CN113252755A - Preparation method of high-purity compact magnetite electrode - Google Patents
Preparation method of high-purity compact magnetite electrode Download PDFInfo
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- CN113252755A CN113252755A CN202110548169.0A CN202110548169A CN113252755A CN 113252755 A CN113252755 A CN 113252755A CN 202110548169 A CN202110548169 A CN 202110548169A CN 113252755 A CN113252755 A CN 113252755A
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title abstract description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 76
- 239000000843 powder Substances 0.000 claims abstract description 48
- 239000011780 sodium chloride Substances 0.000 claims abstract description 38
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000001953 recrystallisation Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000010453 quartz Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005498 polishing Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 238000003754 machining Methods 0.000 claims abstract description 4
- 238000003466 welding Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 27
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 238000004026 adhesive bonding Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000005553 drilling Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a preparation method of a high-purity compact magnetite electrode, which comprises the following steps: (1) and (3) recrystallization treatment: putting high-purity ferroferric oxide powder into a quartz tube, putting the quartz tube into a pure nickel tube with one sealed end, adding a small amount of water, welding and sealing the other end of the pure nickel tube, then putting the tube into a heating furnace, and recrystallizing at 550-650 ℃; (2) pressing the ferroferric oxide powder subjected to recrystallization treatment into a ferroferric oxide cylinder under the condition of 0.5MPa, and wrapping the ferroferric oxide cylinder by using a platinum foil; (3) grinding sodium chloride into powder of more than 200 meshes and drying; (4) preparing a sodium chloride cylinder containing a ferroferric oxide cylinder; (5) putting the cylinder into a high-pressure assembly block, and heating, pressurizing and sintering by using a large-cavity press; (6) machining the magnetite into a cylinder, and grinding and polishing to obtain the high-purity compact magnetite electrode. The preparation method can obtain the high-purity compact magnetite electrode with good strength.
Description
Technical Field
The invention relates to a preparation method of a magnetite electrode, in particular to a preparation method of a high-purity compact magnetite electrode.
Background
Magnetite is the most important iron-containing mineral in nature, and the dissolution and evolution process of magnetite relates to the geochemical cycle of iron element, and is an important geochemical process. In the field of metal corrosion and protection research, magnetite is an important product after corrosion of iron-based alloy, and has an important effect on delaying corrosion of metal, so that the dissolution and evolution processes of magnetite are a subject of great attention in the field of metal corrosion and protection.
The natural magnetite contains many impurities, such as vanadium, titanium and other elements, which are often doped in the magnetite crystal lattice, and in addition, maghemite and sulfide are often symbiotic with the magnetite and are difficult to distinguish and screen. The chemical action of the doping elements in the magnetite and the primary battery between the symbiotic minerals can interfere the dissolution and evolution process of the magnetite and greatly influence the experimental result. Therefore, the preparation of high-purity magnetite electrode becomes a necessary condition for electrochemical corrosion research. However, it is extremely difficult to find natural bulk magnetite as a research object, which has a high purity. In addition, magnetite has high hardness, brittleness, and poor ductility, and is difficult to process into electrodes required for electrochemical studies.
The prior magnetite bulk electrode preparation technology is to carry out high-temperature sintering under normal pressure or to process and form natural magnet ore bulk. The magnetite electrode sintered at high temperature under normal pressure has large porosity, poor strength and frangibility. Due to the large porosity, water can permeate into magnetite through pores, so that crevice corrosion can be formed on one hand, the electrochemical experiment result is interfered, and on the other hand, high-pressure water can leak through the pores in the electrode, so that the electrochemical experiment under the high-pressure hydrothermal condition cannot be performed. In addition, the natural magnetite block often coexists with other minerals or other elements are doped in the crystal lattice, which affects the accuracy of the electrochemical test result, and pores are often developed in the natural magnetite block, and fluid leakage can also occur under high pressure.
Disclosure of Invention
The invention aims to provide a preparation method of a high-purity compact magnetite electrode, which solves the problems that the existing magnetite electrode has poor electrochemical result accuracy caused by low purity, high porosity and poor strength and cannot be applied to a high-pressure hydrothermal environment, can obtain the high-purity compact magnetite electrode and has good strength.
