CN112430080A - 一种高功率和高剩磁比的石榴石铁氧体材料及其制备方法 - Google Patents

一种高功率和高剩磁比的石榴石铁氧体材料及其制备方法 Download PDF

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CN112430080A
CN112430080A CN202011160669.9A CN202011160669A CN112430080A CN 112430080 A CN112430080 A CN 112430080A CN 202011160669 A CN202011160669 A CN 202011160669A CN 112430080 A CN112430080 A CN 112430080A
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ball milling
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李小靖
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Beijing Institute of Radio Measurement
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Abstract

本发明公开一种高功率和高剩磁比的石榴石铁氧体材料及其制备方法。本发明首先提供了高功率和高剩磁比的石榴石铁氧体材料，化学式为Y3‑a‑b‑(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5‑c‑d‑e‑f‑g‑δO12，其中0≤a≤1.5，0.01≤b≤0.1，0≤c≤0.3，0≤d≤0.3，0≤e≤0.3，0≤f≤0.15，0≤g≤0.5，0≤δ≤0.3，且a和b不同时为0，δ为工艺缺铁量。本发明进一步提供了上述材料的制备方法。本发明石榴石铁氧体材料，兼具高自选波线宽ΔHk、高剩磁比Rs和低的电磁损耗，能满足包括锁式微波铁氧体器件在内的各类微波器件对高功率材料的需求。

Description

一种高功率和高剩磁比的石榴石铁氧体材料及其制备方法
技术领域
本发明涉及微波技术和磁性材料技术领域。更具体地，涉及一种高功率和高剩磁比的石榴石铁氧体材料及其制备方法。
背景技术
低场下工作的微波铁氧体器件，当微波激励功率超过某一临界值Pc(Pc∝hc2，hc为激发自旋波的临界微波磁场，也就是高功率非线性效应临界场)时，自旋波迅速增长，导致材料非线性损耗迅速增大。为了提高微波铁氧体器件承受峰值功率的能力，对铁氧体材料来说就必须提高hc，材料的hc与材料的自旋波线宽ΔHk成正比，因此具备高功率承受能力的铁氧体就是ΔHk尽可能大的铁氧体。表征微波铁氧体材料损耗性能的共振线宽ΔH(其值越低材料损耗越小)，以及表征材料高功率特性的自旋波线宽ΔHk，在材料的配方设计中是相互矛盾的，单一追求其中一个指标高是相对容易的。
虽然关于高功率石榴石铁氧体材料及制备方法已有研究，但为了获得小的损耗和较高的居里温度基本都以钇钆钙钒石榴石为基础配方进行离子取代获得所需的性能。钇钆钙钒石榴石铁氧体因其剩磁比(Br/Bm)比较低(特别是在CaV的取代量比较大的时候剩磁比往往低于0.7)，更适用于隔离器和环行器这类对剩磁比没有要求的恒场微波器件。而移相器和开关这类锁式微波器件要求石榴石材料的剩磁比最好在0.75以上，剩磁比越高越有利于器件的小型化和承受更高的峰值功率。目前的高功率石榴石铁氧体的研究要么只列出了共振线宽ΔH数据要么只给出了自旋波线宽ΔHk数据，难以同时具备高功率和小损耗特性。更缺乏同时具备高功率和高剩磁比性能的石榴石材料满足高功率移相器和开关对材料的需求。
因此，需要提供一种能同时具备高功率和高剩磁比性能的石榴石铁氧体材料。
发明内容
本发明的一个目的在于提供一种同时具备高功率、高剩磁比和低损耗的石榴石铁氧体材料，以满足包括锁式微波铁氧体器件在内的各类微波器件对高功率材料的需求。
