CN116655371A - Preparation method of tin dioxide electrode and tin dioxide electrode - Google Patents
Preparation method of tin dioxide electrode and tin dioxide electrode Download PDFInfo
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- CN116655371A CN116655371A CN202310717709.2A CN202310717709A CN116655371A CN 116655371 A CN116655371 A CN 116655371A CN 202310717709 A CN202310717709 A CN 202310717709A CN 116655371 A CN116655371 A CN 116655371A
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 338
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 26
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 14
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 10
- 239000005751 Copper oxide Substances 0.000 claims description 10
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 10
- 229910000431 copper oxide Inorganic materials 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 235000019353 potassium silicate Nutrition 0.000 claims description 9
- 230000001603 reducing effect Effects 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- 229910001887 tin oxide Inorganic materials 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 41
- 229910052757 nitrogen Inorganic materials 0.000 description 21
- 239000000203 mixture Substances 0.000 description 8
- 238000007873 sieving Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000002706 hydrostatic effect Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 235000015173 baked goods and baking mixes Nutrition 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
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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
- C04B35/453—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
- C04B35/457—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/02—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/235—Heating the glass
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The application relates to the technical field of tin oxide electrodes, in particular to a preparation method of a tin dioxide electrode, which comprises the following steps: providing a tin dioxide cooked blank; and (3) preserving the temperature of the tin dioxide cooked blank at 1200-1300 ℃ for 4-6 hours under an inert atmosphere, and performing heat treatment to prepare the tin dioxide electrode. According to the preparation method of the tin dioxide electrode, the tin dioxide cooked blank is subjected to heat treatment, so that the prepared tin dioxide electrode is low in resistance, and the porosity and density of the tin dioxide cooked blank are not changed. The preparation method has the advantages of simple process, easy operation, short production period, low production cost and stable and reliable product quality, and is suitable for industrial production.
Description
Technical Field
The application relates to the technical field of tin oxide electrodes, in particular to a preparation method of a tin dioxide electrode and the tin dioxide electrode.
Background
Tin dioxide is a ceramic material with good glass erosion resistance, and can be used as an electrode material in a glass kiln. Conventional tin dioxide electrodes have a relatively high room temperature resistance, and there are techniques related to reducing the resistance by adjusting the composition of the tin dioxide electrode. However, the adjustment of the components affects the physical properties of the electrode itself, such as porosity, bulk density, etc., thereby reducing the thermal stability and erosion resistance of the tin dioxide electrode.
Therefore, there is a need for a method for preparing a tin dioxide electrode that can reduce the resistance without changing other physical properties.
Disclosure of Invention
Based on this, it is necessary to provide a method for producing a tin dioxide electrode, which is capable of reducing the resistance without changing other physical properties.
In one aspect of the present application, there is provided a method for preparing a tin dioxide electrode, comprising the steps of:
providing a tin dioxide cooked blank;
and (3) carrying out heat treatment on the tin dioxide cooked blank for 4-6 hours at 1200-1300 ℃ under an inert atmosphere to prepare the tin dioxide electrode.
In one embodiment, the method for preparing the tin dioxide electrode includes the following steps:
directly reducing the temperature to 1200-1300 ℃ after firing the tin dioxide cooked blank, preserving the heat for 4-6 hours, and carrying out heat treatment on the fired tin dioxide cooked blank;
or cooling the fired tin dioxide cooked blank to room temperature, heating the fired tin dioxide cooked blank to 1200-1300 ℃ at a heating rate of 20-25 ℃/h, and preserving heat for 4-6 h, and performing heat treatment on the fired tin dioxide cooked blank.
In one embodiment, firing the tin dioxide green comprises the steps of:
preparing a tin dioxide green body;
sintering the tin dioxide green body at a high temperature of 1400-1480 ℃ for more than or equal to 12 hours to prepare a tin dioxide cooked blank.
In one embodiment, the preparing a green tin dioxide comprises the steps of:
mixing the raw materials, and drying to prepare a drying material;
and carrying out static pressure forming on the dried material to prepare the tin dioxide green body.
In one embodiment, the mixing method is mixed grinding, and the grinding ball medium is zirconia balls; and/or the moisture of the drying material is less than or equal to 0.4 percent by mass percent.
In one embodiment, the mesh number of the drying materials is less than or equal to 60 mesh.
