CN108409331A - A kind of preparation method of layered porous ceramic skeleton material - Google Patents
A kind of preparation method of layered porous ceramic skeleton material Download PDFInfo
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- CN108409331A CN108409331A CN201810243268.6A CN201810243268A CN108409331A CN 108409331 A CN108409331 A CN 108409331A CN 201810243268 A CN201810243268 A CN 201810243268A CN 108409331 A CN108409331 A CN 108409331A
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Abstract
The present invention provides a kind of preparation methods of layered porous ceramic skeleton material, include the following steps：(1) by dispersant and tert-butyl alcohol stirring and dissolving；(2) hexagonal boron nitride, binder, silicon carbide, polyvinyl alcohol, modified manometer silicon dioxide, aluminium borate whisker and mango oyster shell whiting is added, stirs evenly；(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；(4) it is transferred in ball mill and carries out ball milling；(5) it is transferred to degasification in vacuum degassing machine；(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；(7) porous body is freeze-dried；(8) green body is sintered in air, argon gas is passed through as protective atmosphere after vacuumizing the air excluded in stove, while continued heating and carrying out liquid-phase sintering to obtain the final product.Material prepared by this method is light, the very high hardness of tool, and bending strength is high, it is most important that, Resisting fractre effect is good.
Description
Technical field
The present invention relates to a kind of preparation methods of layered porous ceramic skeleton material.
Background technology
With the fast development in the fields such as building, traffic, space flight and aviation and electronics industry, application of the mankind to material
More stringent requirements are proposed for energy.Traditional homogenous material early has been unable to meet industry (such as ceramics, metal and high molecular material) and answers
With requiring.Following significant challenge is new stronger, more tough and lightweight the structural material of exploitation.Metal-base composites is
One of wherein optimal material, it has the advantage of metal and ceramics concurrently, not only has high specific strength, high ratio modulus, wear-resistant,
It is light-weight, higher operating temperature can be born, but also there is good thermophysical property, therefore can both be used as it is against corrosion,
Wear-resisting, heat safe structural member, but also as conduction, heat conduction, radiation-resistant functional material, demand is growing.But it loses
Regret, this kind of material also seldom realize commercialization, trace it to its cause at present：First, production cost is high, secondary operation is difficult；Second is that
With the increase of ceramic phase reinforcement content, the toughness of composite material declines, and work to break is reduced, and performance is unstable, uses not
Enough safety, this is also the bottleneck problem that ceramic particle reinforced metal base composites never solve for many years.Meanwhile mechanics
Research confirms, when reinforced phase in the composite containing same volume but different-shape (such as stratiform, graininess, threadiness), layer
Maximum toughening effect will be presented in shape structure, and therefore, the good ceramic skeleton material of research and development stratiform, comprehensive performance is compeled in eyebrow
Eyelash.
Invention content
Technical problems to be solved：The object of the present invention is to provide a kind of preparation sides of layered porous ceramic skeleton material
Method, prepared material is light, the very high hardness of tool, and bending strength is high, it is most important that, Resisting fractre effect is good.
Technical solution：A kind of preparation method of layered porous ceramic skeleton material, ingredient by weight, including following step
Suddenly：
(1) by 3-6 parts of dispersants and the 40-70 parts of tert-butyl alcohols, stirring and dissolving；
(2) 5-10 parts of hexagonal boron nitrides, 5-8 parts of binders, 20-50 parts of silicon carbide, 1-2 parts of polyvinyl alcohol, 3-5 parts of modifications are added
Nano silicon dioxide, 5-10 part aluminium borate whisker and 5-8 parts of mango oyster shell whitings, stir evenly；
(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；
(4) it is transferred in ball mill and carries out ball milling, Ball-milling Time 8-9h, rotating speed 100-120r/min；
(5) it is transferred to degasification 20-30min in vacuum degassing machine；
(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；
(7) porous body is put into freeze drier, 48h is freeze-dried under low temperature, low pressure；
(8) green body in 370-380 DEG C of air is kept the temperature into 15min, is continuously heating to 1200 DEG C, be sintered 1h, vacuumize exclusion stove
Be passed through after interior air purity be 99.9% argon gas as protective atmosphere, while be continuously heating to 1500 DEG C heat preservation 2h progress liquid phases
It is sintered to obtain the final product, heating and cooling rate are 5 DEG C in entire sintering process.
