CN112939098B - Process method for preparing magnetic nickel ferrite powder in dry state at low temperature - Google Patents
Process method for preparing magnetic nickel ferrite powder in dry state at low temperature Download PDFInfo
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- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000000843 powder Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000003513 alkali Substances 0.000 claims abstract description 30
- 239000011812 mixed powder Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000004090 dissolution Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000001179 sorption measurement Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 8
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 7
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 7
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 230000005415 magnetization Effects 0.000 claims description 5
- XZUAPPXGIFNDRA-UHFFFAOYSA-N ethane-1,2-diamine;hydrate Chemical compound O.NCCN XZUAPPXGIFNDRA-UHFFFAOYSA-N 0.000 claims description 2
- JEUXZUSUYIHGNL-UHFFFAOYSA-N n,n-diethylethanamine;hydrate Chemical compound O.CCN(CC)CC JEUXZUSUYIHGNL-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 2
- WTHDKMILWLGDKL-UHFFFAOYSA-N urea;hydrate Chemical compound O.NC(N)=O WTHDKMILWLGDKL-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000012071 phase Substances 0.000 abstract description 14
- 230000015572 biosynthetic process Effects 0.000 abstract description 9
- 238000003786 synthesis reaction Methods 0.000 abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000002131 composite material Substances 0.000 abstract description 6
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 24
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 7
- 238000001237 Raman spectrum Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 238000005049 combustion synthesis Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000713 high-energy ball milling Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229940032296 ferric chloride Drugs 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- 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
- C01P2006/42—Magnetic properties
Abstract
The invention discloses a process method for preparing magnetic nickel ferrite powder in a dry state at low temperature, which comprises the steps of adding a nickel source and an iron source into a solvent for dissolution, stirring and mixing to obtain a uniform solution, volatilizing the solvent, and drying to obtain mixed powder; and then carrying out heat treatment on the mixed powder in an alkali steam environment at the temperature of 100-190 ℃, namely standing for crystallization reaction, and carrying out magnetic adsorption separation, water washing and drying on the obtained reaction product to obtain crystallized nickel ferrite powder. The invention realizes the preparation of the low-temperature solid-state synthesized nickel ferrite powder, effectively reduces the synthesis temperature of the highly crystallized nickel ferrite powder, and avoids the problem of component interdiffusion during the high-temperature synthesis of the composite second phase; meanwhile, the problem of redissolution of the second phase possibly caused by low crystallinity or composite second phase caused by liquid phase synthesis is avoided, so that a new preparation way is provided for preparing the nickel ferrite-based composite material. The invention has simple operation and control, needs few focused variables and is beneficial to large-scale synthesis and use.
Description
Technical Field
The invention relates to the technical field of magnetic nickel ferrite powder, in particular to a preparation method of magnetic nickel ferrite powder.
Background
Spinel type ferrite nickel ferrite has excellent performances of high magnetic permeability, high resistance, low eddy current loss, moderate saturation magnetization and the like in a high-frequency region, and is widely applied to the fields of antennas, medicines, catalysis, storage, electronic components and the like, so that the spinel type ferrite nickel ferrite is always a research hot spot.
The synthesis method of nickel ferrite is endlessly layered and can be generally divided into two major categories from top to bottom and from bottom to top. The top-down route includes solid phase reaction, high energy ball milling, pulsed laser deposition, self-propagating combustion synthesis, etc. Solid phase reactions and self-propagating combustion synthesis typically involve high temperatures, and there is a problem of interdiffusion in compounding the second phase, which reduces performance; in the long-time ball milling process of the high-energy ball milling, the friction contact between the medium and the raw material can bring impurity pollution risks; pulsed laser deposition places higher demands on the equipment. The bottom-up routes are sol-gel, co-deposition, hydrothermal (solvothermal), microwave, electrochemical, microemulsion, etc. These methods are all independent of liquids as media. The powder prepared by sol-gel and codeposition still needs subsequent calcination treatment to obtain high crystallinity; hydrothermal (solvothermal) can give a fine crystalline powder, but when this method is used for compounding with the second phase, it tends to result in re-dissolution of the second phase or unavailability of the target product; the microemulsion process has a low yield and also has a low crystallinity.
