CN108410422B - Preparation method of silicon-containing wave-absorbing material - Google Patents
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Abstract
The invention relates to the field of wave-absorbing material preparation, in particular to a preparation method of a silicon-containing wave-absorbing material; adding 1-4 parts of metal chloride, 12-24 parts of ferric chloride, 4-8 parts of ferrous chloride and solid powder into 150 parts of 100-fold-doped water, preparing metal oxide magnetic powder by using a gel method under the protection of nitrogen, adding 180 parts of 100-fold-doped ethanol into a reaction kettle, heating to 40-45 ℃, sequentially adding 30-50 parts of water, 40-60 parts of ammonia water and 10-20 parts of ethyl orthosilicate under mechanical stirring, reacting for 10-15min under stirring, adding a metal oxide magnetic powder dispersion liquid, and reacting to obtain a silicon-containing wave absorbing material; the wave-absorbing material provided by the invention has a silicon dioxide shell layer, can resist the corrosion of a solvent and the environment, improves the stability of particles, and can effectively increase the anisotropy and improve the dielectric loss.
Description
Technical Field
The invention relates to the field of wave-absorbing material preparation, in particular to a preparation method of a silicon-containing wave-absorbing material.
Background
The wave-absorbing material can convert and consume electromagnetic energy or enable the electromagnetic wave to disappear or weaken and deflect a target due to interference, is a branch of electromagnetic shielding materials, and becomes an important component of stealth and protection technology. The method can be widely applied to the aspects of aerospace, military target radar stealth, microwave darkroom, electromagnetic compatibility, electronic devices, civil facility protection, electromagnetic radiation shielding and the like.
CN103834064B discloses a bacterial cellulose/ferrite composite wave-absorbing material and a preparation method thereof. Relates to a wave-absorbing material preparation technology. The method comprises the following steps: weighing iron salt, dissolving the iron salt in ethylene glycol, adding one or more of zinc salt, nickel salt, magnesium salt, copper salt and cobalt salt, adding bacterial cellulose, performing ultrasonic dispersion, adding anhydrous sodium acetate and a dispersing agent, mechanically stirring, putting the mixture into a reaction kettle after the powder is completely dissolved, naturally cooling to room temperature after the reaction is finished, washing with deionized water, and drying to obtain the composite wave-absorbing material with ferrites uniformly distributed in the bacterial cellulose three-dimensional network. The preparation process is green and environment-friendly, simple and feasible, convenient to operate and low in cost, and the obtained wave-absorbing material is strong in electromagnetic wave absorption, wide in absorption frequency band, good in mechanical property, ultrathin and ultralight.
CN103342982B discloses a hollow spherical ferroferric oxide/graphene composite wave-absorbing material, and relates to a wave-absorbing material. The invention aims to solve the problems that ferroferric oxide loaded by a ferroferric oxide/graphene composite wave-absorbing material prepared by the existing method is of a solid spherical structure, high in density and easy to generate aggregation of graphene and nano magnetic particles. A hollow spherical ferroferric oxide/graphene composite wave-absorbing material is prepared by taking graphene as a matrix and loading hollow spherical ferroferric oxide; the method comprises the following steps: firstly, uniformly mixing liquid state; secondly, in-situ nucleation growth. According to the invention, the preparation of the composite material is completed in one-step reaction, so that the pollution introduced into the final material is reduced, and meanwhile, the one-step method can also prevent the aggregation of graphene sheets. The invention is used for preparing the hollow spherical ferroferric oxide/graphene composite wave-absorbing material.
CN102977480B discloses a preparation method of a rubber substrate flexible wave-absorbing material, which relates to the field of civil wave-absorbing materials and comprises the following steps: A. mixing the filler and the rubber according to the proportion of 90: 10-91: 9, adding an organic solvent which accounts for 1.2-2% of the total mass of the filler and the rubber and is compatible with the rubber in the mixing process, mixing, and uniformly mixing the filler and the rubber powder; B. and (3) placing for a period of time after mixing is finished, volatilizing the organic solvent, and then calendering to prepare the wave-absorbing patch. The invention can obviously improve the filling concentration and realize the filling concentration to be more than 90 percent, thereby improving the performance of the material, and does not need complicated chemical process control or professional auxiliary equipment, and has convenient operation and lower cost.
