CN110540419B - Cordierite honeycomb ceramic carrier and preparation method thereof - Google Patents
Cordierite honeycomb ceramic carrier and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a cordierite honeycomb ceramic carrier and a preparation method thereof, wherein the preparation method comprises the following steps: preparing 3D printing slurry by adopting raw materials comprising a component A, a component B and a silica gel binder, then performing direct-writing 3D printing by adopting the 3D printing slurry to prepare a molded blank body, and sintering the molded blank body; wherein the component A is magnesium oxide and/or magnesium hydroxide, the component B is aluminum oxide and/or aluminum hydroxide, and the grain diameters of the two are below 30 mu m. Through the mode, the printing parameters are determined for direct-writing 3D printing and forming through the allocation of the 3D printing slurry and according to the parameter requirements of the target honeycomb ceramic carrier, so that the rapid forming of honeycomb ceramic carriers with different hole types, different hole wall thicknesses and different hole densities can be realized; the preparation method is simple and easy to implement, and the cordierite honeycomb ceramic carrier with high pore density can be prepared, and the performance of the obtained cordierite honeycomb ceramic carrier is good.
Description
Technical Field
The invention relates to the technical field of porous honeycomb ceramics, in particular to a cordierite honeycomb ceramic carrier and a preparation method thereof.
Background
The honeycomb ceramic is used as a combustion catalytic carrier, is widely applied to the industry for removing VOCs pollution and helping to recycle heat energy; meanwhile, the gas stove can also be applied to a household gas stove, the heat efficiency of gas combustion can be improved, and the emission of harmful substances is reduced. Studies have shown that increasing the specific surface area of the honeycomb ceramic can significantly improve the catalytic efficiency, while the specific surface area of the honeycomb ceramic increases as the number of unit cells increases. The density of the honeycomb ceramic pores is mostly concentrated at 62-93 pores/cm at present2To (c) to (d); 93-140 holes/cm have been developed in America and Japan2Even up to 186 holes/cm2The high-density porous honeycomb ceramics of (1); in contrast, the preparation process of the Chinese honeycomb ceramics is relatively lagged behind and can be used for producing the honeycomb ceramicsYield 62 holes/cm293 holes/cm2The research on extrusion forming dies has also been primarily successful.
The current main development directions of the honeycomb ceramics are near-zero expansion coefficient, higher pore density, thinner partition walls (the thickness can be smaller than the diameter of human hair) and the like, but the preparation cost is increased and the preparation process is more complicated as the pore density is increased. The cordierite honeycomb ceramic has the advantages of low thermal expansion coefficient, good thermal stability, good adsorption performance and the like, and is a honeycomb ceramic carrier with excellent performance. However, the cordierite green hole prepared by the traditional processing technology has small density and is limited to further improvement of the performance. Therefore, there is a need for a new method suitable for producing high pore density cordierite honeycomb ceramics.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a cordierite honeycomb ceramic carrier and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
in a first aspect of the present invention, there is provided a method for producing a cordierite honeycomb ceramic carrier, comprising the steps of:
s1, preparing 3D printing slurry by adopting raw materials of cordierite honeycomb ceramic carriers;
s2, performing direct-writing 3D printing by using the 3D printing slurry to obtain a molded blank;
s3, sintering the formed blank to obtain a cordierite honeycomb ceramic carrier;
in step S1, the raw materials of the cordierite honeycomb ceramic carrier include a component a, a component B, and a silica gel binder; the component A is magnesium oxide and/or magnesium hydroxide, the component B is aluminum oxide and/or aluminum hydroxide, and the particle sizes of the component A and the component B are below 30 mu m; the mass ratio of the component A to the component B to the silica gel binder is 1: (0.1-10): (0.1-10).
Direct-write 3D printing is a 3D printing technology that forms in an extrusion manner, and the key to forming is the control of rheological properties of the slurry. The slurry needs to have suitable viscosity, modulus and shear thinning characteristics, and be sufficiently uniform so that it can flow continuously and smoothly from the finer needles without clogging the needles, and also have sufficient strength to ensure that the structure does not collapse after forming. The 3D printing slurry prepared in the step S1 adopts the silica gel binder as the raw material, because the rheological property of the silica gel can meet the requirements of the direct-writing 3D printing technology and is suitable for direct-writing 3D printing and molding, the silica gel binder is used as the raw material to be mixed with the component A and the component B to prepare the 3D printing slurry, and the rheological property of the slurry can meet the requirements of the direct-writing 3D printing technology; in addition, silica gel is decomposed into silicon dioxide at high temperature, which is one of main raw materials for synthesizing cordierite, the silica gel is used as a silicon source for synthesizing the cordierite, the synthesis of the cordierite and the 3D printing and forming are integrated, and the two are combined into one, so that the forming step can be simplified. According to some embodiments of the invention, in step S1, the silicone adhesive is at least one selected from polydimethylsiloxane, glass cement, and room temperature vulcanized silicone rubber (i.e., RTV silicone).
