CN114932376B - Hollow fiber electrode batch heat treatment device, manufacturing method and application - Google Patents
Hollow fiber electrode batch heat treatment device, manufacturing method and application Download PDFInfo
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- CN114932376B CN114932376B CN202210494162.XA CN202210494162A CN114932376B CN 114932376 B CN114932376 B CN 114932376B CN 202210494162 A CN202210494162 A CN 202210494162A CN 114932376 B CN114932376 B CN 114932376B
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 294
- 239000012510 hollow fiber Substances 0.000 title claims abstract description 225
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 50
- 238000005192 partition Methods 0.000 claims abstract description 126
- 238000003466 welding Methods 0.000 claims abstract description 48
- 239000002994 raw material Substances 0.000 claims abstract description 41
- 238000005452 bending Methods 0.000 claims abstract description 15
- 238000005520 cutting process Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 84
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 70
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 55
- 229910052786 argon Inorganic materials 0.000 claims description 35
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 27
- 239000010949 copper Substances 0.000 claims description 25
- 239000010936 titanium Substances 0.000 claims description 21
- 229910052719 titanium Inorganic materials 0.000 claims description 21
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 18
- 229910052721 tungsten Inorganic materials 0.000 claims description 18
- 239000010937 tungsten Substances 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 230000000630 rising effect Effects 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 238000005266 casting Methods 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 3
- 229910001887 tin oxide Inorganic materials 0.000 claims description 3
- 239000013077 target material Substances 0.000 abstract description 11
- 238000013461 design Methods 0.000 abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 230000001413 cellular effect Effects 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 238000001354 calcination Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
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- 239000004408 titanium dioxide Substances 0.000 description 4
- 230000003321 amplification Effects 0.000 description 3
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- 238000011161 development Methods 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000000452 restraining effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 241000561734 Celosia cristata Species 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 210000001520 comb Anatomy 0.000 description 1
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- 239000002803 fossil fuel Substances 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a batch heat treatment device for hollow fiber electrodes, a manufacturing method and application, wherein the manufacturing method comprises the following steps: s1, mechanically cutting and bending raw materials into a box body, and welding and forming; s2, fixing the periphery of the box body; s3, arranging a plurality of isolating layers in the box body, and then placing the box body in a tube furnace for roasting treatment to obtain the heat treatment device. The hollow fiber electrode batch heat treatment device manufactured by the manufacturing method is applied to batch heat treatment of the hollow fiber electrode. The invention provides the device which is simple in design, simple and convenient to operate and capable of being rapidly and efficiently used for the batch heat treatment of the hollow fiber electrodes, and partition layers with different structural forms are arranged in the device, so that the uniformity and the repeatability of the heat treatment of target materials are ensured, the target materials can be rapidly and massively subjected to the heat treatment, and the production efficiency is greatly improved.
Description
Technical Field
The invention belongs to the technical field of chemical engineering and processes, and particularly relates to a batch heat treatment device for hollow fiber electrodes, a manufacturing method and application thereof.
Background
The ever-increasing total energy demand and the over-exploitation of fossil fuels results in global CO 2 The total amount of emissions continues to rise, causing increasingly serious environmental problems. The method combines the development and utilization of renewable energy sources with rapid development, develops the electrochemical conversion synthesis chemicals driven by renewable electric energy, and has important significance for improving the energy structure, driving economic and social sustainable development and industrial upgrading.
Compared with the traditional electrode catalyst prepared by the conductive agent and the adhesive, the self-supporting hollow fiber electrode has good conductivity and catalytic activity, and the unique structure can be used as an ideal place for the reaction of gas and liquid raw materials, so that the contact of reaction media is fully promoted, and the diffusion and migration of reactants and products are facilitated. Meanwhile, the composite material has good mechanical strength and stability, can maintain stable structure and performance in long-period test, and has great industrial application potential. However, the high aspect ratio of the hollow fiber electrode is not ideal in the efficiency and the product yield of the large-scale heat treatment. Therefore, the design of the system capable of rapidly and efficiently carrying out batch heat treatment on the hollow fiber electrode is beneficial to improving the production efficiency, ensuring the uniformity and the repeatability of the electrode material and further improving the industrial application prospect.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a batch heat treatment device for hollow fiber electrodes, a manufacturing method and an application thereof, which are used for solving the problems that the prior art cannot perform efficient batch heat treatment on the hollow fiber electrodes, resulting in low production efficiency, and cannot ensure uniformity and repeatability of electrode materials.
To achieve the above and other related objects, the present invention provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, the method comprising the steps of:
s1, mechanically cutting and bending raw materials into a box body, and welding and forming;
s2, fixing the periphery of the box body;
s3, arranging a plurality of isolating layers in the box body, and then placing the box body in a tube furnace for roasting treatment to obtain the heat treatment device.
Preferably, the raw material in the step S1 is one or a combination of a titanium plate, a titanium mesh, a tungsten plate and a tungsten mesh.
Preferably, the thickness of the raw material in step S1 is 0.1 to 2.5mm.
Preferably, the shape of the box in the step S1 is one of cuboid, cylinder, semi-cylinder, 3/4 cylinder, and 2/3 cylinder.
Preferably, the welding method in the step S1 is one or a combination of welding rod arc welding, argon arc welding and laser welding.
Preferably, the fixing manner in the step S2 is one of titanium rod constraint fixing, tungsten rod constraint fixing and mechanical casting fixing.
Preferably, in step S3, the distance between two adjacent partition layers is 5-10 mm.
Preferably, the shape of the isolating layer in step S3 is one or a combination of zigzag, corrugated and honeycomb.
Preferably, in step S3, the setting direction of the isolating layer is one or more of a transverse isolating layer, a longitudinal isolating layer and an oblique isolating layer.
Preferably, the roasting atmosphere in the step S3 is oxygen or air atmosphere, and the flow rate of the roasting atmosphere is 100-300 mL/min.
Preferably, the temperature rising rate of the roasting in the step S3 is 1-20 ℃/min, the roasting temperature is 400-1000 ℃, and the roasting time is 4-12 h.
The invention also provides a hollow fiber electrode batch heat treatment device manufactured by the manufacturing method of the hollow fiber electrode batch heat treatment device, which comprises the following steps:
the box body is in a cuboid shape, a cylinder shape, a semi-cylinder shape, a 3/4 cylinder shape and a 2/3 cylinder shape, and an anti-deformation structure is fixed along the length direction of the box body;
The partition layer is provided with a plurality of partition layers, a plurality of partition layers are uniformly arranged in the box body, and the partition layers are zigzag, corrugated or honeycomb-shaped.
