CN106243712A - A kind of preparation method of electromagnetic shielding function elementary material - Google Patents
A kind of preparation method of electromagnetic shielding function elementary material Download PDFInfo
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- CN106243712A CN106243712A CN201610636411.9A CN201610636411A CN106243712A CN 106243712 A CN106243712 A CN 106243712A CN 201610636411 A CN201610636411 A CN 201610636411A CN 106243712 A CN106243712 A CN 106243712A
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention relates to the preparation method of a kind of electromagnetic shielding function elementary material, belong to shielding material preparing technical field.The present invention prepares silicon oxide particle first with rice husk, again it is carried out nanorize process, obtain nano silicon, then, after being stirred mixing with the material such as iron nitrate solution, carborundum by it, through calcining, nano-complex is obtained, it is placed on again in sodium hydroxide solution and is stirred reaction, obtain caged nitrided iron and nitrided iron/nanometer silicon carbide mixture, finally it is carried out ball milling with homemade electrically conductive polyaniline and mix, i.e. can get electromagnetic shielding function elementary material.Electromagnetic shielding function elementary material electromagnetic shielding frequency range width prepared by the present invention, shield effectiveness is good, and electromagnetic shielding frequency range is in the range of 30MHz～1.0GHz, and its shielding attenuation value reaches 55～65dB；Its intensity is higher, and hot strength reaches more than 35.65MPa, and bending strength reaches more than 55MPa.
Description
Technical field
The present invention relates to the preparation method of a kind of electromagnetic shielding function elementary material, belong to shielding material preparing technical field.
Background technology
Owing to electromagnetic device is commonly used in modern society, bring increasing electromagnetic interference problem, inorganic compounding electromagnetism
Shielding material is because of its high stability, easy compatibility, high-fire resistance, as the building of a kind of anti-electromagnetic interference, communication tool etc.
The potential material of aspect attracts wide attention.Electromagnetic shielding material not only needs good reflection electromagnetic wave performance, and
Needing good performance of absorbing electromagnetic wave, " thin, light, wide, strong " composite wave-suction material is the focus of electromagnetic-wave absorbent research
And difficult point.Carbon back powder density is low, specific surface area big, is a kind of well light material.Receive in carbon back powder Surface coating magnetic
The composite construction of rice metallic particles designs the radio-radar absorber with " thin, light, wide, strong " characteristic, can be camouflage coating material
Material assembles, and the developmental research of Combined Electromagnetic Shielding Materials provides a new way.Nanometer clad composite material has due to it
The features such as structure diversification, composition and performance are adjustable, the most compound, can be as the Combined Electromagnetic Shielding Materials of function admirable.
Existing research has metal dust, such as copper, silver, ferrum, nickel, gold etc.；Carbons, such as graphite, carbon fiber etc.；Conduction
Type polymer carrier；And core is magnetic fibre, such as nickel fiber, Fe3O4Fiber or ferrite doped calcium fiber, doped chemical is
Mn, Mg, Zn or Ba, or core is metallic nickel magnetic-particle, ferrite magnetic particle or ferro-aluminum boron magnetic alloy granule, and shell is for leading
The single components of screener such as electric metal (i.e. silver or copper) or the uniform filling of composite components is dispersed in polymeric matrix or
Person passes through coating, metal meltallizing, plating/chemical plating, Vacuum Deposition/sputtering plating, top layer affixed metal thin film etc. at polymeric matrix
Composite bed etc. is prepared on surface, and reprocessing prepares electromagnetic shielding material.But the electromagnetic shielding frequency range of these electromagnetic shielding materials is narrow, low
Spectrum mask usefulness is undesirable, and the most general filler particles is thick, is often substantially reduced material while ensureing shield effectiveness originally
The mechanical property of body.
