CN106278280B - A kind of preparation method of composite ceramics that resisting PEST - Google Patents

A kind of preparation method of composite ceramics that resisting PEST Download PDF

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CN106278280B
CN106278280B CN201610646140.5A CN201610646140A CN106278280B CN 106278280 B CN106278280 B CN 106278280B CN 201610646140 A CN201610646140 A CN 201610646140A CN 106278280 B CN106278280 B CN 106278280B
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mosi
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pest
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CN106278280A (en
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张小立
孙斌
李佳科
沈松钦
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Zhongyuan University of Technology
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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 kind of preparation methods of composite ceramics for resisting PEST, and its step are as follows: (1) by C, Si, B, B4C、MoSi2Binder is added after mixing, ball mill mixing is simultaneously pressed and molded, and drying obtains blank；(2) blank immigration is covered in the vacuum sintering furnace of Si powder, keeps vacuum degree 10‑2‑10‑3Pa, heating rate are then charged with nitrogen or argon gas then in 1400-1430 DEG C of heat preservation 5-60min for 1-10 DEG C/min, are warming up to 1450-1500 DEG C of heat preservation 5-60min；It vacuumizes, and is warming up to 1500-1550 DEG C of heat preservation 5-40min, finally cool down, obtain composite ceramics.The composite ceramics preparation cost of resistance PEST is low obtained by this method, is suitble to commercial scale.

