CN115196976A - Gradient porous ceramic and preparation method thereof - Google Patents
Gradient porous ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of gradient porous ceramic, which comprises the following steps: respectively preparing ceramic slurry of each pore layer in the gradient porous ceramic; pouring ceramic slurry into a water-absorbing mold in sequence according to the arrangement sequence of pore layers in the gradient porous ceramic, after pouring the ceramic slurry of one pore layer, solidifying the ceramic slurry to a preset thickness by utilizing the water absorption of the water-absorbing mold, pouring out the residual ceramic slurry in the water-absorbing mold, and pouring the ceramic slurry of another pore layer in the same way until the pouring of the ceramic slurry of all the pore layers is finished to obtain a gradient porous ceramic blank; and demolding, drying, removing glue and sintering the gradient porous ceramic blank to obtain the gradient porous ceramic. The preparation method is suitable for preparing the plate-shaped, arc-shaped and conical gradient porous ceramics, and the prepared gradient porous ceramics have good interface binding property and are not easy to crack or delaminate.
Description
Technical Field
The invention belongs to the technical field of porous ceramic material preparation, and particularly relates to gradient porous ceramic and a preparation method thereof.
Background
Silicon nitride-based ceramic is one of the best materials in structural ceramics, has high mechanical strength, good thermal stability, lower dielectric constant and good wave-transmitting material, is one of ceramic materials which are mainly researched at home and abroad, gradient porous ceramic is ceramic with different porosity of each layer in multilayer ceramic, and the integration of the functions of light weight, support, filtering and wave-transmitting of silicon nitride ceramic can be realized through the structural design of multiple layers with different porosity of each layer, but the key and difficult point of research on how to realize the multilayer structure and high interlayer combination is always.
The patent CN102417366A discloses a gradient porous silicon carbide ceramic and a preparation method thereof, mixed powder containing different pore-forming agents is paved on a metal mold layer by layer, and is sintered after being pressed and formed to obtain the gradient porous silicon carbide ceramic.
The patent CN 111728273A provides a preparation method of a gradient porous material for improving the binding force of interfaces between gradients, which has high requirements on process equipment and thin functional layers, and cannot meet the requirements of actual processing for expanding application.
Patent CN108101544A discloses a lamellar gradient porous silicon carbide ceramic and a preparation method thereof, the invention obtains the gradient porous silicon carbide ceramic by means of freeze drying technology and utilizing different sedimentation rates of large and small particles in slurry; patent CN108083811A also discloses a silicon nitride ceramic with hierarchical pore structure and a preparation method thereof by means of freeze drying technology, which can solve the problem of poor interface bonding between porous material gradients, but is prone to through cracks.
Patent CN106588074A discloses a method for preparing gradient porous silicon nitride ceramics by slip casting combined with vacuum foaming, which comprises adding foaming agent into slurry, injecting into a mold with gypsum at the bottom, vacuumizing, keeping temperature and pressure, and preparing gradient porous silicon nitride ceramics by using pressure drop change and pore distribution in the slurry.
Moreover, the method is only limited to preparing the gradient porous ceramics with the plate-type structure, and is not suitable for preparing the gradient porous ceramics with the arc-shaped and conical structures, and for the dry powder static pressure method, the preparation of the gradient porous ceramics with the arc-shaped and conical structures adopts a secondary static pressure mode, namely, one material is pre-pressed firstly, and then the other material is distributed for secondary pressing, so that the pre-pressed green body is easily crushed, and the interface bonding effect is worse; for the slip casting combined with the vacuum foaming method, when preparing the gradient porous ceramics with arc and cone structures, the normal distribution of the pore diameter distribution direction is difficult to realize, so that the gradient porous ceramics except for the flat plate cannot be prepared at all.
Therefore, a preparation method of gradient porous ceramic with good interface binding property and capable of preparing arc-shaped and conical structures is needed.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention discloses a preparation method of gradient porous ceramic, which comprises the following specific technical scheme:
a preparation method of gradient porous ceramics comprises the following steps:
respectively preparing ceramic slurry of each pore layer in the gradient porous ceramic;
pouring ceramic slurry into a water-absorbing mold in sequence according to the arrangement sequence of pore layers in the gradient porous ceramic, after pouring the ceramic slurry of one pore layer, solidifying the ceramic slurry to a preset thickness by utilizing the water absorption of the water-absorbing mold, pouring out the residual ceramic slurry in the water-absorbing mold, and pouring the ceramic slurry of another pore layer in the same way until the pouring of the ceramic slurry of all the pore layers is finished to obtain a gradient porous ceramic blank;
and demolding, drying, removing glue and sintering the gradient porous ceramic blank to obtain the gradient porous ceramic.
