CN102592769A - Preparation method of nickel nanometer particle/silicon nanometer wire magnetic composite material - Google Patents
Preparation method of nickel nanometer particle/silicon nanometer wire magnetic composite material Download PDFInfo
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- CN102592769A CN102592769A CN2012100547052A CN201210054705A CN102592769A CN 102592769 A CN102592769 A CN 102592769A CN 2012100547052 A CN2012100547052 A CN 2012100547052A CN 201210054705 A CN201210054705 A CN 201210054705A CN 102592769 A CN102592769 A CN 102592769A
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Abstract
The invention discloses a preparation method of a nickel nanometer particle/silicon nanometer wire magnetic composite material, comprising the steps of: developing a silicon nanometer wire on a silicon wafer; and then depositing nickel nanometer particles on the silicon nanometer wire to obtain the nickel nanometer particle/silicon nanometer wire magnetic composite materials; the nickel nanometer particles of the material are spherical nanometer particles with uniform size, and the diameters of the nickel nanometer particles are 35-40 nm; the nickel nanometer particles are singly dispersed on the surface of the silicon nanometer wire with a diameter of 20-300 nm and a length of 70-75 microns and are independent to each other without interference; and the nickel nanometer particles have the magnetic characteristics such as high blocking temperature (370 K), high coercive force and low saturation magnetization intensity and the like (when the blocking temperature is 5 K, the saturation magnetization intensity is 4.5 emu/g, and the coercive force is 375.3 Oe; and when the blocking temperature is 400 K, the saturation magnetization intensity is 2.6 emu/g, and the coercive force is 33.3 Oe). The preparation method is simple, low in cost, high in repeatability, low in requirement for preparation environment and suitable for large-scale industrial production. The prepared nickel nanometer particle/silicon nanometer wire magnetic composite material can be applied to the fields of magnetic nanometer materials, nanometer magnetic storage and the like.
Description
Technical field
The present invention relates to magnetic Nano material, nanometer magnetic storage technical field, the preparation method of specifically a kind of nano nickel particles/silicon nanowires magnetic composite.
Background technology
Magnetic nano-particle can be widely used in numerous areas, for example: magnetic fluid, catalysis, biotechnology/medical science, magnetic resonance imaging, storage and environmental engineering etc.Therefore silicon nanowires is deposited on the surface of silicon nanowires with paramagnetic defective with magnetic nanoparticle because there are a large amount of paramagnetic defectives in the surface, forms magnetic composite, will represent the magnetic characteristic that makes new advances.And the preparation process of this type magnetic composite relative complex all at present, preparation condition is harsh, and cost is higher.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of nano nickel particles/silicon nanowires magnetic composite; Harsh to solve existing magnetic composite preparation condition, the problem that cost is high provides a kind of low to environmental requirement; Method is simple; Low cost, high duplication is applicable to the new method of large-scale industrial production.
For realizing the foregoing invention purpose, the concrete technical scheme that the present invention adopts is:
The preparation method of a kind of nano nickel particles/silicon nanowires magnetic composite, this method comprises following concrete steps:
(1) standard RCA cleaning step cleaning silicon chip (< 100>crystal orientation, resistivity is 0.1-10 Ω cm for p-Si, twin polishing), nitrogen dries up subsequent use;
RCA standard cleaning step is:
A) cleaned 10 minutes under the DHF solution room temperature, the DHF solution concentration is 5% the dilution HF aqueous solution;
B) flushing repeatedly under a large amount of deionized water room temperatures;
C) SPM solution cleaned 10 minutes for 120 ℃, and SPM solution is that (Sulfuric Peroxide Mixture, SPM), concrete solution is formulated as H to Piranha
2SO
4: H
2O
2Volume ratio be V
H2O2: V
H2SO4=3: 1;
D) flushing repeatedly under a large amount of deionized water room temperatures;
E) APM solution cleaned 10 minutes for 60 ℃, and APM solution is that (Hydrochloric Peroxide Mixture, APM), concrete solution is formulated as NH to the SC-1 cleaning fluid
4OH: H
2O
2: H
2The volume ratio of O is V
NH4OH: V
H2O2: V
H2O=1: 1: 5;
F) flushing repeatedly under a large amount of deionized water room temperatures;
G) HPM solution cleaned 10 minutes for 60 ℃, and HPM solution is that (Hydrochloric Peroxider Mixture, HPM), concrete solution allocation is HCl: H to the SC-2 cleaning fluid
2O
2: H
2The volume ratio of O is V
HCl: V
H2O2: V
H2O=1: 1: 6;
H) flushing repeatedly under a large amount of deionized water room temperatures;
I) nitrogen dries up.
