CN103102867A - Metal ion doped barium ferrite wave absorbing powder and preparation method thereof - Google Patents
Metal ion doped barium ferrite wave absorbing powder and preparation method thereof Download PDFInfo
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- CN103102867A CN103102867A CN2013100258485A CN201310025848A CN103102867A CN 103102867 A CN103102867 A CN 103102867A CN 2013100258485 A CN2013100258485 A CN 2013100258485A CN 201310025848 A CN201310025848 A CN 201310025848A CN 103102867 A CN103102867 A CN 103102867A
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Abstract
The invention discloses a metal ion doped barium ferrite wave absorbing powder and a preparation method thereof. The metal ion doped in the barium ferrite wave absorbing powder is metal ion with above tetravalence, the barium ferrite is a single phase crystal, and the barium ferrite simultaneously comprises Fe<3+> and Fe<2+>. The wave absorbing material has good wave absorbing property (a double absorption peak appears in a frequency range of 26.5-40GHz, the bandwidth can reach 12GHz, and the maximum reflection loss can reach minus 45dB at an absorption peak), the barium ferrite powder material can be used in wave absorbing coatings, and has wide application in the field of electromagnetic shielding and hiding.
Description
Technical field
The present invention relates to a kind of barium ferrite absorbing material and preparation method thereof, belong to the absorbing material technical field.
Background technology
In recent years, along with the fast development of the electronic information technologies such as local area network, mobile telephone, satellite television, radar system, hertzian wave is ubiquitous, and its application and impact are also increasingly extensive.The problems such as the electromagnetic interference that is produced by various electronicss and Contamination of Electromagnetic Wave are having a strong impact on people's work and life.In order to improve anti-electromagnetic interference capability, electronics can be run well; In order to reduce electromagnetic radiation pollution, people are lived in healthy environment, the research of absorbing material has become the important component part of national economy technical field.And then in modern military defence field, the exploitation of absorbing material has also become the key content of various countries' military field engineering.As seen, no matter wave-absorbing coating material all has important Research Significance and using value in civil area or military field.
Absorption of electromagnetic wave ability and the material properties such as its dielectric, magnetic and resistivity of material are closely related.Ferrite Material also shows the medium of certain dielectric properties simultaneously as a kind of magnetic property with excellence, higher magnetic permeability is arranged under high frequency, and resistivity is also higher, can avoid the skin effect of metallic conductor, hertzian wave is easy to enter and is decayed fast, thereby is widely used in electromagnetic shielding and stealthy field.Studies show that hexagonal Ba-ferrite (BaFe
12O
19), because it has larger magnetocrystalline anisotropy field, high saturation magnetization, large coercive force, high resistivity and outstanding chemical stability, be the most potential class material of high frequency microwave Application Areas.
As absorbing material, magnetic coupling utmost point natural resonance phenomenon in the ferritic main magnetic loss mechanism of high frequency band, when electromagnetic frequency equals or during near the free precession frequency of ferrite magnetic moment, the natural resonance phenomenon occurs, cause the ferrite electromagnetic wave absorption energy of decaying consumingly.Yet, although material has strong absorption behavior for hertzian wave under resonant frequency, but generally its mechanism that resonates determines, thereby resonant frequency is single, also namely usually for single-material, though inhale under resonant frequency intensity of wave high effectively inhale the ripple frequency range narrower (inhale the ripple frequency range be often referred to inhale wave reflection loss RL<-range of frequency of 10dB), generally lower than 6GHz.In order to satisfy actual suction ripple frequency range requirement, usually need multiple material to coordinate and realize.If can break through the difficult point that realizes that in a kind of material broadband absorbs, obviously have great importance for practical, the cost degradation of absorbing material and simplification preparation technology etc.
Research finds, for some high-valence cationics (as Ti
4+, Zr
4+, Nb
5+), when it to the Fe in barium ferrite
3+When replacing, system own is in order to keep electric neutrality, wherein the Fe of high price
3+Can correspondingly be transformed into Fe at a low price
2+Due to adjacent Fe
3+And Fe
2+Between the superexchange coupling, its coupling magnetic moment free precession frequency can be higher than Fe
3+The precession frequency of magnetic moment.Also namely, if suitably control this doping, can there be simultaneously two kinds of difference resonance mechanisms with different resonant frequencies in system, form the double resonance system of the non-single mechanism that resonates, the double resonance loss peak will occur like this.Because each resonance mechanism in this double resonance mechanism has separately resonant frequency, and has suitable frequency difference, if thereby can effectively use this double resonance phenomenon in absorbing material, this double resonance might cause and absorbs respectively and absorb synergistic effect to different frequency range is electromagnetic, thereby might reach the purpose that wideband absorbs.
