CN108046834B - Preparation process of porous ceramic heating body with mosaic structure - Google Patents
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
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Abstract
The invention discloses a preparation process of a porous ceramic heating body with an embedded structure, and relates to the technical field of chemical products; the process comprises the steps of mixing materials, ball milling, defoaming, molding, drying, sintering, grouting, metallized sintering and electrode connection; the invention has the beneficial effects that: the whole manufacturing process is simple, the production efficiency is high, the sintering temperature is low, and the large-scale production is favorably realized; the porous ceramic heating body prepared simultaneously has high strength and stable structure, solves the problem that the heating material of the porous ceramic heating body in the prior art is easy to fall off, and the mosaic structure enables the heating to be more uniform.
Description
Technical Field
The invention relates to the technical field of chemical products, in particular to a preparation process of a porous ceramic heating body with an embedded structure.
Background
The porous ceramic is a solid material containing pores, and generally, the volume fraction of the pores in the porous ceramic body is between 20% and 95%. The porous ceramic is widely applied to the fields of environmental protection, chemical engineering, metallurgical medicine, biomedicine and the like as a solid-liquid separation medium, a catalyst carrier for liquid filtration and purification, gas purification and chemical reaction and the like. Diatomite is formed by silicate remains after death of unicellular algae which are collectively called diatoms, is water-containing amorphous SiO2 in nature, and is widely applied to occasions of sewage treatment, various fillers, coating additives and the like due to the characteristics of huge specific surface, strong adsorbability, surface electrical property and the like. The diatomite has wide source and low price, has a large amount of micropores, and is an ideal raw material for preparing porous ceramics.
The porous ceramic heating body in the prior art is generally complex in manufacturing process, is not beneficial to large-scale production, and meanwhile, the heating material of the porous ceramic heating body is easy to fall off and is not uniformly heated.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation process of a porous ceramic heating body with an embedded structure, the process is simple, and the porous ceramic heating body prepared by the preparation process has high strength and more uniform heating.
The technical scheme adopted by the invention for solving the technical problems is as follows: the improvement of a preparation process of a porous ceramic heating body with a mosaic structure is as follows: the preparation process comprises the following steps:
A. mixing materials: weighing 10-40% of diatomite, 20-40% of starch, 0-2% of nano silicon dioxide solution and 30-50% of deionized water according to the mass percentage, and uniformly mixing and stirring to prepare ceramic matrix slurry;
weighing 20-50% of resistance slurry, 20-40% of starch and 10-30% of organic solvent according to the mass percentage, and uniformly mixing and stirring to prepare the resistance slurry with the pore-forming agent;
B. ball milling: adding grinding balls into the ceramic matrix slurry prepared in the step A, and putting the ceramic matrix slurry into a ball milling tank for wet ball milling for 4-24 hours;
adding grinding balls into the resistance slurry prepared in the step A, and putting the resistance slurry into a ball milling tank for wet ball milling for 24-48 h;
C. defoaming: b, defoaming the ceramic matrix slurry subjected to wet ball milling in the step B under a vacuum condition;
b, defoaming the resistance slurry subjected to wet ball milling in the step B under a vacuum condition;
D. forming and drying: c, pouring the ceramic matrix slurry prepared in the step C into a ceramic matrix with a required shape by using a pouring machine, and drying the ceramic matrix to form a blank;
E. and (3) sintering: d, placing the blank prepared in the step D into a graphite crucible, embedding isolation powder, sintering the blank embedded in the isolation powder by using a box-type furnace under normal pressure, wherein the sintering atmosphere is oxygen, and sintering the blank to obtain a semi-finished product of the porous ceramic heating body substrate;
F. grouting: c, immersing the semi-finished product of the porous ceramic heating body substrate prepared in the step E into the resistance slurry prepared in the step C, wherein the resistance slurry is filled in pores of the porous ceramic heating body substrate;
G. metallization and sintering: placing the substrate with the porous ceramic heating body prepared in the step F into a graphite crucible, and then placing the graphite crucible into a box-type furnace to carry out starch discharging and metallized sintering of the resistance slurry;
H. electrode connection: and G, carrying out surface nickel plating treatment on two ends of the heating body blank prepared in the step G, and then carrying out brazing extraction electrode on the part subjected to the nickel plating treatment to obtain a porous ceramic heating body finished product.
Furthermore, in the step E, the temperature rise rate during sintering is 1-20 ℃/min, the sintering temperature is 900-.
Furthermore, in the step G, the temperature rise rate during the metallization sintering is 1-5 ℃/min, the metallization sintering temperature is 800-.
Further, in the step a, the ceramic matrix slurry is composed of the following raw materials by mass:
20 percent of diatomite
Starch 35%
1 percent of nano silicon dioxide solution
44% of deionized water.
