CN103192088B - Method for preparing cone-shaped magnetic nickel nanocrystals - Google Patents
Method for preparing cone-shaped magnetic nickel nanocrystals Download PDFInfo
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- CN103192088B CN103192088B CN201310055117.5A CN201310055117A CN103192088B CN 103192088 B CN103192088 B CN 103192088B CN 201310055117 A CN201310055117 A CN 201310055117A CN 103192088 B CN103192088 B CN 103192088B
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Abstract
The invention discloses a method for preparing cone-shaped magnetic nickel nanocrystals. The method comprises the following steps: taking a metal nickel sheet, ultrasonic cleaning, and removing a surface oxidation layer to obtain a basal nickel sheet; adding a reducing agent in a nickel salt water solution with nickel salt concentration of 0.01-3.00 mol/L to form a reaction liquid, and the mass percent concentration of the reducing agent in the total weight of the reaction liquid is 1-30%; and putting the reaction liquid and the basal nickel sheet into a high pressure reactor for heating reaction to obtain the cone-shaped magnetic nickel nanocrystals distributed on the basal nickel sheet. The cone-shaped magnetic nickel nanocrystals with stable quality can be prepared at large scale by the method, and the method as a hydrothermal method is novel, simple in technology, low in energy consumption and high in operability.
Description
Technical field
The present invention relates to the preparation method of technical field of nano material, be specifically related to a kind of preparation method of taper magnetic nickel nano crystalline substance.
Background technology
Nickel (Ni) is a kind of ferromagnetic metal, and the material of its nano-scale has many excellent performances, as magnetic, catalysis and hydrogen storage property etc., is with a wide range of applications at industrial circles such as electronic information, chemical industry, national defence space flight.In recent years, the Ni being applied to every field of various shape is nanocrystalline to be synthesized, as: Ni nano particle, Ni nano wire, Ni nano chain, Ni nanobelt, Ni nanocone and Ni nanometer tree branches structure etc.
Wherein the Ni of taper is nanocrystalline, has the top acicular texture of unique nano-scale, because most advanced and sophisticated enhancement effect shows excellent Field Electron Emission characteristic.Field emission has application very widely, as field emission scanning electron microscope, flat-panel monitor, parallel electron beam photoetching, cathode-ray tube, pressure sensor, vacuum microwave amplifier etc.Therefore for the growth mechanism of its crystal and the aspect that manufactures and designs of advanced function material, there is important researching value and meaning.
Through finding existing literature search, prepare the nanocrystalline technical method all adopting electro-deposition or electro-deposition to combine with anodic oxidation of taper Ni, the method can cause heavier environmental pollution in preparation process medium quantity batch processing, and cost is higher; Therefore, develop a kind of nanocrystalline method of taper Ni of preparing that technique is simple, with low cost, energy consumption is low and there is very major and immediate significance.
Summary of the invention
The object of the invention is to the deficiency existed for above-mentioned prior art, provide that a kind of technique is simple, with low cost, the preparation method of the taper magnetic nickel nano crystalline substance of environmental protection.
The object of the invention is to be achieved through the following technical solutions:
The present invention relates to a kind of preparation method of taper magnetic nickel nano crystalline substance, comprise the following steps:
A, get metal nickel sheet, ultrasonic cleaning, remove surface oxide layer, obtain substrate nickel sheet;
B, at nickel salt concentration be 0.01 ~ 3.00mol/L nickel salt aqueous solution in add amino and go back original reagent forming reactions liquid, it is 1 ~ 30% that described amino goes back the mass percent concentration that original reagent accounts for reactant liquor gross weight;
C, described reactant liquor and substrate nickel sheet are put into autoclave, add thermal response, the described taper magnetic nickel nano that must be distributed in substrate nickel sheet is brilliant.
Preferably, in steps A, described ultrasonic cleaning is specially: described metal nickel sheet is placed in successively each ultrasonic cleaning 10 ~ 30min of acetone, ethanol and deionized water.
Further preferably, in steps A, described removal surface oxide layer is specially: the ultrasonic 40 ~ 60min of the dilute sulfuric acid metal nickel sheet after ultrasonic cleaning being placed in 15 ~ 25wt%.
Preferably, in step B, described nickel salt is nickel chloride, nickel acetate, nickelous sulfate or nickel nitrate.
Preferably, in step B, it is hydrazine hydrate, hydrazine, ethylenediamine or ammoniacal liquor that described amino goes back original reagent.
Preferably, in step C, described in add thermal response adopt hydro-thermal method, heating-up temperature is 70 ~ 150 DEG C, and the heat time is 5 ~ 20 hours.
Compared with prior art, the beneficial effect that the present invention has is: preparation method's technique of the present invention is simple, energy consumption is low, workable; The present invention carries out adjustment optimization by parameters such as nickel ion concentration, reaction time, reaction temperatures in change reactant liquor to the tapering of taper magnetic nickel nano crystalline substance and density.
