CN101525161B - Method for preparing nickel oxide one dimension nano material - Google Patents

Abstract

The invention relates to a method for preparing nickel oxide one dimension nano material, comprising the process: organic complex aqueous solution with the mass concentration of 1-6% is prepared; metal salt containing nickel element and the organic complex aqueous solution are evenly mixed with each other according to the mass ratio of 1:5-5:1; a base plate is dipped into the mixed solution and tiled at the bottom of the solution; the mixed solution with the base plate is put into a baking oven and heated up to 120-150 DEG C at the speed of 5-20 DEG C/min and then the temperature is maintained for 0.5-3h; the manufactured sample is transferred into a box-type resistance furnace and heated up to 290-310 DEG C at the speed of 5-20 DEG C/min, then the temperature is maintained for 0.5-1h; the temperature is risen to 530-560 DEG C at the speed of 5-20 DEG C/min, and temperature is maintained for 0.5-3h; finally, the nickel oxide one dimension nano material is formed on the base plate. The technique provided by the invention can be used for preparing the nano material with smaller and more uniform size; the method is also further simplified, and the optional scope of the raw materials is wider, thus further reducing the manufacturing cost.

Description

A kind of method for preparing nickel oxide one dimension nano material

Technical field

The invention belongs to the monodimension nanometer material technical field, relate to a kind of method for preparing nickel oxide one dimension nano material, belong to the technology that sintering prepares nickel oxide one dimension nano material.

Background technology

Nickel oxide is a kind of broad stopband metal-oxide semiconductor (MOS) of the 3d of having electronic structure, the energy gap 3.5-3.7eV under the normal temperature.Because nano-nickel oxide has volume effect, quantum size effect, surface effects and macro quanta tunnel effect, thereby possessed excellent catalytic activity, superparamagnetism and thermo-sensitivity, possesses high conductivity and susceptibility, hertzian wave there are strong absorptive character, can also improve transducer sensitivity.Nano-nickel oxide is widely used in fields such as battery electrode, high performance catalyst, magneticsubstance and ceramic coloring material, is a kind of important inorganic nano material.Nickel oxide belongs to NaCl type cube crystalline substance, and its oxygen level is indefinite, can change within the specific limits, and its lattice parameter also changes according to oxygen level, because this inherent lattice imperfection makes it to become a kind of good P-type semiconductor material.The color of nickel oxide changes along with oxygen level, and according to the order that oxygen level reduces, the color of powder is grey black, greyish-green and the green that arrive.

The method for preparing at present nano-nickel oxide has chemical precipitation method, spray pyrolysis, microemulsion method, microwave irradiation, solid phase method and sol-gel method etc.The method for preparing nickel oxide one dimension nano material in the bibliographical information so far mainly concentrates on hydrothermal method, but this type of reaction needed is carried out under the autoclave environment, the equipment complexity, and the very long reaction times of needs more than 24 hours, the popularization that these have all limited this technology is difficult to realize extensive growth.

The patent No. is 200510122214 patent of invention " method for preparing zinc oxide nanowire or zinc oxide nano-belt ", and a kind of method for preparing zinc oxide nanowire or zinc oxide nano-belt is provided.The contriver finds in follow-up technical study, when the nano wire of the prepared that adopts this patent to provide such as ZnO and so on or nano belt, can be because the increase of holding stage, and make the oversize of nano material, and this technology more complicated, cost of manufacture is also than higher.Aspect material choice,, then can limit to the design of technology simultaneously if be restricted to metal acetate salt and polyvinyl alcohol.

Summary of the invention

Purpose of the present invention provides a kind of method for preparing nickel oxide one dimension nano material, and this procedure is simple, and expense is lower, can with unicircuit, semiconductor technology compatibility.

