CN101733049A - Method for preparing core-shell structure composite material by Gamma-ray irradiation - Google Patents
Method for preparing core-shell structure composite material by Gamma-ray irradiation Download PDFInfo
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- CN101733049A CN101733049A CN200810137542A CN200810137542A CN101733049A CN 101733049 A CN101733049 A CN 101733049A CN 200810137542 A CN200810137542 A CN 200810137542A CN 200810137542 A CN200810137542 A CN 200810137542A CN 101733049 A CN101733049 A CN 101733049A
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Abstract
The invention relates to a method for preparing a core-shell structure composite material by Gamma-ray irradiation, relating to a preparation method of a core-shell structure composite material. The invention solves the defects of multiple steps, easy side product introduction and difficult scavenging of side products during the reduction of a reducing agent in preparing the core-shell structure composite material by using a traditional chemical plating method. The method comprises the steps of: firstly, purifying nano materials or micron materials, adding into a metal salt solution, then adding a free radical scavenger, adjusting pH value, and ultrasonically dispersing; and secondly, irradiating by using Gamma-rays, washing, centrifugally separating, and drying in vacuum. The method has mild reaction condition, simple operation, strong controllability, good repeatability, less content of purities of products, and stable quality of obtained products.
Description
Technical field
The present invention relates to a kind of preparation method of nucleocapsid structure composite.
Background technology
Nuclear shell structured nano-(or micron) composite is a kind of new material that has the important development prospect in the Materials Science and Engineering field, owing to have unique physicochemical property and excellent application performance, has caused people's extensive studies interest.
Yet the defective that existing electroless plating method prepares that the nucleocapsid structure composite exists that step is many, introduce accessory substance and can't remove easily in the reducing agent reduction process.
Summary of the invention
The objective of the invention is to prepare in order to solve existing electroless plating method that the nucleocapsid structure composite exists that step is many, introducing accessory substance and the defective that can't remove easily in the reducing agent reduction process; And provide a kind of gamma-ray irradiation to prepare the method for nuclear-shell structured nano-composite material.
The method that gamma-ray irradiation prepares the nucleocapsid structure composite among the present invention is finished by following step: one, nano material or micro materials (nuclear) are carried out purifying, join in the metal salt solution again, add free radical scavenger then, regulating the pH value is 8-12, ultrasonic dispersion 30～60min; Two, adopt gamma-ray irradiation again, irradiation dose is 1 * 10
3～1 * 10
5Gy, radiation dose rate are 1～1 * 10
3Gy/min, more successively with ammoniacal liquor, distilled water and ethanol washing, centrifugation then, vacuum drying 4-8h under 50～80 ℃ of conditions promptly obtains the nucleocapsid structure composite; Wherein the mass ratio of nano material or micro materials and metal ion is 10～1: 1 in the step 1.
The present invention can also be after step 2 be carried out vacuum drying, does under protection gas, 600～800 ℃ of conditions at inert gas again, and the 3～8h that is recrystallized obtains the nucleocapsid structure composite; Wherein said inert gas is nitrogen or argon gas.
The described nano material of step 1 is CNT, nano silicon carbide granulate or nano silicon carbide silica fibre; Described micro materials is micron order tiny balloon, micron order carbon black, micron order carbon fiber, micron order silicon-carbide particle or micron silicon carbide fibre; Metal salt solution is a kind of or wherein several mixing in Fe salting liquid, Co salting liquid, Ni salting liquid, Au salting liquid, Pt salting liquid, Ag salting liquid, Pd salting liquid, Cd salting liquid, Sn salting liquid, the Cu salting liquid; Free radical scavenger is isopropyl alcohol, ethanol, n-butanol, propyl alcohol, n-octyl alcohol or n-amyl alcohol.The gamma ray projector that gamma-ray irradiation adopts in the step 2 is
60Co,
137Cs or
192Ir.