In one embodiment, the raw materials comprise 96-98 parts by mass of tin dioxide, 1-1.5 parts by mass of antimony oxide, 0.2-0.5 part by mass of copper oxide, 0.05-0.1 part by mass of dispersing agent and 35-40 parts by mass of water.
In one embodiment, the dispersing agent is water glass solution, and the content of sodium silicate in the water glass solution is 38-42% by mass percent.
In still another aspect, the application provides a tin dioxide electrode, which is prepared by the preparation method of the tin dioxide electrode.
In yet another aspect of the application, a glass furnace is provided comprising the tin dioxide electrode described above.
According to the preparation method of the tin dioxide electrode, the tin dioxide cooked blank is subjected to heat treatment, so that the prepared tin dioxide electrode is low in resistance, and the porosity and density of the tin dioxide cooked blank are not changed. The preparation method has the advantages of simple process, easy operation, short production period, low production cost and stable and reliable product quality, and is suitable for industrial production.
Drawings
Fig. 1 is a photograph of a green and cooked tin dioxide blank of an embodiment.
Reference numerals:
100: a tin dioxide green body; 200: tin dioxide cooked blank.
Detailed Description
In order that the application may be readily understood, a more complete description of the application will be rendered by reference to the embodiments that are illustrated below. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
In one aspect of the present application, there is provided a method for preparing a tin dioxide electrode, comprising the steps of:
firing a tin dioxide cooked blank;
and (3) carrying out heat treatment on the fired tin dioxide cooked blank for 4-6 hours at 1200-1300 ℃ under inert atmosphere to prepare the tin dioxide electrode.
The resistance of the tin dioxide electrode can be effectively reduced by controlling the heat treatment temperature within the range of 1200-1300 ℃. Specifically, the resistance of the tin dioxide electrode can be reduced by introducing nitrogen above 900 ℃, but the effect of reducing the resistance is poor when the heat treatment temperature is lower than 1200 ℃. The heat treatment temperature is controlled within the range of 1200-1300 ℃, which is favorable for avoiding the problem of poor resistance reducing effect caused by too low temperature and also for avoiding the problems of low production efficiency and too high cost caused by too high temperature. It is preferable to control the heat treatment temperature within the above range in view of both performance and cost efficiency. The heat treatment time is controlled within the range of 4-6 h, so that the problem that the resistance cannot be effectively reduced due to too short heat preservation time is solved, and the problems of low production efficiency and too high cost due to too long heat treatment time are solved. It is preferable to control the heat treatment time within the above range in view of both performance and cost efficiency.
In one example, the temperature of the heat treatment is 1200 ℃ to 1300 ℃, specifically, the temperature of the heat treatment may be 1200 ℃, 1210 ℃, 1220 ℃, 1230 ℃, 1240 ℃, 1250 ℃, 1260 ℃, 1270 ℃, 1280 ℃, 1290 ℃, or 1300 ℃.
The tin dioxide content of the tin dioxide cooked blank is less than or equal to 98 percent by mass percent. Specifically, the tin dioxide content of the tin dioxide preform may be 93%, 94%, 95%, 96%, 97%, 98% or any numerical range above.
In one example, the pressure of the heat treatment is 0.001MPa to 0.005MPa to ensure the nitrogen concentration in the furnace. Specifically, the gas pressure of the heat treatment may be in the range of 0.001MPa, 0.002MPa, 0.003MPa, 0.004MPa, 0.005MPa or any of the above values.
In one example, the inert atmosphere is nitrogen.
In one example, after the heat treatment is cooled to 900 ℃, the inert gas is stopped from being introduced, and the temperature is naturally cooled to room temperature.
Further, the nitrogen heat treatment is carried out within the temperature range of 900-1300 ℃ to achieve the effect of reducing the normal temperature resistance of the electrode, and no nitrogen is required to be introduced when the temperature is lower than 900 ℃.
In one example, the preparation method of the tin dioxide electrode comprises the following steps:
directly reducing the temperature to 1200-1300 ℃ after firing the tin dioxide cooked blank, preserving the heat for 4-6 hours, and carrying out heat treatment on the fired tin dioxide cooked blank;
in one example, the preparation method of the tin dioxide electrode comprises the following steps:
and (3) cooling the fired tin dioxide cooked blank to room temperature, heating the fired tin dioxide cooked blank to 1200-1300 ℃ at a heating rate of 20-25 ℃ per hour, preserving heat for 4-6 hours, and performing heat treatment on the fired tin dioxide cooked blank.