In order to achieve the above object, the present invention provides a method for preparing a high-purity compact magnetite electrode, comprising:
(1) and (3) recrystallizing high-purity ferroferric oxide powder: putting high-purity ferroferric oxide powder into a quartz tube, putting the quartz tube into a pure nickel tube with one sealed end, adding 0.1-0.5 mL of water (the water is added to provide steam, the amount of the water needs to be controlled, and excessive water is added to cause overlarge pressure in the nickel tube and burst the nickel tube), welding and sealing the other end of the pure nickel tube, then putting the pure nickel tube into a heating furnace, carrying out recrystallization treatment at 550-650 ℃ for 5-10 days, then taking out the powder, and drying the powder; wherein the purity of the high-purity ferroferric oxide powder is 99 percent (containing a small amount of Fe)2O3Impurities); the quartz tube is not closed, the quartz tube has the function of preventing the powder from directly contacting with the nickel tube, so that nickel elements are prevented from entering magnetite crystal lattices, and the powder after recrystallization has no impurity peak in a spectrum through a powder crystal XRD test;
(2) pressing the recrystallized ferroferric oxide powder into a ferroferric oxide cylinder under the condition of 1MPa, and wrapping the ferroferric oxide cylinder by using a platinum foil, a gold foil or a silver foil; isolating magnetite and a pressure transmission medium by adopting platinum foil, gold foil or silver foil (inert metal) to prevent the magnetite from reacting in a high-temperature environment (subsequent sintering process);
(3) grinding sodium chloride into powder of more than 200 meshes and drying;
(4) preparing a sodium chloride cylinder containing a ferroferric oxide cylinder by using the dried sodium chloride powder;
(5) putting a sodium chloride cylinder containing a ferroferric oxide cylinder into a high-pressure assembly block, and heating, pressurizing and sintering;
(6) and machining the sintered high-purity compact magnetite block into a cylinder, and grinding and polishing to obtain the high-purity compact magnetite electrode.
Preferably, in step (1), the drying conditions are: 5-30 min at 30-60 ℃.
Preferably, in step (3), the powder of sodium chloride is dried at 150 ℃ for 2 h.
Preferably, in the step (4), the method for preparing the sodium chloride cylinder containing the ferroferric oxide cylinder comprises the following steps: and (2) pressing sodium chloride powder into a cylinder in a powder tablet press, then placing the ferroferric oxide cylinder wrapped by the platinum foil at the middle position of the upper surface of the sodium chloride cylinder (sodium chloride is used as a pressure transmission medium and provides a quasi-isostatic pressure environment), adding the sodium chloride powder to cover, and compacting in the powder tablet press under the condition of 1MPa to obtain the sodium chloride cylinder containing the ferroferric oxide cylinder.
Preferably, in the step (5), a sodium chloride cylinder containing a ferroferric oxide cylinder is put into the high-pressure assembly block, and the implementation method comprises the following steps:
(5.1) selecting a pyrophyllite block, and drilling a circular through hole in the center of the pyrophyllite block;
(5.2) sleeving a circular stainless steel heating furnace in the through hole;
(5.3) placing a sodium chloride cylinder sample containing a ferroferric oxide cylinder in the middle of a stainless steel heating furnace;
and (5.4) sealing the upper end and the lower end of the round stainless steel heating furnace by pyrophyllite plugs.
Preferably, in the step (5), the sintering under heating and pressure is performed by putting the high-pressure assembly block into a 6 x 600t cubic press for sintering under heating and pressure, wherein the pressure is set to be 0.2-2.0 GPa, the temperature is set to be 200-700 ℃, and the reaction time is 10-90 min.
Preferably, in the step (5), a thermocouple is disposed in the high-pressure assembly block.
Preferably, in step (6), the sintered high-purity compact magnetite block is machined into a cylinder and polished, and comprises:
(6.1) gluing the sintered high-purity compact magnetite block body on a titanium rod by using an AB glue;
(6.2) processing the sintered high-purity compact magnetite block into a cylinder by using a grinding machine;
(6.3) polishing the end face of the cylinder;
and (6.4) ultrasonically cleaning the polished cylinder in acetone for 10-20 min, naturally airing, and then placing in an inert gas atmosphere or a vacuum environment for storage.