In the raw materials of 3D printing paste, the silica gel binder is the key that 3D printing can extrusion moulding directly, and the particle size of the component A and the component B of mixing into has decided the internal diameter size of the printing syringe needle of selecting for use, and the printing syringe needle internal diameter size has decided minimum wall thickness and the biggest pore density of through-hole in the cordierite honeycomb ceramic carrier again, and the particle size of raw materials is less, can correspond the printing syringe needle of selecting little internal diameter to be applicable to the honeycomb ceramic carrier of preparation high pore density.
In the cordierite honeycomb ceramic carrier raw material, the particle diameters of the component A and the component B are generally 30 μm or less. If the aim is to achieve 1000 holes/cm2The above ultra-high pore density is generally required to have a particle size of the raw material of 10 μm or less and an inner diameter of the printing needle of 200 μm or less. If the particle size of the powder doped with the component A and the component B is too large, such as 30-50 mu m, a needle head with the diameter of 400-1 mm is adopted for printing, and the pore density of the formed cordierite honeycomb ceramic carrier is 100 pores/cm2The following.
According to some embodiments of the invention, in step S1, the component a is magnesium oxide, the component B is aluminum oxide, and the silica gel binder is polydimethylsiloxane; the mass ratio of the component A to the component B to the silica gel binder is 1: 2.53: 4.60; and mixing and preparing 3D printing slurry according to the proportion, and obtaining the pure-phase cordierite honeycomb ceramic carrier after direct-writing 3D printing molding and sintering.
The direct-write 3D printing in step S2 specifically includes: the method comprises the following steps of firstly obtaining a three-dimensional model of a cordierite honeycomb ceramic carrier structure by computer-assisted modeling, and then generating a printable G code program by using slicing software, or directly writing the G code program; and then loading the 3D printing slurry into a charging barrel of a 3D printing device, and performing direct-writing 3D printing on the three-dimensional honeycomb ceramic carrier structure according to the path set by the G code.
The G code program is obtained by firstly obtaining a three-dimensional model of a cordierite honeycomb ceramic carrier structure through computer-aided modeling, then carrying out two-dimensional slicing processing through slicing software to obtain two-dimensional slicing data, and then generating the G code program. The direct writing of the G code program can be specifically realized by firstly obtaining a macrostructure model of the cordierite honeycomb ceramic carrier according to preset requirements (including hole type, hole size, through hole density, wall thickness and the like) of the structure, then designing a printing path according to the macrostructure model and writing the G code program. The pore density, the specific surface area and the through porosity of the cordierite honeycomb ceramic carrier can be calculated through basic parameters such as pore type, pore size, wall thickness and the like of the cordierite honeycomb ceramic carrier and the arrangement mode.
According to some embodiments of the invention, in step S2, the inner diameter of the printing needle used for the direct-writing 3D printing is 10 to 200 μm, the extrusion pressure is 10 to 100psi, and the moving speed is 0.3 to 30 mm/S.
According to some embodiments of the invention, in step S3, the sintering temperature of the sintering process is 1300 ℃ to 1400 ℃. The sintering time is generally 2-12 h.
According to some embodiments of the present invention, in step S3, before the sintering process is performed on the formed green body, the binder removal process is performed on the formed green body.
According to some embodiments of the invention, the glue discharging treatment is specifically heat preservation glue discharging at 500-600 ℃. The glue discharging time is generally 2-4 h.
In a second aspect of the present invention, there is provided a cordierite honeycomb ceramic carrier produced by any one of the methods for producing a cordierite honeycomb ceramic carrier according to the first aspect of the present invention.
