CN104058736A - Preparation method of nickel-iron-zirconium compound ferrite - Google Patents
Preparation method of nickel-iron-zirconium compound ferrite Download PDFInfo
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- CN104058736A CN104058736A CN201410252845.XA CN201410252845A CN104058736A CN 104058736 A CN104058736 A CN 104058736A CN 201410252845 A CN201410252845 A CN 201410252845A CN 104058736 A CN104058736 A CN 104058736A
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- preparation
- zirconium
- ferrite
- ferronickel
- complex ferrite
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- FSXAFHNLPUBAOL-UHFFFAOYSA-N [Fe].[Ni].[Zr] Chemical compound [Fe].[Ni].[Zr] FSXAFHNLPUBAOL-UHFFFAOYSA-N 0.000 title abstract 3
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 150000002815 nickel Chemical class 0.000 claims abstract description 9
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 150000003754 zirconium Chemical class 0.000 claims abstract description 6
- 238000004448 titration Methods 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229910000863 Ferronickel Inorganic materials 0.000 claims description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- 229910052726 zirconium Inorganic materials 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 6
- 239000002244 precipitate Substances 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 150000002505 iron Chemical class 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 12
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910017706 MgZn Inorganic materials 0.000 description 1
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000002180 anti-stress Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of a nickel-iron-zirconium compound ferrite. The preparation method comprises the specific steps of mixing nickel salt, iron salt and zirconium salt solutions together, and then carrying out titration by use of an alkali liquor under an ultrasonic condition for precipitating, and filtering, drying and sintering at a high temperature the precipitate, thereby obtaining the nickel-iron-zirconium compound ferrite. The compound ferrite shows excellent wave absorbing capacity; all the components are mixed more evenly.
Description
Technical field
The present invention relates to a kind of ferritic preparation method, particularly a kind of preparation method of ferronickel zirconium complex ferrite.
Background technology
Ferrite is to be formed by the oxide compound of iron and other batching sintering, generally can be divided into three kinds of permanent-magnet ferrite, soft magnetic ferrite and gyromagnetic ferrites.Permanent-magnet ferrite is again ferrite magnetic steel, is exactly the black small magnet that we see at ordinary times.Soft magnetic ferrite is to be formed by ferric oxide and one or more other metal oxides (such as nickel oxide, zinc oxide, manganese oxide, magnesium oxide, barium oxide, strontium oxide etc.) preparation sintering.Gyromagnetic ferrite refers to the Ferrite Material with gyromagnet characteristic.
At present application maximum, research is the hottest is exactly soft magnetic ferrite.CN102603278B provides a kind of preparation method of nickel-zinc ferrite, the preparation of employing conventional ceramic technique, sintering under certain condition, after sintering, the crystallization grain-size of goods is 20～30 μ m, there is obvious crystal boundary, goods have under stress inductance and change less feature, the requirement of the power inductance that meets the needs of resin package to the anti-stress of Ferrite Material.Patent 200910309272.9 discloses a kind of preparation method of Mg-Mn-Zn based ferrite, adopts MgZn ferrite and Mn-Zn ferrite to mix, and has obtained higher relaxation frequency, has also obtained the frequency of utilization of wideband.
Synthetic method, the ferritic synthetic general mixing direct sintering of oxide compound that adopts forms, and the whole homogeneity of material is weak, and the mixing between each component is difficult for reaching uniform state.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method of ferronickel zirconium complex ferrite, to reach more homogeneous of the mixing that makes between each component, the whole homogeneity of material is improved, the object of easy handling.
For achieving the above object, technical scheme of the present invention is as follows:
A preparation method for ferronickel zirconium complex ferrite, comprises following operation steps:
1) nickel salt that is 0.1～1mol/L by amount of substance concentration, molysite and zirconium salt solution are made into mixing solutions according to a certain percentage, and the alkali-titration that is 0.1～1.0mol/L by amount of substance concentration under Ultrasonic Conditions makes its precipitation;
2) by after the standing 12～24h of gained throw out, filter, with after hot wash 3～5 times, use again washing with alcohol 5～6 times, then oven dry, bake out temperature is 60～80 ℃, the time is 5～8h;
3) last, high-temperature calcination at 700～900 ℃, calcining temperature-rise period is that 5～8 ℃/min rises to 400 ℃, insulation 1h, then rise to 700～900 ℃ of target temperatures with 1～2 ℃/min, insulation 2～4h, obtains ferronickel zirconium complex ferrite.
Preferably, step 1) in, the volumetric usage of described nickel salt, molysite and zirconium salt solution is than being 1:1:1, consumption is 10～40mL, by controlling the volumetric usage of nickel salt, molysite and zirconates, regulate its amount of substance concentration, regulate the ratio of each metal oxide in the complex ferrite synthesizing.
Preferably, step 1) in, described alkali lye is ammoniacal liquor, sodium hydroxide or potassium hydroxide, and consumption is 20～60mL, adds after alkali lye, and nickel salt, molysite and zirconates can generate nickel oxide, ferric oxide and zirconic presoma---oxyhydroxide.
