CN112939098A - Process method for preparing magnetic nickel ferrite powder at low temperature in dry state - Google Patents
Process method for preparing magnetic nickel ferrite powder at low temperature in dry state Download PDFInfo
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- CN112939098A CN112939098A CN202110351764.5A CN202110351764A CN112939098A CN 112939098 A CN112939098 A CN 112939098A CN 202110351764 A CN202110351764 A CN 202110351764A CN 112939098 A CN112939098 A CN 112939098A
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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 64
- 239000000843 powder Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 35
- 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 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000001179 sorption measurement Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 9
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 8
- 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
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 6
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical group O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 6
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical group O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 6
- 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
- 239000012071 phase Substances 0.000 abstract description 14
- 230000015572 biosynthetic process Effects 0.000 abstract description 11
- 238000003786 synthesis reaction Methods 0.000 abstract description 11
- 238000002360 preparation method Methods 0.000 abstract description 9
- 239000002131 composite material Substances 0.000 abstract description 6
- 238000009792 diffusion process Methods 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 6
- 238000001237 Raman spectrum Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 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
- 238000013329 compounding 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
- 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
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910003264 NiFe2O4 Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000006555 catalytic reaction 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
- 230000001404 mediated effect Effects 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Images
Classifications
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- 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 at low temperature in a dry state, which comprises the steps of adding a nickel source and an iron source into a solvent for dissolving, 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 100-190 ℃, namely standing and crystallizing, and carrying out magnetic adsorption separation, washing and drying on an obtained reaction product to obtain crystallized nickel ferrite powder. The invention realizes the preparation of the low-temperature solid-state synthesis nickel ferrite powder, effectively reduces the synthesis temperature of the highly crystallized nickel ferrite powder, and avoids the problem of mutual diffusion of components when a composite second phase is synthesized at high temperature; meanwhile, the problem of secondary phase redissolution caused by low crystallinity or composite secondary phase due to liquid phase synthesis is avoided, thereby providing a new preparation way for preparing the nickel ferrite based composite material. The invention has simple operation and control and few concerned 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
The spinel type ferrite nickel ferrite has excellent performances of high magnetic conductivity, 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 hotspot.
The synthesis of nickel ferrite is very diversified, and generally, the synthesis can be divided into two categories, namely top-down and bottom-up. The top-down route comprises solid phase reaction, high-energy ball milling, pulsed laser deposition, self-propagating combustion synthesis and the like. Solid-phase reaction and self-propagating combustion synthesis generally involve high temperatures, and there is a problem of mutual diffusion to degrade performance when a second phase is compounded; in the long-time ball milling process of the high-energy ball milling, the friction contact between a medium and raw materials can bring impurity pollution risks; pulsed laser deposition places higher demands on the equipment. The bottom-up route is sol-gel, co-deposition, hydrothermal (solvothermal), microwave, electrochemical, micro-emulsion, etc. These methods are not liquid-mediated. The powder prepared by sol-gel and codeposition still needs subsequent calcination treatment to obtain high crystallinity; hydrothermal (solvothermal) synthesis of a powder with excellent crystallization, but the second phase may be re-dissolved or the target product may not be obtained when the powder is combined with the second phase by this method; the micro-emulsion method has low yield and also has the problem of low crystallinity.
With the development of science and technology, a single phase cannot meet the requirements of new applications, and it becomes more and more important to obtain new properties by compounding nickel ferrite with a second phase. As mentioned above, the traditional method is difficult to satisfy the composite requirement, so it is very important to develop a new synthesis method to avoid the mutual diffusion of two phases at high temperature and obtain the nickel ferrite powder with good crystallization.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a dry-state low-temperature preparation method of magnetic nickel ferrite powder, which has the advantages of simple process, wide raw material source, stable reaction process and simple and convenient operation, so as to overcome the defect that the nickel ferrite powder with high crystallinity meeting the requirement can be prepared only under the condition of high-temperature calcination or liquid phase in the prior art, and solve the problem of performance reduction generated when the nickel ferrite is compounded with a second phase, thereby preparing the nickel ferrite powder simply, safely and efficiently.
