CN110183214B - Porous hollow bowl-shaped alumina powder material and preparation method of alumina ceramic - Google Patents
Porous hollow bowl-shaped alumina powder material and preparation method of alumina ceramic Download PDFInfo
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Abstract
A porous hollow bowl-shaped alumina powder material and a preparation method of alumina ceramic belong to the field of inorganic material preparation. Dispersing hollow bowl-shaped carbon in an aluminum salt solution with a certain concentration by using hollow bowl-shaped carbon powder as a template, stirring for a certain time at normal temperature to enable aluminum ions to permeate into a carbon bowl, and cleaning and drying; transferring the dried powder to a furnace for calcining, heating to a temperature in a protective atmosphere, and preserving heat; directly opening the flange without cooling operation, introducing air, continuously heating and preserving heat, carrying out secondary calcination, and cooling to obtain porous hollow bowl-shaped alumina powder; mixing porous hollow bowl-shaped alumina powder and a sintering aid in proportion to prepare mixed powder: mixing the mixed powder and a binder according to a proportion to prepare a feed; preparing a molded blank body from the feed by adopting an injection molding technology; placing the formed blank body in a degreasing furnace, raising the temperature at a certain heating speed, preserving the temperature and degreasing; and heating and sintering the degreased blank at a certain speed, and preserving heat to prepare the porous alumina ceramic product.
Description
Technical Field
The invention belongs to the technical field of inorganic material preparation, and particularly relates to a porous hollow bowl-shaped alumina powder material and a preparation method of alumina ceramic.
Background
The porous ceramic is an inorganic non-metallic material with a large number of pores (communicated with each other or closed pores) in the material, can be applied to various fields by utilizing the characteristics of higher surface area, material quality and the like, and has wide development prospect. The alumina porous ceramic is an important material in porous ceramic materials, has the characteristics of high hardness, high temperature resistance, corrosion resistance, high electrical insulation, low dielectric loss and the like of alumina, has a high specific surface area in a material body, is low in cost, simple in production process and high in cost performance, is widely applied to various fields of gas and liquid filtration, purification and separation, chemical catalytic carriers, biological implantation materials, sound absorption, shock absorption, sensor materials and the like, and has the advantages of rapidly widening application fields, increasing market demand and very wide prospect. With the continuous progress of the preparation technology of porous ceramics, the application of porous alumina ceramic materials is increasingly wide, and simultaneously, higher requirements on the performance of the porous alumina ceramic materials are also provided. Different preparation methods have limitations, the prepared porous alumina ceramics have different structures and performances, and raw material powders with different shapes and sizes can also generate larger influence on the pore structures of the ceramics, so that the preparation method of the porous alumina ceramics is imperative to widen.
In view of the above, the method described in the patent (201910032940.1) is used to prepare a hydrothermal carbon hollow bowl material, then the hollow bowl carbon material is used as a template, aluminum salt is used as an aluminum source, aluminum ions are made to penetrate into the carbon bowl in a liquid phase medium, and the porous hollow bowl-shaped alumina material is obtained by calcining, and is used as a raw material to prepare the porous alumina ceramic by an injection molding process.
Disclosure of Invention
The invention aims to prepare a porous hollow bowl-shaped alumina powder material and prepare porous alumina ceramics by adopting an injection molding process.
A preparation method of a porous hollow bowl-shaped alumina powder material and alumina ceramic is characterized by comprising the following preparation steps:
1) preparing hydrothermal carbon hollow bowl-shaped carbon powder;
2) dispersing the hollow bowl-shaped carbon in an aluminum salt solution with a certain concentration, stirring for a certain time at normal temperature to enable aluminum ions to permeate into the carbon bowl, and cleaning and drying;
3) transferring the dried powder to a furnace for calcining, heating to a certain temperature in a protective atmosphere, and keeping the temperature for a certain time;
4) directly opening the flange without cooling, introducing air, continuously heating to a certain temperature, preserving the temperature for a period of time, carrying out secondary calcination, and cooling to obtain porous hollow bowl-shaped alumina powder;
5) preparing a mixed powder: mixing porous hollow bowl-shaped alumina powder and sintering aid according to a certain proportion, drying and sieving to obtain mixed powder
6) Preparing a feed: mixing the mixed powder and a binder according to a certain proportion to prepare a feed;
7) injection molding: preparing a molded blank body from the feed by adopting an injection molding technology;
8) degreasing: placing the formed blank body in a degreasing furnace, heating to a certain temperature at a certain heating speed, and preserving heat for a period of time for degreasing;
9) and heating the degreased blank to a certain temperature at a certain speed for sintering, and preserving the heat for a period of time to prepare the porous alumina ceramic product.