Accompanying drawing explanation
By reading the detailed description done non-limiting example with reference to the following drawings, other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is the SEM figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 1;
Fig. 2 is the XRD figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 1;
Fig. 3 is the SEM figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 2;
Fig. 4 is the XRD figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 2;
Fig. 5 is the SEM figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 3;
Fig. 6 is the XRD figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 3;
Fig. 7 is the SEM figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 4;
Fig. 8 is the XRD figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 4;
Fig. 9 is the SEM figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 5;
Figure 10 is the XRD figure of taper magnetic nickel nano crystalline substance prepared by the embodiment of the present invention 5.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make certain adjustments and improvements.These all belong to protection scope of the present invention.The experimental technique of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.
embodiment 1
The present embodiment relates to a kind of preparation method of taper magnetic nickel nano crystalline substance, and concrete steps are as follows:
Step one, gets a metal nickel sheet and is placed in each ultrasonic cleaning 20min of acetone, ethanol and deionized water successively, be then placed on ultrasonic 50min in 20wt% dilute sulfuric acid, removes the oxide layer on surface.
Step 2, gets 1.5mmol Nickel dichloride hexahydrate (NiCl
26H
2o) be dissolved in the deionized water of 30mL, ultrasonic 0.5 hour, fully dissolve to nickel chloride, obtained nickel chloride solution, then drip 2mL hydrazine hydrate reduction reagent.
Step 3, solution nickel sheet cleaned for step one and step 2 configured is placed in the polytetrafluoroethylene (PTFE) stainless steel autoclave that capacity is 50mL in the lump, the baking oven putting into 95 DEG C reacts 10h, after question response terminates, nickel sheet is taken out, obtain being distributed in the suprabasil taper magnetic nickel nano of nickel sheet brilliant.
ESEM and the X ray diffracting spectrum of preparing product are distinguished as shown in Figure 1, 2, and the top end diameter of nickel nanocone is about 10nm, and drift angle is about 20 °; Crystallinity is very good.
embodiment 2
The present embodiment relates to a kind of preparation method of taper magnetic nickel nano crystalline substance, and concrete steps are as follows:
Step one, gets a metal nickel sheet and is placed in each ultrasonic cleaning 20min of acetone, ethanol and deionized water successively, be then placed on ultrasonic 50min in 20wt% dilute sulfuric acid, removes the oxide layer on surface.
Step 2, gets 3mmol Nickel dichloride hexahydrate (NiCl
26H
2o) be dissolved in the deionized water of 30mL, ultrasonic 0.5 hour, fully dissolve to nickel chloride, obtained nickel chloride solution, then drip 2mL hydrazine hydrate reduction reagent.
Step 3, solution nickel sheet cleaned for step one and step 2 configured is placed in the polytetrafluoroethylene (PTFE) stainless steel autoclave that capacity is 50mL in the lump, the baking oven putting into 95 DEG C reacts 10h, after question response terminates, nickel sheet is taken out, obtain being distributed in the suprabasil taper magnetic nickel nano of nickel sheet brilliant.
ESEM and the X ray diffracting spectrum of preparing product are distinguished as shown in Figure 3,4, and the top end diameter of nickel nanocone is about 20nm, and drift angle is about 40 °, and crystallinity is very good.
embodiment 3
The present embodiment relates to a kind of preparation method of taper magnetic nickel nano crystalline substance, and concrete steps are as follows:
Step one, gets a metal nickel sheet and is placed in each ultrasonic cleaning 20min of acetone, ethanol and deionized water successively, be then placed on ultrasonic 50min in 20wt% dilute sulfuric acid, removes the oxide layer on surface.
Step 2, gets 1.5mmol nickel acetate and is dissolved in the deionized water of 30mL, ultrasonic 0.5 hour, fully dissolves to nickel acetate, obtained Ni-acetate solution, then drips 2mL hydrazine hydrate reduction reagent.
Step 3, solution nickel sheet cleaned for step one and step 2 configured is placed in the polytetrafluoroethylene (PTFE) stainless steel autoclave that capacity is 50mL in the lump, the baking oven putting into 95 DEG C reacts 10h, after question response terminates, nickel sheet is taken out, obtain being distributed in the suprabasil taper magnetic nickel nano of nickel sheet brilliant.
ESEM and the X ray diffracting spectrum of preparing product are distinguished as shown in Figure 5,6, and the top end diameter of nickel nanocone is about 10nm, and drift angle is about 20 °; Crystallinity is not fine; With the ESEM of embodiment 1 and the more known of X ray diffracting spectrum: the surfaces versus rough of the nickel nanocone formed, the crystalline quality of cone is relatively poor, does not form perfect crystal.
embodiment 4
The present embodiment relates to a kind of preparation method of taper magnetic nickel nano crystalline substance, and concrete steps are as follows:
Step one, gets a metal nickel sheet and is placed in each ultrasonic cleaning 10min of acetone, ethanol and deionized water successively, be then placed on ultrasonic 40min in 15wt% dilute sulfuric acid, removes the oxide layer on surface.