Description

A kind of preparation method of composite ceramics that resisting PEST
Technical field
The present invention relates to a kind of technologies of preparing of composite ceramics for resisting ' PEST ', belong to the low of new type high temperature strength ceramic Cost production techniques field.
Background technique
Three most important parameters of selection aviation high-temperature structural material are the fusing point, specific gravity and high temperature antioxygen of substance 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 comprehensive performance, since its is at high cost, it is also only limited to aerospace, the only metal material of particle or short fiber reinforced There is large-scale popularization in civilian possibility.Due to intermetallic compound MoSi2, there are high-melting-point (2030 °C), moderate density (6.24×103kg/m3), good thermal conductivity and electric conductivity and there is excellent high temperature antioxygen in all metal silicides Change ability and become the material for being most hopeful to meet this requirement.In the adverse circumstances of high temperature, its continuous oxygen can be resisted The ability of change.
But it is worth mentioning that, molybdenum disilicide (MoSi2) under conditions of low temperature, the trend of oxidation is bigger.Especially When between 400-600 DEG C, molybdenum disilicide (MoSi2) material usually can become powder due to violent oxidation, cause material It is entirely ineffective, here it is molybdenum disilicide (MoSi2) " PESTING " phenomenon for being occurred in low temperature.How this low temperature is improved Antioxygenic property and molybdenum disilicide (MoSi2) material property improve a problem.It is understood that molybdenum disilicide (MoSi2) logical It is often used under the environmental condition of high temperature, heating can all pass through this low-temperature range, often so repeatedly, molybdenum disilicide every time (MoSi2) service life will be greatly reduced.Molybdenum disilicide (MoSi is improved thus2) low-temperature oxidation it is also imperative, one kind is supported The technology of preparing of the composite ceramics of anti-' PEST ' provides the method for improving its low-temperature oxidation.
Summary of the invention
It is an object of the invention to prepare to have using the infiltration technique under protective atmosphere to resist the compound of PEST phenomenon Ceramics.
The technical scheme is that a kind of preparation method for the composite ceramics for resisting PEST, its step are as follows:
(1) by following mass fraction prepare composite ceramics raw material: C 1-5%, Si 0.1-0.5%, B 0.1-0.5% and B4C 1-5%, surplus MoSi2, by C, Si, B, B4C、MoSi2Binder is added after mixing, ball mill mixing is simultaneously molded into Type, drying, obtains blank；
(2) blank immigration is covered in the vacuum sintering furnace of Si powder, keeps vacuum degree 10-2-10-3Pa, heating rate are 1-10 DEG C/min, then in 1400-1430 DEG C of heat preservation 5-60min, it is then charged with nitrogen or argon gas, is warming up to 1450-1500 DEG C Keep the temperature 5-60min；It vacuumizes, and is warming up to 1500-1550 DEG C of heat preservation 5-40min, finally cool down, obtain composite ceramics.
Binder in the step (1) is water, alcohol or phenolic resin, the quality of the water, alcohol or phenolic resin For C, Si, B, B4C、MoSi2The 10-30% of gross mass.
Binder in the step (1) is the mixture of alcohol and phenolic resin, the quality of the alcohol is C, Si, B, B4C、MoSi2The 10-20% of gross mass, the quality of the phenolic resin are C, Si, B, B4C、MoSi2The 10-20% of gross mass.
The quality of Si powder is C, Si, B, B in the step (2)4C、MoSi2The 10-20% of gross mass.
The beneficial effects of the present invention are: the present invention utilizes MoSi2, C, Si, B and B4C element powder, addition alcohol or water Jie, Binder ball mill mixing, compression molding, infiltration Si is sintered under protective atmosphere, and resulting materials can resist PEST phenomenon, and And residual intensity is up to 70% after low-temperature oxidation, the composite ceramics preparation cost of resistance PEST is low obtained by this method, is suitble to industry rule Mould.
Specific embodiment
Embodiment 1
A kind of preparation method of composite ceramics that resisting PEST, its step are as follows:
Weigh MoSi in proportion respectively2 91.8g、C 3g、B4C 5g, Si 0.1g, B0.1g, after evenly mixing ball milling 48 hr.After the above powder to be added to the phenolic resin of 20g and the mixture of alcohol, mixes and be pressed and molded.After being dried in air It is dried in 110 degree of baking ovens.It moves in the vacuum sintering furnace for being covered with 12g metallic silicon power and is sintered.Heating rate is 3 DEG C/min, Vacuum degree is 10-3Pa or so.It is warming up to 1400-1430 DEG C of heat preservation 30min；After being filled with argon gas, 1500 DEG C are warming up to, heat preservation 30min.1550 DEG C are warming up to, 10min, vacuum degree 10 are kept the temperature-3Pa, then furnace cooling, cool down feeding, then at 500 DEG C 3hr is heated in air furnace, measuring composite ceramics residual intensity is 130MPa, does not have ' PEST ' phenomenon.
Embodiment 2
A kind of preparation method of composite ceramics that resisting PEST, its step are as follows:
Weigh MoSi in proportion respectively2 90.5g、C3.75g、B 0.25g、B4C 5g, Si 0.5g, after evenly mixing ball milling 48hr.After the above powder to be added to the phenolic resin of 25g and the mixture of alcohol, mixes and be pressed and molded.After being dried in air It is dried in 110 degree of baking ovens.It moves in the vacuum sintering furnace for being covered with 15g metallic silicon power and is sintered.Heating rate be 5 DEG C/ Min, vacuum degree 10-3Pa or so.It is warming up to 1400-1430 DEG C of heat preservation 20min；After being filled with argon gas, 1500 DEG C are warming up to, heat preservation 20min.1550 DEG C are warming up to, 10min, vacuum degree 10 are kept the temperature-3Pa.Then furnace cooling, cool down feeding.Then at 500 DEG C 3hr is heated in air furnace, measuring composite ceramics residual intensity is 127 MPa.There is no ' PEST ' phenomenon.
Embodiment 3
A kind of preparation method of composite ceramics that resisting PEST, its step are as follows:
Weigh MoSi in proportion respectively2 95g、C 1.25g、B4C 5g, B 0.5g, Si 0.25g are uniformly mixed Ball milling 48hr afterwards.After the above powder to be added to the phenolic resin of 30g and the mixture of alcohol, mixes and be pressed and molded.In air It is dried in 110 degree of baking ovens after drying.It moves in the vacuum sintering furnace for being covered with 18g metallic silicon power and is sintered.Heating rate is 5 DEG C/min, vacuum degree is 10-3Pa or so.It is warming up to 1400-1430 DEG C of heat preservation 20min；After being filled with nitrogen, 1500 DEG C are warming up to, Keep the temperature 25min.1550 DEG C are warming up to, 15min, vacuum degree 10 are kept the temperature-3Pa.Then furnace cooling, cool down feeding.Then exist 3hr is heated in 500 DEG C of air furnaces, measuring composite ceramics residual intensity is 119 MPa.There is no ' PEST ' phenomenon.
Embodiment 4
A kind of preparation method of composite ceramics that resisting PEST, its step are as follows:
A kind of preparation method of composite ceramics that resisting PEST, its step are as follows:
(1) raw material of composite ceramics: C 1%, Si 0.1%, B 0.1% and B is prepared by following mass fraction4C 1%, surplus For MoSi2, by C, Si, B, B4C、MoSi2Phenolic resin is added after mixing, the quality of phenolic resin is C, Si, B, B4C、 MoSi2The 10% of gross mass, ball mill mixing are simultaneously pressed and molded, and drying obtains blank；
(2) blank immigration is covered in the vacuum sintering furnace of Si powder, keeps vacuum degree 10-2 Pa, heating rate be 1 DEG C/ Min is then charged with nitrogen or argon gas then in 1400 DEG C of heat preservation 5min, is warming up to 1450 DEG C of heat preservation 5min；It vacuumizes, and rises Temperature finally cools down to 1500 DEG C of heat preservation 5min, obtains composite ceramics.
Embodiment 5
A kind of preparation method of composite ceramics that resisting PEST, its step are as follows:
A kind of preparation method of composite ceramics that resisting PEST, its step are as follows:
(1) raw material of composite ceramics: C 5%, Si 0.5%, B 0.5% and B is prepared by following mass fraction4C 5%, surplus For MoSi2, by C, Si, B, B4C、MoSi2The mixture of alcohol and phenolic resin, the quality of the alcohol are added after mixing For C, Si, B, B4C、MoSi2The 10% of gross mass, the quality of the phenolic resin are C, Si, B, B4C、MoSi2Gross mass 20%, ball mill mixing is simultaneously pressed and molded, and drying obtains blank；
(2) blank immigration is covered in the vacuum sintering furnace of Si powder, keeps vacuum degree 10-3Pa, heating rate be 10 DEG C/ Min is then charged with nitrogen or argon gas then in 1430 DEG C of heat preservation 60min, is warming up to 1500 DEG C of heat preservation 60min；It vacuumizes, and 1550 DEG C of heat preservation 40min are warming up to, finally cools down, obtains composite ceramics.
Binder in the step (1) is water, alcohol or phenolic resin, the quality of the water, alcohol or phenolic resin For C, Si, B, B4C、MoSi2The 10-30% of gross mass.
Embodiment 6
A kind of preparation method of composite ceramics that resisting PEST, its step are as follows:
A kind of preparation method of composite ceramics that resisting PEST, its step are as follows:
(1) raw material of composite ceramics: C 2%, Si 0.2%, B 0.2% and B is prepared by following mass fraction4C 3%, surplus For MoSi2, by C, Si, B, B4C、MoSi2The mixture of alcohol and phenolic resin, the quality of the alcohol are added after mixing For C, Si, B, B4C、MoSi2The 15% of gross mass, the quality of the phenolic resin are C, Si, B, B4C、MoSi2Gross mass 20%, ball mill mixing is simultaneously pressed and molded, and drying obtains blank；
(2) blank immigration is covered in the vacuum sintering furnace of Si powder, keeps vacuum degree 10-3Pa, heating rate be 5 DEG C/ Min is then charged with nitrogen or argon gas then in 1430 DEG C of heat preservation 20min, is warming up to 1480 DEG C of heat preservation 40min；It vacuumizes, and 1520 DEG C of heat preservation 30min are warming up to, finally cools down, obtains composite ceramics.
Binder in the step (1) is water, alcohol or phenolic resin, the quality of the water, alcohol or phenolic resin For C, Si, B, B4C、MoSi2The 10-30% of gross mass.