The ionising radiation of the inventive method gamma-rays makes water generation ionization and excites, and generates free radical H and aqueous electron (e
Aq -) and the OH free radical etc.Remove oxidative free radicals such as OH by the alcohols free radical scavenger, and then the reproducibility of the hierarchy of control.This reduction system can be reduced into metal ion low valence metal ion and then be reduced into zero-valent metal.Nano material (or micro materials) outer surface forms certain " defect point " under the effect of radiation, these " defect points " become the active site of metal atomic cluster deposition.Metal atomic cluster newly-generated on the position of active site is in nano material (or micro materials) surface aggregation nucleation, grow into the nano particle of metal gradually by the self-catalysis of metal, be deposited on nano material (or micro materials) surface, finally form the nucleocapsid structure composite.
Compared with prior art, the present invention has following advantage.
1, mild condition is carried out in the present invention's reaction at normal temperatures and pressures.
2, method of the present invention is simple, and controllability is strong, favorable reproducibility, and the products obtained therefrom steady quality.
3, product purity height of the present invention; Free radical scavenger does not participate in reaction, and removes easily, has improved the purity of product.
4, adopt the iron-cobalt-nickel magnetic metal to make product by the inventive method and compare with nano material (or micro materials), magnetic property is greatly increased.
5, the nucleocapsid structure composite of the inventive method preparation has stable nucleocapsid structure, avoids the reunion between the particle.
6, the applied range of product of the present invention can be used for fields such as biology, pharmacy, medical treatment, Industrial Catalysis, chemical, aviation, military affairs.
Description of drawings
Fig. 1 is the EDS figure of the specific embodiment 32 products.Fig. 2 is the XRD figure of the specific embodiment 32 products, and (a) represents the XRD figure of CNT among the figure, (b) represents the XRD figure through the vacuum drying afterproduct, (c) XRD figure of the expression specific embodiment 32 products.Fig. 3 is the SEM figure of the specific embodiment 32 products, and 1 represents Ni among Fig. 3, and 2 represent CNT.Fig. 4 is the real part of permittivity and the test frequency graph of a relation of the specific embodiment 32 products.Fig. 5 is the dielectric constant imaginary part and the test frequency graph of a relation of the specific embodiment 32 products.Fig. 6 is the magnetic conductivity real part and the test frequency graph of a relation of the specific embodiment 32 products.Fig. 7 is the magnetic conductivity imaginary part and the test frequency graph of a relation of the specific embodiment 32 products.Fig. 8 is the dielectric loss factor and the test frequency graph of a relation of the specific embodiment 32 products.Fig. 9 is the magnetic loss factor and the test frequency graph of a relation of the specific embodiment 32 products.Figure 10 be the specific embodiment 32 products hysteresis curve figure.Wherein a represents CNT among Fig. 4-10, and b represents the product of the specific embodiment 32.Figure 11 is the EDX figure of the specific embodiment 30 three products.Figure 12 is the XRD figure of the specific embodiment 30 three products; A is the tiny balloon XRD figure among Figure 10, b be in the specific embodiment 33 product XRD figure.Figure 13 is the SEM figure of tiny balloon.Figure 14 is the SEM figure of product in the specific embodiment 33.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: gamma-ray irradiation prepares the method for nucleocapsid structure composite in the present embodiment, it is characterized in that the method that gamma-ray irradiation prepares the nucleocapsid structure composite finished by following step: one, nano material or micro materials are carried out purifying, join in the metal salt solution again, add free radical scavenger then, regulating the pH value is 10, ultrasonic dispersion 30～60min; Two, adopt again
60Co is the gamma-ray irradiation of irradiation bomb, and irradiation dose is 1 * 10
3～1 * 10
5Gy, radiation dose rate are 1～1 * 10
3Gy/min, more successively with ammoniacal liquor, distilled water and ethanol washing, centrifugation then, vacuum drying 2h under 50～80 ℃ of conditions promptly obtains nuclear shell structured nano-/micron composite; Wherein the mass ratio of nano material or micro materials and metal ion is 10～1: 1 in the step 1.
Every liter of metal salt solution adds 1～10 mole of free radical scavenger in the present embodiment step 1.
