CN102584240A - Sintering method of ZrB2-SiC superhigh temperature ceramics - Google Patents
Sintering method of ZrB2-SiC superhigh temperature ceramics Download PDFInfo
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Abstract
The invention discloses a sintering method of ZrB2-SiC superhigh temperature ceramics and relates to a sintering method of superhigh temperature ceramics. The invention aims at solving the problems of high sintering temperature and high energy consumption in the existing process of preparing ZrB2-SiC superhigh temperature ceramics. The method comprises the following steps of: weighing ZrB2 powder, SiC powder and citric acid; ball-milling and mixing to obtain slurry; drying the slurry to obtain composite powder; and performing vacuum sintering at the temperature of 1500 to 1600 DEG C to obtain the ZrB2-SiC superhigh temperature ceramics. According to the sintering method of the ZrB2-SiC superhigh temperature ceramics provided by the invention, the sintering temperature is lowered by about 300 DEG C, thus energy consumption is reduced. The density of the obtained product can achieve 98%, thus the requirement of being used in oxygen-containing atmosphere at the temperature of 1800 DEG C is met. The method is used for preparing the ZrB2-SiC superhigh temperature ceramics.
Description
Technical field
The present invention relates to a kind of sintering method of ultrahigh-temperature pottery.
Background technology
In the superhigh temperature ceramic material system, ZrB
2Because of having relatively low density (6.09gcm
-3), the higher hardness (Mohs' hardness is 9, and microhardness is 22.1GPa) of high melt point (3245 ℃), (thermal conductivity is 23～25Wm to good thermal conductivity
-1K
-1) and good electrical conductivity (electrical conductivity at room temperature is～1 * 108Sm
-1) etc. characteristics and in fields such as high temperature resistant structure ceramics, ceramic matric composite, used widely and pay close attention to.In recent years along with the development of aerospace industry, ZrB
2The research of based ultra-high temperature stupalith receives the great attention of each developed country; Become development one of material very rapidly; Especially aspect antioxidant property, obtain significant achievement, successfully developed the ZrB in oxygen-containing atmosphere more than 1800 ℃ that to be on active service the beginning of this century
2-SiC superhigh temperature ceramic material.
The ultrahigh-temperature pottery need have very high density, and general density could realize it in the effect aspect the thermal protection greater than 95% ultrahigh-temperature pottery, so in order to obtain higher density, the prior hot pressing sintering temperature is all more than 1800 ℃.Use traditional preparation process technology sintering and prepare superhigh temperature ceramic material, because sintering temperature is high, energy expenditure is huge, has limited the application of superhigh temperature ceramic material.
Summary of the invention
The present invention will solve existing preparation ZrB
2The technology of-SiC ultrahigh-temperature pottery exists sintering temperature high, the problem that energy consumption is big, and a kind of ZrB is provided
2The sintering method of-SiC ultrahigh-temperature pottery.
A kind of ZrB of the present invention
2The sintering method of-SiC ultrahigh-temperature pottery carries out according to the following steps: one, take by weighing ZrB
2Powder, SiC powder and Hydrocerol A, ZrB
2The volume ratio of powder and SiC powder is (3～5): 1, and the quality of Hydrocerol A is ZrB
21%～3% of powder and SiC powder total mass, ZrB
2The median size of powder and SiC powder is 50～70nm; Two, in ball grinder, add absolute ethyl alcohol as solvent medium, add the Hydrocerol A, the ZrB that take by weighing in the step 1 then successively
2Powder and SiC powder, Ball milling obtains slurry; Three, the slurry oven dry that step 2 is obtained obtains composite granule; Four, composite granule is placed graphite jig, sintering under vacuum condition, sintering temperature is 1500～1600 ℃, and sintering pressure is 25～35MPa, and sintering time is 1～1.5h, is cooled to room temperature then, obtains ZrB
2-SiC ultrahigh-temperature pottery.
Starting material of the present invention adopt the less nano-powder of particle diameter, are dispersion agent with the Hydrocerol A, in ethanol system, carry out dispersion treatment, open the reunion between the powder, cooperate ball-milling technology that nano-powder is mixed uniformly.Because the alcoholic acid surface tension is little,, make the powder that mixes keep nano shape so in drying process, be difficult for secondary agglomeration takes place.The powder specific surface area of small particle size is big, and the densification process in sintering process is more prone to carry out, so can under the condition that is lower than the normal sintering temperature, realize sintering densification, obtains the superhigh temperature ceramic material of high-compactness.
The invention has the beneficial effects as follows: ZrB of the present invention
2The sintering method of-SiC ultrahigh-temperature pottery is compared with traditional sintering method, and sintering temperature has been reduced about 300 ℃, has reduced energy consumption, the ZrB that the inventive method makes
2-SiC ultrahigh-temperature pottery, its density can reach 98%, satisfies its request for utilization in 1800 ℃ of oxygen-containing atmospheres.
