CN115745618A - Method for improving mechanical strength of porous silicon carbide film - Google Patents
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- CN115745618A CN115745618A CN202211452696.2A CN202211452696A CN115745618A CN 115745618 A CN115745618 A CN 115745618A CN 202211452696 A CN202211452696 A CN 202211452696A CN 115745618 A CN115745618 A CN 115745618A
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Abstract
The invention discloses a method for improving the mechanical strength of a porous silicon carbide film. According to the invention, a proper amount of large particles are introduced into the small-particle silicon carbide particle aggregate, so that the bending strength of the porous silicon carbide film is increased. Compared with the porous silicon carbide film prepared by using the silicon carbide powder with smaller average grain size, the prepared porous silicon carbide film has the advantages of obviously improved mechanical strength and equivalent average pore size, and can effectively prolong the service life of the ceramic film. The method for improving the mechanical strength of the porous silicon carbide film is simple in process, the material is high in mechanical strength, and the method can be well suitable for cleaning pollution of ceramic films by using chemical cleaning reagents in industry; meanwhile, the high-strength silicon carbide ceramic membrane has long service life and has good application prospect in the field of oil-water separation.
Description
Technical Field
The invention belongs to the technical field of porous ceramic material preparation, and relates to a method for improving the mechanical strength of a porous silicon carbide film.
Background
The membrane separation technology has been widely used in the fields of sewage treatment, high-temperature flue gas purification and the like due to the characteristics of low energy consumption, high efficiency and the like. The ceramic membrane has excellent mechanical, chemical and thermal stability, can basically keep stable in high-temperature, strong acid and strong alkali environments, and has higher flux and anti-pollution capability in water treatment. In addition, under extreme environmental conditions, after contamination, chemical cleaning can be carried out to restore their performance, a property which makes them useful for long-term industrial applications. Among a plurality of ceramic membranes, the silicon carbide (SiC) ceramic membrane has incomparable advantages of other membrane materials in harsh environments such as sewage treatment, high-temperature flue gas purification and the like due to low thermal expansion coefficient, high thermal shock resistance, excellent hydrophilicity and surface electronegativity.
The mechanical strength of the ceramic membrane is the basis for determining the service performance and the service life of the ceramic membrane, and different methods are invented by scholars at home and abroad for improving the strength of the ceramic membrane. For example, chinese patent CN109336632a reports a method for preparing glass fiber reinforced quartz ceramic. In addition, the preparation of the high-strength ceramic membrane can be realized by selecting a proper low-temperature sintering aid and optimizing the content. For example, in the chinese invention patents CN105884394a and CN107082628a, the porous silicon carbide ceramic membrane support with good permeability and mechanical strength is successfully prepared by respectively introducing organic/inorganic composite auxiliary agents and molecular sieve membrane synthesis residual liquid in the preparation process of porous silicon carbide. It can be seen that the introduction of the fiber material and the sintering aid is a common method for enhancing the strength of the porous silicon carbide ceramic membrane.
In addition, considering that the small particles have a large specific surface area and a high sintering activity, many neck connections are formed between the particles under high temperature conditions, and the bending strength is also high. In order to improve the strength of the porous ceramic membrane material, the Chinese patent CN111533572A reports a preparation method of a porous silicon carbide ceramic support body, firstlyTaking mixed silicon carbide powder, silicon dioxide powder, a foaming agent, a dispersing agent and thermosetting polymer emulsion as main raw materials, uniformly mixing to obtain high-solid silicon carbide slurry, and then pouring and pressureless sintering to form the high-solid silicon carbide slurry; the mixed silicon carbide powder is prepared by introducing a small amount of small-size silicon carbide particles (3.0 to 5.0 micrometers) into a matrix of large-size silicon carbide particles (6.5 to 9.5 micrometers) and mixing. The porous silicon carbide support prepared by the method has the advantages of high strength, high temperature resistance, acid and alkali corrosion resistance and the like. Recently, wei Wei et al (Sep Purif Technol 2022, 302, 122075) significantly improves the mechanical strength of porous silicon carbide ceramic filters by incorporating small amounts of small sized silicon carbide particles into large sized silicon carbide particles.
