CN110105063A - 一种5g通信用自旋铁氧体材料及其制备方法 - Google Patents
一种5g通信用自旋铁氧体材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种5G通信用自旋铁氧体材料及其制备方法,用Bi和Cu取代部分Y,可起到促进固相反应、提高密度、降低烧结温度的作用,从而有利于产品在较低的烧结温度下获得高密度、细晶粒的显微结构,减低了能耗,节约了成本。用Gd取代部分Y,用In取代部分Fe,用Mn取代部分Fe可以提高材料性能。取代完成后制备出符合5G通信的自旋铁氧体材料。
Description
技术领域
本发明涉及微波铁氧体材料技术领域,尤其涉及一种用于5G通信的自旋铁氧体材料及其制备方法。
背景技术
石榴石铁氧体晶体的分子式一般表示为其中R为Y和稀土金属离子。具有低的介电损耗、低的各向异性场、高密度、低磁损耗和窄共振线宽△H,在国防、卫星通讯和移动通信等领域应用广泛。
目前,制备石榴石铁氧体材料需要用到大量的稀土材料Y2O3,而Y2O3量少且提纯工艺复杂,因此,其成本较高。
申请公布号为CN107417266A,申请公布日为2017年12月1日的中国发明专利申请公布了一种无稀土石榴石铁氧体材料及其制备方法,该专利申请用Bi3+和Ca2+完全取代Y3+,得到无稀土的石榴石微波铁氧体材料,从而大大降低了石榴石微波铁氧体材料的成本。但是该发明还存在如下缺陷:
1、烧结温度较高,能耗高,提高了生产成本。
2、密度较低。
3、磁矩和功率并不是很理想。
发明内容
本发明为了解决现有石榴石铁氧体材料存在的上述缺陷,提供了一种5G通信用自旋铁氧体材料,该材料降低了磁矩,增大了功率,用少量Bi、Cu取代部分Y可起到促进固相反应、提高密度、降低烧结温度的作用,从而有利于产品在较低的烧结温度下获得高密度、细晶粒的显微结构,减低了能耗,节约了成本。
为解决上述技术问题,本发明所采用的技术方案是:
一种5G通信用自旋铁氧体材料,其特征在于:其配方分子式:
{Y3+ 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-,其中:
0≤a≤1,0≤b≤0.3,0≤c≤0.6,0.2≤d≤0.4,0.1≤e≤0.3,0.04≤x≤0.06
本发明还提供了上述5G通信用自旋铁氧体材料的制备方法,其特征在于:包括如下步骤:
步骤1,配方设计
根据配方分子式{Y3+ 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-进行配方设计;
步骤2,称料
根据步骤1配方设计结果,计算并称取各种原料,所述原料为Fe2O3、Bi2O3、Y2O3、CuO、CaCO3、Gd2O3、In2O3、V2O5、Mn2O3;
步骤3,一次湿法球磨
将步骤2称取的各种原料混合装入球磨罐中,并加入球和稀释剂,进行原料一次湿法混合球磨;
步骤4,一次烧结
将经过步骤3后的浆料烘干,经过分样筛制备成粉料,然后放入烧结炉内进行烧结,温度为1050℃,时间为5h;
步骤5,二次湿法球磨
将经过步骤4的粉料,装入球磨罐中,加入球和稀释剂,进行二次湿法球磨,得到浆料;
步骤6,造粒
将步骤5球磨后的浆料烘干,然后加入胶合剂进行造粒;
步骤7,压制成型
将步骤6得到的颗粒放入模具进行压制,压制压强为50MPa-250Mpa,得到材料生坯;
步骤8,二次烧结
将步骤7得到生坯装入氧气气氛炉中进行二次烧结,烧结温度为900-1200℃,时间为5h。
与现有技术相比,本发明具有以下有益效果:
本发明用Bi和Cu取代了部分Y,可起到促进固相反应、提高密度、降低烧结温度的作用,从而有利于产品在较低的烧结温度下获得高密度、细晶粒的显微结构,减低了能耗,节约了成本。本发明用Gd3+替代部分Y3+ ,饱和磁化强度温度系数小,用In3 +置换Fe3+ , 铁氧体磁晶各向异性常数K1 下降, 使ΔH 下降,Ca2+,V5+是低熔点离子, 在较低的烧结温度下, 生成单相致密的石榴石铁氧体, 为保持电中性条件, 掺入的Ca2+, V5+ 的比为2∶1 。本发明一次烧结温度为1050℃,二次烧结温度为900-1200℃,提高预烧温度, 降低烧结温度, 减小晶粒平均尺寸也可以提高hc。本发明用Mn3+替代Fe3 +可以提高铁氧体性能。通过上述替代之后,使得制备出来的铁氧体材料磁矩低,功率大,高密度、低磁损耗和窄共振线宽△H,完全符合5G通信的要求。
附图说明
图1为Mn3+对YGdCaVInIG铁氧体电阻率的影响;
图2为Mn3 + 对YGdCaVInIG 的tgδe 的影响;
