高旋磁特性的LiZn铁氧体及其应用研究
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摘要
LiZn铁氧体材料具有饱和磁化强度可调范围宽、居里温度高、剩磁对应力敏感性低以及成本低廉等特点，是制造高功率微波移相器等微波/毫米波器件的优良材料。如Ka波段铁氧体移相器是高精度相控阵雷达的关键组件，要求应用于其中的LiZn铁氧体具有良好的旋磁性（饱和磁化强度高）、软磁性（矫顽力低）和矩磁性（剩磁比高），并具有低微波损耗（铁磁共振线宽和介电损耗低），以缩小器件体积、降低移相器驱动电流和插入损耗。基于上述，本文就高旋磁特性LiZn铁氧体的制备技术和静态磁性能、微波性能及其影响机理与应用展开研究。
本文首先结合自蔓延燃烧工艺对LiZn铁氧体纳米粉Sol-Gel制备工艺技术进行研究，并对LiZn铁氧体纳米粉的烧结性能进行分析。结果表明：1）采用Sol-Gel自蔓延燃烧工艺可在较低温度下（约500℃）获得高活性的LiZn铁氧体纳米粉，适宜的柠檬酸与金属硝酸盐配比（r=1:1）是保证通过自蔓延燃烧获得单一晶相LiZn铁氧体的前提；2）在800℃煅烧时会出现Li挥发现象，导致Fe3+析出，形成Fe_2O_3另相；3）提高溶胶反应温度可稍降低自蔓延燃烧粉体颗粒尺寸和粉体比饱和磁化强度；4）Sol-Gel法自蔓延粉体的烧结样品气孔率较高（大于10％），密度较低（约4.4g·cm-3）。
其次，对Sol-Gel工艺和氧化物工艺进行探索性比对研究，分析了氧化物工艺制备低矫顽力的高旋磁性LiZn铁氧体的优势。接着分别讨论了预烧温度、二次球磨时间、烧结条件和气氛对材料性能的影响。结果表明：1）预烧温度为800℃时，LiZn铁氧体粉料活性、烧结材料的显微结构理想，材料饱和磁化强度和剩磁比高，矫顽力和铁磁共振线宽相对较低；2）在1100℃烧结时，二次球磨时间大于4h时样品饱和磁化强度变化不大，但在1160℃烧结时，二次球磨时间大于4h时会引起样品饱和磁化强度下降，矫顽力上升。LiZn铁氧体适宜的二次球磨时间为3h；3）对于1wt%Bi_2O_3掺杂LiZn铁氧体，为了保证材料具有良好的矩磁特性，以便获取高剩磁，应在低于1100℃的环境中进行烧结；4）氧气氛烧结时，LiZn铁氧体材料电阻率提高非常显著；负压烧结可提高材料密度和饱和磁化强度，降低材料矫顽力。
在氧化物工艺参数明确后，本文分析了LiZn铁氧体中离子分布和超交换作用对材料磁参数和温度特性的影响，还分析了缺铁量和富锂量对LiZn铁氧体微波损耗的影响。结果表明：1）Zn2+能够有效提高LiZn铁氧体的饱和磁化强度，降低材料矫顽力和铁磁共振线宽，但会引起剩磁比和居里温度下降。2）在主配方中适量缺铁能够有效抑制Fe2+，降低介电损耗，但会引起居里温度下降；3）在主配方中适量富锂可以降低介电损耗，但过量富锂会导致饱和磁化强度和剩磁下降，引起铁磁共振线宽和矫顽力增大。
本文还展开了多种添加剂（V2O5、CuO、Bi_2O_3、Mn_3O_4和NiO）对材料晶粒生长、烧结特性及磁电性能的影响研究，分析了烧结温度和Bi_2O_3添加量对Li挥发的影响。结果表明：1）添加V2O5可以有效地促进烧结致密化和晶粒生长，降低H c，但非磁性的V5+离子取代会降低材料饱和磁化强度。适宜的V2O5添加量应该控制在0.25wt%以下；2）在1000～1100℃烧结时，添加CuO可有效地促进烧结致密化和晶粒生长，降低烧结温度，提高LiZn铁氧体密度、饱和磁化强度和剩磁，降低材料矫顽力，但矫顽力仍较高。在1130℃烧结时，CuO的助烧作用不明显；3）在1000℃烧结时，添加2.00～3.00wt%Bi_2O_3时能够获得低矫顽力的高旋磁性LiZn铁氧体。在1100℃烧结时，添加3.00wt%Bi_2O_3可使Li挥发量由8wt%降至1wt%；4）Mn_3O_4含量和添加方式对LiZn铁氧体性能影响较大。920℃烧结时在配方中添加适量的Mn_3O_4可提高LiZn铁氧体饱和磁化强度和剩磁，降低矫顽力，而在预烧料中掺Mn_3O_4对饱和磁化强度和剩磁影响不大。在950℃烧结时，两种样品矫顽力显著下降，且在配方中添加Mn_3O_4的样品矫顽力相对较高。两种方式添加适量的Mn_3O_4均能通过抑制Fe2+和Fe3+间的电子跃迁来提高材料电阻率，对于Li0.35Zn0.30Fe2.29MnxO4±δ铁氧体，当x=0.06时两种样品电阻率达峰值，且在配方中添加Mn_3O_4的样品电阻率较高。在1000℃烧结时，添加Mn_3O_4仍有助于提高材料电阻率，但与950℃烧结样品相比，样品电阻率因Li挥发而下降；5）少量NiO有助于提高材料剩磁比，但会导致材料矫顽力上升。