Further, in the above-mentioned case,
respectively mixing and grinding the raw materials of the ceramic slurry of each pore layer, ageing, adding a defoaming agent, and carrying out vacuum stirring and degassing to obtain the ceramic slurry of each pore layer;
the ceramic slurry comprises the following raw materials in percentage by mass: 100% of ceramic powder, 8-10% of sintering aid, 0-30% of pore-forming agent, 0.5-1.5% of dispersing agent, 0.05-0.15% of PH regulator, 0-3% of reinforcing agent, 25-45% of water, 0.5-3% of one or more of methyl cellulose, ethyl cellulose or Arabic gum;
the ceramic slurry of different pore layers has different pore-forming agent contents.
In a further aspect of the present invention,
the ceramic powder is one or more of silicon nitride, aluminum oxide, silicon oxide and silicon carbide.
In a further aspect of the present invention,
the ceramic powder is silicon nitride, the silicon nitride is an alpha crystalline phase, and the phase content is more than or equal to 90%.
In a further aspect of the present invention,
the solid content of the ceramic slurry of any pore layer is in the range of 49vol% to 54 vol%;
or
The ceramic powder comprises a first powder and a second powder, wherein the grain diameter of the first powder is 0.8-1.5 mu m, the grain diameter of the second powder is 8-10 mu m, and the mass ratio of the first powder to the second powder is 3-5.
In a further aspect of the present invention,
the sintering aid is Y 2 O 3 、Yb 2 O 3 、La 2 O 3 、Sm 2 O 3 One or more of the above;
the pore-forming agent is PMMA;
the dispersant is one or more of polymethacrylic acid amine, polyethyleneimine and ammonium citrate;
the pH regulator is ammonia water or tetramethyl ammonium hydroxide aqueous solution.
The reinforcing agent is PVA or PEG water solution with the concentration of 2-5%.
Further, in the above-mentioned case,
the water-absorbing mold is a gypsum mold, and the water content of the gypsum mold is controlled to be 5-7% before use.
Further, in the above-mentioned case,
before pouring ceramic slurry, a layer of boron nitride alcohol suspension is coated on the inner surface of a water-absorbing mould, and after alcohol is volatilized, the ceramic slurry is poured.
The invention also discloses gradient porous ceramic prepared by any one of the preparation methods.
Further, the gradient porous ceramic is plate-shaped, arc-shaped or conical.
By adopting the technical scheme, the invention has the beneficial effects that:
according to the invention, the gradient porous ceramic is prepared by using a water-absorbing mould in a way of layer-by-layer pouring and continuous slurry-absorbing solidification, and the ceramic slurry bonding interface of two pore layers is in a liquid-liquid transition state, so that the bonding property of the formed gradient porous ceramic interface is better, the problem of poor bonding property of the gradient layer interface is effectively solved, and the defect of gradient layer connection caused by a layer-by-layer pressing method is avoided; secondly, because the ceramic blank is primarily cured and molded by utilizing the water absorption of the die, the pore layers of the blank in the die are uniformly attached on the inner wall of the die layer by layer, the thickness of the pore layers is controllable, and the thickness of the layer can meet the requirements of subsequent grinding processing; the gradient porous ceramics with different shapes, such as arc, cone and the like, can be prepared by replacing the moulds with different shapes, and the interface bonding property of the gradient porous ceramics is not influenced by the shape.