Further, in the step A, the resistance paste is composed of the following raw materials in percentage by mass:
40 percent of resistance sizing agent
Starch 35%
25% of organic solvent.
Further, in the step a, the ceramic matrix slurry is composed of the following raw materials by mass:
10 percent of diatomite
Starch 40%
50% of deionized water.
Further, in the step A, the resistance paste is composed of the following raw materials in percentage by mass:
50 percent of resistance sizing agent
Starch 40%
10% of organic solvent.
Further, in the step a, the ceramic matrix slurry is composed of the following raw materials by mass:
40 percent of diatomite
28% of starch
2 percent of nano silicon dioxide solution
30% of deionized water.
Further, in the step A, the resistance paste is composed of the following raw materials in percentage by mass:
30 percent of resistance sizing agent
Starch 40%
30% of organic solvent.
The invention has the beneficial effects that: the whole manufacturing process is simple, the blank body is sintered by adopting a box-type furnace under the oxidizing atmosphere and normal pressure, the production efficiency is high, the sintering temperature is low, and the large-scale production is favorably realized; meanwhile, the porous ceramic heating body prepared by the process is embedded together by the porous ceramic and the porous resistor, so that the strength is high, the structure is stable, the problem that the heating material of the porous ceramic heating body in the prior art is easy to fall off is solved, and the heating is more uniform due to the embedded structure.
Drawings
Fig. 1 is a process flow diagram of a preparation process of a porous ceramic heater with a damascene structure according to the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
The conception, the specific structure, and the technical effects produced by the present invention will be clearly and completely described below in conjunction with the embodiments and the accompanying drawings to fully understand the objects, the features, and the 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. In addition, all the connection/connection relations referred to in the patent do not mean that the components are directly connected, but mean that a better connection structure can be formed by adding or reducing connection auxiliary components according to specific implementation conditions. All technical characteristics in the invention can be interactively combined on the premise of not conflicting with each other.
Example 1
Referring to fig. 1, the invention discloses a preparation process of a porous ceramic heating body with a mosaic structure, which specifically comprises the following steps:
A. mixing materials: weighing 20% of diatomite, 35% of starch, 1% of nano-silica solution and 44% of deionized water according to the mass percentage, and uniformly mixing and stirring to prepare ceramic matrix slurry;
weighing 40% of resistance slurry, 35% of starch and 25% of organic solvent according to the mass percentage, and uniformly mixing and stirring to prepare the resistance slurry with the pore-forming agent;
B. ball milling: adding grinding balls into the ceramic matrix slurry prepared in the step A, and putting the ceramic matrix slurry into a ball milling tank for wet ball milling for 12 hours; adding grinding balls into the resistance slurry prepared in the step A, and putting the resistance slurry into a ball milling tank for wet ball milling for 24 hours;
C. defoaming: b, defoaming the ceramic matrix slurry subjected to wet ball milling in the step B under a vacuum condition; b, defoaming the resistance slurry subjected to wet ball milling in the step B under a vacuum condition;
D. forming and drying: c, pouring the ceramic matrix slurry prepared in the step C into a ceramic matrix with a required shape by using a pouring machine, and drying the ceramic matrix to form a blank;
E. and (3) sintering: d, placing the blank prepared in the step D into a graphite crucible, embedding isolation powder, sintering the blank embedded in the isolation powder by using a box-type furnace under normal pressure, wherein the sintering atmosphere is oxygen, and sintering the blank to obtain a semi-finished product of the porous ceramic heating body substrate; the heating rate during sintering is 5 ℃/min, the sintering temperature is 1100 ℃, and the heat preservation time is 4 h;
F. grouting: c, immersing the semi-finished product of the porous ceramic heating body substrate prepared in the step E into the resistance slurry prepared in the step C, wherein the resistance slurry is filled in pores of the porous ceramic heating body substrate;
G. metallization and sintering: placing the substrate with the porous ceramic heating body prepared in the step F into a graphite crucible, and then placing the graphite crucible into a box-type furnace to carry out starch discharging and metallized sintering of the resistance slurry; the temperature rise rate of the metallization sintering is 5 ℃/min, the metallization sintering temperature is 850 ℃, and the time is 1 h;
H. electrode connection: and G, carrying out surface nickel plating treatment on two ends of the heating body blank prepared in the step G, and then carrying out brazing extraction electrode on the part subjected to the nickel plating treatment to obtain a porous ceramic heating body finished product.
