CN111620682A - 梯度饱和磁化强度微波铁氧体材料、制成的铁氧体基板及其制备方法 - Google Patents

梯度饱和磁化强度微波铁氧体材料、制成的铁氧体基板及其制备方法 Download PDF

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CN111620682A
CN111620682A CN202010563037.0A CN202010563037A CN111620682A CN 111620682 A CN111620682 A CN 111620682A CN 202010563037 A CN202010563037 A CN 202010563037A CN 111620682 A CN111620682 A CN 111620682A
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saturation magnetization
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CN111620682B (zh
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杨菲
袁红兰
任仕晶
冯涛
廖杨
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CETC 9 Research Institute
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Abstract

本发明公开了一种梯度饱和磁化强度微波铁氧体材料,其原料的化学组成为BihGdkY3‑h‑k‑(a+c+2d+f)Caa+c+2d+ fSnaInbZrcVdAleGefFe5‑a‑b‑c‑d‑e‑f‑δ1O12、Ni1‑x+y‑ zZnxDynSnyCozMnmFe2‑2y‑m‑n‑δ2O4,其中,0≤a≤0.5,0≤b≤0.5,0≤c≤0.5,0≤d≤1.0,0≤e≤1.0;0≤f≤0.5;0≤h≤1.5;0≤k≤0.7;0≤x≤0.5;0≤y≤0.15;0≤z≤0.06;0≤m≤0.1;δ为缺铁量,0.02≤δ1≤0.3,0.02≤δ2≤0.2,上述原料在所述基板上形成至少两个不同的饱和磁化强度区域;本发明的梯度饱和磁化强度微波铁氧体基板上的饱和磁化强度梯度可在47kA/m~414kA/m范围内任意组合,其不同饱和磁化强度区域可为任意形状,通过不同梯度的饱和磁化强度组合解决微波器件小型化、集成化问题,以及倍频、三倍频宽带器件体积小型化、高隔离、低插耗的技术难题,本发明的制备方法工艺合理,适于推广应用。

Description

梯度饱和磁化强度微波铁氧体材料、制成的铁氧体基板及其 制备方法
技术领域
本发明涉及微波技术及磁性材料领域领域,尤其涉及一种梯度饱和磁化强度微波铁氧体基板及其制备方法。
背景技术
从现代微波通信设备系统、电子对抗系统、遥控遥测系统的集成化、模块化、小型多功能化的总体发展趋势。尤其是5G通讯的发展来看,对微波铁氧体器件的带宽、体积要求越来越高。传统的宽带微波铁氧体器件,其设计思路是基于单一性能的铁氧体材料,通过电路展宽带宽。单一性能的铁氧体材料其饱和磁化强度单一,最佳工作点只能在某一特定的区域,难以满足超倍频、三倍频的技术需求,在其基础上制作的器件性能无法实现宽带的高质量工作。通过多种不同饱和磁化强度铁氧体材料组合,组成梯度饱和磁化强度微波铁氧体材料,可为电路的宽带匹配提供更为丰富的工作区域,从而拓展器件带宽,解决超倍频、三倍频宽带器件高隔离、低插耗的技术难题。同样,电路设计对微波铁氧体器件体积小型化作用已趋于极致,通过同一材料上多个铁氧体材料结构匹配可以实现器件的小型化及集成化。