It is further preferred that the preparation method of the modified manometer silicon dioxide is：
The first step：By 1-3 parts of gamma-aminopropyl-triethoxy-silanes and 1-3 parts of γ-(methacryloxypropyl) propyl trimethoxy silicon
5-10min is mixed in alkane and 10-20 parts of ethyl acetate；
Second step：3-5 parts of nano silicon dioxides are added, stir 10-20min；
Third walks：Filtering, drying.
It is further preferred that the dispersant is lecithin, polyoxyethylene carboxylate, cetanol, sucrose fatty ester or spits
One or more of temperature.
It is further preferred that the binder is one in urea formaldehyde resin, lac, Abietyl modified aldol resin or gum dammar
Kind is several.
It is further preferred that low temperature is ＜ -55 DEG C in the step (7), low pressure is ＜ 8Pa.
It is further preferred that the tween is Tween-20, Tween-40 or Tween-60.
Advantageous effect：
1. by adjusting the method for the present invention step parameter, it can get uniform pores, intercommunication hole, homogeneous layered or gradient and be distributed
Material.
2. by changing slurry solid concentration and freezing conditions, the control to material microstructure can be realized in wide range
System, keeps the microstructure of the biomaterials such as its microstructure and tooth, bone more similar, increases substantially toughness of material.
3. porosity is higher, and has open-celled structure.
4. the material property that the method for the present invention obtains is good, there is higher hardness, bending strength and good toughness.
5. can be applied to manufacture biomimetic material or biomaterial, have great application prospect.
Specific implementation mode
Embodiment 1
A kind of preparation method of layered porous ceramic skeleton material, ingredient by weight, include the following steps：
(1) by 3 parts of lecithin and 40 parts of tert-butyl alcohols, stirring and dissolving；
(2) 5 parts of hexagonal boron nitrides, 5 portions of lacs, 20 parts of silicon carbide, 1 part of polyvinyl alcohol, 3 parts of modified manometer silicon dioxides, 5 are added
Part aluminium borate whisker and 5 parts of mango oyster shell whitings, stir evenly；
(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；
(4) it is transferred in ball mill and carries out ball milling, Ball-milling Time 8h, rotating speed 100r/min；
(5) it is transferred to degasification 20min in vacuum degassing machine；
(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；
(7) porous body is put into freeze drier, 48h is freeze-dried at -57 DEG C, 7MPa；
(8) green body is kept the temperature into 15min in 370 DEG C of air, is continuously heating to 1200 DEG C, be sintered 1h, vacuumized and exclude in stove
Be passed through after air purity be 99.9% argon gas as protective atmosphere, while be continuously heating to 1500 DEG C heat preservation 2h progress liquid-phase sinterings
To obtain the final product, heating and cooling rate are 5 DEG C in entire sintering process.
Embodiment 2
A kind of preparation method of layered porous ceramic skeleton material, ingredient by weight, include the following steps：
(1) by 4 parts of polyoxyethylene carboxylates and 50 parts of tert-butyl alcohols, stirring and dissolving；
(2) 6 parts of hexagonal boron nitrides, 6 parts of Abietyl modified aldol resins, 30 parts of silicon carbide, 1.5 parts of polyvinyl alcohol, 4 parts of modifications are added
Nano silicon dioxide, 6 parts of aluminium borate whiskers and 6 parts of mango oyster shell whitings, stir evenly；
(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；
(4) it is transferred in ball mill and carries out ball milling, Ball-milling Time 8.5h, rotating speed 110r/min；
(5) it is transferred to degasification 25min in vacuum degassing machine；
(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；
(7) porous body is put into freeze drier, 48h is freeze-dried at -58 DEG C, 7MPa；
(8) green body is kept the temperature into 15min in 375 DEG C of air, is continuously heating to 1200 DEG C, be sintered 1h, vacuumized and exclude in stove
Be passed through after air purity be 99.9% argon gas as protective atmosphere, while be continuously heating to 1500 DEG C heat preservation 2h progress liquid-phase sinterings
To obtain the final product, heating and cooling rate are 5 DEG C in entire sintering process.
Embodiment 3
A kind of preparation method of layered porous ceramic skeleton material, ingredient by weight, include the following steps：
(1) by 5 parts of cetanols and 60 parts of tert-butyl alcohols, stirring and dissolving；
(2) 8 parts of hexagonal boron nitrides, 7 parts of gum dammars, 40 parts of silicon carbide, 1.5 parts of polyvinyl alcohol, 4 parts of modified nano-silicas are added
SiClx, 8 parts of aluminium borate whiskers and 7 parts of mango oyster shell whitings, stir evenly；
(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；
(4) it is transferred in ball mill and carries out ball milling, Ball-milling Time 8.5h, rotating speed 110r/min；
(5) it is transferred to degasification 25min in vacuum degassing machine；
(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；
(7) porous body is put into freeze drier, 48h is freeze-dried at -57 DEG C, 6MPa；
(8) green body is kept the temperature into 15min in 375 DEG C of air, is continuously heating to 1200 DEG C, be sintered 1h, vacuumized and exclude in stove
Be passed through after air purity be 99.9% argon gas as protective atmosphere, while be continuously heating to 1500 DEG C heat preservation 2h progress liquid-phase sinterings
To obtain the final product, heating and cooling rate are 5 DEG C in entire sintering process.
