CN105198433B - A kind of preparation method of molybdenum disilicide/silicon carbide/carbon boron three-phase intensity composite ceramics - Google Patents
A kind of preparation method of molybdenum disilicide/silicon carbide/carbon boron three-phase intensity composite ceramics Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of molybdenum disilicide/silicon carbide/carbon boron three-phase intensity composite ceramics.This method uses MoSi2, C and B4C element powder compression molding, by adjusting vacuum and infiltration Si is sintered, obtain MoSi2/SiC/B4C three-phase intensity composite ceramicses, for resulting materials porosity 10% or less, intensity is more than 180MPa.This method supplements existing high-temperature oxidation resistant strength materials kind, is compared with existing refractory ceramics, obtains the strength ceramic kind used under more high antioxygenic property environment, value is can further improve after process optimization.The method technique is simple, can large-scale production.
Description
Technical field
The present invention relates to MoSi2/SiC/B4The technology of preparing of C three-phase intensity composite ceramicses, belong to the low of novel intensity ceramics
Cost production techniques field.
Background technology
Select the fusing point, proportion and high temperature antioxygen that aviation is material with three most important parameters of high-temperature structural material
Change performance.Refractory ceramics is widely used in Aeronautics and Astronautics, metallurgy and field of traffic.From the point of view of high-temperature material, metal-based compound material
Though material has preferable combination property, because its cost is high, the metal material of aerospace, only particle or short fiber reinforced is also only limited to
There is large-scale popularization in civilian possibility.The high-temperature oxidation-resistant material for being operated in less than 1000 DEG C at present mainly has Ni-based, cobalt-based to surpass
Alloy.Compound is small with its proportion among titanium and titanium aluminium, has a broad prospect of application in space mechanism, but further study show that, this
The temperature in use of class material has no compared with Ni based alloys and significantly improved, and operating temperature is 600-1000 °C.Carbon composite can
Up to 2500 °C, but oxidation resistance is too poor, is only used for rocket, guided missile, and its manufacturing cost is sufficiently expensive due to changing between metal
Compound MoSi2, there is high-melting-point (2030 °C), moderate density (6.24 × 103kg/m3), good thermal conductivity and electric conductivity with
And there is excellent high-temperature oxidation resistance in all metal silicides and turn into the material for being most hopeful to meet this requirement.
SiC has very high elevated temperature strength and oxidation resistance, and and MoSi2With good chemical compatibility and Thermodynamically stable
Property, thus SiC enhancings MoSi2The obdurability of composite can largely be improved.Thus the composite has
Higher obdurability, especially MoSi2/ SiC composite ceramicses, possess higher temperature in use and more preferable antioxygenic property, it is light
And mechanical property is good.Because boron carbide has anti-oxidant, resistant to elevated temperatures characteristic, it is used as advanced setting and unsetting fire proofed wood
Material is widely used in metallurgical every field, such as steel stove, kiln furnitures.Due to its above characteristic, MoSi2/SiC/B4C three-phase composites
Ceramics will have broader high-temperature oxidation environment application value.
By infiltration in vacuum reaction sintering, MoSi is prepared2/SiC/B4C three-phase composites ceramics, have higher-strength, hole
Rate is less than 10%, and cost is low, the features such as efficiency high.
The content of the invention
It is an object of the invention to be combined using vacuum reaction sintering and infiltration technique to prepare MoSi2/SiC/B4C tri-
Phase composite ceramics.Increase the kind of elevated temperature strength ceramics, supplement the new thing phase composition of existing high temperature molybdenum disilicide composite.
The invention utilizes MoSi2, C and B4C element powder compression molding, infiltration in vacuum Si are sintered, and resulting materials intensity stabilization is maintained at
180MPa or more.
The technical scheme is that：A kind of preparation side of molybdenum disilicide/silicon carbide/carbon boron three-phase intensity composite ceramics
Method, it the step of it is as follows：
（1）By MoSi2Powder, C powder and B4C powder ball mill mixings, the MoSi2Powder, C powder and B4The weight ratio of C powder is 50-95：
1-10：0.1-30, incorporation time are 8-72 hr, add MoSi2Powder, C powder and B4C powder gross weights 5-20% binding agent, and be molded
Shaping, obtains blank；
（2）Blank room temperature is dried, then enters oven for drying 1-72hr；
（3）Blank after drying is moved into and is covered with MoSi2Powder, C powder and B4The vacuum of C powder gross weights 2-20% metal Si powder
In sintering furnace, vacuum is kept 10-2-10-3Pa, heating rate are 1-15 DEG C/min；
（4）10-60min is incubated at 1200-1480 DEG C, and reduces vacuum >=10-1Pa is kept；It is warming up to 1500-1650
DEG C insulation 10-60min, and reduces vacuum >=10-1Pa is kept；1650-1700 DEG C of insulation 10-40min is warming up to, improves vacuum
Degree≤10-2Pa is kept, and MoSi is obtained after cooling2/SiC/B4C three-phase intensity composite ceramicses.