The preparation method of the high-purity compact magnetite electrode solves the problems of poor electrochemical result accuracy and poor machinability caused by low purity, high porosity and poor strength of the existing magnetite electrode and cannot be applied to a high-pressure hydrothermal environment, and has the following advantages:
the invention takes high-purity ferroferric oxide powder as a raw material under the conditions of high temperature and high pressure, eliminates the interface between crystal particles by a recrystallization method of solid-phase diffusion reaction, leads the crystal particles to grow up, leads the ferroferric oxide powder to form a block material, reaches the required strength within the pressure and temperature range (heating and pressurizing sintering step) in which the ferroferric oxide stably exists, and processes and shapes the block material to successfully prepare the high-purity compact magnetite electrode, thereby solving the problems that the existing magnetite electrode has poor accuracy of electrochemical results and cannot be applied in high-pressure hydrothermal environment due to low purity, high porosity and poor strength. The magnetite electrode in the invention has high purity, compactness and high strength, avoids the occurrence of crevice corrosion and galvanic cell effect, improves the accuracy of electrochemical test, can be used for electrochemical experiments under the condition of high pressure hydrothermal, and has been successfully applied in the high pressure hydrothermal electrochemical experiments at present.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for preparing a high purity dense magnetite electrode, comprising:
(1) carrying out recrystallization treatment on the commercial high-purity ferroferric oxide powder to remove ferric oxide impurities and improve the degree of crystallization; the treatment method of recrystallization comprises the following steps: putting commercial high-purity ferroferric oxide powder into a quartz tube, putting the quartz tube into a pure nickel tube with one sealed end, adding a small amount of water, welding and sealing the other end of the pure nickel tube, then putting the tube into a heating furnace, carrying out recrystallization treatment at 550-650 ℃ for 5-10 days, then taking out the powder, and drying and storing the powder in a vacuum drying oven for later use; powder crystal XRD test shows that the powder after recrystallization has no impurity peak in its pattern;
(2) weighing 0.6-0.8 g of recrystallized ferroferric oxide powder, pressing into a ferroferric oxide cylinder in a powder tablet press under the condition of 1MPa, and wrapping with platinum foil;
(3) grinding sodium chloride into powder of more than 200 meshes, and drying in an oven at 150 ℃ for 2 hours;
(4) preparing a sodium chloride cylinder containing a ferroferric oxide cylinder by using the dried sodium chloride powder;
(5) putting a sodium chloride cylinder containing a ferroferric oxide cylinder into a high-pressure assembly block, and heating, pressurizing and sintering;
(6) and machining the sintered sample into a cylinder, and grinding and polishing to obtain the high-purity compact magnetite electrode.
In the step (1), the drying conditions are as follows: 5-30 min at 30-60 ℃.
In the pressure and temperature range where ferroferric oxide exists stably, the interface between crystal particles is eliminated by a recrystallization method of solid phase diffusion reaction, and the crystal particles grow up.
In the step (4), the method for preparing the sodium chloride cylinder containing the ferroferric oxide cylinder comprises the following steps: and pressing sodium chloride powder into a cylinder in a powder tablet press, then placing the ferroferric oxide cylinder wrapped by platinum foil at the middle position of the upper surface of the sodium chloride cylinder, adding sodium chloride powder to cover, and compacting in the powder tablet press under the condition of 1MPa to obtain the sodium chloride cylinder containing the ferroferric oxide cylinder.
In the step (5), a sodium chloride cylinder containing a ferroferric oxide cylinder is placed in a high-pressure assembly block, and the implementation method comprises the following steps:
(5.1) selecting a pyrophyllite block, and drilling a circular through hole in the center of the pyrophyllite block;
(5.2) sleeving a circular stainless steel heating furnace in the through hole;
(5.3) placing a sodium chloride cylinder sample containing a ferroferric oxide cylinder in the middle of a stainless steel heating furnace;
and (5.4) sealing the upper end and the lower end of the round stainless steel heating furnace by pyrophyllite plugs.
In the step (5), the heating and pressurizing sintering is carried out by putting the high-pressure assembly block into a 6 x 600t cubic press for heating and pressurizing sintering, wherein the set pressure is 0.2-2.0 GPa, the set temperature is 200-700 ℃, and the reaction time is 10-90 min.
In the step (5), a thermocouple is arranged in the high-pressure assembly block.
In the step (6), the sintered sample is mechanically processed into a cylinder and polished to obtain the high-purity compact magnetite electrode, which comprises:
(6.1) gluing the sintered high-purity compact magnetite block body on a titanium rod by using an AB glue;
(6.2) processing the sintered magnetite blocks into cylinders by using a grinding machine;
(6.3) polishing the end face of the cylinder;
and (6.4) ultrasonically cleaning the polished cylinder in acetone for 10-20 min, naturally airing, and then placing in an inert gas atmosphere or a vacuum environment for storage for later use.
