CN111233478B - Layered slurry preparation method of titanium carbide gradient porous ceramic - Google Patents
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Abstract
The invention discloses a layered slurry preparation method of titanium carbide gradient porous ceramic, which is realized by the following technical scheme: titanium powder and carbon powder are used as raw materials, the titanium powder and the carbon powder are weighed according to the molar ratio of 1: 0.5-1, and a certain amount of PVB and absolute ethyl alcohol are added to prepare slurry; the method comprises the steps of taking 20-60 PPI organic sponge as a template, dividing the template into 2-6 layers along a certain direction, sequentially coating slurry on each layer of the template, gradually increasing the slurry coating times between every two layers by 1-2 times, drying the slurry coated template, and sintering under no pressure to obtain the titanium carbide gradient porous ceramic. The porosity of the titanium carbide porous ceramic prepared by the method is in gradient distribution, and the porosity and gradient change rate of two sides can be regulated and controlled through the number of layers of the template and the number difference of interlayer slurry hanging times; the method has the advantages of simple process, strong operability and low cost.
Description
Technical Field
The invention relates to the field of porous ceramics, in particular to a layered slurry preparation method of titanium carbide gradient porous ceramics.
Background
The porous ceramic is a novel functional material, has stable physical and chemical properties and higher porosity, can be used as materials for sound insulation, heat preservation, filtration, catalyst carriers and the like, and is widely applied to a plurality of fields of biology, energy, smelting, chemical industry, environmental protection and the like. Due to different preparation methods, the porous ceramics have different properties such as porosity, mechanical strength and the like, so that the functions and the applications of the porous ceramics are different. The porous ceramic prepared by the particle stacking and forming method has uniform pore distribution, and the pore size is in direct proportion to the particle size of the aggregate; porous ceramics with different apertures and shapes can be prepared by adding a pore-forming agent method, but the porosity of the porous ceramics is generally not more than 50 percent, and the ceramic sample is easy to break due to overhigh porosity; the porous ceramic prepared by the foaming process has the characteristics of high strength, high porosity (about 60 percent), narrow pore size distribution and the like, but the method has strict requirements on raw materials, and partial reaction conditions are difficult to control in the experimental process; the porous ceramic with a more complex pore structure can be prepared by a freeze-drying method, the process control is simple, the sintering shrinkage of a blank body is small, but the preparation cost is high; the discharge plasma sintering method can obtain porous ceramics with higher quality at lower temperature, but the sample prepared by the process has single structure and serious loss of the die; the organic foam impregnation method can prepare porous ceramic with a three-dimensional reticular skeleton structure, is novel ceramic with a special structure, has the advantages of small fluid pressure loss, large specific surface area, light weight and the like, and good filter materials are mostly in the structure. However, the porosity of the porous ceramic prepared by the method is uniformly distributed in the whole material.
The gradient porous ceramic is porous ceramic with porosity in gradient distribution in a certain direction, and the structure can realize continuous filtration in various scales when used as a filter, and can be used as a prefabricated reinforcement to be compounded with a metal matrix to form a porous ceramic/metal gradient composite material, so that two sides of the composite material present distinct properties, and the problem of interface stress can be effectively solved when the gradient porous ceramic is used as a connecting layer between ceramic and metal. The method for preparing the gradient porous ceramic mainly adopts a centrifugal forming technology, namely, the large particles contained in slurry are deposited to the outer layer and the small particles are deposited to the inner layer by utilizing the different deposition speeds of particles with different particle sizes during high-speed centrifugation to form a gradient structure. In addition, the gradient porous ceramic can also be prepared through reasonable grain composition and a special sintering process, for example, a pore gradient structure can be constructed by stacking grains with different grain sizes according to a certain proportion, but uneven shrinkage in the sintering process can influence the compactness, thereby influencing the porosity. The traditional gradient porous ceramic preparation method has the defects that the preparation process is complex and sintering is difficult due to uneven structure, and the separation phenomenon among layers is often generated in the preparation process.