The nucleocapsid structure composite of present embodiment preparation has stable nucleocapsid structure, avoids the reunion between the particle.
The specific embodiment two: the difference of the present embodiment and the specific embodiment one is: after step 2 is carried out vacuum drying, do under protection gas, 600～800 ℃ of conditions in inert gas, 3～8h is recrystallized again; Obtain nuclear shell structured nano-/micron composite.Other reactions steps and parameter are identical with the specific embodiment one.
Inert gas described in the present embodiment is nitrogen or argon gas.
The specific embodiment three: what present embodiment and the specific embodiment two were different is: do under protection gas, 650～750 ℃ of conditions in inert gas, 5～7h is recrystallized.
The specific embodiment four: what present embodiment and the specific embodiment two were different is: do under protection gas, the 700 ℃ of conditions in inert gas, 6h is recrystallized.
The specific embodiment five: what present embodiment and the specific embodiment two were different is: inert gas is a nitrogen.Other reactions steps and parameter are identical with the specific embodiment two.
The specific embodiment six: what present embodiment was different with the specific embodiment one or two is: the described nano material of step 1 is CNT, nano silicon carbide granulate or nano silicon carbide silica fibre.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment seven: what present embodiment and the specific embodiment six were different is: CNT is multi-walled carbon nano-tubes or SWCN.Other is identical with the specific embodiment three.
The specific embodiment eight: what present embodiment and the specific embodiment six were different is: the external diameter of CNT is 40～60nm.Other is identical with the specific embodiment six.
The specific embodiment nine: what present embodiment and the specific embodiment six were different is: the external diameter of CNT is 20～30nm.Other is identical with the specific embodiment six.
The specific embodiment ten: what present embodiment was different with the specific embodiment one or two is: the described micro materials of step 1 is micron order tiny balloon, micron order carbon black, micron order carbon fiber, micron order silicon-carbide particle or micron silicon carbide fibre.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 11: what present embodiment and the specific embodiment ten were different is: the external diameter of micron order tiny balloon is 0.5～25 μ m.Other is identical with the specific embodiment ten.
The specific embodiment 12: the present embodiment specific embodiment one or two different is: the concentration of metal salt solution is 0.01～2.0mol/L in the step 1.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 13: the present embodiment specific embodiment one or two different is: the concentration of metal salt solution is 0.05mol/L in the step 1.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 14: the present embodiment specific embodiment one or two different is: the concentration of metal salt solution is 1.0mol/L in the step 1.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 15: what present embodiment and the specific embodiment one were different is: metal salt solution is a kind of or wherein several mixing in Fe salting liquid, Co salting liquid, Ni salting liquid, Au salting liquid, Pt salting liquid, Ag salting liquid, Pd salting liquid, Cd salting liquid, Sn salting liquid, the Cu salting liquid in the step 1.Other reactions steps and parameter are identical with the specific embodiment one.
When the metal salt solution of present embodiment is mixture, press between various metal salt solutions arbitrarily than mixing.
The specific embodiment 16: what present embodiment and the specific embodiment 15 were different is: Fe salt is ferric trichloride, ferric sulfate, ferric nitrate, frerrous chloride or carbonyl iron.Other is identical with the specific embodiment 15.
The specific embodiment 17: what present embodiment and the specific embodiment 15 were different is: Co salt is cobalt chloride, cobalt oxalate, cobaltous sulfate or cobalt nitrate.Other is identical with the specific embodiment 15.
The specific embodiment 18: what present embodiment and the specific embodiment 15 were different is: Ni salt is nickel acetate, nickelous sulfate or nickel chloride.Other is identical with the specific embodiment 15.
The specific embodiment 19: what present embodiment and the specific embodiment 15 were different is: Au salt is chlorauride or gold chloride.Other is identical with the specific embodiment 15.
The specific embodiment 20: what present embodiment and the specific embodiment 15 were different is: Pt salt is chloroplatinic acid or platinum nitrate.Other is identical with the specific embodiment 15.
The specific embodiment 21: what present embodiment and the specific embodiment 15 were different is: Ag salt is silver nitrate.Other is identical with the specific embodiment 15.
