CN106374233A - High-efficiency wave absorbing composite material - Google Patents
High-efficiency wave absorbing composite material Download PDFInfo
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- CN106374233A CN106374233A CN201611108285.6A CN201611108285A CN106374233A CN 106374233 A CN106374233 A CN 106374233A CN 201611108285 A CN201611108285 A CN 201611108285A CN 106374233 A CN106374233 A CN 106374233A
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- Prior art keywords
- temperature
- composite material
- constant temperature
- suction composite
- wave suction
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
- H01Q17/007—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems with means for controlling the absorption
Abstract
The invention discloses a high-efficiency wave absorbing composite material. Dual crystallization is carried out on iron chloride, aluminum chloride and nickel chloride by taking oxalate as a coordination agent and crown ether as an covering agent to obtain a mixed magnetic material, the mixed magnetic material is mixed with graphene powder, an adhesive, a coupling agent and a dispersing agent to form a suspended dispersion liquid, and the suspended dispersion liquid is pulled through and kept in a constant temperature to obtain the wave absorbing material. The method is simple, technical conditions are not strict, the production cost is low, the material structure is stable and not damaged by high temperature, magnetic performance is kept complete, the total performance is high, the surface density is low, and the absorption frequency range is wide.
Description
Technical field
The invention belongs to inhaling wave technology field and in particular to a kind of efficient Wave suction composite material.
Background technology
Absorbing material, refers to absorb a class material of the electromagnetic wave energy projecting its surface.On engineer applied, except will
Ask absorbing material electromagnetic wave to be had outside high absorbance in broad frequency band, also require it have light weight, heatproof, moisture-proof,
The performance such as anticorrosive.Absorbing material is a kind of important functional material, is applied at first in military affairs, with scientific and technical development
Start to be applied to civil area, such as microwave dark room material, anti-electromagnetic-radiation and interference, microwave attenuator element and electromagnetic compatibility
Facility.Using more universal wave absorbing agent in 12- 18ghz frequency range at present is ferrite magnetic material, but ferrite magnetic material
Density larger (density of such as manganese-zinc ferrite be 4.82g/cm3, the density of ferrum oxide is 5.24g/cm3), non-refractory,
And do not possess fluorescent effect.
Content of the invention
It is an object of the invention to provide a kind of efficient Wave suction composite material, the inventive method simplicity, process conditions are gentle, raw
Produce low cost, material structure is stable, without high temperature, magnetic retains completely, and overall performance is good, and surface density is low, absorbs
Frequency range width.
A kind of efficient Wave suction composite material, its preparation process is as follows:
Step 1, iron chloride, aluminum chloride and Nickel dichloride. is added to water, carries out constant temperature stirring reaction 2-4h, then pass to ammonia
Carry out aerated reaction 2-4h, filter pressing can be precipitated mixture；
Step 2, precipitation mixture is dissolved in distilled water and stirs, and is subsequently adding potassium oxalate and ammonium oxalate, and slight fever stirs
Until being completely dissolved, obtain mixed liquor；
Step 3, mixed liquor is boiled altogether 3-5h, then constant temperature distillation and concentration 3-7h, forms stable concentrated solution；
Step 4, concentrated solution low temperature maturation 2-8h obtains crystal settling, obtains mixed crystal after filtration washing；
Step 5, crystal is added to dehydrated alcohol, adds crown ether, heating sealing stirring 10-15h, obtains lysate, standing
Evaporation at constant temperature, obtains secondary crystallization body, obtains two recrystallization after filtration；
Step 6, two recrystallization are added to isopropanol, after stirring, add Graphene powder, binding agent, coupling agent and divide
Powder, ultrasonic obtains suspended dispersion liquid；
Step 7, by suspended dispersion liquid with Best-Effort request mode plated film on base material, carry out constant temperature 3-6h, efficiently inhaled ripple multiple
Condensation material.