Most wave-absorbing materials prepared by the invention and the prior art are metal oxides, and the requirements of processing and complex and diversified use environments are difficult to meet due to the poor corrosion resistance and acid resistance, so that the application of the wave-absorbing agent is greatly limited.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a silicon-containing wave-absorbing material.
A preparation method of a silicon-containing wave-absorbing material comprises the following synthetic technical scheme:
step 1
Adding 1-4 parts of metal chloride, 12-24 parts of ferric chloride, 4-8 parts of ferrous chloride and solid powder into 100-150 parts of water according to the mass fraction, stirring and heating to 70-85 ℃ under the protection of nitrogen; adding 45-60 parts of citric acid into a reaction kettle, stirring and dissolving, then adding alkali to adjust the pH value to be =7, keeping the temperature and stirring for 30min to ensure that gel is formed, continuously reacting at 80-90 ℃ for 5-8h, drying the gel in a drying oven at the temperature of 100-110 ℃, calcining for 2-6 h in a sintering furnace according to the programmed temperature, cooling along with the furnace, grinding and sieving to obtain metal oxide magnetic powder; dispersing the obtained metal oxide magnetic powder in 20-60 parts of distilled water and carrying out ultrasonic treatment for 10-30 min for later use;
step 2
Adding 100 parts of ethanol into a reaction kettle, heating to 40-55 ℃, sequentially adding 30-50 parts of water, 40-60 parts of ammonia water, 0.01-0.05 part of 1,1' -dibutyryl ferrocene, 10-20 parts of ethyl orthosilicate, 0.01-0.1 part of 2- (triisopropylsilyl) oxazole-5-formaldehyde and 0.5-2 parts of 6-anilino-1, 3, 5-triazine-2, 4-dithiol under mechanical stirring, reacting for 10-15min, adding a metal oxide magnetic powder dispersion liquid, reacting for 30-60min, centrifuging, filtering and drying to obtain the silicon-containing wave-absorbing material.
The metal chloride is nickel chloride or cobalt chloride or lithium chloride or zinc chloride.
The alkali for adjusting the pH value is ammonia water or ethylenediamine or triethylamine.
The particle size of the metal oxide magnetic powder is 300-400 meshes.
The temperature rising procedure is as follows: normal temperature is 500 ℃ below zero, and the temperature is 100 ℃/h; 500 ℃ and 800 ℃, 150 ℃/h; 800 ℃ and 1000 ℃ at 200 ℃/h.
The wave-absorbing material prepared by the method has a silicon dioxide shell layer, can resist the corrosion of a solvent and the environment, improves the stability of particles, can effectively increase the anisotropy and improves the dielectric loss; the silica is used as another important component of the microwave absorbing material, and the matrix material playing a role of bearing and bonding also determines the overall effect of the wave absorbing material.
Detailed Description
The invention is further illustrated by the following specific examples:
example 1
A preparation method of a silicon-containing wave-absorbing material comprises the following synthetic technical scheme:
step 1
Adding 4g of cobalt chloride, 24g of ferric chloride and 8g of ferrous chloride solid powder into 150g of water according to mass fraction, stirring and heating to 75 ℃ under the protection of nitrogen; adding 60g of citric acid into a reaction kettle, stirring and dissolving, then adding alkali to adjust the pH value to be =7, keeping the temperature and stirring for 30min to ensure that gel is formed, continuously reacting for 8h at 85-90 ℃, drying the gel in a drying oven at 105-110 ℃, calcining for 4 h in a sintering furnace according to the programmed temperature, cooling along with the furnace, grinding and sieving to obtain metal oxide magnetic powder; dispersing the obtained metal oxide magnetic powder in 60g of distilled water and carrying out ultrasonic treatment for 30min for later use;
step 2
Adding 100g of ethanol into a reaction kettle, heating to 45 ℃, sequentially adding 39g of water, 45g of ammonia water, 0.02g of 1,1' -dibutyryl ferrocene, 16g of ethyl orthosilicate, 0.031g of 2- (triisopropylsilyl) oxazole-5-formaldehyde and 1g of 6-anilino-1, 3, 5-triazine-2, 4-dithiol under mechanical stirring, reacting for 12min, adding a metal oxide magnetic powder dispersion, reacting for 40min, centrifuging, filtering and drying to obtain the silicon-containing wave absorbing material.