The invention also provides application of the hollow fiber electrode batch heat treatment device, which is applied to batch heat treatment of the hollow fiber electrode, and specifically comprises the following steps:
a1, providing the hollow fiber electrode batch heat treatment device;
a2, sequentially placing hollow fiber electrode blanks pre-filled in a liner tube into the partition layers of the heat treatment device in batches;
a3, placing the heat treatment device with the hollow fiber electrode green bodies in a tube furnace, performing first heat treatment in an air atmosphere, and performing second heat treatment in a gas atmosphere to obtain a batch of hollow fiber electrodes.
Preferably, in the step A2, the hollow fiber electrode blank is made of one of silver, copper, iron, cobalt, nickel, titanium, bismuth oxide and tin oxide;
the length of the hollow fiber electrode green body is 100-200 mm.
Preferably, the atmosphere of the first heat treatment in the step A3 is air; the flow rate of the atmosphere of the first heat treatment is 100-200 mL/min; the heating rate of the first heat treatment is 1-5 ℃/min; the temperature of the first heat treatment is 550-600 ℃; the time of the first heat treatment is 4-6 h.
Preferably, the atmosphere of the second heat treatment in the step A3 is one of hydrogen, argon and hydrogen/argon mixture; the flow rate of the atmosphere of the second heat treatment is 50-1000 mL/min; the temperature rising rate of the second heat treatment is 1-20 ℃/min, the temperature of the second heat treatment is 100-1600 ℃, and the time of the second heat treatment is 0.5-24 h.
As described above, the hollow fiber electrode batch heat treatment device, the manufacturing method and the application of the invention have the following beneficial effects:
the invention provides a device which is simple in design, simple and convenient to operate and capable of being rapidly and efficiently used for batch heat treatment of hollow fiber electrodes, adopts high-melting-point, low-mass-density, strong bending ductility, strong corrosion resistance and strong oxidation resistance metallic titanium or tungsten as a raw material of the device, is formed by mechanical cutting, bending welding and fixing, is internally provided with partition layers with different structural forms, ensures that the device can keep stable under high-temperature oxidation or reduction conditions, does not pollute target materials, controls the uniformity of a heat radiation field and a gas flow field in the heat treatment process, ensures the uniformity and repeatability of heat treatment of the target materials, and can rapidly and massively heat treat the target materials, thereby greatly improving the production efficiency.
The batch heat treatment device can treat hundreds to thousands of hollow fiber electrode samples in batches at a time, effectively simplify the batch production flow of the hollow fiber electrodes, improve the production efficiency, form an efficient, stable and low-cost preparation process amplification scheme, promote the large-scale production and application of the hollow fiber electrodes, can be widely applied to the production process of various hollow fiber electrodes, and has extremely high application prospect.
Drawings
FIG. 1 is a front view showing a hollow fiber electrode batch heat treatment apparatus in embodiment 5 of the present invention.
FIG. 2 is a left side view showing a hollow fiber electrode batch heat treatment apparatus in embodiment 5 of the present invention.
Description of element reference numerals
10. A case; 20. a barrier layer.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
Please refer to fig. 1-2. It should be noted that, the illustrations provided in the present embodiment merely illustrate the basic concept of the present invention by way of illustration, and only the components related to the present invention are shown in the drawings and are not drawn according to the number, shape and size of the components in actual implementation, and the form, number and proportion of the components in actual implementation may be arbitrarily changed, and the layout of the components may be more complex.
The invention provides a device which is simple in design, simple and convenient to operate and capable of being rapidly and efficiently used for batch heat treatment of hollow fiber electrodes, adopts high-melting-point, low-mass-density, strong bending ductility, strong corrosion resistance and strong oxidation resistance metallic titanium or tungsten as a raw material of the device, is formed by mechanical cutting, bending welding and fixing, and is internally provided with partition layers with different structural forms, so that the device can be kept stable under high-temperature oxidation or reduction conditions, pollution to target materials is avoided, the uniformity of a heat radiation field and a gas flow field in the heat treatment process is controlled, the uniformity and the repeatability of the heat treatment of the target materials are ensured, and the heat treatment of the target materials can be rapidly and massively carried out, thereby greatly improving the production efficiency; the batch heat treatment device can treat hundreds to thousands of hollow fiber electrode samples in batches at a time, effectively simplify the batch production flow of the hollow fiber electrodes, improve the production efficiency, form an efficient, stable and low-cost preparation process amplification scheme, promote the large-scale production and application of the hollow fiber electrodes, can be widely applied to the production process of various hollow fiber electrodes, and has extremely high application prospect.
The invention provides a manufacturing method of a hollow fiber electrode batch heat treatment device, which comprises the following steps:
s1, mechanically cutting and bending raw materials into a box body 10, and welding and forming;
s2, fixing the outer periphery of the box body 10;
s3, arranging a plurality of isolating layers 20 in the box body 10, and then placing the box body in a tube furnace for roasting treatment to prepare the heat treatment device.
As an example, in step S1, the raw material is one or a combination of a titanium plate, a titanium mesh, a tungsten plate, and a tungsten mesh.
Specifically, the metal titanium or the metal tungsten has high melting point, strong corrosion resistance and strong oxidation resistance, and the metal titanium or the metal tungsten is used as a raw material of the box body 10, so that the electrode material is not affected no matter whether the metal titanium or the metal tungsten is oxidized or reduced when the metal titanium or the metal tungsten is subjected to heat treatment of the hollow fiber electrode sample; preferably, the raw material is a titanium mesh with a pore size of 2×4mm.
By way of example, the thickness of the raw material in step S1 is 0.1 to 2.5mm, such as 0.1mm, 0.5mm, 1.0mm, 1.5mm, 2.0mm, 2.5mm, etc.
Preferably, the thickness of the raw material is 1.0 to 1.5mm, such as 1.0mm, 1.1mm, 1.2mm, 1.3mm, 1.4mm, 1.5mm, etc.
By way of example, the length of the raw material in step S1 is 400 to 700mm, such as 400mm, 500mm, 600mm, 700mm, etc.
Specifically, the length of the raw material to be used is determined according to the length of the hollow fiber electrode green body to be actually treated, and is not excessively limited herein, and preferably the length of the raw material is 500 to 650mm, such as 500mm, 550mm, 600mm, 650mm, etc.
As an example, the shape of the case 10 in step S1 is one of a rectangular parallelepiped, a cylinder, a half cylinder, a 3/4 cylinder, and a 2/3 cylinder.