Drawings
FIG. 1 is a schematic view of arc mold grouting of example 1;
FIG. 2 is a schematic view of the plate mold grouting of example 2;
FIG. 3 is an arc-shaped gradient porous ceramic prepared in example 1;
FIG. 4 is a plate-like gradient porous ceramic prepared in example 2;
FIG. 5 is an electron microscope scanning image of the interlayer interface of the gradient porous ceramic prepared in example 1;
FIG. 6 is an electron microscope scan of the interlayer interface of the gradient porous ceramic prepared in example 2;
among them, 1-arc gypsum mold, 2-first void layer of example 1, 3-second void layer of example 1, 4-plate gypsum mold, 5-first void layer of example 2, 6-second void layer of example 2, and 7-third void layer of example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention discloses a preparation method of gradient porous ceramic, which comprises the following steps:
the method comprises the following steps: respectively preparing ceramic slurry of each pore layer in the gradient porous ceramic;
step two: pouring ceramic slurry into a water-absorbing mold in sequence according to the arrangement sequence of pore layers in the gradient porous ceramic, solidifying the ceramic slurry to a preset thickness by using the water absorption of the water-absorbing mold after pouring the ceramic slurry of one pore layer, pouring out the residual ceramic slurry in the water-absorbing mold, and pouring the ceramic slurry of another pore layer in the same way until the pouring of the ceramic slurry of all the pore layers is finished to obtain a gradient porous ceramic blank;
step three: and demolding, drying, removing glue and sintering the gradient porous ceramic blank to obtain the gradient porous ceramic.
The invention adopts a water-absorbing mould to pour layer by layer and continuously absorb slurry to solidify, because the ceramic slurry is solidified by the water-absorbing mould, the rest ceramic slurry is poured out, the ceramic slurry solidified on the mould is far away from one side of the mould, and is in a viscous liquid state, when the ceramic slurry of the other pore layer is poured, the combination interface of the ceramic slurry of the two pore layers is in a liquid-liquid transition state, and the two liquid slurries at the combination part can flow and uniformly mix, so that the formed gradient porous ceramic interface has better combination property, is not easy to generate cracks and faults, effectively solves the problem of poor combination property of the gradient layer interface, and avoids the gradient layer connection defect caused by a layer-by-layer pressing method; secondly, because the ceramic blank is primarily cured and molded by utilizing the water absorption of the die, the pore layers of the blank in the die are uniformly attached on the inner wall of the die layer by layer, the thickness of the pore layers is controllable, and the thickness of the layer can meet the requirements of subsequent grinding processing; thirdly, the invention can prepare gradient porous ceramics with different shapes, such as arc shape, cone shape and the like, by replacing moulds with different shapes, and the interface bonding property of the gradient porous ceramics is not influenced by the shape due to the particularity of the preparation method.
Specifically, the ceramic slurry in the first step comprises the following raw materials in percentage by mass:
100 percent of ceramic powder, wherein the ceramic powder can be one or more of silicon nitride, aluminum oxide, silicon oxide and silicon carbide,
8 to 10% of a sintering aid, for example, 8%, 9%, 10%, etc., and the sintering aid may be Y 2 O 3 、Yb 2 O 3 、La 2 O 3 、Sm 2 O 3 One or more of the above;
0-30% of pore-forming agent, wherein the content of the pore-forming agent is mainly selected according to the porosity required to be achieved by each pore layer, and can be, for example, 5%, 10%, 20%, 30%, and the like, the basic difference of the ceramic slurry of each pore layer is that the content of the pore-forming agent in the ceramic slurry is different, and certainly, the pore-forming agent is not added, is PMMA (polymethyl methacrylate) particles, and preferably has a median particle size of 3-5 μm;
0.5-1.5% of dispersant, such as 0.5%, 1.0%, 1.5% and the like, wherein the dispersant is one or more of polymethacrylic acid amine, polyethyleneimine and ammonium citrate;
0.05-0.15% of pH regulator, such as 0.05%, 0.10%, 0.15%, etc., wherein the pH regulator is ammonia water or tetramethylammonium hydroxide aqueous solution, and the pH regulator is used for regulating the pH value of the ceramic slurry to be between 9 and 11;
0 to 3% of a reinforcing agent, for example 1%, 2%, 3% and the like;
0.5 to 3 percent of one or more of methyl cellulose, ethyl cellulose or Arabic gum, and the methyl cellulose, the ethyl cellulose or the Arabic gum is added into the slurry, so that the phenomenon of particle rearrangement of the slurry solidified on a mold when a water-absorbing mold absorbs water can be inhibited, and the density and the components of the same pore layer of the gradient porous ceramic are prevented from changing.
25 to 45% of water, for example, 25%, 30%, 45% and the like.
