CN104927761A - Preparation method of SiC@C core-shell structured nanowires - Google Patents
Preparation method of SiC@C core-shell structured nanowires Download PDFInfo
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- CN104927761A CN104927761A CN201510245661.5A CN201510245661A CN104927761A CN 104927761 A CN104927761 A CN 104927761A CN 201510245661 A CN201510245661 A CN 201510245661A CN 104927761 A CN104927761 A CN 104927761A
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Abstract
The invention discloses a preparation method of SiC@C core-shell structured nanowires, and relates to a preparation method of core-shell structured nanowires. The invention aims at solving a problem of low frequency dispersion property of existing SiC. The method comprises the following steps: 1, a mixture is prepared by mixing; 2, a reactant is obtained through a reaction; 3, separation and drying are carried out, such that solid powder is obtained; and 4, a high-temperature carbonization treatment is carried out, such that the SiC@C core-shell structured nanowires are obtained. The method has the following advantages: 1, the entire process is simple; operation is convenient; equipment is simple; cost is low; and pollution is prevented; 2, impurity introduction and structural defect problems are avoided; the prepared SiC@C core-shell structured nanowires have smooth shell surfaces and compact and uniform coatings; 3, the adopted carbon source raw materials is cheap and is easy to obtain; and the thickness of the coating shell can be effectively controlled through regulating the concentration of the reaction liquid; and 4, the product has good wave absorption performance. The method is mainly used for preparing the SiC@C core-shell structured nanowires.
Description
Technical field
The present invention relates to a kind of preparation method of nuclear shell structure nano line.
Background technology
In modernized war, absorbing material is applied in the positions such as the main wing of air fighter, the vertical fin wing, the horizontal tail wing and covering, the hertzian wave that acquisition radar is launched can be consumed by the mode of energy transformation and scattering, effectively decrease the probability arrived by radar detection, improve the handiness of viability afield and penetration ability and operation, become the focus of each military power of world research.Except military field, in daily life, electromagnetic radiation pollution source is ubiquitous especially, often can touch the product with radiation, as household appliances, mobile phone, computer, wireless network etc. can produce the hertzian wave of different frequency and energy.At present, Contamination of Electromagnetic Wave has been listed in the fourth-largest public hazards of the mankind, it is a kind of novel environmental pollution, there are some researches show, electromagnetic radiation has impact in various degree to the central nervous system of human body, immunity system, cardiovascular systems, reproductive system and genetic system, and the serious normal cell that also can make launches canceration.Therefore the research carrying out absorbing material has important and far-reaching meaning at military and civil area.
Si-C covalent linkage in SiC has higher intensity, have high temperature resistant, corrosion-resistant, high rigidity, the features such as good mechanical property, and there is wider energy gap, high electronic mobility, little specific inductivity, the performance that high carrier saturation drift velocity etc. are excellent, become high frequency, superpower, less energy-consumption, high temperature resistant, the ideal materials such as radio-radar absorber, especially in suction ripple field, SiC is a kind of dielectric type absorbing material, and there is lower density, high stability etc. are widely used in space industry, nano-photon, the preparation of opto-electronic device, field-electron emission cathode material, reinforced composite, photochemical catalysis, there is good application prospect in many fields such as sensing and Chu Qing, in the research of numerous monodimension nanometer material, the synthesis of One, Dimensional Semiconductor Nano Materials and study on the modification obtain to be paid close attention to widely.
Inhale ripple field by the SiC material of modification at high temperature and have larger researching value, and existing more ripe relevant technology of preparing, but the problem that SiC Dispersion is low.
Summary of the invention
The object of the invention is to solve existing SiC and there is the low problem of Dispersion, and a kind of preparation method of SiCC nuclear shell structure nano line is provided.