Preferably, the case 10 is in the shape of a 3/4 cylinder, as shown with reference to FIGS. 1 and 2.
As an example, the method of welding in step S1 is one or a combination of welding rod arc welding, argon arc welding, and laser welding.
Preferably, the welding method is argon arc welding.
As an example, the fixing manner in step S2 is one of titanium rod constraint fixing, tungsten rod constraint fixing, and mechanical casting fixing.
Specifically, the titanium rod constraint fixing or the tungsten rod constraint fixing is to wind the titanium rod or the tungsten rod around the box body 10; preferably, the fixing mode is titanium rod constraint fixing; more preferably, the shape of the titanium rod used for the restraint fixation is circular arc.
As an example, the distance between adjacent two partition layers 20 in step S3 is 5 to 10mm, such as 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, etc.
Preferably, the distance between two adjacent partition layers 20 is 6 to 8mm, such as 6mm, 6.5mm, 7mm, 7.5mm, 8mm, etc.
As an example, the shape of the isolation layer 20 in step S3 is one or a combination of zigzag, corrugated, honeycomb.
Preferably, the shape of the partition layer 20 is honeycomb-shaped.
As an example, the arrangement direction of the partition 20 in step S3 is one or more of a lateral partition, a longitudinal partition, and an oblique partition.
Specifically, the arrangement of the partition layer 20 can improve the heating uniformity of the material and the sufficiency of contact with the air flow in the heat treatment process, and meanwhile, the arrangement of the partition layer 20 can divide the internal space of the box body 10 into a plurality of independent spaces, so that the heat treatment operation can be rapidly performed in a large scale; preferably, the partition layer 20 is disposed in a direction of lateral partition.
As an example, the roasting atmosphere in the step S3 is oxygen or air, and the roasting atmosphere flow rate is 100-300 mL/min, such as 100mL/min, 150mL/min, 200mL/min, 250mL/min, 300mL/min, etc.
Preferably, the roasting atmosphere flow rate is 100-200 mL/min, such as 100mL/min, 120mL/min, 140mL/min, 160mL/min, 180mL/min, 200mL/min, etc.
As an example, the temperature rising rate of the firing in step S3 is 1 to 20 ℃/min, such as 1 ℃/min, 2 ℃/min, 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min, etc., the firing temperature is 400 to 1000 ℃, such as 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃, etc., and the firing time is 4 to 12 hours, such as 4 hours, 6 hours, 8 hours, 10 hours, 12 hours, etc.
Specifically, a dense oxide layer is generated on the surface of the raw material through high-temperature roasting; preferably, the temperature rise rate of the calcination is 1 to 10 ℃/min, such as 1 ℃/min, 3 ℃/min, 5 ℃/min, 7 ℃/min, 9 ℃/min, 10 ℃/min, etc., the calcination temperature is 600 to 800 ℃, such as 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃, etc., and the calcination time is 6 to 8 hours, such as 6 hours, 6.5 hours, 7 hours, 7.5 hours, 8 hours, etc.
The invention also provides a batch heat treatment device for the hollow fiber electrodes, which is manufactured by adopting the manufacturing method, and comprises the following steps: the box body 10 and the partition layer 20, wherein the box body 10 is in a cuboid shape, a cylinder shape, a semi-cylinder shape, a 3/4 cylinder shape and a 2/3 cylinder shape, and an anti-deformation structure is fixed along the length direction of the box body 10; the isolating layers 20 are provided in plurality, the isolating layers 20 are uniformly arranged in the box body 10, and the isolating layers 20 are zigzag, corrugated or honeycomb.
In order to better understand the device and the method for batch heat treatment of the hollow fiber electrodes, the invention also provides an application of the device for batch heat treatment of the hollow fiber electrodes, which is applied to batch heat treatment of the hollow fiber electrodes and specifically comprises the following steps:
A1, providing the hollow fiber electrode batch heat treatment device;
a2, placing hollow fiber electrode blanks pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches in sequence;
and A3, placing the heat treatment device with the hollow fiber electrode green bodies in a tube furnace, performing primary heat treatment in an air atmosphere, and performing secondary heat treatment in a gas atmosphere to obtain the hollow fiber electrodes in batches.
As an example, the hollow fiber electrode green body in the step A2 is made of one of silver, copper, iron, cobalt, nickel, titanium, bismuth oxide, and tin oxide; the length of the hollow fiber electrode green body is 100-200 mm, such as 100mm, 120mm, 140mm, 160mm, 180mm, 200mm and the like; preferably, the length of the hollow fiber electrode green body is 160mm and 180mm.
Specifically, the hollow fiber electrode soft body is straightened, dried, kept stand and then cut to obtain cut hollow fiber electrode blanks, the hollow fiber electrode blanks are filled into corresponding liners and subjected to subsequent heat treatment, and in the invention, the hollow fiber electrode blanks pre-filled in the liners are placed in a heat treatment device to be subjected to heat treatment.
As an example, the atmosphere of the first heat treatment in step A3 is air; the flow rate of the atmosphere for the first heat treatment is 100-200 mL/min, such as 100mL/min, 120mL/min, 140mL/min, 160mL/min, 180mL/min, 200mL/min, etc.; the heating rate of the first heat treatment is 1-5 ℃/min, such as 1 ℃/min, 2 ℃/min, 3 ℃/min, 4 ℃/min, 5 ℃/min and the like; the temperature of the first heat treatment is 550-600deg.C, such as 550 deg.C, 560 deg.C, 570 deg.C, 580 deg.C, 590 deg.C, 600 deg.C, etc.; the time of the first heat treatment is 4-6 h, such as 4h, 4.5h, 5h, 5.5h, 6h and the like.
Specifically, the first heat treatment is an oxidation process in air so as to sufficiently remove organic impurities in the hollow fiber electrode green body while causing sintering of the metal particles.
As an example, the atmosphere of the second heat treatment in step A3 is one of hydrogen, argon, and a hydrogen/argon mixture; the flow rate of the atmosphere of the second heat treatment is 50-1000 mL/min, such as 50mL/min, 100mL/min, 300mL/min, 500mL/min, 700mL/min, 900mL/min, 1000mL/min, etc.; the temperature rising rate of the second heat treatment is 1-20 ℃/min, such as 1 ℃/min, 3 ℃/min, 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and the like, the temperature of the second heat treatment is 100-1600 ℃, such as 100 ℃, 300 ℃, 600 ℃, 900 ℃, 1200 ℃, 1500 ℃, 1600 ℃ and the like, and the time of the second heat treatment is 0.5-24 h, such as 0.5h, 1h, 5h, 10h, 15h, 20h, 24h and the like.