The present invention is used to prepare ZrB
2-SiC ultrahigh-temperature pottery.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of ZrB of this embodiment
2The sintering method of-SiC ultrahigh-temperature pottery carries out according to the following steps: one, take by weighing ZrB
2Powder, SiC powder and Hydrocerol A, ZrB
2The volume ratio of powder and SiC powder is (3～5): 1, and the quality of Hydrocerol A is ZrB
21%～3% of powder and SiC powder total mass, ZrB
2The median size of powder and SiC powder is 50～70nm; Two, in ball grinder, add absolute ethyl alcohol as solvent medium, add the Hydrocerol A, the ZrB that take by weighing in the step 1 then successively
2Powder and SiC powder, Ball milling obtains slurry; Three, the slurry oven dry that step 2 is obtained obtains composite granule; Four, composite granule is placed graphite jig, sintering under vacuum condition, sintering temperature is 1500～1600 ℃, and sintering pressure is 25～35MPa, and sintering time is 1～1.5h, is cooled to room temperature then, obtains ZrB
2-SiC ultrahigh-temperature pottery.
The starting material of this embodiment adopt the less nano-powder of particle diameter, are dispersion agent with the Hydrocerol A, in ethanol system, carry out dispersion treatment, open the reunion between the powder, cooperate ball-milling technology that nano-powder is mixed uniformly.Because the alcoholic acid surface tension is little,, make the powder that mixes keep nano shape so in drying process, be difficult for secondary agglomeration takes place.The powder specific surface area of small particle size is big, and the densification process in sintering process is more prone to carry out, so can under the condition that is lower than the normal sintering temperature, realize sintering densification, obtains the superhigh temperature ceramic material of high-compactness.
The beneficial effect of this embodiment is: this embodiment ZrB
2The sintering method of-SiC ultrahigh-temperature pottery is compared with traditional sintering method, and sintering temperature has been reduced about 300 ℃, has reduced energy consumption, the ZrB that the inventive method makes
2-SiC ultrahigh-temperature pottery, its density can reach 98%, satisfies its request for utilization in 1800 ℃ of oxygen-containing atmospheres.
Embodiment two: what this embodiment and embodiment one were different is: ZrB in the step 1
2The median size of powder and SiC powder is 55～65nm.Other is identical with embodiment one.
Embodiment three: what this embodiment was different with embodiment one or two is: ZrB in the step 1
2The volume ratio of powder and SiC powder is (3.5～4): 1, and the quality of Hydrocerol A is ZrB
21.5%～2.5% of powder and SiC powder total mass.Other is identical with embodiment one or two.
Embodiment four: what this embodiment was different with one of embodiment one or three is: be under the condition of 300～400r/min at rotating speed in the step 2, Ball milling 10～12h obtains slurry.Other is identical with one of embodiment one or three.
Embodiment five: what this embodiment was different with one of embodiment one or four is: the volume of absolute ethyl alcohol is 80%～95% of a ball grinder volume in the step 2, ZrB
2The TV of powder and SiC powder is 20%～25% of a ball grinder volume.Other is identical with one of embodiment one or four.
Embodiment six: what this embodiment was different with one of embodiment one or five is: adopt Rotary Evaporators in the step 3, under 70～80 ℃ condition, the slurry oven dry that step 2 is obtained obtains composite granule.Other is identical with one of embodiment one or five.
Embodiment seven: what this embodiment was different with one of embodiment one or six is: sintering temperature is 1520～1580 ℃ in the step 4, and sintering pressure is 28～32MPa, and sintering time is 1.1～1.4h.Other is identical with one of embodiment one or six.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment one:
A kind of ZrB of present embodiment
2The sintering method of-SiC ultrahigh-temperature pottery carries out according to the following steps: one, take by weighing ZrB
2Powder, SiC powder and Hydrocerol A, ZrB
2The volume ratio of powder and SiC powder is 3: 1, and the quality of Hydrocerol A is ZrB
21% of powder and SiC powder total mass, ZrB
2The median size of powder and SiC powder is 50nm; Two, in ball grinder, add absolute ethyl alcohol as solvent medium, add the Hydrocerol A, the ZrB that take by weighing in the step 1 then successively
2Powder and SiC powder are that Ball milling 12h obtains slurry under the condition of 300r/min at rotating speed; Three, adopt Rotary Evaporators, under 70 ℃ condition, the slurry oven dry that step 2 is obtained obtains composite granule; Four, composite granule being placed graphite jig, is 10 in vacuum tightness
-1Pa, temperature is 1500 ℃, and pressure is under the condition of 30MPa, and sintering 1h postcooling obtains ZrB to room temperature
2-SiC ultrahigh-temperature pottery.
