CN101665635A - Method for preparing high-performance wave-absorbing composite powder - Google Patents
Method for preparing high-performance wave-absorbing composite powder Download PDFInfo
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- CN101665635A CN101665635A CN200910196314A CN200910196314A CN101665635A CN 101665635 A CN101665635 A CN 101665635A CN 200910196314 A CN200910196314 A CN 200910196314A CN 200910196314 A CN200910196314 A CN 200910196314A CN 101665635 A CN101665635 A CN 101665635A
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Abstract
The invention belongs to the technical field of microwave absorbing material, and more particularly relates to a preparation method of high-performance wave-absorbing composite powder, comprising thesteps of: respectively adding distilled water into soluble metal nitrate, ferric nitrate and citric acid for dissolving, and then mixing the water solutions to prepare a precursor; dripping ammonia water solution to adjust the pH value of the mixed solution to be neutral; putting the solution into water bath with the temperature of 70-90 DEG C to be stirred, adding inorganic porous medium and modifying agent in the stirring process, stirring until the liquid is sticky colloid; drying the prepared colloidal sol for 7.5-8.5h at the temperature of 115-125 DEG C, and obtaining dried gel; putting the gel into a muffle furnace for calcining, heating up to 850 DEG C, preserving the temperature for 1-2h, naturally and slowly cooling, and obtaining ferrite composite powder; and finally, mixing thecomposite power and carbonyl iron powder, and then obtaining the needed product. The stoichiometric proportion among the nitrate, the ferric nitrate and the citric acid is 1: 12: 19 or 1: 2: 4, the ratio between the theoretical value of the ferrite and the mass of the modifying agent is 1: 0.1-1:0.05, the ratio between the theoretical value of the ferrite and the mass of the porous medium is 1: 0.2-1: 5, and the mass ratio between ferrite-porous medium composite power and the carbonyl iron powder is 1: 0.2-1: 5. Compared with the traditional product, the wave-absorbing powder improves the wave-absorbing performance, and has good covering effect and a certain function of heat insulation. Therefore, the method can be used for preparing building wave-absorbing paint.
Description
Technical field
The invention belongs to the microwave absorbing material technical field, be specifically related to a kind of preparation method of high-performance wave-absorbing composite powder.
Background technology
Ferrite Material is present main electromagnetic-wave absorbent, yet single ferrite density is bigger, makes that absorbing material is difficult to satisfy that absorption band is wide, the requirement of light weight, thin thickness, and cost is higher.The carbonyl iron dust absorbing property is stable, and at low-frequency range wave absorbing efficiency height, but density is bigger, and is easily aging.Cenosphere, pearlstone are novel wave-absorbing materials, have characteristics such as light weight, porous, cheapness, and hollow medium has insulation effect simultaneously.This project studies show that carbonyl iron dust low-frequency range absorbing property is better, ferrite Mid Frequency absorbing property is better, hollow medium high band absorbing property is better, the three inhales the ripple frequency range in compound back and widens, and have the characteristic that density is low, cost is low, preparation coating has good fluidity and volume stability.Porous medium has certain heat-insulating property concurrently in addition.Therefore, prepared composite wave-absorbing powder is a kind of promising absorbing material.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high-performance composite wave-absorbing powder.
The preparation method of the high-performance wave-absorbing composite powder that the present invention proposes is to be raw material with metal nitrate, citric acid, porous medium, prepares ferrite-porous medium composite granule, mixes the composite granule that obtains high absorbing property again with carbonyl iron dust.Concrete steps are as follows:
(1) with metal nitrate, iron nitrate, citric acid, add dissolved in distilled water respectively, be mixed with into presoma then, splash into ammonia soln regulator solution pH value again to neutral, solution places 70 ℃～90 ℃ stirred in water bath even, and when metal nitrate was nitrate of baryta, strontium nitrate, the stoichiometric ratio of metal nitrate, iron nitrate and citric acid was 1: 12: 19, when metal nitrate was Xiao Suangu, nickelous nitrate, the stoichiometric ratio of metal nitrate, iron nitrate and citric acid was 1: 2: 4;
(2) in the presoma of step (1) stirring in water bath, add porous medium, properties-correcting agent, be stirred to the thickness colloidal, wherein ferrite theoretical value and properties-correcting agent mass ratio are 1: 0.1～1: 0.05, and ferrite theoretical value and porous medium mass ratio are 1: 0.2～1: 5;
(3) gained colloid in the step (2) being put into baking oven dried by the fire under 115-125 ℃ of temperature 7.5 hours-8.5 hours, obtain the exsiccant gel, gel placed in the retort furnace calcine, slowly be warming up to 850 ℃, behind insulation 1h～2h, naturally cooling promptly gets ferrite-porous medium composite granule, and this ferrite-porous medium composite granule and carbonyl iron dust are mixed, and promptly gets desired product; Wherein ferrite-porous medium composite granule and carbonyl iron dust mass ratio are 1: 0.2～1: 5.