Described Wave suction composite material to prepare formula as follows:
Iron chloride 10-15 part, aluminum chloride 2-5 part, Nickel dichloride. 2-4 part, potassium oxalate 30-40 part, ammonium oxalate 5-10 part, crown ether 15-
20 parts, Graphene powder 6-10 part, binding agent 3-5 part, coupling agent 1-3 part, dispersant 1-3 part.
Described adhesive adopts polyacrylate, described coupling agent to adopt four epoxide titanate esters, and described dispersant is using hard
Fat acid calcium.
The speed of the constant temperature stirring in described step 1 is 200-500r/min, the amount of the material of described ammonia be iron chloride,
3.5-4.3 times of the amount of the material of aluminum chloride and Nickel dichloride., described aerating gas flow velocity is 30-35ml/min, and described aeration is anti-
Aerated reaction should be sealed using constant temperature, described aeration temperature is 60-80 DEG C, the pressure of described filter pressing is 0.8-1.2mpa；This step
Suddenly iron ion, aluminium ion and nickel ion are carried out by hydroxide precipitation using ammonia aeration, there is good mixed effect, protect
Demonstrate,prove the mixed effect of three metal ion species, adopt the sedimentation method by Impurity removal simultaneously.
The temperature of the slight fever stirring in described step 2 is 40-60 DEG C, and described mixing speed is 500-1000r/min；This step
By the way of the rapid stirring using slight fever, formation metal ion-based oxalic acid potassium salt, tool are reacted with mixed precipitation by potassium oxalate and ammonium oxalate
There is good dissolubility.
Temperature of boiling altogether in described step 3 is 100-110 DEG C, and the temperature of described constant temperature distillation is 80-100 DEG C, described steaming
Evaporating concentrated solution is original 0.05-0.15；This step is passed through to boil stablizing of guarantee metal ion-based oxalic acid potassium salt altogether, removes excessive
Ammonium oxalate.
Aging Temperature in described step 4 is 0-6 DEG C, and described low temperature maturation adopts still aging method, described filtration washing
Using absolute ethanol washing, described drying mode is to be dried using the volatile standing of dehydrated alcohol；This step pass through metal from
Subbase oxalic acid potassium salt dissolubility difference at different temperatures, metal ion-based oxalic acid potassium salt is deposited in the form of crystal, protects
The stability of card metal ion-based oxalic acid potassium salt and purity.
The temperature of the heating sealing stirring in described step 5 is 50-70 DEG C, and the temperature of described standing evaporation at constant temperature is 30
℃；This step is reacted with crown ether by metal ion-based oxalic acid potassium salt, forms cladded type magnetic material, and by dehydrated alcohol
Hybrid metal crown ether material is carried out secondary crystallization by dissolubility, forms crystalline material, can not only obtain the higher magnetic of degree of purity
Property material, also ensure that the magnetic temperature stability of magnetic material simultaneously.
Supersonic frequency in described step 6 is 10-15khz, and this step is by the way of ultrasonic by graphene powder and magnetic
Property crystalline material mixing, be aided with auxiliary agent and form stable suspended dispersive material.
Thermostat temperature in described step 7 is 20-30 DEG C, and described Best-Effort request speed is 50-600mm/min；This step
Material is coated in by substrate surface with czochralski method, there is good dispersibility, be baked under constant temperature simultaneously, provide not only
Good adhesion connectivity, prevents high temperature sintering from causing magnetic to lose simultaneously.
Compared with prior art, the method have the advantages that
1st, the inventive method is easy, and process conditions are gentle, low production cost, and material structure is stable, without high temperature, magnetic
Retain complete, overall performance is good, and surface density is low, absorb frequency range width.
2nd, efficiently, favorable repeatability, to thunderstorm activity effect substantially it is shown that it is in radar for the process is simple of the present invention
The wide application prospect in the stealthy field of ripple and electromagnetic shielding field.
Brief description
Fig. 1 is the stereoscan photograph of the Wave suction composite material of the embodiment of the present invention 1 preparation.
Fig. 2 is the absorbing property test of the Wave suction composite material of the embodiment of the present invention 1 preparation.
