CN106588074A - Method for preparation of gradient porous ceramic by process combining slip casting and vacuum foaming - Google Patents
Method for preparation of gradient porous ceramic by process combining slip casting and vacuum foaming Download PDFInfo
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Abstract
The invention relates to a method for preparation of a gradient porous ceramic by a process combining slip casting and vacuum foaming. The method includes the steps of: a) adding a sintering aid, a binder and ceramic powder into water, conducting ball-mill mixing for a period of time, then adding a foaming agent, and further performing ball milling to obtain a stable incompletely foamed water-based slurry; b) casting the water-based slurry obtained by step a) into a hygroscopic mold, performing standing for a period of time, transferring the material into a vacuum drying box overall before molding, conducting vacuum pumping and pressure maintaining under a constant temperature condition, thus obtaining a gradient porous ceramic green body; and c) removing the binder from the gradient porous ceramic green body prepared by step b), and conducting sintering to obtain a gradient porous ceramic material. The method provided by the invention has the advantages of simple process, rapidity and low cost, and is suitable for large-scale application.
Description
Technical field
This law invention is related to the method that a kind of injection forming-vacuum foam technique prepares gradient porous ceramics, belongs to porous ceramicss
Field.
Background technology
Porous ceramicss are the materials that a class has wide application prospect, and its low-density, high porosity, uniform microcosmic are tied
Structure, low-k and three-dimensional netted air hole structure make its can apply to energy storage, catalysis reduce, be separated by filtration,
The fields such as radar filtering, sensor.The gradient porous structure ceramic of corrosion-and high-temp-resistant then further can be widened on this basis
Application.The preparation technology of gradient porous ceramics is mainly comprising lay-up method, centrifuging, 3 D-printing, template etc..Lamination
Gradient porous material technique prepared by method is especially complex, needs by monolayer multiple stacking, and general interface layer is obvious；As in
Disclosed in state's patent CN102916251A, a kind of can pass through with wideband wave transparent performance reduces thermal stress and lifts high-temperature mechanics
The gradient stack-design of energy.Chinese patent CN103896624A discloses a kind of many using centrifugation Freeze Drying Technique preparation gradient
The technique of hole ceramics, has obtained a kind of " interior close outer thin ", the ceramics of the bionic gradient without sharp interface, but the method and has been only applicable to
The preparation of column functionally gradient material (FGM), limits range of application.Chinese patent CN101690828A discloses one kind and adopts 3 D-printing
What technology was realized, outer layer densification, the loose gradient porous ceramics support of internal layer can be prepared.Although the method no matter from precision also
It is all have very much practicality for structural complexity, but which must relies on expensive experimental facilitiess realize that production cost is high.Closely
Nian Lai, the porous ceramicss method for preparing high porosity using foaming are also gradually used by people, such as Chinese patent
CN104311114A discloses the technique that a kind of vacuum foam prepares orientation gradient porous ceramics with reference to Freeze Drying Technique, the work
Skill needs to prepare under cryogenic, and lyophilization is a kind of higher process of production cost, does not meet wanting for low-carbon environment-friendly
Ask.
Have much with regard to how to prepare the research with depth-graded porous structure ceramic, but one-time formed technics comparing
It is few, thus it is how simple, quick, prepare gradient porous ceramics at low cost and be still a problem for requiring study.
The content of the invention
For the problem that prior art is present, it is an object of the invention to provide a kind of prepare ladder simply, quickly, at low cost
The method of degree porous ceramicss.
Here, the present invention provides a kind of method for preparing gradient porous ceramics material, comprise the following steps：
A) sintering aid, binding agent, ceramic powder are added to the water, ball milling mixing adds foaming agent for a period of time afterwards, continue ball milling
Obtain the stable water-based slurry not foamed completely；
B) water-based slurry obtained by step a) is cast in water absorption mould, stands a period of time, it is overall before shaping to move to
In vacuum drying oven, the evacuation pressurize under constant temperature obtains gradient porous ceramics biscuit；
C) the gradient porous ceramics biscuit for preparing step b) takes off binding agent, sintering and obtains gradient porous ceramics material.