(2) 25 mmol L
-1AgNO
3Solution and concentration are that 40% hydrofluoric acid mixes, and obtain mixed solution, its 25 mmol L
-1AgNO
3Solution and concentration are that 40% hydrofluoric acid volume ratio is 1:1, and the ultrasonic mixed solution that makes evenly distributes; To be submerged in fully through the silicon chip that cleans and carry out etching in the mixed solution, in etching process, silicon chip surface is vertical with the mixed solution liquid level; And guaranteeing that silicon chip two sides etch rate is identical, in 60～70 minutes reaction time, the two-sided growth of silicon chip has silicon nanowires; Its diameter is 20～300 nm, and length is 70～75 μ m, then; Use a large amount of deionized water rinsings, remove chemical agent residue; Remove depositing silver with nitric acid; A large amount of deionized water rinsings are removed chemical agent residue, and nitrogen dries up subsequent use;
(3) preparation nano nickel particles/silicon nanowires magnetic composite
A) plating bath configuration
With 1 mol L
-1Six hydration nickel sulfate, 0.5 mol L
-1Ammonium sulfate, 0.4 mmolL
-1Neopelex, 2.5 mol L
-1Ammonium fluoride and 0.2 mol L
-1Natrium citricum mixes, and forms mixed solution, and under ammoniacal liquor adjustment mixed solution pH value to 8.5～9.0, the 85 ℃ condition, magnetic agitation is evenly mixed, and is green transparent solution until mixed solution;
The growth that b) will make has the silicon chip of silicon nanowires to place plating bath to react 3～5 seconds; Nano nickel particles is deposited on surface of silicon nanowires, and its diameter is 35～40 nm, then; Use a large amount of deionized water rinsings; Remove surface residue, under nitrogen atmosphere, dry up, obtain nano nickel particles/silicon nanowires magnetic composite.
Said preparation method carries out under normal temperature and pressure conditions.
Outstanding feature of the present invention is:
(1) nano nickel particles is an evenly spherical nanoparticles of size, and diameter is greatly about about 35 nm;
(2) the nano nickel particles list is dispersed in surface of silicon nanowires, and is relatively independent, noiseless mutually;
(3) nano nickel particles/silicon nanowires magnetic composite has high blocking temperature (370 K), magnetic characteristics such as high-coercive force and low saturation magnetic moment;
(4) preparation method is simple, and cost is low, and high duplication is applicable to large-scale industrial production;
(5) normal temperature and pressure prepares environment, and common laboratory equipment can both reach requirement;
(6) can be applicable to numerous areas such as magnetic Nano material, nanometer magnetic storage.
Description of drawings
Fig. 1 is nano nickel particles/silicon nanowires magnetic composite X diffraction (XRD) figure;
Fig. 2 is nano nickel particles/silicon nanowires magnetic composite scanning electron microscopy (SEM) figure;
Fig. 3 is nano nickel particles/silicon nanowires magnetic composite FC/ ZFC figure, and wherein, the physical property tester is under the 100 Oe conditions in magnetic field, adopts cold (FC) null field cold (ZFC) test mode, blocking temperature (T
B) be 370K, magnetic susceptibility (
χ -1) inverse meet Ju Li – weiss law;
Fig. 4 is in the 5-400 K temperature range, nano nickel particles/silicon nanowires magnetic composite magnetic hysteresis loop figure, and during 5 K, saturation magnetization is 4.5 emu/g, coercive force is 375.3 Oe; During 400 K, saturation magnetization is 2.6 emu/g, and coercive force is 33.3 Oe.