Specific embodiment
With reference to embodiment, the present invention is described further:
Embodiment 1
A kind of efficient Wave suction composite material, its preparation process is as follows:
Step 1, iron chloride, aluminum chloride and Nickel dichloride. is added to water, carries out constant temperature stirring reaction 2h, then pass to ammonia and enter
Row aerated reaction 2h, filter pressing can be precipitated mixture；
Step 2, precipitation mixture is dissolved in distilled water and stirs, and is subsequently adding potassium oxalate and ammonium oxalate, and slight fever stirs
Until being completely dissolved, obtain mixed liquor；
Step 3, mixed liquor is boiled altogether 3h, then constant temperature distillation and concentration 3h, forms stable concentrated solution；
Step 4, concentrated solution low temperature maturation 2h obtains crystal settling, obtains mixed crystal after filtration washing；
Step 5, crystal is added to dehydrated alcohol, adds crown ether, heating sealing stirring 10h, obtains lysate, stand constant temperature
Evaporation, obtains secondary crystallization body, obtains two recrystallization after filtration；
Step 6, two recrystallization are added to isopropanol, after stirring, add Graphene powder, binding agent, coupling agent and divide
Powder, ultrasonic obtains suspended dispersion liquid；
Step 7, by suspended dispersion liquid with Best-Effort request mode plated film on base material, carry out constant temperature 3h, efficiently inhaled ripple be combined
Material.
Described Wave suction composite material to prepare formula as follows:
10 parts of iron chloride, 2 parts of aluminum chloride, 2 parts of Nickel dichloride., 30 parts of potassium oxalate, 5 parts of ammonium oxalate, 15 parts of crown ether, 6 parts of Graphene powder,
3 parts of binding agent, coupling agent 1- part, 1 part of dispersant.
Described adhesive adopts polyacrylate, described coupling agent to adopt four epoxide titanate esters, and described dispersant is using hard
Fat acid calcium.
The speed of the constant temperature stirring in described step 1 is 200r/min, and the amount of the material of described ammonia is iron chloride, chlorination
3.5 times of the amount of the material of aluminum and Nickel dichloride., described aerating gas flow velocity is 30ml/min, and described aerated reaction adopts constant temperature close
Envelope aerated reaction, described aeration temperature is 60 DEG C, and the pressure of described filter pressing is 0.8mpa.
The temperature of the slight fever stirring in described step 2 is 40 DEG C, and described mixing speed is 500r/min.
Temperature of boiling altogether in described step 3 is 100 DEG C, and the temperature of described constant temperature distillation is 80 DEG C, described distilled and concentrated solution
For original 0.05.
Aging Temperature in described step 4 is 0 DEG C, and described low temperature maturation adopts still aging method, and described filtration washing is adopted
With absolute ethanol washing, described drying mode is to be dried using the volatile standing of dehydrated alcohol.
The temperature of the heating sealing stirring in described step 5 is 50 DEG C, and the temperature of described standing evaporation at constant temperature is 30 DEG C.
Supersonic frequency in described step 6 is 10khz.
Thermostat temperature in described step 7 is 20 DEG C, and described Best-Effort request speed is 50mm/min.
As seen from Figure 1, in the Wave suction composite material of this example preparation, magnetic metal material is evenly distributed, effective and Graphene
It is combined with each other.From Figure 2 it can be seen that the absorbing property of the Wave suction composite material of this example preparation is good, in the range of 2-18ghz, should
The absorption frequency range that absorbing material is less than -5db reaches 15ghz, and the absorption frequency range less than -10db reaches 4.6ghz.