Disclosure of Invention
The invention aims to improve the mechanical strength of a porous silicon carbide film so as to meet the use requirements of different fields. Different from the method disclosed and reported in the publication, the invention proposes to increase the bending strength of the porous silicon carbide film by introducing a proper amount of large particles into small-particle silicon carbide particle aggregates. The method can improve the strength of the porous silicon carbide film, can obtain the silicon carbide film with smaller aperture, and realizes the preparation of the silicon carbide film with high strength and high separation precision.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
(1) Adding a small amount of silicon carbide powder with larger size into the small-size silicon carbide powder, wherein the proportion of the silicon carbide powder with the average grain diameter of 0.1-5 mu m in the total mass of the silicon carbide is 70-90%, and the proportion of the silicon carbide powder with the average grain diameter of 10-50 mu m in the total mass of the silicon carbide is 10-30%;
(2) Mixing the silicon carbide ceramic powder with the two sizes and a sintering aid NaA molecular sieve according to a certain proportion, wherein the grinding time is 20 minutes;
(3) Adding a certain amount of polyvinyl alcohol (PVA) solution and water into the silicon carbide powder obtained in the step (2) and continuously mixing uniformly, wherein the final state of the powder is free from caking;
(4) Pressing the silicon carbide powder obtained in the step (3) into a sheet or strip blank by a tablet press under the pressure of 5-10 MPa;
(5) Drying the blank at 25 ℃ for 8 h, and then drying in an oven at 80-120 ℃ for 1 h;
(6) And (3) placing the dried blank into a muffle furnace for sintering, heating to 500 ℃ at the speed of 1 ℃/min, preserving heat for 3 h, then heating to 1000 to 1300 ℃ at the speed of 1 ℃/min, preserving heat for 3 h, and finally cooling to room temperature along with the furnace.
Preferably, the mass of the NaA molecular sieve added in the step (2) is 10 to 20 percent of the mass of the silicon carbide powder.
Preferably, the concentration of the PVA solution added in the step (3) is 5-10%, the adding amount of the PVA solution is 2-10% of the mass of the silicon carbide powder in the step (1), and the adding amount of the water is 1~5% of the mass of the silicon carbide powder in the step (1).
Preferably, 2 to 3 g of the uniformly mixed powder in the step (4) is weighed, and the mixed powder is pressed into a green body of a sheet (Φ 30 mm × 3 mm) and a strip (50 mm × 6 mm × 6 mm) by a tablet press under 5 to 10 MPa.
The silicon carbide powder can be non-oxide ceramic powder such as silicon nitride, titanium carbide and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, a small amount of large-size silicon carbide particles are doped in small-size silicon carbide particles to prepare the porous silicon carbide film, the aperture of the porous silicon carbide film is equivalent to that of the porous silicon carbide film prepared by using the small-size silicon carbide particles as raw materials, and the mechanical strength can be improved by regulating and controlling the content of the large-size silicon carbide particles;
2. according to the invention, the large-size silicon carbide particles are introduced into the small-size silicon carbide particles, and the large-size silicon carbide particles and the small-size silicon carbide particles belong to the same substance, so that the negative influence of the introduction of a second heterogeneous phase on the chemical uniformity and stability of the porous ceramic membrane can be avoided;
3. the cost of the small-size silicon carbide particles is higher than that of the large-size silicon carbide particles, so that the reduction of the use of part of the small-size silicon carbide particles is beneficial to reducing the preparation cost and large-scale preparation.
Drawings
Fig. 1 is a surface SEM image of the silicon carbide ceramic membrane support prepared in example 1.
FIG. 2 is a graph showing the distribution of the pore diameter of the silicon carbide ceramic membrane support prepared in example 4.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1
A method for improving the mechanical strength of a porous silicon carbide film comprises the following specific steps:
(1) Silicon carbide powder with average grain sizes of 5 microns and 16 microns respectively is adopted, wherein the mass proportion of the silicon carbide powder with the average grain size of 5 microns is 90%, the mass proportion of the silicon carbide powder with the average grain size of 16 microns is 10%, the mass of the added NaA molecular sieve is 10% of the total mass of the silicon carbide powder, and the grinding time is 20 minutes.
