CN108467281B - Preparation method of zirconia porous ceramic - Google Patents
Preparation method of zirconia porous ceramic Download PDFInfo
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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Abstract
The invention relates to a preparation method of zirconia porous ceramic, which comprises the following steps: step 1: putting zirconia powder and carbon fiber into a container, adding a proper amount of water, stirring and mixing, adding a foaming agent and a foam stabilizer in the stirring process until bubbling is uniform, and then adding a binder to obtain a mixed material; step 2: pouring the mixed material into a forming die, and naturally airing and forming to obtain a green body; and step 3: putting the green body into a closed box, vacuumizing, then filling butane and oxygen to normal pressure, standing, igniting by electronic fire after 1.5-3 hours to enable the butane to burn, and obtaining a perforated green body after the burning is finished; and 4, step 4: and sintering the blank with the opening at high temperature to obtain the zirconia porous ceramic. The carbon fibers are connected in a cross way to form a network framework which is used for firmly supporting the zirconia powder and other materials, so that the toughness and the strength of the ceramic are improved; the foam stabilizer is introduced to control the time of foam breakage, so that the porous material with uniform pore diameter and compact arrangement is obtained, and the preparation process is green and environment-friendly.
Description
Technical Field
The invention relates to the technical field of ceramic products, in particular to a preparation method of zirconia porous ceramic.
Background
The application of porous ceramics began in the 70's of the 19 th century, when only used as uranium purification materials and bacterial filtration materials. With the continuous expansion of the application range of the porous ceramics, the application field of the porous ceramics is gradually expanded, and the porous ceramics are gradually expanded to the fields of heat insulation, sound absorption, electronics, photoelectricity, sensing, environmental biology and chemistry from the fields of filtration, thermal engineering and the like.
Structurally, the porous ceramic is a high porosity porous ceramic body having a three-dimensional lattice structure, and is shaped like a toughened foamed plastic or a vitrified sponge. Because of its high porosity, large specific surface area, thermal shock resistance, high temperature resistance, chemical corrosion resistance, good mechanical strength and filtering and adsorbing properties, it can be widely used in heat exchange materials, gas distribution materials, automobile exhaust devices, purification and metallurgy industries for filtering molten metal, heat energy recovery, light industry spraying industry, industrial sewage treatment, heat and sound insulation materials, as chemical catalyst carrier, electrolytic diaphragm and separation and dispersion elements, etc.
Therefore, it is necessary to prepare a porous ceramic body having high strength and uniform pore size, and to broaden and develop the applications of the porous ceramic in various domestic industries.
Disclosure of Invention
Based on the method, no toxic substances are generated in the preparation process, the method is green and environment-friendly, and the prepared zirconia porous ceramic is uniform in pore size, good in toughness and strength.
A preparation method of zirconia porous ceramic comprises the following steps:
step 1: putting zirconia powder and carbon fiber into a container, adding a proper amount of water, stirring and mixing, adding a foaming agent and a foam stabilizer in the stirring process until bubbling is uniform, and then adding a binder to obtain a mixed material;
step 2: pouring the mixed material into a forming die, and naturally airing and forming to obtain a green body;
and step 3: putting the green body into a closed box, vacuumizing, then filling butane and oxygen to normal pressure, standing for 1.5-3 hours, igniting by using electronic fire to combust the butane, and obtaining a perforated green body after the combustion is finished;
and 4, step 4: and sintering the blank with the opening at high temperature to obtain the zirconia porous ceramic.
According to the preparation method of the zirconia porous ceramic, the carbon fiber has light specific gravity, can be attached to the outer wall of the foam, is in cross connection to form a network framework, and is used for firmly supporting zirconia powder and other materials, so that the toughness and strength of the ceramic are improved, and the structure of the porous ceramic is stable and firm; introducing a foam stabilizer into a reaction system to control the foam breaking time, ensuring that the foam is not easy to break before forming after the foaming agent is foamed, and obtaining multiple holes with uniform pore diameter and compact arrangement after the steps of air-drying forming and opening; and no poison is generated in the preparation process, so that the preparation method is green and environment-friendly.
