CN1843673A - Metal nano nickel tube and preparation method thereof - Google Patents
Metal nano nickel tube and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a metallic nanometer nickel tube and relative preparation. Wherein, said metallic nanometer nickel tube is a nanometer nickel tube whose outer diameter is 15-150 nanometers. Said preparing method comprises: (1) using porous template of anode alumina which has been sensitized and activated as the cathode of electrochemistry reaction; using nickel material as anode of electrochemistry reaction; using the solution of nickel salt and boric acid as plating liquid; (2) dipping the anode and cathode into plating liquid, switching on the power source, and using direct current to deposit nickel on said alumina template; dissolving the template with alkali solution, to attain metallic nanometer nickel tube. The inventive method has simple process, with high yield and wider application.
Description
Technical field
The invention belongs to the technical field of preparation nano material.Be particularly related to metal nano nickel tube and preparation method.
Background technology
Nano material is that a kind of typical Jie sees system, it causes characteristics such as unusual mechanics, electricity, magnetics, calorifics, optics and chemism owing to have skin effect, small-size effect, quantum size effect and objective quantum tunneling effect etc., make it in national defence, electronics, nuclear technology, metallurgy, aviation, light industry, medicine and other fields, have important use and be worth, thereby start the upsurge of people nano material preparation and research.According to the free degree meter that is not retrained in the three dimensions, be broadly divided into the nanometer powder (particle or elementide) of zero dimension, the nanofiber (pipe) of one dimension, the nanometer film of two dimension, three-dimensional nano block etc. by nanoscale.Wherein the nanometer powder development time the longest, technology is the most ripe, is the basis that produces other three series products; Nano bulk material is based on the fine and close or non-compact solid that other low-dimensional materials constitute.As seen, the development potentiality of current nanofiber is very huge comprising nano wire, nano wire, nanometer rods, nanotube, nanometer band etc.Nano metal material has skin effect.Along with particle diameter diminishes, its specific area will enlarge markedly, and illustrates that the shared percentage of surface atom will increase significantly.Huge specific area causes the serious mismatch of key attitude, many activated centres occur, and surface step and roughness increase, and the surface shows the chemical valence of balance, non-integer coordination non-chemically, causes the chemical property of nanometer system and Chemical Equilibria Systems very big difference to occur.Therefore the surface of metal ultramicro powder has very high activity.
Summary of the invention
The invention provides the method for metal nano nickel tube and preparation, for the extensive use of metal nano nickel tube lays the foundation.
Metal nano nickel tube of the present invention is that external diameter is the 15-150 nano nickel tube.
The preparation method of metal nano nickel tube, step is as follows:
Negative electrode when (1) adopting anodised aluminium foraminous die plate through sensitization and activation as electrochemical reaction; With the nickel material is the anode of electrochemical reaction; To contain nickel salt, the solution of boric acid is electroplate liquid;
(2) with in negative electrode and the anode immersion plating liquid, connect power supply, under the direct current effect on alumina formwork plated metal nickel; Template can obtain metal nano nickel tube through the alkaline solution dissolving.
Sensitization of the present invention is that sensitized porous aluminium oxide is touched plate in acid stannous salt solution or tin-salt solution; Sensitization time is 0.5-10 minute at ambient temperature.
Activation of the present invention is that the activation Woelm Alumina is touched plate in silver salt or palladium salting liquid; Soak time is 0.5-10 minute under ℃ condition of room temperature～50.
Sensitizing solution of the present invention and activating solution prescription are as follows:
The prescription of the inferior solution of tin of acid divalence is stannous chloride 10-30g/L, hydrochloric acid 0.1-2mol/L;
The prescription of tin-salt solution is stannic chloride 12-60g/L, potassium pyrophosphate 120-140g/L or natrium citricum 20-80g/L or sodium tartrate 20-80g/L or sodium ethylene diamine tetracetate 20-80g/L and this type of polycarboxylic acid or multi-hydroxy carboxy acid or multi-hydroxy multi-carboxy acid or their alkaline-earth metal salt equivalent concentration.
The prescription of silver salt activating solution is: silver nitrate 0.5-5g/L, or silver nitrate 0.5-5g/L and add ammoniacal liquor to solution becomes and clarify;
The prescription of palladium salt activating solution is: palladium bichloride 0.2-5g/L, hydrochloric acid 0.1-2mol/L, or palladium bichloride 0.2-5g/L, hydrochloric acid 0.1-2mol/L, stannous chloride 30-50g/L.
The nickel salt of electroplate liquid of the present invention is a nickelous sulfate, nickel chloride, and nickel sulfamic acid or their composition, nickel salt concentration are 40-300g/L; Boric acid concentration is 30-50g/L.