Preferably, step 1) in, described ultrasonic frequency is 20～80KHz, and the time is 2～8h, and the ultrasonic wave in this range of frequency is best to the dispersion cavitation effect of metal salt solution.
Pass through technique scheme, the preparation method of ferronickel zirconium complex ferrite provided by the invention is after nickel salt, molysite and zirconium salt solution are mixed, under Ultrasonic Conditions, use alkali-titration, make its precipitation, precipitation after filtration, dry, after burning, high temperature can obtain new complex ferrite ferronickel zirconium complex ferrite, utilize more even that hyperacoustic cavitation effect makes that when alkali-titration nickel salt, molysite and zirconates mix, the material composition being settled out is homogeneous more, this complex ferrite shows good wave-sucking performance, and the mixing between each component is homogeneous more.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, will the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below.
Fig. 1 is that common ferrite amplifies the SEM figure of 10000 times;
Fig. 2 is that the disclosed a kind of ferronickel zirconium complex ferrite of the embodiment of the present invention one amplifies the SEM figure of 10000 times.
Embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described.
The preparation method who the invention provides a kind of ferronickel zirconium complex ferrite, the method is simple to operate, and the complex ferrite wave-sucking performance making is strong, and whole homogeneity improves.
Embodiment mono-:
Get nickelous nitrate, iron nitrate, the zirconium tetrachloride that volume is 20mL and be mixed with mixing solutions, wherein, the amount of substance concentration of nickelous nitrate is 0.2mol/L, the amount of substance concentration of iron nitrate is 0.5mol/L, the amount of substance concentration of zirconium tetrachloride is 0.1mol/L, in ultrasonic frequency, be under 40KHz, 50mL1mol/L sodium hydroxide solution is dropwise added drop-wise in mixing solutions, precipitate standing 24h, filter, with hot wash 5 times, then use washing with alcohol 5 times, the solid sediment obtaining is dried 8h in 80 ℃ of baking ovens.After taking-up, in tube furnace, calcine, during calcining, heating schedule is that 8 ℃/min rises to 400 ℃, insulation 1h, then rise to 850 ℃ of target temperatures with 2 ℃/min, insulation 4h, takes out solid and is 2NiO-5Fe after cooling
2o
3-ZrO
2complex ferrite.
Embodiment bis-:
Get nickelous nitrate, iron nitrate, the zirconium tetrachloride that volume is 20mL and be mixed with mixing solutions, wherein, the amount of substance concentration of nickelous nitrate is 0.1mol/L, the amount of substance concentration of iron nitrate is 0.8mol/L, the amount of substance concentration of zirconium tetrachloride is 0.1mol/L, in ultrasonic frequency, be under 40KHz, 60mL1mol/L sodium hydroxide solution is dropwise added drop-wise in mixing solutions, precipitate standing 24h, filter, with hot wash 5 times, then use washing with alcohol 5 times, the solid sediment obtaining is dried 8h in 80 ℃ of baking ovens.After taking-up, in tube furnace, calcine, during calcining, heating schedule is that 8 ℃/min rises to 400 ℃, insulation 1h, then rise to 850 ℃ of target temperatures with 2 ℃/min, insulation 4h, takes out solid after cooling, obtain NiO-8Fe
2o
3-ZrO
2.
Embodiment tri-:
Get nickelous nitrate, iron nitrate, the zirconium tetrachloride that volume is 15mL and be mixed with mixing solutions, wherein, the amount of substance concentration of nickelous nitrate is 0.3mol/L, the amount of substance concentration of iron nitrate is 0.9mol/L, the amount of substance concentration of zirconium tetrachloride is 0.1mol/L, in ultrasonic frequency, be under 40KHz, 60mL1mol/L sodium hydroxide solution is dropwise added drop-wise in mixing solutions, precipitate standing 24h, filter, with hot wash 5 times, then use washing with alcohol 5 times, the solid sediment obtaining is dried 8h in 80 ℃ of baking ovens.After taking-up, in tube furnace, calcine, during calcining, heating schedule is that 8 ℃/min rises to 400 ℃, insulation 1h, then rise to 850 ℃ of target temperatures with 2 ℃/min, insulation 4h, takes out solid after cooling, obtain 3NiO-4.5Fe
2o
3-ZrO
2.
Comparative example:
Scheme is with embodiment mono-, and difference is not for there is no hyperacoustic participation.
The test of absorbing property:
Adopt the intensification situation of microwave radiometry complex ferrite, get the synthetic complex ferrite of 5g and common ferrite and be placed in quartz reactor, microwave radiation 1min, temperature rise situation is as table 1.