Embodiment 2
A kind of efficient Wave suction composite material, its preparation process is as follows:
Step 1, iron chloride, aluminum chloride and Nickel dichloride. is added to water, carries out constant temperature stirring reaction 4h, then pass to ammonia and enter
Row aerated reaction 4h, filter pressing can be precipitated mixture；
Step 2, precipitation mixture is dissolved in distilled water and stirs, and is subsequently adding potassium oxalate and ammonium oxalate, and slight fever stirs
Until being completely dissolved, obtain mixed liquor；
Step 3, mixed liquor is boiled altogether 5h, then constant temperature distillation and concentration 7h, forms stable concentrated solution；
Step 4, concentrated solution low temperature maturation 8h obtains crystal settling, obtains mixed crystal after filtration washing；
Step 5, crystal is added to dehydrated alcohol, adds crown ether, heating sealing stirring 15h, obtains lysate, stand constant temperature
Evaporation, obtains secondary crystallization body, obtains two recrystallization after filtration；
Step 6, two recrystallization are added to isopropanol, after stirring, add Graphene powder, binding agent, coupling agent and divide
Powder, ultrasonic obtains suspended dispersion liquid；
Step 7, by suspended dispersion liquid with Best-Effort request mode plated film on base material, carry out constant temperature 6h, efficiently inhaled ripple be combined
Material.
Described Wave suction composite material to prepare formula as follows:
15 parts of iron chloride, 5 parts of aluminum chloride, 4 parts of Nickel dichloride., 40 parts of potassium oxalate, 10 parts of ammonium oxalate, 20 parts of crown ether, Graphene powder 10
Part, 5 parts of binding agent, 3 parts of coupling agent, 3 parts of dispersant.
Described adhesive adopts polyacrylate, described coupling agent to adopt four epoxide titanate esters, and described dispersant is using hard
Fat acid calcium.
The speed of the constant temperature stirring in described step 1 is 500r/min, and the amount of the material of described ammonia is iron chloride, chlorination
4.3 times of the amount of the material of aluminum and Nickel dichloride., described aerating gas flow velocity is 35ml/min, and described aerated reaction adopts constant temperature close
Envelope aerated reaction, described aeration temperature is 80 DEG C, and the pressure of described filter pressing is 1.2mpa.
The temperature of the slight fever stirring in described step 2 is 60 DEG C, and described mixing speed is 1000r/min.
Temperature of boiling altogether in described step 3 is 110 DEG C, and the temperature of described constant temperature distillation is 100 DEG C, described distilled and concentrated solution
For original 0.15.
Aging Temperature in described step 4 is 6 DEG C, and described low temperature maturation adopts still aging method, and described filtration washing is adopted
With absolute ethanol washing, described drying mode is to be dried using the volatile standing of dehydrated alcohol.
The temperature of the heating sealing stirring in described step 5 is 70 DEG C, and the temperature of described standing evaporation at constant temperature is 30 DEG C.
Supersonic frequency in described step 6 is 15khz.
Thermostat temperature in described step 7 is 30 DEG C, and described Best-Effort request speed is 600mm/min.
Embodiment 3
A kind of efficient Wave suction composite material, its preparation process is as follows:
Step 1, iron chloride, aluminum chloride and Nickel dichloride. is added to water, carries out constant temperature stirring reaction 3h, then pass to ammonia and enter
Row aerated reaction 3h, filter pressing can be precipitated mixture；
Step 2, precipitation mixture is dissolved in distilled water and stirs, and is subsequently adding potassium oxalate and ammonium oxalate, and slight fever stirs
Until being completely dissolved, obtain mixed liquor；
Step 3, mixed liquor is boiled altogether 4h, then constant temperature distillation and concentration 5h, forms stable concentrated solution；
Step 4, concentrated solution low temperature maturation 5h obtains crystal settling, obtains mixed crystal after filtration washing；
Step 5, crystal is added to dehydrated alcohol, adds crown ether, heating sealing stirring 12h, obtains lysate, stand constant temperature
Evaporation, obtains secondary crystallization body, obtains two recrystallization after filtration；
Step 6, two recrystallization are added to isopropanol, after stirring, add Graphene powder, binding agent, coupling agent and divide
Powder, ultrasonic obtains suspended dispersion liquid；
Step 7, by suspended dispersion liquid with Best-Effort request mode plated film on base material, carry out constant temperature 4h, efficiently inhaled ripple be combined
Material.