The beneficial effects of the invention are as follows：The present invention utilizes MoSi2, C and B4C element powder compression molding, by adjusting vacuum
And infiltration Si is sintered, MoSi is obtained2/SiC/B4C three-phase intensity composite ceramicses, resulting materials porosity less than 10% or with
Under, intensity is more than 180MPa.The three-phase intensity composite ceramics porosity and intensity can be by adjusting mixed-powder obtained by this method
Granularity is regulated and controled, is adapted to commercial scale.
Embodiment
Embodiment 1
Weigh MoSi in proportion respectively2、C、B4C powder 180g, 6g, 10g, ball milling 48hr after uniformly mixing.By above powder
Simultaneously compression molding is mixed after adding 20g phenolic resin.Dried after being dried in air in 110 degree of baking ovens.Move to and be covered with 14g gold
Belong to and being sintered in the vacuum sintering furnace of silica flour.Programming rate is 3 DEG C/min, vacuum 10-3Pa or so.It is warming up to 1400-
1450 DEG C, it is 10 to reduce vacuum-1Pa, it is incubated 30min；1550 DEG C are warming up to, is incubated 30min, vacuum 10-1Pa.Heating
To 1650 DEG C, 10min, vacuum 10 are incubated-3Pa.Then furnace cooling, cool feeding.Molybdenum disilicide/silicon carbide/carbon of survey
It is 10% to change boron three-phase intensity composite ceramics porosity, intensity 180MPa.
Embodiment 2
Weigh MoSi in proportion respectively2、C、B4C powder 170g, 7.5g, 10g, ball milling 48hr after uniformly mixing.By above powder
Material is mixed after adding 19g phenolic resin and compression molding.Dried after being dried in air in 100 degree of baking ovens.Move to and be covered with 12g
It is sintered in the vacuum sintering furnace of metallic silicon power.Programming rate is 5 DEG C/min, vacuum 10-3Pa or so.It is warming up to
1400-1450 DEG C, it is 10 to reduce vacuum-1Pa, it is incubated 25min；1550 DEG C are warming up to, is incubated 30min, vacuum 10- 1Pa.1650 DEG C are warming up to, is incubated 10min, vacuum 10-3Pa.Then furnace cooling, cool feeding.The molybdenum disilicide of survey/
Silicon carbide/carbon boron three-phase intensity composite ceramics porosity is 7%, intensity 180MPa.
Embodiment 3
Weigh MoSi in proportion respectively2、C、B4C powder 190g, 2.5g, 10g, ball milling 48hr after uniformly mixing.By above powder
Material is mixed after adding 11% phenolic resin and compression molding.Dried after being dried in air in 100 degree of baking ovens.Move to and be covered with 12g
It is sintered in the vacuum sintering furnace of metallic silicon power.Programming rate is 4 DEG C/min, vacuum 10-3Pa or so.It is warming up to
1410-1450 DEG C, it is 10 to reduce vacuum-1Pa, it is incubated 30min；1550 DEG C are warming up to, is incubated 30min, vacuum 10- 1Pa.1700 DEG C are warming up to, is incubated 10min, vacuum 10-3Pa.Then furnace cooling, cool feeding.The molybdenum disilicide of survey/
Silicon carbide/carbon boron three-phase intensity composite ceramics porosity is 4%, intensity 185MPa.
Embodiment 4
A kind of preparation method of molybdenum disilicide/silicon carbide/carbon boron three-phase intensity composite ceramics, it the step of it is as follows：
（1）By MoSi2Powder, C powder and B4C powder ball mill mixings, the MoSi2Powder, C powder and B4The weight ratio of C powder is 50：1：
0.1, incorporation time is 8 hr, adds MoSi2Powder, C powder and B4The binding agent of C powder gross weight 5%, and compression molding, obtain blank；
（2）Blank room temperature is dried, then enters oven for drying 1hr；
（3）Blank after drying is moved into and is covered with MoSi2Powder, C powder and B4The vacuum of the metal Si powder of C powder gross weight 2% is burnt
In freezing of a furnace, vacuum is kept 10-2Pa, heating rate are 1 DEG C/min；
（4）10min is incubated at 1200 DEG C, and reduces vacuum >=10-1Pa is kept；1500 DEG C of insulation 10min are warming up to, and
Reduce vacuum >=10-1Pa is kept；1650 DEG C of insulation 10min are warming up to, improve vacuum≤10-2Pa is kept, and is obtained after cooling
MoSi2/SiC/B4C three-phase intensity composite ceramicses.