Step 2, gets 90mmol nickel chloride and is dissolved in the deionized water of 30mL, ultrasonic 0.5 hour, fully dissolves to nickel chloride, and obtained nickel chloride solution, then drips 10mL hydrazine also original reagent.
Step 3, solution nickel sheet cleaned for step one and step 2 configured is placed in the polytetrafluoroethylene (PTFE) stainless steel autoclave that capacity is 50mL in the lump, the baking oven putting into 150 DEG C reacts 5h, after question response terminates, nickel sheet is taken out, obtain being distributed in the suprabasil taper magnetic nickel nano of nickel sheet brilliant.
ESEM and the X ray diffracting spectrum of preparing product are distinguished as shown in Figure 7,8, and the top end diameter of nickel nanocone is about 20nm, and drift angle is about 30 °; With the ESEM of embodiment 1 and the more known of X ray diffracting spectrum: when nickel ion concentration is higher, the speed of growth of nickel nanocone crystalline substance is very fast, and growth fully, even forms thicker sheet nickel in some local several nickel nanocone growth nanocrystalline together; The crystalline quality of nickel nanocone crystalline substance is better.
embodiment 5
The present embodiment relates to a kind of preparation method of taper magnetic nickel nano crystalline substance, and concrete steps are as follows:
Step one, gets a metal nickel sheet and is placed in each ultrasonic cleaning 30min of acetone, ethanol and deionized water successively, be then placed on ultrasonic 60min in 25wt% dilute sulfuric acid, removes the oxide layer on surface.
Step 2, gets 0.3mmol nickelous sulfate and is dissolved in the deionized water of 30mL, ultrasonic 0.5 hour, fully dissolves to nickelous sulfate, and obtained nickel sulfate solution, then drips 0.2mL ammoniacal liquor also original reagent.
Step 3, solution nickel sheet cleaned for step one and step 2 configured is placed in the polytetrafluoroethylene (PTFE) stainless steel autoclave that capacity is 50mL in the lump, the baking oven putting into 70 DEG C reacts 20h, after question response terminates, nickel sheet is taken out, obtain being distributed in the suprabasil taper magnetic nickel nano of nickel sheet brilliant.
Prepare the ESEM of product and X ray diffracting spectrum respectively as shown in Fig. 9,10, now because nickel ion concentration in solution is lower, in nucleation process, energy is lower, and the growth of cone crystalline substance is not fully carried out, so the crystal mass of the nickel nanocone finally obtained is relatively slightly poor.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (4)
1. a preparation method for taper magnetic nickel nano crystalline substance, is characterized in that, comprises the following steps:
A, get metal nickel sheet, ultrasonic cleaning, remove surface oxide layer, obtain substrate nickel sheet;
B, at nickel salt concentration be 3.00mol/L nickel salt aqueous solution in add amino and go back original reagent forming reactions liquid, it is 1 ~ 30% that described amino goes back the mass percent concentration that original reagent accounts for reactant liquor gross weight;
C, described reactant liquor and substrate nickel sheet are put into autoclave, add thermal response, the described taper magnetic nickel nano that must be distributed in substrate nickel sheet is brilliant;
Described nickel salt is nickel chloride, and it is hydrazine that described amino goes back original reagent.
2. the preparation method of taper magnetic nickel nano crystalline substance according to claim 1, is characterized in that, in steps A, described ultrasonic cleaning is specially: described metal nickel sheet is placed in successively each ultrasonic cleaning 10 ~ 30min of acetone, ethanol and deionized water.
3. the preparation method of taper magnetic nickel nano crystalline substance according to claim 1, is characterized in that, in steps A, described removal surface oxide layer is specially: the ultrasonic 40 ~ 60min of the dilute sulfuric acid metal nickel sheet after ultrasonic cleaning being placed in 15 ~ 25wt%.
4. the preparation method of taper magnetic nickel nano crystalline substance according to claim 1, is characterized in that, in step C, described in add thermal response adopt hydro-thermal method, heating-up temperature is 70 ~ 150 DEG C, and the heat time is 5 ~ 20 hours.
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| CN201310055117.5A CN103192088B (en) | 2013-02-20 | 2013-02-20 | Method for preparing cone-shaped magnetic nickel nanocrystals |
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| CN201310055117.5A CN103192088B (en) | 2013-02-20 | 2013-02-20 | Method for preparing cone-shaped magnetic nickel nanocrystals |
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| JPS59170209A (en) * | 1983-03-14 | 1984-09-26 | Hitachi Maxell Ltd | Production of magnetic metallic powder for magnetic recording |
| JP4187953B2 (en) * | 2001-08-15 | 2008-11-26 | キャボットスーパーメタル株式会社 | Method for producing nitrogen-containing metal powder |
| KR100564142B1 (en) * | 2004-02-04 | 2006-03-27 | 김선재 | Mass production method for nano-crystal metallic oxide by using ultrasonic spraying heating method |
| CN102633309A (en) * | 2012-01-13 | 2012-08-15 | 沈阳理工大学 | Hydrothermal preparation method for NiS2 with controllable shape |
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