CN101041180A - Nanometer Al contained Ni and the preparing method - Google Patents
Nanometer Al contained Ni and the preparing method Download PDFInfo
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Abstract
The invention discloses a nanometer nickel-coated aluminum powder and the preparing method. On the surface of ball aluminum powder a layer of nanometer nickel is coated. The preparing method is that nickel salt and aluminum powder are stock; borohydride and hydrazine hydrate are used as reducing agent; the water solution of nickel salt is poured into the container of ball aluminum powder with water solution of reducing agent; it is not mixed rapidly until when the water solution of nickel salt becomes colorless the nanometer nickel-coated aluminum powder is generated. When the mixing is stopped, after the nanometer nickel-coated aluminum powder is sunk to the bottom rapidly, residual nanometer nickel powder on the upper of water solution is abandoned. After it is washed by water in many times and it is set statically, upper clearing solution is abandoned. Finally as it is filtered and it is dried in flow argon atmosphere, the nanometer nickel-coated aluminum powder with good dispersion is prepared. The invention is provided with high burning efficiency and large releasing energy. The preparing method is provided with simple producing process and easy operation. It can be produced in a large scale and the thickness of nanometer nickel layer can be controlled.
Description
Technical field
The present invention relates to a kind of nanometer Al contained Ni and preparation method thereof.
Background technology
Ball aluminum powder all has been widely used at aspects such as chemical metallurgy, fuel, explosive, deoxidier, agricultural chemicals.Ball aluminum powder widely can fuel as containing in the solid fuel propellant.But in the solid fuel propellant, add ball aluminum powder, oxidant and combustion adjuvant, incomplete combustion often, also has the part activated aluminum in the residue after the burning, mainly be because the alumina layer of the skim densification that forms on the ball aluminum powder surface has adverse influence to burning, cause its efficiency of combustion low.
Nano-nickel powder is meant the nickel powder of granularity less than 100 nanometers.The particle size of nano-nickel powder is little, and its specific surface is big, and chemism is strong.In explosive, add the power that nano-nickel powder can improve explosive; Adding nano-nickel powder in the solid fuel propellant can improve efficiency of combustion and discharge higher energy.
Ball aluminum powder generally adopts the spray-on process preparation, can be controlled at the granularity of ball aluminum powder in certain scope like this.The preparation method of nano-nickel powder has multiple, as vacuum vapor deposition method, metallo-organic compound thermal decomposition method, chemical vapour deposition technique, chemical replacement reducing process etc.Wherein chemical replacement reducing process can be carried out at normal temperatures and pressures; In addition, the way of also available hydro-thermal method pressurized hydrogen reduction prepares nano-nickel powder.Zhou Hui etc. have applied for that name is called the patent of " a kind of method for preparing nano metal nickel powder " (patent No. is ZL01144702.8), provides the method for utilizing the chemical replacement reduction method for preparing nanometer nickel powder.
The alumina layer that removes the ball aluminum powder surface is a kind of effective way that improves the efficiency of combustion of ball aluminum powder, secondly adds nano-nickel powder and also can improve its efficiency of combustion and can discharge higher energy in ball aluminum powder.
Summary of the invention
For addressing the above problem, the object of the present invention is to provide a kind of nanometer Al contained Ni that coats one deck nano-nickel powder on the ball aluminum powder surface.Efficiency of combustion height of the present invention, energy is big.
Another object of the present invention provides simple, the easy-operating nanometer Al contained Ni preparation method of a kind of technology.
For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of nanometer Al contained Ni of the present invention is to coat one deck nano-nickel powder in surface of ball aluminum powder.
Above-mentioned nanometer Al contained Ni obtains by following preparation method:
With nickel salt and ball aluminum powder is raw material, and adding hydrazine hydrate with boron hydride is reducing agent, dissolves nickel salt with pure water, add dispersant stir the aqueous solution of nickel salt; Reducing agent is dissolved in the pure water, and the amount of pure water should be enough to soak ball aluminum powder, ball aluminum powder is immersed in the aqueous solution of reducing agent again; The aqueous solution of nickel salt is poured in the container that fills reducing agent immersion ball aluminum powder, stirred constantly, continue after reduction reaction is finished to stir; After stopping to stir, leave standstill clarification, remove supernatant, stay sediment; With filtering after the pure water washing precipitation 3～6 times; Dry under the argon atmospher that flows then, promptly get nanometer Al contained Ni of the present invention.
