CN110903103A - Light high-strength SiC porous material and preparation method thereof - Google Patents
Light high-strength SiC porous material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a light high-strength SiC porous material and a preparation method thereof, wherein the preparation method comprises the following steps: extruding hydrogel slurry containing the SiC one-dimensional nano material in a 3D printing mode, and superposing and forming layer by layer to obtain a blank; and degreasing and removing the glue of the obtained blank, placing the blank in a protective atmosphere, and sintering the blank at 1750-2100 ℃ for 1-3 hours to obtain the light high-strength SiC porous material.
Description
Technical Field
The invention relates to a light high-strength SiC porous material composed of directionally arranged SiC nanowires/whiskers and a preparation method thereof, belonging to the field of preparation of porous ceramic materials.
Background
The porous silicon carbide ceramic has excellent high-temperature strength, high thermal shock resistance, high chemical stability and oxidation resistance, and is widely applied to the aspects of heat insulation materials, catalytic carriers, liquid metal or gas filtration. At present, the traditional methods for preparing porous ceramics mainly comprise a pore-forming agent adding method, an injection molding method, a template method, a freeze drying method, a foaming method and the like. For example, chinese publication No. CN101323524A reports a method for preparing directional porous silicon carbide; the chinese application No. 201511032054.7 discloses a method for preparing porous silicon carbide by injection molding; document 1(materials letters 68(2012) 75-77) prepares porous silicon nitride ceramics by freeze drying.
The silicon carbide nano-wire/whisker has excellent mechanical property and is widely used for reinforcing and toughening ceramics, metals, resins and the like. Compared with the porous silicon carbide ceramic sintered by conventional SiC particles, the porous ceramic composed of SiC nanowires/whiskers or reinforced by SiC nanowires/whiskers has more excellent mechanical properties. As reported in document 2(adv. funct. mater.2016,26, 1636-1645), a porous body of SiC whisker is prepared by a freeze-drying method, and then sintered to prepare the SiC whisker porous ceramic, which has the characteristics of light weight and high strength. However, at present, the orientation of the SiC nanowire/whisker composition/reinforced porous SiC ceramic nanowire/whisker is random, so that the nanowire/whisker has limited contribution to the strength of the porous ceramic.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a light-weight and high-strength SiC porous material sintered from directionally arranged SiC nanowires/whiskers and a preparation method thereof.
A preparation method of a light high-strength SiC porous material is characterized by comprising the following steps:
extruding hydrogel slurry containing the SiC one-dimensional nano material in a 3D printing mode, and superposing and forming layer by layer to obtain a blank; and degreasing and removing the glue of the obtained blank, placing the blank in a protective atmosphere, and sintering the blank at 1750-2100 ℃ for 1-3 hours to obtain the light high-strength SiC porous material.
Preferably, the SiC one-dimensional nano material has a diameter of 5-1000 nm and an aspect ratio of more than 10, and is preferably at least one of a nanowire and a whisker.
Preferably, after extrusion, the Si one-dimensional nanomaterial is arranged in an oriented manner, and the degree of orientation is greater than 85%.
Preferably, the 3D printing mode is a direct ink writing/printing (DIW/DIP), Fused Deposition Modeling (FDM), or Robocasting mode.
Preferably, the diameter of the needle used in the 3D printing mode is larger than the length of the SiC one-dimensional nano material, preferably 50-2000 μm, and more preferably 100-500 μm; the pressure of 3D printing is 0.1-0.8 MPa. To achieve high degree of orientation and to prevent needle clogging, the diameter (inner diameter) of the needle needs to be larger than the length of the SiC one-dimensional nanomaterial (e.g., SiC nanowires/whiskers).
Preferably, the volume content of the SiC one-dimensional nanomaterial in the hydrogel slurry is 1 to 30 vol%. Firstly, the high volume fraction nanowire content can be ensured, and in addition, the high orientation degree can be ensured.