Further, because best microwave penetrating window mouth appears at 8.0 ~ 1000.0mm, also namely in common alleged centimetric wave scope, at this moment transmitance approximately 100%.On the other hand, the millimeter wave radar wave beam is narrow, and angular resolution is high, bandwidth, and good concealment, immunity from interference is strong.These characteristics have promoted its widespread use at numerous areas.And the microwave in frequency is 26.5 ~ 40GHz scope, its not only had centimetric wave round-the-clock characteristics, but also the characteristics of the better imaging resolution of millimeter wave are arranged, had radar in many types of this wave band etc. to be applied in military field at present.Thereby, promote the exploitation of absorbing material corresponding to this wave band, will help it to be widely used in the specific ripple field of inhaling.
Greater than 40GHz, also namely less than 7.5mm, so need to control the natural resonant frequency of this material, make the frequency of its electromagnetic wave absorption in 26.5 ~ 40GHz frequency range due to the natural resonant frequency of barium ferrite itself.The research discovery, ferritic natural resonant frequency is proportional to the anisotropy field of material, and cation doping can change the anisotropy field of barium ferrite, and then change its natural resonant frequency.Obviously, utilize to change this concept of its natural resonant frequency, be expected to reach the purpose that changes absorbed hertzian wave frequency range.
Summary of the invention
The object of the present invention is to provide barium ferrite wave-absorbing powder of a kind of metal ion mixing with wide absorption of electromagnetic wave range of frequency and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is: the metal ion that adulterates in the barium ferrite wave-absorbing powder of metal ion mixing of the present invention is the above metal ion of tetravalence, and described barium ferrite is single-phase crystal, has simultaneously Fe in barium ferrite
3+And Fe
2+
Preferably, the metal ion that adulterates of the present invention is Ti
4+
Further, the metal ion and the Ba that adulterate of the present invention
2+Mol ratio be 0.6 ~ 0.8:1, Fe
3+And Fe
2+Total moles and Ba
2+The ratio of mole number be 11.2 ~ 11.4:1.
The preparation method of the barium ferrite wave-absorbing powder of metal ion mixing of the present invention comprises the steps:
1) nitrate of baryta, iron nitrate and citric acid are mixed 1:11.2 ~ 11.4:17.8 ~ 18.1 in molar ratio, add the deionized water and stirring dissolving to obtain the first solution; In described the first solution, the total mol concentration of nitrate of baryta and iron nitrate is 0.5 ~ 2.0mol/L;
2) tetrabutyl titanate is dissolved in obtains the second solution in dehydrated alcohol; In described the second solution, the volumetric molar concentration of tetrabutyl titanate is 1.0 ~ 2.0mol/L;
3) citric acid is joined obtain the 3rd solution in the second solution; In described the 3rd solution, the mol ratio of tetrabutyl titanate and citric acid is 1:1.0 ~ 2.0;
4) slowly join the 3rd solution in the first solution and stir and obtain the 4th solution; In the 4th solution, the mol ratio of tetrabutyl titanate and nitrate of baryta is 6 ~ 8:10;
5) the 4th solution is heated and concentrates obtain colloidal sol, then the colloidal sol drying is obtained xerogel;
6) with xerogel perfect combustion, then with products of combustion at 800 ~ 950 ℃ of insulation 1.0 ~ 3.0h, and be rapidly heated 1100 ℃ ~ 1300 ℃ with the speed of 30 ~ 40 ℃/min and be incubated 1 ~ 3h.
Compare with background technology, the beneficial effect that the present invention has is: the present invention is by the above metal ion of comprehensive tetravalence (Ti for example
4+) control metal ion mixing (as titanium doped) and oxygen vacancy defect, efficiently realize double resonance loss mechanism in barium ferrite absorbing material system, hertzian wave is produced bimodal absorption, has good absorbing property, suction ripple frequency band is controlled in 26.5 ~ 40GHz range of frequency, maximum Effective frequency width of absorption approximately 12GHz(frequency range can improve 2 ~ 3 times), the best reflection loss RL in CF place value approximately-45dB.Wave-absorbing powder material preparation technique of the present invention is simple, with low cost.The barium ferrite wave-absorbing powder of metal ion mixing of the present invention can be used for preparing microwave absorbing coating, is expected to be used widely at electromagnetic wave shielding and stealthy field.