The method that the present invention combines vacuum foam using injection forming, using the slurry for non-fully foaming, it is ensured that slurry
Mobility, is conducive to which to be full of the mould of complicated shape；In combination with vacuum foam, can artificially regulate and control foaming as needed
Degree.Base pastes moisture is partially absorbed by water absorption mould, and adopt vacuum foam so that the upper strata porosity shows
Writing increases, and aperture significantly increases.Under constant temperature, with slurry moisture reduce, base substrate can gradually molding, so as to define
From bottom to top by densification to loose gradient-structure.Present invention process is simple, quick, low cost, is suitable for large-scale application.
It is preferred that the gradient porous ceramics material is Si3N4、SiC、Al2O3、ZrO2Or mullite；Step a)
In, the ceramic powder is powder corresponding with the gradient porous ceramics material.
It is preferred that in step a), the sintering aid is Y2O3、Al2O3、Yb2O3、Lu2O3、Sm2O3、
SiO2、Nd2O3、Eu2O3In at least one.
It is preferred that in step a), the binding agent be water-soluble binder Isobam, polyvinyl alcohol, Polyethylene Glycol and
At least one in water solublity isobutylene-based polymer, preferably isobutylene maleic acid anhydride copolymer Isobam, which can be in pottery
Carry out slurry by other dispersants need not be added during the function of binding agent and dispersant, i.e. slurry are functioned simultaneously as in porcelain slurry
Preferably disperse.
It is preferred that in step a), the foaming agent is n -Propyl gallate.
It is preferred that in step a), the sintering aid, the ratio between binding agent, foaming agent, ceramic powder and water are
(0.2～25)：(0.05～10)：(0.1～10)：(10～250)：100.
It is preferred that in step a), the rotational speed of ball-mill before adding foaming agent and/or after addition foaming agent is 150～350 revs/min
Clock, adds the Ball-milling Time before foaming agent to be 0.1～3 hour, and after adding foaming agent, Ball-milling Time is 0.1～3 hour, altogether
Ball-milling Time is 1.5～4 hours.
It is preferred that in step b), time of repose is 0～3 hour.
It is preferred that in step b), the temperature of the constant temperature is 0～80 DEG C, and vacuum pressure is 5～90kPa, the dwell time
It is 12～48 hours.
It is preferred that in step b), the water absorption mould is gypsum mold, the gypsum mold be monoblock gypsum mold or
The combination of polylith gypsum mold；Or the water absorption mould is the combination of water absorption mould and unwetted mould.
It is preferred that in step c), the de- binding agent is under air conditionses, with 0.2～5 DEG C of heating rate per minute
400～800 DEG C are warming up to, 0.5～5 hour is incubated.
It is preferred that in step c), the sintering is under inert atmosphere conditions, 1500 are risen to 1～10 DEG C/min～
1950 DEG C, 1～12 hour is incubated, the pressure of inert atmosphere is 0.1～5M Pa.
It is preferred that gradient obtained by being controlled as the vacuum of the content of foaming agent and/or step b) in regulating step a) is more
The porosity of hole ceramics, controls the gradient-structure of porous ceramicss by the time of repose of regulation and control step b) injection formings.
The porous ceramicss that obtained of the present invention be increased continuously by bottom to the top layer porosity, the gradient knot of the continuous increase in aperture
Structure, its average porosity are 60～95%, and pore size distribution range is 0.1～300 μm.
Description of the drawings
Fig. 1 shows the pictorial diagram of porous silicon nitride ceramic obtained in an embodiment of the invention；
Fig. 2 shows porous silicon nitride XRD tests collection of illustrative plates obtained in an embodiment of the invention；
Fig. 3 shows the microcosmic shape of the different multiplying under a scanning electron microscope of porous silicon nitride obtained in an embodiment of the invention
Looks figure.
Specific embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and following embodiments, it should be appreciated that accompanying drawing and following embodiments are only
For illustrating the present invention, and the unrestricted present invention.
