CN112624793A - Preparation method of alumina-based porous ceramic material - Google Patents
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Abstract
The invention relates to a preparation method of a porous ceramic material, in particular to a preparation method of an alumina-based porous ceramic material, which comprises the following steps in percentage by weight: preparing raw materials: in the raw materials, the content of alumina powder is 35-50%, the content of a binder is 2-6%, the content of a sintering aid is 0.5-2%, the content of a pore-forming agent is 42-65%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is CaO and ZrO2The pore-forming agent is superfine polymethyl methacrylate powder; ball milling mixerPressing the mixture into a blank, sintering and cooling to obtain the alumina-based porous ceramic material. The alumina-based porous ceramic material obtained by adopting a proper preparation process has the advantages of low sintering temperature, simple process, low cost, high porosity and good toughness.
Description
Technical Field
The invention relates to a preparation method of a porous ceramic material, in particular to a preparation method of an alumina-based porous ceramic material.
Background
The porous ceramic material has the excellent properties of a ceramic matrix, large porosity, adjustable pore diameter, pore distribution and the like, and excellent electrical, thermal, magnetic and other properties.
The alumina-based porous ceramic material is a porous ceramic material with the widest application field, has good heat resistance, excellent chemical stability and higher hardness, is commonly used for filtering molten metal, can be used as a sensor material, and can also be used as a sound absorption material, a refractory material, a heat exchanger and the like. However, when the alumina porous ceramic is prepared, the sintering temperature is high, which leads to increased energy consumption and increased cost, and the alumina porous ceramic material has low corresponding strength when the porosity is high, which are difficult to obtain, and the fracture toughness of the alumina porous ceramic is still to be improved.
At present, in order to prepare a ceramic material with low cost and high porosity, in patent document 1(CN103232228A), diatomite is used as a pore-forming agent to produce a ceramic material with high porosity, but the sintering temperature is not reduced, and the overall performance is not satisfactory. Patent document 2(CN104130004A) has good flexural strength, but the production process is complicated, the porosity is not high, the toughness is also poor, and there is room for further improvement.
Disclosure of Invention
In view of the problems of the prior art, an object of the present invention is to provide a method for producing an alumina-based porous ceramic material having high porosity and excellent toughness.
In order to achieve the purpose, the invention adopts the following technical scheme: the preparation method of the alumina-based porous ceramic material is characterized by comprising the following steps:
(1) preparing raw materials: in the raw materials, the content of alumina powder is 35-50% by mass, the content of a binder is 2-6%, the content of a sintering aid is 0.5-2%, the content of a pore-forming agent is 42-65%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is prepared from CaO and ZrO2The pore-forming agent is superfine polymethyl methacrylate powder;
(2) weighing the components according to the mass percentage, mixing the alumina powder, the sintering aid and the binder, performing ball milling, and drying a first mixture obtained after ball milling to obtain a second mixture;
(3) mixing the second mixture with a pore-forming agent to obtain a third mixture;
(4) pressing the third mixture into a blank, and drying the blank to obtain a blank body;
(5) placing the blank body into a sintering furnace, wherein the sintering temperature is 1050-;
(6) cooling to room temperature, and taking out the blank to obtain the alumina-based porous ceramic material.
Preferably, the mass percentage of the alumina powder is 40-45%.
Preferably, the particle size of the alumina powder is 20 to 200 nm.
Preferably, the particle size of the ultrafine polymethylmethacrylate powder is 10 to 80um, further 15 to 75 μm, and further 20 to 70 μm.
Preferably, the sintering aid is 1-1.5% by mass.
Preferably, CaO and ZrO in the sintering aid2The mass ratio of (A) to (B) is 2: (2-4).
Preferably, the sintering temperature is 1100-1160 ℃, and the holding time is 1-2 h.
The lower grain diameter of the alumina powder can improve the surface free energy and reduce the sintering temperature, and after the grain diameter is lower than 20nm, the lower grain diameter does not continue to obviously reduce the sintering temperature, and the grain diameter of the alumina powder between 20nm and 200nm can achieve the required purpose.
Selecting CaO and ZrO2The mixture is used as a sintering aid, so that the sintering temperature of the alumina can be reduced, the energy consumption is saved, and the cost is reduced. CaO, ZrO2And the crystal grains can be refined, and the toughness of the alumina-based porous ceramic material is improved. When CaO and ZrO2The mass ratio of (A) to (B) is 2: (2-4), the toughness is best, and the porosity is high, probably because of CaO and ZrO during high-temperature sintering2Eutectic compound is generated with raw materials such as alumina, the expansion of alumina grain boundary is limited, and the improvement of the porosity of the alumina-based porous ceramic material is promoted.