目前实用化的微波铁氧体材料主要有石榴石和尖晶石铁氧体。两类材料因各自晶系特点,应用于不同的微波频段。石榴石微波铁氧体具有各向异性场小、电阻率高、密度高、低磁损耗和窄共振线宽△H等优点,在微波低频段应用占统治地位。尖晶石微波铁氧体材料具有饱和磁化强度高、居里温度高、温度稳定性好、损耗低等特性,在X-毫米波段广泛应用。
石榴石铁氧体材料的烧结温度多在1350℃以上,尖晶石铁氧体材料烧结温度低于1250℃。两种材料的晶体结构、固相反应温度、烧结收缩率差异较大,传统方法不能将其结合在一起。
发明内容
本发明的目的之一,就在于提供一种梯度饱和磁化强度微波铁氧体材料,以解决上述问题。
为了实现上述目的,本发明采用的技术方案是这样的:一种梯度饱和磁化强度微波铁氧体材料,所述微波铁氧体原料的化学组成为BihGdkY3-h-k-(a+c+2d+f)Caa+c+2d+ fSnaInbZrcVdAleGefFe5-a-b-c-d-e-f-δ1O12、Ni1-x+y-zZnxDynSnyCozMnmFe2-2y-m-n-δ2O4,其中,0≤a≤0.5,0≤b≤0.5,0≤c≤0.5,0≤d≤1.0,0≤e≤1.0;0≤f≤0.5;0≤h≤1.5;0≤k≤0.7;0≤x≤0.5;0≤y≤0.15;0≤z≤0.06;0≤m≤0.1;0≤n≤0.1;δ为缺铁量,0.02≤δ1≤0.3,0.02≤δ2≤0.2,
上述原料中,BihGdkY3-h-k-(a+c+2d+f)Caa+c+2d+fSnaInbZrcVdAleGefFe5-a-b-c-d-e-f-δ1O1为石榴石铁氧体材料,Ni1-x+y-zZnxDynSnyCozMnmFe2-2y-m-n-δ2O4为尖晶石铁氧体材料,本发明的发明人通过大量试验,在前述的石榴石材料中加入Bi3+、Cu2+等低熔点离子降低其烧结温度;在前述的尖晶石材料中采用高熔点离子Dy3+取代Fe3+,提高其烧结温度;创造性地通过不同种类和不同含量的低熔点离子及高熔点离子取代,将两种体系的烧结温度调至相同,在同一块样品上实现饱和磁化强度47kA/m~414kA/m范围内一体化烧结。
本发明提供的梯度饱和磁化强度微波铁氧体材料针对传统铁氧体材料因其技术参数单一无法满足倍频程宽带器件需求以及微波器件小型化、集成化发展前景,克服现有铁氧体材料技术缺陷,使之兼具石榴石与尖晶石铁氧体材料的性能优点,通过不同饱和磁化强度微波铁氧体梯度材料使用,拓展器件带宽、减小器件体积,解决倍频、三倍频宽带器件高隔离、低插耗的技术难题,实现器件的小型化及集成化,尤其是5G用环行器及隔离器。
本发明的目的之二,在于提供采用上述材料制成的铁氧体基板,其技术方案为:所述原料在铁氧体基板上形成至少两个不同的饱和磁化强度区域,饱和磁化强度范围为47kA/m~414kA/m,所述不同的饱和磁化强度区域为任意形状。
本发明通过多种不同饱和磁化强度铁氧体材料组合,组成梯度饱和磁化强度微波铁氧体基板,可为电路的宽带匹配提供更为丰富的工作区域,从而拓展器件带宽,解决倍频、三倍频宽带器件高隔离、低插耗的技术难题。同样,电路设计对微波铁氧体器件体积小型化作用已趋于极致,通过同一基板上多个铁氧体材料结构匹配可以实现器件的小型化及集成化。
本发明的目的之三,在于提供一种上述的梯度饱和磁化强度微波铁氧体基板的制备方法,采用的技术方案为,包括以下步骤:
(1)配方设计,根据所述化学组成,按所需饱和磁化强度分别进行材料A、材料B、材料n配方设计;
(2)称料,根据步骤(1)中材料A、材料B、材料n配方设计结果,分别计算并称取所需各种原料,所述原料为Y2O3、Fe2O3、Bi2O3、Gd2O3、CaCO3、V2O5、ZrO2、SnO2、In2O3、Al(OH)3、GeO2、NiO、ZnO、Dy2O3、Co2O3、MnCO3
(3)原料一次湿法球磨,将步骤(2)称取的材料A、材料B、材料n原料分别装入球磨罐1、球磨罐2、球磨罐n中,并加入球和稀释剂,进行原料一次湿法混合球磨,分别得到一次浆料;
(4)预烧,将经步骤(3)处理后的材料A、材料B、材料n的一次浆料分别烘干及过筛,然后分别放入烧结炉内进行预烧,预烧温度为700℃~1260℃,保温2小时~7小时;