Embodiment
Embodiment
A) silicon chip cleans
Get size for 1cm * 1cm silicon chip (< 100>crystal orientation, resistivity is 0.1-10 Ω cm for p type, twin polishing), dry up subsequent use with standard RCA cleaning step cleaning silicon chip nitrogen.
B) silicon chip chemical etching solution preparation
Dispose 25 mmol L
-1AgNO
3, hydrofluoric acid (HF concentration is 40%) mixed solution (25 mmol L
-1AgNO
3With concentration be 1:1 for the 40%HF volume ratio) 200 mL, the ultrasonic mixed solution that makes evenly distributes.
C) silicon chip chemical etching, the preparation silicon nanowires
The chemical replacement reaction takes place in silicon chip in chemical etching solution; Silicon chip surface is etched, and forms silicon nanowire structure, with silicon chip place vertical support frame (the support effect be guarantee silicon chip put into solution after silicon face vertical with the liquid level maintenance) put into solution (silicon chip is flooded by solution fully); Guarantee that silicon chip two sides etch rate is identical; Reaction time is 65 minutes, and the silicon nanowires diameter of two-sided growth is at 100～150 nm, and length is at 70～75 μ m; Use a large amount of deionized water rinsings, remove chemical agent residue; Remove depositing silver with nitric acid; A large amount of deionized water rinsings are removed chemical agent residue, and nitrogen dries up subsequent use.
D) nano nickel particles plating bath configuration
With 1 mol L
-1Six hydration nickel sulfate, 0.5 mol L
-1Ammonium sulfate, 0.4 mmol L
-1Neopelex, 2.5 mol L
-1Ammonium fluoride, 0.2 mol L
-1Natrium citricum and ammoniacal liquor (adjustment pH value to 8.5) are made into 100 mL mixed solutions, and under 85 ℃ of conditions, magnetic agitation is evenly mixed, and is green transparent solution until solution.
E) preparation nano nickel particles/silicon nanowires magnetic composite
Place plating bath to react 3～5 seconds the silicon nanowires for preparing, nano nickel particles is deposited on surface of silicon nanowires, and nano nickel particles is that size is even, and spherical, dispersed nano particle, diameter are greatly about 35～40 nm; Use a large amount of deionized water rinsings, remove surface residue, under nitrogen atmosphere, dry up, preparation generates nano nickel particles/silicon nanowires magnetic composite.
F) size of silicon chip, silicon chip chemical etching solution and nano nickel particles plating bath increase according to aforementioned proportion, and nano nickel particles/silicon nanowires magnetic composite that preparation generates also increases in proportion, is applicable to large-scale industrial production.
G) said preparation method carries out under normal temperature and pressure conditions.