Woelm Alumina of the present invention is touched plate: adopting high-purity aluminium sheet is anode, electrolyte is oxalic acid solution or the phosphoric acid solution of 2%-5% or the sulfuric acid solution of 2%-5% of 2%-5%, negative electrode is titanium net or carbon-point, anodic oxidation voltage 20-110 volt, oxidization time is 0.5-6 hour, and temperature is 5-25 ℃.
The electric current of electronickelling of the present invention is 5-100mA/cm
2Direct current, electroplating time are 0.5-10 minute, and temperature is 40-60 ℃.
Alkaline solution of the present invention is NaOH or potassium hydroxide solution.
Can be refined as following steps in the concrete operations: (1) makes porous alumina formwork with anodizing; (2) acid stannous salt solution or the sensitized porous aluminium oxide of tin-salt solution are touched plate; (3) silver salt or palladium salting liquid activation Woelm Alumina is touched plate, makes the active oxidation aluminum alloy pattern plate, the negative electrode during as electrochemical reaction; (4) to contain nickel salt, the solution of boric acid is electroplate liquid; (5) be the anode of electrochemical reaction with nickel screen or nickel sheet; (6) with in negative electrode and the anode immersion plating liquid, connect power supply, under the direct current effect on alumina formwork plated metal nickel; (7) template can obtain the powder metal nano nickel tube through the alkaline solution dissolving behind the cleaning-drying.
Characteristics of the present invention are: at first found nano nickel tube and effective preparation method thereof, for the metal nano-tube extended familys have increased new a member.The method manufacture craft is simple, and nickel pipe output height, and very big actual application value is arranged.Metallic nickel is employed in a lot of places as functional material.For example skeleton nickel can be used as the electrode with catalytic activity, and nickel powder is as the hydrogenation catalyst of electrode material and hydro carbons, and the nickel fiber is as oxidation catalyst of methyl alcohol etc. etc.The nanometer nickel of tubulose is expected to improve the using value of nickel as functional material because its above-mentioned special construction may show some unusual physics and chemical functionals.
Figure of description
Fig. 1: single external diameter is about the nickel pipe Electronic Speculum figure of 15 nanometers;
Fig. 2: single external diameter is about the nickel pipe Electronic Speculum figure of 50 nanometers;
Fig. 3: single external diameter is about the nickel pipe Electronic Speculum figure of 150 nanometers;
Fig. 4: the Electronic Speculum figure of many root nano nickel tubes.
The specific embodiment
Embodiment 1:
With purity is that high-purity aluminium sheet of 99.99% is an anode, and the titanium net is a negative electrode, and under 40 volts of direct currents, in 3% oxalic acid solution, the room temperature electrolysis obtained porous alumina formwork in 1.5 hours under 15 ℃.To contain stannous chloride 10g/L, the solution of hydrochloric acid 0.2mol/L is activating solution, the porous alumina formwork that makes is soaked under 20 ℃ and carries out sensitization in 0.5 minute.Porous alumina formwork immersion with above-mentioned sensitization under 20 ℃ contains silver nitrate 0.5g/L, and activation made active porous alumina formwork in 0.5 minute in the solution of ammoniacal liquor 8ml/L (mass fraction 37%).With sulfur acid nickel 30g/L, nickel sulfamic acid 10g/L, the solution of boric acid 30g/L is made anode as electrolyte with nickel screen, under 40 ℃ at 5mA/cm
2Direct current under cold galvanising nickel is deposited on the active porous alumina formwork.The above-mentioned alumina formwork that deposits nickel is cleaned up with distilled water, immerse then in 10% the sodium hydroxide solution and dissolve template,, can obtain the metal nano nickel tube of diameter in the 15-150 nanometer with the precipitation cleaning-drying that obtains.
Embodiment 2:
With purity is that high-purity aluminium sheet of 99.99% is an anode, and carbon-point is a negative electrode, and under 100 volts of direct currents, in 2% sulfuric acid solution liquid, the room temperature electrolysis obtained porous alumina formwork in 6 hours under 5 ℃.To contain stannous chloride 30g/L, the solution of hydrochloric acid 2mol/L is activating solution, the porous alumina formwork that makes is soaked under 20 ℃ and carries out sensitization in 10 minutes.Porous alumina formwork immersion with above-mentioned sensitization under 30 ℃ contains silver nitrate 5g/L, and activation made active porous alumina formwork in 10 minutes in the solution of ammoniacal liquor 18ml/L (mass fraction 37%).With sulfur acid nickel 240g/L, nickel chloride 40g/L, the solution of boric acid 50g/L make anode as electrolyte with the nickel plate, in 40 ℃ at 100mA/cm
2Direct current under cold galvanising nickel is deposited on the active porous alumina formwork.The above-mentioned alumina formwork that deposits nickel is cleaned up with distilled water, immerse then in 2% the potassium hydroxide solution and dissolve template,, can obtain the metal nano nickel tube of diameter in the 15-150 nanometer with the precipitation cleaning-drying that obtains.