The invention relates to a double-gradient porous ceramic material and a preparation method thereof (application number: CN201711340250.X), which prepares water system slurry by adding a certain amount of dispersant and sintering aid, and sequentially carries out processes of freezing, freeze drying, binder removal sintering and the like on the slurry to obtain the porous ceramic material with double gradients in structure and components. The process can prepare gradient structure ceramics with different material lamella spacing and from top to bottom, but the gradient change rate of the gradient ceramic structure prepared by the process is difficult to control, and the practical application difficulty is higher. The invention discloses a silver-loaded gradient porous ceramic material prepared by a vacuum foaming process and a preparation method thereof (application number: CN 201710559204.2). the gradient porous ceramic material is prepared by the processes of crushing ceramic powder, adding a binder and a foaming agent, grouting, vacuumizing, maintaining pressure, sintering at high temperature and the like. Therefore, the development of a preparation method of the gradient porous ceramic, which is simple and easy to operate, strong in applicability and low in cost, has important significance. The layered slurry-coating preparation method of the titanium carbide gradient porous ceramic provided by the invention can be used for preparing the gradient porous ceramic with adjustable porosity, pore size and gradient change rate, is simple to operate, strong in applicability and low in cost, and can be simultaneously used for preparing other carbide, oxide, nitride ceramic and metal gradient porous materials.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing titanium carbide gradient porous ceramic by taking organic sponge as a template and titanium powder and carbon powder as main raw materials.
The invention adopts the technical scheme that a layered slurry preparation method of titanium carbide gradient porous ceramic is provided, which is characterized by comprising the following steps:
(1) selecting and designing a template: selecting organic sponge with a certain aperture as a template, pretreating, dividing the template into a plurality of layers according to needs along a certain direction, and marking the positions of the layers on the template;
(2) preparing slurry: weighing a certain amount of titanium powder, carbon powder, PVB (polyvinyl butyral) and absolute ethyl alcohol, and preparing slurry by ball milling and mixing;
(3) slurry coating of a template: immersing an organic sponge template into slurry layer by layer according to the gradient layer number designed in the step (1), sequentially coating slurry from top to bottom or from bottom to top, and drying to obtain a gradient porous ceramic blank;
(4) and (3) sintering: and (4) sintering the blank obtained in the step (3) in a furnace to obtain the titanium carbide gradient porous ceramic.
The invention is also characterized in that: the organic sponge in the step (1) has a pore size range of 20-60 PPI (Pores Per Inc); the pretreatment method comprises the steps of soaking sponge in a 10% NaOH solution for 10 hours, and then soaking sponge in a CMC (sodium carboxymethylcellulose) solution for 20 hours; the layering method is to divide the sponge into 2-6 layers uniformly or non-uniformly along a certain direction.
The invention is also characterized in that: the preparation method of the slurry in the step (2) comprises the following steps: weighing a certain amount of PVB and absolute ethyl alcohol to prepare a PVB ethyl alcohol solution of 2-5 wt.%; weighing titanium powder and carbon powder according to the molar ratio of 1: 0.5-1, adding a PVB ethanol solution into the titanium powder and the carbon powder according to the mass ratio of 1:1, and performing roller ball milling for 8-24 hours to obtain slurry.
The invention is also characterized in that: the template slurry coating method in the step (3) comprises the following steps: layering and slurry hanging from top to bottom: firstly, immersing the whole template into slurry for slurry coating for 3-5 times, then immersing the rest parts of the template except the uppermost layer into the slurry for slurry coating for 1-2 times, and coating slurry on each layer of the lower part of the template in sequence by the method so as to increase the slurry coating times of the whole template from top to bottom; secondly, layering and grouting from bottom to top: firstly, immersing the lowest layer of a template into slurry for slurry hanging for 1-2 times, then immersing the two layers of the lowest layer of the template into the slurry for slurry hanging for 1-2 times, sequentially hanging slurry on each layer of the template according to the method, and finally immersing the whole template into the slurry for slurry hanging for 3-5 times; the drying method in the step (3) comprises the following steps: naturally drying at room temperature or drying by heating in an oven.
The invention is also characterized in that: the sintering process conditions in the step (4) are as follows: the sintering temperature is 1400-1600 ℃, and the temperature is kept for 0.5-2 hours under the protection of vacuum or inert gas.