Description of drawings
Fig. 1 is the wave-absorbing powder material B aFe that embodiment 1 obtains
11.4Ti
0.6O
19XRD figure;
Fig. 2 is the wave-absorbing powder material B aFe that embodiment 1 obtains
11.4Ti
0.6O
19Absorbing property with the variation relation curve of frequency;
Fig. 3 is the wave-absorbing powder material B aFe that embodiment 2 obtains
11.3Ti
0.7O
19XRD figure;
Fig. 4 is the wave-absorbing powder material B aFe that embodiment 2 obtains
11.3Ti
0.7O
19Absorbing property with the variation relation curve of frequency;
Fig. 5 is the wave-absorbing powder material B aFe that embodiment 3 obtains
11.2Ti
0.8O
19XRD figure;
Fig. 6 is the wave-absorbing powder material B aFe that embodiment 3 obtains
11.2Ti
0.8O
19Absorbing property with the variation relation curve of frequency.
Embodiment
The metal ion that adulterates in the barium ferrite wave-absorbing powder of metal ion mixing of the present invention is the above metal ion of tetravalence, and wherein, barium ferrite is single-phase crystal, has simultaneously Fe in barium ferrite
3+And Fe
2+As the preferred embodiment of the present invention, the metal ion that adulterates is Ti
4+Preferably, the metal ion that adulterates and Ba
2+Mol ratio be 0.6 ~ 0.8:1, Fe
3+And Fe
2+Total moles and Ba
2+The ratio of mole number be 11.2 ~ 11.4:1.
Below further illustrate the present invention with specific embodiment.
In fact, for the xerogel of titanium doped barium ferrite, when descending at a lower temperature sintering, more Ti easily mixes the required doped barium ferrite of formation in barium ferrite, but easily produces α-Fe in system
2O
3Dephasign; And under comparatively high temps during sintering, Ti easily forms another kind of titaniferous dephasign (Ba simultaneously when forming the doped barium ferrite
6Fe
45Ti
17O
106).The former forms α-Fe because Fe is consumed in
2O
3Dephasign has reduced Fe
3+Change Fe into
2+Amount, be unfavorable for controlling and Fe
2+The formation of relevant resonance mechanism realizes that the double resonance peak absorbs thereby be an impediment to; Latter due to the content that has reduced titanium doped barium ferrite and decrease the relative Ti content in the system, suppressed the ability of modulation barium ferrite to the frequency range of absorption of electromagnetic wave, namely be difficult to reach the purpose that reduces resonant frequency, be unfavorable for too efficiently realizing double resonance peak absorption.Thereby the present invention descends sintering to guarantee having enough titanium doped (Ti in material at lesser temps (800 ~ 950 ℃)
4+And Ba
2+Mol ratio when being 0.6 ~ 0.8:1), then decompose established low-temperature phase α-Fe comparatively high temps (1100 ~ 1300 ℃) is lower
2O
3, reach and both realize having in barium ferrite enough titanium doped, eliminate again α-Fe
2O
3Phase, and suppress simultaneously dephasign Ba
6Fe
45Ti
17O
106The purpose that produces.Further, the at high temperature thermal treatment through certain hour also helps the oxygen vacancy defect that increases in material, is conducive to promote better Fe
3+Change Fe into
2+Thereby, strengthen and Fe
2+The formation of relevant resonance mechanism.Clearly, this high performance material is formed, what also namely guarantee Ti effectively mixes effective generation with double resonance mechanism, and it is crucial controlling and forming technique.
Embodiment 1:
1) with the 1:11.4:18.1 mixing in molar ratio of nitrate of baryta, iron nitrate and citric acid, add the deionized water and stirring dissolving to obtain the first solution; In described the first solution, nitrate of baryta and iron nitrate total mol concentration are 2.0mol/L;
2) tetrabutyl titanate is dissolved in obtains the second solution in dehydrated alcohol; In described the second solution, the volumetric molar concentration of tetrabutyl titanate is 1.0mol/L;
3) citric acid is joined obtain the 3rd solution in the second solution; In described the 3rd solution, the mol ratio 1:1.5 of tetrabutyl titanate and citric acid;
4) slowly join the 3rd solution in the first solution and stir and obtain the 4th solution; In the 4th solution, the mol ratio of tetrabutyl titanate and nitrate of baryta is 3:5;
5) the 4th solution is heated and concentrates obtain colloidal sol, then the colloidal sol drying is obtained the puffy xerogel;
6) with the perfect combustion of puffy xerogel, then with products of combustion at 800 ℃ of insulation 3.0h, and be rapidly heated 1100 ℃ with the speed of 40 ℃/min, being incubated the mol ratio that 3h obtains titanium and barium is the titanium doped barium ferrite (BaFe of 0.6:1
11.4Ti
0.6O
19) absorbing material.