Sample number DC-1.
Example 2
A preparation method of a silicon-containing wave-absorbing material comprises the following synthetic technical scheme:
step 1
Adding 1g of nickel chloride, 12g of ferric chloride and 4g of ferrous chloride solid powder into 100g of water according to mass fraction, stirring and heating to 70 ℃ under the protection of nitrogen; adding 45g of citric acid into a reaction kettle, stirring and dissolving, then adding ammonia water to adjust the pH value to be =7, keeping the temperature and stirring for 30min to ensure that gel is formed, continuously reacting for 5h at 80-85 ℃, drying the gel in an oven at 105 ℃ of 100-85 ℃, calcining for 2 h in a sintering furnace according to the programmed temperature, cooling along with the furnace, grinding and sieving to obtain metal oxide magnetic powder; dispersing the obtained metal oxide magnetic powder in 20g of distilled water and carrying out ultrasonic treatment for 10min for standby;
step 2
Adding 100g of ethanol into a reaction kettle, heating to 40 ℃, sequentially adding 30g of water, 40g of ammonia water, 0.01g of 1,1' -dibutyryl ferrocene, 10g of ethyl orthosilicate, 0.01g of 2- (triisopropylsilicon) oxazole-5-formaldehyde and 0.5g of 6-anilino-1, 3, 5-triazine-2, 4-dithiol under mechanical stirring, reacting for 10min, adding a metal oxide magnetic powder dispersion, reacting for 30min, centrifuging, filtering and drying to obtain the silicon-containing wave absorbing material.
Sample No. DC-2.
Example 3
A preparation method of a silicon-containing wave-absorbing material comprises the following synthetic technical scheme:
step 1
Adding 2.5g of lithium chloride, 18g of ferric chloride and 6g of ferrous chloride into 125g of water according to mass fraction, stirring and heating to 85 ℃ under the protection of nitrogen; adding 54gg of citric acid into a reaction kettle, stirring and dissolving, then adding alkali to adjust the pH value to be =7, keeping the temperature and stirring for 30min to ensure that gel is formed, continuously reacting for 7h at 85-90 ℃, drying the gel in a drying oven at 105-110 ℃, calcining for 6 h in a sintering furnace according to the programmed temperature, cooling along with the furnace, grinding and sieving to obtain metal oxide magnetic powder; dispersing the obtained metal oxide magnetic powder in 40g of distilled water and carrying out ultrasonic treatment for 20 min for standby;
step 2
Adding 100 parts of ethanol into a reaction kettle, heating to 55 ℃, sequentially adding 50 parts of water, 60 parts of ammonia water, 0.05 part of 1,1' -dibutyryl ferrocene, 20 parts of ethyl orthosilicate, 0.1 part of 2- (triisopropylsilyl) oxazole-5-formaldehyde and 2 parts of 6-anilino-1, 3, 5-triazine-2, 4-dithiol under mechanical stirring, reacting for 15min, adding a metal oxide magnetic powder dispersion liquid, reacting for 60min, centrifuging, filtering and drying to obtain the silicon-containing wave absorbing material.
Sample No. DC-3.
Comparative example 1
The same procedure as in example 1 was repeated except that cobalt chloride was not added to obtain sample No. DC-4.
Comparative example 2
The same procedure as in example 1 was repeated except that ferric chloride was not added to obtain sample No. DC-5.
Comparative example 3
The procedure was as in example 1, sample No. DC-6, except that no silica coating was used.
Comparative example 4
The same procedure as in example 1 was repeated except that 1,1' -dibutyryl ferrocene was not added, and sample No. DC-7 was used.
Comparative example 5
The procedure of example 1 was repeated except that 2- (triisopropylsilyl) oxazole-5-carbaldehyde was not added, and the sample was designated as DC-8.
Comparative example 6
The procedure of example 1 was repeated except that 6-anilino-1, 3, 5-triazine-2, 4-dithiol was not added, and the sample was designated as DC-9.
Example 4
Acid resistance measurement of samples
The obtained wave-absorbing material is soaked in an ethanol solvent containing 0.01mol/L acetic acid, and then the electromagnetic parameters of the wave-absorbing material are measured.
