CN102745982B - Method for preparing nanometer arsenic trioxide (ATO)/nanometer ferrite composite wave absorbing material - Google Patents

Abstract

The invention discloses a method for preparing a nanometer arsenic trioxide (ATO)/nanometer ferrite composite wave absorbing material. The method comprises the following steps of: firstly, preparing nanometer ferrite BaMnMgAlxFe<16-x>O27, wherein x is more than or equal to 0 and is small than 1; secondary, adding the nanometer ferrite into a nanometer ATO aqueous solution to prepare a mixed seriflux, dispersing, washing and drying; and finally, roasting at a high temperature in an atmosphere of nitrogen, and thus obtaining the nanometer ATO/nanometer ferrite composite wave absorbing material.By adopting good electric conductivity and wave absorbing performance of nanometer ATO and combining the nanometer ATO with the nanometer ferrite wave absorbing material, the absorption performance of the material on electromagnetic wave can be improved.

Description

The preparation method of a kind of nano ATO/nanometer ferrite composite wave-suction material

Technical field

The present invention relates to a kind of absorbing material, particularly the preparation method of a kind of nano ATO/nanometer ferrite composite wave-suction material.

Background technology

Absorbing material is a kind of a kind of material that can absorb its surface electromagnetic wave of projection, the composite wave-suction material of light weight, wide-band and wave-absorbing, absorptive character and good thermal stability can be used in national defense construction, can make space base and continental rise equipment have " stealthy " and prominent anti-performance, simultaneously in civilian each field, as at microwave communication, microwave unreflected chamber, anti-electromagnetic-radiation and prevent that electromagnetic pollution etc. from also having good function.

The research of ferrite wave-absorbing material started from the beginning of last century, along with the development of high frequency radio new technology, pressed for the high material of ferromegnetism and resistivity.Patent CN 1800089A discloses a kind of preparation nanometer ferrite SrZnCoFe ₁₆O ₂₇The preparation method of powder, this powdered material absorbing property is better, but the frequency band that absorbs is too narrow, is not suitable for actual needs.Therefore be necessary in single ferrite micropowder, to add some additives and carry out composite modifiedly, make that the electromagnetic parameter of absorbing material can be mated preferably.Patent CN 1807537A discloses a kind of composite wave-suction material that the in-situ deposition method makes of using, though this composite wave-suction material absorption band is wideer, and complex manufacturing, production cost is big.

Summary of the invention

The present invention provides the preparation method of a kind of nano ATO/nanometer ferrite composite wave-suction material in order to solve the narrow problem of absorption band that exists in the background technology.

In order to realize purpose of the present invention, the present invention by the following technical solutions: the preparation method of a kind of nano ATO/nanometer ferrite composite wave-suction material, at first adopt coprecipitation method to prepare nanometer ferrite BaMnMgAl _xFe _16-xO ₂₇(0≤x＜1) joins this nanometer ferrite in the nano ATO aqueous solution then and makes mixed serum, and disperses, washs and drying, and high-temperature roasting under nitrogen atmosphere at last makes nano ATO/nanometer ferrite composite wave-suction material.

Characterization step of the present invention is as follows:

(1) adopts coprecipitation method, at first with raw material BaCl ₂2H ₂O, FeCl ₃6H ₂O, MnCl ₂2H ₂O, AlCl ₃And MgCl ₂6H ₂O puts into by the molecular formula stoichiometric ratio NaOH and Na is housed ₂CO ₃In the solution, n (BaCl wherein ₂2H ₂O): n (MnCl ₂2H ₂O): n (MgCl ₂6H ₂O): n (AlCl ₃): n (FeCl ₃6H ₂O): n (NaOH): n (Na ₂CO ₃)=1: 1: 1: x: 16-x: 40: 9, be made into mixing solutions, staticly settle, it is carried out heated and stirred half hour, and Heating temperature is 60 ℃, and to regulate pH with the HCl solution of concentration 10% be neutral, to precipitate washing and filtration again, make nanometer ferrite BaMnMgAl _xFe _16-xO ₂₇(0≤x＜1);

(2) in the deionized water of 50ml, add prepared nanometer ferrite BaMnMgAl in nano ATO powder and the step (1) _xFe _16-xO ₂₇(0≤x＜1), wherein nanometer ferrite BaMnMgAl _xFe _16-xO ₂₇The Theoretical Mass of (0≤x＜1) is 1: 1 with the ratio of nano ATO powder quality, and to its ultra-sonic dispersion, puts into 80～100 ℃ of oven for drying after half an hour;

(3) nanometer powder after the oven dry is carried out high-temperature calcination: under the protection of nitrogen atmosphere, be heated to 270 ℃ from room temperature, temperature rise rate is 4 ℃/min, and keeps 270 ℃ of half an hour; Be heated to 500 ℃ from 270 ℃, temperature rise rate is 6 ℃/min, and keep 500 ℃ 1 hour; Be heated to 1000 ℃ from 500 ℃, temperature rise rate is 2 ℃/min, keep 1000 ℃ 1 hour, at last under nitrogen protection with the stove cooling, make nano ATO/nanometer ferrite composite wave-suction material.

