CN102432327A - Method for preparing aluminum oxide porous ceramic with composite structure by adopting freeze drying process - Google Patents
Method for preparing aluminum oxide porous ceramic with composite structure by adopting freeze drying process Download PDFInfo
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- CN102432327A CN102432327A CN2011102645303A CN201110264530A CN102432327A CN 102432327 A CN102432327 A CN 102432327A CN 2011102645303 A CN2011102645303 A CN 2011102645303A CN 201110264530 A CN201110264530 A CN 201110264530A CN 102432327 A CN102432327 A CN 102432327A
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Abstract
The invention discloses a method for preparing aluminum oxide porous ceramic with a composite structure by adopting a freeze drying process. In the method, ice crystal is taken as a pore-forming template, a porous biscuit is obtained by adjusting the slurry concentration and the freezing temperature, and porous ceramic is obtained by performing high-temperature sintering. The entire process has the advantages of no need of any pore-forming agent or organic additive, simple processing process, environmental friendliness and low cost, and is an environmentally-friendly process for preparing oriented porous ceramic with high porosity rate and a complex structure. The method comprises the following steps of: adding distilled water, an inorganic bonding agent, a composite sintering agent and a dispersing agent into aluminum oxide powder; fully grinding at the room temperature to obtain a suspension; degassing in vacuum; injecting into a polypropylene mold; rapidly refrigerating the suspension at low temperature; performing freeze drying in vacuum; directly sublimating the ice crystal to form pores; and putting into a high-temperature tank type electric oven for sintering to obtain aluminum oxide porous ceramics. Due to the adoption of the method, the apparent porosity and mechanical strength of the porous ceramic are greatly increased.
Description
Technical field
The present invention relates to the preparation method of a method of porous alumina ceramics, particularly a kind ofly adopt freeze drying process preparation to have the method for composite structure alumina porous ceramic.
Background technology
Porous ceramic film material has equally distributed relatively micropore, low volume density, 3 D stereo network skeleton structure, high specific surface area and unique physical surface properties; The liquids and gases medium had good selection perviousness, energy absorption or damping characteristic; High temperature resistant; Corrosion-resistant etc., be a kind of ideal support of the catalyst, thereby become a wonderful work of " energy-saving and emission-reduction " material.In addition, porous ceramic film material has broad application prospects at aspects such as gas-liquid filtration, purification separation, sound absorption damping, senior lagging material, biological implantation material, extraordinary materials for walls.The technology of preparing of porous material is the key factor of decision its structure, character and Application Areas.Ideal technology not only claimed structure is controlled, and mechanical property is reliable, and requires technology simple, and cost is low.At present, there has been kinds of processes to be used for the preparation of porous material, like organic foam impregnation method, add pore-forming material method, foaming, sol-gel method, chemical vapor infiltration or sedimentation, biomimetic synthesis etc.1. the foam impregnation legal system is equipped with ceramic foam, and its hole dimension depends primarily on the hole dimension of organic foam body, and article shape density is wayward, and organic compound combustion pollutes the environment; 2. add the pore-forming material legal system and be equipped with ceramic foam, its even air hole distribution property is poor, is not suitable for preparing the goods of high porosity; 3. foaming adds organic or inorganic chemistry material, produces foam through generation volatile gaseses such as chemical reactions, makes ceramic foam through super-dry with burning till again, and technological process is wayward; 4. sol-gel method obtains hole through phase transformation or chemical reaction, and preparation cost is high; 5. chemical vapor infiltration or sedimentation processing requirement are strict, and pore morphology is wayward, and energy expenditure is big; 6. biomimetic synthesis is a template with the natural porous organization of plant mainly, makes ceramic foam through permeable reactive, but needs to remove biological template, and technology is various and complicated, is difficult for promoting.Most of preparing methods mainly still depend on and in preparation, use organic filler, whipping agent to wait to form pore structure, see to a certain extent, caused environmental pollution.
Summary of the invention
The objective of the invention is to propose a kind ofly adopt freeze drying process preparation to have the method for composite structure alumina porous ceramic,, thereby obtain the ceramic foam of different porosities, complicated shape through critical processes such as regulation and control paste consistency, freezing temps.This method operating procedure is simple, and cost is low and need not add organic pore-forming agents etc., has avoided environmental pollution, is a kind of environment-friendly type technique.