The specific preparation process of the ceramic slurry of each pore layer comprises the following steps: mixing and grinding raw materials of the ceramic slurry of each pore layer for 1-2 h, preferably ball milling, aging for 10-14 h, such as 10h, 12h and 14h, adding a small amount of defoaming agent, and vacuum stirring and degassing for 0.5-2 h, such as 0.5h, 1h and 2h to obtain the ceramic slurry of each pore layer;
of course, the raw materials and preparation method of the ceramic slurry are not limited, and other types of slurries in the prior art can also be used for preparing the gradient porous ceramic by using the preparation method of the invention.
In the second step, the ceramic slurry is cured to a preset thickness, the cured thickness can be controlled according to the curing time in the actual production, for example, the thickness of about 5mm can be cured in about 20min if a gypsum mold is adopted, and the specific thickness can be adjusted according to the actually adopted mold and the type of the prepared ceramic.
In the third step, the specific method for demolding comprises the following steps: placing the gradient porous ceramic blank and the water-absorbing mold in a constant-temperature constant-humidity environment, drying in the shade for 72-96 h, controlling the room temperature to be 25 +/-1 ℃ and the humidity to be 50-70%, and demolding after drying in the shade; the specific drying method comprises the following steps: continuously drying the demolded gradient porous ceramic blank in the shade to constant weight (the weight is not reduced obviously any more), transferring the blank into an oven for drying, and controlling the temperature to be 30-40 ℃; the specific method for binder removal sintering comprises the following steps: heating to 600-700 deg.C at 1-2 deg.C/min, maintaining at micro-positive pressure for 1-3 h for degreasing, and maintaining at 0.4-0.6 Mpa N 2 Heating to 1600-1700 ℃ at a speed of 1-3 ℃/min in the environment, preserving heat for 1-3 h, and cooling along with the furnace.
In a preferred scheme of the invention, the solid content of the ceramic slurry of any one of the pore layers is in the range of 49-54 vol%, and the ceramic powder, the pore-forming agent and the sintering aid in the ceramic slurry contribute to the solid content, so that the solid content in the ceramic slurry is high, the skeleton particle content is high, the shrinkage rate of the blank is less than 1.5%, and the stress defect caused by size shrinkage in the drying and shrinkage processes of the blank is effectively reduced.
In another preferred embodiment of the present invention, the ceramic powder is preferably silicon nitride powder, and when silicon nitride powder is selected, the silicon nitride powder is preferably alpha crystalline phase with a phase content of 90% or more.
In still another aspect of the present invention, the ceramic powder includes a first powder and a second powder, the first powder has a particle size of 0.8 to 1.5 μm, the second powder has a particle size of 8 to 10 μm, and the mass ratio of the first powder to the second powder is 3 to 5.
The water-absorbing mold is preferably a gypsum mold, the gypsum mold can be formed by pouring gypsum slurry with the mass ratio of gypsum powder to water being 6.
The invention also discloses gradient porous ceramic which can be in a plate-shaped, arc-shaped or conical structure and is prepared by adopting any one of the methods.
The scheme of the invention will be further explained by combining the specific embodiments as follows:
example 1
(1) 1800g of silicon nitride mixed powder (the first powder and the second powder are mixed according to the mass ratio of 3 2 O 3 Powder, 90gYb 2 O 3 Adding the powder into a ball milling tank, weighing 14g of polymethacrylic acid amine, 1.6g of ammonia water, 490g of water and 9g of methyl cellulose in a beaker, uniformly mixing, adding into the ball milling tank, carrying out ball milling for 1h, ageing for 12h, adding 0.2g of defoaming agent, carrying out vacuum stirring and degassing for 1h, and using the mixture as first pore layer slurry, wherein the viscosity of the slurry is 95-100 mPa & s.
(2) 1800g of silicon nitride mixed powder (the first powder and the second powder are mixed according to the mass ratio of 3 2 O 3 Powder, 90gYb 2 O 3 Adding powder and 200g of PMMA pore-forming agent into a ball-milling tank, weighing 16g of ammonium polymethacrylate, 1.6g of ammonia water, 18g of PVA, 619.2g of water and 18g of methylcellulose into a beaker, uniformly mixing, adding into the ball-milling tank, carrying out ball milling for 1h, ageing for 12h, adding 0.4g of defoaming agent, carrying out vacuum stirring and degassing for 1h, using as second pore layer slurry, and enabling the slurry to have the viscosity of 105-120 mPa & s.