Among the present invention, metal nitrate described in the step (1) is an one to multiple kind in nitrate of baryta, strontium nitrate, Xiao Suangu or the nickelous nitrate.
Among the present invention, properties-correcting agent described in the step (2) be in ethylene glycol or the polyoxyethylene glycol any; Described porous medium is 60 orders, 150 orders, 300 orders, 800 orders or 1250 order cenospheres, or in perforate pearlstone or the closed-cell expanded perlite any.
Utilize the present invention to obtain wave-absorbing powder to have that absorbing property is good, product homogeneous, density are low, cheap, insulation, easily dispose characteristics such as coating, the preparation that can be used for building antiradar coatings.
Beneficial effect of the present invention
1. utilizing the present invention to obtain wave-absorbing powder is raw material with nitrate, porous medium, carbonyl iron dust, and by dissolving, water-bath, stirring, the preparation of incinerating process, production method is simple and easy to do.The porous medium cost that mixes is low, has significantly reduced expensive ferrite, the consumption of carbonyl iron dust.
2. utilize the present invention to obtain wave-absorbing powder, make properties-correcting agent, significantly improved the covered effect of ferrite, thereby improved the absorbing property of composite granule to a certain extent on the porous medium surface with ethylene glycol, polyoxyethylene glycol.
3. utilize the present invention to obtain wave-absorbing powder, calcination process has been owing to adopted stage to burn slowly, the ferrite purity height of preparing, and impurity is few.
4. utilize the present invention to obtain wave-absorbing powder, the carbonyl iron dust that mixes can change the main suction ripple frequency range of composite granule, thereby is applied to the needs of different-waveband, has more practical value.
Embodiment
Further specify the present invention below by embodiment.
Embodiment 1
Take by weighing nitrate of baryta 2.6134g, iron nitrate 48.48g, citric acid 54.6364g, add dissolved in distilled water respectively and mix then, splash into ammonia soln regulator solution pH value to 7 again.Solution places 90 ℃ of stirred in water bath, adds 800 order cenosphere 22.231g and 1.1116g ethylene glycol in the whipping process.Stirred solution is put into 120 ℃ of bakings of baking oven 8h then to the thickness colloidal, obtains desiccant gel.Gel placed in the retort furnace calcine, temperature increasing schedule is 100 ℃/h for 100 ℃～400 ℃; 400 ℃～610 ℃ is 30 ℃/h; 610 ℃～850 ℃ is 50 ℃/h.Naturally slowly cool off behind the insulation 1h and promptly get the ferrite composite granule.Promptly get desired product after this composite granule and 33.34g carbonyl iron dust mixed.Waveguide method detects this product can reach 10dB at 812GHz frequency range suction ripple, inhales the ripple major part greater than 10dB in the 13-18GHz frequency range.And absorption peak is more.
Embodiment 2
Take by weighing strontium nitrate 2.163g, iron nitrate 48.48, citric acid 54.6364g, add dissolved in distilled water respectively and mix then, splash into ammonia soln regulator solution pH value to 7 again.Solution places 90 ℃ of stirred in water bath, adds 1250 order cenosphere 55.5765g and polyoxyethylene glycol 0.0058g in the whipping process.Stirred solution is put into 120 ℃ of bakings of baking oven 8h then to the thickness colloidal, obtains desiccant gel.Gel placed in the retort furnace calcine, be incubated 2h after 60 ℃ of temperature increasing schedules/h to 850 ℃, slowly cooling promptly gets the ferrite composite granule naturally.Promptly get desired product after this composite granule and 50g carbonyl iron dust mixed.Waveguide method detects this product can reach 10dB at 8-12GHz frequency range suction ripple, inhales the ripple major part greater than 10dB in the 13-18GHz frequency range.And absorption peak is more.
Embodiment 3
Take by weighing Xiao Suangu 8.7309g, nitric acid 24.2712g, citric acid 25.2126g, add dissolved in distilled water respectively and mix then, splash into ammonia soln regulator solution pH value to 7 again.Solution places 80 ℃ of stirred in water bath, adds closed-cell expanded perlite 3g and polyoxyethylene glycol 0.6g in the whipping process.Stirred solution is put into 120 ℃ of bakings of baking oven 8h then to the thickness colloidal, obtains desiccant gel.Gel placed in the retort furnace calcine, be incubated 2h after 60 ℃ of temperature increasing schedules/h to 850 ℃, slowly cooling promptly gets the ferrite composite granule naturally.Promptly get desired product after this composite granule and 2g carbonyl iron dust mixed.Waveguide method detects this product can reach 10dB at 8-12GHz frequency range suction ripple, inhales the ripple major part greater than 10dB in the 13-18GHz frequency range.And absorption peak is more.