Wherein the hydrogen/argon mixture gas comprises 10% of hydrogen and 90% of argon by volume fraction; preferably, the flow rate of the atmosphere of the second heat treatment is 100-200 mL/min, such as 100mL/min, 120mL/min, 140mL/min, 160mL/min, 180mL/min, 200mL/min, etc.; the temperature rising rate of the second heat treatment is 1-5 ℃/min, such as 1mL/min, 2mL/min, 3mL/min, 4mL/min, 5mL/min and the like, the temperature of the second heat treatment is 600-800 ℃, such as 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃ and the like, and the time of the second heat treatment is 6-8 h, such as 6h, 6.5h, 7h, 7.5h, 8h and the like.
For a better understanding of the apparatus, method of making, and use of the present invention for batch heat treatment of hollow fiber electrodes, the present invention is described below with reference to examples, which are merely illustrative and not intended to limit the invention in any way.
Example 1
The embodiment provides a manufacturing method of a hollow fiber electrode batch heat treatment device, which specifically comprises the following steps:
s1, selecting a titanium plate with the thickness of 1.0mm and the length of 500mm as a raw material, mechanically cutting, bending into a rectangular box body 10, and welding and forming by adopting a welding rod arc welding method;
s2, in order to prevent deformation, shaping and fixing are carried out on the periphery of the box body 10 by using mechanical casting;
s3, arranging a plurality of longitudinally distributed isolating layers 20 in the box body 10, and then placing the isolating layers in a tube furnace for roasting treatment to obtain a heat treatment device; wherein, the interval between every two adjacent partition layers 20 is 6mm, and the partition layers 20 are zigzag; the calcination treatment is to heat up from 20 ℃ to 600 ℃ at a heating rate of 2 ℃/min under an air flow rate of 200ml/min, and keep the temperature for 6 hours, so as to produce a dense titanium dioxide oxide layer on the surface of the box body 10.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of cuboid shape, partition layer 20 vertically distributes in box body 10 and sets up, and partition layer 20 is the zigzag.
The batch heat treatment device for the hollow fiber electrode in the embodiment is applied to batch heat treatment of the Ag hollow fiber electrode, and specifically comprises the following steps:
a1, providing a hollow fiber electrode batch heat treatment device in the embodiment;
a2, placing the Ag hollow fiber electrode blanks with the length of 160mm pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches in sequence;
a3, placing a heat treatment device with the hollow fiber electrode green body in a tubular furnace, performing primary heat treatment at a heating rate of 1 ℃/min to 600 ℃ for 6 hours under the atmosphere with an air flow rate of 100mL/min so as to sufficiently remove organic impurities in the green body and simultaneously cause sintering of silver particles, and performing secondary heat treatment at a heating rate of 1 ℃/min to 300 ℃ for 4 hours under the atmosphere with a hydrogen/argon mixed gas flow rate of 100mL/min to obtain batches of Ag hollow fiber electrodes.
In the embodiment, 265 Ag hollow fiber electrodes processed in a single batch are achieved, and the conductivity and the strength of the Ag hollow fiber electrodes with more than 90% meet the requirements.
Example 2
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 1 in that: in the step S1, a titanium mesh with the thickness of 1.5mm, the length of 650mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a cylindrical box body 10, and is welded and formed by an argon arc welding method; in step S2, in order to prevent deformation, a titanium rod is used for constraint fixation on the periphery of the box 10; in the step S3, a plurality of isolating layers 20 which are transversely distributed are arranged in the box body 10, and the constant temperature time of the roasting treatment is 8 hours; other methods and steps are the same as those in embodiment 1, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of cylinder form, the partition layer 20 transversely distributes and sets up in the inside box body 10, and the partition layer 20 is the zigzag.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Ag hollow fiber electrodes, and the specific steps are different from those in embodiment 1 in that: the heating rate of the first heat treatment in the step A3 is 2 ℃/min, the constant temperature time of the second heat treatment is 6h, and other steps and methods are the same as those in the embodiment 1, and are not repeated here.
In the embodiment, the number of the Ag hollow fiber electrodes processed in a single batch is up to 460, and the conductivity and the strength of the Ag hollow fiber electrodes with the number of more than 92% meet the requirements.
Example 3
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 1 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 500mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a cylindrical box body 10, and is welded and formed by an argon arc welding method; in step S2, in order to prevent deformation, a titanium rod is used for constraint fixation on the periphery of the box 10; in the step S3, uniformly distributed partition layers 20 are arranged in the box body 10, the distance between every two adjacent partition layers 20 is 8mm, the partition layers 20 are honeycomb-shaped, and the constant temperature time of roasting treatment is 8 hours; other methods and steps are the same as those in embodiment 1, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: a cylindrical case 10 and a partition layer 20, wherein the partition layer 20 is honeycomb-shaped.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Ag hollow fiber electrodes, and the specific steps are different from those in embodiment 1 in that: the first heat treatment in the step A3 is to keep the temperature for 6 hours from the heating rate of 2 ℃/min to 600 ℃ under the atmosphere with the air flow rate of 200mL/min, and the second heat treatment is to keep the temperature for 4 hours from the heating rate of 1 ℃/min to 300 ℃ under the atmosphere with the hydrogen/argon mixed gas flow rate of 200 mL/min; other steps and methods are the same as those in embodiment 1, and will not be described here.
In the embodiment, 340 Ag hollow fiber electrodes processed in a single batch are achieved, and the conductivity and the strength of the Ag hollow fiber electrodes with the concentration of more than 96% meet the requirements.
Example 4
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 1 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 500mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a rectangular box body 10, and is welded and formed by an argon arc welding method; in step S2, in order to prevent deformation, the outer periphery of the case 10 is fixed by mechanical casting; in the step S3, the partition layers 20 which are obliquely distributed are arranged in the box body 10, the distance between every two adjacent partition layers 20 is 10mm, the partition layers 20 are corrugated, and the constant temperature time of roasting treatment is 8 hours; other methods and steps are the same as those in embodiment 1, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of cuboid shape, the partition layer 20 is in the inside slant distribution of box body 10, and the partition layer 20 is the ripple shape.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Ag hollow fiber electrodes, and the specific steps are different from those in embodiment 1 in that: the length of the Ag hollow fiber electrode blank in the step A2 is 140mm; the heating rate of the first heat treatment in the step A3 is 5 ℃/min, the heating rate of the second heat treatment is 2 ℃/min, the constant temperature time is 6h, and other steps and methods are the same as those in the embodiment 1, and are not repeated here.