Preferably, the hydrogel slurry further comprises a sintering aid, and the sintering aid is Al2O3、Y2O3At least one of MgO; preferably, the addition amount of the sintering aid is 1-20 wt% of the SiC one-dimensional nano material.
Preferably, the hydrogel slurry also comprises a binder and an antifoaming agent, wherein the binder is at least one of polyethylene glycol, gelatin, chitosan, pluronic acid and methyl cellulose, and the antifoaming agent is at least one of 1-octanol and isopropanol; preferably, the addition amount of the bonding agent is 5-30 wt% of the mass of water, and the addition amount of the defoaming agent is 0.2-3% of the mass of water.
Preferably, the temperature of degreasing and degumming is 500-1000 ℃ and the time is 0.5-3 hours.
Preferably, the parameters of the 3D printing mode include: the printing distance is more than or equal to 0 mu m, the interlayer distance is 70-100% of the diameter (inner diameter) of the printing needle head, and the printing speed is 5-30 mm/s.
Preferably, the protective atmosphere is at least one of argon, nitrogen and helium.
On the other hand, the invention also provides a light high-strength SiC porous material prepared by the preparation method. In the invention, the light high-strength SiC porous material is porous ceramic formed by SiC nanowires/whiskers which are arranged in an oriented mode, and the one-dimensional orientation degree of the SiC nanowires/whiskers is more than 85%.
Preferably, the porosity of the SiC porous material is 40-95%, and the compressive strength is 3-245 MPa.
In the invention, the light and high-strength SiC porous material sintered by the directionally arranged SiC nanowires/whiskers has low density and high strength, and is obviously superior to other types of SiC porous materials.
Drawings
FIG. 1 is an SEM photograph of an oriented SiC nanowire porous ceramic in accordance with the present invention;
FIG. 2 is a comparison of the performance of the oriented SiC nanowire porous ceramics of the present invention with porous SiC materials.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the present disclosure, the SiC porous material is sintered from SiC one-dimensional nanomaterials (silicon carbide nanowires/whiskers) arranged in an oriented manner. Specifically, based on a 3D printing mode (FDM/DIW or Robocasting) of slurry extrusion, SiC nanowire/whisker slurry is arranged in a one-dimensional orientation mode along an extrusion direction under the action of shear stress, a specific structure is constructed in a layer-by-layer printing mode under program control, and the SiC nanowire/whisker slurry is sintered at 1750-2100 ℃ after glue removal. In the invention, the SiC porous material has the characteristics of light weight and high strength. The following exemplarily illustrates a method for preparing a light weight, high strength SiC porous material.
Uniformly dispersing the SiC one-dimensional nano material (SiC nanowire/whisker) and the sintering aid, and adding a bonding agent, a defoaming agent and the like to prepare the hydrogel slurry with the shear thinning characteristic. In an alternative embodiment, the SiC one-dimensional nano material has a diameter of 5-1000 nm and an aspect ratio of > 10, and is preferably in the shape of at least one of a nanowire and a whisker. Wherein the diameter of the SiC nanowire is 100-1000 nm, the length-diameter ratio is more than 10, and the diameter of the SiC whisker is 100-1000 nm, and the length-diameter ratio is more than 50. The binder can be polyethylene glycol, gelatin, chitosan, pluronic acid, methylcellulose, etc. The defoamer can be a conventional hydrogel binder/defoamer system such as 1-octanol, isopropanol, and the like. The binder may be added to the hydrogel slurry in an amount of 5 to 30wt% based on the mass of water (e.g., deionized water). The amount of the defoaming agent added may be 0.2 to 3 wt% based on the mass of water (e.g., deionized water). The sintering aid can be Al2O3、Y2O3And MgO, and the like. The addition amount of the sintering aid can be 1-20 wt% of the mass of the SiC one-dimensional nano material. The volume content of the SiC one-dimensional nano material in the hydrogel slurry can be 1-30 vol%. Preferably, after extrusion molding, the Si one-dimensional nano material is arranged in an oriented manner, and the orientation degree is more than 85%.