The invention provides a layered slurry preparation method of titanium carbide gradient porous ceramic, which has the beneficial effects that: 1) the invention can prepare the titanium carbide porous ceramic with gradient porosity; 2) the porosity and gradient change rate of the two sides of the prepared titanium carbide gradient porous ceramic can be regulated and controlled by changing the aperture of the template, the number of layers of the template and the number difference of interlayer slurry coating times, and the method has the advantages of simple process, strong operability and low cost; 3) the method of the invention can also be used for preparing other carbide, oxide, nitride ceramics and metal gradient porous materials.
Drawings
Fig. 1 is a schematic diagram of a gradient porous ceramic with 4 layers in example two, wherein 1, 2, 3, and 4 are gradient layers obtained by organic sponge template slurry coating for 4, 6, 8, and 10 times, respectively.
FIG. 2 is a diagram of a titanium carbide gradient porous ceramic material having 4 layers in the second example.
Detailed Description
The following description of the present invention will be made with reference to the accompanying drawings and examples, but the present invention is not limited to the above description.
Example one
Selecting a sponge template with 20PPI, soaking the sponge template in a NaOH solution with the concentration of 10% for 10 hours, then soaking the sponge template in a CMC (sodium carboxymethylcellulose) solution for 20 hours, drying the sponge template, uniformly dividing the sponge template into 2 layers along a certain direction, and marking the interface position; weighing 2 g of PVB powder, 98 g of absolute ethyl alcohol to prepare a PVB ethanol solution, weighing 48 g of titanium powder and 12 g of carbon powder, adding 60 g of the prepared PVB ethanol solution, carrying out roller ball milling for 12h to prepare slurry, carrying out layered slurry coating on the layered organic sponge from top to bottom, firstly immersing the whole template into the slurry for 5 times, then immersing the lower layer of the template into the slurry for 2 times, drying the slurry-coated template in an oven at 60 ℃ to obtain a gradient porous ceramic blank, finally placing the blank into a high-temperature furnace, heating to 1400 ℃ under the protection of argon gas, carrying out heat preservation for 2h, and carrying out pressureless sintering to obtain the titanium carbide gradient porous ceramic.
The porosities of the upper and lower layers of the titanium carbide gradient porous ceramic were measured to be 92.6% and 89.2%, respectively.
Example two
Selecting a sponge template with 30PPI, soaking the sponge template in a NaOH solution with the concentration of 10% for 10 hours, then soaking the sponge template in a CMC solution for 20 hours, drying the sponge template, uniformly dividing the sponge template into 4 layers along a certain direction, and marking the positions of all the layers; weighing 3 g of PVB powder, 97 g of absolute ethyl alcohol to prepare a PVB ethanol solution, weighing 48 g of titanium powder and 10 g of carbon powder, adding 58 g of the prepared PVB ethanol solution, carrying out roller ball milling for 16h to prepare slurry, carrying out layered slurry coating on the layered organic sponge from top to bottom, firstly immersing the whole template into the slurry for slurry coating for 4 times, then immersing the rest three layers of the template except the top layer into the slurry for slurry coating for 2 times, sequentially carrying out slurry coating on each layer of the template according to the method to enable each layer of the template to be coated with slurry for 4, 6, 8 and 10 times, then putting the slurry-coated template into a drying oven to be dried at 60 ℃ to obtain a gradient porous ceramic blank, finally putting the blank into a high-temperature furnace, heating to 1500 ℃ under the protection of nitrogen, and carrying out non-pressure sintering to obtain the titanium carbide gradient porous ceramic.
The porosities of the respective layers of the above titanium carbide gradient porous ceramic were measured to be 92.9%, 89.2%, 85.3%, and 81.1%, respectively.