(2) After the powder is uniformly mixed, adding a PVA solution with the mass fraction of 5% into the silicon carbide powder in the step (1), wherein the mass of the PVA solution is 10% of the total mass of the silicon carbide powder in the step (1), the mass of the added water is 1% of the total mass of the silicon carbide powder in the step (1), and the grinding time is 20 minutes until the powder has no agglomeration and is uniform and small balls.
(3) 2 to 3 g of the uniformly mixed powder was weighed, and the mixed powder was pressed into a green body of a sheet (Φ 30 mm × 3 mm) or a strip (50 mm × 6 mm × 6 mm) under a pressure of 5 MPa by a tablet press.
(4) The ceramic green body was dried at 25 ℃ 8 h and dried in an 80 ℃ oven at 1 h.
(5) Raising the temperature to 500 ℃ at 1 ℃/min in the air atmosphere, preserving the heat of 3 h, then raising the temperature to 1100 ℃ at 1 ℃/min, preserving the heat of 3 h, and finally cooling the temperature to the room temperature along with the furnace.
The microstructure of the surface of the silicon carbide film is observed by a scanning electron microscope, and as can be seen from the figure of fig. 1, the prepared silicon carbide film has a porous structure, and obvious neck connection exists among particles.
The bending strength and the porosity of the prepared porous silicon carbide film are tested by adopting a fine ceramic three-point bending method and an Archimedes drainage method, and the results show that the strength is over 26 MPa and the porosity is about 48 percent.
Example 2
A method for improving the mechanical strength of a porous silicon carbide film comprises the following specific steps:
(1) Silicon carbide powder with average grain sizes of 0.1 micron and 10 micron is adopted, wherein the mass proportion of the silicon carbide powder with the average grain size of 0.1 micron is 90 percent, the mass proportion of the silicon carbide powder with the average grain size of 10 micron is 10 percent, the mass of the added NaA molecular sieve is 10 percent of the total mass of the silicon carbide powder, and the grinding time is 20 minutes.
(2) After the powder is uniformly mixed, adding 10% by mass of PVA solution into the silicon carbide powder in the step (1), wherein the mass of the PVA solution is 2% of the total mass of the silicon carbide powder in the step (1), the mass of the added water is 1% of the total mass of the silicon carbide powder in the step (1), and the grinding time is 20 minutes until the powder has no agglomeration and is uniform and small balls.
(3) Weighing 2 to 3 g of uniformly mixed powder, and pressing the mixed powder into a blank of a sheet shape (phi 30 mm multiplied by 3 mm) and a strip shape (50 mm multiplied by 6 mm multiplied by 6 mm) under the pressure of 8 MPa by a tablet press.
(4) The ceramic green body was dried at 25 ℃ 8 h and dried in a 100 ℃ oven at 1 h.
(5) Raising the temperature to 500 ℃ at 1 ℃/min in an air atmosphere, preserving the heat of the 3 h, then raising the temperature to 1100 ℃ at 1 ℃/min, preserving the heat of the 3 h, and finally cooling the mixture to room temperature along with a furnace.
The bending strength and the porosity of the prepared porous silicon carbide film are tested by adopting a fine ceramic three-point bending method and an Archimedes drainage method, and the results show that the strength is more than 34 MPa and the porosity is about 45 percent.
Example 3
A method for improving the mechanical strength of a porous silicon carbide film comprises the following specific steps:
(1) Silicon carbide powder with the average grain diameter of 1 mu m and 16 mu m respectively is adopted, wherein the mass proportion of the silicon carbide powder with the average grain diameter of 1 mu m is 80 percent, the mass proportion of the silicon carbide powder with the average grain diameter of 16 mu m is 20 percent, the mass of the added NaA molecular sieve is 10 percent of the total mass of the silicon carbide powder, and the grinding time is 20 minutes.
(2) After the powder is uniformly mixed, adding a PVA solution with the mass fraction of 5% into the silicon carbide powder in the step (1), wherein the mass of the PVA solution is 10% of the total mass of the silicon carbide powder in the step (1), the mass of the added water is 1% of the total mass of the silicon carbide powder in the step (1), and the grinding time is 20 minutes until the powder has no agglomeration and is uniform and small balls.