The present invention provides the technique that a kind of injection forming prepares gradient porous ceramics with reference to vacuum drying.The ceramics include but not
It is limited to Si3N4、SiC、Al2O3、ZrO2Or mullite etc..In one embodiment, preparation process is as follows.
1) sintering aid, binding agent, foaming agent, ceramic powder are added in aqueous solvent (such as deionized water), ball milling
It is mixed to get uniform water-based slurry.
Wherein ceramic powder is corresponding with the ceramic material that need to be prepared, for example, can be Si3N4Powder body, SiC powder, Al2O3Powder
Body, ZrO2Powder body or 3Al2O3·2SiO2Powder body etc..
Sintering aid can be Y2O3、Al2O3、Yb2O3、Lu2O3、Sm2O3、SiO2、Nd2O3、Eu2O3In it is any one
Plant or the two or more mixture constituted with arbitrary proportion.
Binding agent (can include water-soluble for water-soluble binder polyvinyl alcohol, Polyethylene Glycol, water solublity isobutylene-based polymer
Property binding agent isobutylene maleic acid anhydride polymer Isobam) etc..Preferably using Isobam as binding agent.So,
Isobam can double as binding agent and dispersant, and without the need for additionally adding dispersant, reduce material composition and experimental procedure.
When using other water-soluble binders, dispersant such as ammonium polyacrylate etc. can also be added simultaneously.In one example, with
Polyvinyl alcohol is binding agent, and with ammonium polyacrylate as dispersant.
Foaming agent includes but is not limited to n -Propyl gallate etc..
Resulting water-based slurry preferably with mobility rather than full foamed slurry, so as to solve full foamed slurry without
Method is completely filled with the problem of mould, is conducive to which to be full of the mould of complicated shape.In one example, the order of addition of each composition
For：First sintering aid, binding agent, ceramic powder are added in aqueous solvent, ball milling mixing adds foaming agent for a period of time afterwards, after
Continuous ball milling obtains the stable water-based slurry not foamed completely.Control Ball-milling Time and rotating speed can make slurry not complete after ball milling mixing
It is complete to foam.For example, rotational speed of ball-mill can be 150-350r/min, add the Ball-milling Time before foaming agent be 0.1-3h, add and send out
After infusion, Ball-milling Time can be 0.1-3h, and Ball-milling Time can be 1.5-4h altogether, and rotational speed of ball-mill may be the same or different twice in front and back.
Ratio between sintering aid, binding agent, foaming agent, ceramic powder and water can be (0.2-25)：(0.05-10)：
(0.1-10)：(10-250)：100.The porosity of gradient porous ceramics as obtained by the content for controlling foaming agent can be controlled.
In the content range of above-mentioned foaming agent, the content of foaming agent is more, and the porosity is bigger.
2) above-mentioned water-based slurry is cast in gypsum mold, stands a period of time, it is then overall to move to vacuum drying oven
In, the evacuation pressurize under constant temperature.In this process, water-based slurry is made to foam completely using lower pressure environment, low pressure constant temperature
A period of time disposed slurry is curing molding.Can be absorbed water by gypsum mold as injection forming stands a period of time disposed slurry bottom, plus
Upper upper slurry gravity causes the bottom base substrate porosity to diminish, and base substrate top is foamed due to vacuum cause, increases aperture
Greatly, thus define and increased continuously by bottom to the top layer porosity, the gradient-structure of the continuous increase in aperture.
Wherein, gypsum mold can be the combination of monoblock gypsum mold or polylith gypsum mold, mould can be make slurry into
Any shape, or gypsum mold of type and the combination of unwetted mould.In addition, it should be understood that in the present invention, mould
It is not limited to gypsum mold, or other water absorption moulds.