图3为Mn3 + 对YGdCaVInIG tgδm 的影响;
图4为Mn3 +对YGdCaVInIG的4πMs 的影响;
图5为Mn3+ 的YGdCaVInIG的4πMs 随温度变化曲线。
具体实施方式
下面结合实施例对本发明作进一步的描述,所描述的实施例仅仅是本发明一部分实施例,并不是全部的实施例。基于本发明中的实施例,本领域的普通技术人员在没有做出创造性劳动前提下所获得的其他所用实施例,都属于本发明的保护范围。
实施例1
一种5G通信用自旋铁氧体材料,其主相结构为石榴石结构,其配方分子式为:{Y3 + 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-,其中,a=1,b=0.1,c=0.1,d=0.2,e=0.1,x=0.04。
其制备方法为:
步骤1,配方设计
根据配方分子式{Y3+ 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-进行配方设计;
步骤2,称料
根据步骤1配方设计结果,计算并称取各种原料,所述原料为Fe2O3、Bi2O3、Y2O3、CuO、CaCO3、Gd2O3、In2O3、V2O5、Mn2O3;
步骤3,一次湿法球磨
将步骤2称取的各种原料混合装入球磨罐中,并加入球和稀释剂,进行原料一次湿法混合球磨;
步骤4,一次烧结
将经过步骤3后的浆料烘干,经过分样筛制备成粉料,然后放入烧结炉内进行烧结,温度为1050℃,时间为5h;
步骤5,二次湿法球磨
将经过步骤4的粉料,装入球磨罐中,加入球和稀释剂,进行二次湿法球磨,得到浆料;
步骤6,造粒
将步骤5球磨后的浆料烘干,然后加入胶合剂进行造粒;
步骤7,压制成型
将步骤6得到的颗粒放入模具进行压制,压制压强为100Mpa,得到材料生坯;
步骤8,二次烧结
将步骤7得到生坯装入氧气气氛炉中进行二次烧结,烧结温度为900℃,时间为5h。
实施例2
一种5G通信用自旋铁氧体材料,其主相结构为石榴石结构,其配方分子式为:{Y3 + 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-,其中,a=0,b=0.3,c=0.6,d=0.4,e=0.3,x=0.05。
其制备方法为:
步骤1,配方设计
根据配方分子式{Y3+ 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-进行配方设计;
步骤2,称料
根据步骤1配方设计结果,计算并称取各种原料,所述原料为Fe2O3、Bi2O3、Y2O3、CuO、CaCO3、Gd2O3、In2O3、V2O5、Mn2O3;
步骤3,一次湿法球磨
将步骤2称取的各种原料混合装入球磨罐中,并加入球和稀释剂,进行原料一次湿法混合球磨;
步骤4,一次烧结
将经过步骤3后的浆料烘干,经过分样筛制备成粉料,然后放入烧结炉内进行烧结,温度为1050℃,时间为5h;
步骤5,二次湿法球磨
将经过步骤4的粉料,装入球磨罐中,加入球和稀释剂,进行二次湿法球磨,得到浆料;
步骤6,造粒
将步骤5球磨后的浆料烘干,然后加入胶合剂进行造粒;
步骤7,压制成型
将步骤6得到的颗粒放入模具进行压制,压制压强为50MPa,得到材料生坯;
步骤8,二次烧结
将步骤7得到生坯装入氧气气氛炉中进行二次烧结,烧结温度为1200℃,时间为5h。
实施例3
一种5G通信用自旋铁氧体材料,其主相结构为石榴石结构,其配方分子式为:{Y3 + 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-,其中,a=0.5,b=0,c=0,d=0.3,e=0.2,x=0.06。
其制备方法为:
步骤1,配方设计
根据配方分子式{Y3+ 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-进行配方设计;
步骤2,称料
根据步骤1配方设计结果,计算并称取各种原料,所述原料为Fe2O3、Bi2O3、Y2O3、CuO、CaCO3、Gd2O3、In2O3、V2O5、Mn2O3;
步骤3,一次湿法球磨
将步骤2称取的各种原料混合装入球磨罐中,并加入球和稀释剂,进行原料一次湿法混合球磨;
步骤4,一次烧结
将经过步骤3后的浆料烘干,经过分样筛制备成粉料,然后放入烧结炉内进行烧结,温度为1050℃,时间为5h;
步骤5,二次湿法球磨
将经过步骤4的粉料,装入球磨罐中,加入球和稀释剂,进行二次湿法球磨,得到浆料;
步骤6,造粒
将步骤5球磨后的浆料烘干,然后加入胶合剂进行造粒;
步骤7,压制成型
将步骤6得到的颗粒放入模具进行压制,压制压强为250Mpa,得到材料生坯;