In this embodiment, 260 Ag hollow fiber electrodes processed in a single batch have conductivity and strength which meet the requirements of more than 93% of Ag hollow fiber electrodes.
Example 5
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 1 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 650mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a 3/4 cylindrical box body 10, and the box body is welded and formed by adopting an argon arc welding method; in step S2, in order to prevent deformation, a titanium rod is used for constraint fixation on the periphery of the box 10; in the step S3, longitudinally distributed partition layers 20 are arranged in the box body 10, the distance between every two adjacent partition layers 20 is 8mm, the partition layers 20 are corrugated, and the constant temperature time of roasting treatment is 8 hours; other methods and steps are the same as those in embodiment 1, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the three-dimensional box comprises a 3/4 cylindrical box body 10 and partition layers 20, wherein the partition layers 20 are longitudinally distributed in the box body 10, and the partition layers 20 are corrugated. See fig. 1 and 2.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Ag hollow fiber electrodes, and the specific steps are different from those in embodiment 1 in that: the heating rate of the first heat treatment in the step A3 is 2 ℃/min, the heating temperature of the second heat treatment is 350 ℃, and other steps and methods are the same as those in the embodiment 1, and are not repeated here.
In the embodiment, 450 Ag hollow fiber electrodes processed in a single batch are adopted, and the conductivity and the strength of more than 95% of the Ag hollow fiber electrodes meet the requirements.
Example 6
The embodiment provides a manufacturing method of a hollow fiber electrode batch heat treatment device, which specifically comprises the following steps:
s1, selecting a titanium plate with the thickness of 0.5mm and the length of 600mm as a raw material, mechanically cutting and bending the titanium plate into a 2/3 cylindrical box body 10, and welding and forming the titanium plate by a laser welding method;
s2, restraining and fixing the outer periphery of the box body 10 by using a titanium rod for preventing deformation;
s3, arranging a plurality of transversely distributed isolating layers 20 in the box body 10, and then placing the box body in a tube furnace for roasting treatment to obtain a heat treatment device; wherein, the interval between every two adjacent partition layers 20 is 8mm, and the partition layers 20 are corrugated; the calcination treatment is to heat up from 20 ℃ to 600 ℃ at a heating rate of 2 ℃/min under an air flow rate of 200ml/min, and keep the temperature for 8 hours, so as to produce a dense titanium dioxide oxide layer on the surface of the box body 10.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of 2/3 cylinder form, the partition layer 20 transversely distributes in the inside of box body 10, and the partition layer 20 is the ripple shape.
The batch heat treatment device for the hollow fiber electrode in the embodiment is applied to batch heat treatment of the Ni hollow fiber electrode, and specifically comprises the following steps:
a1, providing a hollow fiber electrode batch heat treatment device in the embodiment;
a2, sequentially placing Ni hollow fiber electrode blanks with the length of 120mm pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches;
a3, placing the heat treatment device with the hollow fiber electrode green body in a tubular furnace, performing primary heat treatment at the temperature rising rate of 2 ℃/min to the constant temperature of 600 ℃ for 6 hours under the atmosphere with the air flow rate of 200mL/min so as to fully remove organic impurities in the green body and cause sintering of Ni particles, and performing secondary heat treatment at the temperature rising rate of 1 ℃/min to the constant temperature of 600 ℃ for 6 hours under the atmosphere with the hydrogen/argon mixed gas flow rate of 200mL/min to obtain batches of Ni hollow fiber electrodes.
In this embodiment, 420 Ni hollow fiber electrodes processed in a single batch have conductivity and strength which meet the requirements of more than 91% Ni hollow fiber electrodes.
Example 7
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 6 in that: in the step S1, a titanium mesh with the thickness of 1.5mm, the length of 650mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a cylindrical box body 10, and the cylindrical box body is welded and formed by a laser welding method; in step S3, cellular partition layers 20 are uniformly distributed in the box 10, and the interval between every two adjacent partition layers 20 is 6mm; other methods and steps are the same as in example 6, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of cylinder form, the partition layer 20 is evenly distributed at the box body 10, and the partition layer 20 is cellular.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Ni hollow fiber electrodes, and the specific steps are different from those in embodiment 6 in that: the length of the Ni hollow fiber electrode blank in the step A2 is 100mm; the heating rate of the first heat treatment in the step A3 is 5 ℃/min, and the heating rate of the second heat treatment is 2 ℃/min; other steps and methods are the same as those in embodiment 6, and will not be described here.
In this example, 690 Ni hollow fiber electrodes were processed in a single batch, and the conductivity and strength of over 97% Ni hollow fiber electrodes were satisfactory.
Example 8
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 6 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 600mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a cylindrical box body 10, and is welded and formed by an argon arc welding method; in step S3, cellular partition layers 20 are uniformly distributed in the box 10, and the interval between every two adjacent partition layers 20 is 6mm; other methods and steps are the same as in example 6, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of cylinder form, the partition layer 20 is evenly distributed at the box body 10, and the partition layer 20 is cellular.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Ni hollow fiber electrodes, and the specific steps are different from those in embodiment 6 in that: the length of the Ni hollow fiber electrode blank in the step A2 is 180mm; the heating rate of the first heat treatment in the step A3 is 5 ℃/min, and the heating rate of the second heat treatment is 2 ℃/min; other steps and methods are the same as those in embodiment 6, and will not be described here.
In this embodiment, 320 Ni hollow fiber electrodes processed in a single batch have conductivity and strength satisfying the requirements of over 93% of Ni hollow fiber electrodes.
Example 9
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 6 in that: in the step S1, a titanium mesh with the thickness of 0.5mm, the length of 500mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a rectangular box body 10, and is welded and formed by an argon arc welding method; in step S2, in order to prevent deformation, mechanical casting is used for shaping and fixing; in the step S3, the partition layers 20 are longitudinally distributed inside the case 10, and the interval between every two adjacent partition layers 20 is 6mm; other methods and steps are the same as in example 6, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 are of a cuboid shape, the partition layer 20 is longitudinally distributed in the box body 10, and the partition layer 20 is zigzag.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Ni hollow fiber electrodes, and the specific steps are different from those in embodiment 6 in that: the length of the Ni hollow fiber electrode blank in the step A2 is 160mm; the air flow rate of the first heat treatment in the step A3 is 100mL/min, the hydrogen/argon mixed gas flow rate of the second heat treatment is 100mL/min, and the heating rate is 2 ℃/min; other steps and methods are the same as those in embodiment 6, and will not be described here.