In one embodiment, the mass ratio of the zirconia powder, the carbon fiber, the foaming agent, the foam stabilizer and the binder is as follows: 100: 15-40: 5-10: 0.1-1.5: 6 to 12.
In one embodiment, the carbon fiber has a diameter of 6 to 20 μm and a length of 3 to 12 mm.
In one embodiment, the particle size of the zirconia powder is 0.2-1 μm.
In one embodiment, the mass content of zirconia in the zirconia powder is more than or equal to 90%.
In one embodiment, the foaming agent is an anionic surfactant.
In one embodiment, the foaming agent is sodium linear alkylbenzene sulfonate, alkyl sulfonate, sodium alpha olefin sulfonate, alpha sulfomonocarboxylic acid and derivatives thereof, fatty acid sulfoalkyl ester or fatty acid sulfoalkyl amide.
In one embodiment, the foam stabilizer is a silicone polyether emulsion.
In one embodiment, the binder is polyvinyl alcohol.
In one embodiment, the high temperature sintering is: heating to 500-750 ℃ at the speed of 0.5-2 ℃/min, preserving heat for 1-2 h, heating to 1400-1600 ℃ at the speed of 2-3 ℃/min, and keeping for 2-4 h.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The invention provides a preparation method of zirconia porous ceramic, which comprises the following steps:
step 1: provides zirconia powder, carbon fiber, foaming agent, foam stabilizer, adhesive and water.
For example, the components, zirconia powder: carbon fiber: foaming agent: foam stabilizer: the binder is 100: 15-40: 5-10: 0.1-1.5: 6 to 12.
Step 2: putting zirconia powder and carbon fiber into a container, adding a proper amount of water, stirring and mixing the water according to the amount of wetting the zirconia powder and the carbon fiber, adding a foaming agent and a foam stabilizer in the stirring process until bubbling is uniform, and then adding a binder to obtain a mixed material.
The carbon fiber has light specific gravity, can be attached to the outer wall of the foam, is connected in a cross way to form a network framework, and is used for firmly supporting zirconia powder and other materials, so that the toughness and the strength of the ceramic are improved, and the structure of the porous ceramic is stable and firm. Preferably, the diameter of the carbon fiber is selected to be 6-20 μm, and the length is selected to be 3-12 mm. Carbon fiber is shorter than 3mm or is longer than 12mm and does not do benefit to the absorption of carbon fiber at the foam outer wall, may form too short and can't form cross connection, or too long and outsourcing foam outer wall is unfavorable for the formation of adjacent foam, leads to the too big problem in foam interval, and the pore-forming rate is low.
The zirconia powder is zirconia powder with a tetragonal crystal structure stabilized by yttria, and the mass content of zirconia in the zirconia powder is more than or equal to 90 percent so as to ensure tight combination among crystal grains and obtain a ceramic product with better mechanical property. The granularity is 0.2-1 μm, the carbon fiber can be filled into a network framework formed by weaving carbon fibers in a fine mode, foam formation is not damaged, and when the granularity of the zirconium oxide powder is larger than 1 μm, foam formation is not facilitated due to the fact that the zirconium oxide powder is rough.
The foaming agent is selected from an anionic surfactant, the reaction system contains water, the anionic surfactant is dissociated in the water to generate hydrophobic anions with surface activity, and foams are formed in the stirring process. Preferably, the foaming agent is selected from linear anionic surfactants, which are easily degraded by microorganisms and are more environmentally friendly, such as sodium linear alkylbenzene sulfonate, alkyl sulfonate, sodium alpha-olefin sulfonate, alpha-sulfomonocarboxylic acid and derivatives thereof, fatty acid sulfoalkyl ester or fatty acid sulfoalkyl amide.