Embodiment 3:
With purity is that high-purity aluminium sheet of 99.99% is an anode, and the titanium net is a negative electrode, under 40 volts of direct currents, 25 ℃ in 3% phosphoric acid acid solution, the room temperature electrolysis obtained porous alumina formwork in 0.5 hour.To contain stannous chloride 12g/L, the solution of hydrochloric acid 1mol/L is activating solution, the porous alumina formwork that makes is soaked under 30 ℃ and carries out sensitization in 3 minutes.Porous alumina formwork immersion with above-mentioned sensitization under 20 ℃ contains palladium bichloride 0.5g/L, in the solution of hydrochloric acid 0.5mol/L, activates 2 minutes and makes active porous alumina formwork.With sulfur acid nickel 240g/L, the solution of boric acid 40g/L is made anode as electrolyte with nickel screen, in 60 ℃ at 40mA/cm
2Direct current under cold galvanising nickel is deposited on the active porous alumina formwork.The above-mentioned alumina formwork that deposits nickel is cleaned up with distilled water, immerse then in 5% the sodium hydroxide solution and dissolve template,, can obtain the metal nano nickel tube of diameter in the 15-150 nanometer with the precipitation cleaning-drying that obtains.
Embodiment 4:
With purity is that high-purity aluminium sheet of 99.99% is an anode, and the titanium net is a negative electrode, under 40 volts of direct currents, 20 ℃ in 3% oxalic acid acid solution, the room temperature electrolysis obtained porous alumina formwork in 2.5 hours.To contain stannic chloride 28g/L, natrium citricum 35g/L solution is activating solution, the porous alumina formwork that makes is soaked under 30 ℃ and carries out sensitization in 3 minutes.Porous alumina formwork immersion with above-mentioned sensitization under 20 ℃ contains palladium bichloride 0.5g/L, in the solution of hydrochloric acid 0.5mol/L, activates 8 minutes and makes active porous alumina formwork.With sulfur acid nickel 240g/L, the solution of boric acid 40g/L is made anode as electrolyte with nickel screen, in 60 ℃ at 40mA/cm
2Direct current under cold galvanising nickel is deposited on the active porous alumina formwork.The above-mentioned alumina formwork that deposits nickel is cleaned up with distilled water, immerse then in 5% the sodium hydroxide solution and dissolve template,, can obtain the metal nano nickel tube of diameter in the 15-150 nanometer with the precipitation cleaning-drying that obtains.
Embodiment 5:
With purity is that high-purity aluminium sheet of 99.99% is an anode, and carbon-point is a negative electrode, under 40 volts of direct currents, 20 ℃ in 3% oxalic acid acid solution, the room temperature electrolysis obtained porous alumina formwork in 2.5 hours.To contain stannic chloride 45g/L, potassium pyrophosphate 130g/L solution is activating solution, the porous alumina formwork that makes is soaked under 30 ℃ and carries out sensitization in 5 minutes.Porous alumina formwork immersion with above-mentioned sensitization under 20 ℃ contains palladium bichloride 0.5g/L, and hydrochloric acid 1.5mol/L in the solution of stannous chloride 30g/L, activates 5 minutes and makes active porous alumina formwork.With sulfur acid nickel 200g/L, nickel chloride 30g/L, the solution of boric acid 50g/L is made anode as electrolyte with nickel screen, in 60 ℃ at 10mA/cm
2Direct current under cold galvanising nickel is deposited on the active porous alumina formwork.The above-mentioned alumina formwork that deposits nickel is cleaned up with distilled water, immerse then in 5% the sodium hydroxide solution and dissolve template,, can obtain the metal nano nickel tube of diameter in the 15-150 nanometer with the precipitation cleaning-drying that obtains.