In one example, the heating rate may be in the range of 20 ℃/h, 21 ℃/h, 22 ℃/h, 23 ℃/h, 24 ℃/h, 25 ℃/h, or any value above.
In one example, firing the tin dioxide green compact includes the steps of:
preparing a tin dioxide green body;
sintering the tin dioxide green body at a high temperature of 1400-1480 ℃ for more than or equal to 12 hours (12-20 hours) to prepare a tin dioxide cooked blank.
Further, the high-temperature sintering time is 12-20 hours.
Specifically, the time of high temperature sintering may be 12 hours, 13 hours, 14 hours, 15 hours, 16 hours, 17 hours, 18 hours, 19 hours, 20 hours, or any range of values above.
In one example, the preparing of the green tin dioxide comprises the steps of:
mixing the raw materials, and drying to prepare a drying material;
and carrying out static pressure forming on the dried material to prepare the tin dioxide green body.
In one example, the method of mixing is a mixing mill and the milling ball media is zirconia balls.
In one example, the moisture of the drying material is less than or equal to 0.4% in mass percent. When the moisture of the drying material is more than 0.4%, the tin dioxide green body is easy to burn. Specifically, the moisture of the baked goods may be in the range of 0.1%, 0.12%, 1.16%, 0.18%, 0.2%, 0.23%, 0.25%, 0.27%, 0.3%, 0.34%, 0.36%, 0.38%, 0.4% or any of the above values.
In one example, before the step of hydrostatic forming, the method further comprises the steps of powdering and sieving the dried material, wherein the number of the sieved meshes is less than or equal to 60 meshes. Further, the mesh number of the screening is 40-60 mesh. The mesh number of screening is controlled in the range, so that the problem that powder is too coarse and difficult to sinter caused by too low mesh number can be avoided, when the powder is too coarse, the sintering temperature needs to be increased, and the tin oxide electrode is partially volatilized due to too high temperature, so that the pore density of the tin oxide electrode is influenced; and the problem that the sintering quality is affected by too fine powder which is easy to crack and is caused by too high mesh number is solved. Specifically, the mesh number of the sieving may be in the range of 40 mesh, 50 mesh, 60 mesh or any numerical value composition thereof.
In one example, the raw materials comprise 96-98 parts by mass of tin dioxide, 1-1.5 parts by mass of antimony oxide, 0.2-0.5 part by mass of copper oxide, 0.05-0.1 part by mass of dispersing agent and 35-40 parts by mass of water. The components of the raw materials are matched in a specific proportion, and the prepared tin dioxide electrode has higher firing quality.
In one example, the tin dioxide content is 96 parts to 98 parts. Specifically, the content of tin dioxide may be 96 parts, 96.2 parts, 96.5 parts, 96.6 parts, 96.9 parts, 97 parts, 97.2 parts, 97.4 parts, 97.5 parts, 97.8 parts, 98 parts, or a range of any of the above numerical values.
In one example, the content of antimony oxide is 1 part to 1.5 parts, specifically, the content of antimony oxide may be 1 part, 1.1 part, 1.2 parts, 1.3 parts, 1.4 parts, 1.5 parts, or a range of any number of the above.
In one example, the content of copper oxide is 0.2 to 0.5 parts, specifically, the content of copper oxide may be in the range of 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, or any numerical composition thereof.
In one example, the content of the dispersant is 0.05 to 0.1 part, and specifically, the content of the dispersant may be 0.05 part, 0.06 part, 0.07 part, 0.08 part, 0.09 part, 0.1 part, or a range of any of the above numerical compositions.
In one example, the water content is 35 to 40 parts, specifically, the water content may be 35 parts, 35.3 parts, 35.5 parts, 35.6 parts, 35.8 parts, 36 parts, 36.6 parts, 37 parts, 37.2 parts, 38 parts, 38.7 parts, 39 parts, 39.2 parts, 39.4 parts, 39.6 parts, 39.8 parts, 40 parts, or a range of any of the above.