The present invention is realized by the following technical programs: a kind of method for preparing nickel oxide one dimension nano material, it is characterized in that, and comprise following process:

1) with at least a organic substance in gelatin, chitosan, cyclodextrin, Xylo-Mucine, the polyvinyl alcohol as organic complexing agent, under 75～95 ℃ of condition of water bath heating, described organic complexing agent is dissolved in the deionized water, be mixed with mass concentration and be 1～6% organic complex agent solution;

2) water-soluble metal salt nickelous chloride or nickelous acetate and described organic complex agent solution down payment are belonged to 1: 5～5: 1 uniform mixing of mass ratio of salt and organic complexing agent;

3) substrate is immersed mixing solutions, be tiled in the solution bottom;

4) mixing solutions that is equipped with substrate of step 3) is placed baking oven and be warming up to 120～150 ℃, insulation 0.5～3h with the speed of 5～20 ℃/min;

1) sample transfer that step 4) is made is in chamber type electric resistance furnace, is warming up to 290～310 ℃, insulation 0.5～1h with the speed of 5～20 ℃/min; Speed with 5～20 ℃/min is warming up to 530～560 ℃, and insulation 0.5～3h forms nickel oxide one dimension nano material on substrate.

The above-mentioned method for preparing nickel oxide one dimension nano material, the described water-soluble metal salt that contains nickel element is nickelous chloride or nickelous acetate; Described substrate is silicon, quartz or glass material.

Beneficial effect of the present invention is: (all water-soluble inorganic salts of nickel are as nickelous chloride etc. to adopt the metal-salt contain nickel element; The water-soluble organic salt of all of nickel, as nickelous acetate etc.) and organic complexing agent (gelatin, chitosan, cyclodextrin, Xylo-Mucine, POTASSIUM BOROHYDRIDE, polyvinyl alcohol etc., be not only limited to these materials, can be used as the material of organic complexing agent, comprise that all contain in hydroxyl, carboxyl, the amino three kinds of functional groups one or more organic substance) the preparation nickel oxide one dimension nano material, have advantages such as controllability is strong, simple to operate, expense is lower, nickel oxide one dimension nano material, length can reach more than the 10 μ m.Because organic complexing agent has functional group abundant, that be evenly distributed (as hydroxyl, carboxyl, amino etc.), functional group on nickel cation and the organic complexing agent interacts, make nickel salt in the space frame of organic complexing agent, locate, arrange, through the program control type thermal treatment that is rapidly heated, reactions such as metal-salt and the organic complexing agent that contains nickel element decomposes stage by stage, cracking, oxidation are by the proportioning realization nickel oxide one dimension nano material controlledly synthesis of sequence of control intensification parameter and different concns.Because thermal treatment temp is low, can with existing integrated circuits, semiconductor technology compatibility.Operational path compared to the preparation zinc oxide nanowire of the application of contriver before, technology provided by the invention, owing to reduced holding stage, can make the littler nano material of size, the size of while nano material is homogeneous more, and the trend that presents array arrangement, and also further simplification of technology, thereby further reduced cost of manufacture.Simultaneously aspect material choice, more wide in range, it is bigger to make the design of synthesis technique and conditional parameter choose the space.

Specific implementation method

Generally, preparation method of the present invention is as follows:

1) under 75～95 ℃ of water-baths or heating condition, with organic complexing agent (gelatin, chitosan, cyclodextrin, Xylo-Mucine, POTASSIUM BOROHYDRIDE, polyvinyl alcohol etc., be not only limited to these materials, can be used as the material of organic complexing agent, comprise that all contain hydroxyl, carboxyl, amino organic substance) dissolve in the deionized water, be mixed with mass concentration and be 1～6% organic complex solution;

2) (all water-soluble inorganic salts of nickel are as nickelous chloride etc. will to contain the metal-salt of nickel element; The water-soluble organic salt of all of nickel is as nickelous acetate etc.) and the organic complex aqueous solution press 1: 5～5: 1 uniform mixing of mass ratio of metal-salt and organic complexing agent;

3) substrate (as silicon, quartz or glass) is immersed mixing solutions, be tiled in the solution bottom;

4) mixing solutions that is equipped with substrate of step 3) is placed baking oven and be warming up to 120～150 ℃, insulation 0.5～3h with the speed of 5～20 ℃/min;

5) sample transfer that step 4) is made is in chamber type electric resistance furnace, is warming up to 290～310 ℃, insulation 0.5～1h with the speed of 5～20 ℃/min; Speed with 5～20 ℃/min is warming up to 530～560 ℃, and insulation 0.5～3h forms nickel oxide one dimension nano material on substrate.

Nickel oxide one dimension nano material with nickelous chloride, nickelous nitrate, nickelous acetate and gelatin, polyvinyl alcohol preparation is that example illustrates how to implement the present invention below, the invention is not restricted to these embodiment.