For achieving the above object, the technical scheme that the present invention adopts is:
1) at first, gets 100g aluminum oxide powder, 150g～300g zero(ppm) water, 30g Na
2SiO
39H
2O sticker, 4g TiO
2Pack in the stainless steel jar mill with 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent, add 650g stainless steel abrading-ball again, on ball mill, carry out abundant ball mill mixing then and be configured to stable suspension liquid in 12 hours;
2) secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3) suspension liquid that will get rid of behind the bubble injects mould; Then mould is placed-30 ℃～-40 ℃ the freezing suspension liquid that makes of vacuum freeze drier to freeze fully; The suspension liquid that will freeze again is the dry back demoulding under vacuum state, obtains the porous Al identical shaped with forming mould
2O
3Biscuit;
4) then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1500 ℃～1600 ℃ with the temperature rise rate of 10 ℃/min from room temperature, is incubated 2 hours;
5) last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the alumina porous ceramic of ad hoc structure.
The machine rotating speed of said step 1) ball milling is 600 rev/mins, and mechanical milling process adopts the mode of intermittent type ball milling, and every ball milling 1 hour stops ball mill cooling 1 hour.
Described dedicated ceramic powder aqueous systems dispersion agent is HFXZ-802.
Described ball mill adopts the planetary four-head fire ball of KQM-X4/B type grinding machine.
Described forming mould is a cylindrical-shaped structure, and mold material is a Vestolen PP 7052, and thickness is 2mm.
Described vacuum freeze drier is the LGJ-10D type.
Described alumina porous ceramic porosity is greater than 50%, and ultimate compression strength is greater than 9MPa.
Frost drying technology (Freezing Casting) is to be the pore-creating template with ice; Freeze to contain the suspension liquid of ceramic particle, ice crystal promotes ceramic particle to the zone between the ice crystal branch in water congeals into ice brilliant process, forms and the microstructure of ice crystal on same scale; The ice crystal distillation is removed after lyophilize; Ceramic particle remains resident in ice intergranular form, obtains the porous microstructure of the negative replica of ice-crystal growth, heredity preferably the ice crystal pattern.Freezing and drying lyophilization has following characteristics: (1) does not have any pollution to environment, need not to add organic or the inorganic chemistry objectionable impurities; (2) formation of pore texture is a kind of physical process, does not need special template, does not also need to remove like calcining, chemical etching etc. the process of template; (3) can obtain multiple yardstick (from micron to nanometer) pore structure and micropore and lamella composite structure simultaneously; (4) facility investment is few, can realize the dead size moulding, is easy to apply.Therefore, along with the rapid expansion of porous material Application Areas with to the pay attention to day by day of environment protection, people more and more pay attention to the technology of preparing of free of contamination porous material.The present invention adopts the freeze drying process preparation to have the composite structure alumina porous ceramic, has the following advantages:
1) alumina porous ceramic of preparation is made up of macroscopic pores (circular port and laminated structure) and microcosmic aperture, has the open-celled structure of mutual perforation, through regulation and control paste consistency and lyophilize temperature, can obtain high porosity, baroque sample;
2) sticker Na
2SiO
39H
2The adding of O makes the sample after the lyophilize keep certain intensity, caves in when the demoulding and be unlikely;
3) complex sintering aids TiO
2With the adding of CuO, can reduce the sintering temperature and the sintering intensity of activation thereof of aluminum oxide;
4) suspension liquid behind the ball milling can be got rid of the bubble that produces in the mechanical milling process through behind the vacuum suction;
5) its void content of the alumina porous ceramic of preparation adopts Archimedes's drainage to measure, and adopts WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure its ultimate compression strength, adopts its microtexture of JSM-6390LV type sem observation.The alumina porous ceramic porosity that detects preparation is greater than 50%, and ultimate compression strength is greater than 9MPa.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Fig. 1 is through the photomacrograph of porous biscuit after-30 ℃ of freeze-dried-demouldings in the embodiment of the invention 1;
Fig. 2 be in the embodiment of the invention 1 through the porous biscuit after-30 ℃ of freeze-dried-demouldings behind 1500 ℃ of sintering, the ceramic foam square section electron scanning micrograph that obtains; Wherein:
Fig. 2 (a) and (b), (c), (d) are the different multiples electron scanning micrograph.