Summary of the invention
The technical problem to be solved: narrow for existing electromagnetic shielding material electromagnetic shielding frequency range, low-frequency range shields
Usefulness is undesirable, and the most general filler particles is thick, is often substantially reduced the mechanics of material itself while ensureing shield effectiveness
The problem of performance, the present invention is silicon oxide particle first with the filtering residue that rice husk prepares, then it is carried out nanorize process,
Obtain nano silicon, after then being stirred mixing with the material such as iron nitrate solution, carborundum by it, through calcining, obtain
Nano-complex, then be placed in sodium hydroxide solution and be stirred reaction, obtain caged nitrided iron and nitrided iron/carborundum
Nano-mixture, finally carries out ball milling by it with homemade electrically conductive polyaniline and mixes, and i.e. can get electro-magnetic screen function primitive material
Material.Electromagnetic shielding function elementary material electromagnetic shielding frequency range width prepared by the present invention, shield effectiveness is good, and relevant mechanical property obtains
To being greatly improved.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
(1) weigh 10～20g rice husk pulverizing to pulverize, cross 200～300 mesh sieves, obtain rice husk powder, rice husk powder is added
Entering in beaker, adding 100～200mL mass concentrations is that 0.1mol/L hydrochloric acid solution soaks 12～14h, filters, obtains
Filtering residue is silicon oxide particle, and being joined by silicon oxide particle and filling 100～200mL mass concentrations is that 0.5mol/L sodium hydroxide is molten
Liquid, stirring reaction 1～2h, adding 100～200mL mass concentrations subsequently is 1mol/L hydrochloric acid solution, stirring reaction 2～3h,
Filter, obtain filtering residue, filtering residue is placed in Muffle furnace, calcine 3～4h at 600～700 DEG C, then naturally cool to room temperature, obtain
Nano silicon；
(2) nano silicon of above-mentioned preparation is joined in there-necked flask, sequentially add 100～200mL mass concentrations
For 0.1mol/L iron nitrate solution, 3～5g carborundum, 10～20mL Polyethylene Glycol, stir 10～20min, sequentially add 5～
10g zinc powder, stirring reaction 2～3h, reactant is placed in vacuum drying oven and is dried 2～3h, dried material is placed in Muffle
In stove, at 500～600 DEG C, it is passed through ammonia with the speed of 1～3L/min, reacts 20～30min, stop being passed through gas so that it is from
So it is cooled to room temperature, obtains nano-complex；
(3) joining in beaker by the nano-complex of above-mentioned preparation, adding 100～200mL mass concentrations is 0.5mol/L
Sodium hydroxide solution, stirring reaction 1～2h, filter, collect filtering residue, by residue washing 3～5 times, obtain caged nitrided iron and nitrogen
Change ferrum/nanometer silicon carbide mixture, standby；
(4) weigh 3～5g graphene oxides and join in beaker, add 100～200mL acetone, be placed in supersonic oscillations
In instrument, ultrasonic disperse 10～20min, obtain graphene oxide dispersion, are joined in flask by dispersion liquid, and are placed in by flask
In water-bath, control temperature, at 80～90 DEG C, sequentially adds 0.3～0.5g3-aminopropyl triethoxysilane, 0.3～0.5g
VTES, stirs 10～20min, adds 5～8g polyanilines, and 3～4h, then distillation of reducing pressure are reacted in stirring,
Obtain electrically conductive polyaniline；
(5) electrically conductive polyaniline of above-mentioned preparation is joined in ball mill, add the caged nitrided iron that above-mentioned steps (3) is standby
With nitrided iron/nanometer silicon carbide mixture, ball milling 6～8h, i.e. available a kind of electromagnetic shielding function elementary material.
Electromagnetic shielding function elementary material electromagnetic shielding frequency range prepared by the present invention in the range of 30MHz～1.0GHz, its
Shielding attenuation value reaches 55～65dB, and elongation at break is 8.5～9.5%, and hot strength reaches more than 35.65MPa, and bending is strong
Degree reaches more than 55MPa.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the electromagnetic shielding function elementary material electromagnetic shielding frequency range width that prepared by the present invention, shield effectiveness is good, electromagnetic shielding frequency range
In the range of 30MHz～1.0GHz, its shielding attenuation value reaches 55～65dB；
(2) its intensity of electromagnetic shielding function elementary material prepared by the present invention is higher, and hot strength reaches more than 35.65MPa, curved
Qu Qiangdu reaches more than 55MPa；
(3) preparation technology of the present invention is simple, and the cost of raw material is low.