Claims (4)

1. a kind of preparation method for the composite ceramics for resisting PEST, it is characterised in that its step are as follows:
(1) raw material of composite ceramics: C 1-5%, Si 0.1-0.5%, B 0.1-0.5% and B is prepared by following mass fraction4C 1- 5%, surplus MoSi2, by C, Si, B, B4C、MoSi2Binder is added after mixing, ball mill mixing is simultaneously pressed and molded, drying, Obtain blank；
(2) blank immigration is covered in the vacuum sintering furnace of Si powder, keeps vacuum degree 10-2-10-3Pa, heating rate 1-10 DEG C/min then in 1400-1430 DEG C of heat preservation 5-60min is then charged with nitrogen or argon gas, it is warming up to 1450-1500 DEG C of heat preservation 5-60min；It vacuumizes, and is warming up to 1500-1550 DEG C of heat preservation 5-40min, finally cool down, obtain composite ceramics.
2. the preparation method of the composite ceramics according to claim 1 for resisting PEST, it is characterised in that: the step (1) In binder be phenolic resin, the quality of the phenolic resin is C, Si, B, B4C、MoSi2The 10-30% of gross mass.
3. the preparation method of the composite ceramics according to claim 1 for resisting PEST, it is characterised in that: the step (1) In binder be alcohol and phenolic resin mixture, the quality of the alcohol is C, Si, B, B4C、MoSi2Gross mass 10-20%, the quality of the phenolic resin are C, Si, B, B4C、MoSi2The 10-20% of gross mass.
4. the preparation method of the composite ceramics according to claim 1 for resisting PEST, it is characterised in that: the step (2) The quality of middle Si powder is C, Si, B, B4C、MoSi2The 10-20% of gross mass.
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Publication number Priority date Publication date Assignee Title
CN103159482A (en) * 2011-12-12 2013-06-19 洛阳新巨能高热技术有限公司 A method for preparing Mo (Sil-x, alx)2/MoSi2complex-phase molybdenum silicide heating element
CN105565816A (en) * 2015-12-12 2016-05-11 中原工学院 Preparation method of MoSi2/MoB/SiC three-phase ceramic

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Publication number Priority date Publication date Assignee Title
JP4515038B2 (en) * 2003-04-04 2010-07-28 日鉱金属株式会社 MoSi2 powder, method for producing the powder, heating element using the powder, and method for producing the heating element

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Publication number Priority date Publication date Assignee Title
CN103159482A (en) * 2011-12-12 2013-06-19 洛阳新巨能高热技术有限公司 A method for preparing Mo (Sil-x, alx)2/MoSi2complex-phase molybdenum silicide heating element
CN105565816A (en) * 2015-12-12 2016-05-11 中原工学院 Preparation method of MoSi2/MoB/SiC three-phase ceramic

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原位SiC颗粒增强MoSi2基复合材料的显微组织和力学性能;张来启等;《金属学报》;20010331;第37卷(第3期);第1304页左栏第4段
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