本发明的另一个目的在于提供一种上述石榴石铁氧体材料的制备方法。
为达到上述目的，本发明采用下述技术方案：
本发明提供了一种高功率和高剩磁比的石榴石铁氧体材料，为单相石榴石结构，其化学式为Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中0≤a≤1.5，0.01≤b≤0.1，0≤c≤0.3，0≤d≤0.3，0≤e≤0.3，0≤f≤0.15，0≤g≤0.5，0≤δ≤0.3，且a和b不同时为0，δ为工艺缺铁量。
本发明还提供了上述高功率和高剩磁比的石榴石铁氧体材料的制备方法，包括以下步骤：
配料：按化学式为Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中0≤a≤1.5，0.01≤b≤0.1，0≤c≤0.3，0≤d≤0.3，0≤e≤0.3，0≤f≤0.15，0≤g≤0.5，0≤δ≤0.3，且a和b不同时为0，δ为工艺缺铁量，计算并称取各种原料，所述原料为Y2O3、Gd2O3、Dy2O3、CaCO3、GeO2、ZrO2、In2O3、Al2O3、MnCO3、Fe2O3；
一次球磨：将各原料、钢球和弥散剂放入球磨机，进行一次球磨，得到一次浆料；
一次烘干：将一次浆料烘干去除弥散剂，得到一次粉料；
预烧：将一次粉料进行预烧，得到预烧后的粉料；
二次球磨：将预烧后的粉料、钢球和弥散剂进行二次球磨，得到二次浆料；
二次烘干：将二次浆料烘干去除弥散剂，得到二次粉料；
造粒：在二次粉料中加入粘合剂进行造粒，得到粒料；
成型：将粒料进行压制成型，得到坯件；
烧结：将坯件进行烧结，得到石榴石铁氧体材料。
为了满足高功率、高剩磁比和小损耗的要求，本发明在原料设计时采用Y、Gd、Al系列为基础配方并通过Mn的微量掺杂提高磁滞回线的矩形度(剩磁比)；通过Gd和Dy的联合取代提高自选波线宽ΔHk实现高功率特性；通过In、Zr的少量取代降低共振线宽ΔH实现小损耗特性；通过Gd、Al和Ge的组合取代调控饱和磁化强度4πMs以适合不同频率器件选用。
进一步，所述一次球磨中各原料的总质量、钢球和弥散剂的质量比为1:2～4:0.9～1.5，一次球磨的时间22h～35h；优选的，所述弥散剂为水，更优选的为去离子水或蒸馏水。
进一步，所述预烧中预烧的温度为1180℃～1250℃，时间为4h～6h。
进一步，所述二次球磨中预烧后的粉料、钢球和弥散剂的质量比1:2～4:0.8～1.2，二次球磨的时间22h～35h；优选的，所述弥散剂为水，更优选的为去离子水或蒸馏水。
进一步，所述造粒中粘合剂为聚乙烯醇的水溶液，其添加量为二次粉料重量的10wt％～18wt％。
进一步，所述成型中成型的压力为1000kg/cm2～1600kg/cm2。
进一步，所述烧结中烧结的温度为1400℃～1460℃，时间为4h～6h。
本发明的有益效果如下：
本发明高功率和高剩磁比的石榴石铁氧体材料，兼具高自选波线宽ΔHk、高剩磁比Rs(20Oe外场下测试)和低的电磁损耗，其中，介电损耗tanδe≤2×10-4，共振线宽ΔH≤85Oe，自选波线宽ΔHk≥15Oe，剩磁比Rs≥0.75，饱和磁化强度4πMs在500Gs～1900Gs可调，不但可满足低场工作承受高峰值功率的环行器和隔离器的需求，而且可以满足大功率下工作的锁式器件(移相器和开关等)对具备高剩磁比的高功率材料的需求，材料饱和磁化强度4πMs形成系列化，提供频率S～X波段高功率器件选用。
具体实施方式
为了更清楚地说明本发明，下面结合优选实施例对本发明做进一步的说明。本领域技术人员应当理解，下面所具体描述的内容是说明性的而非限制性的，不应以此限制本发明的保护范围。
实施例1一种高功率和高剩磁比的石榴石铁氧体材料的制备方法
一种高功率和高剩磁比的石榴石铁氧体材料，单相石榴石结构，化学式为Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝c＝d＝e＝g＝0，b＝0.06，f＝0.04，δ＝0.2。
具体制备方法如下：