Further, the step 1) of preparing the hydrothermal carbonaceous hollow bowl-shaped carbon powder comprises the following steps:
a. raw materials: comprises a carbon source, a solvent and a soft template agent; the carbon source is biological raw material and waste material; the biological raw materials comprise apples, pears, grapes, peaches, litchis and sugarcanes, the biological waste materials comprise residual apple seeds, pear seeds and fruit peels thereof, grape fruit peels, bagasse, rotten apples, pears, grapes, peaches, litchis, sugarcanes and the like which can not be eaten by people; the soft template agent is formed by anionic surfactant and nonionic surfactant together, and the solvent is deionized water;
b. juicing biological raw materials or waste materials, filtering and washing to finally obtain clear juice;
c. preparing a precursor solution: respectively dissolving two surfactants in deionized water to form a solution, then mixing the solution with the biological raw material or the waste juice, and uniformly stirring;
d. hydrothermal carbonization: putting the mixed solution into a hydrothermal reaction kettle, and keeping the temperature at 50-250 ℃ for 0.5-80 hours;
e. and (4) taking out the reaction kettle, cooling to room temperature, opening the container, pouring out the precipitate, and repeatedly washing with water and alcohol for multiple times to obtain the product.
Further, the aluminum salt in the step 2) comprises aluminum nitrate, aluminum chloride, aluminum acetate, aluminum sulfate, aluminum silicate and the like and hydrates thereof, and one or more of the aluminum nitrate, the aluminum chloride, the aluminum acetate, the aluminum sulfate, the aluminum silicate and the like are taken as raw materials; the solvent includes one or more of water, ethanol, acetone, methanol, formamide, tetrahydrofuran, etc.
Further, the heat preservation temperature in the step 3) is 50-500 ℃, and the heat preservation time is 0.5-30 hours.
Further, the heat preservation temperature in the step 4) is 400-800 ℃, and the heat preservation time is 0.5-30 hours.
Further, the proportion of the sintering aid in the step 5) to the porous hollow bowl-shaped alumina powder is 0.1-20%, and the sintering aid comprises one or more of lanthanum oxide, yttrium oxide, cerium oxide and calcium fluoride.
Further, the adhesive in the step 6) comprises the following components in parts by weight: 6-8 parts of paraffin, 1-2 parts of polyethylene, 1-3 parts of polypropylene and 0.5-1.5 parts of stearic acid; the ratio of the mixed powder to the binder is in the range of 1-1.5: 1.
Further, the temperature rise speed in the step 8) is in the range of 1.5-2 ℃/min; the heat preservation temperature is 400-600 ℃; the heat preservation time is 2-3 h.
Further, the temperature rise speed in the step 9) is in the range of 2-4 ℃/min; the heat preservation temperature is 1000-1700 ℃; the heat preservation time is 1-10 h.
The material obtained by the invention is particles of a hollow bowl-shaped structure of alumina, inherits the shape of a carbon template, has a hollow structure inside and is in a concave bowl shape, has high dispersibility, narrow particle size distribution and uniform and controllable particle size, and the bowl-shaped structure is favorable for regulating and controlling the tap density of powder so as to regulate the porosity and the pore structure of the porous alumina ceramic.
The obtained material is porous alumina ceramic with controllable pore structure, the material takes porous hollow bowl-shaped alumina powder as a raw material, and the purpose of adjusting the porosity and the pore structure of the ceramic is achieved by regulating and controlling the size and the shape of an inner cavity of the raw material powder and assisting a sintering aid and a sintering process.