Embodiment 5
A kind of preparation method of molybdenum disilicide/silicon carbide/carbon boron three-phase intensity composite ceramics, it the step of it is as follows：
（1）By MoSi2Powder, C powder and B4C powder ball mill mixings, the MoSi2Powder, C powder and B4The weight ratio of C powder is 95：10：
30, incorporation time is 72 hr, adds MoSi2Powder, C powder and B4The binding agent of C powder gross weight 20%, and compression molding, obtain base
Material；
（2）Blank room temperature is dried, then enters oven for drying 72hr；
（3）Blank after drying is moved into and is covered with MoSi2Powder, C powder and B4The vacuum of the metal Si powder of C powder gross weight 20% is burnt
In freezing of a furnace, vacuum is kept 10-3Pa, heating rate are 15 DEG C/min；
（4）60min is incubated at 1480 DEG C, and reduces vacuum >=10-1Pa is kept；It is warming up to 1650 DEG C of insulation 10-
60min, and reduce vacuum >=10-1Pa is kept；1700 DEG C of insulation 10-40min are warming up to, improve vacuum≤10-2Pa is protected
Hold, MoSi is obtained after cooling2/SiC/B4C three-phase intensity composite ceramicses.
Embodiment 6
A kind of preparation method of molybdenum disilicide/silicon carbide/carbon boron three-phase intensity composite ceramics, it the step of it is as follows：
（1）By MoSi2Powder, C powder and B4C powder ball mill mixings, the MoSi2Powder, C powder and B4The weight ratio of C powder is 90：3：
5, incorporation time is 24 hr, adds MoSi2Powder, C powder and B4The binding agent of C powder gross weight 19.6%, and compression molding, obtain base
Material；
（2）Blank room temperature is dried, then enters the hr of oven for drying 24；
（3）Blank after drying is moved into and is covered with MoSi2Powder, C powder and B4The vacuum of the metal Si powder of C powder gross weight 14.3%
In sintering furnace, vacuum is kept 10-2Pa, heating rate are 12 DEG C/min；
（4）30min is incubated at 1400 DEG C, and reduces vacuum >=10-1Pa is kept；1600 DEG C of insulation 30min are warming up to, and
Reduce vacuum >=10-1Pa is kept；1650 DEG C of insulation 30min are warming up to, improve vacuum≤10-2Pa is kept, and is obtained after cooling
MoSi2/SiC/B4C three-phase intensity composite ceramicses.
Claims (1)
- A kind of 1. preparation method of molybdenum disilicide/silicon carbide/carbon boron three-phase intensity composite ceramics, it is characterised in that its step It is rapid as follows：（1）By MoSi2Powder, C powder and B4C powder ball mill mixings, the MoSi2Powder, C powder and B4The weight ratio of C powder is 50-95：1-10： 0.1-30, incorporation time are 8-72 hr, add MoSi2Powder, C powder and B4C powder gross weights 5-20% binding agent, and compression molding, Obtain blank；（2）Blank room temperature is dried, then enters oven for drying 1-72hr；（3）Blank after drying is moved into and is covered with MoSi2Powder, C powder and B4The vacuum-sintering of C powder gross weights 2-20% metal Si powder In stove, vacuum is kept 10-2-10-3Pa, heating rate are 1-15 DEG C/min；（4）10-60min is incubated at 1200-1480 DEG C, and reduces vacuum >=10-1Pa is kept；It is warming up to 1500-1650 DEG C of guarantor Warm 10-60min, and reduce vacuum >=10-1Pa is kept；Be warming up to 1650-1700 DEG C insulation 10-40min, improve vacuum≤ 10-2Pa is kept, and MoSi is obtained after cooling2/SiC/B4C three-phase intensity composite ceramicses.
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| CN106242576B (en) * | 2016-08-09 | 2023-11-24 | 中原工学院 | Ceramic-based Mo (Si, al) 2 Preparation method of-CBN superhard material |
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| CN107628818B (en) * | 2017-08-30 | 2020-09-25 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of carbon fiber powder reinforced molybdenum disilicide-based composite material |
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