In order to stabilize the foam before the porous ceramic is formed, a foam stabilizer is added. Of course, the more the foam stabilizer, the better, and if the foam does not break, the interconnected porosity of the ceramic will not be formed, so that it is necessary to control the amount of the foam stabilizer to control the timing of the break of the foam or the thickness of the foam. The invention selects a foaming agent and a foam stabilizer with a mass ratio of 5-10: 0.1-1.5, the foam can stably exist in a stirring state, when the foam is dried and formed, due to the reduction of moisture, molecules of the foaming agent shrink, the thin side wall of the foam presents pores along with the molecular shrinkage, or the thickness of the side wall is reduced, when butane is combusted, the thin wall of the pore can be punched by the impulse force of flame, the pores are opened, and the problem of cracking of the porous ceramic cannot be caused due to the network structure of the carbon fiber.
Preferably, the foam stabilizer is a silicone polyether emulsion, and the arrangement sequence of the inner molecules of the foaming agent is changed to ensure that the foam is tightly and tidily arranged between the bubbles so as to form a compact inner layer film, so that the anti-pressure capability is particularly strong, the structural stability of a bubble liquid film can be controlled, the foaming agent molecules are orderly distributed in the bubble liquid film, the foam is endowed with good elasticity and self-repairing capability, and a particularly ideal foam stabilizing effect is achieved.
The adhesive is polyvinyl alcohol, the mass concentration of the polyvinyl alcohol aqueous solution is 2.5 wt%, good adhesive force is provided for the forming of the porous ceramic, and the adhesive is easy to remove during adhesive discharge.
Step 3: and pouring the mixed material into a forming die, and naturally airing and forming to obtain a green body. The forming die can be a square or round or other irregular die, and the mixed material can be taken out after being dried and formed, so as to carry out the next working procedure.
And 4, step 4: the green body is placed in a closed box, evacuated and then charged with butane and oxygen to atmospheric pressure (typically 1 atm). Butane and oxygen are mixed and then are filled into the closed box together, so that the problem of uneven combustion caused by uneven mixing of butane and oxygen is avoided. The gas filling flow is 5-10L/min, so that the gas flow has certain impact force and can be filled into the pores of the green body, and certain fluidity is kept in a certain time, so that the gas is uniformly mixed. And (3) after the gas is filled, keeping standing for 1.5-3 hours, enabling butane and oxygen gas to be uniformly filled into pores of the green body, igniting by an electronic fire to enable the butane to be combusted, enabling the combustion temperature of the butane to reach 800-1000 ℃, enabling flame to be blown into the pores, discharging part of the binder, the foaming agent and the foam stabilizer, opening the pores, and penetrating through the pores in a certain direction to enable the pores to be uniformly opened. And after the combustion is finished, naturally cooling to 50-100 ℃ to obtain a blank with a hole.
And 5: sintering the blank with the hole at high temperature, heating to 500-750 ℃ at the speed of 0.5-2 ℃/min, preserving heat for 1-2 h, slowly heating to ensure that the temperature slowly permeates into the pore, and uniformly sintering the inner wall of the pore; and then heating to 1400-1600 ℃ at the speed of 2-3 ℃/min, and keeping for 2-4 h to ensure that the green body is sintered compactly. And (5) after high-temperature sintering, obtaining the zirconia porous ceramic.
According to the preparation method of the zirconia porous ceramic, carbon fibers are introduced into a reaction system to form a network skeleton, so that firm support is provided for the porous ceramic, the strength and the toughness of the porous ceramic are improved, the performance is stable, after foaming of a foaming agent, foam is not easy to break before forming by using a foam stabilizer, and pores with uniform pore diameter and compact arrangement are obtained after the steps of air-drying forming and opening.
The following are descriptions of specific embodiments.
Example 1
The preparation method of the zirconia porous ceramic of the embodiment comprises the following steps:
step 1: providing the following components in parts by weight: 100 parts of zirconia powder, 15 parts of carbon fiber, 6 parts of foaming agent, 0.5 part of foam stabilizer, 10 parts of binder and a proper amount of water.
The diameter of the carbon fiber is 6-12 μm, and the length is 3-8 mm.
The zirconia powder is yttria-stabilized zirconia powder with a tetragonal crystal structure, wherein the mass content of zirconia in the zirconia powder is 95%, and the granularity is 0.2-0.6 mu m.