EXAMPLE III
Selecting a sponge template with 50PPI, soaking the sponge template in a NaOH solution with the concentration of 10% for 10 hours, then soaking the sponge template in a CMC solution for 20 hours, drying the sponge template, dividing the sponge template into 3 uneven layers along a certain direction, and marking the positions of all the layers; weighing 4 g of PVB powder, 96 g of absolute ethyl alcohol to prepare a PVB ethanol solution, weighing 48 g of titanium powder and 6 g of carbon powder, adding 54 g of the prepared PVB ethanol solution, carrying out roller ball milling for 8h to prepare slurry, layering and slurry-coating the layered organic sponge from bottom to top, firstly immersing the lowest layer of a template into the slurry for slurry-coating for 1 time, then slurry-coating the lowest layer of the template for 1 time, and finally slurry-coating the whole template for 4 times, so that slurry-coating is carried out on each layer of the template for 4, 5 and 6 times, naturally drying the slurry-coated template at room temperature to obtain a gradient porous ceramic blank, finally placing the blank into a high-temperature furnace, heating to 1600 ℃ in a vacuum environment, and carrying out non-pressure sintering for 0.5h to obtain the titanium carbide gradient porous ceramic.
The porosity of each layer of the titanium carbide gradient porous ceramic was measured to be 88.2%, 85.0% and 81.7%, respectively.
Example four
Selecting a sponge template with 50PPI, soaking the sponge template in a NaOH solution with the concentration of 10% for 10 hours, then soaking the sponge template in a CMC solution for 20 hours, drying the sponge template, uniformly dividing the sponge template into 5 layers along a certain direction, and marking the positions of all the layers; weighing 5 g of PVB powder and 95 g of absolute ethyl alcohol to prepare a PVB ethanol solution, weighing 48 g of titanium powder and 8 g of carbon powder, adding 56 g of the prepared PVB ethanol solution, carrying out roller ball milling for 24h to prepare slurry, carrying out layered slurry coating on the layered organic sponge from top to bottom, firstly immersing the whole template into the slurry for slurry coating for 3 times, then immersing the rest of the template except the top layer into the slurry for slurry coating for 2 times, sequentially carrying out slurry coating on all the layers of the template according to the method, carrying out slurry coating on all the layers of the template for 3, 5, 7, 9 and 11 times respectively, then putting the slurry-coated template into a drying oven for drying at 60 ℃ to obtain a gradient porous ceramic blank, finally putting the blank into a high-temperature furnace, heating to 1450 ℃ under the protection of argon gas, and carrying out non-pressure sintering to obtain the titanium carbide gradient porous ceramic.
The porosity of each layer of the titanium carbide gradient porous ceramic was measured to be 91.4%, 85.2%, 78.8%, 72.3% and 65.5%, respectively.
EXAMPLE five
Selecting a 60PPI sponge template, soaking the sponge template in a 10% NaOH solution for 10 hours, then soaking the sponge template in a CMC solution for 20 hours, drying, uniformly dividing the sponge template into 3 layers along a certain direction, and marking the positions of all the layers; weighing 4 g of PVB powder, 96 g of absolute ethyl alcohol to prepare a PVB ethanol solution, weighing 48 g of titanium powder and 12 g of carbon powder, adding 60 g of the prepared PVB ethanol solution, carrying out roller ball milling for 18h to prepare slurry, carrying out layered slurry coating on the layered organic sponge from bottom to top, firstly immersing the lowest layer of a template into the slurry for slurry coating for 2 times, then carrying out slurry coating on the lowest layer of the template for 2 times, and finally carrying out slurry coating on the whole template for 3 times, so that the slurry coating is carried out on each layer of the template for 3, 5 and 7 times respectively, putting the slurry coated template into a drying oven to be dried at 60 ℃ to obtain a gradient porous ceramic blank, finally putting the blank into a high-temperature furnace, heating to 1500 ℃ under the protection of argon gas, carrying out heat preservation for 1h, and carrying out pressureless sintering to obtain.
The porosities of the respective layers of the above titanium carbide gradient porous ceramic were measured to be 89.7%, 82.5%, and 74.9%, respectively.