The purpose of the invention is realized by the following technical scheme:
the invention provides a process method for preparing magnetic nickel ferrite powder at low temperature in a dry state, which comprises the following steps:
(1) adding a nickel source and an iron source into a solvent according to the mass ratio of 0.25-0.65: 1 to dissolve, 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 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 in 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 vapor in the step (2) of the invention 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 6 mol/L. The volume-mass ratio of the alkali solution to the mixed powder is 1mL to 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 invention separately carries out the preparation of the mixed powder of ferric chloride and nickel chloride and the synthesis of the nickel ferrite crystal by alkali steam treatment. In the alkali steam treatment process, the alkali solution is not in direct contact with the mixed powder in a liquid state, but the gas phase formed by high-temperature evaporation is in contact with the dried mixed powder, so that the nickel ferrite crystallization and the product purity are improved, the crystallization is performed at a lower temperature, the subsequent calcination treatment is not needed, and the high-crystallization pure nickel ferrite material (the saturation magnetization is more than 25emu/G, the residual magnetization is 0.5-6 emu/G, and the coercive force is 30-80G) is obtained at a low temperature.
(2) The invention realizes the preparation of low-temperature solid-state synthesized nickel ferrite powder, and discloses a preparation method for preparing the nickel ferrite powder by a low-temperature dry method for the first time, thereby effectively reducing the synthesis temperature of the highly crystallized nickel ferrite powder and avoiding the problem of mutual diffusion of components when a composite second phase is synthesized at high temperature; meanwhile, the preparation of the nickel ferrite is synthesized in a dry state, so that the problem of low crystallinity caused by liquid phase synthesis or secondary phase redissolution possibly caused by compounding the secondary phase 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 and few concerned variables, and is beneficial to large-scale synthesis and use.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 shows Raman spectra and FTIR spectra (a: Raman spectra; b: FTIR spectra) of nickel ferrite powder prepared according to the first embodiment of the present invention;
FIG. 2 is a Raman spectrum of the nickel ferrite powder prepared in example two of the present invention;
FIG. 3 is a Raman spectrum of the nickel ferrite powder prepared in the third embodiment of the present invention;
FIG. 4 shows 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
The first embodiment is as follows:
the embodiment of the invention relates to a process method for preparing magnetic nickel ferrite powder at low temperature in a dry state, which 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 dissolving and mixing, stirring at room temperature for 15min to obtain a uniform solution, then stirring at low speed at room temperature to naturally volatilize ethanol, and drying at 55 ℃ to obtain mixed powder;
(2) and (2) carrying out heat treatment on the mixed powder at 150 ℃ in an alkali steam environment, namely, standing and crystallizing for 8h, wherein an alkali solution adopted by alkali steam is an ammonia water solution with the concentration of 5mol/L, the volume mass ratio of the alkali solution to the mixed powder is 1mL to 0.2g, and carrying out magnetic adsorption separation, water washing and drying on a reaction product obtained after heat treatment to obtain crystallized nickel ferrite powder.
As shown in FIG. 1a, the wave numbers of the nickel ferrite powder prepared in this example are 694, 570, 485 and 330cm-1Four Raman characteristic peaks are arranged near the center and matched with the nickel ferrite crystal; as shown in FIG. 1b, at 420 and 570-525 cm-1The area has absorption vibration peak, which is consistent with nickel ferrite crystal. The result shows that the obtained powder is nickel ferrite powder.
Example two:
the embodiment of the invention relates to a process method for preparing magnetic nickel ferrite powder at low temperature in a dry state, which 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 dissolving and mixing, stirring at room temperature for 15min to obtain a uniform solution, then stirring at low speed at room temperature to naturally volatilize ethanol, and drying at 40 ℃ to obtain mixed powder;
(2) and (2) carrying out heat treatment on the mixed powder at 140 ℃ in an alkali steam environment, namely standing and crystallizing for 16h, 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), the volume mass ratio of the alkali solution to the mixed powder is 1mL to 0.1g, and a reaction product obtained after the heat treatment is subjected to magnetic adsorption separation, water washing and drying to obtain crystallized nickel ferrite powder.
The wave numbers of the nickel ferrite powder prepared by the embodiment are 685, 560, 471 and 326cm respectively as shown in FIG. 2-1Four Raman characteristic peaks are arranged near the center and are matched with the nickel ferrite crystal, and the obtained powder is nickel ferrite powder.