A preparation method for SiCC nuclear shell structure nano line, specifically completes according to the following steps:
One, mix: utilize deionized water or ethanol that cats product is configured to the cationic surfactant solution that concentration is 0.01mol/L ~ 0.05mol/L by cats product, be that cationic surfactant solution and the ammoniacal liquor of 0.01mol/L ~ 0.05mol/L adds solvent by concentration, and carry out ultrasonic disperse, obtain mixture; Concentration described in step one is the cationic surfactant solution of 0.01mol/L ~ 0.05mol/L and the volume ratio of solvent is 1:(150 ~ 300); Concentration described in step one is the cationic surfactant solution of 0.01mol/L ~ 0.05mol/L and the volume ratio of ammoniacal liquor is 1:(0.5 ~ 3);
Two, react: SiC nanowire is added in mixture, and ultrasonic disperse 1h ~ 3h, obtain containing SiC nanowire mixed system, add Resorcinol to containing in SiC nanowire mixed system, then magnetic agitation 0.5h ~ 3h, then adds formaldehyde, and magnetic agitation 15h ~ 24h, obtain reactant; The quality of the SiC nanowire described in step 2 and the volume ratio of mixture are (0.03 ~ 0.6) g:30mL; The mass ratio of the SiC nanowire described in step 2 and Resorcinol is 1:(0.5 ~ 3); The mol ratio of the formaldehyde described in step 2 and Resorcinol is 1:(1 ~ 3);
Three, be separated: carry out centrifugation to reactant, the solid obtained first adopts deionized water to wash, and washs 3 ~ 5 times, then adopts ethanol to wash, and wash 3 ~ 5 times, the solid after washing carries out drying treatment, obtains pressed powder;
Four, high temperature cabonization process: carry out high temperature cabonization process to pressed powder, namely obtains SiCC nuclear shell structure nano line.
Advantage of the present invention:
One, whole technique is simple, easy to operate, and use equipment simple, cost is low, can not pollute;
Two, method provided by the invention avoids introducing and the textural defect problem of impurity, and the SiCC nuclear shell structure nano line case surface of preparation is smooth, and coating layer densification is homogeneous;
Three, carbon source raw material used is cheap and easy to get, can by the thickness regulating reaction solution concentration effectively to control coated shell;
Four, the SiCC nuclear shell structure nano line that prepared by the present invention is dielectric loss type absorbing material, has good absorbing property.
Accompanying drawing explanation
Fig. 1 is the TEM figure that test one obtains SiCC nuclear shell structure nano line;
Fig. 2 is that the amplification TEM that test one obtains SiCC nuclear shell structure nano line schemes;
Fig. 3 is the infrared spectrum that test one step 3 obtains pressed powder;
Fig. 4 is the XRD energy spectrogram that test one obtains SiCC nuclear shell structure nano line;
Fig. 5 is 2 ~ 18GHz absorbing property analysis chart that test one obtains SiCC nuclear shell structure nano line.
Embodiment
Embodiment one: present embodiment is a kind of preparation method of SiCC nuclear shell structure nano line, specifically completes according to the following steps:
One, mix: utilize deionized water or ethanol that cats product is configured to the cationic surfactant solution that concentration is 0.01mol/L ~ 0.05mol/L by cats product, be that cationic surfactant solution and the ammoniacal liquor of 0.01mol/L ~ 0.05mol/L adds solvent by concentration, and carry out ultrasonic disperse, obtain mixture; Concentration described in step one is the cationic surfactant solution of 0.01mol/L ~ 0.05mol/L and the volume ratio of solvent is 1:(150 ~ 300); Concentration described in step one is the cationic surfactant solution of 0.01mol/L ~ 0.05mol/L and the volume ratio of ammoniacal liquor is 1:(0.5 ~ 3);
Two, react: SiC nanowire is added in mixture, and ultrasonic disperse 1h ~ 3h, obtain containing SiC nanowire mixed system, add Resorcinol to containing in SiC nanowire mixed system, then magnetic agitation 0.5h ~ 3h, then adds formaldehyde, and magnetic agitation 15h ~ 24h, obtain reactant; The quality of the SiC nanowire described in step 2 and the volume ratio of mixture are (0.03 ~ 0.6) g:30mL; The mass ratio of the SiC nanowire described in step 2 and Resorcinol is 1:(0.5 ~ 3); The mol ratio of the formaldehyde described in step 2 and Resorcinol is 1:(1 ~ 3);
Three, be separated: carry out centrifugation to reactant, the solid obtained first adopts deionized water to wash, and washs 3 ~ 5 times, then adopts ethanol to wash, and wash 3 ~ 5 times, the solid after washing carries out drying treatment, obtains pressed powder;
Four, high temperature cabonization process: carry out high temperature cabonization process to pressed powder, namely obtains SiCC nuclear shell structure nano line.
Carbon is a kind of good conductor, and the Dispersion of itself is fine, and density is low, good stability, is also a kind of dielectric loss material, and therefore present embodiment selects in-stiu coating carbon in SiC nanowire, effectively can improve the low shortcoming of SiC Dispersion.