配料：根据化学式Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝c＝d＝e＝g＝0，b＝0.06，f＝0.04，δ＝0.2，计算并称取各种原料，所述原料为Y2O3、Dy2O3、MnCO3、Fe2O3。
一次球磨：将各原料、钢球、蒸馏水装入滚动式球磨机，各原料的总质量、钢球、去离子水的质量比为1:3:0.9，滚动球磨22h，得到浆料。
一次烘干：将球磨后的浆料倒入钢盘中，放入烘箱烘干，得到粉料。
预烧：将烘干后的粉料装入坩埚中，放入钟罩炉内在空气气氛中预烧，预烧的温度为1220℃，时间5h，得到预烧后的粉料。
二次球磨：将预烧后的粉料、钢球、蒸馏水装入滚动式球磨机，粉料、钢球、去离子水的质量比为1:3:0.9，滚动球磨24h，得到浆料。
二次烘干：将球磨后的料浆倒入钢盘中，放入烘箱烘干，得到粉料。
造粒：将聚乙烯醇的水溶液(其重量是粉料重量的15wt％)加入粉料中进行造粒，得到粒料。
成型：将造粒后的粒料放入所需形状的模具，用压机压制成型为相应的压坯坯件，压制成型的压力为1400kg/cm2，得到压坯。
烧结：将坯件装入匣钵中，放入钟罩炉中在空气气氛中烧结，烧结温度1420℃，时间5h，得到石榴石铁氧体材料。
具体性能参数如表1所示。
实施例2一种高功率和高剩磁比的石榴石铁氧体材料的制备方法
一种高功率高剩磁比石榴石铁氧体材料，单相石榴石结构，化学式为Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝0.9，b＝0.04，c＝d＝g＝0，e＝0.1，f＝0.04，δ＝0.2。
具体制备方法如下：
配料：根据化学式Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝0.9，b＝0.04，c＝d＝g＝0，e＝0.1，f＝0.04，δ＝0.2，计算并称取各种原料，所述原料为Y2O3、Gd2O3、Dy2O3、In2O3、MnCO3、Fe2O3。
一次球磨：将各原料、钢球、蒸馏水装入滚动式球磨机，各原料的总质量、钢球、去离子水的质量比为1:3:0.8，滚动球磨30h，得到浆料。
一次烘干：将球磨后的浆料倒入钢盘中，放入烘箱烘干，得到粉料。
预烧：将烘干后的粉料装入坩埚中，放入钟罩炉内在空气气氛中预烧，预烧的温度为1240℃，时间5h，得到预烧后的粉料。
二次球磨：将预烧后的粉料、钢球、蒸馏水装入滚动式球磨机，粉料、钢球、去离子水的质量比为1:3:0.8，滚动球磨24h，得到浆料。
二次烘干：将球磨后的浆料倒入钢盘中，放入烘箱烘干，放入烘箱烘干，得到粉料。
造粒：将聚乙烯醇的水溶液(其重量是粉料重量的15wt％)加入粉料中进行造粒，得到粒料。
成型：将造粒后的粒料放入所需形状的模具，用压机压制成型为相应的压坯坯件，压制成型的压力为1400kg/cm2，得到压坯。
烧结：将坯件装入匣钵中，放入钟罩炉中在空气气氛中烧结，烧结温度1430℃，时间5h，得到石榴石铁氧体材料。
具体性能参数如表1所示。
实施例3一种高功率和高剩磁比的石榴石铁氧体材料的制备方法
一种高功率高剩磁比石榴石铁氧体材料，单相石榴石结构，化学式为Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝1.3，b＝0.04，d＝e＝0.1，c＝g＝0，f＝0.04，δ＝0.2。
具体制备方法如下：
配料：根据化学式Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝1.3，b＝0.04，d＝e＝0.1，c＝g＝0，f＝0.04，δ＝0.2，计算并称取各种原料，所述原料为Y2O3、Gd2O3、Dy2O3、CaCO3、ZrO2、In2O3、MnCO3、Fe2O3。
一次球磨：将各原料、钢球、蒸馏水装入滚动式球磨机，各原料的总质量、钢球、去离子水的质量比为1:3:1.2，滚动球磨22h，得到浆料。
一次烘干：将球磨后的浆料倒入钢盘中，放入烘箱烘干，得到粉料。