(5)二次湿法球磨,将经步骤(4)预烧后的材料A、材料B、材料n粉料,分别装入球磨罐1、球磨罐2、球磨罐n中,并加入球和稀释剂,进行二次湿法球磨,分别得到二次浆料;
(6)造粒,将步骤(5)球磨后的材料A、材料B、材料n的二次浆料分别烘干,然后加入胶合剂分别造粒;
(7)成型,将步骤(6)得到的材料A、材料B、材料n颗粒分别放入模具进行压制,压制压强为50MPa~250MPa,得到梯度饱和磁化强度微波铁氧体生坯;
(8)烧结,将步骤(7)得到生坯装入空气气氛或氧化气氛炉中进行烧结,即得梯度饱和磁化强度微波铁氧体毛坯;
(9)加工,将步骤(8)得到梯度饱和磁化强度微波铁氧体毛坯加工至所需尺寸,得到梯度饱和磁化强度微波铁氧体基板。
作为优选的技术方案:步骤(2)中的原料纯度为分析纯。
作为优选的技术方案:步骤(3)中,球:原料:稀释剂的质量比为(1.5~3.5):1:(0.4~1.5),球磨时间为1小时~24小时,所述球为不锈钢球或氧化锆球,所述稀释剂为去离子水或分析纯的无水酒精。
作为优选的技术方案:步骤(4)中所述分样筛规格大小为20目~60目。
作为优选的技术方案:步骤(5)中,球:粉料:稀释剂的质量比为(1.5~3.5):1:(0.4~1),球磨时间为1小时~24小时,所述球为不锈钢球或氧化锆球,所述稀释剂为去离子水或分析纯的无水酒精。
作为优选的技术方案:步骤(6)中,所述胶合剂为聚乙烯醇水溶液,浓度为5wt%~15wt%。
作为优选的技术方案:步骤(7)中,材料A、材料B、材料n在同一块生坯中分别成型出各梯度饱和磁化强度区域所需形状,成型压强为50MPa~250MPa。
作为优选的技术方案:步骤(8)中,所述烧结温度为900℃~1450℃,保温时间为2小时~20小时。
与现有技术相比,本发明的优点在于:传统的石榴石铁氧体及尖晶石铁氧体材料技术参数单一,无法满足超带宽及小型化微波器件要求;而本发明的梯度饱和磁化强度微波铁氧体基板上的饱和磁化强度梯度可在47kA/m~414kA/m范围内任意组合,其不同饱和磁化强度区域可为任意形状。通过不同梯度的饱和磁化强度组合解决微波器件小型化、集成化问题,以及超倍频、三倍频宽带器件体积小型化、高隔离、低插耗的技术难题。本发明的制备方法工艺合理,适于推广应用。
附图说明
图1为本发明梯度饱和磁化强度微波铁氧体基板制备方法工艺流程图;
图2为实施例1所得饱和磁化强度微波铁氧体基板结构示意图;
图3为实施例2所得饱和磁化强度微波铁氧体基板结构示意图;
图4为实施例3所得饱和磁化强度微波铁氧体基板结构示意图。
图中:1、材料A;2、材料B;3、材料C。
具体实施方式
下面将结合附图对本发明作进一步说明。
实施例1:
一种梯度饱和磁化强度微波铁氧体基板的制备方法,如图1所示,包括以下步骤:
(1)配方设计,根据组成化学式BihGdkY3-h-k-(a+c+2d+f)Caa+c+2d+ fSnaInbZrcVdAleGefFe5-a-b-c-d-e-f-δ1O12进行材料A1配方设计,其中a=0.25,b=0,c=0.15,d=0.5,e=0.28,f=0.12,h=0,k=0.1,δ1=0.02;根据组成化学式BihGdkY3-h-k-(a+c+2d+f)Caa+c+2d+fSnaInbZrcVdAleGefFe5-a-b-c-d-e-f-δ1O12进行材料B2配方设计,其中a=0.15,b=0.2,c=0,d=0,e=0,f=0,h=0.2,k=0,δ1=0.02;
(2)称料,根据步骤(1)中材料A1、材料B2配方设计结果,分别计算并称取所需各种原料,所述原料为Y2O3、Fe2O3、Bi2O3、Gd2O3、CaCO3、V2O5、ZrO2、SnO2、In2O3、Al(OH)3、GeO2
(3)原料一次湿法球磨,将步骤(2)称取的材料A1各种原料混合装入球磨罐1中,并按照氧化锆球:原料:稀释剂=3:1:1,加入氧化锆球和去离子水,进行材料一次湿法混合球磨,球磨时间为15小时;将步骤(2)称取的材料B2各种原料混合装入球磨罐2中,并按照氧化锆球:原料:稀释剂=3:1:1,加入氧化锆球和去离子水,进行材料一次湿法混合球磨,球磨时间为5小时;