The preparation method of above-mentioned nanometer Al contained Ni comprises the steps:
(1), nickel salt is made into the aqueous solution of 0.02～0.1mol/l, add dispersant again, stir and make its dissolving, obtain solution I, wherein the molal quantity ratio of the amount of nickel and dispersant is 1: 0.1～0.5 in the nickel salt;
(2), be granularity that 10～30 microns ball aluminum powder is soaked in the sodium hydrate aqueous solution that concentration is 0.02～0.05mol/l, stirred 10～60 minutes; Add reducing agent then, stir, solution II, wherein the molal quantity ratio of the amount of nickel and reducing agent is 1: 1.0～1.5 in the nickel salt;
(3), solution I is joined in the solution II, stirred 30～60 minutes; The reaction back produces sediment, leaves standstill then, removes supernatant, stays sediment;
(4), use pure water cleaning step (3) gained sediment 3～6 times, filtration then;
(5), will filter the gained sediment under the argon atmospher that flows in 80～120 ℃ of dry processing 10～20 hours, promptly get nanometer Al contained Ni.
Nickel salt described in the above-mentioned preparation method is a kind of of nickelous sulfate, nickel chloride or nickel nitrate etc.
Water described in the above-mentioned preparation method is a kind of of ion exchange pure water, distilled water etc.
Dispersant described in the above-mentioned preparation method is a kind of of polyvinyl alcohol, Triton X-100 or polyoxyethylene alkyl ether etc.
Reducing agent described in the above-mentioned preparation method is potassium borohydride or sodium borohydride+hydrazine hydrate, and the concentration of the reducing agent aqueous solution is 0.1～0.5mol/1; Wherein potassium borohydride or sodium borohydride are 1: 0.1～0.3 with the molal quantity ratio of hydrazine hydrate.
The granularity of the ball aluminum powder described in the above-mentioned preparation method is 10～30 microns.
Nano-nickel powder described in the present invention can prepare with the chemical replacement reducing process, concrete grammar can be referring to patent " a kind of method for preparing nano metal nickel powder " (patent No. is ZL01144702.8), and the granularity of its prepared nano-nickel powder is 20～30 nanometer (see figure 1)s.
Before soaking ball aluminum powder with reducing agent, the purpose with sodium hydrate aqueous solution immersion ball aluminum powder is to remove the aluminium oxide on ball aluminum powder surface earlier in preparation method's step of the present invention (2).
The temperature of reduction reaction is 0～40 ℃ among the preparation method of the present invention.
Can adopt diverse ways to coat one deck nano-nickel powder in surface of ball aluminum powder.The technology and the cladding process of preparation nano-nickel powder can carry out respectively, also can carry out simultaneously.Coating one deck nano-nickel powder on surface of ball aluminum powder promptly is nanometer Al contained Ni.
Among the present invention in the nanometer Al contained Ni weight ratio of nickel determine with chemical analysis.As adopt the weight ratio of nickel element in the complexometry quantitative analysis nanometer Al contained Ni.
Determine that with weight-loss method the nanometer Al contained Ni product is before heat treatment and determine the water content of nanometer Al contained Ni through 120 ℃ of later weight differences of heat treatment in 24 hours in the argon atmospher that flows.
X light diffracting analysis adopts APD-10X optical diffraction instrument, copper target X-ray diffraction, and sweep speed is 4 °/minute, determines phase constituent with the diffraction that draws is linear.Detect composition, the phase structure of nanometer Al contained Ni with the X-ray diffractometer.
The granularity of thickness, uniformity and the nano-nickel powder of ball aluminum powder nano surface nickel aluminium coating can be observed multiplication factor * 5K～50K with the JEM-2000FX transmission electron microscope among the present invention.
Can detect the composition of nickel clad with the energy dispersion X-ray spectrum (EDS power spectrum) of transmission electron microscope.
Along with the nano nickel layer progressive additive that the ball aluminum powder surface is coated, its color becomes Dark grey by light gray gradually.