As an example of preparing a hydrogel slurry, there is included: firstly, dispersing SiC nanowires/whiskers in deionized water by using ultrasonic waves, wherein the volume fraction of the SiC nanowires/whiskers is 1-30%; secondly, sequentially adding a sintering aid into the uniformly dispersed suspension of the SiC nanowires/whiskers, and further performing ultrasonic dispersion, wherein the content of the sintering aid is 1-20 wt% of the mass of the SiC nanowires/whiskers; and thirdly, adding a bonding agent and a defoaming agent into the ceramic slurry prepared in the second step, and mechanically stirring and uniformly mixing to prepare the hydrogel slurry with the shear thinning characteristic, wherein the content of the bonding agent is 5-30%, and the defoaming agent is 0.2-3% of the mass of water.
And extruding the hydrogel slurry in a 3D printing mode, and laminating and forming to obtain a blank. Wherein, the diameter of the 3D printing extrusion needle head can be 50-2000 μm, and preferably 100-500 μm. The pressure of the extrusion molding can be 0.1-0.8 MPa. The printing distance is more than or equal to 0 mu m, the interlayer distance is 70-100% of the inner diameter of the printing needle head, and the printing speed is 5-30 mm/s. . Specifically, the prepared hydrogel slurry is placed into a charging barrel of a 3D printer based on an extrusion molding mode, the charging barrel is set at a proper temperature, the hydrogel slurry is extruded out through a printing needle under the action of pressure, and the hydrogel slurry is printed into a specific shape and a specific size under the control of a program. In alternative embodiments, the extrusion molding may be direct ink writing/printing (DIW/DIP), Fused Deposition Modeling (FDM), or Robocasting.
And degreasing and removing the glue of the green body, placing the green body in a protective atmosphere, and sintering at 1750-2100 ℃ for 1-3 hours to obtain the light high-strength SiC porous material. In an optional embodiment, the sintering temperature is 1800-2100 ℃, the protective atmosphere can be Ar gas, nitrogen gas, helium gas and the like, the sintering is carried out under normal pressure, and the sintering time can be 1-3 hours. Wherein the temperature of degreasing and degumming is 500-1000 ℃, and the time is 0.5-3 hours.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
Putting SiC nanowires (with the length-diameter ratio of 50-100 and the diameter of-100 nm) into deionized water for several times, preparing 10 vol% SiC nanowire slurry in an ultrasonic dispersion mode, and then adding 10% Al nanowire mass fraction2O3/Y2O3(molar ratio 3:2) adding the sintering aid into the dispersed SiC nanowire slurry, and further performing ultrasonic dispersion to uniformly disperse. The obtained slurry is screened by a 60-mesh screen to filter out large-size aggregates which are difficult to disperse. Adding polyethylene glycol with the water mass of 10 wt% into the slurry obtained by filtering, mechanically stirring for 6h at high speed, then adding 1-octanol defoaming agent with the water content of 1%, and continuously stirring for 1h to obtain the final paste suitable for printing. And transferring the obtained slurry into a material cylinder of 3D printing equipment formed based on a slurry extrusion mode, extruding the paste in the material cylinder through a needle head with the diameter of 420 micrometers under the action of 0.45MPa pressure under the condition of room temperature under the control of a program, and arranging the SiC nanowires in a one-dimensional orientation along the extrusion direction under the action of shear stress. The print pitch (distance between fibers formed of extruded SiC one-dimensional nanomaterial) was 420 μm, and the interlayer pitch was 350 μm. And 3D printing and forming to obtain the structural body without obvious macroscopic gaps. Drying the printed material at room temperature for 24 hours, removing glue at the temperature rising rate of 1 ℃/min for 1 hour at the temperature of 500 ℃ in an air environment, placing the material after glue removal into a carbon tube furnace in an argon atmosphere, raising the temperature at 5 ℃/min to 1850 ℃ and preserving the heat for 2 hours, and cooling to obtain the SiC porous ceramic completely consisting of the directionally arranged SiC nanowires, wherein the porosity of the material is 58.5%, and the compression strength is 108 MPa. The microstructure of the SiC nanowire is shown in an SEM picture shown in figure 1, and the SiC nanowires are arranged in a one-dimensional orientation, and the SiC nanowire contact points are sintered together through a sintering aid.