最后，基于研制的高旋磁特性LiZn铁氧体材料进行应用研究。采用背脊式波导结构在高旋磁性LiZn铁氧体材料基础上进行移相器仿真设计和研制，结果表明：1）优化波导和铁氧体矩形环的横截面尺寸能够有效减小插入损耗；2）在-60～+100℃温度范围内，实现360°差相移所需的铁氧体矩形环长度至少应为25.5mm；（3）以29.6mm长的铁氧体矩形环研制的移相器可在25℃实现420°差相移，以34GHz为中心频率的6%带宽内插入损耗小于1.3dB，驻波比小于1.4。
LiZn ferrite, which performs a wide range of variable saturation magnetization, highCurie temperature, low stress sensitivity and low fabrication cost, is apt to be fabricatedinto microwave/millimeter wave devices, e.g. ferrite phase shifter. Ka-band ferrite phaseshifter is a crucial component of phase array radar, and the LiZn ferrite applied in itshould have excellent gyromagnetic property (high saturation magneticzation), goodsoft magnetic property (low coercivity) and rectangular characteristic (high remanenceratio). Furthermore, low microwave losses (low ferromagnetic resonance line width anddielectric loss) are required to reduce insertion loss. For the features given above, thepreparation process, the influence mechanism of the static magnetic characteristics andmicrowave properties, and its application of high gyromagnetic LiZn ferrite areresearched and analyzed.
Firstly, the auto-combustion method used for preparation of LiZn ferrite nanopowder was researched and the sintering characteristic of LiZn ferrite nano powder wasanalyzed. The results are as follows.1) High activity LiZn ferrite nano powder can beobtained by auto-combustion process at low temperature (about500℃), and anappropriate ratio of citric acid and metal nitrates (r=1:1) is the prerequisite to obtain thesingle crystalline phase LiZn ferrite;2) LiZn ferrite nano powder is so active thatlithium volatilization ocurrs when sintered at800℃, which causes the Fe3+precipitatedand Fe_2O_3phase formed;3) When the reaction temperature off Sol-Gel is heighten, thepowder size and the specific saturation magnetization decrease slightly;4) The sinteredbulk sample, derived from self-propagating nano powder which is fabricated by theSol-Gel method, has high porosity (>10%) and low density (about4.4g·cm-3).