In this embodiment, 255 Ni hollow fiber electrodes processed in a single batch have conductivity and strength satisfying the requirements for 93% or more of the Ni hollow fiber electrodes.
Example 10
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 6 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 600mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a 3/4 cylindrical box body 10, and the box body is welded and formed by adopting an argon arc welding method; in the step S3, zigzag partition layers 20 are obliquely distributed in the box body 10, and the interval between every two adjacent partition layers 20 is 6mm; other methods and steps are the same as in example 6, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of 3/4 cylinder form, the partition layer 20 is in the inside slant distribution of box body 10, and the partition layer 20 is the cockscomb structure.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Ni hollow fiber electrodes, and the specific steps are different from those in embodiment 6 in that: in the step A3, the heating rate of the first heat treatment is 5 ℃/min, the flow rate of the hydrogen/argon mixture of the second heat treatment is 100mL/min, and the heating rate is 2 ℃/min to 600 ℃ and the temperature is kept constant for 4 hours; other steps and methods are the same as those in embodiment 6, and will not be described here.
In this embodiment, 500 Ni hollow fiber electrodes processed in a single batch have conductivity and strength which meet the requirements of more than 90% Ni hollow fiber electrodes.
Example 11
The embodiment provides a manufacturing method of a hollow fiber electrode batch heat treatment device, which specifically comprises the following steps:
s1, selecting a titanium plate with the thickness of 1.0mm and the length of 650mm as a raw material, mechanically cutting and bending the titanium plate into a cylindrical box body 10, and welding and forming the titanium plate by a laser welding method;
s2, restraining and fixing the outer periphery of the box body 10 by using a titanium rod for preventing deformation;
s3, arranging a plurality of longitudinally distributed isolating layers 20 in the box body 10, and then placing the isolating layers in a tube furnace for roasting treatment to obtain a heat treatment device; wherein, the interval between every two adjacent partition layers 20 is 10mm, and the partition layers 20 are corrugated; the calcination treatment is to heat up from 20 ℃ to 600 ℃ at a heating rate of 2 ℃/min under an air flow rate of 200ml/min, and keep the temperature for 8 hours, so as to produce a dense titanium dioxide oxide layer on the surface of the box body 10.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of cylinder form, the partition layer 20 vertically distributes in the inside of box body 10, and the partition layer 20 is the ripple shape.
The batch heat treatment device for the hollow fiber electrode in the embodiment is applied to batch heat treatment of the Cu hollow fiber electrode, and specifically comprises the following steps:
a1, providing a hollow fiber electrode batch heat treatment device in the embodiment;
a2, placing Cu hollow fiber electrode blanks with the length of 160mm pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches in sequence;
a3, placing the heat treatment device with the hollow fiber electrode green body in a tubular furnace, performing primary heat treatment at the temperature rising rate of 5 ℃/min to the constant temperature of 550 ℃ for 4 hours under the atmosphere with the air flow rate of 200mL/min so as to fully remove organic impurities in the green body and cause sintering of Cu particles, and performing secondary heat treatment at the temperature rising rate of 1 ℃/min to the constant temperature of 600 ℃ for 6 hours under the atmosphere with the hydrogen/argon mixed gas flow rate of 200mL/min to obtain batches of Cu hollow fiber electrodes.
In this embodiment, 450 Cu hollow fiber electrodes processed in a single batch have conductivity and strength which meet the requirements of more than 90% of the Cu hollow fiber electrodes.
Example 12
The present embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 11 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 650mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a 2/3 cylindrical box body 10, and the box body is welded and formed by adopting an argon arc welding method; in step S3, the honeycomb partition layers 20 with the interval of 8mm are uniformly distributed in the box body 10; other methods and steps are the same as those in embodiment 11, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the device comprises a 2/3 cylindrical box body 10 and partition layers 20, wherein the partition layers 20 are uniformly distributed in the box body 10, and the partition layers 20 are honeycomb-shaped.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Cu hollow fiber electrodes, and the specific steps are different from those in embodiment 11 in that: the length of the Cu hollow fiber electrode blank in the step A2 is 140mm; the temperature rising rate of the first heat treatment in the step A3 is 2 ℃/min, and the temperature is kept for 6 hours; other steps and methods are the same as those in embodiment 11, and will not be described here.
In this embodiment, 340 Cu hollow fiber electrodes processed in a single batch have conductivity and strength satisfying the requirements of more than 97% Cu hollow fiber electrodes.
Example 13
The present embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 11 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 550mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a rectangular box body 10, and is welded and formed by an argon arc welding method; in step S2, in order to prevent deformation, mechanical casting is used for shaping and fixing; in step S3, the honeycomb partition layers 20 with the interval of 8mm are uniformly distributed in the box body 10; other methods and steps are the same as those in embodiment 11, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of cuboid form, the partition layer 20 evenly distributes in the box body 10, and the partition layer 20 is the honeycomb.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Cu hollow fiber electrodes, and the specific steps are different from those in embodiment 11 in that: the length of the Cu hollow fiber electrode blank in the step A2 is 120mm; in the step A3, the first heat treatment is carried out for 6 hours at the temperature rising rate of 2 ℃/min to 600 ℃ under the atmosphere with the air flow rate of 200mL/min, and the second heat treatment is carried out for 8 hours; other steps and methods are the same as those in embodiment 11, and will not be described here.
In this embodiment, 300 Cu hollow fiber electrodes processed in a single batch have conductivity and strength which meet the requirements of more than 98% of the Cu hollow fiber electrodes.
Example 14
The present embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 11 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 500mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a cylindrical box body 10, and is welded and formed by an argon arc welding method; in the step S3, the zigzag-shaped isolating layers 20 with the interval of 6mm are transversely and uniformly distributed in the box body 10; other methods and steps are the same as those in embodiment 11, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 are in a cylindrical shape, the partition layer 20 is transversely and uniformly distributed in the box body 10, and the partition layer 20 is zigzag.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Cu hollow fiber electrodes, and the specific steps are different from those in embodiment 11 in that: the length of the Cu hollow fiber electrode blank in the step A2 is 180mm; in the step A3, the first heat treatment is carried out for 6 hours at the constant temperature of 600 ℃ at the heating rate of 2 ℃/min under the atmosphere with the air flow rate of 200 mL/min; other steps and methods are the same as those in embodiment 11, and will not be described here.