(3) 2 to 3 g of the uniformly mixed powder was weighed, and the mixed powder was pressed into a green body of a sheet (Φ 30 mm × 3 mm) or a strip (50 mm × 6 mm × 6 mm) under a pressure of 8 MPa by a tablet press.
(4) The ceramic green body was dried at 25 ℃ 8 h and dried in a 120 ℃ oven at 1 h.
(5) Raising the temperature to 500 ℃ at 1 ℃/min in an air atmosphere, preserving the heat of the mixture for 3 h, then raising the temperature to 1300 ℃ at 1 ℃/min, preserving the heat of the mixture for 3 h, and finally cooling the mixture to room temperature along with a furnace.
The bending strength and the porosity of the prepared porous silicon carbide film are tested by adopting a fine ceramic three-point bending method and an Archimedes drainage method, and the results show that the strength is more than 30 MPa and the porosity is about 42 percent.
Example 4
A method for improving the mechanical strength of a porous silicon carbide film comprises the following specific steps:
(1) Silicon carbide powder with average grain sizes of 5 microns and 16 microns respectively is adopted, wherein the mass proportion of the silicon carbide powder with the average grain size of 5 microns is 85%, the mass proportion of the silicon carbide powder with the average grain size of 16 microns is 15%, the mass of the added NaA molecular sieve is 10% of the total mass of the silicon carbide powder, and the grinding time is 20 minutes.
(2) After the powder is uniformly mixed, adding a PVA solution with the mass fraction of 5% into the silicon carbide powder in the step (1), wherein the mass of the PVA solution is 10% of the total mass of the silicon carbide powder in the step (1), the mass of the PVA solution added into the silicon carbide powder in the step (1) is 1% of the total mass of the silicon carbide powder in the step (1), and the grinding time is 20 minutes until the powder does not have the phenomenon of agglomeration and is uniform and small balls.
(3) 2 to 3 g of the uniformly mixed powder was weighed, and the mixed powder was pressed into a green body of a sheet (Φ 30 mm × 3 mm) or a strip (50 mm × 6 mm × 6 mm) under a pressure of 8 MPa by a tablet press.
(4) The ceramic green body was dried at 25 ℃ 8 h and dried in an 80 ℃ oven at 1 h.
(5) Raising the temperature to 500 ℃ at 1 ℃/min in an air atmosphere, preserving the heat of the 3 h, then raising the temperature to 1100 ℃ at 1 ℃/min, preserving the heat of the 3 h, and finally cooling the mixture to room temperature along with a furnace.
The pore size distribution of the prepared porous silicon carbide film is tested by a bubble pressing method, as shown in figure 2, the average pore size is about 0.95 micron, and the pore size distribution is narrow.
The bending strength and the porosity of the prepared porous silicon carbide film are tested by adopting a fine ceramic three-point bending method and an Archimedes drainage method, and the results show that the strength is more than 20 MPa and the porosity is about 47 percent.
Example 5
A method for improving the mechanical strength of a porous silicon carbide film comprises the following specific steps:
(1) Silicon carbide powder with the average grain diameter of 5 mu m and 50 mu m respectively is adopted, wherein the mass proportion of the silicon carbide powder with the average grain diameter of 10 mu m is 70 percent, the mass proportion of the silicon carbide powder with the average grain diameter of 50 mu m is 30 percent, the mass of the added NaA molecular sieve is 20 percent of the total mass of the silicon carbide powder, and the grinding time is 20 minutes.
(2) After the powder is uniformly mixed, adding a PVA solution with the mass fraction of 5% into the silicon carbide powder in the step (1), wherein the mass of the PVA solution is 10% of the total mass of the silicon carbide powder in the step (1), the mass of the added water is 1% of the total mass of the silicon carbide powder in the step (1), and the grinding time is 20 minutes until the powder has no agglomeration and is uniform and small balls.
(3) 2 to 3 g of the uniformly mixed powder was weighed, and the mixed powder was pressed into a green body of a sheet (Φ 30 mm × 3 mm) or a strip (50 mm × 6 mm × 6 mm) under a pressure of 10 MPa by a tablet press.
(4) The ceramic green body was dried at 25 ℃ 8 h and dried in an 80 ℃ oven at 1 h.