Detailed description of the invention
First weigh 10～20g rice husk pulverizing to pulverize, cross 200～300 mesh sieves, obtain rice husk powder, by rice husk
Powder joins in beaker, and adding 100～200mL mass concentrations is that 0.1mol/L hydrochloric acid solution soaks 12～14h, filters,
The filtering residue obtained is silicon oxide particle, and being joined by silicon oxide particle and filling 100～200mL mass concentrations is 0.5mol/L hydrogen-oxygen
Changing sodium solution, stirring reaction 1～2h, adding 100～200mL mass concentrations subsequently is 1mol/L hydrochloric acid solution, stirs reaction 2
～3h, filter, obtain filtering residue, filtering residue is placed in Muffle furnace, calcine 3～4h at 600～700 DEG C, then naturally cool to room temperature,
Obtain nano silicon；The nano silicon of above-mentioned preparation is joined in there-necked flask, sequentially add 100～
200mL mass concentration is 0.1mol/L iron nitrate solution, 3～5g carborundum, 10～20mL Polyethylene Glycol, stirs 10～20min,
Sequentially add 5～10g zinc powders, stirring reaction 2～3h, reactant is placed in vacuum drying oven and is dried 2～3h, will be dried
Material be placed in Muffle furnace, at 500～600 DEG C, be passed through ammonia with the speed of 1～3L/min, react 20～30min, stop
It is passed through gas so that it is naturally cool to room temperature, obtains nano-complex；Again the nano-complex of above-mentioned preparation is joined beaker
In, adding 100～200mL mass concentrations is 0.5mol/L sodium hydroxide solution, stirring reaction 1～2h, filters, collects filter
Slag, by residue washing 3～5 times, obtains caged nitrided iron and nitrided iron/nanometer silicon carbide mixture, standby；Then weigh 3～
5g graphene oxide joins in beaker, adds 100～200mL acetone, is placed in ultrasonic disperse 10 in supersonic oscillations instrument
～20min, obtain graphene oxide dispersion, dispersion liquid is joined in flask, and flask is placed in water-bath, control temperature
Degree, at 80～90 DEG C, sequentially adds 0.3～0.5g3-aminopropyl triethoxysilane, 0.3～0.5g vinyl triethoxyl
Silane, stirs 10～20min, adds 5～8g polyanilines, stirring reaction 3～4h, then distillation of reducing pressure, obtains electrically conductive polyaniline；
Finally the electrically conductive polyaniline of above-mentioned preparation is joined in ball mill, add above-mentioned standby caged nitrided iron and nitrided iron/
Nanometer silicon carbide mixture, ball milling 6～8h, i.e. available a kind of electromagnetic shielding function elementary material.
Example 1
First weigh 20g rice husk pulverizing to pulverize, cross 300 mesh sieves, obtain rice husk powder, rice husk powder is joined beaker
In, adding 200mL mass concentration is that 0.1mol/L hydrochloric acid solution soaks 14h, filters, and the filtering residue obtained is silicon oxide particle,
Being joined by silicon oxide particle and filling 200mL mass concentration is 0.5mol/L sodium hydroxide solution, stirring reaction 2h, adds the most again
Entering 200mL mass concentration is 1mol/L hydrochloric acid solution, stirring reaction 3h, filters, obtains filtering residue, be placed in Muffle furnace by filtering residue,
Calcine 4h at 700 DEG C, then naturally cool to room temperature, obtain nano silicon；The nano silicon of above-mentioned preparation is added
In there-necked flask, sequentially adding 200mL mass concentration is 0.1mol/L iron nitrate solution, 5g carborundum, the poly-second of 20mL two
Alcohol, stirs 20min, sequentially adds 10g zinc powder, stirring reaction 3h, is placed in vacuum drying oven by reactant and is dried 3h, will be dry
Material after dry is placed in Muffle furnace, at 600 DEG C, is passed through ammonia with the speed of 3L/min, reacts 30min, stops being passed through gas,
Make it naturally cool to room temperature, obtain nano-complex；Again the nano-complex of above-mentioned preparation is joined in beaker, add
200mL mass concentration is 0.5mol/L sodium hydroxide solution, stirring reaction 2h, filters, collects filtering residue, by residue washing 5 times,
To caged nitrided iron and nitrided iron/nanometer silicon carbide mixture, standby；Then weigh 5g graphene oxide and join in beaker,
Add 200mL acetone, be placed in ultrasonic disperse 20min in supersonic oscillations instrument, obtain graphene oxide dispersion, will dispersion
Liquid joins in flask, and is placed in water-bath by flask, and control temperature, at 90 DEG C, sequentially adds 0.5g3-aminopropyl three second
TMOS, 0.5g VTES, stir 20min, adds 8g polyaniline, stirring reaction 4h, then steaming of reducing pressure
Evaporate, obtain electrically conductive polyaniline；Finally the electrically conductive polyaniline of above-mentioned preparation is joined in ball mill, add above-mentioned standby cage
Shape nitrided iron and nitrided iron/nanometer silicon carbide mixture, ball milling 8h, i.e. available a kind of electromagnetic shielding function elementary material.Warp
Detection, electromagnetic shielding function elementary material electromagnetic shielding frequency range prepared by the present invention is 30MHz, and its shielding attenuation value reaches
55dB, elongation at break is 9.5%, and hot strength reaches 35.78MPa, and bending strength reaches 58MPa.