The whole technique of present embodiment is simple, easy to operate, and use equipment simple, cost is low, can not pollute;
Present embodiment avoids introducing and the textural defect problem of impurity, and the SiCC case surface of preparation is smooth, and coating layer densification is homogeneous;
Carbon source raw material used is cheap and easy to get, can by the thickness regulating reaction solution concentration effectively to control coated shell;
SiCC nuclear shell structure nano line prepared by present embodiment is dielectric loss type absorbing material, has good absorbing property.
Embodiment two: the difference of present embodiment and embodiment one is: the cats product described in step one is cetyl trimethylammonium bromide (CTAB).Other are identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two difference is: the solvent described in step one is deionized water, dehydrated alcohol or aqueous ethanolic solution.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: the massfraction of ammoniacal liquor described in step one is 25%.Other are identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four difference is: the centrifugation detailed process described in step 3 is as follows: carry out centrifugation to reactant under rotating speed is 7000r/min ~ 12000r/min, remove supernatant liquid, obtain solid.Other are identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five difference is: the deionized water wash detailed process described in step 3 is as follows: first by solid dispersal in deionized water, then centrifugation under rotating speed is 7000r/min ~ 12000r/min, namely completes deionized water wash.Other are identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six difference is: the deionized water wash detailed process described in step 3 is as follows: by the solid dispersal that obtains after deionized water wash in ethanol, then centrifugation under rotating speed is 7000r/min ~ 12000r/min, namely completes washing with alcohol.Other are identical with embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven difference is: the drying treatment detailed process described in step 3 is as follows: to the solid forced air drying 8h after washing at temperature is 80 DEG C, obtain pressed powder.Other are identical with embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight difference is: the high temperature cabonization process detailed process described in step 4 is as follows: carry out vacuum carburization process 4h ~ 10h to pressed powder at temperature is 500 ~ 700 DEG C, namely complete high temperature cabonization process, obtain SiCC nuclear shell structure nano line.Other are identical with embodiment one to eight.
Embodiment ten: present embodiment and embodiment nine difference are: the high temperature cabonization process detailed process described in step 4 is as follows: carry out carbonizing treatment 4h ~ 10h to pressed powder at temperature is 500 ~ 700 DEG C He under inert gas atmosphere, namely complete high temperature cabonization process, obtain SiCC nuclear shell structure nano line; Described rare gas element is N
2gas or Ar gas.Other are identical with embodiment nine.
Adopt following verification experimental verification effect of the present invention
Test one: a kind of preparation method of SiCC nuclear shell structure nano line, specifically completes according to the following steps:
One, mix: utilize deionized water or ethanol that cetyl trimethylammonium bromide (CTAB) is configured to the cationic surfactant solution that concentration is 0.01mol/L, to be the cationic surfactant solution of 0.01mol/L and 0.1mL massfraction by 0.1mL concentration be 25% ammoniacal liquor add in 30mL deionized water, and carry out ultrasonic disperse, obtain mixture;
Two, react: 0.1g SiC nanowire is added in the mixture that step one obtains, and ultrasonic disperse 2h, obtain containing SiC nanowire mixed system, 0.08g Resorcinol is added to containing in SiC nanowire mixed system, then magnetic agitation 0.5h, then 0.16mL formaldehyde is added, and magnetic agitation 15h, obtain reactant;
Three, be separated: carry out centrifugation to reactant, the solid obtained first adopts deionized water to wash, and washs 3 times, then adopts ethanol to wash, and wash 3 times, the solid after washing carries out drying treatment, obtains pressed powder;
Four, high temperature cabonization process: carry out vacuum carburization process 6h to pressed powder at temperature is 700 DEG C, namely completes high temperature cabonization process, obtains SiCC nuclear shell structure nano line.
Centrifugation detailed process described in step 3 is as follows: under rotating speed is 12000r/min, carry out centrifugation to reactant, removes supernatant liquid, obtains solid.
Deionized water wash detailed process described in step 3 is as follows: first by solid dispersal in deionized water, then centrifugation under rotating speed is 12000r/min, namely completes deionized water wash.
Deionized water wash detailed process described in step 3 is as follows: by the solid dispersal that obtains after deionized water wash in ethanol, then centrifugation under rotating speed is 12000r/min, namely completes washing with alcohol.
Drying treatment detailed process described in step 3 is as follows: to the solid forced air drying 8h after washing at temperature is 80 DEG C, obtain pressed powder.
