CN1320176C - Magnetic modified nanometer zinc oxide whiskers and production thereof - Google Patents
Magnetic modified nanometer zinc oxide whiskers and production thereof Download PDFInfo
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- CN1320176C CN1320176C CNB2005100208655A CN200510020865A CN1320176C CN 1320176 C CN1320176 C CN 1320176C CN B2005100208655 A CNB2005100208655 A CN B2005100208655A CN 200510020865 A CN200510020865 A CN 200510020865A CN 1320176 C CN1320176 C CN 1320176C
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- zinc oxide
- oxide whiskers
- magnetic
- hydrosol
- magnetic nano
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 4
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 claims abstract 6
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract 4
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract 3
- 241001455273 Tetrapoda Species 0.000 claims abstract 2
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000013067 intermediate product Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims 2
- 238000013329 compounding Methods 0.000 claims 1
- 150000002431 hydrogen Chemical class 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 10
- 239000002122 magnetic nanoparticle Substances 0.000 abstract description 6
- 238000004891 communication Methods 0.000 abstract description 2
- 238000010304 firing Methods 0.000 abstract 2
- 230000007123 defense Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 235000013980 iron oxide Nutrition 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
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- Compounds Of Iron (AREA)
- Soft Magnetic Materials (AREA)
Abstract
本发明提供一种磁性纳米改性氧化锌晶须的制备方法，是将四针状氧化锌晶须均匀地悬浮在溶有二氯化铁的聚乙二醇水溶胶中，调整水溶胶的pH值为7～12，加入过氧化氢反应，过滤反应产物，将滤渣真空干燥，然后通氮进行第一次培烧，再通氢进行第二次培烧，随炉冷却，得到在四针状氧化锌晶须表面均匀地合成有磁性纳米颗粒的磁性纳米改性氧化锌晶须。操作简单，成本低，易于工业化推广，产品具有良好的磁性能及综合性能，主要用于国防设备、电器设备及通讯设备等领域。
The invention provides a method for preparing magnetic nano-modified zinc oxide whiskers, which is to uniformly suspend tetrapod zinc oxide whiskers in polyethylene glycol hydrosol dissolved with ferric chloride, and adjust the pH of the hydrosol The value is 7-12, add hydrogen peroxide to react, filter the reaction product, vacuum-dry the filter residue, then pass nitrogen for the first firing, then pass hydrogen for the second firing, and cool with the furnace to obtain four-needle Magnetic nano-modified zinc oxide whiskers with magnetic nanoparticles uniformly synthesized on the surface of the zinc oxide whiskers. The operation is simple, the cost is low, and it is easy to promote in industrialization. The product has good magnetic properties and comprehensive performance, and is mainly used in the fields of national defense equipment, electrical equipment and communication equipment.
Description
Technical field
The present invention relates to a kind of preparation method of magneticsubstance, particularly relate to a kind of preparation method of magnetic modified nanometer zinc oxide whiskers.
Background technology
ZnOw is a kind of crystalline material with three-dimensional four acicular structures, and four acicular structures of its uniqueness combine with the semiconducting behavior of excellence has given ZnOw powerful multi-functional characteristic.And by ZnOw being carried out the magnetic modification, magnetic indexs such as the magnetic permeability of raising ZnOw, the specific magnetising moment will be given ZnOw strong functions characteristic more.Such as the time, its electromagnetic shielding and stealth effect are improved largely as electromagnetic shielding material and stealth material.At present, carry out the magnetic modification and mainly contain two approach.First doped magnetic metal ion, because the restriction of oxidated zinc lattice dimensions and doped metal ion radius, only there are only a few metal ions such as iron ion can mix zinc oxide lattice at present, but its doping is very little, and doping process needs could realize under the hot conditions more than 800 ℃, power consumption is big, and the gained doped products does not have tangible magnetic and improves effect; It two is to mix inorganic magnetic, though this method has certain magnetic to improve effect, its mixing uniformity is poor, thereby the magnetic stability of product is poor, as mixing with mechanical means such as ball milleds, and four acicular structures that also can disruptive oxidation zinc whisker.