With the development of technology, a single phase has failed to meet new application requirements, and it has become increasingly important to obtain new properties by compositing nickel ferrite with a second phase. As described above, the conventional method is difficult to meet the compounding requirement, so it is very important to develop a new synthesis method to avoid the two-phase high-temperature interdiffusion and obtain well-crystallized nickel ferrite powder.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a process method for preparing magnetic nickel ferrite powder at low temperature in a dry state, which has the advantages of simple process, wide raw material sources, stable reaction process and simple and convenient operation, so as to overcome the defect that the prior art needs high-temperature calcination or can prepare the nickel ferrite powder with high crystallinity meeting the requirements under the condition of liquid phase, solve the problem of performance reduction generated when the nickel ferrite is compounded with a second phase, and prepare the nickel ferrite powder simply, safely and efficiently.
The aim of the invention is realized by the following technical scheme:
the invention provides a process method for preparing magnetic nickel ferrite powder in a dry state at low temperature, which comprises the following steps:
(1) Adding a nickel source and an iron source into a solvent according to the mass ratio of the nickel source to the iron source=0.25-0.65:1, dissolving, stirring and mixing to obtain a uniform solution, volatilizing the solvent, and drying to obtain mixed powder;
(2) And (3) carrying out heat treatment on the mixed powder in an alkali steam environment at 100-190 ℃, namely standing for crystallization reaction for 6-72 h, and carrying out magnetic adsorption separation, water washing and drying on a reaction product obtained after the heat treatment to obtain crystallized nickel ferrite powder.
In the scheme, the nickel source is nickel chloride hexahydrate, and the iron source is ferric chloride hexahydrate. The stirring time of the step (1) is 10-30 min, and the drying temperature is 40-80 ℃.
In the above scheme, the alkali solution adopted by the alkali steam in the step (2) is one or a combination of an ammonia water solution, a urea water solution, an ethylenediamine water solution, a triethylamine water solution, a tetrapropylammonium hydroxide water solution and a tetrabutylammonium hydroxide water solution; the concentration of the alkali solution is less than or equal to 6mol/L. The volume mass ratio of the alkali solution to the mixed powder=1 mL:0.1-1.5 g.
Further, the reaction temperature of the step (2) is 120-180 ℃, and the standing crystallization reaction time is 6-28 h.
The invention has the following beneficial effects:
(1) The preparation of the mixed powder of ferric chloride and nickel chloride and the synthesis of the nickel ferrite crystal by alkali vapor treatment are carried out separately. In the alkali vapor treatment process, the alkali solution is not in direct contact with the mixed powder in a liquid state, but in a gas phase formed by high-temperature evaporation is in contact with the dried mixed powder, so that the crystallization of nickel ferrite and the purity of a product are improved, the process is carried out at a lower temperature without subsequent calcination treatment, and a highly crystallized pure nickel ferrite material (saturation magnetization > 25emu/G, residual magnetization=0.5-6 emu/G and coercive force=30-80G) is obtained at a low temperature.
(2) The invention realizes the preparation of low-temperature solid-state synthesized nickel ferrite powder, and for the first time discloses a preparation method for preparing the nickel ferrite powder by a low-temperature dry method, which effectively reduces the synthesis temperature of the highly crystallized nickel ferrite powder and avoids the problem of component interdiffusion during high-temperature synthesis of a composite second phase; meanwhile, the preparation of the nickel ferrite is synthesized in a dry state, so that the problem of redissolution of a second phase possibly caused by low crystallinity or composite of the second phase due to liquid phase synthesis is avoided, and a new preparation way is provided for preparing the nickel ferrite-based composite material.
(3) The invention has simple operation and control, needs few focused variables and is beneficial to large-scale synthesis and use.
Drawings
The invention will be described in further detail with reference to examples and figures:
FIG. 1 is a Raman spectrum and an FTIR spectrum (a: raman spectrum; b: FTIR spectrum) of a nickel ferrite powder prepared according to an embodiment of the present invention;
FIG. 2 is a Raman spectrum of the nickel ferrite powder prepared in the second embodiment of the invention;
FIG. 3 is a Raman spectrum of nickel ferrite powder prepared in the third embodiment of the invention;
FIG. 4 is a Raman spectrum and an XRD spectrum (a: raman spectrum; b: XRD spectrum) of the nickel ferrite powder prepared in example four of the present invention.
