CN104311114A - Method of preparing gradient porous silicon nitride ceramic material - Google Patents
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Abstract
The invention relates to a method of preparing a gradient porous silicon nitride ceramic material. The method comprises the following steps: 1) mixing and ball-milling silicon nitride powder, a sintering aid, a binder and water to obtain water-based slurry; 2) foaming the water-based slurry under a vacuum degree of 50-90kPa and freezing, and then performing freeze-drying to obtain a gradient porous silicon nitride ceramic biscuit; and 3) removing the binder from the gradient porous silicon nitride ceramic biscuit and sintering to obtain the gradient porous silicon nitride ceramic material.
Description
Technical field
The present invention relates to a kind of preparation method of gradient porous silicon nitride ceramic material, belong to porous ceramic film material preparing technical field.
Background technology
Porous silicon-nitride ceramic material owing to having lightweight, the feature such as high temperature resistant, corrosion-resistant, and also exists β-Si in porous silicon nitride system
3n
4the mechanism and enhancement mechanism that elongated grain is cross-linked with each other, has more excellent mechanical property and thermal shock resistance than other porous ceramics, therefore has wide practical use in fields such as high temperature air filtration, sensor, support of the catalyst, separatory membranes.For meeting the demand of different field, there is a lot of reports about porous silicon nitride ceramic preparation method, but relatively less for the report of gradient porous ceramics.Chinese patent CN101182233A discloses a kind of casting method and has opening directional hole structure and high porosity and the aperture porous ceramic film in film thickness direction graded in conjunction with lyophilize preparation.Chen reports a kind of hot-spraying techniques and prepares compact silicon nitride acquisition gradient-structure (Fei Chen, Journal of the Ceramic Society of Japan 117 [4] 445-4482009) at nitride porous silicon face.Chinese patent CN101698605A discloses a kind of using down alkene as solvent, and realize down alkene forms the dendroid of changing from small to big at certain orientation by controlling freezing thermograde, after lyophilize, acquisition has the vesicular structure of gradient.Chinese patent CN103145438A discloses a kind of slurry of repeatedly freezing different components, obtains porosity and reduces from inside to outside, has biomimetic features gradient porous material close outside interior dredging.
In view of the practicality of gradient porous silicon nitride ceramic material, how to prepare one of this material research direction remaining these those skilled in the art easily.
Summary of the invention
The present invention is intended to the preparation method expanding gradient porous silicon nitride ceramic material further, the invention provides a kind of method preparing gradient porous silicon nitride ceramic material easily.
The invention provides a kind of method preparing gradient porous silicon nitride ceramic material, described method comprises:
1) by beta-silicon nitride powder, sintering aid, binding agent and water mixing and ball milling, water-based slurry is obtained;
2) by step 1) water-based slurry prepared foams and carries out freezing freezing simultaneously, then carrying out lyophilize, thus obtain gradient porous silicon nitride ceramics biscuit under the vacuum tightness of 50 ~ 90kPa;
3) by step 2) the gradient porous silicon nitride ceramics biscuit prepared takes off binding agent, sintering obtains gradient porous silicon nitride ceramic material.
Preferably, step 1) in, sintering aid is Y
2o
3, Al
2o
3, Yb
2o
3, Lu
2o
3, Sm
2o
3, SiO
2, Nd
2o
3, Eu
2o
3in at least one.
Preferably, step 1) in, silicon nitride, sintering aid, ratio between binding agent and water are (10 ~ 250): (0.2 ~ 25): (0.05 ~ 10): 100.
Preferably, step 1) in, described binding agent is water-soluble binder, comprises polyvinyl alcohol, polyoxyethylene glycol, water-soluble isobutylene-based polymer comprise isobutylene maleic acid anhydride polymkeric substance.
Preferably, step 2) in, the described freezing temperature freezed is-70 ~-10 DEG C, and the time is 1 ~ 48 hour.
Preferably, step 2) in, described cryodesiccated vacuum tightness is 1 ~ 100Pa, and drying temperature is 0 ~ 80 DEG C, and time of drying is 24 ~ 48 hours.
Preferably, step 3) in, de-binding agent is under air conditions, is warming up to 400 ~ 800 DEG C with the temperature rise rate of 0.2 ~ 2 DEG C/min, is incubated 0.5 ~ 5 hour.