The sintering temperature is too high, so that mass transfer among particles is intensified, and the porosity of the ceramic is reduced, but the porosity is not linearly reduced along with the reduction of the sintering temperature, but is higher between 1100-1160 ℃. The bending strength can be improved by increasing the sintering temperature, but the improvement is not obvious after 1160 ℃, and the performance of the ceramic is not influenced by overhigh sintering temperature and overlong sintering time.
Porosity was measured according to GB1966-1996, flexural strength according to GB/T4741-1999, fracture toughness according to GBT 23806-2009. Tests show that the finished product has a porosity of 60-75%, a bending strength of 90-125MPa and a fracture toughness of 2.3-3.2 MPa.m1/2In addition, the method has the advantages of low sintering temperature, simple process, low cost, high porosity and good toughness.
The invention has the beneficial effects that:
1. the preparation method of the alumina-based porous ceramic material provided by the invention controls the particle size of alumina powder and selects CaO and ZrO2As a sintering aid, the sintering temperature of the alumina ceramic material is reduced, the cost is reduced, and the toughness of the alumina-based porous ceramic material is improved.
2. The preparation process is simple, and the prepared alumina-based porous ceramic material has high porosity and good toughness. Tests show that the finished product has a porosity of 60-75%, a bending strength of 90-125MPa and a fracture toughness of 2.3-3.2 MPa.m1/2And the comprehensive performance is good and superior to that of patent documents 1 and 2, and the application prospect is wide.
Detailed Description
The present invention will be described in further detail with reference to the following examples. The specific embodiments are to be considered as illustrative and not restrictive in character.
Embodiment 1, a method for preparing an alumina-based porous ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of alumina powder is 35%, the content of a binder is 6%, the content of a sintering aid is 2%, the content of a pore-forming agent is 57%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is prepared from CaO and ZrO2Composition of CaO and ZrO in sintering aid2The mass ratio of (A) to (B) is 2: 1; the pore-forming agent is superfine polymethyl methacrylatePulverizing; the grain diameter of the alumina powder is 200 nm; the particle size of the superfine polymethyl methacrylate powder is 10 um;
(2) weighing the components according to the mass percentage, mixing the alumina powder, the sintering aid and the binder, performing ball milling, and drying a first mixture obtained after ball milling to obtain a second mixture;
(3) mixing the second mixture with a pore-forming agent to obtain a third mixture;
(4) pressing the third mixture into a blank, and drying the blank to obtain a blank body;
(5) placing the blank into a sintering furnace, wherein the sintering temperature is 1250 ℃, and the heat preservation time is 1 h;
(6) cooling to room temperature, and taking out the blank to obtain the alumina-based porous ceramic material.
Embodiment 2, a method for preparing an alumina-based porous ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of alumina powder is 50%, the content of a binder is 2%, the content of a sintering aid is 0.5%, the content of a pore-forming agent is 47.5%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is prepared from CaO and ZrO2Composition of CaO and ZrO in sintering aid2The mass ratio of (1): 3; the pore-forming agent is superfine polymethyl methacrylate powder; the grain diameter of the alumina powder is 20 nm; the particle size of the superfine polymethyl methacrylate powder is 80 um;
(2) weighing the components according to the mass percentage, mixing the alumina powder, the sintering aid and the binder, performing ball milling, and drying a first mixture obtained after ball milling to obtain a second mixture;
(3) mixing the second mixture with a pore-forming agent to obtain a third mixture;
(4) pressing the third mixture into a blank, and drying the blank to obtain a blank body;
(5) placing the blank into a sintering furnace, wherein the sintering temperature is 1050 ℃, and the heat preservation time is 3 hours;
(6) cooling to room temperature, and taking out the blank to obtain the alumina-based porous ceramic material.
Embodiment 3, a method for preparing an alumina-based porous ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of alumina powder is 45%, the content of a binder is 6%, the content of a sintering aid is 1%, the content of a pore-forming agent is 48%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is prepared from CaO and ZrO2Composition of CaO and ZrO in sintering aid2The mass ratio of (A) to (B) is 2: 1; the pore-forming agent is superfine polymethyl methacrylate powder; the grain diameter of the alumina powder is 200 nm; the particle size of the superfine polymethyl methacrylate powder is 10 um;
(2) weighing the components according to the mass percentage, mixing the alumina powder, the sintering aid and the binder, performing ball milling, and drying a first mixture obtained after ball milling to obtain a second mixture;
(3) mixing the second mixture with a pore-forming agent to obtain a third mixture;
(4) pressing the third mixture into a blank, and drying the blank to obtain a blank body;
(5) placing the blank into a sintering furnace, wherein the sintering temperature is 1250 ℃, and the heat preservation time is 1 h;
(6) cooling to room temperature, and taking out the blank to obtain the alumina-based porous ceramic material.