The specific embodiment 22: what present embodiment and the specific embodiment 15 were different is: Pd salt is palladium bichloride.Other is identical with the specific embodiment 15.
The specific embodiment 23: what present embodiment and the specific embodiment 15 were different is: Cd salt is cadmium sulfate solution.Other is identical with the specific embodiment 15.
The specific embodiment 24: what present embodiment and the specific embodiment 15 were different is: Sn salt is stannic chloride.Other is identical with the specific embodiment 15.
The specific embodiment 25: what present embodiment and the specific embodiment 15 were different is: Cu salt is copper sulphate, copper chloride or copper nitrate.Other is identical with the specific embodiment 15.
The specific embodiment 26: what present embodiment was different with the specific embodiment one or two is: the free radical scavenger in the step 1 is isopropyl alcohol, ethanol, n-butanol, propyl alcohol, n-octyl alcohol or n-amyl alcohol.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 27: what present embodiment was different with the specific embodiment one or two is: the gamma ray projector that gamma-ray irradiation adopts in the step 2 is
60Co,
137Cs or
192Ir.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 28: what present embodiment was different with the specific embodiment one or two is: irradiation dose is 1.5 * 10 in the step 2
4～4 * 10
4Gy.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 29: what present embodiment was different with the specific embodiment one or two is: irradiation dose is 2 * 10 in the step 2
4Gy.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 30: what present embodiment was different with the specific embodiment one or two is: radiation dose rate is 50～200Gy/min in the step 2.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 31: what present embodiment was different with the specific embodiment one or two is: radiation dose rate is 80Gy/min in the step 2.Other reactions steps and parameter are identical with the specific embodiment one or two.
The specific embodiment 32: gamma-ray irradiation prepares that the method for nucleocapsid structure composite finished by following reaction in the present embodiment: one, CNT is carried out purifying, add to go into then in the nickel acetate aqueous solution (molar concentration 0.05mol/L), add isopropyl alcohol then, with mass concentration is that to regulate the pH value be 10 for 25% ammoniacal liquor, add ultrasonic dispersion 30min again, isopropyl alcohol molar concentration 1M; Two, adopt again
60Co is the gamma-ray irradiation of irradiation bomb, and irradiation dose is 2 * 10
4Gy, radiation dose rate are 80Gy/min, centrifugation then, and more successively with ammoniacal liquor, water and ethanol washing, vacuum drying 6h under 50 ℃ of conditions does under protection gas, the 600 ℃ of conditions at nitrogen, and the 8h that is recrystallized promptly obtains the nucleocapsid structure composite.
Present embodiment is made product test, see Fig. 1-3.
By Fig. 1,2 and 3 as seen, in carbon nano tube surface the nickel deposition is arranged.
Curve a, the b of comparison diagram 2, c are as can be known, metallic nickel is deposited on carbon nano tube surface, but the peak type of curve b is very not sharp-pointed, the deposition form that shows nickel mainly is a unformed shape, degree of crystallinity is bad, but behind the recrystallization, and 2 θ are that 44.347 ℃, 51.673 ℃, 76.095 ℃ diffraction maximum is corresponding to (111), (200), (220) crystal face of nickel, three characteristic peaks become fairly obvious, and the degree of crystallinity of nickel improves greatly.
Dielectric constant and magnetic conductivity to present embodiment are tested, and test result is seen Fig. 4-9.As shown in Figure 4, compare with CNT, the real part of permittivity of present embodiment product obviously reduces at 2-10GHz, and be improved to some extent at 10-18GHz (referring to Fig. 4).As shown in Figure 5, compare with CNT, the dielectric constant imaginary part of present embodiment product all has significantly in whole test frequency and reduces.As shown in Figure 6, compare with CNT, the magnetic conductivity real part of present embodiment product is the whole trend that descends and afterwards increase earlier that is in 2～18GHz frequency range, consistent substantially with CNT, but obviously greater than the magnetic conductance real part of CNT, reducing to a certain degree arranged and compare CNT in 12～18GHz frequency range in 2～18GHz frequency range.And the magnetic conductance imaginary part that present embodiment makes product in the test frequency range lifting trend and the also basically identical (referring to Fig. 7) of CNT, different is slightly descends in 2～5GHz frequency range magnetic conductivity imaginary part, and is greatly increased at the magnetic conductivity that 5～18GHz frequency range present embodiment makes product.By the hysteresis curve map analysis of Figure 10 present embodiment product, the magnetic property of material is greatly increased.