The volume of absolute ethyl alcohol is 90% of a ball grinder volume in this embodiment step 2, ZrB
2The TV of powder and SiC powder is 20% of a ball grinder volume, ball and ZrB
2The ratio of powder and SiC powder total mass is 3: 1, and the material of ball is SiC, absolute ethyl alcohol, ZrB
2Powder and SiC powder all are to buy from market to obtain.
Present embodiment ZrB
2The sintering method of-SiC ultrahigh-temperature pottery is compared with traditional sintering method, and sintering temperature has been reduced about 300 ℃, has reduced energy consumption, the ZrB that present embodiment makes
2-SiC ultrahigh-temperature pottery, its density is 98%, satisfies its request for utilization in oxygen-containing atmosphere more than 1800 ℃.
Density (specific density) measuring method:
One, adopt Archimedes's method to measure the prepared ZrB of present embodiment
2The actual density of-SiC ultrahigh-temperature pottery uses photoelectric analytical balance (precision 0.0001g) accurately to measure ZrB
2-SiC ultrahigh-temperature aerial quality m of pottery and ZrB
2The quality m of-SiC ultrahigh-temperature pottery in zero(ppm) water
Water,, calculate ZrB according to formula 1
2The actual density ρ of-SiC ultrahigh-temperature pottery.Before measuring the specimen surface cleaning is dried up, measure three appearance at least, average.
M---the aerial quality of sample (g);
m
Water---the quality (g) of sample in zero(ppm) water;
ρ
Water---the density (g/cm of zero(ppm) water under the probe temperature
3).
Two,, calculate ZrB according to mixing rule formula 2
2The theoretical density ρ of-SiC ultrahigh-temperature pottery
Theoretical
ρ
Theoretical=∑ ρ
iV
i(2)
Three,, calculate ZrB according to mixing rule formula 2
2The specific density of-SiC ultrahigh-temperature pottery, i.e. density η.
Embodiment two:
A kind of ZrB of present embodiment
2The sintering method of-SiC ultrahigh-temperature pottery carries out according to the following steps: one, take by weighing ZrB
2Powder, SiC powder and Hydrocerol A, ZrB
2The volume ratio of powder and SiC powder is 5: 1, and the quality of Hydrocerol A is ZrB
23% of powder and SiC powder total mass, ZrB
2The median size of powder and SiC powder is 70nm; Two, in ball grinder, add absolute ethyl alcohol as solvent medium, add the Hydrocerol A, the ZrB that take by weighing in the step 1 then successively
2Powder and SiC powder are that Ball milling 10h obtains slurry under the condition of 400r/min at rotating speed; Three, adopt Rotary Evaporators, under 80 ℃ condition, the slurry oven dry that step 2 is obtained obtains composite granule; Four, composite granule being placed graphite jig, is 10 in vacuum tightness
-1Pa, temperature is 1500 ℃, and pressure is under the condition of 30MPa, and sintering 1h postcooling obtains ZrB to room temperature
2-SiC ultrahigh-temperature pottery.
The volume of absolute ethyl alcohol is 80% of a ball grinder volume in this embodiment step 2, ZrB
2The TV of powder and SiC powder is 25% of a ball grinder volume, ball and ZrB
2The ratio of powder and SiC powder total mass is 2: 1, and the material of ball is SiC, absolute ethyl alcohol, ZrB
2Powder and SiC powder all are to buy from market to obtain.
Present embodiment ZrB
2The sintering method of-SiC ultrahigh-temperature pottery is compared with traditional sintering method, and sintering temperature has been reduced about 300 ℃, has reduced energy consumption, the ZrB that present embodiment makes
2-SiC ultrahigh-temperature pottery, its density is 98%, satisfies its request for utilization in oxygen-containing atmosphere more than 1800 ℃.
Claims (7)
1. ZrB
2The sintering method of-SiC ultrahigh-temperature pottery is characterized in that ZrB
2The sintering method of-SiC ultrahigh-temperature pottery carries out according to the following steps: one, take by weighing ZrB
2Powder, SiC powder and Hydrocerol A, ZrB
2The volume ratio of powder and SiC powder is (3～5): 1, and the quality of Hydrocerol A is ZrB
21%～3% of powder and SiC powder total mass, ZrB
2The median size of powder and SiC powder is 50～70nm; Two, in ball grinder, add absolute ethyl alcohol as solvent medium, add the Hydrocerol A, the ZrB that take by weighing in the step 1 then successively
2Powder and SiC powder, Ball milling obtains slurry; Three, the slurry oven dry that step 2 is obtained obtains composite granule; Four, composite granule is placed graphite jig, sintering under vacuum condition, sintering temperature is 1500～1600 ℃, and sintering pressure is 25～35MPa, and sintering time is 1～1.5h, is cooled to room temperature then, obtains ZrB
2-SiC ultrahigh-temperature pottery.