In one example, the tin dioxide is a powder, and the average particle diameter D50 is 0.8 μm to 2 μm. Specifically, the average particle diameter D50 may be in the range of 0.8 μm, 0.9 μm, 1.0 μm, 1.1 μm, 1.2 μm, 1.3 μm, 1.4 μm, 1.5 μm, 1.6 μm, 1.7 μm, 1.8 μm, 1.9 μm, 2.0 μm or any numerical composition thereof. In one example, the antimony oxide and copper oxide are technical grade powders.
In one example, the dispersing agent is a water glass solution, and the content of sodium silicate in the water glass solution is 38% -42% by mass. Specifically, the sodium silicate content of the water glass solution may be in the range of 38%, 39%, 40%, 41%, 42% or any of the above numerical compositions.
In one example, the preparation method of the tin dioxide electrode comprises the following steps:
s100: the raw materials of 96-98 parts of tin dioxide, 1-1.5 parts of antimony oxide, 0.2-0.5 part of copper oxide, 0.05-0.1 part of dispersing agent and 35-40 parts of water are mixed and ground, and the grinding ball medium is zirconia balls.
S110: and (3) drying the mixed and ground mixture to prepare a drying material, wherein the moisture of the drying material is less than or equal to 0.4% in percentage by mass.
S120: pulverizing the dried material, sieving, and sieving with the mesh number less than or equal to 60 mesh.
S130: and carrying out hydrostatic forming on the screened dried material to prepare a tin dioxide green body.
S140: sintering the tin dioxide green body at the high temperature of 1400-1480 ℃ for 12-20 hours to prepare a tin dioxide cooked blank.
S150: after the tin dioxide cooked blank is fired, the temperature is directly reduced to 1200-1300 ℃, nitrogen is continuously introduced into the furnace, the nitrogen pressure is kept at 0.001-0.005 MPa, the temperature is kept for 4-6 hours at 1200-1300 ℃, the fired tin dioxide cooked blank is subjected to heat treatment, after the temperature is reduced to 900 ℃, the introduction of nitrogen is stopped, and the tin dioxide electrode is prepared by natural cooling to the room temperature.
In one example, the preparation method of the tin dioxide electrode comprises the following steps:
s200: the raw materials of 96-98 parts of tin dioxide, 1-1.5 parts of antimony oxide, 0.2-0.5 part of copper oxide, 0.05-0.1 part of dispersing agent and 35-40 parts of water are mixed and ground, and the grinding ball medium is zirconia balls.
S210: and (3) drying the mixed and ground mixture to prepare a drying material, wherein the moisture of the drying material is less than or equal to 0.4% in percentage by mass.
S220: pulverizing the dried material, sieving, and sieving with the mesh number less than or equal to 60 mesh.
S230: and carrying out hydrostatic forming on the screened dried material to prepare a tin dioxide green body.
S240: sintering the tin dioxide green body at the high temperature of 1400-1480 ℃ for 12-20 hours to prepare a tin dioxide cooked blank.
S250: cooling the fired tin dioxide cooked blank to room temperature, heating the fired tin dioxide cooked blank to 1200-1300 ℃ at a heating rate of 20-25 ℃/h, continuously introducing nitrogen into the furnace, keeping the nitrogen pressure at 0.001-0.005 MPa, preserving the temperature at 1200-1300 ℃ for 4-6 hours, performing heat treatment on the fired tin dioxide cooked blank, cooling to 900 ℃, stopping introducing nitrogen, and naturally cooling to room temperature to prepare the tin dioxide electrode.
In one example, the preparation method of the tin dioxide electrode comprises the following steps:
s300: providing a tin dioxide cooked blank;
s310: and (3) cooling the tin dioxide cooked blank to room temperature, heating the fired tin dioxide cooked blank to 1300 ℃ at a heating rate of 20-25 ℃/h, continuously introducing nitrogen into the furnace, keeping the nitrogen pressure at 0.001-0.005 MPa, preserving the temperature at 1200-1300 ℃ for 4-6 hours, performing heat treatment on the fired tin dioxide cooked blank, cooling to 900 ℃, stopping introducing nitrogen, and naturally cooling to room temperature to prepare the tin dioxide electrode.
In still another aspect, the application provides a tin dioxide electrode, which is prepared by the preparation method of the tin dioxide electrode.