And then， the comparation between Sol-Gel process and oxide process isperformed, And the oxide process was choosed to fabricate LiZn-ferrite materials usedfor Ka band phase shifter. The advantages of oxide process to fabricate LiZn-ferritewere analyzed. The influence of calcining temperature, second ball milling time,sintering conditions and atmosphere on the material performance was discussed. Theresults are as follows.1) When the calcining temperature is800℃, the LiZn ferrite powder posesses a high activity, and the sintered LiZn ferrite has a perfectmicrostructure, uniform grain size, less pore, high saturation magnetization and highremanence ratio, relatively low coercivity, and low ferromagnetic resonance linewidth;2) When sintered at1100℃, if the second ball milling time is more than4hours, it haslittle impact on saturation magnetization. But sintered at1160℃, saturationmagnetization decreases and coercivity increases when second ball milling time exceeds4hours;3) For the1wt%Bi_2O_3doped LiZn-ferrite, in order to get a rectangularproperty so that high remanence can be obtained, it should be sintered below1100℃;4)When sintered in oxygen atmosphere, the resistivity of LiZn-ferrite is enhancedobvously. Sintered at a negative air pressure is benefit to increase saturationmagnetization and decrease coercivity.
The effect of Zn substitution on the ions distribution and superexchange interactionof LiZn ferrite was researched. The effect of ions distribution and superexchangeinteraction on the magnetic parameter and temperature characteristic was analyzed,together with the effect of iron deficiency and Li overdose on the microwave loss ofLiZn ferrite. The results are as follows.1) The Zn2+can enhance the saturationmagnetization and decrease the coercivity and ferromagnetic resonance linewidth, but ata price of decreasing the remanence ratio and Curie temperature;2) In the main recipe, amoderate iron deficiency can suppress the appeareance of Fe2+effectively. And then thedielectric loss can be decreased;3) A proper Li overdose in the main recipe can reducethe dielectric loss, but the existence of too much Li will cause a drop in the saturationmagnetization and remanence ratio, and then make the ferromagnetic resonancelinewidth and coercivity to increase.
In addition, the paper carried out a series of additives research systematically,including V2O5, CuO, Bi_2O_3, Mn_3O_4, and NiO on grain growth, sintering characteristics,magnetic property. Furthermore, the effect of sintering temperature and Bi_2O_3concentration on Li volatilization is investigated. The results are as follows.1）V2O5caneffectively promote sintering densification and grain growth and decrease coercivity, butnonmagnetic V5+ions substitution can result in a decline in saturation magnetizationsignificantly. So V2O5concentration should be controlled below0.25wt%, in order toobtain high saturation magnetization LiZn ferrite materials;2）Sintering at1000～1100℃, CuO doping can effectively promote sintering densification and grain growth, reduce the sintering temperature, enhance density, saturation magnetization, andremanence, reduce coercive force, but coercive force is still higher. Sintering at1130℃,the CuO aid is not obvious;3）Sintered at1000℃, the appropriate dosage of Bi_2O_3is2～3wt%. Li volatilization in1100℃sintered magnet decreases from8wt%to1wt%by doping3wt%Bi_2O_3;4） content of Mn_3O_4and adding method have great impact onthe performance for LiZn ferrite. In920℃sintered sample, adding appropriate amountof Mn_3O_4into the raw materials can enhance saturation magnetization and remanence,and reduce coercive force. Whereas adding Mn_3O_4into the presintering powder affectslittle on saturation magnetization and remanence. Sintered at950℃, coercive force ofthe samples fabricated by the both Mn_3O_4adding methods decreases significantly,furthermore, the coercivity is higher when adding Mn_3O_4into the raw materials. For theboth adding methods, Moderate Mn_3O_4content can improve resistivity via inhibitingthe electron hopping between Fe2+and Fe3+. Both resistivities ofLi0.35Zn0.30Fe2.29MnxO4±δ(0.02≤x≤0.08) ferrite reach the peak value when x=0.06,furthermore, resistivity is higher when adding Mn_3O_4into the raw materials. Mn_3O_4stillhelps to improve resistivity sintering at1000℃, but the resistivity declines comparedwith that of950℃sintered samples;5）A small amount of NiO helps to improveremanence ratio, but it increases coercivity.