Description of drawings
Fig. 1. the images of transmissive electron microscope * 50K of nanometer nickel
Fig. 2. the images of transmissive electron microscope * 5K of nanometer Al contained Ni
Fig. 3. the images of transmissive electron microscope * 5K of ball aluminum powder
Fig. 4. the EDS power spectrum of nanometer Al contained Ni superficial layer
The invention has the advantages that: (1), the present invention have increased the combustion activity of ball aluminum powder, the efficiency of combustion height; (2), preparation method of the present invention restores process and the ball aluminum powder table of nano-nickel powder from nickel salt in the aqueous solution The process that bread covers nano-nickel powder is carried out simultaneously, makes reduction and coat a step to finish; The nano nickel that generates coats Layer thickness is more even; (3), preparation method's technological process of the present invention is simple, easy operating; (4), this Bright preparation method can also reclaim the nano-nickel powder that does not coat, and avoids causing the wasting of resources and environmental pollution.
The specific embodiment
The present invention will be further described by the following examples, but the present invention is not constituted any restriction.
Embodiment 1
The preparation of nanometer Al contained Ni, carry out according to following steps:
(1), with 130 the gram nickelous sulfates (commercially available, analyze pure, molecular formula NiSO
46H
2O) be dissolved in 3 liters of pure water, and add 10 gram polyvinyl alcohol, stir and make its dissolving, get solution I;
(2), 500 gram (trade mark is FLQT3) ball aluminum powder (its sem image is seen Fig. 3) are soaked in 2 liters of sodium hydrate aqueous solutions that concentration is 0.02 mol; Stir 10～30 minutes to remove the oxide-film on aluminium powder surface; Again 200 ml water solution and 5 milliliters of hydrazine hydrates of containing 15 gram potassium borohydrides are poured in this container, stirred, get solution II;
(3), solution I is poured in the solution II into lasting the stirring 30 minutes, generation sediment;
(4), stop to stir, leave standstill, tipping upper water solution stays sediment;
(5), use pure water washing and precipitating thing 5 times, filtration then;
(6), sediment that step (5) was cleaned in 120 ℃ of dry processing 12 hours, promptly gets nanometer Al contained Ni under the argon atmospher that flows.
Embodiment 2
Nanometer Al contained Ni to embodiment 1 preparation is done chemical composition analysis.
Compleximetry is adopted in quantitative analysis.Taking by weighing 1 gram composition is that the nanometer Al contained Ni of 3wt% nickel content places 250 ml beakers, adds 1: 1 and analyzes 20 milliliters of the pure HCl aqueous solution, after the nanometer Al contained Ni dissolving, adds pure water and is diluted to 200 milliliters.Get 20 milliliters of above-mentioned solution, regulate pH value to＜6.Add the low amount of fluorinated ammonium in the solution and make the aluminium ion screening agent.The xylenol orange aqueous solution that adds several 3% is made indicator.Come nickel in this solution of titration with EDTA (ethylenediamine tetra-acetic acid) standard liquid of 0.05M.Reaction end becomes yellow by reddish violet.Can calculate the nickel content in the solution.The result shows that nickel shared weight ratio in nanometer Al contained Ni is 2.94wt%.
Embodiment 3
According to usual way the nanometer Al contained Ni of embodiment 1 preparation is done transmission electron microscope and detect, the result shows that the thickness of nano nickel layer is 120 nanometer (see figure 2)s, illustrates to have coated one deck nanometer nickel on the ball aluminum powder surface.
Embodiment 4
Detect the composition of nickel clad of the nanometer Al contained Ni of embodiment 1 gained with the energy dispersion X-ray of transmission electron microscope spectrum (EDS power spectrum), the result shows one deck nickel (see figure 4) on the nanometer Al contained Ni surface.
Embodiment 5
Nanometer Al contained Ni and ball aluminum powder be the combustion test contrast in propellant, carry out combustion test in the FLQT3 ball aluminum powder adding propellant with gained FLQT3 nanometer Al contained Ni among the embodiment 1 and not coating, measure the content of activated aluminum in its residue, active aluminium content in the former the twice combustion test back residue is respectively 0.34wt% and 0.46wt% as a result, and the active aluminium content in the residue of latter's twice combustion test back is respectively 1.5wt% and 1.8wt%.More than the burning of test explanation nanometer Al contained Ni is more abundant, and the active aluminium content in its residue reduces significantly.