In yet another aspect of the application, a glass furnace is provided comprising the tin dioxide electrode described above.
According to the preparation method of the tin dioxide electrode, the tin dioxide cooked blank is subjected to heat treatment, so that the prepared tin dioxide electrode is low in resistance, and the porosity and density of the tin dioxide cooked blank are not changed. The preparation method has the advantages of simple process, easy operation, short production period, low production cost and stable and reliable product quality, and is suitable for industrial production. The preparation method of the tin dioxide electrode provided by the application is further described by the specific examples.
Example 1:
the specific preparation process of the tin dioxide electrode in this embodiment is as follows:
and (3) finely grinding the surfaces of tin dioxide cooked blanks 1# and 2# with the size of 100 x 150mm, drying, placing in an atmosphere furnace, heating the tin dioxide cooked blanks to 1300 ℃ at a heating rate of 20 ℃/hour, continuously introducing nitrogen into the furnace, keeping the pressure of the nitrogen at 0.001MPa, preserving the heat for 4 hours at 1300 ℃, performing heat treatment on the fired tin dioxide cooked blanks, cooling to 900 ℃, stopping introducing the nitrogen, and naturally cooling to room temperature to obtain the tin dioxide electrodes 1# and 2#.
The porosity and density of the above-mentioned tin dioxide blank and tin dioxide electrode were tested by referring to the test method of bulk density and apparent porosity of the GBT2997-2000 compact shaped refractory product, and the ordinary temperature resistance of the above-mentioned tin dioxide blank and tin dioxide electrode was tested by using a Victor VC89C multimeter, and the test results are shown in Table 1.
Table 1 performance test
| Sample of | Porosity (%) | Density (g/cm) 3 ) | Normal temperature resistor (omega) |
| Tin dioxide cooked blank 1# | 0.6 | 6.63 | 130000 |
| Tin dioxide electrode 1 #) | 0.6 | 6.63 | 5.4 |
| Tin dioxide cooked blank 2# | 0.59 | 6.64 | 110000 |
| Tin dioxide electrode 2 #) | 0.6 | 6.64 | 3.8 |
Example 2:
the specific preparation process of the tin dioxide electrode in this embodiment is as follows:
1. the raw materials of 98 parts of tin dioxide, 1.5 parts of antimony oxide, 0.5 part of copper oxide, 0.1 part of water glass with the concentration of 40wt% and 40 parts of water are mixed by adopting a mixing grinding mode, and the grinding ball medium is zirconia balls.
2. And (3) drying the mixed solution to prepare a drying material, wherein the moisture of the drying material is 0.18%.
3. Pulverizing the above drying materials, sieving with 60 mesh sieve, and performing static pressure molding under 220MPa to obtain tin dioxide green body.
4. And placing the tin dioxide green body with the size of 122 x 180mm in an atmosphere furnace, and sintering at the high temperature of 1460 ℃ for 12 hours to prepare a tin dioxide cooked blank.
5. After the tin dioxide cooked blank is fired, the temperature is directly reduced to 1300 ℃, nitrogen is continuously introduced into the furnace, the nitrogen pressure is kept at 0.001MPa, the temperature is kept for 4 hours at 1300 ℃, the fired tin dioxide cooked blank is subjected to heat treatment, the temperature is reduced to 900 ℃, the introduction of nitrogen is stopped, and the nitrogen is naturally cooled to the room temperature, so that the tin dioxide electrode is prepared.
The porosity and density of the above-mentioned tin dioxide blank and tin dioxide electrode were tested by referring to the test method of bulk density and apparent porosity of the GBT2997-2000 compact shaped refractory product, and the ordinary temperature resistance of the above-mentioned tin dioxide blank and tin dioxide electrode was tested by using a Victor VC89C multimeter, and the test results are shown in Table 2.
Table 2 performance test
| Sample of | Porosity (%) | Density (g/cm) 3 ) | Normal temperature resistor (omega) |
| Example 2 | 0.58 | 6.65 | 8.2 |
Comparative example 1
The specific preparation process of the tin dioxide electrode of the comparative example is as follows:
1. the raw materials of 98 parts of tin dioxide, 1.5 parts of antimony oxide, 0.5 part of copper oxide, 0.1 part of water glass with the concentration of 40wt% and 40 parts of water are mixed by adopting a mixing grinding mode, and the grinding ball medium is zirconia balls.