Finally, the suitable main recipe and process are given and the application isinvestigated for high gyromagnetic LiZn ferrite. Simulation design for ferrite phaseshifter with back ridged waveguide is developed. The results are as follows.1)Modifying the section size of grooved waveguide and ferrite rectangular helps todecrease insertion loss;2) To insure differential phase shift being360°in the wholerange of-60～+100℃, the length of ferrite rectangular loop should be at least25.5mm;3) Ferrite phase shifter with29.6mm ferrite rectangular was fabricated, and420°differential phase shift was achieved at25℃. VSWR and insertion loss at33～35GHzis less than1.4and1.3dB, respectively.
本文首先结合自蔓延燃烧工艺对LiZn铁氧体纳米粉Sol-Gel制备工艺技术进行研究，并对LiZn铁氧体纳米粉的烧结性能进行分析。结果表明：1）采用Sol-Gel自蔓延燃烧工艺可在较低温度下（约500℃）获得高活性的LiZn铁氧体纳米粉，适宜的柠檬酸与金属硝酸盐配比（r=1:1）是保证通过自蔓延燃烧获得单一晶相LiZn铁氧体的前提；2）在800℃煅烧时会出现Li挥发现象，导致Fe3+析出，形成Fe_2O_3另相；3）提高溶胶反应温度可稍降低自蔓延燃烧粉体颗粒尺寸和粉体比饱和磁化强度；4）Sol-Gel法自蔓延粉体的烧结样品气孔率较高（大于10％），密度较低（约4.4g·cm-3）。
其次，对Sol-Gel工艺和氧化物工艺进行探索性比对研究，分析了氧化物工艺制备低矫顽力的高旋磁性LiZn铁氧体的优势。接着分别讨论了预烧温度、二次球磨时间、烧结条件和气氛对材料性能的影响。结果表明：1）预烧温度为800℃时，LiZn铁氧体粉料活性、烧结材料的显微结构理想，材料饱和磁化强度和剩磁比高，矫顽力和铁磁共振线宽相对较低；2）在1100℃烧结时，二次球磨时间大于4h时样品饱和磁化强度变化不大，但在1160℃烧结时，二次球磨时间大于4h时会引起样品饱和磁化强度下降，矫顽力上升。LiZn铁氧体适宜的二次球磨时间为3h；3）对于1wt%Bi_2O_3掺杂LiZn铁氧体，为了保证材料具有良好的矩磁特性，以便获取高剩磁，应在低于1100℃的环境中进行烧结；4）氧气氛烧结时，LiZn铁氧体材料电阻率提高非常显著；负压烧结可提高材料密度和饱和磁化强度，降低材料矫顽力。
在氧化物工艺参数明确后，本文分析了LiZn铁氧体中离子分布和超交换作用对材料磁参数和温度特性的影响，还分析了缺铁量和富锂量对LiZn铁氧体微波损耗的影响。结果表明：1）Zn2+能够有效提高LiZn铁氧体的饱和磁化强度，降低材料矫顽力和铁磁共振线宽，但会引起剩磁比和居里温度下降。2）在主配方中适量缺铁能够有效抑制Fe2+，降低介电损耗，但会引起居里温度下降；3）在主配方中适量富锂可以降低介电损耗，但过量富锂会导致饱和磁化强度和剩磁下降，引起铁磁共振线宽和矫顽力增大。
本文还展开了多种添加剂（V2O5、CuO、Bi_2O_3、Mn_3O_4和NiO）对材料晶粒生长、烧结特性及磁电性能的影响研究，分析了烧结温度和Bi_2O_3添加量对Li挥发的影响。结果表明：1）添加V2O5可以有效地促进烧结致密化和晶粒生长，降低H c，但非磁性的V5+离子取代会降低材料饱和磁化强度。适宜的V2O5添加量应该控制在0.25wt%以下；2）在1000～1100℃烧结时，添加CuO可有效地促进烧结致密化和晶粒生长，降低烧结温度，提高LiZn铁氧体密度、饱和磁化强度和剩磁，降低材料矫顽力，但矫顽力仍较高。在1130℃烧结时，CuO的助烧作用不明显；3）在1000℃烧结时，添加2.00～3.00wt%Bi_2O_3时能够获得低矫顽力的高旋磁性LiZn铁氧体。在1100℃烧结时，添加3.00wt%Bi_2O_3可使Li挥发量由8wt%降至1wt%；4）Mn_3O_4含量和添加方式对LiZn铁氧体性能影响较大。920℃烧结时在配方中添加适量的Mn_3O_4可提高LiZn铁氧体饱和磁化强度和剩磁，降低矫顽力，而在预烧料中掺Mn_3O_4对饱和磁化强度和剩磁影响不大。在950℃烧结时，两种样品矫顽力显著下降，且在配方中添加Mn_3O_4的样品矫顽力相对较高。两种方式添加适量的Mn_3O_4均能通过抑制Fe2+和Fe3+间的电子跃迁来提高材料电阻率，对于Li0.35Zn0.30Fe2.29MnxO4±δ铁氧体，当x=0.06时两种样品电阻率达峰值，且在配方中添加Mn_3O_4的样品电阻率较高。在1000℃烧结时，添加Mn_3O_4仍有助于提高材料电阻率，但与950℃烧结样品相比，样品电阻率因Li挥发而下降；5）少量NiO有助于提高材料剩磁比，但会导致材料矫顽力上升。
最后，基于研制的高旋磁特性LiZn铁氧体材料进行应用研究。采用背脊式波导结构在高旋磁性LiZn铁氧体材料基础上进行移相器仿真设计和研制，结果表明：1）优化波导和铁氧体矩形环的横截面尺寸能够有效减小插入损耗；2）在-60～+100℃温度范围内，实现360°差相移所需的铁氧体矩形环长度至少应为25.5mm；（3）以29.6mm长的铁氧体矩形环研制的移相器可在25℃实现420°差相移，以34GHz为中心频率的6%带宽内插入损耗小于1.3dB，驻波比小于1.4。
LiZn ferrite, which performs a wide range of variable saturation magnetization, highCurie temperature, low stress sensitivity and low fabrication cost, is apt to be fabricatedinto microwave/millimeter wave devices, e.g. ferrite phase shifter. Ka-band ferrite phaseshifter is a crucial component of phase array radar, and the LiZn ferrite applied in itshould have excellent gyromagnetic property (high saturation magneticzation), goodsoft magnetic property (low coercivity) and rectangular characteristic (high remanenceratio). Furthermore, low microwave losses (low ferromagnetic resonance line width anddielectric loss) are required to reduce insertion loss. For the features given above, thepreparation process, the influence mechanism of the static magnetic characteristics andmicrowave properties, and its application of high gyromagnetic LiZn ferrite areresearched and analyzed.
Firstly, the auto-combustion method used for preparation of LiZn ferrite nanopowder was researched and the sintering characteristic of LiZn ferrite nano powder wasanalyzed. The results are as follows.1) High activity LiZn ferrite nano powder can beobtained by auto-combustion process at low temperature (about500℃), and anappropriate ratio of citric acid and metal nitrates (r=1:1) is the prerequisite to obtain thesingle crystalline phase LiZn ferrite;2) LiZn ferrite nano powder is so active thatlithium volatilization ocurrs when sintered at800℃, which causes the Fe3+precipitatedand Fe_2O_3phase formed;3) When the reaction temperature off Sol-Gel is heighten, thepowder size and the specific saturation magnetization decrease slightly;4) The sinteredbulk sample, derived from self-propagating nano powder which is fabricated by theSol-Gel method, has high porosity (>10%) and low density (about4.4g·cm-3).
And then， the comparation between Sol-Gel process and oxide process isperformed, And the oxide process was choosed to fabricate LiZn-ferrite materials usedfor Ka band phase shifter. The advantages of oxide process to fabricate LiZn-ferritewere analyzed. The influence of calcining temperature, second ball milling time,sintering conditions and atmosphere on the material performance was discussed. Theresults are as follows.1) When the calcining temperature is800℃, the LiZn ferrite powder posesses a high activity, and the sintered LiZn ferrite has a perfectmicrostructure, uniform grain size, less pore, high saturation magnetization and highremanence ratio, relatively low coercivity, and low ferromagnetic resonance linewidth;2) When sintered at1100℃, if the second ball milling time is more than4hours, it haslittle impact on saturation magnetization. But sintered at1160℃, saturationmagnetization decreases and coercivity increases when second ball milling time exceeds4hours;3) For the1wt%Bi_2O_3doped LiZn-ferrite, in order to get a rectangularproperty so that high remanence can be obtained, it should be sintered below1100℃;4)When sintered in oxygen atmosphere, the resistivity of LiZn-ferrite is enhancedobvously. Sintered at a negative air pressure is benefit to increase saturationmagnetization and decrease coercivity.
The effect of Zn substitution on the ions distribution and superexchange interactionof LiZn ferrite was researched. The effect of ions distribution and superexchangeinteraction on the magnetic parameter and temperature characteristic was analyzed,together with the effect of iron deficiency and Li overdose on the microwave loss ofLiZn ferrite. The results are as follows.1) The Zn2+can enhance the saturationmagnetization and decrease the coercivity and ferromagnetic resonance linewidth, but ata price of decreasing the remanence ratio and Curie temperature;2) In the main recipe, amoderate iron deficiency can suppress the appeareance of Fe2+effectively. And then thedielectric loss can be decreased;3) A proper Li overdose in the main recipe can reducethe dielectric loss, but the existence of too much Li will cause a drop in the saturationmagnetization and remanence ratio, and then make the ferromagnetic resonancelinewidth and coercivity to increase.
In addition, the paper carried out a series of additives research systematically,including V2O5, CuO, Bi_2O_3, Mn_3O_4, and NiO on grain growth, sintering characteristics,magnetic property. Furthermore, the effect of sintering temperature and Bi_2O_3concentration on Li volatilization is investigated. The results are as follows.1）V2O5caneffectively promote sintering densification and grain growth and decrease coercivity, butnonmagnetic V5+ions substitution can result in a decline in saturation magnetizationsignificantly. So V2O5concentration should be controlled below0.25wt%, in order toobtain high saturation magnetization LiZn ferrite materials;2）Sintering at1000～1100℃, CuO doping can effectively promote sintering densification and grain growth, reduce the sintering temperature, enhance density, saturation magnetization, andremanence, reduce coercive force, but coercive force is still higher. Sintering at1130℃,the CuO aid is not obvious;3）Sintered at1000℃, the appropriate dosage of Bi_2O_3is2～3wt%. Li volatilization in1100℃sintered magnet decreases from8wt%to1wt%by doping3wt%Bi_2O_3;4） content of Mn_3O_4and adding method have great impact onthe performance for LiZn ferrite. In920℃sintered sample, adding appropriate amountof Mn_3O_4into the raw materials can enhance saturation magnetization and remanence,and reduce coercive force. Whereas adding Mn_3O_4into the presintering powder affectslittle on saturation magnetization and remanence. Sintered at950℃, coercive force ofthe samples fabricated by the both Mn_3O_4adding methods decreases significantly,furthermore, the coercivity is higher when adding Mn_3O_4into the raw materials. For theboth adding methods, Moderate Mn_3O_4content can improve resistivity via inhibitingthe electron hopping between Fe2+and Fe3+. Both resistivities ofLi0.35Zn0.30Fe2.29MnxO4±δ(0.02≤x≤0.08) ferrite reach the peak value when x=0.06,furthermore, resistivity is higher when adding Mn_3O_4into the raw materials. Mn_3O_4stillhelps to improve resistivity sintering at1000℃, but the resistivity declines comparedwith that of950℃sintered samples;5）A small amount of NiO helps to improveremanence ratio, but it increases coercivity.
Finally, the suitable main recipe and process are given and the application isinvestigated for high gyromagnetic LiZn ferrite. Simulation design for ferrite phaseshifter with back ridged waveguide is developed. The results are as follows.1)Modifying the section size of grooved waveguide and ferrite rectangular helps todecrease insertion loss;2) To insure differential phase shift being360°in the wholerange of-60～+100℃, the length of ferrite rectangular loop should be at least25.5mm;3) Ferrite phase shifter with29.6mm ferrite rectangular was fabricated, and420°differential phase shift was achieved at25℃. VSWR and insertion loss at33～35GHzis less than1.4and1.3dB, respectively.
引文
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