Embodiment 6,
Nanometer Al contained Ni among the embodiment 1 (3wt%) and the FLQT3 ball aluminum powder that does not coat are compared test in certain model engine propellant.Make fuel (accounting for the 20wt% of total materials) with above-mentioned ball aluminum powder and nanometer Al contained Ni respectively, potassium bichromate is made oxidant (accounting for the 80wt% of total materials) as potassium oxide, by the required weight charging of this engine propellant, after the igniting, can measure combustion speed and specific impulse etc.
Result of the test (seeing Table 1) nanometer Al contained Ni (3wt%) is compared with the ball aluminum powder that does not coat, and has significantly improved the efficiency of combustion of certain model engine propellant.
Certain model engine propellant test result of table 1.
Annotate: the N.s/Kg of unit of specific impulse is newton. second/kilogram, the energy that sends during with fuel combustion is relevant.The high more then energy of specific impulse is big more.
Claims (8)
1, a kind of nanometer Al contained Ni is characterized in that coating one deck nano-nickel powder in surface of ball aluminum powder.
2, according to the described nanometer Al contained Ni of claim 1, it is characterized in that obtaining by following preparation method: with nickel salt and ball aluminum powder is raw material, adding hydrazine hydrate with boron hydride is reducing agent, dissolves nickel salt with pure water, add dispersant stir the aqueous solution of nickel salt; Reducing agent is dissolved in the pure water, and the amount of pure water should be enough to soak ball aluminum powder, ball aluminum powder is immersed in the aqueous solution of reducing agent again; The aqueous solution of nickel salt is poured in the container that fills reducing agent immersion ball aluminum powder, stirred constantly, continue after reduction reaction is finished to stir; After stopping to stir, leave standstill clarification, remove supernatant, stay sediment; With filtering after the pure water washing precipitation 3～6 times; Dry under the argon atmospher that flows then, promptly get nanometer Al contained Ni.
3, the preparation method of claim 1 or 2 described nanometer Al contained Nis comprises the steps:
(1), nickel salt is made into the aqueous solution of 0.02～0.1mol/l, add dispersant again, stir and make its dissolving, obtain solution I, wherein the molal quantity ratio of the amount of nickel and dispersant is 1: 0.1～0.5 in the nickel salt;
(2), be granularity that 10～30 microns ball aluminum powder is soaked in the sodium hydrate aqueous solution that concentration is 0.02～0.05mol/l, stirred 10～60 minutes; Add reducing agent then, stir, get solution II, wherein the amount of nickel salt nickel is 1: 1.0～1.5 with the molal quantity ratio of reducing agent;
(3), solution I is joined in the solution II, stirred 30～60 minutes; The reaction back produces sediment, leaves standstill then, removes supernatant, stays sediment;
(4), use pure water cleaning step (3) gained sediment 3～6 times, filtration then;
(5), will filter the gained sediment under the argon atmospher that flows in 80～120 ℃ of dry processing 10～20 hours, promptly get nanometer Al contained Ni.
4,, it is characterized in that its described nickel salt is a kind of of nickelous sulfate, nickel chloride or nickel nitrate etc. according to the described preparation method of claim 3.
5,, it is characterized in that its described water is a kind of of ion exchange pure water, distilled water etc. according to the described preparation method of claim 3.
6,, it is characterized in that its described dispersant is a kind of of polyvinyl alcohol, Triton X-100 or polyoxyethylene alkyl ether etc. according to the described preparation method of claim 3.
7, according to the described preparation method of claim 3, it is characterized in that its described reducing agent is potassium borohydride or sodium borohydride+hydrazine hydrate, the concentration of the reducing agent aqueous solution is 0.1～0.5mol/l.
8,, it is characterized in that potassium borohydride in its described reducing agent or sodium borohydride and the molal quantity ratio of hydrazine hydrate are 1: 0.1～0.3 according to the described preparation method of claim 7.