Embodiment 6:
With purity is that high-purity aluminium sheet of 99.99% is an anode, and the titanium net is a negative electrode, under 40 volts of direct currents, 20 ℃ in 3% oxalic acid acid solution, the room temperature electrolysis obtained porous alumina formwork in 2.5 hours.To contain stannic chloride 45g/L, potassium pyrophosphate 130g/L solution is activating solution, the porous alumina formwork that makes is soaked under 30 ℃ and carries out sensitization in 3 minutes.Porous alumina formwork immersion with above-mentioned sensitization under 20 ℃ contains in the solution of silver nitrate 2g/L, activates 6 minutes and makes active porous alumina formwork.With sulfur acid nickel 40g/L, nickel sulfamic acid 50g/L, the solution of boric acid 30g/L is made anode as electrolyte with nickel screen, in 40 ℃ at 8mA/cm
2Direct current under cold galvanising nickel is deposited on the active porous alumina formwork.The above-mentioned alumina formwork that deposits nickel is cleaned up with distilled water, immerse then in 5% the sodium hydroxide solution and dissolve template,, can obtain the metal nano nickel tube of diameter in the 15-150 nanometer with the precipitation cleaning-drying that obtains.
The method that the present invention prepares open and being used to of proposing metal nano nickel tube is related process extremely, and those skilled in the art can be by using for reference this paper content, and the appropriate change raw material is formed with link such as proportioning and realized.Product of the present invention and method are described by preferred embodiment, person skilled obviously can be in not breaking away from content of the present invention, spirit and scope to method as herein described with product is changed or suitably change and combination, realize the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (10)
1. metal nano nickel tube, the external diameter that it is characterized in that nano nickel tube is the 15-150 nanometer.
2. the preparation method of metal nano nickel tube as claimed in claim 1, step is as follows:
Negative electrode when (1) adopting anodised aluminium foraminous die plate through sensitization and activation as electrochemical reaction; With the nickel material is the anode of electrochemical reaction; To contain nickel salt, the solution of boric acid is electroplate liquid;
(2) with in negative electrode and the anode immersion plating liquid, connect power supply, under the direct current effect on alumina formwork plated metal nickel; Template can obtain the powder metal nano nickel tube through the alkaline solution dissolving.
3. the preparation method of metal nano nickel tube as claimed in claim 2 is characterized in that described sensitization is that sensitized porous aluminium oxide is touched plate in acid stannous salt solution or tin-salt solution; Sensitization time is 0.5-10 minute, room temperature.
4. the preparation method of metal nano nickel tube as claimed in claim 2 is characterized in that described activation is that the activation Woelm Alumina is touched plate in silver salt or palladium salting liquid; Soak time is 0.5-10 minute, room temperature～50 ℃.
5. the preparation method of metal nano nickel tube as claimed in claim 3 is characterized in that described
The prescription of the inferior solution of tin of acid divalence is stannous chloride 10-30g/L, hydrochloric acid 0.1-2mol/L;
The prescription of tin-salt solution is stannic chloride 12-60g/L, pyrophosphoric acid 120-140g/L or natrium citricum 20-80g/L or sodium tartrate 20-80g/L or sodium ethylene diamine tetracetate 20-80g/L and this type of polycarboxylic acid or multi-hydroxy carboxy acid or multi-hydroxy multi-carboxy acid or their alkaline-earth metal salt equivalent concentration.
6. the preparation method of metal nano nickel tube as claimed in claim 4 is characterized in that described
The prescription of silver salt activating solution is: silver nitrate 0.5-5g/L, or silver nitrate 0.5-5g/L and add ammoniacal liquor to solution becomes and clarify;
The prescription of palladium salt activating solution is: palladium bichloride 0.2-5g/L, hydrochloric acid 0.1-2mol/L, or palladium bichloride 0.2-5g/L, hydrochloric acid 0.1-2mol/L, stannous chloride 30-50g/L.
7. the preparation method of metal nano nickel tube as claimed in claim 2, the nickel salt that it is characterized in that described electroplate liquid is a nickelous sulfate, nickel chloride, nickel sulfamic acid or their composition, nickel salt concentration are 40-300g/L; Boric acid concentration is 30-50g/L.
8. the preparation method of metal nano nickel tube as claimed in claim 2, it is characterized in that described Woelm Alumina touches plate and be: adopting high-purity aluminium sheet is anode, electrolyte is oxalic acid solution or the phosphoric acid solution of 2%-5% or the sulfuric acid solution of 2%-5% of 2%-5%, negative electrode is titanium net or carbon-point, anodic oxidation voltage 20-110 volt, oxidization time is 0.5-6 hour, and temperature is 5-25 ℃.
9. the preparation method of metal nano nickel tube as claimed in claim 2 is characterized in that described direct current effect is that electric current is 5-100mA/cm
2Direct current, the time is 0.5-10 minute, temperature is 40-60 ℃.
10. the preparation method of metal nano nickel tube as claimed in claim 2 is characterized in that described alkaline solution is NaOH or potassium hydroxide solution.
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