Example 2
Referring to fig. 1, the invention discloses a preparation process of a porous ceramic heating body with a mosaic structure, which specifically comprises the following steps:
A. mixing materials: weighing 10% of diatomite, 40% of starch and 50% of deionized water according to the mass percentage, and uniformly mixing and stirring to prepare ceramic matrix slurry; weighing 50% of resistance slurry, 40% of starch and 10% of organic solvent according to the mass percentage, and uniformly mixing and stirring to prepare the resistance slurry with the pore-forming agent;
B. ball milling: adding grinding balls into the ceramic matrix slurry prepared in the step A, and putting the ceramic matrix slurry into a ball milling tank for wet ball milling for 24 hours; adding grinding balls into the resistance slurry prepared in the step A, and putting the resistance slurry into a ball milling tank for wet ball milling, wherein the wet ball milling time is 48 hours;
C. defoaming: b, defoaming the ceramic matrix slurry subjected to wet ball milling in the step B under a vacuum condition; b, defoaming the resistance slurry subjected to wet ball milling in the step B under a vacuum condition;
D. forming and drying: c, pouring the ceramic matrix slurry prepared in the step C into a ceramic matrix with a required shape by using a pouring machine, and drying the ceramic matrix to form a blank;
E. and (3) sintering: d, placing the blank prepared in the step D into a graphite crucible, embedding isolation powder, sintering the blank embedded in the isolation powder by using a box-type furnace under normal pressure, wherein the sintering atmosphere is oxygen, and sintering the blank to obtain a semi-finished product of the porous ceramic heating body substrate; the heating rate during sintering is 1 ℃/min, the sintering temperature is 900 ℃, and the heat preservation time is 2 h;
F. grouting: c, immersing the semi-finished product of the porous ceramic heating body substrate prepared in the step E into the resistance slurry prepared in the step C, wherein the resistance slurry is filled in pores of the porous ceramic heating body substrate;
G. metallization and sintering: placing the substrate with the porous ceramic heating body prepared in the step F into a graphite crucible, and then placing the graphite crucible into a box-type furnace to carry out starch discharging and metallized sintering of the resistance slurry; the heating rate during the metallization sintering is 1 ℃/min, the metallization sintering temperature is 800 ℃, and the time is 1 h;
H. electrode connection: and G, carrying out surface nickel plating treatment on two ends of the heating body blank prepared in the step G, and then carrying out brazing extraction electrode on the part subjected to the nickel plating treatment to obtain a porous ceramic heating body finished product.
Example 3
Referring to fig. 1, the invention discloses a preparation process of a porous ceramic heating body with a mosaic structure, which specifically comprises the following steps:
A. mixing materials: weighing 40% of diatomite, 28% of starch, 2% of nano-silica solution and 30% of deionized water according to the mass percentage, and uniformly mixing and stirring to prepare ceramic matrix slurry; weighing 30% of resistance slurry, 40% of starch and 30% of organic solvent according to the mass percentage, and uniformly mixing and stirring to prepare the resistance slurry with the pore-forming agent;
B. ball milling: adding grinding balls into the ceramic matrix slurry prepared in the step A, and putting the ceramic matrix slurry into a ball milling tank for wet ball milling, wherein the wet ball milling time is 14 hours; adding grinding balls into the resistance slurry prepared in the step A, and putting the resistance slurry into a ball milling tank for wet ball milling for 36 hours;
C. defoaming: b, defoaming the ceramic matrix slurry subjected to wet ball milling in the step B under a vacuum condition;
b, defoaming the resistance slurry subjected to wet ball milling in the step B under a vacuum condition;
D. forming and drying: c, pouring the ceramic matrix slurry prepared in the step C into a ceramic matrix with a required shape by using a pouring machine, and drying the ceramic matrix to form a blank;
E. and (3) sintering: d, placing the blank prepared in the step D into a graphite crucible, embedding isolation powder, sintering the blank embedded in the isolation powder by using a box-type furnace under normal pressure, wherein the sintering atmosphere is oxygen, and sintering the blank to obtain a semi-finished product of the porous ceramic heating body substrate; the heating rate during sintering is 20 ℃/min, the sintering temperature is 1400 ℃, and the heat preservation time is 12 h;
F. grouting: c, immersing the semi-finished product of the porous ceramic heating body substrate prepared in the step E into the resistance slurry prepared in the step C, wherein the resistance slurry is filled in pores of the porous ceramic heating body substrate;
G. metallization and sintering: placing the substrate with the porous ceramic heating body prepared in the step F into a graphite crucible, and then placing the graphite crucible into a box-type furnace to carry out starch discharging and metallized sintering of the resistance slurry; the heating rate during the metallization sintering is 5 ℃/min, the metallization sintering temperature is 1000 ℃, and the time is 2 h;
H. electrode connection: and G, carrying out surface nickel plating treatment on two ends of the heating body blank prepared in the step G, and then carrying out brazing extraction electrode on the part subjected to the nickel plating treatment to obtain a porous ceramic heating body finished product.