Summary of the invention
The objective of the invention is to overcome above-mentioned shortcoming, provide a kind of simple to operate, cost is low, is easy to industrialization promotion, and products obtained therefrom had both kept four acicular structures of ZnOw, had again preferably, the preparation method of the magnetic modified nanometer zinc oxide whiskers of stabilized magnetic energy.
Among the preparation method of magnetic modified nanometer zinc oxide whiskers of the present invention its feed composition cooperate ratio by weight the percentage ratio meter be:
Four acicular type zinc oxide crystal whisker (ZnOw) 15～55%,
Ferrous chloride (FeCL
24H
2O) 4～10%,
Polyoxyethylene glycol (PEG) 38～75%.
Preparation process is as follows:
1) with FeCL
24H
2It is in 30～60% the PEG water-sol that O is dissolved in concentration expressed in percentage by weight.
2) will the ZnOw after ultrasonication evenly being suspended in above-mentioned 1) in the PEG water-sol, wherein, ultrasonic power is 120 watts, 10 minutes treatment times.
3) adopting the sodium hydroxide of 20% (weight) to adjust above-mentioned 2) pH value of the water-sol is 7～12, adds concentration 30% (weight) hydrogen peroxide (H
2O
2) aqueous solution, stirring reaction is 3～5 hours under 50～70 ℃ of temperature, gets reaction product.Wherein, by weight, feed composition: H
2O
2=100: 1.2～3.0, stirring velocity is controlled to be 300～800 rev/mins.
4) with 3) reaction product is filtered, and the vacuum-drying filter residue, gets intermediate product.General vacuum-drying condition be 50 ℃ ,-0.09MPa.
5) with 4) the gained intermediate product under 250～300 ℃ of temperature, feed N
2Gas roasting 1～2 hour feeds H then
2Gas in 500～530 ℃ of roasting temperatures 2～3 hours, cools to room temperature with the furnace under hydrogen atmosphere, magnetic modified nanometer zinc oxide whiskers of the present invention.
Utilize the activity of PEG among the preparation method of the present invention, make it, make the PEG can be well attached to the ZnOw surface as the bridging thing.Add hydrogen peroxide as oxidant, Oxidation of Fe
2+Obtain newly-generated ferric oxide, can form coordination with the ether in the PEG molecule and combine, magnetic nanoparticle ferric oxide original position is synthesized on the ZnOw surface.For guaranteeing that the PEG micella becomes Fe
2+The main generation place of oxidizing reaction, the concentration expressed in percentage by weight that should control PEG is 30～60%.The pH value of the hierarchy of control is 7～12, helps Fe in the system
2+Oxidation, and control stirring velocity, temperature of reaction and reaction times, then help realizing the size of magnetic nanoparticle and control magnetic-particle synthetic improving the homogeneity of magnetic nanoparticle in the ZnOw surface arrangement at the ZnOw surface in situ.Intermediate product in the system feeds nitrogen and carries out the roasting first time, is to make the PEG in the system that decomposition reaction take place, and decomposes the gaseous state small molecules that produces and then gets rid of with nitrogen, eliminates the influence of PEG to magnetic.After stopping logical nitrogen, change logical hydrogen immediately, the rising furnace temperature is carried out the roasting second time, and reducing iron oxides guarantee that PEG decomposes the back magnetic nanoparticle and still is distributed in the ZnOw surface uniformly and stably.Can adjust by the time of controlling logical hydrogen that magnetic components is Fe in the magnetic modified nanometer zinc oxide whiskers
3O
4, FeO, Fe or its mixture, thereby specific saturation magnetization, magnetic permeability, coercive force equimagnetic performance index by the adjusting of product magnetic components being regulated and control product, thereby obtain a series of products that satisfy multiple needs.