步骤8,二次烧结
将步骤7得到生坯装入氧气气氛炉中进行二次烧结,烧结温度为1000℃,时间为5h。
提高峰值功率必须提高自旋波不稳定激发的临界场hc , 以防止非线性损耗的发生, 这种非线性效应的临介场hc为:
加入Gd3+置换部分Y3+ ,饱和磁化强度温度系数小,形成稀土复合YGdIG 石榴石铁氧体材料。
加入In3 +置换Fe3+ , 铁氧体磁晶各向异性常数K1 下降, 使ΔH 下降,Ca2+,V5+是低熔点离子, 在较低的烧结温度下, 生成单相致密的石榴石铁氧体, 为保持电中性条件, 掺入Ca2+, V5+ 的比为2∶1 。
提高预烧温度, 降低烧结温度, 减小晶粒平均尺寸也可以提高hc
通过以上三点的,石榴石铁氧体是一种复合稀土石榴石铁氧体,简写成:YGdCaVInIG。
制备
㈠按照制备石榴石铁氧体工艺特点和要求, 采用氧化物工艺程序, 制备了YGdCaVInIG多晶铁氧体,为了进一步优化铁氧体的特性,我们探测性的掺入微量Mn离子代替部分三价Fe离子,研究Mn元素对铁氧体性能的影响。
如图1所示,Mn对YGdCaVInIG铁氧体电阻率的影响
如图1所示,YIG铁氧体本身电阻率较高, 损耗较低, 但铁氧体很难处于正确的组分,往往存在Fe2+, 使其电阻率ρ下降。用Mn3+替代Fe3 + , 抑制了Fe2 +产生, 铁氧体电阻率ρ随Mn3+ 含量x 增加而上升。
如图2所示, Mn3 +对YGdCaVInIG 的tgδe 的影响(lgδe ∞ 1/ερ式中ε为介电常数, ρ为电阻率),如图3所示, Mn3 +对YGdCaVInIG tgδm 的影响,如图4所示 Mn3 +对YGdCaVInIG的4πMs 的影响,如图5所示,掺Mn3+的YGdCaVInIG的4πMs 随温度变化曲线。
一次烧结温度对铁氧体性能影响
以100 ℃·h - 1速度升温, 选择了4 种不同的预烧温度, 空气中预烧, 1360 ℃烧结, 保温5 h , 制备x 为0. 04 掺Mn 的YGdCaVInIG铁氧体, 在1050 ℃保温5 h预烧性能较好。
Mn3+对YGdCaVInIG铁氧体晶体结构影响
Mn3+对多晶铁氧体的晶体结构没有影响, 只是晶格常数在1. 25057~1.25101 nm 之间变化, 处于复合型石榴石铁氧体点阵常数1.23~1.28 nm之间。单胞分子数n 为7.75~7.80 , 单组分立方晶系石榴石型铁氧体单胞分子数应为8。掺Mn3 +的YGdCaVInIG铁氧体n< 8 , 说明最后形成的晶体结构中, 用Mn3+ 或其他离子置换Fe3+或Y3 + , 存在点阵空位。
二、结论
⒈YGdCaVInIG铁氧体是低磁矩、大功率微波铁氧体材料。
⒉以少量Mn3+替代Fe3 + ,可以提高铁氧体性能,Mn 掺入量以x为0.04~0.06 比较合适。
⒊最佳预烧温度为1050℃, 保温5h 。
Claims (2)
1.一种5G通信用自旋铁氧体材料,其特征在于:其配方分子式:
{Y3+ 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-,其中:
0≤a≤1,0≤b≤0.3,0≤c≤0.6,0.2≤d≤0.4,0.1≤e≤0.3,0.04≤x≤0.06。
2.一种如权利要求1所述的5G通信用自旋铁氧体材料的制备方法,其特征在于:包括如下步骤:
步骤1,配方设计
根据配方分子式{Y3+ 3-a-2b-d-eGd3+ aCa2+ 2bBi3+ dCu2+ e}〔Fe3+ 2-cIn3+ c〕(Fe3+ 3-b-xVb 5+Mn3+ x)O12 2-进行配方设计;
步骤2,称料
根据步骤1配方设计结果,计算并称取各种原料,所述原料为Fe2O3、Bi2O3、Y2O3、CuO、CaCO3、Gd2O3、In2O3、V2O5、Mn2O3;
步骤3,一次湿法球磨
将步骤2称取的各种原料混合装入球磨罐中,并加入球和稀释剂,进行原料一次湿法混合球磨;
步骤4,一次烧结
将经过步骤3后的浆料烘干,经过分样筛制备成粉料,然后放入烧结炉内进行烧结,温度为1050℃,时间为5h;
步骤5,二次湿法球磨
将经过步骤4的粉料,装入球磨罐中,加入球和稀释剂,进行二次湿法球磨,得到浆料;
步骤6,造粒
将步骤5球磨后的浆料烘干,然后加入胶合剂进行造粒;
步骤7,压制成型
将步骤6得到的颗粒放入模具进行压制,压制压强为50MPa-250Mpa,得到材料生坯;
步骤8,二次烧结
将步骤7得到生坯装入氧气气氛炉中进行二次烧结,烧结温度为900-1200℃,时间为5h。
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