Detailed Description
Example 1
Uniformly mixing 24g of deionized water solution containing 5g of anhydrous glucose, 3g of sodium oleate solution (2mmol/L) and 3g of P123 solution (0.125mmol/L), transferring the mixture into a 50ml of stainless steel water heating tank with a polytetrafluoroethylene lining, screwing a cover, putting the water heating tank into a 160 ℃ oven, keeping the temperature for 12 hours, taking out the water heating tank for air cooling, washing the precipitate with anhydrous ethanol, drying, and preparing a plurality of batches for later use; dispersing 5g of carbon bowls in 3mol/L aluminum nitrate aqueous solution, stirring for a certain time, cleaning and drying, transferring dried powder to a tubular furnace for calcination, heating to 350 ℃ in a nitrogen atmosphere, preserving heat for 2 hours, opening a flange, introducing air, continuously heating to 600 ℃, preserving heat for 2 hours to obtain a porous bowl-shaped alumina material, cooling, collecting powder, and preparing for later use in multiple batches; weighing 200g of porous bowl-shaped alumina material and 10g of sintering aid yttrium oxide, ball-milling and mixing in alcohol, drying and sieving to obtain mixed powder, preparing 105g of binder according to 6 parts by weight of paraffin, 1 part by weight of polyethylene, 2 parts by weight of polypropylene and 1 part by weight of stearic acid, mixing the mixed powder and the binder to prepare a feed, crushing the feed, molding by using an injection machine to prepare a molded blank, degreasing the molded blank in a degreasing furnace at a temperature of 2 ℃/min to 500 ℃, placing the degreased blank in a crucible, transferring to a high-temperature furnace, sintering at a temperature of 4 ℃/min to 1500 ℃, and preserving heat for 8 hours to obtain the porous alumina ceramic product.
Example 2
Uniformly mixing 24g of deionized water solution containing 5g of fructose, 3g of sodium oleate solution (2mmol/L) and 3g of P123 solution (0.125mmol/L), transferring the mixture into a 50ml of stainless steel water heating tank with a polytetrafluoroethylene lining, screwing a cover, putting the water heating tank into a 130 ℃ oven, keeping the temperature for 12 hours, taking out the mixture for air cooling, washing the precipitate with absolute ethyl alcohol, drying, and preparing for later use in multiple batches; dispersing 5g of carbon bowls in 3mol/L aluminum nitrate aqueous solution, stirring for a certain time, cleaning and drying, transferring dried powder to a tubular furnace for calcination, heating to 320 ℃ in a nitrogen atmosphere, preserving heat for 3 hours, opening a flange, introducing air, continuously heating to 650 ℃, preserving heat for 3 hours to obtain a porous bowl-shaped alumina material, cooling, collecting powder, and preparing for later use in multiple batches; weighing 400g of porous bowl-shaped alumina material and 30g of sintering aid yttrium oxide, ball-milling and mixing in alcohol, drying and sieving to obtain mixed powder, preparing 105g of binder according to 7 parts by weight of paraffin, 1.5 parts by weight of polyethylene, 2.5 parts by weight of polypropylene and 1 part by weight of stearic acid, mixing the mixed powder and the binder to prepare a feed, crushing the feed, forming by using an injection machine, degreasing the formed blank by placing the formed blank in a degreasing furnace at the temperature of 2 ℃/min to 500 ℃, placing the degreased blank in a crucible, transferring to a high-temperature furnace, sintering at the temperature of 3 ℃/min to 1500 ℃, and preserving heat for 8 hours to obtain the porous alumina ceramic product.