(3) Coating a layer of boron nitride alcohol suspension on the surface of a gypsum mould with an arc-shaped inner cavity, after alcohol is volatilized, pouring the first pore layer slurry into the mould, absorbing slurry and solidifying for 20min, wherein the thickness of a blank is about 5mm, pouring out the residual slurry, pouring out the second pore layer slurry, absorbing slurry and solidifying for 35min, accumulating and solidifying the thickness of the blank by 10-11 mm, pouring out the residual slurry to obtain a double-layer gradient pore silicon nitride blank, coating the contact surface of the blank slurry with a preservative film to prevent rapid water loss, placing the blank and the mould in a drying chamber for drying, controlling the room temperature to be 25 +/-1 ℃, the humidity to be 50%, drying for 72h, demoulding, continuously drying the demoulded blank in an indoor environment until the quality is not obviously reduced any more, transferring the blank to an oven, and controlling the temperature to be 30 ℃ until the blank is completely dried;
(4) Placing the dried blank body into an air pressure furnace for degreasing and sintering integrated treatment, heating to 650 ℃ at the speed of 1.5 ℃, carrying out micro-positive pressure heat preservation for 2 hours for degreasing, and then carrying out N treatment at the pressure of 0.5Mpa 2 Heating to 1650 ℃ at a speed of 2 ℃/min in the environment, preserving heat for 2h, and cooling along with the furnace to obtain the silicon nitride ceramic with double gradient pores.
Fig. 1 is a schematic view of arc-shaped mold grouting of example 1, fig. 3 is a schematic view of a silicon nitride ceramic with dual gradient pores prepared in example 1, and fig. 5 is a scanning electron microscope image of an interlayer interface of the silicon nitride ceramic with dual gradient pores prepared in example 1, and it can be seen from fig. 5 that interface bonding between different pore layers is good.
Example 2
(1) 1800g of silicon nitride mixed powder (the first powder and the second powder are mixed according to the mass ratio of 5 2 O 3 Powder, 90gYb 2 O 3 Adding the powder into a ball milling tank, weighing 14g of ammonium citrate, 1.6g of tetramethylammonium hydroxide aqueous solution, 490g of water and 9g of Arabic gum in a beaker, uniformly mixing, adding into the ball milling tank, rapidly ball milling for 1h, ageing for 12h, adding 0.2g of defoaming agent, vacuum stirring and degassing for 1h, and using as first pore layer slurry with the viscosity of 90-95 mPa & s.
(2) 1800g of silicon nitride mixed powder (the first powder and the second powder are mixed according to the mass ratio of 5 2 O 3 Powder, 90gYb 2 O 3 Powder (18 g)PVE and 200g of PMMA pore-forming agent are added into a ball milling tank, 16g of ammonium citrate, 1.6g of tetramethylammonium hydroxide aqueous solution, 619.2g of water and 18g of Arabic gum are weighed and mixed uniformly in a beaker, then the mixture is added into the ball milling tank, the mixture is rapidly ball milled for 1 hour, aged for 12 hours, 0.4g of antifoaming agent is added, the mixture is vacuum stirred and degassed for 1 hour and is used as second pore layer slurry, and the viscosity of the slurry is 105-110 mPa & s.
(3) 1800g of silicon nitride mixed powder (the first powder and the second powder are mixed according to the mass ratio of 5 2 O 3 Powder, 90gYb 2 O 3 Adding powder and 400g of PMMA pore-forming agent into a ball milling tank, weighing 20g of ammonium citrate, 1.6g of tetramethylammonium hydroxide aqueous solution, 35g of PVE, 788g of water and 36g of Arabic gum into a beaker, uniformly mixing, adding into the ball milling tank, rapidly ball milling for 1h, ageing for 12h, adding 0.4g of defoaming agent, vacuum-stirring and degassing for 1h, using as third pore layer slurry, and enabling the slurry to have the viscosity of 120-135 mPa & s.