The density of the obtained sample was measured to be 5.196. + -. 0.012g/cm using an electronic densitometer (DH-1200, DAHON, Japan)3Close to its theoretical density.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (8)
1. A method for preparing a high purity dense magnetite electrode, comprising:
(1) and (3) recrystallizing high-purity ferroferric oxide powder: putting high-purity ferroferric oxide powder into a quartz tube, putting the quartz tube into a pure nickel tube with one sealed end, adding 0.1-0.5 mL of water, welding and sealing the other end of the pure nickel tube, then putting the tube into a heating furnace, carrying out recrystallization treatment at 550-650 ℃ for 5-10 days, then taking out the powder, and drying the powder; wherein the purity of the high-purity ferroferric oxide powder is 99 percent;
(2) pressing the recrystallized ferroferric oxide powder into a ferroferric oxide cylinder under the condition of 1MPa, and wrapping the ferroferric oxide cylinder by using a platinum foil, a gold foil or a silver foil;
(3) grinding sodium chloride into powder of more than 200 meshes and drying;
(4) preparing a sodium chloride cylinder containing a ferroferric oxide cylinder by using the dried sodium chloride powder;
(5) putting a sodium chloride cylinder containing a ferroferric oxide cylinder into a high-pressure assembly block, and heating, pressurizing and sintering;
(6) and machining the sintered high-purity compact magnetite block into a cylinder, and grinding and polishing to obtain the high-purity compact magnetite electrode.
2. The method for preparing a high-purity compact magnetite electrode according to claim 1, wherein in step (1), the drying conditions are: 5-30 min at 30-60 ℃.
3. The method for preparing a high-purity compact magnetite electrode according to claim 1, characterized in that in step (3), the powder of sodium chloride is dried at 150 ℃ for 2 h.
4. The method for preparing the high-purity compact magnetite electrode according to claim 1, wherein in the step (4), the method for preparing the sodium chloride cylinder containing the ferroferric oxide cylinder comprises the following steps: and pressing sodium chloride powder into a cylinder in a powder tablet press, then placing the ferroferric oxide cylinder wrapped by platinum foil at the middle position of the upper surface of the sodium chloride cylinder, adding sodium chloride powder to cover, and compacting in the powder tablet press under the condition of 1MPa to obtain the sodium chloride cylinder containing the ferroferric oxide cylinder.
5. The method for preparing a high-purity compact magnetite electrode according to claim 1, wherein in step (5), the sodium chloride cylinder containing the ferroferric oxide cylinder is placed in a high-pressure assembly block, and the method comprises:
(5.1) selecting a pyrophyllite block, and drilling a circular through hole in the center of the pyrophyllite block;
(5.2) sleeving a circular stainless steel heating furnace in the through hole;
(5.3) placing a sodium chloride cylinder sample containing a ferroferric oxide cylinder in the middle of a stainless steel heating furnace;
and (5.4) sealing the upper end and the lower end of the round stainless steel heating furnace by pyrophyllite plugs.
6. The method for preparing a high-purity compact magnetite electrode according to claim 1, wherein in the step (5), the heating and pressurizing sintering is carried out by putting the high-pressure assembly block into a 6 x 600t cubic press, heating and pressurizing sintering are carried out, the set pressure is 0.2-2.0 GPa, the set temperature is 200-700 ℃, and the reaction time is 10-90 min.
7. The method of preparing a high purity densified magnetite electrode according to claim 1, wherein in step (5), a thermocouple is positioned within the high pressure assembly block.
8. The method of preparing a high purity densified magnetite electrode according to claim 1, wherein in step (6), the sintered high purity densified magnetite mass is machined into a cylinder and polished to include:
(6.1) gluing the sintered high-purity compact magnetite block body on a titanium rod by using an AB glue;
(6.2) processing the sintered high-purity compact magnetite block into a cylinder by using a grinding machine;
(6.3) polishing the end face of the cylinder;
and (6.4) ultrasonically cleaning the polished cylinder in acetone for 10-20 min, naturally airing, and then placing in an inert gas atmosphere or a vacuum environment for storage.
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| WO2023105037A1 (en) * | 2021-12-10 | 2023-06-15 | Basf Se | Process for the refining of iron oxides, iron oxides resulting thereof and their use |
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| CN106205857A (en) * | 2016-06-24 | 2016-12-07 | 中国科学院地球化学研究所 | A kind of preparation method of magnetic iron ore electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1172105A (en) * | 1966-06-11 | 1969-11-26 | Philips Electronic Associated | Improvements relating to Methods of Manufacturing Finely-Divided Fe2O3 |
| US3620841A (en) * | 1970-02-16 | 1971-11-16 | Ibm | Process for making continuous magnetite films |
| US4136049A (en) * | 1976-08-09 | 1979-01-23 | Toda Kogyo Corp. | Process for treating acicular magnetite containing co to stabilize the magnetic properties thereof |
| CN106044867A (en) * | 2016-06-24 | 2016-10-26 | 中国科学院地球化学研究所 | Preparation method of pyrite electrode |
| CN106205857A (en) * | 2016-06-24 | 2016-12-07 | 中国科学院地球化学研究所 | A kind of preparation method of magnetic iron ore electrode |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023105037A1 (en) * | 2021-12-10 | 2023-06-15 | Basf Se | Process for the refining of iron oxides, iron oxides resulting thereof and their use |
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