The titanium doped barium ferrite wave-absorbing powder material that the present embodiment is obtained and solid paraffin 8:3 in mass ratio evenly mix, and then mixture are incubated 1 ~ 2h at 80 ~ 90 ℃, paraffin is melted fully obtain molten mixture.This molten mixture is inserted in the thick red copper mould rectangle hole slot of 2.8mm, made the stopping composition consolidation, surfacing.Utilize specific inductivity, magnetic permeability and the absorbing property of the titanium doped barium ferrite absorbing material of Agilent vector network analyzer E8363C test.
Fig. 1 is the XRD figure spectrum of the titanium doped barium ferrite wave-absorbing powder of the present embodiment acquisition, can see, material has only formed the single-phase crystal of barium ferrite.Fig. 2 is the absorbing property of the titanium doped barium ferrite wave-absorbing powder material that obtains of the present embodiment and the relation curve of frequency.Can see, in 26.5 ~ 40GHz range of frequency, an absorption peak has respectively appearred in 29.3GHz and 38.9GHz place, has formed double resonance loss mechanism in visible titanium doped barium ferrite powder, shows Fe
3+And Fe
2+Exist simultaneously; In addition, effectively inhale the ripple frequency range (be RL<-10dB) about 11.8GHz, best at the absorbing property at 29.3GHz place, approach-45.8dB.
Embodiment 2:
1) with the 1:11.3:17.95 mixing in molar ratio of nitrate of baryta, iron nitrate and citric acid, add the deionized water and stirring dissolving to obtain the first solution; In described the first solution, nitrate of baryta and the volumetric molar concentration of iron nitrate total amount in this solution are 1.0mol/L;
2) tetrabutyl titanate is dissolved in obtains the second solution in dehydrated alcohol; In described the second solution, the volumetric molar concentration of tetrabutyl titanate in this solution is 1.5mol/L;
3) citric acid is joined obtain the 3rd solution in the second solution; In described the 3rd solution, the mol ratio of tetrabutyl titanate and citric acid is 1:1.0;
4) slowly join the 3rd solution in the first solution and stir and obtain the 4th solution; In the 4th solution, the mol ratio of tetrabutyl titanate and nitrate of baryta is 7:10;
5) the 4th solution is heated and concentrates obtain colloidal sol, then the colloidal sol drying is obtained the puffy xerogel;
6) with the perfect combustion of puffy xerogel, then with products of combustion at 900 ℃ of insulation 2.0h, and be rapidly heated 1200 ℃ ℃ with the speed of 40 ℃/min, being incubated the mol ratio that 2h obtains titanium and barium is the titanium doped barium ferrite (BaFe of 0.7:1
11.3Ti
0.7O
19) absorbing material.
The titanium doped barium ferrite wave-absorbing powder material that the present embodiment is obtained and solid paraffin 8:3 in mass ratio evenly mix, and then mixture are incubated 1 ~ 2h at 80 ~ 90 ℃, paraffin is melted fully obtain molten mixture.This molten mixture is inserted in the thick red copper mould rectangle hole slot of 2.9mm, made the stopping composition consolidation, surfacing.Utilize specific inductivity, magnetic permeability and the absorbing property of the titanium doped barium ferrite absorbing material of Agilent vector network analyzer E8363C test.
Fig. 3 is the XRD figure spectrum of the titanium doped barium ferrite wave-absorbing powder of the present embodiment acquisition, can see, material has only formed the single-phase crystal of barium ferrite.Fig. 4 is the absorbing property of the titanium doped barium ferrite wave-absorbing powder material that obtains of the present embodiment and the relation curve of frequency.Can see, in 26.5 ~ 40GHz range of frequency, an absorption peak has respectively appearred in 28.8GHz and 38.5GHz place, has formed double resonance loss mechanism in visible titanium doped barium ferrite powder, shows Fe
3+And Fe
2+Exist simultaneously; In addition, effectively inhale the ripple frequency range (be RL<-10dB) about 11.8GHz, best at the absorbing property at 28.8GHz place, approach-45.0dB.