The preparation method of magnetic modified nanometer zinc oxide whiskers of the present invention, its advantage is the supersound process by ZnOw, the original position generation of ferric oxide and the bridge linking effect of PEG, realized that magnetic receives particle evenly synthetic on the ZnOw surface, obtained composition and the adjustable magnetic modified nanometer zinc oxide whiskers of magnetic by roasting.Do not destroy four acicular structures of former ZnOw, simple to operate, reproducibility is good, and cost is low, is easy to industrialization promotion.The products obtained therefrom magnetic modified nanometer zinc oxide whiskers has preferably, stable magnetic property and excellent comprehensive performance, and the specific saturation magnetization when room temperature reaches 2.10～7.01emu/g, and coercive force reaches 60～115Oe.This product can be widely used in fields such as defence equipment, electrical equipment, communication equipment.This product is compared with the invisible coating of the common zinc oxide whisker that uses same amount, when coating density is 1.2kg/m during as the main wave absorbing agent in stealthy (suction ripple) coating
2The time, the qualified bandwidth of-4dB is extended to 4～18GHz by 8 original～18GHz, and coat-thickness is reduced to 1mm by original 2mm.
Description of drawings
Fig. 1: comparative example scanning electron microscope diagram
Fig. 2: embodiment 1 magnetic modified nanometer zinc oxide whiskers scanning electron microscope diagram
Fig. 3: embodiment 3 magnetic modified nanometer zinc oxide whiskers scanning electron microscope diagrams
Fig. 4: embodiment 5 magnetic modified nanometer zinc oxide whiskers scanning electron microscope diagrams
Fig. 5: embodiment 12 magnetic modified nanometer zinc oxide whiskers scanning electron microscope diagrams
Fig. 6: embodiment 1 magnetic modified nanometer zinc oxide whiskers X-ray diffraction figure
Fig. 7: embodiment 5 magnetic modified nanometer zinc oxide whiskers X-ray diffraction figure
Fig. 8: embodiment 12 magnetic modified nanometer zinc oxide whiskers X-ray diffraction figure
Embodiment
Feed composition proportioning and the processing condition of table 1: embodiment
| ZnOw consumption (g) | FeCl 2Consumption (g) | PEG consumption (g) | H 2O 2Consumption (g) | The PH value | Temperature of reaction (℃) | Reaction times (h) | Stirring velocity (r/min) | Logical N 2Time (h) | Logical H 2Time (h) | |
| Embodiment 1 | 54.8 | 5.5 | 39.7 | 1.7 | 7 | 50±2 | 3 | 300 | 1 | 2 |
| Embodiment 2 | 40.0 | 4.0 | 56.0 | 1.2 | 8 | 50±2 | 3 | 400 | 1 | 2 |
| Embodiment 3 | 40.0 | 8.0 | 52.0 | 2.4 | 9 | 60±2 | 4 | 500 | 1 | 2 |
| Embodiment 4 | 25.0 | 10.0 | 65.0 | 3.0 | 10 | 60±2 | 4 | 600 | 1 | 2 |
| Embodiment 5 | 20.0 | 10.0 | 70.0 | 3.0 | 11 | 70±2 | 5 | 700 | 1.5 | 2.5 |
| Embodiment 6 | 15.0 | 10.0 | 75.0 | 3.0 | 12 | 70±2 | 5 | 800 | 1.5 | 2.5 |
| Embodiment 7 | 54.8 | 5.5 | 39.7 | 1.7 | 12 | 50±2 | 4 | 600 | 1.5 | 2.5 |
| Embodiment 8 | 40.0 | 4.0 | 56.0 | 1.2 | 11 | 50±2 | 4 | 500 | 1.5 | 2.5 |
| Embodiment 9 | 40.0 | 8.0 | 52.0 | 2.4 | 10 | 70±2 | 3 | 700 | 2 | 3 |
| Embodiment 10 | 25.0 | 10.0 | 65.0 | 3.0 | 9 | 70±2 | 3 | 800 | 2 | 3 |