Fig. 1 is the TEM figure that test one obtains SiCC nuclear shell structure nano line, Fig. 2 is that the amplification TEM that test one obtains SiCC nuclear shell structure nano line scheme, and as can be seen from the figure well, case surface is smooth, and coating layer densification is homogeneous for carbon covered effect.
Fig. 3 is the infrared spectrum that test one step 3 obtains pressed powder, as we can see from the figure at 1469cm
-1under there is absorption peak, illustrate that product has methylene radical (-CH
2-) existence of group, 1615cm
-1the absorption peak of corresponding is phenyl ring, these two absorption peaks can define RF chain and be coated in SiC nanowire.
Fig. 4 is the XRD energy spectrogram that test one obtains SiCC nuclear shell structure nano line, can find out that diffraction peak that XRD power spectrum occurs is all the main diffraction peak of SiC, be the bulge of steamed bun shape at about 20 °, do not observe the diffraction peak of crystalline state carbon, this illustrates that coated carbon exists in the mode of unformed shape.
Fig. 5 is 2 ~ 18GHz absorbing property analysis chart that test one obtains SiCC nuclear shell structure nano line, absorbing property analytic curve when A represents d=5mm in figure, absorbing property analytic curve when B represents d=4mm in figure, absorbing property analytic curve when C represents d=3mm in figure, when can find out that thickness is 5mm by figure, when frequency is 7.1GHz, minimum reflection loss can reach-20dB, and the frequency span of reflection loss below-5dB is 5.5GHz.
Test two: a kind of preparation method of SiCC nuclear shell structure nano line, specifically completes according to the following steps:
One, mix: utilize deionized water or ethanol that cetyl trimethylammonium bromide (CTAB) is configured to the cationic surfactant solution that concentration is 0.01mol/L, to be the cationic surfactant solution of 0.01mol/L and 0.1mL massfraction by 0.1mL concentration be 25% ammoniacal liquor add in 30mL deionized water, and carry out ultrasonic disperse, obtain mixture;
Two, react: 0.1g SiC nanowire is added in the mixture that step one obtains, and ultrasonic disperse 2h, obtain containing SiC nanowire mixed system, 0.08g Resorcinol is added to containing in SiC nanowire mixed system, then magnetic agitation 0.5h, then 0.16mL formaldehyde is added, and magnetic agitation 15h, obtain reactant;
Three, be separated: carry out centrifugation to reactant, the solid obtained first adopts deionized water to wash, and washs 3 times, then adopts ethanol to wash, and wash 3 times, the solid after washing carries out drying treatment, obtains pressed powder;
Four, high temperature cabonization process: in step 4 at temperature is 500 DEG C and N
2under gas atmosphere, carbonizing treatment 5h is carried out to pressed powder, namely complete high temperature cabonization process, obtain SiCC nuclear shell structure nano line.
Centrifugation detailed process described in step 3 is as follows: under rotating speed is 12000r/min, carry out centrifugation to reactant, removes supernatant liquid, obtains solid.
Deionized water wash detailed process described in step 3 is as follows: first by solid dispersal in deionized water, then centrifugation under rotating speed is 12000r/min, namely completes deionized water wash.
Deionized water wash detailed process described in step 3 is as follows: by the solid dispersal that obtains after deionized water wash in ethanol, then centrifugation under rotating speed is 12000r/min, namely completes washing with alcohol.
Drying treatment detailed process described in step 3 is as follows: to the solid forced air drying 8h after washing at temperature is 80 DEG C, obtain pressed powder.