Preferably, step 3) in, sintering is under a nitrogen atmosphere, rises to 1500 ~ 1950 DEG C with 1 ~ 10 DEG C/min, is incubated 1 ~ 12 hour, and the pressure of nitrogen is 0.1-5MPa.
Preferably, by regulating step 2) in described vacuum tightness control the void content of the gradient porous silicon nitride ceramic material of gained.Vacuum tightness is less, and void content is larger.
Preferably, the void content of the gradient porous silicon nitride ceramic material of gained is 72 ~ 95%, and pore size distribution is 0.1 ~ 300 μm, is preferably 0.3 ~ 200 μm.
Beneficial effect of the present invention:
The object of the invention is by vacuum foam in conjunction with freeze-drying, technique is simple, and method with low cost prepares gradient porous silicon nitride ceramics.Void content can reach 80 ~ 95%, and pore size distribution is 0.1-300 μm.Void content can be regulated by the size of vacuum tightness.
Accompanying drawing explanation
Fig. 1 shows the XRD figure of silicon nitride base substrate (a) and the porous silicon nitride ceramic (b) prepared in an embodiment of the invention;
Fig. 2 shows the profile scanning electron microscopic picture of the porous silicon nitride ceramic prepared in an embodiment of the invention;
Fig. 3 shows in an embodiment of the invention the pore size distribution preparing gradient porous silicon nitride ceramics;
Fig. 4 shows in an embodiment of the invention the photo in kind preparing gradient porous silicon nitride ceramics.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
The invention provides a kind of technique simple, method with low cost prepares gradient porous silicon nitride ceramics.Void content is 72 ~ 95%, and be preferably 80 ~ 95%, pore size distribution is 0.1-300 μm, is preferably 0.3-200 μm.
The invention discloses a kind of preparation method of gradient porous silicon nitride ceramic material, as an example, comprise the steps:
Water and water-soluble poval are uniformly mixed the formation aqueous solution by A;
B adds stablizer, sintering aid and beta-silicon nitride powder in the aqueous solution, obtains water-based slurry after ball milling;
Slurry to be poured in mould and is put into homemade freeze drier by C, and 50 ~ 90kPa realizes gradient foaming, and then by freezing for the platform of sample, and then lyophilize obtains ceramic body;
Ceramic body is carried out sintering and obtains gradient porous silicon nitride ceramics by D.
In steps A and B, the ratio of silicon nitride, sintering aid, polyvinyl alcohol and water is recommended as (10 ~ 250) successively: (0.2 ~ 25): (0.05 ~ 10): 100.
Sintering aid described in step B is Y
2o
3, Al
2o
3, Yb
2o
3, Lu
2o
3, Sm
2o
3, SiO
2, Nd
2o
3, Eu
2o
3in any one or two or more with arbitrary proportion composition mixture.
Mould described in step C comprises rubber mold, glass mold or metal die, and the vacuum tightness of foaming is 50 ~ 90kPa, and freezing temp is-70 ~-10 DEG C, is preferably-70 ~-20 DEG C; Cryodesiccated vacuum tightness is 1 ~ 100Pa, and drying temperature is 0 ~ 80 DEG C.
De-binding agent described in step D is under air conditions, temperature rise rate be 0.2 ~ 2 DEG C/min to 600 DEG C, insulation 0.5 ~ 5h.
Sintering described in step D is under a nitrogen atmosphere, rises to 1500 ~ 1950 DEG C with 1 ~ 10 DEG C/min, is incubated 1 ~ 12 hour, and the pressure of nitrogen is 0.1-5MPa.
Compared to the prior art comparatively, the present invention has following beneficial effect:
(1) technique is simple, and gradient pore is even, and without gradient interface;
(2) void content can be regulated by the size of vacuum tightness.
Below some exemplary embodiments are listed further better the present invention to be described.Should understand; the above-mentioned embodiment that the present invention describes in detail; and following examples are only not used in for illustration of the present invention and limit the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.In addition, concrete proportioning, time, temperature etc. in following processing parameter are also only exemplary, and those skilled in the art can select suitable value in the scope of above-mentioned restriction.