Detailed Description
Embodiment one:
the process method for preparing the magnetic nickel ferrite powder at the low temperature in a dry state comprises the following steps:
(1) Sequentially adding 0.50g of nickel chloride hexahydrate, 0.83g of ferric chloride hexahydrate and 15mL of ethanol into a reaction bottle for dissolution and mixing, stirring at room temperature for 15min to obtain a uniform solution, stirring at low speed at room temperature for naturally volatilizing ethanol, and drying at 55 ℃ to obtain mixed powder;
(2) And (3) carrying out heat treatment on the mixed powder in an alkali steam environment at 150 ℃, namely standing and crystallizing for 8 hours, wherein an alkali solution adopted by alkali steam is an ammonia water solution with the concentration of 5mol/L, and the volume mass ratio of the alkali solution to the mixed powder=1 mL to 0.2g, and carrying out magnetic adsorption separation, water washing and drying on a reaction product obtained after the heat treatment to obtain crystallized nickel ferrite powder.
As shown in FIG. 1a, the nickel ferrite powder prepared in this example has wave numbers of 694, 570, 485, and 330cm, respectively -1 Four Raman characteristic peaks are arranged near the center and are matched with the nickel ferrite crystal; as shown in FIG. 1b, at 420 and 570-525 cm -1 The absorption vibration peak exists in the region, which is consistent with the nickel ferrite crystal. The result shows that the obtained powder is nickel ferrite powder.
Embodiment two:
the process method for preparing the magnetic nickel ferrite powder at the low temperature in a dry state comprises the following steps:
(1) Sequentially adding 0.37g of nickel chloride hexahydrate, 0.79g of ferric chloride hexahydrate and 10mL of ethanol into a reaction bottle for dissolution and mixing, stirring at room temperature for 15min to obtain a uniform solution, stirring at low speed at room temperature for naturally volatilizing ethanol, and drying at 40 ℃ to obtain mixed powder;
(2) And (3) carrying out heat treatment on the mixed powder in an alkali steam environment at 140 ℃, namely standing and crystallizing for 16 hours, wherein an alkali solution adopted by alkali steam is a mixed solution of ammonia water, urea and ethylenediamine (containing 1.5mol/L of ammonia, 1mol/L of urea and 0.6mol/L of ethylenediamine), and the crystallized nickel ferrite powder is obtained by magnetically adsorbing, separating, washing and drying a reaction product obtained after the heat treatment according to the volume-mass ratio of the alkali solution to the mixed powder = 1mL to 0.1 g.
As shown in FIG. 2, the nickel ferrite powder prepared in this example has wave numbers of 685, 560, 471 and 326cm, respectively -1 Four Raman characteristic peaks are arranged near the center and coincide with nickel ferrite crystals, which indicates that the obtained powder is nickel ferrite powder.
Embodiment III:
the process method for preparing the magnetic nickel ferrite powder at the low temperature in a dry state comprises the following steps:
(1) Sequentially adding 0.002g of nickel chloride hexahydrate, 0.004g of ferric chloride hexahydrate and 8mL of ethanol into a reaction bottle for dissolution and mixing, stirring at room temperature for 15min to obtain a uniform solution, then stirring at low speed at room temperature for naturally volatilizing ethanol, and drying at 40 ℃ to obtain mixed powder;
(2) And (3) carrying out heat treatment on the mixed powder in an alkali steam environment at 140 ℃, namely standing and crystallizing for 24 hours, wherein an alkali solution adopted by alkali steam is a mixed solution of ammonia water, ethylenediamine and tetrabutylammonium hydroxide (containing 3mol/L of ethylenediamine, 0.2mol/L of ethylenediamine and 0.1mol/L of tetrabutylammonium hydroxide), and the reaction product obtained after the heat treatment is subjected to magnetic adsorption separation, water washing and drying according to the volume-mass ratio of alkali solution to mixed powder = 1mL: 0.1g, so as to obtain crystallized nickel ferrite powder.
As shown in FIG. 3, the nickel ferrite powder prepared in this example has wave numbers of 680, 540,472、300、197cm -1 5 Raman characteristic peaks are arranged near the center and coincide with the nickel ferrite crystal, which indicates that the obtained powder is nickel ferrite powder.
Embodiment four:
the process method for preparing the magnetic nickel ferrite powder at the low temperature in a dry state comprises the following steps:
(1) Sequentially adding 0.003g of nickel chloride hexahydrate, 0.0062g of ferric chloride hexahydrate and 12mL of ethanol into a reaction bottle for dissolution and mixing, stirring at room temperature for 15min to obtain a uniform solution, stirring at low speed at room temperature for naturally volatilizing ethanol, and drying at 40 ℃ to obtain mixed powder;
(2) And (3) carrying out heat treatment on the mixed powder for 48 hours in an alkali steam environment at 140 ℃, namely standing, crystallizing, wherein an alkali solution adopted by alkali steam is a mixed solution of ammonia water and ethylenediamine (containing 3mol/L and 0.4mol/L of ethylenediamine), and carrying out magnetic adsorption separation, water washing and drying on a reaction product obtained after the heat treatment according to the volume-mass ratio of the alkali solution to the mixed powder=1 mL to 0.3g, so as to obtain crystallized nickel ferrite powder.