Embodiment 3:
1) with the 1:11.2:17.8 mixing in molar ratio of nitrate of baryta, iron nitrate and citric acid, add the deionized water and stirring dissolving to obtain the first solution; In described the first solution, nitrate of baryta and the volumetric molar concentration of iron nitrate total amount in this solution are 0.5mol/L;
2) tetrabutyl titanate is dissolved in obtains the second solution in dehydrated alcohol; In described the second solution, the volumetric molar concentration of tetrabutyl titanate in this solution is 2.0mol/L;
3) citric acid is joined obtain the 3rd solution in the second solution; In described the 3rd solution, the mol ratio of tetrabutyl titanate and citric acid is 1:2.0;
4) slowly join the 3rd solution in the first solution and stir and obtain the 4th solution; In the 4th solution, the mol ratio of tetrabutyl titanate and nitrate of baryta is 4: 5;
5) the 4th solution is heated and concentrates obtain colloidal sol, then the colloidal sol drying is obtained the puffy xerogel;
6) with the perfect combustion of puffy xerogel, then with products of combustion at 950 ℃ of insulation 1.0h, and be rapidly heated 1300 ℃ ℃ with the speed of 30 ℃/min, be incubated mol ratio that 1h obtains titanium and barium and be 0.8 titanium doped barium ferrite (BaFe
11.2Ti
0.8O
19) the powder absorbing material.
The titanium doped barium ferrite wave-absorbing powder material that the present embodiment is obtained and solid paraffin 8:3 in mass ratio evenly mix, and then mixture are incubated 1 ~ 2h at 80 ~ 90 ℃, paraffin is melted fully obtain molten mixture.This molten mixture is inserted in the thick red copper mould rectangle hole slot of 2.74mm, made the stopping composition consolidation, surfacing.Utilize specific inductivity, magnetic permeability and the absorbing property of the titanium doped barium ferrite absorbing material of Agilent vector network analyzer E8363C test.
The XRD figure spectrum of the titanium doped barium ferrite wave-absorbing powder that Fig. 5 the present embodiment obtains can see that material has only formed the single-phase crystal of barium ferrite.Fig. 6 is the absorbing property of the titanium doped barium ferrite wave-absorbing powder material that obtains of the present embodiment and the relation curve of frequency.Can see, in 26.5 ~ 40GHz range of frequency, an absorption peak has respectively appearred in 28.4GHz and 39.0GHz place, has formed double resonance loss mechanism in visible titanium doped barium ferrite powder, shows Fe
3+And Fe
2+Exist simultaneously; In addition, effectively inhale the ripple frequency range (be RL<-10dB) about 12.2GHz, best at the absorbing property at 28.4GHz place, approach-43.7dB.
Claims (4)
1. the barium ferrite wave-absorbing powder of a metal ion mixing, it is characterized in that: the metal ion that adulterates is the above metal ion of tetravalence, and described barium ferrite is single-phase crystal, has simultaneously Fe in barium ferrite
3+And Fe
2+
2. the barium ferrite wave-absorbing powder of metal ion mixing according to claim 1, it is characterized in that: the metal ion that adulterates is Ti
4+
3. the barium ferrite wave-absorbing powder of metal ion mixing according to claim 1 and 2, is characterized in that: the metal ion that adulterates and Ba
2+Mol ratio be 0.6 ~ 0.8:1, Fe
3+And Fe
2+Total moles and Ba
2+The ratio of mole number be 11.2 ~ 11.4:1.
4. the preparation method of the barium ferrite wave-absorbing powder of a claim 1 or 2 metal ion mixing, is characterized in that, comprises the steps:
1) nitrate of baryta, iron nitrate and citric acid are mixed 1:11.2 ~ 11.4:17.8 ~ 18.1 in molar ratio, add the deionized water and stirring dissolving to obtain the first solution; In described the first solution, the total mol concentration of nitrate of baryta and iron nitrate is 0.5 ~ 2.0mol/L;
2) tetrabutyl titanate is dissolved in obtains the second solution in dehydrated alcohol; In described the second solution, the volumetric molar concentration of tetrabutyl titanate is 1.0 ~ 2.0mol/L;
3) citric acid is joined obtain the 3rd solution in the second solution; In described the 3rd solution, the mol ratio of tetrabutyl titanate and citric acid is 1:1.0 ~ 2.0;
4) slowly join the 3rd solution in the first solution and stir and obtain the 4th solution; In the 4th solution, the mol ratio of tetrabutyl titanate and nitrate of baryta is 6 ~ 8:10;
5) the 4th solution is heated and concentrates obtain colloidal sol, then the colloidal sol drying is obtained xerogel;
6) with xerogel perfect combustion, then with products of combustion at 800 ~ 950 ℃ of insulation 1.0 ~ 3.0h, and be rapidly heated 1100 ℃ ~ 1300 ℃ with the speed of 30 ~ 40 ℃/min and be incubated 1 ~ 3h.
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