Embodiment 1

In quartz beaker, under 75～95 ℃ of water-baths or heating condition, the 4g polyvinyl alcohol is dissolved in the 100ml deionized water; Add the 2g nickelous chloride, adopt magnetic agitation 0.5h, rotating speed 800 commentaries on classics/min are with the ultrasonic dispersing 0.5h of 40KHz, 150W.Quartz glass substrate is tiled in the quartz beaker bottom.Then quartz beaker is placed baking oven and be warming up to 120 ℃ with the speed of 5 ℃/min, insulation 0.5h is until oven dry.Sample transfer in chamber type electric resistance furnace, is warming up to 300 ℃ of following thermal treatment 0.5h with the speed of 5 ℃/min; Speed with 5 ℃/min is warming up to 550 ℃, insulation 1h.SEM observes discovery, and formation diameter 30～50nm, length surpass the nano wire of 15 μ m on substrate.

Embodiment 2

Present embodiment to implement 1 similarly, difference is that the consumption of nickelous acetate and gelatin is 4g in the step 2, is warming up to 130 ℃ with the speed of 10 ℃/min, insulation 0.5h is until oven dry.Sample transfer in chamber type electric resistance furnace, is warming up to 310 ℃ of following thermal treatment 0.5h with the speed of 10 ℃/min; Speed with 10 ℃/min is warming up to 560 ℃, insulation 1h.SEM observes discovery, and product is the nanometer rod of the about 50～80nm of diameter, length 10 μ m.

Embodiment 3

Present embodiment is similar to example 1, and difference is that the consumption of nickelous nitrate and gelatin is 4g and 2g in the step 2, is warming up to 150 ℃ with the speed of 15 ℃/min, and insulation 1h is until oven dry.With sample transfer in chamber type electric resistance furnace, with 310 ℃ of the speed of 15 ℃/min, insulation 1h; Speed with 15 ℃/min is warming up to 560 ℃, insulation 3h.SEM observes discovery, and product is the nanometer rod of the about 80～100nm of diameter, length 10 μ m.

Embodiment 4

Present embodiment is similar to example 1, and difference is that the consumption of nickelous chloride and gelatin is 4g and 2g in the step 2, is warming up to 140 ℃ with the speed of 20 ℃/min, and insulation 1h is until oven dry.With sample transfer in chamber type electric resistance furnace, with 315 ℃ of the speed of 20 ℃/min, insulation 1h; Speed with 20 ℃/min is warming up to 550 ℃, insulation 2h.SEM observes discovery, and product is the nanometer rod of the about 100～150nm of diameter, length 10 μ m.

Embodiment 5

Present embodiment is similar to example 3, and difference is in the step 2 that present embodiment only adopts mechanical stirring 0.5h, rotating speed 800 commentaries on classics/min.SEM observes discovery, and the nano wire of diameter 100～1000nm, the about 10 μ m of length is arranged in the product.

Claims (2)

1. a method for preparing nickel oxide one dimension nano material is characterized in that, comprises following process:

1) with at least a organic substance in gelatin, chitosan, cyclodextrin, Xylo-Mucine, the polyvinyl alcohol as organic complexing agent, under 75～95 ℃ of condition of water bath heating, described organic complexing agent is dissolved in the deionized water, be mixed with mass concentration and be 1～6% organic complex agent solution;

2) water-soluble metal salt nickelous chloride or nickelous acetate and described organic complex agent solution down payment are belonged to 1: 5～5: 1 uniform mixing of mass ratio of salt and organic complexing agent;

3) substrate is immersed mixing solutions, be tiled in the solution bottom;

4) mixing solutions that is equipped with substrate of step 3) is placed baking oven and be warming up to 120～150 ℃, insulation 0.5～3h with the speed of 5～20 ℃/min;

5) sample transfer that step 4) is made is in chamber type electric resistance furnace, is warming up to 290～310 ℃, insulation 0.5～1h with the speed of 5～20 ℃/min; Speed with 5～20 ℃/min is warming up to 530～560 ℃, and insulation 0.5～3h forms nickel oxide one dimension nano material on substrate.

2. the method for preparing nickel oxide one dimension nano material according to claim 1 is characterized in that, described substrate is silicon, quartz or glass material.