Example three:
the embodiment of the invention relates to a process method for preparing magnetic nickel ferrite powder at low temperature in a dry state, which 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 dissolving and mixing, stirring at room temperature for 15min to obtain a uniform solution, then stirring at low speed at room temperature to naturally volatilize ethanol, and drying at 40 ℃ to obtain mixed powder;
(2) and (2) 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 ammonia, 0.2mol/L of ethylenediamine and 0.1mol/L of tetrabutylammonium hydroxide), and the volume mass ratio of the alkali solution to the mixed powder is 1mL to 0.1g, 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. 3, the wave numbers of the nickel ferrite powder prepared in this example are 680, 540, 472, 300 and 197cm respectively-15 Raman characteristic peaks are arranged near the center and matched with the nickel ferrite crystal, and the obtained powder is nickel ferrite powder.
Example four:
the embodiment of the invention relates to a process method for preparing magnetic nickel ferrite powder at low temperature in a dry state, which 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 dissolving and mixing, stirring at room temperature for 15min to obtain a uniform solution, then stirring at low speed at room temperature to naturally volatilize ethanol, and drying at 40 ℃ to obtain mixed powder;
(2) and (2) carrying out heat treatment on the mixed powder for 48h at 140 ℃ in an alkali steam environment, namely, adopting an alkali solution as a mixed solution of ammonia water and ethylenediamine (containing 3mol/L of ammonia and 0.4mol/L of ethylenediamine) in the alkali steam of the standing crystallization reaction according to the volume-mass ratio of the alkali solution to the mixed powder of 1mL to 0.3g, and carrying out magnetic adsorption separation, water washing and drying on a reaction product obtained after the heat treatment to obtain the crystallized nickel ferrite powder.
As shown in FIG. 4a, the wave numbers of the nickel ferrite powder prepared by this embodiment are 698, 560-590, 488 and 330cm-14 Raman characteristic peaks are arranged near the center and matched with the nickel ferrite crystal, and the obtained powder is nickel ferrite powder. As shown in fig. 4b, 2 θ is at 35.6 °, 30.2 °, 43.3 °, and 57.4 ° respectively62.8 degree and NiFe2O4(pdf #54-0964) showed a consistent result, indicating that the powder obtained was nickel ferrite powder.
The VSM results of the nickel ferrite powder prepared in the examples of the present invention are shown in table 1.
TABLE 1 VSM results of nickel ferrite powder prepared in the examples of the present invention
Claims (6)
1. A process method for preparing magnetic nickel ferrite powder at low temperature in a dry state is characterized by comprising the following steps:
(1) adding a nickel source and an iron source into a solvent according to the mass ratio of 0.25-0.65: 1 to dissolve, 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 heat treatment to obtain crystallized nickel ferrite powder.
2. The process method for preparing the magnetic nickel ferrite powder at low temperature in a dry state according to claim 1, which is characterized in that: the nickel source is nickel chloride hexahydrate, and the iron source is ferric chloride hexahydrate.
3. The process method for preparing the magnetic nickel ferrite powder at low temperature in a dry state according to claim 1, which is characterized in that: the stirring and mixing time of the step (1) is 10-30 min, and the drying temperature is 40-80 ℃.
4. The process method for preparing the magnetic nickel ferrite powder at low temperature in a dry state according to claim 1, which is characterized in that: 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 6 mol/L.
5. The process method for preparing the magnetic nickel ferrite powder at low temperature in a dry state according to claim 4, which is characterized in that: the volume-mass ratio of the alkali solution to the mixed powder is 1mL to 0.1-1.5 g.
6. The process method for preparing the magnetic nickel ferrite powder at low temperature in a dry state according to claim 1, which is characterized in that: the reaction temperature of the step (2) is 120-180 ℃, and the standing crystallization reaction time 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, pages: 113 * |
| 木提拉•阿曼等: "水热法合成铁酸镍纳米磁性粉体及表征", 《新疆大学学报(自然科学版)》, vol. 29, no. 2, 31 May 2012 (2012-05-31), pages 196 * |
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