(4) Coating a layer of boron nitride alcohol suspension on the surface of a gypsum mold with a flat inner cavity, after alcohol volatilizes, pouring the first pore layer slurry into the mold, absorbing slurry and curing for 20min, wherein the thickness of a blank is about 5mm, pouring out the residual slurry, pouring out the second pore layer slurry, absorbing slurry and curing for 35min, the accumulated curing thickness of the blank is 10-11 mm, pouring out the residual slurry, pouring out the third pore layer slurry, absorbing slurry and curing for 60min, the accumulated curing thickness of the blank is 14-15 mm, pouring out the residual slurry to obtain a three-layer gradient pore silicon nitride ceramic blank, coating the contact surface of the blank slurry with a preservative film to prevent rapid water loss, placing the blank and the mold in a drying chamber for drying, controlling the room temperature to be 25 +/-1 ℃, the humidity to be 70%, drying for 72h, demolding, continuously drying the demolded blank in an indoor environment until the quality is not obviously reduced, transferring the blank to an oven, and controlling the temperature to be 40 ℃ to be completely dried;
(5) Putting the dried green body into an air pressure furnace for degreasing and sintering, and performing integration by 1
Heating to 600 deg.C, maintaining at micro-positive pressure for 1 hr for degreasing, and maintaining at 0.4Mpa N 2 Heating to 1600 ℃ at a speed of 1 ℃/min in the environment, preserving heat for 1h, and cooling along with the furnace to obtain the nitrogen with three-layer gradient poresA silicon oxide ceramic.
Fig. 2 is a schematic diagram of plate mold grouting in example 2, fig. 4 is a schematic diagram of silicon nitride ceramic with three layers of gradient pores prepared in example 2, and fig. 6 is an electron microscope scanning image of an interlayer interface (a bonding surface between two layers) of silicon nitride ceramic with three layers of gradient pores prepared in example 2, and it can be seen from fig. 6 that the interface bonding property between different pore layers is good.
Example 3
(1) 1800g of a silicon carbide mixed powder (first powder and second powder mixed in a mass ratio of 4 2 O 3 Powder 64g Sm 2 O 3 Adding the powder into a ball milling tank, weighing 9g of polyethyleneimine, 0.9g of tetramethylammonium hydroxide aqueous solution, 450g of water and 18g of methylcellulose into a beaker, uniformly mixing, adding into the ball milling tank, quickly milling for 1 hour, aging for 10 hours, adding 0.18g of defoaming agent, vacuum stirring and degassing for 0.5 hour, and using as first pore layer slurry with the viscosity of 90-95 mPa & s.
(2) 1800g of a silicon carbide mixed powder (first powder and second powder mixed at a mass ratio of 4 2 O 3 Powder 80g Sm 2 O 3 Adding 180g of PMMA pore-forming agent into a ball-milling tank, weighing 18g of polyethyleneimine, 1.8g of tetramethylammonium hydroxide aqueous solution, 18g of PVA, 540g of water and 36g of ethyl cellulose, uniformly mixing in a beaker, adding into the ball-milling tank, rapidly ball-milling for 1h, ageing for 12h, adding 0.36g of defoaming agent, vacuum-stirring and degassing for 1h, using as second pore layer slurry, wherein the viscosity of the slurry is 105-110 mPas.
(3) 1800g of silicon carbide mixed powder (the first powder and the second powder are mixed according to a mass ratio of 4 2 O 3 Powder, 90g Sm 2 O 3 And 540g of PMMA pore former is added into a ball milling tank, 27g of polyethyleneimine, 2.7g of tetramethylammonium hydroxide aqueous solution, 40g of PVA, 810g of water and 54g of ethyl cellulose are weighed and uniformly mixed in a beaker, then the mixture is added into the ball milling tank, the mixture is rapidly ball milled for 2 hours and aged for 14 hours, 0.54g of defoaming agent is added, the mixture is vacuum stirred and degassed for 2 hours and is used as third pore layer slurry, and the viscosity of the slurry is 120-135 mPa & s.