The foaming agent is linear alkyl benzene sodium sulfonate.
The foam stabilizer is silicone polyether emulsion.
The adhesive is polyvinyl alcohol, and the mass concentration of the polyvinyl alcohol aqueous solution is 2.5 wt%.
Step 2: putting zirconia powder and carbon fiber into a container, adding a proper amount of water, stirring and mixing, adding a foaming agent and a foam stabilizer in the stirring process until bubbling is uniform, and then adding a binder to obtain a mixed material.
And step 3: and pouring the mixed material into a forming die, and naturally airing and forming to obtain a green body.
And 4, step 4: and putting the green body into a closed box, vacuumizing, then filling butane and oxygen to normal pressure, mixing the butane and the oxygen, filling the mixture into the closed box, filling gas at a flow rate of 5L/min, and keeping standing for 2 hours after filling the gas. After the combustion is finished, naturally cooling to 100 ℃ to obtain a blank with a hole.
And 5: and (3) sintering the blank with the hole at high temperature, heating to 600 ℃ at the speed of 0.5 ℃/min, preserving the heat for 1.5h, heating to 1500 ℃ at the speed of 2 ℃/min, and keeping the temperature for 2 h. And (5) after high-temperature sintering, obtaining the zirconia porous ceramic.
The zirconia foamed ceramic is detected to have a porosity of 72% and a bending strength of 96 MPa.
Example 2
The preparation method of the zirconia porous ceramic of the embodiment comprises the following steps:
step 1: providing the following components in parts by weight: 100 parts of zirconia powder, 20 parts of carbon fiber, 5 parts of foaming agent, 0.2 part of foam stabilizer, 8 parts of binder and a proper amount of water.
The diameter of the carbon fiber is selected to be 8-10 mu m, and the length is selected to be 5-8 mm.
The zirconia powder is yttria-stabilized zirconia powder with a tetragonal crystal structure, wherein the mass content of zirconia in the zirconia powder is 98%, and the granularity is 0.4-0.8 mu m.
The foaming agent is selected from alkyl sulfonate.
The foam stabilizer is silicone polyether emulsion.
The adhesive is polyvinyl alcohol, and the mass concentration of the polyvinyl alcohol aqueous solution is 2.5 wt%.
Step 2: putting zirconia powder and carbon fiber into a container, adding a proper amount of water, stirring and mixing, adding a foaming agent and a foam stabilizer in the stirring process until bubbling is uniform, and then adding a binder to obtain a mixed material.
Step 3: and pouring the mixed material into a forming die, and naturally airing and forming to obtain a green body.
And 4, step 4: and putting the green body into a closed box, vacuumizing, then filling butane and oxygen to normal pressure, mixing the butane and the oxygen, filling the mixture into the closed box, filling gas at the flow rate of 6L/min, and keeping standing for 1.5 hours after filling the gas. After the combustion is finished, naturally cooling to 90 ℃ to obtain a blank with a hole.
And 5: and (3) sintering the blank with the opening at high temperature, heating to 500 ℃ at the speed of 1 ℃/min, preserving the heat for 2h, heating to 1400 ℃ at the speed of 2 ℃/min, keeping the temperature for 3h, and obtaining the zirconia porous ceramic after the sintering at high temperature.
The zirconia foamed ceramic is detected to have a porosity of 78% and a bending strength of 105 MPa.
Example 3
The preparation method of the zirconia porous ceramic of the embodiment comprises the following steps:
step 1: providing the following components in parts by weight: 100 parts of zirconia powder, 25 parts of carbon fiber, 8 parts of foaming agent, 0.8 part of foam stabilizer, 10 parts of binder and a proper amount of water.
The diameter of the carbon fiber is 10-20 μm, and the length is 3-8 mm.
The zirconia powder is yttria-stabilized zirconia powder with a tetragonal crystal structure, wherein the mass content of zirconia in the zirconia powder is 98%, and the granularity is 0.3-0.8 mu m.