The specific embodiment 33: what present embodiment and the specific embodiment 32 were different is: what adopt in the step 1 is the cenosphere place of carbon nanotubes.Other reactions steps and parameter are identical with the specific embodiment 32.
By Figure 11,12 and 14 as seen, at the cenosphere surface deposition nickel is arranged.
Claims (10)
1. gamma-ray irradiation prepares the method for nucleocapsid structure composite, it is characterized in that the method that gamma-ray irradiation prepares the nucleocapsid structure composite finished by following step: one, nano material or micro materials are carried out purifying, join in the metal salt solution again, add free radical scavenger then, regulating the pH value is 8～12, ultrasonic dispersion 30～60min; Two, adopt gamma-ray irradiation again, irradiation dose is 1 * 10
3～1 * 10
5Gy, radiation dose rate are 1～1 * 10
3Gy/min, more successively with ammoniacal liquor, distilled water and ethanol washing, centrifugation then, vacuum drying 4～8h under 50～80 ℃ of conditions promptly obtains the nucleocapsid structure composite; Wherein the mass ratio of nano material or micro materials and metal ion is 10～1: 1 in the step 1.
2. gamma-ray irradiation according to claim 1 prepares the method for nucleocapsid structure composite, it is characterized in that step 2 is carried out vacuum drying after, do under protection gas, 600～800 ℃ of conditions at inert gas again, 3～8h is recrystallized.
3. gamma-ray irradiation according to claim 1 and 2 prepares the method for nucleocapsid structure composite, it is characterized in that the described nano material of step 1 is CNT, nano silicon carbide granulate or nano silicon carbide silica fibre.
4. gamma-ray irradiation according to claim 1 and 2 prepares the method for nucleocapsid structure composite, it is characterized in that the gamma ray projector that gamma-ray irradiation adopts in the step 2 is
60Co,
137Cs or
192Ir.
5. gamma-ray irradiation according to claim 1 and 2 prepares the method for nucleocapsid structure composite, it is characterized in that the described micro materials of step 1 is micron order tiny balloon, micron order carbon black, micron order carbon fiber, micron order silicon-carbide particle or micron silicon carbide fibre.
6. gamma-ray irradiation according to claim 1 and 2 prepares the method for nucleocapsid structure composite, it is characterized in that metal salt solution is a kind of or wherein several mixing in Fe salting liquid, Co salting liquid, Ni salting liquid, Au salting liquid, Pt salting liquid, Ag salting liquid, Pd salting liquid, Cd salting liquid, Sn salting liquid, the Cu salting liquid.
7. gamma-ray irradiation according to claim 6 prepares the method for nucleocapsid structure composite, it is characterized in that Ni salt is nickel acetate, nickelous sulfate or nickel chloride.
8. gamma-ray irradiation according to claim 1 and 2 prepares the method for nucleocapsid structure composite, it is characterized in that the free radical scavenger in the step 1 is isopropyl alcohol, ethanol, n-butanol, propyl alcohol, n-octyl alcohol or n-amyl alcohol.
9. gamma-ray irradiation according to claim 1 and 2 prepares the method for nucleocapsid structure composite, it is characterized in that irradiation dose is 1.5 * 10 in the step 2
4～4 * 10
4Gy, radiation dose rate are 50～200Gy/min.
10. gamma-ray irradiation according to claim 1 and 2 prepares the method for nucleocapsid structure composite, it is characterized in that irradiation dose is 2 * 10 in the step 2
4Gy, radiation dose rate are 80Gy/min.
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