Example 2
In the embodiment, the porous silicon carbide ceramic mainly prepared is composed of latticed oriented SiC nanowires with visible macropores. The material was prepared in the same manner as in example 1. The printing parameters were adjusted to a printing pitch of 500 μm. After sintering, the porosity of the material is 68.2%, and the compressive strength is 38 MPa.
Example 3
In this example, a porous silicon carbide ceramic composed of oriented SiC whiskers (aspect ratio of 10 to 50, diameter of about 1 μm) was mainly introduced, and the specific preparation method was the same as in example 1. The porosity of the material is 53.9%, and the compressive strength is 123 MPa.
Example 4
Putting SiC nanowires (with the length-diameter ratio of 50-100 and the diameter of about 100nm) into deionized water in batches, and dispersing by using ultrasonic wavesPreparing 15 vol% SiC nanowire slurry, and then mixing the nanowire with 5% of Al by mass2O3/Y2O3(3:2) adding the sintering aid into the dispersed SiC nanowire slurry, and further performing ultrasonic dispersion uniformly. The obtained slurry is screened by a 60-mesh screen to filter out large-size aggregates which are difficult to disperse. Adding pluronic acid with the water content of 20wt% into the slurry obtained by filtering, stirring for 1.5 hours at a high speed through a low-temperature machine, then adding a 1-octanol defoaming agent with the water content of 1%, and continuously stirring for 1 hour to obtain the final paste suitable for printing. The obtained slurry is transferred to a material cylinder of 3D printing equipment formed based on a slurry extrusion mode, under the condition of program control and room temperature, paste (slurry) in the material cylinder is extruded out through a needle head with the diameter of 200 microns under the action of pressure of 0.6MPa, and SiC nanowires are arranged in a one-dimensional orientation along the extrusion direction under the action of shear stress. The print pitch was 200 μm and the interlayer pitch was 160 μm. And 3D printing and forming to obtain the structural body without obvious macroscopic gaps. Drying the printed material at room temperature for 24 hours, removing glue at the temperature rising rate of 1 ℃/min for 1 hour at the temperature of 500 ℃ in the air environment, placing the material after glue removal into a carbon tube furnace in the argon atmosphere, raising the temperature at 5 ℃/min to 1950 ℃, preserving the heat for 2 hours, and cooling to obtain the SiC porous ceramic completely consisting of directionally arranged SiC nanowires, wherein the porosity of the material is 41.0%, and the compression strength is 246 MPa.
FIG. 2 is a comparison graph of the performance of the oriented SiC nanowire porous Ceramic of the present invention and other porous SiC materials, wherein the oriented SiCNW is porous SiC prepared by sintering conventional particles (examples 3 and 4), the porous SiC is porous SiC prepared by sintering conventional particles (see Journal of Alloys and Compounds 684 (2016)) 615; Journal of the European Ceramic Society 34(2014)837 and 840; J.Am.C.Soc., 94[2] 344-347 (2011)), and the SiCNW/SiC is porous material prepared by chemical vapor deposition of non-oriented SiC nanowire reinforcement (see Journal of the European Ceramic Society 37(2017) 915-921). As can be seen from the comparison of FIG. 2, the strength of the porous material sintered by the one-dimensional oriented SiC nanowires/whiskers prepared by the method is significantly superior to that of the porous SiC ceramic sintered by the traditional SiC ceramic particles. Compared with the non-oriented SiC nanowire reinforced SiC porous ceramic, the material has higher porosity under the same strength and has the remarkable advantages of light weight and high strength.