Embodiment 4, a method for preparing an alumina-based porous ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of alumina powder is 45%, the content of a binder is 6%, the content of a sintering aid is 1%, the content of a pore-forming agent is 48%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is prepared from CaO and ZrO2Composition of CaO and ZrO in sintering aid2The mass ratio of (A) to (B) is 2: 3; the pore-forming agent is superfine polymethyl methacrylate powder; the grain diameter of the alumina powder is 200 nm; the particle size of the superfine polymethyl methacrylate powder is 10 um;
(2) weighing the components according to the mass percentage, mixing the alumina powder, the sintering aid and the binder, performing ball milling, and drying a first mixture obtained after ball milling to obtain a second mixture;
(3) mixing the second mixture with a pore-forming agent to obtain a third mixture;
(4) pressing the third mixture into a blank, and drying the blank to obtain a blank body;
(5) placing the blank into a sintering furnace, wherein the sintering temperature is 1250 ℃, and the heat preservation time is 1 h;
(6) cooling to room temperature, and taking out the blank to obtain the alumina-based porous ceramic material.
Embodiment 5, a method for preparing an alumina-based porous ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of alumina powder is 45%, the content of a binder is 6%, the content of a sintering aid is 1%, the content of a pore-forming agent is 48%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is prepared from CaO and ZrO2Composition of CaO and ZrO in sintering aid2The mass ratio of (A) to (B) is 2: 3; the pore-forming agent is superfine polymethyl methacrylate powder; the grain diameter of the alumina powder is 200 nm; the particle size of the superfine polymethyl methacrylate powder is 10 um;
(2) weighing the components according to the mass percentage, mixing the alumina powder, the sintering aid and the binder, performing ball milling, and drying a first mixture obtained after ball milling to obtain a second mixture;
(3) mixing the second mixture with a pore-forming agent to obtain a third mixture;
(4) pressing the third mixture into a blank, and drying the blank to obtain a blank body;
(5) placing the green body into a sintering furnace, wherein the sintering temperature is 1160 ℃, and the heat preservation time is 1 h;
(6) cooling to room temperature, and taking out the blank to obtain the alumina-based porous ceramic material.
Comparative example 1, a method for preparing an alumina-based porous ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of alumina powder is 35%, the content of a binder is 6%, the content of a sintering aid is 2%, the content of a pore-forming agent is 57%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is MgO and ZrO2Composition of MgO and ZrO in sintering aid2The mass ratio of (A) to (B) is 2: 1; the pore-forming agent is superfine polymethyl methacrylate powder; the grain diameter of the alumina powder is 200 nm; the particle size of the superfine polymethyl methacrylate powder is 10 um;
(2) weighing the components according to the mass percentage, mixing the alumina powder, the sintering aid and the binder, performing ball milling, and drying a first mixture obtained after ball milling to obtain a second mixture;
(3) mixing the second mixture with a pore-forming agent to obtain a third mixture;
(4) pressing the third mixture into a blank, and drying the blank to obtain a blank body;
(5) placing the blank into a sintering furnace, wherein the sintering temperature is 1250 ℃, and the heat preservation time is 1 h;
(6) cooling to room temperature, and taking out the blank to obtain the alumina-based porous ceramic material.
Comparative example 2, a method for preparing an alumina-based porous ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of alumina powder is 35%, the content of a binder is 6%, the content of a sintering aid is 8%, the content of a pore-forming agent is 51%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is prepared from CaO and ZrO2Composition of CaO and ZrO in sintering aid2The mass ratio of (A) to (B) is 2: 1; the pore-forming agent is superfine polymethyl methacrylate powder; the grain diameter of the alumina powder is 500 nm; the particle size of the superfine polymethyl methacrylate powder is 10 um;
(2) weighing the components according to the mass percentage, mixing the alumina powder, the sintering aid and the binder, performing ball milling, and drying a first mixture obtained after ball milling to obtain a second mixture;
(3) mixing the second mixture with a pore-forming agent to obtain a third mixture;
(4) pressing the third mixture into a blank, and drying the blank to obtain a blank body;
(5) placing the blank into a sintering furnace, wherein the sintering temperature is 1550 ℃, and the heat preservation time is 4 hours;
(6) cooling to room temperature, and taking out the blank to obtain the alumina-based porous ceramic material.