In this embodiment, 275 Cu hollow fiber electrodes processed in a single batch have conductivity and strength which meet the requirements of more than 90% of the Cu hollow fiber electrodes.
Example 15
The present embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 11 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 600mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a 3/4 cylindrical box body 10, and the box body is welded and formed by adopting an argon arc welding method; in the step S3, honeycomb partition layers 20 with the interval of 8mm are uniformly distributed in the box body 10, and the interval between every two adjacent partition layers 20 is 6mm; other methods and steps are the same as those in embodiment 11, and will not be described here.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of 3/4 cylinder form, the partition layer 20 evenly distributes in the box body 10, and the partition layer 20 is cellular.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Cu hollow fiber electrodes, and the specific steps are different from those in embodiment 11 in that: the length of the Cu hollow fiber electrode blank in the step A2 is 140mm; the first heat treatment in the step A3 is carried out for 6 hours at constant temperature; other steps and methods are the same as those in embodiment 11, and will not be described here.
In this embodiment, 365 Cu hollow fiber electrodes are processed in a single batch, and the conductivity and strength of at least 96% of the Cu hollow fiber electrodes meet the requirements.
Example 16
The embodiment provides a manufacturing method of a hollow fiber electrode batch heat treatment device, which specifically comprises the following steps:
s1, selecting a titanium mesh with the thickness of 1.0mm, the length of 600mm and the aperture of 2X 4mm as a raw material, mechanically cutting and bending the titanium mesh into a 3/4 cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method;
s2, restraining and fixing the outer periphery of the box body 10 by using a titanium rod for preventing deformation;
S3, arranging a plurality of partition layers 20 which are uniformly distributed in the box body 10, and then placing the partition layers in a tube furnace for roasting treatment to obtain a heat treatment device; wherein, the interval between every two adjacent partition layers 20 is 8mm, and the partition layers 20 are honeycomb-shaped; the calcination treatment is to heat up from 20 ℃ to 600 ℃ at a heating rate of 2 ℃/min under an air flow rate of 200ml/min, and keep the temperature for 8 hours, so as to produce a dense titanium dioxide oxide layer on the surface of the box body 10.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of 3/4 cylinder form, the partition layer 20 is evenly distributed in the inside of box body 10, and the partition layer 20 is cellular.
The batch heat treatment device for the hollow fiber electrode in the embodiment is applied to batch heat treatment of the Fe hollow fiber electrode, and specifically comprises the following steps:
a1, providing a hollow fiber electrode batch heat treatment device in the embodiment;
a2, placing the Fe hollow fiber electrode blanks with the length of 140mm pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches in sequence;
a3, placing a heat treatment device with the hollow fiber electrode green body in a tubular furnace, performing primary heat treatment at a temperature rising rate of 5 ℃/min to 600 ℃ for 6 hours under the atmosphere with an air flow rate of 200mL/min so as to fully remove organic impurities in the green body and cause sintering of Fe particles, and performing secondary heat treatment at a temperature rising rate of 2 ℃/min to 600 ℃ for 6 hours under the atmosphere with a hydrogen/argon mixed gas flow rate of 200mL/min to obtain a batch of Fe hollow fiber electrodes.
In this embodiment, 365 Fe hollow fiber electrodes are processed in a single batch, and the conductivity and strength of more than 98% of the Fe hollow fiber electrodes meet the requirements.
Example 17
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 16 in that: in the step S1, a titanium plate with the thickness of 1.0mm and the length of 550mm is selected as a raw material, and is welded and formed by adopting an argon arc welding method through mechanical cutting and bending into a cuboid box body 10; in step S2, in order to prevent deformation, mechanical casting is used for shaping and fixing; in the step S3, corrugated partition layers 20 with the interval of 8mm are transversely distributed in the box body 10; other methods and steps are the same as in example 16, and will not be described here again.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of cuboid form, the partition layer 20 transversely distributes in box body 10, and the partition layer 20 is the ripple shape.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Fe hollow fiber electrodes, and the specific steps are the same as those in embodiment 16: the length of the Fe hollow fiber electrode blank in the step A2 is 120mm; the heating rate of the first heat treatment in the step A3 is 2 ℃/min, and the heating rate of the second heat treatment is 1 ℃/min; other steps and methods are the same as in example 16, and will not be described here.
In this embodiment, 310 Fe hollow fiber electrodes processed in a single batch have conductivity and strength that meet the requirements for more than 92% of the Fe hollow fiber electrodes.
Example 18
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 16 in that: in the step S1, a titanium mesh with the thickness of 1.0mm, the length of 500mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a cylindrical box body 10, and is welded and formed by an argon arc welding method; in the step S3, the zigzag-shaped isolating layer 20 with the interval of 8mm is obliquely distributed in the box body 10; other methods and steps are the same as in example 16, and will not be described here again.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 are in a cylindrical shape, the partition layer 20 is obliquely distributed in the box body 10, and the partition layer 20 is zigzag.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Fe hollow fiber electrodes, and the specific steps are the same as those in embodiment 16: the length of the Fe hollow fiber electrode blank in the step A2 is 160mm; in the step A3, the first heat treatment is carried out for 4 hours at constant temperature, and the second heat treatment is carried out for heating to 800 ℃; other steps and methods are the same as in example 16, and will not be described here.
In this embodiment, 335 single-batch Fe hollow fiber electrodes, and more than 94% of the Fe hollow fiber electrodes have conductivity and strength that meet the requirements.
Example 19
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 16 in that: in the step S1, a titanium mesh with the thickness of 1.5mm, the length of 650mm and the aperture of 2X 4mm is selected as a raw material, and is mechanically cut and bent into a 2/3 cylindrical box body 10, and the box body is welded and formed by adopting an argon arc welding method; in the step S3, corrugated partition layers 20 with the interval of 8mm are longitudinally distributed in the box body 10, and the baking treatment is carried out for 10 hours; other methods and steps are the same as in example 16, and will not be described here again.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of 2/3 cylinder form, the partition layer 20 vertically distributes in the box body 10, and the partition layer 20 is the ripple shape.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Fe hollow fiber electrodes, and the specific steps are the same as those in embodiment 16: the length of the Fe hollow fiber electrode blank in the step A2 is 100mm; the heating rate of the first heat treatment in the step A3 is 2 ℃/min; other steps and methods are the same as in example 16, and will not be described here.
In this embodiment, 520 Fe hollow fiber electrodes are processed in a single batch, and the conductivity and strength of the Fe hollow fiber electrodes are all satisfied.