In conclusion, the invention provides a preparation process of a porous ceramic heating body with an embedded structure, the whole manufacturing process is simple, the blank body is sintered by adopting a box-type furnace under the oxidizing atmosphere and normal pressure, the production efficiency is high, the sintering temperature is low, and the large-scale production is favorably realized; meanwhile, the porous ceramic heating body prepared by the process is embedded together by the porous ceramic and the porous resistor, so that the strength is high, the structure is stable, the problem that the heating material of the porous ceramic heating body in the prior art is easy to fall off is solved, and the heating is more uniform due to the embedded structure.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A preparation process of a porous ceramic heating body with an embedded structure is characterized by comprising the following steps: the preparation process comprises the following steps:
A. mixing materials: weighing 10-40% of diatomite, 20-40% of starch, 0-2% of nano silicon dioxide solution and 30-50% of deionized water according to the mass percentage, and uniformly mixing and stirring to prepare ceramic matrix slurry;
weighing 20-50% of resistance slurry, 20-40% of starch and 10-30% of organic solvent according to the mass percentage, and uniformly mixing and stirring to prepare the resistance slurry with the pore-forming agent;
B. ball milling: adding grinding balls into the ceramic matrix slurry prepared in the step A, and putting the ceramic matrix slurry into a ball milling tank for wet ball milling for 4-24 hours;
adding grinding balls into the resistance slurry prepared in the step A, and putting the resistance slurry into a ball milling tank for wet ball milling for 24-48 h;
C. defoaming: b, defoaming the ceramic matrix slurry subjected to wet ball milling in the step B under a vacuum condition;
b, defoaming the resistance slurry subjected to wet ball milling in the step B under a vacuum condition;
D. forming and drying: c, pouring the ceramic matrix slurry prepared in the step C into a ceramic matrix with a required shape by using a pouring machine, and drying the ceramic matrix to form a blank;
E. and (3) sintering: d, placing the blank prepared in the step D into a graphite crucible, embedding isolation powder, sintering the blank embedded in the isolation powder by using a box-type furnace under normal pressure, wherein the sintering atmosphere is oxygen, and sintering the blank to obtain a semi-finished product of the porous ceramic heating body substrate;
F. grouting: c, immersing the semi-finished product of the porous ceramic heating body substrate prepared in the step E into the resistance slurry prepared in the step C, wherein the resistance slurry is filled in pores of the porous ceramic heating body substrate;
G. metallization and sintering: placing the substrate with the porous ceramic heating body prepared in the step F into a graphite crucible, and then placing the graphite crucible into a box-type furnace to carry out starch discharging and metallized sintering of the resistance slurry;
H. electrode connection: and G, carrying out surface nickel plating treatment on two ends of the heating body blank prepared in the step G, and then carrying out brazing extraction electrode on the part subjected to the nickel plating treatment to obtain a porous ceramic heating body finished product.
2. The process for preparing a porous ceramic heater with a mosaic structure according to claim 1, wherein: in the step E, the temperature rise rate during sintering is 1-20 ℃/min, the sintering temperature is 900-.
3. The process for preparing a porous ceramic heater with a mosaic structure according to claim 1, wherein: in the step G, the temperature rise rate during the metallization sintering is 1-5 ℃/min, the metallization sintering temperature is 800-.
4. The process for preparing a porous ceramic heater with a mosaic structure according to claim 1, wherein: in the step A, the ceramic matrix slurry consists of the following raw materials in percentage by mass:
20 percent of diatomite
Starch 35%
1 percent of nano silicon dioxide solution
44% of deionized water.
5. The process for preparing a porous ceramic heater with a mosaic structure according to claim 4, wherein: in the step A, the resistance slurry is composed of the following raw materials in percentage by mass:
40 percent of resistance sizing agent
Starch 35%
25% of organic solvent.
6. The process for preparing a porous ceramic heater with a mosaic structure according to claim 1, wherein: in the step A, the ceramic matrix slurry consists of the following raw materials in percentage by mass:
10 percent of diatomite
Starch 40%
50% of deionized water.
7. The process for preparing a porous ceramic heater with a mosaic structure according to claim 6, wherein: in the step A, the resistance slurry is composed of the following raw materials in percentage by mass:
50 percent of resistance sizing agent
Starch 40%
10% of organic solvent.
8. The process for preparing a porous ceramic heater with a mosaic structure according to claim 1, wherein: in the step A, the ceramic matrix slurry consists of the following raw materials in percentage by mass:
40 percent of diatomite
28% of starch
2 percent of nano silicon dioxide solution
30% of deionized water.
9. The process for preparing a porous ceramic heater with a mosaic structure according to claim 8, wherein: in the step A, the resistance slurry is composed of the following raw materials in percentage by mass:
30 percent of resistance sizing agent
Starch 40%
30% of organic solvent.
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| PCT/CN2018/074110 WO2019119610A1 (en) | 2017-12-21 | 2018-01-25 | Preparation process for ceramic heating body having mosaic structure |
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| WO2019119610A1 (en) | 2019-06-27 |
| CN108046834A (en) | 2018-05-18 |
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