Embodiment 1
(1) water of 19g and the water-soluble poval of 1g are uniformly mixed the formation aqueous solution;
(2) transfer in ball grinder by the above-mentioned aqueous solution, then add the silicon nitride ball of 40g, 0.8g sintering aid yttrium oxide and 20g beta-silicon nitride powder to ball grinder, drum's speed of rotation is 200rpm/h, and ball milling obtained water-based slurry after 3 hours;
(3) pour slurry into rubber mold, put into self-control freeze drier, control vacuum tightness is 80kPa, opens freezingly to freeze sample simultaneously, and freezing temp is-10 DEG C, keeps 24 hours, makes sample fully charge.Then lyophilize 24 hours under the environment of 0-80 DEG C and 5-100Pa, makes the ice crystal in freezing base substrate distil, thus formation porous body;
(4) ceramic body is risen to 600 DEG C with 2 DEG C/min in retort furnace, insulation 2h takes off binding agent.Then in atmosphere furnace, 0.1MPa nitrogen pressure 1680 DEG C is incubated 2 hours, and furnace cooling after sintering, obtains porous silicon nitride ceramic; The porosity of the gradient silicon nitride ceramic material that this example obtains is 76%;
Fig. 1 illustrates the XRD figure of silicon nitride base substrate (a) that the present embodiment system prepares and porous silicon nitride ceramic (b), and as can be seen from Figure 1, after high temperature sintering, silicon nitride is β phase by α phase in version.
Embodiment 2
(1) water of 19.4g and the water-soluble poval of 0.6g are uniformly mixed the formation aqueous solution;
(2) transfer in ball grinder by the above-mentioned aqueous solution, then add the silicon nitride ball of 40g, 0.8g sintering aid yttrium oxide and 20g beta-silicon nitride powder to ball grinder, drum's speed of rotation is 200rpm/h, and ball milling obtained water-based slurry after 3 hours;
(3) pour slurry into aluminum die, put into self-control freeze drier, control vacuum tightness is 90kPa, opens freezingly to freeze sample simultaneously, and freezing temp is-10 DEG C, keeps 24 hours, makes sample fully charge.Then lyophilize 24 hours under the environment of 0-80 DEG C and 5-100Pa, makes the ice crystal in freezing base substrate distil, thus formation porous body;
(4) ceramic body is risen to 600 DEG C with 2 DEG C/min in retort furnace, insulation 2h takes off binding agent.Then in atmosphere furnace, 0.3MPa nitrogen pressure 1750 DEG C is incubated 2 hours, and furnace cooling after sintering, obtains porous silicon nitride ceramic.The porosity of the gradient silicon nitride ceramic material that this example obtains is 72%;
Fig. 2 illustrates the profile scanning electron microscopic picture of the porous silicon nitride ceramic that the present embodiment obtains, and as can be seen from Figure 2, sample presents gradient porous structure, and wherein macropore is obtained by foaming, and aperture forms gap by the staggered growth of beta phase silicon nitride.
Embodiment 3
(1) water of 18g and the water-soluble poval of 2g are uniformly mixed the formation aqueous solution;
(2) transfer in ball grinder by the above-mentioned aqueous solution, then add the silicon nitride ball of 40g, 0.8g sintering aid yttrium oxide and 20g beta-silicon nitride powder to ball grinder, drum's speed of rotation is 200rpm/h, and ball milling obtained water-based slurry after 3 hours;
(3) pour slurry into aluminum die, put into self-control freeze drier, control vacuum tightness is 60kPa, opens freezingly to freeze sample simultaneously, and freezing temp is-10 DEG C, keeps 24 hours, makes sample fully charge.Then lyophilize 24 hours under the environment of 0-80 DEG C and 5-100Pa, makes the ice crystal in freezing base substrate distil, thus formation porous body;
(4) ceramic body is risen to 600 DEG C with 2 DEG C/min in retort furnace, insulation 2h takes off binding agent.Then in atmosphere furnace, 1MPa nitrogen pressure 1900 DEG C is incubated 2 hours, and furnace cooling after sintering, obtains porous silicon nitride ceramic.The porosity of the gradient silicon nitride ceramic material that this example obtains is 85%;
Fig. 3,4 illustrates the pore size distribution of the porous silicon nitride ceramic that the present embodiment obtains and photo in kind respectively, as can be seen from Fig. 3 and Fig. 4, pore size distribution presents three peak distributions, and macropore size is 60 ~ 300 μm, mesopore is 20 ~ 60 μm, and aperture is 0.3 ~ 1.1 μm.Sample presents obvious uniform gradient structure.