(4)预烧,将经步骤(3)后的材料A1、材料B2浆料分别烘干,经过30目分样筛制备成相应粒径大小的粉料,然后放入烧结炉内进行预烧,预烧温度为1050℃,保温时间6小时;
(5)二次湿法球磨,将经步骤(4)后的材料A1粉料,装入球磨罐1中,并按照球:料:稀释剂=3:1:0.8,加入氧化锆球和去离子水,进行二次湿法球磨,球磨时间10小时;将经步骤(4)后的材料B2粉料,装入球磨罐2中,并按照球:料:稀释剂=3:1:0.8,加入不锈钢球和无水酒精,进行二次湿法球磨,球磨时间5小时;
(6)造粒,将步骤(5)球磨后的材料A1浆料烘干,然后加入浓度为9wt%的聚乙烯醇水溶液进行造粒;将步骤(5)球磨后的材料B2浆料烘干,然后加入浓度为9wt%的聚乙烯醇水溶液进行造粒;
(7)成型,将步骤(6)得到的材料A1、材料B2颗粒先后放入模具进行压制,压制压力为100MPa,得到梯度饱和磁化强度微波铁氧体生坯;
(8)烧结,将步骤(7)得到生坯装入空气气氛炉中进行烧结,烧结温度为1200℃,保温时间6小时,得到梯度饱和磁化强度微波铁氧体毛坯;
(9)加工,将步骤(8)得到的毛坯进行加工,得到φ10mm×1.5mm的梯度饱和磁化强度微波铁氧体基板,如图2所示。
梯度饱和磁化强度微波铁氧体样品经过相应加工后进行性能测试,电磁性能测试结果如表1所示。
表1实施例1制得的铁氧体电磁性能测试结果
Figure BDA0002546801080000081
实施例2:
一种梯度饱和磁化强度微波铁氧体基板的制备方法,包括以下步骤:
(1)配方设计,根据组成化学式Ni1-x+y-zZnxDynSnyCozMnmFe2-2y-m-n-δ2O4进行材料A1配方设计,其中x=0.2,y=0.1,z=0.01,m=0.08,n=0.02,δ2=0.1;根据组成化学式Ni1-x+y-zZnxDynSnyCozMnmFe2-2y-m-n-δ2O4进行材料B2配方设计,其中x=0.45,y=0,z=0.02,m=0.04,n=0.05,δ2=0.1;
(2)称料,根据步骤(1)中材料A1、材料B2配方设计结果,分别计算并称取所需各种原料,所述原料为Fe2O3、SnO2、NiO、ZnO、Dy2O3、Co2O3、MnCO3
(3)原料一次湿法球磨,将步骤(2)称取的材料A1各种原料混合装入球磨罐1中,并按照不锈钢球:原料:稀释剂=3:1:1,加入不锈钢球和无水酒精,进行材料一次湿法混合球磨,球磨时间为5小时;将步骤(2)称取的材料B2各种原料混合装入球磨罐2中,并按照不锈钢球:原料:稀释剂=3:1:1,加入不锈钢球和无水酒精,进行材料一次湿法混合球磨,球磨时间为5小时;
(4)预烧,将经步骤(3)后的材料A1、材料B2浆料分别烘干,经过30目分样筛制备成相应粒径大小的粉料,然后放入烧结炉内进行预烧,预烧温度为1050℃,保温时间6小时;
(5)二次湿法球磨,将经步骤(4)后的材料A1粉料,装入球磨罐1中,并按照球:料:稀释剂=3:1:0.8,加入不锈钢球和无水酒精,进行二次湿法球磨,球磨时间5小时;将经步骤(4)后的材料B2粉料,装入球磨罐2中,并按照球:料:稀释剂=3:1:0.8,加入不锈钢球和无水酒精,进行二次湿法球磨,球磨时间5小时;
(6)造粒,将步骤(5)球磨后的材料A1浆料烘干,然后加入浓度为9wt%的聚乙烯醇水溶液进行造粒;将步骤(5)球磨后的材料B2浆料烘干,然后加入浓度为9wt%的聚乙烯醇水溶液进行造粒;
(7)成型,将步骤(6)得到的材料A1、材料B2颗粒先后放入模具进行压制,压制压力为100MPa,得到梯度饱和磁化强度微波铁氧体生坯;
(8)烧结,将步骤(7)得到生坯装入空气气氛炉中进行烧结,烧结温度为1200℃,保温时间6小时,得到梯度饱和磁化强度微波铁氧体毛坯;
(9)加工,将步骤(8)得到的毛坯进行加工,得到20mm×17mm×0.8mm的梯度饱和磁化强度微波铁氧体基板,如图3所示。