Advantage of the present invention:

1. because nano ATO has good conductivity, under the hertzian wave effect, the nano ATO of conduction will produce eddy current, the ferrite of magnetic conduction then produces magnetic loss, the two recombination energy is had matrix material than maelstrom loss and magnetic loss simultaneously, thereby improve material to the absorption of electromagnetic wave performance, and nano ATO itself just has the function that absorbs microwave, so it is compound that the present invention adopts nano ATO and nanometer ferrite material to carry out, can improve material to the absorption of electromagnetic wave performance.

2. use coprecipitation method to prepare nanometer ferrite, can obtain good dispersity, the uniform crystal grain of particle diameter after the drying.

3. preparation technology of the present invention is simple, and what the calcining manners of absorbing material was adopted is interim calcining, and the matrix material purity that makes is higher, and impurity is few.

Description of drawings

Fig. 1 is preparation technology's schema of nano ATO/nanometer ferrite composite wave-suction material.

Embodiment

Embodiment 1

(1) x is 0, and the nanometer ferrite molecular formula is BaMnMgFe ₁₆O ₂₇At first by the molecular formula stoichiometric ratio respectively with the BaCl of 0.005mol ₂2H ₂The FeCl of O, 0.08mol ₃6H ₂The MnCl of O, 0.005mol ₂2H ₂The MgCl of O and 0.005mol ₂6H ₂O puts into the NaOH that 0.2mol is housed, the Na of 0.045mol ₂CO ₃In the solution of 150mL deionized water, stir and be made into mixing solutions, after staticly settling, it is 60 ℃ of water bath with thermostatic control heated and stirred half hours that beaker is put into temperature, and to regulate pH with the HCl solution of concentration 10% be neutral, will precipitate and wash and filtration.

(2) in the deionized water of 50ml, add the precipitation nanometer W type ferrite after the filtration in the 7.72 nano ATO powder that restrain and the first step, nanometer ferrite BaMnMgFe ₁₆O ₂₇The ratio of Theoretical Mass and nano ATO quality be 1: 1, and to its ultra-sonic dispersion, put into 80 ℃ of oven for drying after half an hour.

(3) nanometer powder after the oven dry is carried out high-temperature calcination: under the protection of nitrogen atmosphere, from room temperature to 270 ℃, temperature rise rate is 4 ℃/min, and keeps half an hour at 270 ℃; From 270 ℃ to 500 ℃, temperature rise rate is 6 ℃/min, and keeps 1 hour at 500 ℃; From 500 ℃ to 1000 ℃, temperature rise rate is 2 ℃/min, keeps 1 hour at 1000 ℃, lowers the temperature with stove under the nitrogen atmosphere protection at last.

Embodiment 2

(1) x is 0.2, and the nanometer ferrite molecular formula is BaMnMgAl _0.2Fe _15.8O ₂₇At first by the molecular formula stoichiometric ratio respectively with the BaCl of 0.005mol ₂2H ₂The FeCl of O, 0.079mol ₃6H ₂The MnCl of O, 0.005mol ₂2H ₂The MgCl of O, 0.005mol ₂6H ₂The AlCl of O and 0.001mol ₃Put into the NaOH that 0.2mol is housed, the Na of 0.045mol ₂CO ₃In the solution of 150mL deionized water, stir and be made into mixing solutions, after staticly settling, it is 60 ℃ of water bath with thermostatic control heated and stirred half hours that beaker is put into temperature, and to regulate pH with the HCl solution of concentration 10% be neutral, will precipitate and wash and filtration.

(2) in the deionized water of 50ml, add the precipitation nanometer ferrite after the filtration in the 7.69 nano ATO powder that restrain and the first step, nanometer ferrite BaMnMgAl _0.2Fe _15.8O ₂₇The ratio of Theoretical Mass and nano ATO quality be 1: 1, and to its ultra-sonic dispersion, put into 100 ℃ of oven for drying after half an hour.