Claims (1)
1. the preparation method of nano nickel particles/silicon nanowires magnetic composite is characterized in that this method comprises following concrete steps:
(1) standard RCA cleaning step cleaning silicon chip (p-Si, twin polishing, < 100>crystal orientation, resistivity is that 0.1-10 W * cm), nitrogen dries up subsequent use;
(2) 25 mmol L
-1AgNO
3Solution and concentration are that 40% hydrofluoric acid mixes, and obtain mixed solution, its 25 mmol L
-1AgNO
3Solution and concentration are that 40% hydrofluoric acid volume ratio is 1:1, and the ultrasonic mixed solution that makes evenly distributes; To be submerged in fully through the silicon chip that cleans and carry out etching in the mixed solution, in etching process, silicon chip surface is vertical with the mixed solution liquid level; And guaranteeing that silicon chip two sides etch rate is identical, in 60～70 minutes reaction time, the two-sided growth of silicon chip has silicon nanowires; Its diameter is 20～300 nm, and length is 70～75 μ m, then; Use a large amount of deionized water rinsings, remove chemical agent residue; Remove depositing silver with nitric acid; A large amount of deionized water rinsings are removed chemical agent residue, and nitrogen dries up subsequent use;
(3) preparation nano nickel particles/silicon nanowires magnetic composite
A) plating bath configuration
With 1 mol L
-1Six hydration nickel sulfate, 0.5 mol L
-1Ammonium sulfate, 0.4 mmolL
-1Neopelex, 2.5 mol L
-1Ammonium fluoride and 0.2 mol L
-1Natrium citricum mixes, and forms mixed solution, and under ammoniacal liquor adjustment mixed solution pH value to 8.5～9.0, the 85 ℃ condition, magnetic agitation is evenly mixed, and is green transparent solution until mixed solution;
The growth that b) will make has the silicon chip of silicon nanowires to place plating bath to react 3～5 seconds; Nano nickel particles is deposited on surface of silicon nanowires, and its diameter is 35～40 nm, then; Use a large amount of deionized water rinsings; Remove surface residue, under nitrogen atmosphere, dry up, obtain nano nickel particles/silicon nanowires magnetic composite; Wherein:
Said silicon chip is p-Si, twin polishing, and < 100>crystal orientation, resistivity is 0.1-10 Ω cm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107482193A (en) * | 2017-08-02 | 2017-12-15 | 合肥国轩高科动力能源有限公司 | The silicon nanowires composite and preparation method that a kind of nano nickel particles and tantnickel nano-substance is modified jointly |
| CN108390051A (en) * | 2018-05-07 | 2018-08-10 | 西南石油大学 | A kind of graphene@silicon composites and preparation method thereof |
| CN111261729A (en) * | 2019-12-31 | 2020-06-09 | 上海匡宇科技股份有限公司 | Silicon slurry for doping, preparation method and doping method of silicon wafer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101266919A (en) * | 2008-04-25 | 2008-09-17 | 华东师范大学 | A method for selectively etching silicon nano line |
| CN101280425A (en) * | 2008-05-23 | 2008-10-08 | 华东师范大学 | Method for non-phosphate electroless nickel plating on silicon nanowires |
| CN101307452A (en) * | 2008-05-23 | 2008-11-19 | 华东师范大学 | Method for preparing Ni/Si nano-wire array and micro-nano humidity sensor based on the nano-wire array |
-
2012
- 2012-03-05 CN CN2012100547052A patent/CN102592769A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101266919A (en) * | 2008-04-25 | 2008-09-17 | 华东师范大学 | A method for selectively etching silicon nano line |
| CN101280425A (en) * | 2008-05-23 | 2008-10-08 | 华东师范大学 | Method for non-phosphate electroless nickel plating on silicon nanowires |
| CN101307452A (en) * | 2008-05-23 | 2008-11-19 | 华东师范大学 | Method for preparing Ni/Si nano-wire array and micro-nano humidity sensor based on the nano-wire array |
Non-Patent Citations (1)
| Title |
|---|
| 殷晋杰: "《金属颗粒—硅纳米线复合结构的制备和应用研究》", 《湘潭大学硕士学位论文》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107482193A (en) * | 2017-08-02 | 2017-12-15 | 合肥国轩高科动力能源有限公司 | The silicon nanowires composite and preparation method that a kind of nano nickel particles and tantnickel nano-substance is modified jointly |
| CN108390051A (en) * | 2018-05-07 | 2018-08-10 | 西南石油大学 | A kind of graphene@silicon composites and preparation method thereof |
| CN108390051B (en) * | 2018-05-07 | 2022-02-11 | 西南石油大学 | Graphene @ silicon composite material and preparation method thereof |
| CN111261729A (en) * | 2019-12-31 | 2020-06-09 | 上海匡宇科技股份有限公司 | Silicon slurry for doping, preparation method and doping method of silicon wafer |
| CN111261729B (en) * | 2019-12-31 | 2022-03-29 | 上海匡宇科技股份有限公司 | Silicon slurry for doping, preparation method and doping method of silicon wafer |
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Application publication date: 20120718 |