梯度饱和磁化强度微波铁氧体样品经过相应加工后进行性能测试,电磁性能测试结果如表2所示。
表2实施例2制得的铁氧体电磁性能测试结果
Figure BDA0002546801080000091
实施例3:
一种梯度饱和磁化强度微波铁氧体基板的制备方法,包括以下步骤:
(1)配方设计,根据组成化学式BihGdkY3-h-k-(a+c+2d+f)Caa+c+2d+ fSnaInbZrcVdAleGefFe5-a-b-c-d-e-f-δ1O12进行材料A1配方设计,其中a=0.2,b=0.2,c=0,d=0.4,e=0.25,f=0,h=0,k=0.07,δ1=0.08;
根据组成化学式Ni1-x+y-zZnxDynSnyCozMnmFe2-2y-m-n-δ2O4进行材料B2配方设计,其中x=0.1,y=0.12,z=0,m=0.1,n=0.05,δ2=0.08;根据组成化学式Ni1-x+y- zZnxSnyCozMnmFe2-2y-m-n-δ2O4进行材料C3配方设计,其中x=0.2,y=0.02,z=0.05,m=0.05,n=0.2,δ2=0.05;
(2)称料,根据步骤(1)中材料A1、材料B2、材料C3配方设计结果,分别计算并称取所需各种原料,所述原料为Y2O3、Fe2O3、Bi2O3、Gd2O3、CaCO3、V2O5、ZrO2、SnO2、In2O3、Al(OH)3、GeO2、NiO、ZnO、Dy2O3、Co2O3、MnCO3
(3)原料一次湿法球磨,将步骤(2)称取的材料A1各种原料混合装入球磨罐1中,并按照氧化锆球:原料:稀释剂=3:1:1,加入氧化锆球和去离子水,进行材料一次湿法混合球磨,球磨时间为15小时;将步骤(2)称取的材料B2各种原料混合装入球磨罐2中,并按照氧化锆球:原料:稀释剂=3:1:1,加入氧化锆球和无水酒精,进行材料一次湿法混合球磨,球磨时间为5小时;将步骤(2)称取的材料C3各种原料混合装入球磨罐3中,并按照氧化锆球:原料:稀释剂=3:1:1,加入氧化锆球和无水酒精,进行材料一次湿法混合球磨,球磨时间为5小时;
(4)预烧,将经步骤(3)后的材料A1、材料B2、材料C3浆料分别烘干,经过30目分样筛制备成相应粒径大小的粉料,然后放入烧结炉内进行预烧,预烧温度为1100℃,保温时间6小时;
(5)二次湿法球磨,将经步骤(4)后的材料A1粉料,装入球磨罐1中,并按照球:料:稀释剂=3:1:0.8,加入氧化锆球和去离子水,进行二次湿法球磨,球磨时间5小时;将经步骤(4)后的材料B2粉料,装入球磨罐1中,并按照球:料:稀释剂=3:1:0.8,加入氧化锆球和无水酒精,进行二次湿法球磨,球磨时间5小时;将经步骤(4)后的材料C3粉料,装入球磨罐1中,并按照球:料:稀释剂=3:1:0.8,加入氧化锆球和无水酒精,进行二次湿法球磨,球磨时间5小时;
(6)造粒,将步骤(5)球磨后的材料A1浆料烘干,然后加入浓度为8wt%的聚乙烯醇水溶液进行造粒;将步骤(5)球磨后的材料B2浆料烘干,然后加入浓度为9wt%的聚乙烯醇水溶液进行造粒;将步骤(5)球磨后的材料C3浆料烘干,然后加入浓度为9wt%的聚乙烯醇水溶液进行造粒;
(7)成型,将步骤(6)得到的材料A1、材料B2、材料C3颗粒先后放入模具进行压制,压制压力为100MPa,得到梯度饱和磁化强度微波铁氧体生坯;
(8)烧结,将步骤(7)得到生坯装入空气气氛炉中进行烧结,烧结温度为1300℃,保温时间6小时,得到梯度饱和磁化强度微波铁氧体毛坯;
(9)加工,将步骤(8)得到的毛坯进行加工,得到20mm×18mm×1.2mm的梯度饱和磁化强度微波铁氧体基板,如图4所示。
梯度饱和磁化强度微波铁氧体样品经过相应加工后进行性能测试,电磁性能测试结果如表3所示。
表3实施例3制得的铁氧体电磁性能测试结果
Figure BDA0002546801080000121
上述实施例1、实施例2和实施例3,对本发明的技术方案,有益效果做了进一步详细说明,但是不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思的前提下,所做的任何修改、等同替换、改进等,都应当视为属于本发明的保护范围。