Embodiment 4
A kind of preparation method of layered porous ceramic skeleton material, ingredient by weight, include the following steps：
(1) by 6 parts of Tween-20s and 70 parts of tert-butyl alcohols, stirring and dissolving；
(2) 10 parts of hexagonal boron nitrides, 8 parts of urea formaldehyde resins, 50 parts of silicon carbide, 2 parts of polyvinyl alcohol, 5 parts of modified Nanos two are added
Silica, 10 parts of aluminium borate whiskers and 8 parts of mango oyster shell whitings, stir evenly；
(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；
(4) it is transferred in ball mill and carries out ball milling, Ball-milling Time 9h, rotating speed 120r/min；
(5) it is transferred to degasification 30min in vacuum degassing machine；
(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；
(7) porous body is put into freeze drier, 48h is freeze-dried at -58 DEG C, 6MPa；
(8) green body is kept the temperature into 15min in 380 DEG C of air, is continuously heating to 1200 DEG C, be sintered 1h, vacuumized and exclude in stove
Be passed through after air purity be 99.9% argon gas as protective atmosphere, while be continuously heating to 1500 DEG C heat preservation 2h progress liquid-phase sinterings
To obtain the final product, heating and cooling rate are 5 DEG C in entire sintering process.
Comparative example 1
The present embodiment is with embodiment 1 the difference is that replacing hexagonal boron nitride with silicon carbide, specially：
A kind of preparation method of layered porous ceramic skeleton material, ingredient by weight, include the following steps：
(1) by 3 parts of lecithin and 40 parts of tert-butyl alcohols, stirring and dissolving；
(2) be added 5 portions of lacs, 25 parts of silicon carbide, 1 part of polyvinyl alcohol, 3 parts of modified manometer silicon dioxides, 5 parts of aluminium borate whiskers and
5 parts of mango oyster shell whitings, stir evenly；
(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；
(4) it is transferred in ball mill and carries out ball milling, Ball-milling Time 8h, rotating speed 100r/min；
(5) it is transferred to degasification 20min in vacuum degassing machine；
(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；
(7) porous body is put into freeze drier, 48h is freeze-dried at -57 DEG C, 7MPa；
(8) green body is kept the temperature into 15min in 370 DEG C of air, is continuously heating to 1200 DEG C, be sintered 1h, vacuumized and exclude in stove
Be passed through after air purity be 99.9% argon gas as protective atmosphere, while be continuously heating to 1500 DEG C heat preservation 2h progress liquid-phase sinterings
To obtain the final product, heating and cooling rate are 5 DEG C in entire sintering process.
Comparative example 2
The present embodiment is with embodiment 1 the difference is that not containing mango oyster shell whiting, specially：
A kind of preparation method of layered porous ceramic skeleton material, ingredient by weight, include the following steps：
(1) by 3 parts of lecithin and 40 parts of tert-butyl alcohols, stirring and dissolving；
(2) be added 5 parts of hexagonal boron nitrides, 5 portions of lacs, 20 parts of silicon carbide, 1 part of polyvinyl alcohol, 3 parts of modified manometer silicon dioxides and
5 parts of aluminium borate whiskers, stir evenly；
(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；
(4) it is transferred in ball mill and carries out ball milling, Ball-milling Time 8h, rotating speed 100r/min；
(5) it is transferred to degasification 20min in vacuum degassing machine；
(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；
(7) porous body is put into freeze drier, 48h is freeze-dried at -57 DEG C, 7MPa；
(8) green body is kept the temperature into 15min in 370 DEG C of air, is continuously heating to 1200 DEG C, be sintered 1h, vacuumized and exclude in stove
Be passed through after air purity be 99.9% argon gas as protective atmosphere, while be continuously heating to 1500 DEG C heat preservation 2h progress liquid-phase sinterings
To obtain the final product, heating and cooling rate are 5 DEG C in entire sintering process.