The foaming agent is fatty acid sulfoalkylamide.
The foam stabilizer is silicone polyether emulsion.
The adhesive is polyvinyl alcohol, and the mass concentration of the polyvinyl alcohol aqueous solution is 2.5 wt%.
Step 2: putting zirconia powder and carbon fiber into a container, adding a proper amount of water, stirring and mixing, adding a foaming agent and a foam stabilizer in the stirring process until bubbling is uniform, and then adding a binder to obtain a mixed material.
Step 3: and pouring the mixed material into a forming die, and naturally airing and forming to obtain a green body.
And 4, step 4: and putting the green body into a closed box, vacuumizing, then filling butane and oxygen to normal pressure, mixing the butane and the oxygen, filling the mixture into the closed box, filling gas at a flow rate of 7L/min, and keeping standing for 2 hours after filling the gas. After the combustion is finished, naturally cooling to 80 ℃ to obtain a blank with a hole.
And 5: and (3) sintering the blank with the opening at high temperature, heating to 500 ℃ at the speed of 2 ℃/min, preserving the heat for 2h, heating to 1600 ℃ at the speed of 2 ℃/min, keeping the temperature for 2h, and obtaining the zirconia porous ceramic after the sintering at high temperature.
The zirconia foamed ceramic is detected to have a porosity of 80% and a bending strength of 107 MPa.
Example 4
The preparation method of the zirconia porous ceramic of the embodiment comprises the following steps:
step 1: providing the following components in parts by weight: 100 parts of zirconia powder, 35 parts of carbon fiber, 9 parts of foaming agent, 1 part of foam stabilizer, 11 parts of binder and a proper amount of water.
The diameter of the carbon fiber is selected to be 8-15 mu m, and the length is selected to be 6-10 mm.
The zirconia powder is yttria-stabilized zirconia powder with a tetragonal crystal structure, wherein the mass content of zirconia in the zirconia powder is 95%, and the granularity is 0.5-1 mu m.
The foaming agent is alpha-olefin sodium sulfonate.
The foam stabilizer is silicone polyether emulsion.
The adhesive is polyvinyl alcohol, and the mass concentration of the polyvinyl alcohol aqueous solution is 2.5 wt%.
Step 2: putting zirconia powder and carbon fiber into a container, adding a proper amount of water, stirring and mixing, adding a foaming agent and a foam stabilizer in the stirring process until bubbling is uniform, and then adding a binder to obtain a mixed material.
Step 3: and pouring the mixed material into a forming die, and naturally airing and forming to obtain a green body.
And 4, step 4: and putting the green body into a closed box, vacuumizing, then filling butane and oxygen to normal pressure, standing, mixing the butane and the oxygen, filling the mixture into the closed box, filling gas with the flow rate of 10L/min, and standing for 2.5 hours after filling the gas. After the combustion is finished, naturally cooling to 70 ℃ to obtain a blank with a hole.
And 5: and (3) sintering the blank with the opening at high temperature, heating to 600 ℃ at the speed of 1.2 ℃/min, preserving the heat for 1h, heating to 1600 ℃ at the speed of 3 ℃/min, keeping the temperature for 2h, and obtaining the zirconia porous ceramic after the sintering at high temperature.
The zirconia foamed ceramic is detected to have the porosity of 79 percent and the bending strength of 102 MPa.
Example 5
The preparation method of the zirconia porous ceramic of the embodiment comprises the following steps:
step 1: providing the following components in parts by weight: 100 parts of zirconia powder, 40 parts of carbon fiber, 9 parts of foaming agent, 1.5 parts of foam stabilizer, 12 parts of binder and a proper amount of water.
The diameter of the carbon fiber is 12-20 μm, and the length is 7-12 mm.
The zirconia powder is yttria-stabilized zirconia powder with a tetragonal crystal structure, wherein the mass content of zirconia in the zirconia powder is 98%, and the granularity is 0.6-1 mu m.
The foaming agent is linear alkyl benzene sodium sulfonate.
The foam stabilizer is silicone polyether emulsion.