The embodiment of the invention has the beneficial technical effects that:
the embodiment of the invention provides a preparation method of a cordierite honeycomb ceramic carrier, which can be used for determining printing parameters to perform direct-writing 3D printing forming through the preparation of 3D printing slurry and according to the parameter requirements of a target honeycomb ceramic carrier, and can realize the rapid forming of honeycomb ceramic carriers with different hole types, different hole wall thicknesses and different hole densities; the preparation method is simple and easy to implement, and the cordierite honeycomb ceramic carrier with high pore density can be prepared, and the performance of the obtained cordierite honeycomb ceramic carrier is good.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
A cordierite honeycomb ceramic carrier is prepared by the following steps:
s1, slurry preparation: weighing 1.088g of magnesia powder with the particle size of 1-5 microns, 2.754g of aluminum oxide powder and 4.55g of PDMS silica gel prepolymer A, fully and uniformly mixing the three materials in a mechanical stirring, grinding or ball milling mode, then adding 0.45g of PDMS silica gel crosslinking agent B, and uniformly stirring to obtain 3D printing slurry; the resulting 3D printing paste was then loaded into a 10mL cartridge to be printed. The PDMS silica gel is purchased from the market directly and comprises a PDMS silica gel prepolymer A and a PDMS silica gel cross-linking agent B, and the mass ratio of the PDMS silica gel prepolymer A to the PDMS silica gel cross-linking agent B is 10: 1 and mixing. Considering that the silica gel is slowly cured, the prepared 3D printing paste needs to complete the forming process within 5 hours.
S2, direct-writing 3D printing and forming: writing a G code program of a square hole structure, wherein the length of the hole edge is set to be 250 micrometers; selecting a glass needle head with the inner diameter of 100 mu m, setting the extrusion pressure to be 70-90 psi and the moving speed to be 5-10 mm/s; performing direct-writing 3D printing according to the path set by the G code to obtain a square-hole honeycomb-structure ceramic carrier blank;
s3, sintering: and carrying out multi-step heat preservation sintering on the printed ceramic carrier green body with the square-hole honeycomb structure. Specifically, the temperature is raised to 600 ℃ at the speed of 1 ℃/min, and the temperature is kept for 4 hours, so that the PDMS silica gel is fully decomposed into silicon dioxide; then heating to 1350 ℃ at the speed of 2 ℃/min, preserving the heat for 10 hours, and carrying out sufficient solid phase sintering reaction to obtain the square-hole cordierite honeycomb ceramic carrier. The thickness of the pore wall of the obtained square-pore cordierite honeycomb ceramic carrier is about 100 mu m, and the pore density reaches 1600 pores/cm2。
Example 2
A cordierite honeycomb ceramic carrier is prepared by the following steps:
s1, slurry preparation: weighing 1.575g of magnesium hydroxide powder with the particle size of less than 10 microns, 2.754g of aluminum oxide powder and 4.55g of PDMS silica gel prepolymer A, fully and uniformly mixing the three materials in a mechanical stirring, grinding or ball milling mode, then adding 0.45g of PDMS silica gel crosslinking agent B, and uniformly stirring to obtain 3D printing slurry; the resulting 3D printing paste was then loaded into a 10mL cartridge to be printed. The PDMS silica gel is purchased from the market directly and comprises a PDMS silica gel prepolymer A and a PDMS silica gel cross-linking agent B, and the mass ratio of the PDMS silica gel prepolymer A to the PDMS silica gel cross-linking agent B is 10: 1 and mixing. Considering that the silica gel is slowly cured, the prepared 3D printing paste needs to complete the forming process within 5 hours.
S2, direct-writing 3D printing and forming: writing a G code program of a triangular hole structure, wherein the side length of the triangular hole is set to be 450 micrometers; selecting a plastic needle with the inner diameter of 160 mu m, setting the extrusion pressure to be 40-60 psi and the moving speed to be 10-15 mm/s; performing direct-writing 3D printing according to the path set by the G code to obtain a triangular honeycomb-structured ceramic carrier blank;
s3, sintering: and carrying out multi-step heat preservation sintering on the printed ceramic carrier green body with the triangular hole honeycomb structure. Specifically, firstly, 1 is addedHeating to 600 ℃ at a speed of 600 ℃/min, and preserving heat for 4h to fully decompose the PDMS silica gel into silicon dioxide; then heating to 1350 ℃ at the speed of 2 ℃/min, preserving the heat for 10 hours, and carrying out sufficient solid phase sintering reaction to obtain the triangular-hole cordierite honeycomb ceramic carrier. The wall thickness of the obtained triangular-hole cordierite honeycomb ceramic carrier is about 160 mu m, and the hole density reaches 1140 holes/cm2。
Comparative example 1
A cordierite honeycomb ceramic carrier is prepared by the following steps:
s1, slurry preparation: weighing 1.088g of magnesia powder, 2.754g of alumina powder and 4.55g of PDMS silica gel prepolymer A with the particle size of 30-50 microns, fully and uniformly mixing the three materials in a mechanical stirring, grinding or ball milling mode, then adding 0.45g of PDMS silica gel crosslinking agent B, and uniformly stirring to obtain 3D printing slurry; the resulting 3D printing paste was then loaded into a 10mL cartridge to be printed. The PDMS silica gel is purchased from the market directly and comprises a PDMS silica gel prepolymer A and a PDMS silica gel cross-linking agent B, and the mass ratio of the PDMS silica gel prepolymer A to the PDMS silica gel cross-linking agent B is 10: 1 and mixing.