(4) Coating a layer of boron nitride alcohol suspension on the surface of a gypsum mold with a conical inner cavity, after alcohol is volatilized, pouring the first pore layer slurry into the mold, absorbing slurry and curing for 20min, pouring out the residual slurry when the thickness of a blank is about 5mm, pouring out the second pore layer slurry, absorbing slurry and curing for 35min, accumulating and curing the blank for 10-11 mm, pouring out the residual slurry, pouring out the third pore layer slurry, absorbing slurry and curing for 60min, accumulating and curing the blank for 14-15 mm, and pouring out the residual slurry to obtain a three-layer gradient pore silicon nitride ceramic blank, coating the contact surface of the slurry of the blank with a preservative film to prevent rapid dehydration, placing the blank and the mold in a drying chamber for drying, controlling the room temperature to be 25 +/-1 ℃, the humidity to be 60%, drying for 96h, demolding, continuously drying the demolded blank in the indoor environment until the quality is not obviously reduced any more, transferring the blank to an oven, and controlling the temperature to be 40 ℃ to be dried completely;
(5) Putting the dried blank into an air pressure furnace for degreasing and sintering, degreasing at the temperature of 2 ℃/700 ℃, preserving the heat for 3h under micro-positive pressure, and then degreasing under the pressure of 0.6Mpa N 2 Heating to 1700 ℃ at the speed of 3 ℃/min in the environment, preserving heat for 3h, and cooling along with the furnace to obtain the conical silicon carbide ceramic with three-layer gradient pores.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art may still modify the technical solutions described in the foregoing embodiments, or may equally substitute some or all of the technical features; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (10)
1. A preparation method of gradient porous ceramics is characterized in that: the method comprises the following steps:
respectively preparing ceramic slurry of each pore layer in the gradient porous ceramic;
pouring ceramic slurry into a water-absorbing mold in sequence according to the arrangement sequence of pore layers in the gradient porous ceramic, solidifying the ceramic slurry to a preset thickness by using the water absorption of the water-absorbing mold after pouring the ceramic slurry of one pore layer, pouring out the residual ceramic slurry in the water-absorbing mold, and pouring the ceramic slurry of another pore layer in the same way until the pouring of the ceramic slurry of all the pore layers is finished to obtain a gradient porous ceramic blank;
and demolding, drying, removing glue and sintering the gradient porous ceramic blank to obtain the gradient porous ceramic.
2. The method of claim 1, wherein:
respectively mixing and grinding the raw materials of the ceramic slurry of each pore layer, ageing, adding a defoaming agent, and carrying out vacuum stirring and degassing to obtain the ceramic slurry of each pore layer;
the ceramic slurry comprises the following raw materials in percentage by mass: 100% of ceramic powder, 8-10% of sintering aid, 0-30% of pore-forming agent, 0.5-1.5% of dispersing agent, 0.05-0.15% of PH regulator, 0-3% of reinforcing agent, 25-45% of water, 0.5-3% of one or more of methyl cellulose, ethyl cellulose or Arabic gum;
the ceramic slurry of different pore layers has different pore-forming agent contents.
3. The method of claim 2, wherein: the ceramic powder is one or more of silicon nitride, aluminum oxide, silicon oxide and silicon carbide.
4. The method of claim 2, wherein: the ceramic powder is silicon nitride, the silicon nitride is alpha crystalline phase, and the phase content is more than or equal to 90%.
5. The method of claim 2, wherein: the solid content of the ceramic slurry of any pore layer is in the range of 49vol% to 54 vol%;
or alternatively
The ceramic powder comprises a first powder and a second powder, wherein the grain diameter of the first powder is 0.8-1.5 mu m, the grain diameter of the second powder is 8-10 mu m, and the mass ratio of the first powder to the second powder is 3-5.
6. The production method according to claim 2, characterized in that:
the sintering aid is Y 2 O 3 、Yb 2 O 3 、La 2 O 3 、Sm 2 O 3 One or more of the above;
the pore-forming agent is PMMA;
the dispersant is one or more of polymethacrylic acid amine, polyethyleneimine and ammonium citrate;
the pH regulator is ammonia water or tetramethyl ammonium hydroxide aqueous solution;
the reinforcing agent is PVA or PEG water solution with the concentration of 2-5%.
7. The method of claim 1, wherein: the water-absorbing mold is a gypsum mold, and the water content of the gypsum mold is controlled to be 5-7% before use.
8. The production method according to claim 1, characterized in that: before pouring ceramic slurry, a layer of boron nitride alcohol suspension is coated on the inner surface of a water-absorbing mould, and after alcohol is volatilized, the ceramic slurry is poured.
9. A gradient porous ceramic, characterized by: the preparation method of the compound is as described in any one of claims 1 to 8.
10. The gradient porous ceramic of claim 9, wherein: the gradient porous ceramic is plate-shaped, arc-shaped or conical.
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