Example 20
The embodiment provides a method for manufacturing a batch heat treatment device for hollow fiber electrodes, which is different from embodiment 16 in that: in the step S1, a titanium mesh with the thickness of 0.5mm, the length of 600mm and the aperture of 2X 4mm is selected as a raw material, and is welded and formed by adopting an argon arc welding method through mechanical cutting and bending into a semi-cylindrical box body 10; in step S3, cellular partition layers 20 with a spacing of 6mm are uniformly distributed in the box body 10; other methods and steps are the same as in example 16, and will not be described here again.
The embodiment also provides a heat treatment device for batch heat treatment of hollow fiber electrodes, which comprises: the box body 10 and the partition layer 20 of semicircle column, the partition layer 20 evenly distributes in the box body 10, and the partition layer 20 is cellular.
The batch heat treatment device for hollow fiber electrodes in this embodiment is applied to batch heat treatment of Fe hollow fiber electrodes, and the specific steps are the same as those in embodiment 16: the length of the Fe hollow fiber electrode blank in the step A2 is 120mm; the heating rate of the first heat treatment in the step A3 is 2 ℃/min, and the temperature of the second heat treatment is raised to 800 ℃ and kept for 8 hours; other steps and methods are the same as in example 16, and will not be described here.
In this embodiment, 380 Fe hollow fiber electrodes are processed in a single batch, and the conductivity and strength of the Fe hollow fiber electrodes of 94% or more meet the requirements.
In summary, the device provided by the invention has the advantages that the design is simple, the operation is simple, the device can be rapidly and efficiently used for the batch heat treatment of the hollow fiber electrode, the titanium or tungsten with high melting point, low mass density, strong bending ductility, strong corrosion resistance and strong oxidation resistance is used as the raw material of the device, the device is mechanically cut, bent, welded and fixedly formed, and partition layers with different structural forms are arranged inside the device, so that the device can keep stability under the oxidation or reduction condition of high temperature, the pollution to target materials is avoided, the uniformity of a heat radiation field and a gas flow field in the heat treatment process is controlled, the uniformity and the repeatability of the heat treatment of the target materials are ensured, the heat treatment of the target materials can be rapidly and massively carried out, and the production efficiency is greatly improved; the batch heat treatment device can treat hundreds to thousands of hollow fiber electrode samples in batches at a time, effectively simplify the batch production flow of the hollow fiber electrodes, improve the production efficiency, form an efficient, stable and low-cost preparation process amplification scheme, promote the large-scale production and application of the hollow fiber electrodes, can be widely applied to the production process of various hollow fiber electrodes, and has extremely high application prospect. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (7)
1. The manufacturing method of the hollow fiber electrode batch heat treatment device is characterized by comprising the following steps of:
s1, mechanically cutting and bending raw materials into a box body, and welding and forming; the raw materials are one or a combination of a titanium plate, a titanium mesh, a tungsten plate and a tungsten mesh; the thickness of the raw materials is 0.1-2.5 mm;
s2, fixing the periphery of the box body;
s3, arranging a plurality of isolating layers in the box body, and then placing the box body in a tube furnace for roasting treatment to obtain a heat treatment device; in the step S3, the distance between two adjacent partition layers is 5-10 mm; the roasting atmosphere in the step S3 is oxygen or air atmosphere, and the flow rate of the roasting atmosphere is 100-300 mL/min; the temperature rising rate of the roasting is 1-20 ℃ per minute, the roasting temperature is 400-1000 ℃, and the roasting time is 4-12 hours.
2. The method for manufacturing the hollow fiber electrode batch heat treatment device according to claim 1, wherein: step S1 includes one or a combination of the following conditions:
the box body is in a shape of one of a cuboid, a cylinder, a semi-cylinder, a 3/4 cylinder and a 2/3 cylinder;
the welding method is one or a combination of welding rod arc welding, argon arc welding and laser welding.
3. The method for manufacturing the hollow fiber electrode batch heat treatment device according to claim 1, wherein: the fixing mode in the step S2 is one of titanium rod constraint fixing, tungsten rod constraint fixing and mechanical casting fixing.
4. The method for manufacturing the hollow fiber electrode batch heat treatment device according to claim 1, wherein: step S3 includes one or a combination of the following conditions:
the shape of the isolating layer is one or a combination of zigzag shape, corrugated shape and honeycomb shape;
the arrangement direction of the isolating layer is one or more of transverse isolating layer, longitudinal isolating layer and oblique isolating layer.
5. A hollow fiber electrode batch heat treatment device manufactured by the manufacturing method of the hollow fiber electrode batch heat treatment device according to any one of claims 1 to 4, characterized in that: the heat treatment apparatus includes:
The box body is one of cuboid, cylinder, semi-cylinder, 3/4 cylinder and 2/3 cylinder, and is fixed with a deformation preventing structure along the length direction of the box body;
the partition layer is provided with a plurality of partition layers, a plurality of partition layers are uniformly arranged in the box body, and the partition layer is in one of zigzag, corrugated or honeycomb shapes.
6. The application of the hollow fiber electrode batch heat treatment device is characterized in that the hollow fiber electrode batch heat treatment device is applied to batch heat treatment of hollow fiber electrodes, and specifically comprises the following steps:
a1, providing a hollow fiber electrode batch heat treatment device according to claim 5;
a2, sequentially placing hollow fiber electrode blanks pre-filled in a liner tube into the partition layers of the heat treatment device in batches;
a3, placing the heat treatment device with the hollow fiber electrode green body in a tube furnace, performing first heat treatment in an air atmosphere, and performing second heat treatment in a gas atmosphere to obtain a batch of hollow fiber electrodes; the atmosphere of the first heat treatment in the step A3 is air; the flow rate of the atmosphere in the first heat treatment is 100-200 mL/min; the heating rate of the first heat treatment is 1-5 ℃/min; the temperature of the first heat treatment is 550-600 ℃; the time of the first heat treatment is 4-6 hours; the atmosphere of the second heat treatment in the step A3 is one of hydrogen, argon and hydrogen/argon mixture; the flow rate of the atmosphere of the second heat treatment is 50-1000 mL/min; the temperature rising rate of the second heat treatment is 1-20 ℃/min, the temperature of the second heat treatment is 100-1600 ℃, and the time of the second heat treatment is 0.5-24 h.
7. The use of the hollow fiber electrode batch heat treatment device according to claim 6, wherein: the hollow fiber electrode blank in the step A2 is made of one of silver, copper, iron, cobalt, nickel, titanium, bismuth oxide and tin oxide;
the length of the hollow fiber electrode green body is 100-200 mm.
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