Electromagnetic parameter determination
The prepared wave-absorbing material and paraffin are prepared into a coaxial ring according to the mass ratio of 7:3, and then the electromagnetic parameters are tested by a vector network analyzer to analyze the electromagnetic performance.
Table: comparison of dielectric constants at 10GHz for test samples made by different processes
| Numbering | Dielectric constant | Dielectric constant (acid bulb) |
| DC-1 | 31.25 | 30.34 |
| DC-2 | 32.54 | 31.64 |
| DC-3 | 31.89 | 31.52 |
| DC-4 | 24.15 | 23.61 |
| DC-5 | 26.51 | 21.64 |
| DC-6 | 31.95 | 17.32 |
| DC-7 | 28.45 | 25.64 |
| DC-8 | 27.58 | 24.55 |
| DC-9 | 25.85 | 23.26 |
Claims (4)
1. A preparation method of a silicon-containing wave-absorbing material is characterized in that the synthesis technical scheme is as follows:
step 1
Adding 1-4 parts of metal chloride, 12-24 parts of ferric chloride, 4-8 parts of ferrous chloride and solid powder into 100-150 parts of water according to the mass fraction, stirring and heating to 70-85 ℃ under the protection of nitrogen; adding 45-60 parts of citric acid into a reaction kettle, stirring and dissolving, then adding alkali to adjust the pH value to be =7, keeping the temperature and stirring for 30min to ensure that gel is formed, continuously reacting at 80-90 ℃ for 5-8h, drying the gel in an oven at the temperature of 100-110 ℃, calcining for 4-6 h in a sintering furnace according to the programmed temperature, cooling along with the furnace, grinding and sieving to obtain metal oxide magnetic powder; dispersing the obtained metal oxide magnetic powder in 20-60 parts of distilled water and carrying out ultrasonic treatment for 10-30 min for later use;
step 2
Adding 100 parts of ethanol into a reaction kettle, heating to 40-55 ℃, sequentially adding 30-50 parts of water, 40-60 parts of ammonia water, 0.01-0.05 part of 1,1' -dibutyryl ferrocene, 10-20 parts of ethyl orthosilicate, 0.01-0.1 part of 2- (triisopropylsilyl) oxazole-5-formaldehyde and 0.5-2 parts of 6-anilino-1, 3, 5-triazine-2, 4-dithiol under mechanical stirring, reacting for 10-15min, adding a metal oxide magnetic powder dispersion liquid, reacting for 30-60min, centrifuging, filtering and drying to obtain the silicon-containing wave-absorbing material;
the metal chloride is nickel chloride or cobalt chloride or lithium chloride or zinc chloride.
2. The method for preparing the silicon-containing wave-absorbing material according to claim 1, wherein the method comprises the following steps: the alkali for adjusting the pH value is ammonia water or ethylenediamine or triethylamine.
3. The method for preparing the silicon-containing wave-absorbing material according to claim 1, wherein the method comprises the following steps: the particle size of the metal oxide magnetic powder is 300-400 meshes.
4. The method for preparing the silicon-containing wave-absorbing material according to claim 1, wherein the method comprises the following steps: the temperature rising procedure is as follows: normal temperature is 500 ℃ below zero, and the temperature is 100 ℃/h; 500 ℃ and 800 ℃, 150 ℃/h; 800 ℃ and 1000 ℃ at 200 ℃/h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0782659A (en) * | 1993-09-08 | 1995-03-28 | Taiho Ind Co Ltd | Fiber raw material containing iron compound, and method for treating fiber raw material |
| CN103755333A (en) * | 2013-11-25 | 2014-04-30 | 胡敏刚 | Nano ferrite wave-absorbing material |
| CN104327794A (en) * | 2013-07-22 | 2015-02-04 | 深圳光启创新技术有限公司 | Wave absorbing composite material and preparation method thereof as well as artificial electromagnetic material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0782659A (en) * | 1993-09-08 | 1995-03-28 | Taiho Ind Co Ltd | Fiber raw material containing iron compound, and method for treating fiber raw material |
| CN104327794A (en) * | 2013-07-22 | 2015-02-04 | 深圳光启创新技术有限公司 | Wave absorbing composite material and preparation method thereof as well as artificial electromagnetic material and preparation method thereof |
| CN103755333A (en) * | 2013-11-25 | 2014-04-30 | 胡敏刚 | Nano ferrite wave-absorbing material |
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