Fig. 3 be in the embodiment of the invention 1 through the porous biscuit after-30 ℃ of freeze-dried-demouldings behind 1500 ℃ of sintering, the ceramic foam longitudinal section electron scanning micrograph that obtains; Wherein:
Fig. 3 (a) and (b) are the different multiples electron scanning micrograph.
Fig. 4 be in the embodiment of the invention 2 through the porous biscuit after-30 ℃ of freeze-dried-demouldings behind 1550 ℃ of sintering, the ceramic foam square section electron scanning micrograph that obtains; Wherein:
Fig. 4 (a) and (b), (c), (d) are the different multiples electron scanning micrograph.
Fig. 5 be in the embodiment of the invention 2 through porous biscuit after-30 ℃ of lyophilize demouldings behind 1550 ℃ of sintering, the ceramic foam longitudinal section electron scanning micrograph that obtains; Wherein:
Fig. 5 (a) and (b), (c) are the different multiples electron scanning micrograph.
Fig. 6 be in the embodiment of the invention 3 through the porous biscuit after-40 ℃ of freeze-dried-demouldings behind 1600 ℃ of sintering, the ceramic foam square section electron scanning micrograph that obtains; Wherein:
Fig. 6 (a) and (b) are the different multiples electron scanning micrograph.
Fig. 7 be in the embodiment of the invention 4 through the porous biscuit after-40 ℃ of freeze-dried-demouldings behind 1500 ℃ of sintering, the ceramic foam square section electron scanning micrograph that obtains; Wherein:
Fig. 7 (a) and (b) are the different multiples electron scanning micrograph.
Embodiment
Embodiment 1:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 150g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-30 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit; Photomacrograph through porous biscuit after-30 ℃ of freeze-dried-demouldings can find out that outward appearance is complete, does not have macroscopical slight crack, and is as shown in Figure 1.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1500 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. the typical microstructure of using the alumina porous ceramic that the present invention prepares as shown in Figures 2 and 3, Fig. 2 is the cross section electron scanning micrograph of ceramic foam that behind 1500 ℃ of sintering, prepares through the porous biscuit after-30 ℃ of freeze-dried-demouldings.Visible by figure, ceramic foam is made up of macroscopical circular hole and the microcosmic aperture that is distributed on the hole wall, and pore distribution is even, has the open-celled structure of mutual perforation.Fig. 3 be through the porous biscuit after-30 ℃ of freeze-dried-demouldings behind 1500 ℃ of sintering, the electron scanning micrograph of the ceramic foam longitudinal section that obtains.Visible by figure, be approximately the circular hole structure.
7. the void content that adopts Archimedes's drainage to measure the alumina porous ceramic that uses the present invention's preparation is 62.92%.
8. adopt WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure and use the ultimate compression strength of the alumina porous ceramic of the present invention's preparation to be 9.30MPa.
Embodiment 2:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 150g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-30 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.Photomacrograph through porous biscuit after-30 ℃ of freeze-dried-demouldings can find out that outward appearance is complete, does not have macroscopical slight crack, and is as shown in Figure 1.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1550 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. use typical microstructure such as Fig. 4 and shown in Figure 5 of the alumina porous ceramic that the present invention prepares, Fig. 4 is the cross section electron scanning micrograph of ceramic foam that behind 1550 ℃ of sintering, prepares through the porous biscuit after-30 ℃ of freeze-dried-demouldings.Visible by figure, ceramic foam is made up of macroscopical slotted eye and the microcosmic aperture that is distributed on the hole wall, and pore distribution is even, has the open-celled structure of mutual perforation.Fig. 5 be through the porous biscuit after-30 ℃ of freeze-dried-demouldings behind 1550 ℃ of sintering, the electron scanning micrograph of the ceramic foam longitudinal section that obtains.Visible by figure, formed the irregular cycle hole.Because sintering temperature raises, thereby makes the duct shape that change take place.
7. the void content that adopts Archimedes's drainage to measure the alumina porous ceramic that uses the present invention's preparation is 52.52%.Compare with embodiment 1, after sintering temperature raise, void content obviously reduced.
8. adopt WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure and use the ultimate compression strength of the alumina porous ceramic of the present invention's preparation to be 12.40MPa.Compare with embodiment 1, after sintering temperature raise, ultimate compression strength increased.