The invention performs a performance test on examples 1-5 and comparative examples 1-2, measuring porosity according to GB1966-1996, bending strength according to GB/T4741-1999, and fracture toughness according to GBT23806-2009, with the test performance shown in Table 1.
TABLE 1 test Properties of alumina-based porous ceramic materials
| Finished product | Porosity/% | Flexural strength/MPa | Fracture toughness/MPa.m1/2) |
| Example 1 | 65 | 90 | 2.5 |
| Example 2 | 60 | 97 | 2.3 |
| Example 3 | 69 | 103 | 2.6 |
| Example 4 | 72 | 112 | 2.9 |
| Example 5 | 75 | 125 | 3.2 |
| Comparative example 1 | 52 | 73 | 1.8 |
| Comparative example 2 | 53 | 74 | 1.6 |
From table 1, it can be seen that: by selecting proper sintering aids CaO and ZrO2Can ensure the porosity, bending strength, fracture toughness and other properties of the alumina-based porous ceramic material. Preferably, appropriate CaO, ZrO are determined2The quality ratio of the ceramic material is more excellent than that of the obtained ceramic material. The porosity of the prepared alumina-based porous ceramic material is between 60 and 75 percent, the bending strength is between 90 and 125MPa, and the fracture toughness is between 2.3 percent-3.2MPa·m1/2In addition, the method has the advantages of low sintering temperature, simple process, low cost, high porosity and good toughness.
The foregoing examples are set forth to illustrate the present invention more clearly and should not be construed as limiting the scope of the present invention, which is intended to be limited thereby, and all such changes and modifications that can be made without departing from the scope of the present invention are intended to be within the scope of the present invention.
Claims (9)
1. The preparation method of the alumina-based porous ceramic material is characterized by comprising the following steps:
(1) preparing raw materials: in the raw materials, the content of alumina powder is 35-50% by mass, the content of a binder is 2-6%, the content of a sintering aid is 0.5-2%, the content of a pore-forming agent is 42-65%, and the sum of the mass percentages of the components is 100%, wherein the binder is phenolic resin, and the sintering aid is prepared from CaO and ZrO2The pore-forming agent is superfine polymethyl methacrylate powder;
(2) weighing the components according to the mass percentage, mixing the alumina powder, the sintering aid and the binder, performing ball milling, and drying a first mixture obtained after ball milling to obtain a second mixture;
(3) mixing the second mixture with a pore-forming agent to obtain a third mixture;
(4) pressing the third mixture into a blank, and drying the blank to obtain a blank body;
(5) placing the blank body into a sintering furnace, wherein the sintering temperature is 1050-;
(6) cooling to room temperature, and taking out the blank to obtain the alumina-based porous ceramic material.
2. The method for preparing the alumina-based porous ceramic material according to claim 1, wherein the mass percentage of the alumina powder is 40-45%.
3. The method for preparing an alumina-based porous ceramic material according to claim 1 or 2, wherein the particle size of the ultrafine polymethylmethacrylate powder is 10 to 80 um.
4. The method for preparing an alumina-based porous ceramic material according to claim 1 or 2, wherein the particle size of the alumina powder is 20 to 200 nm.
5. The method for producing an alumina-based porous ceramic material according to claim 1 or 2, wherein the content of the sintering aid in the raw material is 1 to 1.5% by mass.
6. The method for preparing alumina-based porous ceramic material according to claim 1 or 2, wherein CaO and ZrO are contained in the sintering aid2The mass ratio of (A) to (B) is 2: (2-4).
7. The method for preparing the alumina-based porous ceramic material as claimed in claim 1 or 2, wherein the sintering temperature is 1100-1160 ℃ and the holding time is 1-2 h.
8. The method for preparing an alumina-based porous ceramic material according to any one of claims 1 to 7, wherein the particle size of the ultrafine polymethylmethacrylate powder is 15 to 75 μm.
9. The method for preparing an alumina-based porous ceramic material according to any one of claims 1 to 8, wherein the particle size of the ultrafine polymethylmethacrylate powder is 20-70 μm.
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| CN114195548A (en) * | 2021-12-30 | 2022-03-18 | 中国工程物理研究院电子工程研究所 | Preparation method of light electric porcelain and light electric porcelain |
| CN114853499A (en) * | 2022-03-31 | 2022-08-05 | 山东大学 | Corundum powder based ultra-low heat conduction foam ceramic material and preparation method thereof |
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