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| CN101927343A (en) * | 2010-08-09 | 2010-12-29 | 山东天诺光电材料有限公司 | Nickel plated aluminum powder and preparation method and application thereof |
| CN102145386A (en) * | 2011-05-06 | 2011-08-10 | 河南煤业化工集团研究院有限责任公司 | Method for preparing metal with surface coated with nano nickel |
| CN102689016A (en) * | 2012-01-15 | 2012-09-26 | 河南科技大学 | Preparation method of superfine nickel powder |
| CN103273061A (en) * | 2013-06-08 | 2013-09-04 | 沈阳化工大学 | Preparation method for electroplating dispersing agent nickel coated aluminum powder |
| CN103433485A (en) * | 2013-08-16 | 2013-12-11 | 北京工业大学 | Nickel package aluminum powder and preparing method thereof |
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| CN101927343B (en) * | 2010-08-09 | 2012-10-03 | 山东天诺光电材料有限公司 | Preparation method of nickel plated aluminum powder |
| CN101927343A (en) * | 2010-08-09 | 2010-12-29 | 山东天诺光电材料有限公司 | Nickel plated aluminum powder and preparation method and application thereof |
| CN102145386A (en) * | 2011-05-06 | 2011-08-10 | 河南煤业化工集团研究院有限责任公司 | Method for preparing metal with surface coated with nano nickel |
| CN102689016B (en) * | 2012-01-15 | 2014-10-22 | 河南科技大学 | Preparation method of superfine nickel powder |
| CN102689016A (en) * | 2012-01-15 | 2012-09-26 | 河南科技大学 | Preparation method of superfine nickel powder |
| CN103273061A (en) * | 2013-06-08 | 2013-09-04 | 沈阳化工大学 | Preparation method for electroplating dispersing agent nickel coated aluminum powder |
| CN103433485A (en) * | 2013-08-16 | 2013-12-11 | 北京工业大学 | Nickel package aluminum powder and preparing method thereof |
| CN103894623B (en) * | 2014-03-19 | 2016-08-17 | 深圳航天科技创新研究院 | A kind of preparation method of antioxidant ultrafine nickel powder |
| CN103894623A (en) * | 2014-03-19 | 2014-07-02 | 深圳航天科技创新研究院 | Preparing method of antioxidant super-fine nickel powder |
| CN104226985A (en) * | 2014-06-29 | 2014-12-24 | 桂林理工大学 | Nickel plating modification method for AB3 type hydrogen storage alloy |
| CN104226985B (en) * | 2014-06-29 | 2016-04-06 | 桂林理工大学 | A kind of AB 3the nickel plating method of modifying of type hydrogen storage alloy |
| CN106077670B (en) * | 2016-08-03 | 2018-07-24 | 杭州科技职业技术学院 | The method that composite codeposition-co-sintering prepares superfine alloy powder |
| CN106077670A (en) * | 2016-08-03 | 2016-11-09 | 杭州科技职业技术学院 | Composite codeposition co-sintering prepares the method for superfine alloy powder |
| CN106825603A (en) * | 2016-12-31 | 2017-06-13 | 西安交通大学青岛研究院 | A kind of aluminium coats the preparation method of titanium composite alloy powder |
| CN108179405A (en) * | 2017-12-18 | 2018-06-19 | 常州市好利莱光电科技有限公司 | A kind of preparation method of Wear-resistant, high-temperature resistant metal-cermic coating |
| CN111774579A (en) * | 2019-04-04 | 2020-10-16 | 南京理工大学 | Al/Ni composite particle and preparation method thereof |
| CN111331130A (en) * | 2020-03-11 | 2020-06-26 | 淮阴师范学院 | Preparation method of flower-shaped nano manganese hydroxide coated aluminum composite material |
| CN111424267A (en) * | 2020-04-24 | 2020-07-17 | 昆明理工大学 | Method for preparing nickel-coated bismuth sulfur chloride |
| CN111424267B (en) * | 2020-04-24 | 2021-10-01 | 昆明理工大学 | Method for preparing nickel-coated bismuth sulfur chloride |
| CN115090876A (en) * | 2022-06-08 | 2022-09-23 | 北京理工大学 | Liquid phase reduction variable frequency ultrasonic amorphous boron nano metal deposition modification method |
| CN116332709A (en) * | 2023-02-22 | 2023-06-27 | 西安近代化学研究所 | Al/polyborane energetic composite material, preparation method and application |
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Effective date of registration: 20160720 Address after: Yang Yanlu 101407 Beijing city Huairou District Yanqi Economic Development Zone No. 88 Patentee after: National standard (Beijing) inspection & Certification Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |