CN103102867B - 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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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 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 being 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.Visible, wave-absorbing coating material, no matter in civil area or military field, all has important Research Significance and using value.
The material properties such as the absorption of electromagnetic wave ability of material and its dielectric, magnetic and resistivity are closely related.Ferrite Material has excellent magnetic property and also shows the medium of certain dielectric properties simultaneously as a kind of, under high frequency, there is higher magnetic permeability, 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.Research shows, 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, in the ferritic main magnetic loss mechanism of high frequency band, it is magnetic coupling utmost point natural resonance phenomenon, when electromagnetic frequency equals or approach the free precession frequency of ferrite magnetic moment, there is natural resonance phenomenon, 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 resonance mechanism determines, thereby resonant frequency is single, also conventionally for single-material, although it is high but effectively inhale ripple frequency range narrower (inhale ripple frequency range and be often referred to the range of frequency of inhaling wave reflection loss RL<-10dB) to inhale intensity of wave under resonant frequency, generally lower than 6GHz.In order to meet actual suction ripple frequency range requirement, conventionally need multiple material to coordinate and realize.If can break through, in a kind of material, realize the difficult point that broadband absorbs, obviously for practical, the cost degradation of absorbing material and simplification preparation technology etc., have great importance.
Research finds, for some high-valence cationics (as Ti
4+, Zr
4+, Nb
5+), when it is to the Fe in barium ferrite
3+while replacing, system own is in order to maintain 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 superexchange coupling, its coupling magnetic moment free precession frequency can be higher than Fe
3+the precession frequency of magnetic moment.Also, if suitably control this doping, in system, can there are two kinds of difference resonance mechanisms with different resonant frequencies simultaneously, form the double resonance system of the non-single mechanism that resonates, so just there will be double resonance loss peak.Because each resonance mechanism in this double resonance mechanism has resonant frequency separately, and there is suitable frequency difference, if thereby can this double resonance phenomenon effectively be used in absorbing material, this double resonance likely causes and absorbs respectively and absorb synergistic effect to different frequency range is electromagnetic, thereby likely reaches the object that wideband absorbs.
Further, because best microwave penetrating window mouth appears at 8.0 ~ 1000.0mm, also, in common alleged centimetric wave scope, at this moment transmitance approximately 100%.On the other hand, millimeter wave radar wave beam is narrow, and angular resolution is high, bandwidth, and good concealment, immunity from interference is strong.These features have promoted its widespread use at numerous areas.And in frequency, be the microwave within the scope of 26.5 ~ 40GHz, its not only had centimetric wave round-the-clock feature, but also have the feature of the better imaging resolution of millimeter wave, had radar in many types of this wave band etc. to be applied in military field at present.Thereby, promote the exploitation of the absorbing material that this wave band is corresponding, will contribute to it in the specific ripple field of inhaling, to be widely used.
Because the natural resonant frequency of barium ferrite itself is greater than 40GHz, be also 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.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 and change this concept of its natural resonant frequency, be expected to reach the object 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 adulterating 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 Fe in barium ferrite simultaneously
3+and Fe
2+.
Preferably, the metal ion that the present invention adulterates is Ti
4+.
Further, the present invention adulterates metal ion 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.
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 deionized water and stirring to dissolve and 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 and in dehydrated alcohol, obtains the second solution; In described the second solution, the volumetric molar concentration of tetrabutyl titanate is 1.0 ~ 2.0mol/L;
3) citric acid is joined and in the second solution, obtain the 3rd solution; In described the 3rd solution, the mol ratio of tetrabutyl titanate and citric acid is 1:1.0 ~ 2.0;
4) the 3rd solution is slowly joined 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 concentrated obtain colloidal sol, then by the dry xerogel that obtains of colloidal sol;
6) by xerogel perfect combustion, then by products of combustion at 800 ~ 950 ℃ of insulation 1.0 ~ 3.0h, and be rapidly heated 1100 ℃ ~ 1300 ℃ and be incubated 1 ~ 3h with the speed of 30 ~ 40 ℃/min.
Compare with background technology, the beneficial effect that the present invention has is: the present invention for example, by the above metal ion of comprehensive tetravalence (Ti
4+) control metal ion mixing (as titanium doped) and oxygen vacancy defect, in barium ferrite absorbing material system, efficiently realize double resonance loss mechanism, hertzian wave is produced to bimodal absorption, there is good absorbing property, can make to inhale ripple frequency band is controlled in 26.5 ~ 40GHz range of frequency, the about 12GHz(frequency range of maximum Effective frequency width of absorption can improve 2 ~ 3 times), at CF place best reflection loss RL value approximately-45dB.The preparation technology of wave-absorbing powder material 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.
Accompanying drawing explanation
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 adulterating 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 Fe in barium ferrite simultaneously
3+and Fe
2+.As the preferred embodiment of the present invention, the metal ion adulterating is Ti
4+.Preferably, the metal ion adulterating 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.
With specific embodiment, further illustrate the present invention below.
In fact, for the xerogel of titanium doped barium ferrite, while descending at a lower temperature sintering, more Ti easily mixes and in barium ferrite, forms required doped 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 when forming doped barium ferrite simultaneously
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 the absorption of double resonance peak thereby be an impediment to; Latter is owing to having reduced the content of titanium doped barium ferrite and significantly having reduced the relative Ti content in system, suppressed the ability of modulation barium ferrite to the frequency range of absorption of electromagnetic wave, be difficult to reach the object that reduces resonant frequency, be unfavorable for too efficiently realizing double resonance peak and absorb.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 be 0.6 ~ 0.8:1) time, then decompose established low-temperature phase α-Fe comparatively high temps (1100 ~ 1300 ℃) is lower
2o
3, reaching both to realize has enough titanium dopedly in barium ferrite, eliminate again α-Fe
2o
3phase, and suppress dephasign Ba simultaneously
6fe
45ti
17o
106the object producing.Further, the at high temperature thermal treatment through certain hour also helps the oxygen vacancy defect increasing 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, make this high performance material form, what also guarantee Ti effectively mixes the effective generation with double resonance mechanism, and it is crucial controlling and forming technique.
Embodiment 1:
1) by the 1:11.4:18.1 mixing in molar ratio of nitrate of baryta, iron nitrate and citric acid, add deionized water and stirring to dissolve and 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 and in dehydrated alcohol, obtains the second solution; In described the second solution, the volumetric molar concentration of tetrabutyl titanate is 1.0mol/L;
3) citric acid is joined and in the second solution, obtain the 3rd solution; In described the 3rd solution, the mol ratio 1:1.5 of tetrabutyl titanate and citric acid;
4) the 3rd solution is slowly joined 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 concentrated obtain colloidal sol, then by the dry puffy xerogel that obtains of colloidal sol;
6) by the perfect combustion of puffy xerogel, then by products of combustion at 800 ℃ of insulation 3.0h, and be rapidly heated 1100 ℃ with the speed of 40 ℃/min, the titanium doped barium ferrite (BaFe that to be incubated mol ratio that 3h obtains titanium and barium be 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 in mass ratio 8:3 evenly mix, and then mixture are incubated to 1 ~ 2h at 80 ~ 90 ℃, paraffin is melted completely and obtain molten mixture.This molten mixture is inserted in the red copper mould rectangle hole slot that 2.8mm is thick, made stopping composition consolidation, surfacing.Utilize Agilent vector network analyzer E8363C to test specific inductivity, magnetic permeability and the absorbing property of titanium doped barium ferrite absorbing material.
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, respectively there is an absorption peak in 29.3GHz and 38.9GHz place, in visible titanium doped barium ferrite powder, formed double resonance loss mechanism, shows Fe
3+and Fe
2+exist simultaneously; In addition, effectively inhale the about 11.8GHz of ripple frequency range (being RL<-10dB), best at the absorbing property at 29.3GHz place, approach-45.8dB.
Embodiment 2:
1) by the 1:11.3:17.95 mixing in molar ratio of nitrate of baryta, iron nitrate and citric acid, add deionized water and stirring to dissolve and 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 and in dehydrated alcohol, obtains the second solution; In described the second solution, the volumetric molar concentration of tetrabutyl titanate in this solution is 1.5mol/L;
3) citric acid is joined and in the second solution, obtain the 3rd solution; In described the 3rd solution, the mol ratio of tetrabutyl titanate and citric acid is 1:1.0;
4) the 3rd solution is slowly joined 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 concentrated obtain colloidal sol, then by the dry puffy xerogel that obtains of colloidal sol;
6) by the perfect combustion of puffy xerogel, then by products of combustion at 900 ℃ of insulation 2.0h, and be rapidly heated 1200 ℃ ℃ with the speed of 40 ℃/min, the titanium doped barium ferrite (BaFe that to be incubated mol ratio that 2h obtains titanium and barium be 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 in mass ratio 8:3 evenly mix, and then mixture are incubated to 1 ~ 2h at 80 ~ 90 ℃, paraffin is melted completely and obtain molten mixture.This molten mixture is inserted in the red copper mould rectangle hole slot that 2.9mm is thick, made stopping composition consolidation, surfacing.Utilize Agilent vector network analyzer E8363C to test specific inductivity, magnetic permeability and the absorbing property of titanium doped barium ferrite absorbing material.
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, respectively there is an absorption peak in 28.8GHz and 38.5GHz place, in visible titanium doped barium ferrite powder, formed double resonance loss mechanism, shows Fe
3+and Fe
2+exist simultaneously; In addition, effectively inhale the about 11.8GHz of ripple frequency range (being RL<-10dB), best at the absorbing property at 28.8GHz place, approach-45.0dB.
Embodiment 3:
1) by the 1:11.2:17.8 mixing in molar ratio of nitrate of baryta, iron nitrate and citric acid, add deionized water and stirring to dissolve and 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 and in dehydrated alcohol, obtains the second solution; In described the second solution, the volumetric molar concentration of tetrabutyl titanate in this solution is 2.0mol/L;
3) citric acid is joined and in the second solution, obtain the 3rd solution; In described the 3rd solution, the mol ratio of tetrabutyl titanate and citric acid is 1:2.0;
4) the 3rd solution is slowly joined 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 concentrated obtain colloidal sol, then by the dry puffy xerogel that obtains of colloidal sol;
6) by the perfect combustion of puffy xerogel, then by products of combustion at 950 ℃ of insulation 1.0h, and be rapidly heated 1300 ℃ ℃ with the speed of 30 ℃/min, the titanium doped barium ferrite (BaFe that to be incubated mol ratio that 1h obtains titanium and barium be 0.8
11.2ti
0.8o
19) powder absorbing material.
The titanium doped barium ferrite wave-absorbing powder material that the present embodiment is obtained and solid paraffin in mass ratio 8:3 evenly mix, and then mixture are incubated to 1 ~ 2h at 80 ~ 90 ℃, paraffin is melted completely and obtain molten mixture.This molten mixture is inserted in the red copper mould rectangle hole slot that 2.74mm is thick, made stopping composition consolidation, surfacing.Utilize Agilent vector network analyzer E8363C to test specific inductivity, magnetic permeability and the absorbing property of titanium doped barium ferrite absorbing material.
The XRD figure spectrum of the titanium doped barium ferrite wave-absorbing powder that Fig. 5 the present embodiment obtains, can see, 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, respectively there is an absorption peak in 28.4GHz and 39.0GHz place, in visible titanium doped barium ferrite powder, formed double resonance loss mechanism, shows Fe
3+and Fe
2+exist simultaneously; In addition, effectively inhale the about 12.2GHz of ripple frequency range (being RL<-10dB), best at the absorbing property at 28.4GHz place, approach-43.7dB.
Claims (1)
1. a preparation method for the barium ferrite wave-absorbing powder of 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 deionized water and stirring to dissolve and 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 and in dehydrated alcohol, obtains the second solution; In described the second solution, the volumetric molar concentration of tetrabutyl titanate is 1.0 ~ 2.0mol/L;
3) citric acid is joined and in the second solution, obtain the 3rd solution; In described the 3rd solution, the mol ratio of tetrabutyl titanate and citric acid is 1:1.0 ~ 2.0;
4) the 3rd solution is slowly joined 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 concentrated obtain colloidal sol, then by the dry xerogel that obtains of colloidal sol;
6) by xerogel perfect combustion, then by products of combustion at 800 ~ 950 ℃ of insulation 1.0 ~ 3.0h, and be rapidly heated 1100 ℃ ~ 1300 ℃ and be incubated 1 ~ 3h with the speed of 30 ~ 40 ℃/min.
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| CN104844182B (en) * | 2015-01-29 | 2017-02-22 | 浙江大学 | Zirconium and titanium-co-doped barium ferrite wave-absorbing powder material and preparation method therefor |
| CN105670456A (en) * | 2016-01-28 | 2016-06-15 | 赵文立 | Material capable of shielding electromagnetic waves caused by groundwater |
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