Embodiment 4
(1) water of 18.4g and the water-soluble poval of 1.6g are uniformly mixed the formation aqueous solution;
(2) transfer in ball grinder by the above-mentioned aqueous solution, then add the silicon nitride ball of 40g, 0.7g sintering aid yttrium oxide and 18g beta-silicon nitride powder to ball grinder, drum's speed of rotation is 200rpm/h, and ball milling obtained water-based slurry after 3 hours;
(3) pour slurry into glass mold, put into self-control freeze drier, control vacuum tightness is 50kPa, opens freezingly to freeze sample simultaneously, and freezing temp is-10 DEG C, keeps 24 hours, makes sample fully charge.Then lyophilize 24 hours under the environment of 0-80 DEG C and 5-100Pa, makes the ice crystal in freezing base substrate distil, thus formation porous body;
(4) ceramic body is risen to 600 DEG C with 2 DEG C/min in retort furnace, insulation 2h takes off binding agent.Then in atmosphere furnace, 0.5MPa nitrogen pressure 1800 DEG C is incubated 2 hours, and furnace cooling after sintering, obtains porous silicon nitride ceramic.The porosity of the gradient silicon nitride ceramic material that this example obtains is 90%.
Claims (10)
1. prepare a method for gradient porous silicon nitride ceramic material, it is characterized in that, described method comprises:
1) by beta-silicon nitride powder, sintering aid, binding agent and water mixing and ball milling, water-based slurry is obtained;
2) water-based slurry step 1) prepared foams and carries out freezing freezing simultaneously under the vacuum tightness of 50-90kPa, then carries out lyophilize, thus obtains gradient porous silicon nitride ceramics biscuit;
3) by step 2) the gradient porous silicon nitride ceramics biscuit prepared takes off binding agent, sintering obtains gradient porous silicon nitride ceramic material.
2. method according to claim 1, is characterized in that, in step 1), sintering aid is Y
2o
3, Al
2o
3, Yb
2o
3, Lu
2o
3, Sm
2o
3, SiO
2, Nd
2o
3, Eu
2o
3in at least one.
3. method according to claim 1 and 2, is characterized in that, in step 1), silicon nitride, sintering aid, ratio between binding agent and water are (10 ~ 250): (0.2 ~ 25): (0.05 ~ 10): 100.
4., according to described method arbitrary in claim 1-3, it is characterized in that, in step 1), described binding agent is water-soluble binder, comprises polyvinyl alcohol, polyoxyethylene glycol, water-soluble isobutylene-based polymer.
5., according to described method arbitrary in claim 1-4, it is characterized in that, step 2) in, the described freezing temperature freezed is-70 ~-10 DEG C, and the time is 1 ~ 48 hour.
6., according to described method arbitrary in claim 1-5, it is characterized in that, step 2) in, described cryodesiccated vacuum tightness is 1-100Pa, and drying temperature is 0-80 DEG C, and time of drying is 24-48 hour.
7. according to described method arbitrary in claim 1-6, it is characterized in that, in step 3), de-binding agent is under air conditions, is warming up to 400-800 DEG C with the temperature rise rate of 0.2-2 DEG C/min, insulation 0.5-5 hour.
8., according to described method arbitrary in claim 1-7, it is characterized in that, in step 3), sintering is under a nitrogen atmosphere, rises to 1500 ~ 1950 DEG C with 1 ~ 10 DEG C/min, is incubated 1 ~ 12 hour, and the pressure of nitrogen is 0.1-5 MPa.
9., according to described method arbitrary in claim 1-8, it is characterized in that, by regulating step 2) in described vacuum tightness control the void content of the gradient porous silicon nitride ceramic material of gained.
10., according to described method arbitrary in claim 1-9, it is characterized in that, the void content of the gradient porous silicon nitride ceramic material of gained is 72 ~ 95%, and pore size distribution is 0.1 ~ 300 μm.
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| CN107935622A (en) * | 2017-12-07 | 2018-04-20 | 中国科学院上海硅酸盐研究所 | The gradient porous capillary wick of a kind of loop circuit heat pipe silicon nitride and its with reference to coating production |
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