S2, 3D printing and forming: writing a G code program of a square hole structure, wherein the length of the hole edge is set to be 1.5 mm; selecting a plastic needle with the inner diameter of 600 mu m, and setting the extrusion pressure of 30-40 psi and the moving speed of 15-20 mm/s; performing direct-writing 3D printing according to the path set by the G code to obtain a square-hole honeycomb-structure ceramic carrier blank;
s3, sintering: and carrying out multi-step heat preservation sintering on the printed ceramic carrier green body with the square-hole honeycomb structure. Specifically, the temperature is raised to 600 ℃ at the speed of 1 ℃/min, and the temperature is kept for 4 hours, so that the PDMS silica gel is fully decomposed into silicon dioxide; then heating to 1350 ℃ at the speed of 2 ℃/min, preserving the heat for 10 hours, and carrying out sufficient solid phase sintering reaction to obtain the square-hole cordierite honeycomb ceramic carrier. The thickness of the pore wall of the obtained square-pore cordierite honeycomb ceramic carrier is about 600 mu m, and the pore density is 44 pores/cm2。
Scanning Electron Microscope (SEM) observation and specific surface area (BET) test were performed on the cordierite honeycomb ceramic supports obtained in example 1, example 2, and comparative example 1, respectively. The test result shows that: the cordierite honeycomb ceramic carriers obtained in examples 1 and 2 were smaller in the size of the through-hole, higher in the pore density and larger in the specific surface area, compared to the cordierite honeycomb ceramic carrier of comparative example 1. The specific surface area is one of the key factors influencing the combustion catalytic performance of the honeycomb ceramic carrier, and the cordierite honeycomb ceramic carriers with higher density and larger specific surface area prepared in the examples 1 and 2 can obviously improve the efficiency of the combustion catalysis after the catalyst is loaded.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A method for preparing a cordierite honeycomb ceramic carrier is characterized by comprising the following steps:
s1, preparing 3D printing slurry by adopting raw materials of cordierite honeycomb ceramic carriers;
s2, performing direct-writing 3D printing by using the 3D printing slurry to obtain a molded blank;
s3, sintering the formed blank to obtain a cordierite honeycomb ceramic carrier;
in step S1, the raw materials of the cordierite honeycomb ceramic carrier include a component a, a component B, and a silica gel binder; the component A is magnesium oxide and/or magnesium hydroxide, the component B is aluminum oxide and/or aluminum hydroxide, and the particle sizes of the component A and the component B are below 30 mu m; the mass ratio of the component A to the component B to the silica gel binder is 1: (0.1-10): (0.1 to 10);
the silica gel binder is at least one selected from polydimethylsiloxane and room temperature vulcanized silicone rubber.
2. The method for producing a cordierite honeycomb ceramic carrier according to claim 1, wherein in step S1, the component a is magnesia, the component B is alumina, and the silica gel binder is polydimethylsiloxane; the mass ratio of the component A to the component B to the silica gel binder is 1: 2.53: 4.60.
3. the method for preparing cordierite honeycomb ceramic carrier according to claim 1, wherein in step S2, the inner diameter of the printing needle used for direct-write 3D printing is 10 to 200 μm, the extrusion pressure is 10 to 100psi, and the moving speed is 0.3 to 30 mm/S.
4. The method of producing cordierite honeycomb ceramic carrier according to claim 1, wherein the sintering temperature of the sintering process in step S3 is 1300 ℃ to 1400 ℃.
5. The method of producing a cordierite honeycomb ceramic carrier according to claim 4, wherein in step S3, the green compact is subjected to a binder removal treatment before the green compact is subjected to the sintering treatment.
6. The method for preparing the cordierite honeycomb ceramic carrier according to claim 5, wherein the binder removal treatment is specifically heat preservation binder removal at 500-600 ℃.
7. A cordierite honeycomb ceramic carrier produced by the method for producing a cordierite honeycomb ceramic carrier according to any one of claims 1 to 6.
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| CN113526975B (en) * | 2020-04-16 | 2022-08-30 | 中国石油天然气股份有限公司 | Alumina carrier material with gradient structure and 3D printing forming method thereof |
| CN113548882B (en) * | 2020-04-24 | 2022-12-20 | 中国科学院宁波材料技术与工程研究所 | Cordierite ceramic device and preparation method and application thereof |
| CN112058317B (en) * | 2020-09-24 | 2021-09-03 | 西安交通大学 | Method for 3D printing of monolithic catalyst |
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