Claims (9)

1.一种梯度饱和磁化强度微波铁氧体材料,其特征在于:其原料的化学组成为BihGdkY3-h-k-(a+c+2d+f)Caa+c+2d+fSnaInbZrcVdAleGefFe5-a-b-c-d-e-f-δ1O12、Ni1-x+y- zZnxDynSnyCozMnmFe2-2y-m-n-δ2O4,其中,0≤a≤0.5,0≤b≤0.5,0≤c≤0.5,0≤d≤1.0,0≤e≤1.0;0≤f≤0.5;0≤h≤1.5;0≤k≤0.7;0≤x≤0.5;0≤y≤0.15;0≤z≤0.06;0≤m≤0.1;0≤n≤0.1;δ为缺铁量,0.02≤δ1≤0.3,0.02≤δ2≤0.2。
2.采用权利要求1的材料所制成的铁氧体基板,其特征在于:所述原料在铁氧体基板上形成至少两个不同的饱和磁化强度区域,饱和磁化强度范围为47kA/m~414kA/m,所述不同的饱和磁化强度区域为任意形状。
3.权利要求2所述的梯度饱和磁化强度微波铁氧体基板的制备方法,其特征在于,包括以下步骤:
(1)配方设计,根据所述化学组成,按所需饱和磁化强度分别进行材料A、材料B、材料n配方设计;
(2)称料,根据步骤(1)中材料A、材料B、材料n配方设计结果,分别计算并称取所需各种原料,所述原料为Y2O3、Fe2O3、Bi2O3、Gd2O3、CaCO3、V2O5、ZrO2、SnO2、In2O3、Al(OH)3、GeO2、NiO、ZnO、Dy2O3、Co2O3、MnCO3
(3)原料一次湿法球磨,将步骤(2)称取的材料A、材料B、材料n原料分别装入球磨罐1、球磨罐2、球磨罐n中,并加入球和稀释剂,进行原料一次湿法混合球磨,分别得到一次浆料;
(4)预烧,将经步骤(3)处理后的材料A、材料B、材料n的一次浆料分别烘干及过筛,然后分别放入烧结炉内进行预烧,预烧温度为700℃~1260℃,保温2小时~7小时;
(5)二次湿法球磨,将经步骤(4)预烧后的材料A、材料B、材料n粉料,分别装入球磨罐1、球磨罐2、球磨罐n中,并加入球和稀释剂,进行二次湿法球磨,分别得到二次浆料;
(6)造粒,将步骤(5)球磨后的材料A、材料B、材料n的二次浆料分别烘干,然后加入胶合剂分别造粒;
(7)成型,将步骤(6)得到的材料A、材料B、材料n颗粒分别放入模具进行压制,压制压强为50MPa~250MPa,得到梯度饱和磁化强度微波铁氧体生坯;
(8)烧结,将步骤(7)得到生坯装入空气气氛或氧化气氛炉中进行烧结,即得梯度饱和磁化强度微波铁氧体毛坯;
(9)加工,将步骤(8)得到梯度饱和磁化强度微波铁氧体毛坯加工至所需尺寸,得到梯度饱和磁化强度微波铁氧体基板。
4.根据权利要求3所述的制备方法,其特征在于:步骤(3)中,球:原料:稀释剂的质量比为(1.5~3.5):1:(0.4~1.5),球磨时间为1小时~24小时,所述球为不锈钢球或氧化锆球,所述稀释剂为去离子水或分析纯的无水酒精。
5.根据权利要求3所述的制备方法,其特征在于:步骤(4)中所述分样筛规格大小为20目~60目。
6.根据权利要求3所述的制备方法,其特征在于:步骤(5)中,球:粉料:稀释剂的质量比为(1.5~3.5):1:(0.4~1),球磨时间为1小时~24小时,所述球为不锈钢球或氧化锆球,所述稀释剂为去离子水或分析纯的无水酒精。
7.根据权利要求3所述的制备方法,其特征在于:步骤(6)中,所述胶合剂为聚乙烯醇水溶液,浓度为5wt%~15wt%。
8.根据权利要求3所述的制备方法,其特征在于:步骤(7)中,材料A、材料B、材料n在同一块生坯中分别成型出各梯度饱和磁化强度区域所需形状,成型压强为50MPa~250MPa。
9.根据权利要求3所述的制备方法,其特征在于:步骤(8)中,所述烧结温度为900℃~1450℃,保温时间为2小时~20小时。
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