(3) nanometer powder after the oven dry is carried out high-temperature calcination: under the protection of nitrogen atmosphere, from room temperature to 270 ℃, temperature rise rate is 4 ℃/min, and keeps half an hour at 270 ℃; From 270 ℃ to 500 ℃, temperature rise rate is 6 ℃/min, and keeps 1 hour at 500 ℃; From 500 ℃ to 1000 ℃, temperature rise rate is 2 ℃/min, keeps 1 hour at 1000 ℃, lowers the temperature with stove under the nitrogen atmosphere protection at last.

Embodiment 3

(1) x is 0.4, and the nanometer ferrite molecular formula is BaMnMgAl _0.4Fe _15.6O ₂₇At first by the molecular formula stoichiometric ratio respectively with the BaCl of 0.005mol ₂2H ₂The FeCl of O, 0.078mol ₃6H ₂The MnCl of O, 0.005mol ₂2H ₂The MgCl of O, 0.005mol ₂6H ₂The AlCl of O and 0.002mol ₃Put into the NaOH that 0.2mol is housed, the Na of 0.045mol ₂CO ₃In the solution of 150mL deionized water, stir and be made into mixing solutions, after staticly settling, it is 60 ℃ of water bath with thermostatic control heated and stirred half hours that beaker is put into temperature, and to regulate pH with the HCl solution of concentration 10% be neutral, will precipitate and wash and filtration.

(2) in the deionized water of 50ml, add the precipitation nanometer ferrite after the filtration in the 7.66 nano ATO powder that restrain and the first step, nanometer ferrite BaMnMgAl _0.4Fe _15.6O ₂₇The ratio of Theoretical Mass and nano ATO quality be 1: 1, and to its ultra-sonic dispersion, put into 100 ℃ of oven for drying after half an hour.

(3) nanometer powder after the oven dry is carried out high-temperature calcination: under the protection of nitrogen atmosphere, from room temperature to 270 ℃, temperature rise rate is 4 ℃/min, and keeps half an hour at 270 ℃; From 270 ℃ to 500 ℃, temperature rise rate is 6 ℃/min, and keeps 1 hour at 500 ℃; From 500 ℃ to 1000 ℃, temperature rise rate is 2 ℃/min, keeps 1 hour at 1000 ℃, lowers the temperature with stove under the nitrogen atmosphere protection at last.

Claims (2)

1. the preparation method of nano ATO/nanometer ferrite composite wave-suction material is characterized in that preparation process is as follows:

(1) adopts coprecipitation method, at first with raw material BaCl ₂2H ₂O, FeCl ₃6H ₂O, MnCl ₂2H ₂O, AlCl ₃And MgCl ₂6H ₂O puts into by the molecular formula stoichiometric ratio NaOH and Na is housed ₂CO ₃In the solution, n (BaCl wherein ₂2H ₂O): n (MnCl ₂2H ₂O): n (MgCl ₂6H ₂O): n (AlCl ₃): n (FeCl ₃6H ₂O): n (NaOH): n (Na ₂CO ₃)=1:1:1:x:16-x:40:9 is made into mixing solutions, staticly settles, it is carried out heated and stirred half hour, and Heating temperature is 60 ℃, and to regulate pH with the HCl solution of concentration 10% be neutral, to precipitate washing and filtration again, make nanometer ferrite BaMnMgAl _xFe _16-xO ₂₇, 0≤x＜1;

(2) in the deionized water of 50mL, add prepared nanometer ferrite BaMnMgAl in nano ATO powder and the step (1) _xFe _16-xO ₂₇, 0≤x＜1, wherein nanometer ferrite BaMnMgAl _xFe _16-xO ₂₇, the Theoretical Mass of 0≤x＜1 is 1:1 with the ratio of nano ATO powder quality, and to its ultra-sonic dispersion, puts into 80～100 ℃ of oven for drying after half an hour;

(3) nanometer powder after the oven dry is carried out high-temperature calcination: under the protection of nitrogen atmosphere, be heated to 270 ℃ from room temperature, temperature rise rate is 4 ℃/min, and keeps 270 ℃ of half an hour; Be heated to 500 ℃ from 270 ℃, temperature rise rate is 6 ℃/min, and keep 500 ℃ 1 hour; Be heated to 1000 ℃ from 500 ℃, temperature rise rate is 2 ℃/min, keep 1000 ℃ 1 hour, at last under nitrogen protection with the stove cooling, make nano ATO/nanometer ferrite composite wave-suction material.

2. the preparation method of nano ATO according to claim 1/nanometer ferrite composite wave-suction material is characterized in that nanometer ferrite BaMnMgAl _xFe _16-xO ₂₇, 0≤x＜1, x gets 0,0.2 or 0.4 in the molecular formula.

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