DEG C/min, 1h is kept the temperature, is pressurized to 30MPa before heat preservation, keeps the temperature the same of end
When release, whole process atmosphere be 1atm argon gas, be made ZrB2Ceramics.
Embodiment 8
1. preparation:
(1) with ZrB2Powder (purity 99%, 0.3 μm of partial size) is raw material, with Si3N4Whisker is the addition for improving ceramic performance
Agent, with MgO-Gd2O3(purity 99%, 0.5 μm of partial size) is sintering aid, by ZrB2:Si3N4Whisker: MgO:Gd2O3Volume ratio
Ingredient is carried out for 75:20:2:3.Using ethyl alcohol as solvent, ZrB2Ball is ball-milling medium, with revolving speed 100r/ on planetary ball mill
Min ball milling mixing 8h obtains ZrB after mixing, dry2-Si3N4Pleasantly surprised Xu-MgO-Gd2O3Mixed powder；
(2) by uniformly mixed ZrB2-Si3N4Whisker-MgO-Gd2O3Mixed powder sieving, then by the powder after sieving
In hot pressing furnace, 1500 DEG C are warming up to the rate of 20 DEG C/min, 1h is kept the temperature, is pressurized to 30MPa before heat preservation, keeps the temperature end
Release simultaneously, whole process atmosphere are 1atm argon gas, and ZrB is made2Ceramics.
2. performance test: above-mentioned obtained ZrB2The relative density of ceramics is about 96%, hardness 25.5GPa, bending resistance
Intensity is 900MPa, fracture toughness 8.6MPam1/2。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of high-performance zirconium boride ceramic, which is characterized in that the zirconium boride ceramic is with ZrB2Powder is raw material, MgO-
Re2O3Mixed powder is sintering aid, adds Si3N4It is mixed after whisker or AlN whisker, obtains ZrB2-Si3N4(AlN) whisker-
MgO-Re2O3Mixed powder, then the mixed powder is sieved, 1450~1550 DEG C of sintering under an inert atmosphere, it is forced into 25~
It keeps the temperature and is made after 35MPa.
2. high-performance zirconium boride ceramic according to claim 1, which is characterized in that the MgO-Re2O3Middle Re=Y, La,
Ce, Pr, Nd, Pm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu.
3. high-performance zirconium boride ceramic according to claim 1, which is characterized in that the ZrB2: Si3N4Whisker or AlN are brilliant
Must: MgO-Re2O3Volume ratio be (75~95): (0~20): 5；The MgO:Re2O3Volume ratio be 2:3.
4. high-performance zirconium boride ceramic according to claim 1, which is characterized in that the heating rate of the sintering be 5~
20 DEG C/min, the time of the heat preservation is 0.5~2h.
5. high-performance zirconium boride ceramic according to claim 1, which is characterized in that the inert atmosphere is argon gas.
6. high-performance zirconium boride ceramic according to claim 1, which is characterized in that the ZrB2The purity of powder be 98~
0.5 μm of 100%, partial size <；The MgO-Re2O3The purity of mixed powder is 98~100%.
7. the preparation method of high-performance zirconium boride ceramic according to claim 1-6, which is characterized in that including such as
Lower specific steps:
S1. by ZrB2Powder, Si3N4Whisker or AlN whisker, MgO-Re2O3It is equal to obtain mixing after ingredient, dry for sintering aid
Even ZrB2-Si3N4(AlN) whisker-MgO-Re2O3Mixed powder；
S2. by ZrB in step S12-Si3N4(AlN) whisker-MgO-Re2O3Mixed powder sieving, pours into hot pressing furnace graphite jig
In, 1450~1550 DEG C are warming up to the rate of 5~20 DEG C/min in an inert atmosphere, keeps the temperature 0.5 after being pressurized to 25~35MPa
High-performance zirconium boride ceramic is made in~2h, release while heat preservation terminates.
8. the preparation method of high-performance zirconium boride ceramic according to claim 7, which is characterized in that described in step S1
ZrB2: Si3N4(AlN) whisker: MgO:Re2O3Volume ratio be 85:10:2:3.
9. the preparation method of high-performance zirconium boride ceramic according to claim 7, which is characterized in that speed described in step S2
Rate is 10 DEG C/min, and the temperature of the heating is 1500 DEG C, and the time of the heat preservation is 1h, and the pressure of the pressurization is 30MPa.
10. high-performance zirconium boride ceramic described in any one of claims 1-6 is in aerospace, weapons, the energy and machinery field
In application.
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| CN101417880A (en) * | 2008-11-21 | 2009-04-29 | 哈尔滨工业大学 | Low temperature sintered boride base ceramic materials and preparation method thereof |
| CN102976760A (en) * | 2012-12-20 | 2013-03-20 | 复旦大学 | RE2O3-added ZrB2-SiC composite ceramic material and preparation method thereof |
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