The adhesive is polyvinyl alcohol, and the mass concentration of the polyvinyl alcohol aqueous solution is 2.5 wt%.
Step 2: putting zirconia powder and carbon fiber into a container, adding a proper amount of water, stirring and mixing, adding a foaming agent and a foam stabilizer in the stirring process until bubbling is uniform, and then adding a binder to obtain a mixed material.
Step 3: and pouring the mixed material into a forming die, and naturally airing and forming to obtain a green body.
And 4, step 4: and putting the green body into a closed box, vacuumizing, then filling butane and oxygen to normal pressure, mixing the butane and the oxygen, filling the mixture into the closed box, filling gas at a flow rate of 10L/min, and keeping standing for 3 hours after filling the gas. After the combustion is finished, naturally cooling to 50 ℃ to obtain a blank with a hole.
And 5: and (3) sintering the blank with the opening at high temperature, heating to 750 ℃ at the speed of 1 ℃/min, preserving heat for 1h, heating to 1400 ℃ at the speed of 2 ℃/min, keeping the temperature for 2h, and obtaining the zirconia porous ceramic after the sintering at high temperature.
The zirconia foamed ceramic is detected to have porosity of 77% and bending strength of 99 MPa.
As can be seen from the cases of examples 1 to 5, the porosity of the porous zirconia ceramics prepared by the preparation method of the porous zirconia ceramics of the present invention is more than 70%, the bending strength is more than 90MPa, and the pore diameter is relatively uniform and has no cracking phenomenon through the pore diameter measurement.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the zirconia porous ceramic is characterized by comprising the following steps:
step 1: putting zirconia powder and carbon fiber into a container, adding a proper amount of water, stirring and mixing, adding a foaming agent and a foam stabilizer in the stirring process until bubbling is uniform, and then adding a binder to obtain a mixed material;
step 2: pouring the mixed material into a forming die, and naturally airing and forming to obtain a green body;
and step 3: putting the green body into a closed box, vacuumizing, then filling butane and oxygen to normal pressure, standing for 1.5-3 hours to enable the butane and the oxygen to be uniformly filled into the pores of the green body, igniting by using electronic fire to enable the butane to burn, utilizing the impulsive force of flame to rush open the thin walls of the pores, and obtaining a perforated green body after the burning is finished;
and 4, step 4: and sintering the blank with the opening at high temperature to obtain the zirconia porous ceramic.
2. The preparation method of the zirconia porous ceramic according to claim 1, wherein the zirconia powder, the carbon fiber, the foaming agent, the foam stabilizer and the binder are in the following mass ratio: 100: 15-40: 5-10: 0.1-1.5: 6-12.
3. The method for preparing a zirconia porous ceramic according to claim 1, wherein the carbon fiber has a diameter of 6 to 20 μm and a length of 3 to 12 mm.
4. The method for preparing the zirconia porous ceramic according to claim 1, wherein the zirconia powder has a particle size of 0.2 to 1 μm.
5. The preparation method of the zirconia porous ceramic according to claim 1, wherein the mass content of zirconia in the zirconia powder is not less than 90%.
6. The method of claim 1, wherein the foaming agent is an anionic surfactant.
7. The method of claim 1, wherein the foaming agent is sodium linear alkylbenzene sulfonate, alkyl sulfonate, sodium alpha-olefin sulfonate, alpha-sulfomonocarboxylic acid and its derivatives, fatty acid sulfoalkyl ester, or fatty acid sulfoalkyl amide.
8. The method for preparing zirconia porous ceramic according to claim 1, wherein the foam stabilizer is silicone polyether emulsion.
9. The method of claim 1, wherein the binder is polyvinyl alcohol.
10. The preparation method of the zirconia porous ceramic according to claim 1, wherein the high temperature sintering is performed by heating to 500-750 ℃ at a rate of 0.5-2 ℃/min, and keeping the temperature for 1-2 h, and then heating to 1400-1600 ℃ at a rate of 2-3 ℃/min, and keeping the temperature for 2-4 h.
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