Embodiment 4
Take by weighing nickelous nitrate 2.908g, iron nitrate 8.08g, citric acid 8.4056g, add dissolved in distilled water respectively and mix then, splash into ammonia soln regulator solution pH value to 7 again.Solution places 80 ℃ of stirred in water bath, adds 60 order cenosphere 0.5g and ethylene glycol 0.25g in the whipping process.Stirred solution is put into 120 ℃ of bakings of baking oven 8h then to the thickness colloidal, obtains desiccant gel.Gel placed in the retort furnace calcine, temperature increasing schedule is 100 ℃/h for 100 ℃～400 ℃; 400 ℃～610 ℃ is 30 ℃/h; 610 ℃～850 ℃ is 50 ℃/h, insulation 2h, and slowly cooling promptly gets the ferrite composite granule naturally.Promptly get desired product after this composite granule and 10g carbonyl iron dust mixed.Waveguide method detects this product can reach 10dB at 8-12GHz frequency range suction ripple, inhales the ripple major part greater than 10dB in the 13-18GHz frequency range.And absorption peak is more.
Embodiment 5
Get nitrate of baryta 2.6134g, Xiao Suangu 8.7309g, iron nitrate 72.7512g, citric acid 134.4854g, add dissolved in distilled water respectively and mix then, splash into ammonia soln regulator solution pH value to 7 again.Solution places 90 ℃ of stirred in water bath, adds 150 order cenosphere 25g and ethylene glycol 2g in the whipping process.Stirred solution is put into 120 ℃ of bakings of baking oven 8h then to the thickness colloidal, obtains desiccant gel.Gel placed in the retort furnace calcine, slowly cool off naturally behind 60 ℃/h to 850 of the temperature increasing schedule ℃ insulation 1h and promptly get the ferrite composite granule.Promptly get desired product after this composite granule and 30g carbonyl iron dust mixed.Waveguide method detects this product can reach 10dB at 8-12GHz frequency range suction ripple, inhales the ripple major part greater than 10dB in the 13-18GHz frequency range.And absorption peak is more.
Claims (2)
1. the preparation method of a high-performance wave-absorbing composite powder is characterized in that concrete steps are as follows:
(1) with metal nitrate, iron nitrate, citric acid, add dissolved in distilled water respectively, be mixed with into presoma then; Splash into ammonia soln regulator solution pH value again to neutral; Solution places 70 ℃～90 ℃ stirred in water bath even; When metal nitrate is nitrate of baryta, strontium nitrate, the stoichiometric ratio of metal nitrate, iron nitrate and citric acid is 1: 12: 19, when metal nitrate was Xiao Suangu, nickelous nitrate, the stoichiometric ratio of metal nitrate, iron nitrate and citric acid was 1: 2: 4;
(2) in the presoma of step (1) stirring in water bath, add porous medium, properties-correcting agent, be stirred to the thickness colloidal; Wherein ferrite theoretical value and properties-correcting agent mass ratio are 1: 0.1～1: 0.05, and ferrite theoretical value and porous medium mass ratio are 1: 0.2～1: 5;
(3) gained colloid in the step (2) is put into baking oven 115-125 ℃ of baking 7.5 hours-8.5 hours, obtained the exsiccant gel; Gel placed in the retort furnace calcine, be warming up to 850 ℃, insulation 1h～2h, naturally cooling promptly gets ferrite-porous medium composite granule; This ferrite-porous medium composite granule and carbonyl iron dust are mixed, promptly get desired product; Wherein ferrite-porous medium composite granule and carbonyl iron dust mass ratio are 1: 0.2～1: 5.