Time of repose can be 0-3h.By controlling time of repose, the degree absorbed water by slurry can be controlled, it is many so as to control
The gradient-structure of hole ceramics.Time of repose is longer, then bottom water suction is more abundant, then expansion is more difficult in vacuum, thus
It is bigger with the air vent aperture difference that upper strata vacuum foam is generated.Meanwhile, time of repose is unsuitable long, if for example time of repose exceedes
3 hours, then slurry can be caused integrally to absorb water excessive and lose plasticity, it is impossible to reach the effect of vacuum foam.Preferably in slurry
Integrally move in vacuum drying oven before material molding.Preferably, time of repose is 0-1 hours.If increasing base substrate height, can fit
When prolongation time of repose.
Vacuum gradient foaming is carried out in vacuum drying oven, constant temperature pressurize is preserved, under constant temperature, with slurry moisture
Reduce, base substrate can gradually molding, so as to define from bottom to top by densification to loose gradient-structure.Vacuum pressure can be 5-
90kPa.Holding temperature can be 0-80 DEG C, and the dwell time can be 12-48h.The present invention adopts vacuum foam mode so that pore
Rate and aperture have bigger artificial adjustability.The porosity of gradient porous ceramics and hole as obtained by control vacuum can be controlled
Footpath, vacuum are less, and air vent aperture is bigger.
3) base substrate of molding is taken out, de- binding agent, sintering obtain gradient porous ceramics material.The concrete bar of de- binding agent
Part can be suitably selected according to selected binding agent.In one example, under air conditionses, with 0.2-5 DEG C per point
The heating rate of clock is warming up to 400-800 DEG C, is incubated 0.5-5 hours.The actual conditions of sintering can be fitted according to the material of ceramics
Work as selection.For example when gradient porous silicon nitride ceramics is prepared, sintering can be under the conditions of inert atmosphere (such as nitrogen),
1500-1950 DEG C is risen to 1-10 DEG C/min, 1-12 hours are incubated, the pressure of inert atmosphere is 0.1-5M Pa.
More specifically, in an example for preparing gradient porous silicon nitride ceramics, comprising the steps：
A water is mixed to form into aqueous solution with water-soluble binder Isobam stirrings)；
B sintering aid and beta-silicon nitride powder ball milling mixing are added for a period of time in aqueous solution), is added foaming agent to continue mix homogeneously and is obtained
To water-based slurry；
C) slurry is poured in gypsum mold, is stood, and is put in vacuum drying oven, 5-90kPa realizes foaming, pressurize at 30 DEG C
12h, obtains final product ceramic body after sample drying；
D ceramic body is carried out into unsticking, sintering) and obtains gradient porous silicon nitride ceramics.
The porous ceramicss microscopic appearance that obtained of the present invention is good, is the porous ceramicss that aperture is incremented by into gradient, its average air
Porosity is 60-95%, preferably 65-93%, and pore size distribution range is 0.1-300 μm, preferably 0.5-250 μm.
The present invention is to combine slip casting by vacuum foam, and process is simple, method with low cost prepare gradient porous
Ceramics.The present invention is applied to gradient porous silicon nitride ceramics, is also suitable preparation SiC, Al2O3、ZrO2, the advanced ladder such as mullite
Degree porous structure ceramic.It is 60-95% that Jing Archimedes's drainages measure the ceramic average porosity of gained, and pore-size distribution is 0.1-
300μm.The porosity and aperture can be adjusted by the size of the content of foaming agent, slip casting time of repose and/or vacuum.Very
Reciprocal of duty cycle is less, and air vent aperture is bigger.Foaming agents content is more, and the porosity is bigger.
Compared to the prior art compared with the present invention has the advantages that：
(1) process is simple, uniform pore diameter gradual change, without gradient interface；
(2) aperture and the porosity can be adjusted by time of repose before the content and foaming of the size of vacuum and foaming agent.
Include some exemplary embodiments further below the present invention is better described.It should be understood that the present invention is described in detail
Above-mentioned embodiment, and following examples are only illustrative of the invention and is not intended to limit the scope of the invention, the skill of this area
Some nonessential modifications and adaptations that art personnel the above of the invention is made belong to protection scope of the present invention.Separately
Outward, in following technological parameters concrete proportioning, time, temperature etc. are also only exemplary, and those skilled in the art can be above-mentioned
Suitable value is selected in the range of restriction.