2. And (3) drying the mixed solution to prepare a drying material, wherein the moisture of the drying material is 0.18%.
3. Pulverizing the above drying materials, sieving with 60 mesh sieve, and performing static pressure molding under 220MPa to obtain tin dioxide green body.
4. The above-mentioned tin dioxide green body as in example 2 was placed in a general electric furnace, sintered at a high temperature of 1460 ℃ for 12 hours, and naturally cooled to room temperature to prepare a tin dioxide electrode.
The porosity and density of the above-mentioned tin dioxide blank and tin dioxide electrode were tested by referring to the test method of bulk density and apparent porosity of the GBT2997-2000 compact shaped refractory product, and the ordinary temperature resistance of the above-mentioned tin dioxide blank and tin dioxide electrode was tested by using a Victor VC89C multimeter, and the test results are shown in Table 3.
Table 3 performance test
| Sample of | Porosity (%) | Density (g/cm) 3 ) | Normal temperature resistor (omega) |
| Comparative example 1 | 0.59 | 6.64 | 98000 |
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present application, which facilitate a specific and detailed understanding of the technical solutions of the present application, but are not to be construed as limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. It should be understood that, based on the technical solutions provided by the present application, those skilled in the art obtain technical solutions through logical analysis, reasoning or limited experiments, all of which are within the scope of protection of the appended claims. The scope of the patent of the application should therefore be determined with reference to the appended claims, which are to be construed as in accordance with the doctrines of claim interpretation.
Claims (10)
1. The preparation method of the tin dioxide electrode is characterized by comprising the following steps of:
providing a tin dioxide cooked blank;
and (3) preserving the temperature of the tin dioxide cooked blank at 1200-1300 ℃ for 4-6 hours under an inert atmosphere, and performing heat treatment to prepare the tin dioxide electrode.
2. The method for preparing a tin dioxide electrode according to claim 1, comprising the steps of:
directly reducing the temperature to 1200-1300 ℃ after firing the tin dioxide cooked blank, preserving the heat for 4-6 hours, and carrying out heat treatment on the fired tin dioxide cooked blank;
or cooling the fired tin dioxide cooked blank to room temperature, heating the fired tin dioxide cooked blank to 1200-1300 ℃ at a heating rate of 20-25 ℃/h, and preserving heat for 4-6 h, and performing heat treatment on the fired tin dioxide cooked blank.
3. The method of preparing a tin dioxide electrode according to claim 2, wherein firing the tin dioxide green compact comprises the steps of:
preparing a tin dioxide green body;
sintering the tin dioxide green body at a high temperature of 1400-1480 ℃ for more than or equal to 12 hours to prepare a tin dioxide cooked blank.
4. A method of preparing a tin dioxide electrode according to claim 3, wherein the preparing of a tin dioxide green body comprises the steps of:
mixing the raw materials, and drying to prepare a drying material;
and carrying out static pressure forming on the dried material to prepare the tin dioxide green body.
5. The method for preparing a tin dioxide electrode according to claim 4, wherein the mixing method is mixed grinding, and the grinding ball medium is zirconia balls; and/or the moisture of the drying material is less than or equal to 0.4 percent by mass percent.
6. The method for producing a tin dioxide electrode according to claim 4, wherein the number of the baked materials is 60 mesh or less.
7. The method for producing a tin dioxide electrode according to any one of claims 1 to 6, wherein the raw materials include 96 to 98 parts by mass of tin dioxide, 1 to 1.5 parts by mass of antimony oxide, 0.2 to 0.5 part by mass of copper oxide, 0.05 to 0.1 part by mass of dispersant and 35 to 40 parts by mass of water.
8. The method for preparing a tin dioxide electrode according to claim 7, wherein the dispersing agent is a water glass solution, and the content of sodium silicate in the water glass solution is 38% -42% by mass.
9. A tin dioxide electrode, characterized in that it is prepared by the method for preparing a tin dioxide electrode according to any one of claims 1 to 8.
10. A glass kiln comprising the tin dioxide electrode of claim 9.
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Cited By (1)
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| CN117285345A (en) * | 2023-11-24 | 2023-12-26 | 淄博工陶新材料集团有限公司 | Tin oxide ceramic electrode and preparation method thereof |
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