2, the preparation method of high-performance wave-absorbing composite powder according to claim 1, it is characterized in that properties-correcting agent described in the step (2) be in ethylene glycol or the polyoxyethylene glycol any; Described porous medium be in 60 orders, 150 orders, 300 orders, 800 orders or 1250 order cenospheres or perforate pearlstone or the closed-cell expanded perlite any.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103131384A (en) * | 2013-02-28 | 2013-06-05 | 湖南大学 | Nanometer composite wave absorbing powder having low density and porous structure, and its preparation method |
| CN103193473A (en) * | 2013-04-19 | 2013-07-10 | 华东理工大学 | Preparation method of microwave absorbing material with three-dimensional ordered macroporous structure |
| CN106399968A (en) * | 2016-08-15 | 2017-02-15 | 武汉艾特米克超能新材料科技有限公司 | Preparation method for oxide ceramic coating on surface of wave-absorbing material powder |
| CN106519816A (en) * | 2016-10-08 | 2017-03-22 | 江苏大使同丰涂料有限公司 | Paint for absorbing electromagnetic wave and preparation method and application thereof |
| CN107721175A (en) * | 2017-11-27 | 2018-02-23 | 侯景颢 | A kind of heat-insulated pottery glaze and its enameling method |
| CN107935635A (en) * | 2017-11-27 | 2018-04-20 | 侯景颢 | A kind of preparation method of pottery lamp part |
| WO2018177177A1 (en) * | 2017-03-31 | 2018-10-04 | 深圳光启高等理工研究院 | Method for preparing wave-absorbing material, and wave-absorbing coating |
| CN110591641A (en) * | 2019-01-25 | 2019-12-20 | 陕西科技大学 | Fe2O3@ MXene composite powder and preparation method thereof |
| CN110940177A (en) * | 2019-11-28 | 2020-03-31 | 深圳市德方纳米科技股份有限公司 | Colloid drying equipment and method |
| CN111117565A (en) * | 2019-12-31 | 2020-05-08 | 天长市中德电子有限公司 | Preparation method of wave-absorbing ferrite composite material |
| CN112744870A (en) * | 2019-10-30 | 2021-05-04 | 洛阳尖端技术研究院 | Aluminum oxide-carbonyl iron microsphere wave absorbing agent and preparation method thereof |
| CN115957764A (en) * | 2023-01-13 | 2023-04-14 | 成都理工大学 | Nickel-doped barium ferrite catalyst for autothermal reforming of acetic acid to produce hydrogen |
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2009
- 2009-09-24 CN CN200910196314A patent/CN101665635A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131384B (en) * | 2013-02-28 | 2014-06-04 | 湖南大学 | Nanometer composite wave absorbing powder having low density and porous structure, and its preparation method |
| CN103131384A (en) * | 2013-02-28 | 2013-06-05 | 湖南大学 | Nanometer composite wave absorbing powder having low density and porous structure, and its preparation method |
| CN103193473A (en) * | 2013-04-19 | 2013-07-10 | 华东理工大学 | Preparation method of microwave absorbing material with three-dimensional ordered macroporous structure |
| CN106399968A (en) * | 2016-08-15 | 2017-02-15 | 武汉艾特米克超能新材料科技有限公司 | Preparation method for oxide ceramic coating on surface of wave-absorbing material powder |
| CN106399968B (en) * | 2016-08-15 | 2018-12-25 | 武汉艾特米克超能新材料科技有限公司 | A kind of preparation method of absorbing material powder surface oxide ceramic coating |
| CN106519816B (en) * | 2016-10-08 | 2018-09-11 | 江苏大使同丰涂料有限公司 | A kind of coating of electromagnetic wave absorption and preparation method thereof and purposes |
| CN106519816A (en) * | 2016-10-08 | 2017-03-22 | 江苏大使同丰涂料有限公司 | Paint for absorbing electromagnetic wave and preparation method and application thereof |
| WO2018177177A1 (en) * | 2017-03-31 | 2018-10-04 | 深圳光启高等理工研究院 | Method for preparing wave-absorbing material, and wave-absorbing coating |
| CN107935635A (en) * | 2017-11-27 | 2018-04-20 | 侯景颢 | A kind of preparation method of pottery lamp part |
| CN107721175A (en) * | 2017-11-27 | 2018-02-23 | 侯景颢 | A kind of heat-insulated pottery glaze and its enameling method |
| CN110591641A (en) * | 2019-01-25 | 2019-12-20 | 陕西科技大学 | Fe2O3@ MXene composite powder and preparation method thereof |
| CN112744870A (en) * | 2019-10-30 | 2021-05-04 | 洛阳尖端技术研究院 | Aluminum oxide-carbonyl iron microsphere wave absorbing agent and preparation method thereof |
| CN110940177A (en) * | 2019-11-28 | 2020-03-31 | 深圳市德方纳米科技股份有限公司 | Colloid drying equipment and method |
| CN111117565A (en) * | 2019-12-31 | 2020-05-08 | 天长市中德电子有限公司 | Preparation method of wave-absorbing ferrite composite material |
| CN115957764A (en) * | 2023-01-13 | 2023-04-14 | 成都理工大学 | Nickel-doped barium ferrite catalyst for autothermal reforming of acetic acid to produce hydrogen |
| CN115957764B (en) * | 2023-01-13 | 2024-02-27 | 成都理工大学 | Nickel-doped barium ferrite catalyst for autothermal reforming of acetic acid to produce hydrogen |
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Open date: 20100310 |