Embodiment 1
(1) 0.1g Isobam are dissolved in 13.3g deionized waters, add 1g Y2O3、20g Si3N4；
(2) above-mentioned slurry is transferred in politef ball grinder, with silicon nitride ball as ball-milling medium, ball grinding stirring 1h, rotating speed
For 300r/min, 0.6g foaming agent is added, continue 300r/min stirring 1h and obtain uniform water-based slurry；
(3) by the slurry cast for stirring in gypsum mold, 1h is stood, is then integrally placed in vacuum drying oven, keep temperature
Spend for 30 DEG C, be evacuated down to 80kPa pressurize 24h；
(4) base substrate of above-mentioned molding is taken out, with the ramp of 5 DEG C/min to 600 DEG C, is incubated two hours and removes Organic substance, so
Afterwards in 0.5MPa N2With the ramp of 10 DEG C/min to 1700 DEG C in environment, two hours are incubated, furnace cooling, finally
To the silicon nitride ceramics of loose structure in gradient from the bottom to top.The porosity of the sample is 64.9%.
Fig. 1 illustrates silicon nitride gradient porous ceramics pictorial diagram prepared by this example, and as can be seen from the figure sample pore is under
It is supreme to change in gradient.
Embodiment 2
(1) 0.15g polyvinyl alcohol is dissolved in 16.2g deionized waters, adds 0.81g Y2O3、20.19g Si3N4, 0.02g gather
Ammonium acrylate；
(2) above-mentioned slurry is transferred in politef ball grinder, with silicon nitride ball as ball-milling medium, ball grinding stirring 0.5h, is turned
Speed is 350r/min, adds 0.88g foaming agent, continues 250r/min ball milling 1.5h and obtains uniform water-based slurry；
(3) by the slurry cast for stirring in gypsum mold, and it is integrally placed in vacuum drying oven, keeping temperature is 40 DEG C,
It is evacuated down to 40KPa pressurize 18h；
(4) base substrate of above-mentioned molding is taken out, with the ramp of 5 DEG C/min to 600 DEG C, is incubated two hours and removes Organic substance, so
Afterwards in 1MPa N2With the ramp of 10 DEG C/min to 1750 DEG C in environment, two hours are incubated, furnace cooling is finally obtained
The silicon nitride ceramics of loose structure in gradient from the bottom to top.The porosity of the sample is 78.6%.
Fig. 2 illustrates the XRD test collection of illustrative plates of silicon nitride gradient porous ceramics prepared by present implementation, can send out from result
It is existing, except β-Si in sample3N4Crystal grain and very small amount Y20Si12O48N4Beyond Grain-Boundary Phase, other crystalline components or crystal grain are had no
Phase.
Embodiment 3
(1) 0.05g Isobam are dissolved in 20.35g deionized waters, add 0.61g Y2O3、20.39g Si3N4；
(2) above-mentioned slurry is transferred in politef ball grinder, with silicon nitride ball as ball-milling medium, ball grinding stirring 1.5h, is turned
Speed is 200r/min, adds 0.46g foaming agent, continues 250r/min stirring 1h and obtains uniform water-based slurry；
(3) by the slurry cast for stirring in gypsum mold, 0.5h is stood, and is integrally placed in vacuum drying oven, keep temperature
Spend for 50 DEG C, be evacuated down to 15kPa pressurize 36h；
(4) base substrate of above-mentioned molding is taken out, with the ramp of 5 DEG C/min to 600 DEG C, is incubated two hours and removes Organic substance, so
Afterwards in 2.5MPa N2With the ramp of 10 DEG C/min to 1800 DEG C in environment, two hours are incubated, furnace cooling, finally
To the silicon nitride ceramics of loose structure in gradient from the bottom to top.The porosity of the sample is 89.1%.