The different ferritic temperature variations of table 1
| Sample | Sample name | Initial temperature/℃ | Outlet temperature/℃ | The temperature difference/℃ |
| Embodiment mono- | 2NiO-5Fe 2O 3-ZrO 2 | 15.1 | 150.3 | 135.2 |
| Embodiment bis- | NiO-8Fe 2O 3-ZrO 2 | 15.2 | 148.1 | 132.9 |
| Embodiment tri- | 3NiO-4.5Fe 2O 3-ZrO 2 | 15.1 | 146.2 | 131.1 |
| Comparative example | 2NiO-5Fe 2O 3-ZrO 2 | 14.9 | 128.1 | 112.2 |
| Common ferrite | Common ferrite | 15 | 117.1 | 102.1 |
As can be seen from Table 1, complex ferrite temperature rise situation under the Ultrasonic Conditions that in the technical program, embodiment mono-to embodiment tri-prepares is obviously better than common ferrite, might as well be a lot of than common ferrite wave-absorbing effect and do not introduce the prepared comparative example ferrite of ultrasonic wave, be because the synergy that the zr element adding plays.But the complex ferrite that the embodiment mono-to embodiment tri-that compares makes, can see that ultrasonic wave plays a significant role in this is synthetic, increases substantially the absorbing property of combined oxidation body.
Electron-microscope scanning test:
2NiO-5Fe to embodiment mono-gained
2o
3-2ZrO
2complex ferrite carries out electron-microscope scanning, the SEM figure obtaining is shown in Fig. 2, common ferritic SEM figure is shown in Fig. 1, can find out, although the complex ferrite making in this programme also has agglomeration to occur from Fig. 1 and Fig. 2, but pattern is better comparatively speaking, be evenly distributed, size dimension is homogeneous more, and relatively all less, mean sizes is about 5 μ m, better dispersed.
Above-mentioned explanation to the disclosed embodiments, makes professional and technical personnel in the field can realize or use the present invention.To the multiple modification of these embodiment, will be apparent for those skilled in the art, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (4)
1. a preparation method for ferronickel zirconium complex ferrite, is characterized in that, comprises following operation steps:
1) nickel salt that is 0.1～1mol/L by amount of substance concentration, molysite and zirconium salt solution are made into mixing solutions according to a certain percentage, and the alkali-titration that is 0.1～1.0mol/L by amount of substance concentration under Ultrasonic Conditions makes its precipitation;
2) by after the standing 12～24h of gained throw out, filter, with after hot wash 3～5 times, use again washing with alcohol 5～6 times, then oven dry, bake out temperature is 60～80 ℃, the time is 5～8h;
3) last, high-temperature calcination at 700～900 ℃, calcining temperature-rise period is that 5～8 ℃/min rises to 400 ℃, insulation 1h, then rise to 700～900 ℃ of target temperatures with 1～2 ℃/min, insulation 2～4h, obtains ferronickel zirconium complex ferrite.
2. the preparation method of a kind of ferronickel zirconium complex ferrite according to claim 1, is characterized in that step 1) in, the volumetric usage of described nickel salt, molysite and zirconium salt solution is than being 1:1:1, consumption is 10～40mL.
3. the preparation method of a kind of ferronickel zirconium complex ferrite according to claim 1, is characterized in that step 1) in, described alkali lye is ammoniacal liquor, sodium hydroxide or potassium hydroxide, consumption is 20～60mL.
4. the preparation method of a kind of ferronickel zirconium complex ferrite according to claim 1, is characterized in that step 1) in, described ultrasonic frequency is 20～80KHz, the time is 2～8h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243580A (en) * | 2016-09-22 | 2016-12-21 | 佛山市飞时达新材料科技有限公司 | A kind of manufacture method of PVC composite cable material |
| CN109637797A (en) * | 2018-12-04 | 2019-04-16 | 天长市昭田磁电科技有限公司 | A kind of preparation method of magnetic Nano material and its preparing the application in magnetic core |
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|---|---|---|---|---|
| CN103193472A (en) * | 2013-04-19 | 2013-07-10 | 南通宝聚颜料有限公司 | Method for synthesizing subsphaeroidal barium ferrite superfine powder by using ultrasound-assisted coprecipitation method |
| CN103382103A (en) * | 2013-06-26 | 2013-11-06 | 蚌埠市高华电子有限公司 | Nickel-zinc-copper soft magnetic ferrite and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193472A (en) * | 2013-04-19 | 2013-07-10 | 南通宝聚颜料有限公司 | Method for synthesizing subsphaeroidal barium ferrite superfine powder by using ultrasound-assisted coprecipitation method |
| CN103382103A (en) * | 2013-06-26 | 2013-11-06 | 蚌埠市高华电子有限公司 | Nickel-zinc-copper soft magnetic ferrite and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243580A (en) * | 2016-09-22 | 2016-12-21 | 佛山市飞时达新材料科技有限公司 | A kind of manufacture method of PVC composite cable material |
| CN109637797A (en) * | 2018-12-04 | 2019-04-16 | 天长市昭田磁电科技有限公司 | A kind of preparation method of magnetic Nano material and its preparing the application in magnetic core |
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