Comparative example 3
The present embodiment is with embodiment 1 the difference is that replacing mango oyster shell whiting with aluminium borate whisker, specially：
A kind of preparation method of layered porous ceramic skeleton material, ingredient by weight, include the following steps：
(1) by 3 parts of lecithin and 40 parts of tert-butyl alcohols, stirring and dissolving；
(2) be added 5 parts of hexagonal boron nitrides, 5 portions of lacs, 20 parts of silicon carbide, 1 part of polyvinyl alcohol, 3 parts of modified manometer silicon dioxides,
10 parts of aluminium borate whiskers and 5 parts of mango oyster shell whitings, stir evenly；
(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；
(4) it is transferred in ball mill and carries out ball milling, Ball-milling Time 8h, rotating speed 100r/min；
(5) it is transferred to degasification 20min in vacuum degassing machine；
(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；
(7) porous body is put into freeze drier, 48h is freeze-dried at -57 DEG C, 7MPa；
(8) green body is kept the temperature into 15min in 370 DEG C of air, is continuously heating to 1200 DEG C, be sintered 1h, vacuumized and exclude in stove
Be passed through after air purity be 99.9% argon gas as protective atmosphere, while be continuously heating to 1500 DEG C heat preservation 2h progress liquid-phase sinterings
To obtain the final product, heating and cooling rate are 5 DEG C in entire sintering process.
The partial properties index of 1 layered porous ceramic skeleton material of table
The partial properties index of layered porous ceramic skeleton material prepared by the method for the present invention is seen the above table, we can be with its tool very
High hardness reaches as high as 21.7GPa, and bending strength is high, reaches as high as 655MPa, it is most important that, crack initiation fracture
Toughness and work to break are up to 14.0MPam respectively1/2And 1672Jm-2, Resisting fractre effect is good.
Claims (6)
1. a kind of preparation method of layered porous ceramic skeleton material, it is characterised in that：Ingredient by weight, including following step
Suddenly：
(1) by 3-6 parts of dispersants and the 40-70 parts of tert-butyl alcohols, stirring and dissolving；
(2) 5-10 parts of hexagonal boron nitrides, 5-8 parts of binders, 20-50 parts of silicon carbide, 1-2 parts of polyvinyl alcohol, 3-5 parts of modifications are added
Nano silicon dioxide, 5-10 part aluminium borate whisker and 5-8 parts of mango oyster shell whitings, stir evenly；
(3) ammonium hydroxide is added, it is 8.5 to make the pH of system；
(4) it is transferred in ball mill and carries out ball milling, Ball-milling Time 8-9h, rotating speed 100-120r/min；
(5) it is transferred to degasification 20-30min in vacuum degassing machine；
(6) it pours into mold, mold is immersed in liquid nitrogen, so that slurry is quickly solidified, obtains porous body；
(7) porous body is put into freeze drier, 48h is freeze-dried under low temperature, low pressure；
(8) green body in 370-380 DEG C of air is kept the temperature into 15min, is continuously heating to 1200 DEG C, be sintered 1h, vacuumize exclusion stove
Be passed through after interior air purity be 99.9% argon gas as protective atmosphere, while be continuously heating to 1500 DEG C heat preservation 2h progress liquid phases
It is sintered to obtain the final product, heating and cooling rate are 5 DEG C in entire sintering process.
2. a kind of preparation method of layered porous ceramic skeleton material according to claim 1, it is characterised in that：It is described to change
The preparation method of property nano silicon dioxide is：
The first step：By 1-3 parts of gamma-aminopropyl-triethoxy-silanes and 1-3 parts of γ-(methacryloxypropyl) propyl trimethoxy silicon
5-10min is mixed in alkane and 10-20 parts of ethyl acetate；
Second step：3-5 parts of nano silicon dioxides are added, stir 10-20min；
Third walks：Filtering, drying.
3. a kind of preparation method of layered porous ceramic skeleton material according to claim 1, it is characterised in that：Described point
Powder is one or more of lecithin, polyoxyethylene carboxylate, cetanol, sucrose fatty ester or tween.
4. a kind of preparation method of layered porous ceramic skeleton material according to claim 1, it is characterised in that：It is described viscous
Knot agent is one or more of urea formaldehyde resin, lac, Abietyl modified aldol resin or gum dammar.
5. a kind of preparation method of layered porous ceramic skeleton material according to claim 1, it is characterised in that：The step
Suddenly low temperature is ＜ -55 DEG C in (7), and low pressure is ＜ 8Pa.
6. a kind of preparation method of layered porous ceramic skeleton material according to claim 3, it is characterised in that：It is described to spit
Temperature is Tween-20, Tween-40 or Tween-60.
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