Fig. 3 shows the microscopic appearance figure of the silicon nitride gradient porous ceramics of present implementation preparation, as can be seen from the figure greatly
Hole aperture is 100-300 μm, and aperture is by β-Si3N4Space composition after whisker bridge joint；β-Si in figure3N4Rod-like crystal whisker has preferable
Draw ratio, rod particularly in gross blow hole is brilliant to have preferable pattern.
Industrial applicability：Present invention can apply to energy storage, catalysis are reduced, are separated by filtration, radar is filtered, sensor
In field.
Claims (11)
1. a kind of method for preparing gradient porous ceramics material, it is characterised in that comprise the following steps：
a）Sintering aid, binding agent, ceramic powder are added to the water, ball milling mixing adds foaming agent for a period of time afterwards, continue ball milling and obtain the stable water-based slurry not foamed completely；
b）By step a）The water-based slurry of gained is cast in water absorption mould, stands a period of time, and overall before shaping to move in vacuum drying oven, the evacuation pressurize under constant temperature obtains gradient porous ceramics biscuit；
c）By step b）The de- binding agent of the gradient porous ceramics biscuit of preparation, sintering obtain gradient porous ceramics material.
2. method according to claim 1, it is characterised in that the gradient porous ceramics material is Si3N4、SiC、Al2O3、ZrO2Or mullite；Step a）In, the ceramic powder is powder corresponding with the gradient porous ceramics material.
3. method according to claim 1 and 2, it is characterised in that step a）In, the sintering aid is Y2O3、Al2O3、Yb2O3、Lu2O3、Sm2O3、SiO2、Nd2O3、Eu2O3In at least one；
The binding agent is at least one in water-soluble binder isobutylene maleic acid anhydride copolymer Isobam, polyvinyl alcohol, Polyethylene Glycol and other water solublity isobutylene-based polymers, preferably isobutylene maleic acid anhydride copolymer Isobam；
The foaming agent is n -Propyl gallate.
4. according to the method in any one of claims 1 to 3, it is characterised in that step a）In, the sintering aid, the ratio between binding agent, foaming agent, ceramic powder and water are（0.2～25）：（0.05～10）：（0.1～10）：（10～250）：100.
5. method according to any one of claim 1 to 4, it is characterised in that step a）In, the rotational speed of ball-mill before adding foaming agent and/or after addition foaming agent is 150～350 revs/min, adds the Ball-milling Time before foaming agent to be 0.1～3 hour, and after adding foaming agent, Ball-milling Time is 0.1～3 hour, and Ball-milling Time is 1.5～4 hours altogether.
6. method according to any one of claim 1 to 5, it is characterised in that step b）In, time of repose is 0～3 hour.
7. method according to any one of claim 1 to 6, it is characterised in that step b）In, the temperature of the constant temperature is 0～80 DEG C, and vacuum pressure is 5～90kPa, and the dwell time is 12～48 hours.
8. method according to any one of claim 1 to 7, it is characterised in that step b）In, the water absorption mould is gypsum mold, and the gypsum mold is the combination of monoblock gypsum mold or polylith gypsum mold；Or the water absorption mould is the combination of water absorption mould and unwetted mould.
9. method according to any one of claim 1 to 8, it is characterised in that step c）In, the de- binding agent is, under air conditionses, to be warming up to 400～800 DEG C with 0.2～5 DEG C of heating rate per minute, is incubated 0.5～5 hour；The sintering is under inert atmosphere conditions, to rise to 1500～1950 DEG C with 1～10 DEG C/min, is incubated 1～12 hour, and the pressure of inert atmosphere is 0.1～5 M Pa.
10. method according to any one of claim 1 to 9, it is characterised in that by regulating step a）The content and/or step b of middle foaming agent）Vacuum come control gained gradient porous ceramics the porosity, by regulate and control step b）The time of repose of injection forming is controlling the gradient-structure of porous ceramicss.
11. methods according to any one of claim 1 to 10, it is characterized in that, the porous ceramicss for being obtained be increased continuously by bottom to the top layer porosity, the gradient-structure of the continuous increase in aperture, its average porosity is 60～95%, and pore size distribution range is 0.1～300 μm.
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