Described Wave suction composite material to prepare formula as follows:
13 parts of iron chloride, 4 parts of aluminum chloride, 3 parts of Nickel dichloride., 35 parts of potassium oxalate, 9 parts of ammonium oxalate, 18 parts of crown ether, 8 parts of Graphene powder,
4 parts of binding agent, 2 parts of coupling agent, 2 parts of dispersant.
Described adhesive adopts polyacrylate, described coupling agent to adopt four epoxide titanate esters, and described dispersant is using hard
Fat acid calcium.
The speed of the constant temperature stirring in described step 1 is 400r/min, and the amount of the material of described ammonia is iron chloride, chlorination
3.9 times of the amount of the material of aluminum and Nickel dichloride., described aerating gas flow velocity is 33ml/min, and described aerated reaction adopts constant temperature close
Envelope aerated reaction, described aeration temperature is 70 DEG C, and the pressure of described filter pressing is 1.0mpa.
The temperature of the slight fever stirring in described step 2 is 50 DEG C, and described mixing speed is 800r/min.
Temperature of boiling altogether in described step 3 is 105 DEG C, and the temperature of described constant temperature distillation is 90 DEG C, described distilled and concentrated solution
For original 0.08.
Aging Temperature in described step 4 is 2 DEG C, and described low temperature maturation adopts still aging method, and described filtration washing is adopted
With absolute ethanol washing, described drying mode is to be dried using the volatile standing of dehydrated alcohol.
The temperature of the heating sealing stirring in described step 5 is 60 DEG C, and the temperature of described standing evaporation at constant temperature is 30 DEG C.
Supersonic frequency in described step 6 is 13khz.
Thermostat temperature in described step 7 is 23 DEG C, and described Best-Effort request speed is 400mm/min.
The foregoing is only one embodiment of the invention, be not intended to limit the present invention, all employing equivalents or equivalent transformation
The technical scheme that obtained of mode, all fall within protection scope of the present invention.
Claims (10)
1. a kind of efficient Wave suction composite material is it is characterised in that its preparation process is as follows:
Step 1, iron chloride, aluminum chloride and Nickel dichloride. is added to water, carries out constant temperature stirring reaction 2-4h, then pass to ammonia
Carry out aerated reaction 2-4h, filter pressing can be precipitated mixture；
Step 2, precipitation mixture is dissolved in distilled water and stirs, and is subsequently adding potassium oxalate and ammonium oxalate, and slight fever stirs
Until being completely dissolved, obtain mixed liquor；
Step 3, mixed liquor is boiled altogether 3-5h, then constant temperature distillation and concentration 3-7h, forms stable concentrated solution；
Step 4, concentrated solution low temperature maturation 2-8h obtains crystal settling, obtains mixed crystal after filtration washing；
Step 5, crystal is added to dehydrated alcohol, adds crown ether, heating sealing stirring 10-15h, obtains lysate, standing
Evaporation at constant temperature, obtains secondary crystallization body, obtains two recrystallization after filtration；
Step 6, two recrystallization are added to isopropanol, after stirring, add Graphene powder, binding agent, coupling agent and divide
Powder, ultrasonic obtains suspended dispersion liquid；
Step 7, by suspended dispersion liquid with Best-Effort request mode plated film on base material, carry out constant temperature 3-6h, efficiently inhaled ripple multiple
Condensation material.
2. a kind of efficient Wave suction composite material according to claim 1 is it is characterised in that the system of described Wave suction composite material
Standby formula is as follows:
Iron chloride 10-15 part, aluminum chloride 2-5 part, Nickel dichloride. 2-4 part, potassium oxalate 30-40 part, ammonium oxalate 5-10 part, crown ether 15-
20 parts, Graphene powder 6-10 part, binding agent 3-5 part, coupling agent 1-3 part, dispersant 1-3 part.
3. a kind of efficient Wave suction composite material according to claim 2 is it is characterised in that described adhesive adopts polypropylene
Acid esters, described coupling agent adopt four epoxide titanate esters, and described dispersant adopts calcium stearate.