Claims (7)
1. The preparation method of the alumina ceramic is characterized by comprising the following preparation steps:
1) preparing hydrothermal carbon hollow bowl-shaped carbon powder;
2) dispersing the hollow bowl-shaped carbon in an aluminum salt solution with a certain concentration, stirring for a certain time at normal temperature to enable aluminum ions to permeate into the carbon bowl, and cleaning and drying;
3) transferring the dried powder to a furnace for calcining, heating to a certain temperature in a protective atmosphere, and keeping the temperature for a certain time;
4) directly opening the flange without cooling, introducing air, continuously heating to a certain temperature, preserving the temperature for a period of time, carrying out secondary calcination, and cooling to obtain porous hollow bowl-shaped alumina powder;
5) preparing a mixed powder: mixing the porous hollow bowl-shaped alumina powder and the sintering aid according to a certain proportion, drying and sieving to obtain mixed powder;
6) preparing a feed: mixing the mixed powder and a binder according to a certain proportion to prepare a feed;
7) injection molding: preparing a molded blank body from the feed by adopting an injection molding technology;
8) degreasing: placing the formed blank body in a degreasing furnace, heating to a certain temperature at a certain heating speed, and preserving heat for a period of time for degreasing;
9) heating the degreased blank at a certain speed to a certain temperature for sintering, and keeping the temperature for a period of time to prepare a porous alumina ceramic product;
step 3), the heat preservation temperature is 50-500 ℃, and the heat preservation time is 0.5-30 hours;
and 4) the heat preservation temperature is 400-.
2. The method for preparing alumina ceramics according to claim 1, wherein the step 1) of preparing the hydrothermal carbonaceous hollow bowl-shaped carbon powder comprises the following steps:
a. raw materials: comprises a carbon source, a solvent and a soft template agent; the carbon source is biological raw material and waste material; the biological raw materials comprise apples, pears, grapes, peaches, litchis and sugarcanes, the biological waste materials comprise residual apple seeds, pear seeds and fruit peels thereof, grape fruit peels, bagasse, and rotten apples, pears, grapes, peaches, litchis and sugarcanes which can not be eaten by people; the soft template agent is formed by anionic surfactant and nonionic surfactant together, and the solvent is deionized water;
b. juicing biological raw materials or waste materials, filtering and washing to finally obtain clear juice;
c. preparing a precursor solution: respectively dissolving two surfactants in deionized water to form a solution, then mixing the solution with the biological raw material or the waste juice, and uniformly stirring;
d. hydrothermal carbonization: putting the mixed solution into a hydrothermal reaction kettle, and keeping the temperature at 50-250 ℃ for 0.5-80 hours;
e. and (4) taking out the reaction kettle, cooling to room temperature, opening the container, pouring out the precipitate, and repeatedly washing with water and alcohol for multiple times to obtain the product.
3. The method of claim 1, wherein the aluminum salt in the step 2) comprises one or more of aluminum nitrate, aluminum chloride, aluminum acetate, aluminum sulfate, aluminum silicate and hydrates thereof as a raw material; the solvent comprises one or more of water, ethanol, acetone, methanol, formamide and tetrahydrofuran.
4. The method according to claim 1, wherein the ratio of the sintering aid in step 5) to the porous hollow bowl-shaped alumina powder is 0.1-20%, and the sintering aid comprises one or more of lanthanum oxide, yttrium oxide, cerium oxide, and calcium fluoride.
5. The method for preparing the alumina ceramic according to claim 1, wherein the binder in the step 6) comprises the following components in parts by weight: 6-8 parts of paraffin, 1-2 parts of polyethylene, 1-3 parts of polypropylene and 0.5-1.5 parts of stearic acid; the ratio of the mixed powder to the binder is in the range of 1-1.5: 1.
6. The method for preparing alumina ceramic according to claim 1, wherein the temperature rise rate in step 8) is in the range of 1.5 to 2 ℃/min; the heat preservation temperature is 400-600 ℃; the heat preservation time is 2-3 h.
7. The method according to claim 1, wherein the temperature rise rate in the step 9) is in the range of 2 to 4 ℃/min; the heat preservation temperature is 1000-1700 ℃; the heat preservation time is 1-10 h.
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| CN113233917A (en) * | 2021-05-28 | 2021-08-10 | 武汉科技大学 | Nano core-shell structure pore-forming agent and preparation method thereof |
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