As shown in FIG. 4a, the nickel ferrite powder prepared in this example has wave numbers of 698, 560-590, 488 and 330cm, respectively -1 4 Raman characteristic peaks are arranged near the center and coincide with the nickel ferrite crystal, which indicates that the obtained powder is nickel ferrite powder. As shown in FIG. 4b, 2. Theta. Is at 35.6 °, 30.2 °, 43.3 °, 57.4 °, 62.8 °, and NiFe, respectively 2 O 4 (pdf # 54-0964) is consistent, indicating that the resulting powder is nickel ferrite powder.
The VSM results of the nickel ferrite powder prepared in the example of the invention are shown in Table 1.
TABLE 1 VSM results of Nickel ferrite powder prepared in accordance with the examples of the invention
Claims (2)
1. A process method for preparing magnetic nickel ferrite powder in a dry state at low temperature is characterized by comprising the following steps:
(1) Nickel chloride hexahydrate according to the mass ratio: ferric chloride hexahydrate=0.25 to 0.65:1, adding nickel chloride hexahydrate and ferric chloride hexahydrate into a solvent for dissolution, stirring and mixing for 10-30 min to obtain a uniform solution, volatilizing the solvent, and drying at the temperature of 40-80 ℃ to obtain mixed powder;
(2) Carrying out heat treatment on the mixed powder in an alkali steam environment at 100-150 ℃, namely standing and crystallizing for 6-72 h, wherein an alkali solution adopted by alkali steam is one or a combination of an ammonia water solution, a urea water solution, an ethylenediamine water solution, a triethylamine water solution, a tetrapropylammonium hydroxide water solution and a tetrabutylammonium hydroxide water solution, the concentration of the alkali solution is less than or equal to 6mol/L, and the alkali solution is prepared according to the volume-mass ratio: mixed powder = 1mL: 0.2-1.5 g, wherein the components do not mutually diffuse and the second phase does not redissolve when the second phase is compounded in the heat treatment process; the reaction product obtained after heat treatment is subjected to magnetic adsorption separation, water washing and drying to obtain the crystallized nickel ferrite powder with saturation magnetization of more than 25emu/G, residual magnetization of 0.5-6 emu/G and coercive force of 30-80G;
the solvent in the step (1) is ethanol.
2. The process for preparing magnetic nickel ferrite powder at low temperature in a dry state according to claim 1, which is characterized in that: and (3) standing and crystallizing reaction time in the step (2) is 6-28 h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0570142A (en) * | 1991-09-11 | 1993-03-23 | Murata Mfg Co Ltd | Method for producing magnetic powder |
| CN101555042A (en) * | 2009-05-19 | 2009-10-14 | 李峰 | Method for preparing spinel type iron-containing oxide nano-materials by low heat solid state reaction |
| CN102515278A (en) * | 2011-12-29 | 2012-06-27 | 东北大学 | Preparation method of nickel ferrite spinel nano-powder |
| CN102989461A (en) * | 2012-11-15 | 2013-03-27 | 苏州科技学院 | Preparation method and application of magnetic nickel ferrite photocatalysis material |
-
2021
- 2021-03-31 CN CN202110351764.5A patent/CN112939098B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0570142A (en) * | 1991-09-11 | 1993-03-23 | Murata Mfg Co Ltd | Method for producing magnetic powder |
| CN101555042A (en) * | 2009-05-19 | 2009-10-14 | 李峰 | Method for preparing spinel type iron-containing oxide nano-materials by low heat solid state reaction |
| CN102515278A (en) * | 2011-12-29 | 2012-06-27 | 东北大学 | Preparation method of nickel ferrite spinel nano-powder |
| CN102989461A (en) * | 2012-11-15 | 2013-03-27 | 苏州科技学院 | Preparation method and application of magnetic nickel ferrite photocatalysis material |
Non-Patent Citations (2)
| Title |
|---|
| 吉林化学工业公司化工技工学校编.《化工设备》.中国工业出版社,1963,第113页. * |
| 水热法合成铁酸镍纳米磁性粉体及表征;木提拉•阿曼等;《新疆大学学报(自然科学版)》;20120531;第29卷(第2期);摘要、第196页第1段至第198页第1段 * |
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