It should be noted that the above-mentioned embodiments are merely examples of the present invention, and it is obvious that the present invention is not limited to the above-mentioned embodiments, and other modifications are possible. All modifications directly or indirectly derived from the disclosure herein by one of ordinary skill in the art are deemed to be within the scope of the present invention.
Claims (10)
1. A preparation method of a light high-strength SiC porous material is characterized by comprising the following steps:
extruding hydrogel slurry containing the SiC one-dimensional nano material in a 3D printing mode, and superposing and forming layer by layer to obtain a blank;
and degreasing and removing the glue of the obtained blank, placing the blank in a protective atmosphere, and sintering the blank at 1750-2100 ℃ for 1-3 hours to obtain the light high-strength SiC porous material.
2. The preparation method of claim 1, wherein the SiC one-dimensional nanomaterial has a diameter of 5-1000 nm and an aspect ratio of > 10, and is preferably in the shape of at least one of a nanowire and a whisker.
3. The method according to claim 1 or 2, wherein after extrusion the Si one-dimensional nanomaterials are in an oriented arrangement with a degree of orientation > 85%.
4. The method according to any one of claims 1 to 3, wherein the 3D printing mode is a direct ink writing/printing (DIW/DIP), Fused Deposition Modeling (FDM), or Robocasting mode.
5. The preparation method according to any one of claims 1 to 4, wherein the diameter of the needle used in the 3D printing mode is larger than the length of the SiC one-dimensional nanomaterial, preferably 50 to 2000 μm, and more preferably 100 to 500 μm; the pressure of 3D printing is 0.1-0.8 MPa.
6. The preparation method according to any one of claims 1 to 5, wherein the volume content of the SiC one-dimensional nanomaterial in the hydrogel slurry is 1 to 30 vol%; preferably, the hydrogel slurry further comprises a sintering aid, and the sintering aid is Al2O3、Y2O3At least one of MgO; preferably, the addition amount of the sintering aid is 1-20 wt% of the SiC one-dimensional nano material.
7. The production method according to any one of claims 1 to 6, characterized in that a binder and an antifoaming agent are further included in the hydrogel slurry, the binder is at least one of polyethylene glycol, gelatin, chitosan, pluronic acid and methyl cellulose, and the antifoaming agent is at least one of 1-octanol and isopropanol; preferably, the addition amount of the bonding agent is 5-30 wt% of the mass of water, and the addition amount of the defoaming agent is 0.2-3% of the mass of water.
8. The preparation method according to any one of claims 1 to 7, wherein the degreasing and degumming temperature is 500 to 1000 ℃ and the time is 0.5 to 3 hours.
9. The method for manufacturing according to any one of claims 1 to 8, wherein the parameters of the 3D printing mode include: the printing distance is more than or equal to 0 mu m, the interlayer distance is 70-100% of the diameter of the printing needle head, and the printing speed is 5-30 mm/s.
10. A lightweight high-strength SiC porous material produced by the production method according to any one of claims 1 to 9.
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Cited By (1)
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|---|---|---|---|---|
| CN113666764A (en) * | 2021-09-15 | 2021-11-19 | 北京理工大学 | Direct-writing forming method for short carbon fiber reinforced silicon carbide ceramic composite material ink |
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| CN105254322A (en) * | 2015-11-04 | 2016-01-20 | 陕西科技大学 | Preparation method of oriented porous SiC ceramic with crystal boundary containing metal phases |
| US20170151733A1 (en) * | 2015-11-30 | 2017-06-01 | President And Fellows Of Harvard College | Method of 4d printing a hydrogel composite structure |
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| CLAUDIO FERRARO等: "Light and Strong SiC Networks", 《ADVANCED FUNCTIONAL MATERIALS》 * |
| 汪长安等: "晶须增韧补强陶瓷基复合材料的若干关键技术研究（Ⅱ）：晶须定向排布工艺及其复合材料力学性能", 《高技术通讯》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113666764A (en) * | 2021-09-15 | 2021-11-19 | 北京理工大学 | Direct-writing forming method for short carbon fiber reinforced silicon carbide ceramic composite material ink |
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