Example 2
First weigh 10g rice husk pulverizing to pulverize, cross 200 mesh sieves, obtain rice husk powder, rice husk powder is joined beaker
In, adding 100mL mass concentration is that 0.1mol/L hydrochloric acid solution soaks 12h, filters, and the filtering residue obtained is silicon oxide particle,
Being joined by silicon oxide particle and filling 100mL mass concentration is 0.5mol/L sodium hydroxide solution, stirring reaction 1h, adds the most again
Entering 100mL mass concentration is 1mol/L hydrochloric acid solution, stirring reaction 2h, filters, obtains filtering residue, be placed in Muffle furnace by filtering residue,
Calcine 3h at 600 DEG C, then naturally cool to room temperature, obtain nano silicon；The nano silicon of above-mentioned preparation is added
In there-necked flask, sequentially adding 100mL mass concentration is 0.1mol/L iron nitrate solution, 3g carborundum, the poly-second of 10mL two
Alcohol, stirs 10min, sequentially adds 5g zinc powder, stirring reaction 2h, is placed in vacuum drying oven by reactant and is dried 2h, will be dried
After material be placed in Muffle furnace, at 500 DEG C, be passed through ammonia with the speed of 1L/min, react 20min, stop being passed through gas, make
It naturally cools to room temperature, obtains nano-complex；Again the nano-complex of above-mentioned preparation is joined in beaker, add
100mL mass concentration is 0.5mol/L sodium hydroxide solution, stirring reaction 1h, filters, collects filtering residue, by residue washing 3 times,
To caged nitrided iron and nitrided iron/nanometer silicon carbide mixture, standby；Then weigh 3g graphene oxide and join in beaker,
Add 100mL acetone, be placed in ultrasonic disperse 10min in supersonic oscillations instrument, obtain graphene oxide dispersion, will dispersion
Liquid joins in flask, and is placed in water-bath by flask, and control temperature, at 80 DEG C, sequentially adds 0.3g3-aminopropyl three second
TMOS, 0.3g VTES, stir 10min, adds 5g polyaniline, stirring reaction 3h, then steaming of reducing pressure
Evaporate, obtain electrically conductive polyaniline；Finally the electrically conductive polyaniline of above-mentioned preparation is joined in ball mill, add above-mentioned standby cage
Shape nitrided iron and nitrided iron/nanometer silicon carbide mixture, ball milling 6h, i.e. available a kind of electromagnetic shielding function elementary material.Warp
Detection, electromagnetic shielding function elementary material electromagnetic shielding frequency range prepared by the present invention is 50MHz, and its shielding attenuation value reaches
60dB, elongation at break is 8.5%, and hot strength reaches 35.70MPa, and bending strength reaches 57MPa.
Example 3
First weigh 15g rice husk pulverizing to pulverize, cross 250 mesh sieves, obtain rice husk powder, rice husk powder is joined beaker
In, adding 150mL mass concentration is that 0.1mol/L hydrochloric acid solution soaks 13h, filters, and the filtering residue obtained is silicon oxide particle,
Being joined by silicon oxide particle and filling 150mL mass concentration is 0.5mol/L sodium hydroxide solution, stirring reaction 1h, adds the most again
Entering 150mL mass concentration is 1mol/L hydrochloric acid solution, stirring reaction 2h, filters, obtains filtering residue, be placed in Muffle furnace by filtering residue,
Calcine 3h at 650 DEG C, then naturally cool to room temperature, obtain nano silicon；The nano silicon of above-mentioned preparation is added
In there-necked flask, sequentially adding 150mL mass concentration is 0.1mol/L iron nitrate solution, 4g carborundum, the poly-second of 15mL two
Alcohol, stirs 15min, sequentially adds 7g zinc powder, stirring reaction 2h, is placed in vacuum drying oven by reactant and is dried 3h, will be dried
After material be placed in Muffle furnace, at 550 DEG C, be passed through ammonia with the speed of 2L/min, react 25min, stop being passed through gas, make
It naturally cools to room temperature, obtains nano-complex；Again the nano-complex of above-mentioned preparation is joined in beaker, add
150mL mass concentration is 0.5mol/L sodium hydroxide solution, stirring reaction 2h, filters, collects filtering residue, by residue washing 4 times,
To caged nitrided iron and nitrided iron/nanometer silicon carbide mixture, standby；Then weigh 4g graphene oxide and join in beaker,
Add 150mL acetone, be placed in ultrasonic disperse 15min in supersonic oscillations instrument, obtain graphene oxide dispersion, will dispersion
Liquid joins in flask, and is placed in water-bath by flask, and control temperature, at 85 DEG C, sequentially adds 0.4g3-aminopropyl three second
TMOS, 0.4g VTES, stir 15min, adds 7g polyaniline, stirring reaction 3h, then steaming of reducing pressure
Evaporate, obtain electrically conductive polyaniline；Finally the electrically conductive polyaniline of above-mentioned preparation is joined in ball mill, add above-mentioned standby cage
Shape nitrided iron and nitrided iron/nanometer silicon carbide mixture, ball milling 7h, i.e. available a kind of electromagnetic shielding function elementary material.Warp
Detection, electromagnetic shielding function elementary material electromagnetic shielding frequency range prepared by the present invention is 1.0GHz, and its shielding attenuation value reaches
65dB, elongation at break is 8.6%, and hot strength reaches 36.65MPa, and bending strength reaches 58MPa.