Embodiment 3:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 200g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: LGJ-10D) the freezing suspension liquid that makes freezes fully, and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-40 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1600 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. use the typical microstructure of the alumina porous ceramic that the present invention prepares as shown in Figure 6, Fig. 6 is the cross section electron scanning micrograph of ceramic foam that behind 1600 ℃ of sintering, prepares through the porous biscuit after-30 ℃ of freeze-dried-demouldings.Visible by figure, formed the stratiform hole of oriented structure, its direction is consistent with the direction of growth of ice crystal, and some micropores are distributing on hole wall.Visible by the high multiple electron scanning micrograph of Fig. 6 (b), formed bridge formation between layer and the layer.
7. the void content that adopts Archimedes's drainage to measure the alumina porous ceramic that uses the present invention's preparation is 70.70%.
8. adopt WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure and use the ultimate compression strength of the alumina porous ceramic of the present invention's preparation to be 10.80MPa.
Embodiment 4:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 200g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-40 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1500 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. use the typical microstructure of the alumina porous ceramic that the present invention prepares as shown in Figure 7, Fig. 7 is the cross section electron scanning micrograph of ceramic foam that behind 1500 ℃ of sintering, prepares through the porous biscuit after-30 ℃ of freeze-dried-demouldings.Visible by figure, formed skewness, irregular laminate structure.Visible by the high multiple electron scanning micrograph of Fig. 7 (b), also formed bridge formation between layer and the layer.Compare with embodiment 3, only sintering temperature is different, causes the difference of structure, also performance is caused than big-difference.
7. the void content that adopts Archimedes's drainage to measure the alumina porous ceramic that uses the present invention's preparation is 65.52%.Compare with embodiment 3, void content reduces, and is relevant with the variation of structure.
8. adopt WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure and use the ultimate compression strength of the alumina porous ceramic of the present invention's preparation to be 16.9.MPa.Compare with embodiment 3, ultimate compression strength obviously increases, with void content reduce relevant.
Embodiment 5:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 260g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-30 ℃～-40 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1520 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. the ceramic foam with method for preparing adopts Archimedes's drainage measurement of gas porosity, adopts WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure its ultimate compression strength, adopts its microtexture of JSM-6390LV type sem observation.
Embodiment 6:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 230g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-36 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1540 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. the ceramic foam with method for preparing adopts Archimedes's drainage measurement of gas porosity, adopts WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure its ultimate compression strength, adopts its microtexture of JSM-6390LV type sem observation.
Embodiment 7:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 150g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-40 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1500 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. the ceramic foam with method for preparing adopts Archimedes's drainage measurement of gas porosity, adopts WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure its ultimate compression strength, adopts its microtexture of JSM-6390LV type sem observation.
Embodiment 8:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 150g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; Then mould being placed--(Beijing Sihuan Scientific Instrument Factory Co., Ltd produces 40 ℃ vacuum freeze drier, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1550 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. the ceramic foam with method for preparing adopts Archimedes's drainage measurement of gas porosity, adopts WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure its ultimate compression strength, adopts its microtexture of JSM-6390LV type sem observation.
Embodiment 9:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 300g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-30 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1500 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. the ceramic foam with method for preparing adopts Archimedes's drainage measurement of gas porosity, adopts WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure its ultimate compression strength, adopts its microtexture of JSM-6390LV type sem observation.
Embodiment 10:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 280g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-38 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1580 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. the ceramic foam with method for preparing adopts Archimedes's drainage measurement of gas porosity, adopts WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure its ultimate compression strength, adopts its microtexture of JSM-6390LV type sem observation.
Embodiment 11:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 260g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; (Beijing Sihuan Scientific Instrument Factory Co., Ltd produces, and model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough then mould to be placed-35 ℃ vacuum freeze drier; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1560 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. the ceramic foam with method for preparing adopts Archimedes's drainage measurement of gas porosity, adopts WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure its ultimate compression strength, adopts its microtexture of JSM-6390LV type sem observation.