EXAMPLE six
Selecting a 60PPI sponge template, soaking the sponge template in a 10% NaOH solution for 10 hours, then soaking the sponge template in a CMC solution for 20 hours, drying, dividing the sponge template into 6 uneven layers along a certain direction, and marking the positions of the layers; weighing 3 g of PVB powder, 97 g of absolute ethyl alcohol to prepare a PVB ethanol solution, weighing 48 g of titanium powder and 9 g of carbon powder, adding 57 g of the prepared PVB ethanol solution, carrying out roller ball milling for 12h to prepare slurry, carrying out layered slurry coating on the layered organic sponge from top to bottom, firstly immersing the whole template into the slurry for slurry coating for 4 times, then immersing the rest of the template except the top layer into the slurry for slurry coating for 1 time, sequentially carrying out slurry coating on all layers of the template according to the method, carrying out slurry coating on all layers of the template for 4, 5, 6, 7, 8 and 9 times respectively, naturally drying the slurry-coated template at room temperature to obtain a gradient porous ceramic blank, and finally putting the blank into a high-temperature furnace, heating to 1600 ℃ in a vacuum environment, carrying out non-pressure sintering for 1h to obtain the titanium carbide gradient porous ceramic.
The porosity of each layer of the titanium carbide gradient porous ceramic was measured to be 86.7%, 83.3%, 79.7%, 75.9%, 72.0%, and 67.8%, respectively.
Claims (2)
1. A layered slurry preparation method of titanium carbide gradient porous ceramic is characterized by comprising the following steps:
(1) selecting and designing a template: selecting organic sponge with a certain aperture as a template, pretreating, dividing the template into a plurality of layers according to needs along a certain direction, and marking the positions of the layers on the template;
wherein the pore size of the organic sponge is 20-60 PPI; the pretreatment method comprises the steps of soaking the sponge in a 10% NaOH solution for 10 hours, and then soaking the sponge in a CMC solution for 20 hours; the layering method comprises the steps of uniformly or non-uniformly dividing the sponge into 2-6 layers along a certain direction;
(2) preparing slurry: weighing a certain amount of titanium powder, carbon powder, PVB and absolute ethyl alcohol, and preparing slurry by ball milling and mixing;
(3) slurry coating of a template: immersing an organic sponge template into slurry layer by layer according to the gradient layer number designed in the step (1), sequentially coating slurry from top to bottom or from bottom to top, and drying to obtain a gradient porous ceramic blank;
the method for layering and hanging the pulp from top to bottom or from bottom to top comprises the following steps: layering and slurry hanging from top to bottom: firstly, immersing the whole template into slurry for slurry coating for 3-5 times, then immersing the rest of the template except the uppermost layer into the slurry for slurry coating for 1-2 times, and coating slurry on each layer of the lower part of the template in sequence according to the method, so that the slurry coating times of the whole template are increased in sequence from top to bottom; secondly, layering and grouting from bottom to top: firstly, immersing the lowest layer of a template into slurry for slurry hanging for 1-2 times, then immersing the two layers of the lowest layer of the template into the slurry for slurry hanging for 1-2 times, sequentially hanging the slurry on each layer of the template from bottom to top according to the method, and finally immersing the whole template into the slurry for slurry hanging for 3-5 times; the drying method comprises the following steps: naturally drying at room temperature or drying by heating in an oven;
(4) and (3) sintering: sintering the blank obtained in the step (3) in a furnace to obtain titanium carbide gradient porous ceramic;
wherein, the sintering process conditions are as follows: the sintering temperature is 1400-1600oAnd C, preserving the heat for 0.5 to 2 hours under the protection of vacuum or inert gas.
2. The layered slurry preparation method of the titanium carbide gradient porous ceramic according to claim 1, characterized in that: the preparation method of the slurry in the step (2) comprises the following steps: weighing a certain amount of PVB and absolute ethyl alcohol to prepare a PVB ethyl alcohol solution of 2-5 wt.%; weighing titanium powder and carbon powder according to the molar ratio of 1: 0.5-1, adding a PVB ethanol solution into the titanium powder and the carbon powder according to the mass ratio of 1:1, and performing roller ball milling for 8-24 hours to obtain slurry.
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| CN114274312B (en) * | 2022-01-25 | 2022-08-30 | 东北大学 | Device and method for preparing foamed ceramic |
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| CN110590367B (en) * | 2019-10-15 | 2020-12-01 | 北京交通大学 | Organic template dip forming-pressureless sintering preparation method of gradient TiC porous ceramic |
| CN110590369B (en) * | 2019-10-31 | 2020-12-22 | 北京交通大学 | Continuous gradient TiC porous ceramic and template compression preparation method thereof |
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