Claims (1)
1. the preparation method of an electromagnetic shielding function elementary material, it is characterised in that concrete preparation process is:
(1) weigh 10～20g rice husk pulverizing to pulverize, cross 200～300 mesh sieves, obtain rice husk powder, rice husk powder is added
Entering in beaker, adding 100～200mL mass concentrations is that 0.1mol/L hydrochloric acid solution soaks 12～14h, filters, obtains
Filtering residue is silicon oxide particle, and being joined by silicon oxide particle and filling 100～200mL mass concentrations is that 0.5mol/L sodium hydroxide is molten
Liquid, stirring reaction 1～2h, adding 100～200mL mass concentrations subsequently is 1mol/L hydrochloric acid solution, stirring reaction 2～3h,
Filter, obtain filtering residue, filtering residue is placed in Muffle furnace, calcine 3～4h at 600～700 DEG C, then naturally cool to room temperature, obtain
Nano silicon；
(2) nano silicon of above-mentioned preparation is joined in there-necked flask, sequentially add 100～200mL mass concentrations
For 0.1mol/L iron nitrate solution, 3～5g carborundum, 10～20mL Polyethylene Glycol, stir 10～20min, sequentially add 5～
10g zinc powder, stirring reaction 2～3h, reactant is placed in vacuum drying oven and is dried 2～3h, dried material is placed in Muffle
In stove, at 500～600 DEG C, it is passed through ammonia with the speed of 1～3L/min, reacts 20～30min, stop being passed through gas so that it is from
So it is cooled to room temperature, obtains nano-complex；
(3) joining in beaker by the nano-complex of above-mentioned preparation, adding 100～200mL mass concentrations is 0.5mol/L
Sodium hydroxide solution, stirring reaction 1～2h, filter, collect filtering residue, by residue washing 3～5 times, obtain caged nitrided iron and nitrogen
Change ferrum/nanometer silicon carbide mixture, standby；
(4) weigh 3～5g graphene oxides and join in beaker, add 100～200mL acetone, be placed in supersonic oscillations
In instrument, ultrasonic disperse 10～20min, obtain graphene oxide dispersion, are joined in flask by dispersion liquid, and are placed in by flask
In water-bath, control temperature, at 80～90 DEG C, sequentially adds 0.3～0.5g3-aminopropyl triethoxysilane, 0.3～0.5g
VTES, stirs 10～20min, adds 5～8g polyanilines, and 3～4h, then distillation of reducing pressure are reacted in stirring,
Obtain electrically conductive polyaniline；
(5) electrically conductive polyaniline of above-mentioned preparation is joined in ball mill, add the caged nitrided iron that above-mentioned steps (3) is standby
With nitrided iron/nanometer silicon carbide mixture, ball milling 6～8h, i.e. available a kind of electromagnetic shielding function elementary material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111063400A (en) * | 2019-12-18 | 2020-04-24 | 哈尔滨工业大学 | Design method of solar spectrum total absorption carbon-based functional material |
| CN111935968A (en) * | 2020-08-21 | 2020-11-13 | 山东大学 | Preparation method of iron/nitrogen/carbon composite material |
-
2016
- 2016-08-05 CN CN201610636411.9A patent/CN106243712A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111063400A (en) * | 2019-12-18 | 2020-04-24 | 哈尔滨工业大学 | Design method of solar spectrum total absorption carbon-based functional material |
| CN111063400B (en) * | 2019-12-18 | 2020-12-11 | 哈尔滨工业大学 | Design method of solar spectrum total absorption carbon-based functional material |
| CN111935968A (en) * | 2020-08-21 | 2020-11-13 | 山东大学 | Preparation method of iron/nitrogen/carbon composite material |
| CN111935968B (en) * | 2020-08-21 | 2021-08-27 | 山东大学 | Preparation method of iron/nitrogen/carbon composite material |
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Application publication date: 20161221 |
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| RJ01 | Rejection of invention patent application after publication |