| | 20.0 | 10.0 | 70.0 | 3.0 | 8 | 60±2 | 5 | 400 | 2 | 3 |
| Embodiment 12 | 15.0 | 10.0 | 75.0 | 3.0 | 7 | 60±2 | 5 | 300 | 2 | 3 |
Table 2: magnetic nanoparticle ZnOw performance
| Specific saturation magnetization (emu/g) | Coercive force (Oe) | Microscopic appearance and composition | |
| Embodiment 1 | 2.10 | 115 | Fig. 2, Fig. 6 |
| Embodiment 2 | 2.12 | 114 | |
| Embodiment 3 | 2.49 | 112 | Fig. 3 |
| Embodiment 4 | 2.90 | 110 | |
| Embodiment 5 | 6.28 | 97 | Fig. 4, Fig. 7 |
| Embodiment 6 | 7.01 | 93 | |
| Embodiment 7 | 2.06 | 86 | |
| Embodiment 8 | 2.07 | 86 | |
| Embodiment 9 | 2.41 | 72 | |
| | 2.80 | 70 | |
| | 6.11 | 65 | |
| Embodiment 12 | 6.80 | 60 | Fig. 5, Fig. 8 |
| Comparative example (ZnOw) | Nonmagnetic | Fig. 1 | |
Claims (3)
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100208655A CN1320176C (en) | 2005-05-08 | 2005-05-08 | Magnetic modified nanometer zinc oxide whiskers and production thereof |
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|---|---|---|---|
| CNB2005100208655A CN1320176C (en) | 2005-05-08 | 2005-05-08 | Magnetic modified nanometer zinc oxide whiskers and production thereof |
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| CN1712577A CN1712577A (en) | 2005-12-28 |
| CN1320176C true CN1320176C (en) | 2007-06-06 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899708B (en) * | 2010-07-23 | 2012-02-01 | 北京航空航天大学 | A tetragonal zinc oxide/ferrite thin film material and its preparation method |
| CN102586881A (en) * | 2010-10-29 | 2012-07-18 | 北京矿冶研究总院 | Preparation method of zinc oxide whisker containing metal nickel copper |
| CN108752782A (en) * | 2018-05-18 | 2018-11-06 | 赵顺全 | A kind of preparation method of modified resin type ceiling |
| CN113072875A (en) * | 2021-04-08 | 2021-07-06 | 湖北金诺誉新材料科技有限公司 | Water-based sealing primer as well as preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4960654A (en) * | 1988-08-29 | 1990-10-02 | Matsushita Electric Industrial Co., Ltd. | Metal composition comprising zinc oxide whiskers |
| CN1298039A (en) * | 1999-12-01 | 2001-06-06 | 肖猛 | Zinc oxide whisker coated with metal layer |
| CN1384056A (en) * | 2002-06-12 | 2002-12-11 | 云南省冶金研究设计院 | Process and apapratus of producing four-needle zine oxide whisker |
| CN1598081A (en) * | 2004-08-12 | 2005-03-23 | 沈阳化工学院 | Technology for continuous producing four-feet shape zine oxide whisker and rotating furnace thereof |
-
2005
- 2005-05-08 CN CNB2005100208655A patent/CN1320176C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4960654A (en) * | 1988-08-29 | 1990-10-02 | Matsushita Electric Industrial Co., Ltd. | Metal composition comprising zinc oxide whiskers |
| CN1298039A (en) * | 1999-12-01 | 2001-06-06 | 肖猛 | Zinc oxide whisker coated with metal layer |
| CN1384056A (en) * | 2002-06-12 | 2002-12-11 | 云南省冶金研究设计院 | Process and apapratus of producing four-needle zine oxide whisker |
| CN1598081A (en) * | 2004-08-12 | 2005-03-23 | 沈阳化工学院 | Technology for continuous producing four-feet shape zine oxide whisker and rotating furnace thereof |
Non-Patent Citations (1)
| Title |
|---|
| 氧化锌晶须的特点及其应用 吴华武等，无机盐工业，第4卷 1996 * |
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