(5) Raising the temperature to 500 ℃ at 1 ℃/min in an air atmosphere, preserving the heat of the 3 h, then raising the temperature to 1000 ℃ at 1 ℃/min, preserving the heat of the 3 h, and finally cooling the mixture to room temperature along with a furnace.
The bending strength and the porosity of the prepared porous silicon carbide film are tested by adopting a fine ceramic three-point bending method and an Archimedes drainage method, and the results show that the strength is more than 20 MPa and the porosity is about 47 percent.
Claims (4)
1. A method for improving the mechanical strength of a porous silicon carbide film is characterized by comprising the following specific steps:
(1) Adding a small amount of silicon carbide powder with larger size into the small-size silicon carbide powder, wherein the proportion of the silicon carbide powder with the average grain diameter of 0.1-5 mu m in the total mass of the silicon carbide is 70-90%, and the proportion of the silicon carbide powder with the average grain diameter of 10-50 mu m in the total mass of the silicon carbide is 10-30%;
(2) Mixing the silicon carbide ceramic powder with the two sizes and a sintering aid NaA molecular sieve according to a certain proportion, wherein the grinding time is 20 minutes;
(3) Adding a certain amount of polyvinyl alcohol (PVA) solution and water into the silicon carbide powder obtained in the step (2) and continuously mixing uniformly, wherein the final state of the powder is free from caking;
(4) Pressing the silicon carbide powder obtained in the step (3) into a sheet or strip blank by a tablet press under the pressure of 5-10 MPa;
(5) Drying the blank at 25 ℃ for 8 h, and then drying in an oven at 80-120 ℃ for 1 h;
(6) And (3) placing the dried blank into a muffle furnace for sintering, heating to 500 ℃ at the speed of 1 ℃/min, preserving heat for 3 h, then heating to 1000 to 1300 ℃ at the speed of 1 ℃/min, preserving heat for 3 h, and finally cooling to room temperature along with the furnace.
2. The method for improving the mechanical strength of a porous silicon carbide film according to claim 1, wherein the silicon carbide powder is a non-oxide ceramic powder such as silicon nitride or titanium carbide.
3. The method for improving the mechanical strength of the porous silicon carbide film as claimed in claim 1, wherein the added mass of the NaA molecular sieve in the step (2) is 10 to 20% of the total mass of the silicon carbide powder.
4. The method for improving the mechanical strength of the porous silicon carbide film according to claim 1, wherein the concentration of the polyvinyl alcohol solution in the step (3) is 5 to 10%, and the addition amount is 2 to 10% of the total mass of the silicon carbide powder.
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| CN108341671A (en) * | 2018-01-26 | 2018-07-31 | 山东四海水处理设备有限公司 | Multichannel silicon carbide ceramics membrane component and preparation method thereof |
| CN111533572A (en) * | 2020-05-08 | 2020-08-14 | 武汉工程大学 | Preparation method of porous silicon carbide ceramic support |
| CN112299871A (en) * | 2020-11-16 | 2021-02-02 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of porous ceramic containing silicon carbide film |
| CN113121241A (en) * | 2021-04-25 | 2021-07-16 | 南京依柯卡特排放技术股份有限公司 | High-flux silicon carbide ceramic filter membrane and preparation method thereof |
| CN114315363A (en) * | 2022-01-11 | 2022-04-12 | 南京工业大学 | Method for regulating and controlling pore structure and surface property of silicon carbide film in one step |
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- 2022-11-21 CN CN202211452696.2A patent/CN115745618A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004231493A (en) * | 2003-01-31 | 2004-08-19 | Toshiba Ceramics Co Ltd | Porous silicon carbide sintered compact and its manufacturing method |
| CN104261867A (en) * | 2014-09-23 | 2015-01-07 | 武汉工程大学 | Preparation method of pure silicon carbide porous ceramic membrane |
| CN108264354A (en) * | 2018-01-26 | 2018-07-10 | 山东四海水处理设备有限公司 | Multichannel silicon carbide ceramic support body and preparation method thereof |
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| CN111533572A (en) * | 2020-05-08 | 2020-08-14 | 武汉工程大学 | Preparation method of porous silicon carbide ceramic support |
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