2. a kind of ZrB according to claim 1
2The sintering method of-SiC ultrahigh-temperature pottery is characterized in that ZrB in the step 1
2The median size of powder and SiC powder is 55～65nm.
3. a kind of ZrB according to claim 1 and 2
2The sintering method of-SiC ultrahigh-temperature pottery is characterized in that ZrB in the step 1
2The volume ratio of powder and SiC powder is (3.5～4): 1, and the quality of Hydrocerol A is ZrB
21.5%～2.5% of powder and SiC powder total mass.
4. a kind of ZrB according to claim 1
2The sintering method of-SiC ultrahigh-temperature pottery is characterized in that in the step 2 at rotating speed being under the condition of 300～400r/min, and Ball milling 10～12h obtains slurry.
5. according to claim 1 or 4 described a kind of ZrB
2The sintering method of-SiC ultrahigh-temperature pottery, the volume that it is characterized in that absolute ethyl alcohol in the step 2 is 80%～95% of a ball grinder volume, ZrB
2The TV of powder and SiC powder is 20%～25% of a ball grinder volume.
6. a kind of ZrB according to claim 1
2The sintering method of-SiC ultrahigh-temperature pottery is characterized in that adopting in the step 3 Rotary Evaporators, and under 70～80 ℃ condition, the slurry oven dry that step 2 is obtained obtains composite granule.
7. according to claim 1,4 or 6 described a kind of ZrB
2The sintering method of-SiC ultrahigh-temperature pottery is characterized in that sintering temperature is 1520～1580 ℃ in the step 4, and sintering pressure is 28～32MPa, and sintering time is 11～1.4h.
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| CN105330330A (en) * | 2015-09-29 | 2016-02-17 | 洛阳暖盈电子技术有限公司 | Preparation method of ZrB2-Al2O3 foamed ceramics |
| CN106478110A (en) * | 2016-10-12 | 2017-03-08 | 黑龙江科技大学 | A kind of ZrB2The preparation method of SiC composite ceramicses |
| CN106747464A (en) * | 2017-01-04 | 2017-05-31 | 广东工业大学 | ZrB2SiC ceramic heater and superhigh temperature firing equipment |
| CN107056334A (en) * | 2017-04-28 | 2017-08-18 | 哈尔滨理工大学 | A kind of ZrC ceramic material surfaces ZrB2The preparation method of SiC composite coatings |
| CN110157998A (en) * | 2019-05-27 | 2019-08-23 | 太原理工大学 | A kind of super-hard self-lubricating cutter material and preparation method thereof |
| CN110153591A (en) * | 2019-05-29 | 2019-08-23 | 安徽工程大学 | A kind of amorphous composite soldering for ceramic soldering and alloy |
| CN110181196A (en) * | 2019-05-29 | 2019-08-30 | 安徽工程大学 | A kind of AgCu composite soldering for ceramic soldering and high temperature alloy |
| CN114380602A (en) * | 2020-10-20 | 2022-04-22 | 中国科学院理化技术研究所 | Preparation method of ultrahigh-temperature ceramic composite powder |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330330A (en) * | 2015-09-29 | 2016-02-17 | 洛阳暖盈电子技术有限公司 | Preparation method of ZrB2-Al2O3 foamed ceramics |
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| CN106747464A (en) * | 2017-01-04 | 2017-05-31 | 广东工业大学 | ZrB2SiC ceramic heater and superhigh temperature firing equipment |
| CN107056334A (en) * | 2017-04-28 | 2017-08-18 | 哈尔滨理工大学 | A kind of ZrC ceramic material surfaces ZrB2The preparation method of SiC composite coatings |
| CN107056334B (en) * | 2017-04-28 | 2020-04-17 | 哈尔滨理工大学 | ZrB ceramic material surface ZrB2Preparation method of-SiC composite coating |
| CN110157998A (en) * | 2019-05-27 | 2019-08-23 | 太原理工大学 | A kind of super-hard self-lubricating cutter material and preparation method thereof |
| CN110153591A (en) * | 2019-05-29 | 2019-08-23 | 安徽工程大学 | A kind of amorphous composite soldering for ceramic soldering and alloy |
| CN110181196A (en) * | 2019-05-29 | 2019-08-30 | 安徽工程大学 | A kind of AgCu composite soldering for ceramic soldering and high temperature alloy |
| CN114380602A (en) * | 2020-10-20 | 2022-04-22 | 中国科学院理化技术研究所 | Preparation method of ultrahigh-temperature ceramic composite powder |
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Application publication date: 20120718 |