4. a kind of efficient Wave suction composite material according to claim 1 is it is characterised in that the constant temperature in described step 1 stirs
The speed mixed is 200-500r/min, and the amount of the material of described ammonia is the amount of the material of iron chloride, aluminum chloride and Nickel dichloride.
3.5-4.3 times, described aerating gas flow velocity is 30-35ml/min, and described aerated reaction adopts constant temperature to seal aerated reaction, described
Aeration temperature is 60-80 DEG C, and the pressure of described filter pressing is 0.8-1.2mpa.
5. a kind of efficient Wave suction composite material according to claim 1 is it is characterised in that the slight fever in described step 2 is stirred
The temperature mixed is 40-60 DEG C, and described mixing speed is 500-1000r/min.
6. a kind of efficient Wave suction composite material according to claim 1 is it is characterised in that boil temperature altogether in described step 3
Spend for 100-110 DEG C, the temperature of described constant temperature distillation is 80-100 DEG C, and described distilled and concentrated solution is original 0.05-0.15.
7. a kind of efficient Wave suction composite material according to claim 1 is it is characterised in that ageing temperature in described step 4
Spend for 0-6 DEG C, described low temperature maturation adopts still aging method, described filtration washing adopts absolute ethanol washing, described drying side
Formula is to be dried using the volatile standing of dehydrated alcohol.
8. a kind of efficient Wave suction composite material according to claim 1 is it is characterised in that the heating in described step 5 is close
The temperature of envelope stirring is 50-70 DEG C, and the temperature of described standing evaporation at constant temperature is 30 DEG C.
9. a kind of efficient Wave suction composite material according to claim 1 is it is characterised in that supersonic frequency in described step 6
Rate is 10-15khz.
10. a kind of efficient Wave suction composite material according to claim 1 is it is characterised in that constant temperature temperature in described step 7
Spend for 20-30 DEG C, described Best-Effort request speed is 50-600mm/min.
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| CN201611108285.6A CN106374233A (en) | 2016-12-06 | 2016-12-06 | High-efficiency wave absorbing composite material |
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| CN201611108285.6A CN106374233A (en) | 2016-12-06 | 2016-12-06 | High-efficiency wave absorbing composite material |
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| CN104530685A (en) * | 2015-01-06 | 2015-04-22 | 中国人民解放军第二炮兵工程大学 | Method for manufacturing carbonyl iron foam wave-absorbing material |
| CN104530467A (en) * | 2015-01-05 | 2015-04-22 | 中国人民解放军第二炮兵工程大学 | Preparation method of light bandwidth wave-absorbing material |
| CN105219345A (en) * | 2015-10-16 | 2016-01-06 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material |
| WO2016117718A1 (en) * | 2015-01-20 | 2016-07-28 | Chang Sung Co., Ltd. | Electromagnetic wave shielding and absorbing sheet and manufacturing method of the same |
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294047A (en) * | 2008-06-04 | 2008-10-29 | 北京航空航天大学 | Radar wave absorbing paint with hollow microsphere as filling material and preparation method thereof |
| CN102703024A (en) * | 2012-06-01 | 2012-10-03 | 江南大学 | Method for preparing multi-layer composite nanometer wave-absorbing materials |
| CN103173056A (en) * | 2012-12-14 | 2013-06-26 | 北京康拓科技有限公司 | Preparation method of Fe/SiO2 nano-multilayer film electromagnetic-wave absorbing material |
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| CN104530467A (en) * | 2015-01-05 | 2015-04-22 | 中国人民解放军第二炮兵工程大学 | Preparation method of light bandwidth wave-absorbing material |
| CN104530685A (en) * | 2015-01-06 | 2015-04-22 | 中国人民解放军第二炮兵工程大学 | Method for manufacturing carbonyl iron foam wave-absorbing material |
| WO2016117718A1 (en) * | 2015-01-20 | 2016-07-28 | Chang Sung Co., Ltd. | Electromagnetic wave shielding and absorbing sheet and manufacturing method of the same |
| CN105219345A (en) * | 2015-10-16 | 2016-01-06 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material |
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Application publication date: 20170201 |