Embodiment 12:
1. at first, difference weighing 100g aluminum oxide powder (Hanzhong Qiyuan New Material Co., Ltd. produces, and crosses 325 orders), 300g zero(ppm) water, 30g Na
2SiO
39H
2O sticker (Kingsoft, Chengdu chemical reagent ltd), 4g TiO
2With 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent (Hefei Xiang positizing subject skill ltd, model: HFXZ-802), in the stainless steel jar mill of packing into; Add 650g stainless steel abrading-ball; Adopt the planetary four-head fire ball of KQM-X4/B type grinding machine to carry out abundant ball mill mixing 12 hours then, be configured to stable suspension liquid, drum's speed of rotation is 600 rev/mins; Every grinding is 1 hour in mechanical milling process, stops ball mill cooling 1 hour.
2. secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3. after; Suspension liquid is injected in the polypropylene molds; Then mould is placed-40 ℃ vacuum freeze drier Beijing Sihuan Scientific Instrument Factory Co., Ltd to produce, model: the freezing suspension liquid that makes freezes fully LGJ-10D), and the suspension liquid that will freeze again successive drying under vacuum state is thorough; The demoulding then obtains the column porous Al similar with the forming mould shape
2O
3Biscuit.
4. then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1600 ℃ with the temperature rise rate of 10 ℃/min, is incubated 2 hours.
5. last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the Al of ad hoc structure
2O
3Ceramic foam.
6. the ceramic foam with method for preparing adopts Archimedes's drainage measurement of gas porosity, adopts WAW-1000 microcomputer controlled electro-hydraulic servo universal testing machine to measure its ultimate compression strength, adopts its microtexture of JSM-6390LV type sem observation.
Claims (7)
1. one kind is adopted the freeze drying process preparation to have the method for composite structure alumina porous ceramic, it is characterized in that:
1) at first, gets 100g aluminum oxide powder, 150g～300g zero(ppm) water, 30g Na
2SiO
39H
2O sticker, 4g TiO
2Pack in the stainless steel jar mill with 2.5g CuO complex sintering aids, 2.6g dedicated ceramic powder aqueous systems dispersion agent, add 650g stainless steel abrading-ball again, on ball mill, carry out abundant ball mill mixing then and be configured to stable suspension liquid in 12 hours;
2) secondly, with the suspension liquid bubble that the eliminating suspension liquid produces in mechanical milling process in the closed container that connects vacuum pump of packing into;
3) suspension liquid that will get rid of behind the bubble injects mould; Then mould is placed-30 ℃～-40 ℃ the freezing suspension liquid that makes of vacuum freeze drier to freeze fully; The suspension liquid that will freeze again is the dry back demoulding under vacuum state, obtains the porous Al identical shaped with forming mould
2O
3Biscuit;
4) then, with the porous Al of the demoulding
2O
3Biscuit is put into the high temperature cabinet-type electric furnace, rises to 1500 ℃～1600 ℃ with the temperature rise rate of 10 ℃/min from room temperature, is incubated 2 hours;
5) last, insulation naturally cools to room temperature with stove after finishing, and promptly obtains having the alumina porous ceramic of ad hoc structure.
2. employing freeze drying process preparation according to claim 1 has the method for composite structure alumina porous ceramic; It is characterized in that: the machine rotating speed of said step 1) ball milling is 600 rev/mins; Mechanical milling process adopts the mode of intermittent type ball milling; Every ball milling 1 hour stops ball mill cooling 1 hour.
3. employing freeze drying process preparation according to claim 1 has the method for composite structure alumina porous ceramic, and it is characterized in that: described dedicated ceramic powder aqueous systems dispersion agent is HFXZ-802.
4. employing freeze drying process preparation according to claim 1 has the method for composite structure alumina porous ceramic, it is characterized in that: described ball mill adopts the planetary four-head fire ball of KQM-X4/B type grinding machine.
5. employing freeze drying process preparation according to claim 1 has the method for composite structure alumina porous ceramic, and it is characterized in that: described forming mould is a cylindrical-shaped structure, and mold material is a Vestolen PP 7052, and thickness is 2mm.
6. employing freeze drying process preparation according to claim 1 has the method for composite structure alumina porous ceramic, and it is characterized in that: described vacuum freeze drier is the LGJ-10D type.
7. employing freeze drying process preparation according to claim 1 has the method for composite structure alumina porous ceramic, and it is characterized in that: described alumina porous ceramic porosity is greater than 50%, and ultimate compression strength is greater than 9MPa.
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