Claims (10)
1. a preparation method for SiCC nuclear shell structure nano line, is characterized in that the preparation method of SiCC nuclear shell structure nano line completes according to the following steps:
One, mix: utilize deionized water or ethanol cats product to be configured to the cationic surfactant solution that concentration is 0.01mol/L ~ 0.05mol/L, be that cationic surfactant solution and the ammoniacal liquor of 0.01mol/L ~ 0.05mol/L adds solvent by concentration, and carry out ultrasonic disperse, obtain mixture; Concentration described in step one is the cationic surfactant solution of 0.01mol/L ~ 0.05mol/L and the volume ratio of solvent is 1:(150 ~ 300); Concentration described in step one is the cationic surfactant solution of 0.01mol/L ~ 0.05mol/L and the volume ratio of ammoniacal liquor is 1:(0.5 ~ 3);
Two, react: SiC nanowire is added in mixture, and ultrasonic disperse 1h ~ 3h, obtain containing SiC nanowire mixed system, add Resorcinol to containing in SiC nanowire mixed system, then magnetic agitation 0.5h ~ 3h, then adds formaldehyde, and magnetic agitation 15h ~ 24h, obtain reactant; The quality of the SiC nanowire described in step 2 and the volume ratio of mixture are (0.03 ~ 0.6) g:30mL; The mass ratio of the SiC nanowire described in step 2 and Resorcinol is 1:(0.5 ~ 3); The mol ratio of the formaldehyde described in step 2 and Resorcinol is 1:(1 ~ 3);
Three, be separated: carry out centrifugation to reactant, the solid obtained first adopts deionized water to wash, and washs 3 ~ 5 times, then adopts ethanol to wash, and wash 3 ~ 5 times, the solid after washing carries out drying treatment, obtains pressed powder;
Four, high temperature cabonization process: carry out high temperature cabonization process to pressed powder, namely obtains SiCC nuclear shell structure nano line.
2. the preparation method of a kind of SiCC nuclear shell structure nano line according to claim 1, is characterized in that the cats product described in step one is cetyl trimethylammonium bromide.
3. the preparation method of a kind of SiCC nuclear shell structure nano line according to claim 1, is characterized in that the solvent described in step one is deionized water, dehydrated alcohol or aqueous ethanolic solution.
4. the preparation method of a kind of SiCC nuclear shell structure nano line according to claim 1, is characterized in that the massfraction of ammoniacal liquor described in step one is 25%.
5. the preparation method of a kind of SiCC nuclear shell structure nano line according to claim 1, it is characterized in that the centrifugation detailed process described in step 3 is as follows: under rotating speed is 7000r/min ~ 12000r/min, centrifugation is carried out to reactant, remove supernatant liquid, obtain solid.
6. the preparation method of a kind of SiCC nuclear shell structure nano line according to claim 1, it is characterized in that the deionized water wash detailed process described in step 3 is as follows: first by solid dispersal in deionized water, then centrifugation under rotating speed is 7000r/min ~ 12000r/min, namely completes deionized water wash.
7. the preparation method of a kind of SiCC nuclear shell structure nano line according to claim 1, it is characterized in that the deionized water wash detailed process described in step 3 is as follows: by the solid dispersal that obtains after deionized water wash in ethanol, then centrifugation under rotating speed is 7000r/min ~ 12000r/min, namely completes washing with alcohol.
8. the preparation method of a kind of SiCC nuclear shell structure nano line according to claim 1, is characterized in that the drying treatment detailed process described in step 3 is as follows: to the solid forced air drying 8h after washing at temperature is 80 DEG C, obtain pressed powder.
9. the preparation method of a kind of SiCC nuclear shell structure nano line according to claim 1, it is characterized in that the high temperature cabonization process detailed process described in step 4 is as follows: at temperature is 500 ~ 700 DEG C, vacuum carburization process 4h ~ 10h is carried out to pressed powder, namely complete high temperature cabonization process, obtain SiCC nuclear shell structure nano line.
10. the preparation method of a kind of SiCC nuclear shell structure nano line according to claim 1, it is characterized in that the high temperature cabonization process detailed process described in step 4 is as follows: at temperature is 500 ~ 700 DEG C He under inert gas atmosphere, carbonizing treatment 4h ~ 10h is carried out to pressed powder, namely complete high temperature cabonization process, obtain SiCC nuclear shell structure nano line; Described rare gas element is N
2gas or Ar gas.
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| CN110368971A (en) * | 2019-08-09 | 2019-10-25 | 陕西科技大学 | A kind of solid waste microwave-assisted depolymerization SiC based composite catalyst and preparation method thereof |
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| CN110368971B (en) * | 2019-08-09 | 2022-01-28 | 陕西科技大学 | SiC-based composite catalyst for microwave-assisted depolymerization of solid waste and preparation method thereof |
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| CN111138206A (en) * | 2020-01-11 | 2020-05-12 | 西安交通大学 | Amorphous carbon modified SiC nanowire continuous three-dimensional network structure wave-absorbing foam and preparation method thereof |
| CN114195539A (en) * | 2021-12-29 | 2022-03-18 | 王云 | SiC/PyC nanowire reinforced Al2O3High-temperature-resistant wave-absorbing ceramic and preparation method thereof |
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