预烧：将烘干后的粉料装入坩埚中，放入钟罩炉内在空气气氛中预烧，预烧温度为1210℃，时间5h，得到预烧后的粉料。
二次球磨：将预烧后的粉料、钢球、蒸馏水装入滚动式球磨机，粉料、钢球、去离子水的质量比为1:3:1.0，滚动球磨35h，得到浆料。
二次烘干：将球磨后的浆料倒入钢盘中，放入烘箱烘干，得到粉料。
造粒：将聚乙烯醇的水溶液(其重量是粉料重量的15wt％)加入粉料中进行造粒，得到粒料。
成型：将造粒后的粒料放入所需形状的模具，用压机压制成型为相应的压坯坯件，压制成型的压力为1400kg/cm2，得到压坯。
烧结：将坯件装入匣钵中，放入钟罩炉中在空气气氛中烧结，烧结温度1420℃，时间5h，得到石榴石铁氧体材料。
具体性能参数如表1所示。
实施例4一种高功率和高剩磁比的石榴石铁氧体材料的制备方法
一种高功率高剩磁比石榴石铁氧体材料，单相石榴石结构，化学式为Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝0.8，b＝0.04，c＝d＝0，e＝0.1，g＝0.5，f＝0.04，δ＝0.15。制备方法如下：
具体制备方法如下：
配料：根据化学式Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝0.8，b＝0.04，c＝d＝0，e＝0.1，g＝0.5，f＝0.04，δ＝0.15，计算并称取各种原料，所述原料为Y2O3、Gd2O3、Dy2O3、In2O3、MnCO3、Al2O3、Fe2O3。
一次球磨：将各原料、钢球、蒸馏水装入滚动式球磨机，各原料的总质量、钢球、去离子水的质量比为1:3:0.9，滚动球磨28h，得到浆料。
一次烘干：将球磨后的的浆料倒入钢盘中，放入烘箱烘干，得到粉料。
预烧：将烘干后的粉料装入坩埚中，放入钟罩炉内在空气气氛中预烧，预烧温度为1250℃，时间5h，得到预烧后的粉料。
二次球磨：将预烧后的粉料、钢球、蒸馏水装入滚动式球磨机，粉料、钢球、去离子水的质量比为1:3:0.9，滚动球磨24h，得到浆料。
二次烘干：将球磨后的的浆料倒入钢盘中，放入烘箱烘干，得到粉料。
造粒：将聚乙烯醇的水溶液(其重量是粉料重量的10wt％)加入粉料中进行造粒，得到粒料。
成型：将造粒后的粒料放入所需形状的模具，用压机压制成型为相应的压坯坯件，压制成型的压力为1000kg/cm2，得到压坯。
烧结：将坯件装入匣钵中，放入钟罩炉中在空气气氛中烧结，烧结温度1460℃，时间5h，得到石榴石铁氧体材料。
具体性能参数如表1所示。
实施例5一种高功率和高剩磁比的石榴石铁氧体材料的制备方法
一种高功率高剩磁比石榴石铁氧体材料，单相石榴石结构，化学式为Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝1.1，b＝0.02，c＝0.2，d＝0，e＝0.1，g＝0.3，f＝0.04，δ＝0.18。制备方法如下：
具体制备方法如下：
配料：根据化学式Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中a＝1.1，b＝0.02，c＝0.2，d＝0，e＝0.1，g＝0.3，f＝0.04，δ＝0.18，计算并称取各种原料，所述原料为Y2O3、Gd2O3、Dy2O3、CaCO3、GeO2、In2O3、MnCO3、Al2O3、Fe2O3。
一次球磨：将各原料、钢球、蒸馏水装入滚动式球磨机，各原料的总质量、钢球、去离子水的质量比为1:3:1.4，滚动球磨22h，得到浆料。
一次烘干：将球磨后的的浆料倒入钢盘中，放入烘箱烘干，得到粉料。
预烧：将烘干后的粉料装入坩埚中，放入钟罩炉内在空气气氛中预烧，预烧温度为1200℃，，时间5h，得到预烧后的粉料。
二次球磨：将预烧后的粉料、钢球、蒸馏水装入滚动式球磨机，粉料、钢球、去离子水的质量比为1:3:1.0，滚动球磨24h，得到浆料。
二次烘干：将球磨后的浆料倒入钢盘中，放入烘箱烘干，得到粉料。
造粒：将聚乙烯醇的水溶液(其重量是粉料重量的18wt％)加入粉料中进行造粒，得到粒料。
成型：将造粒后的粒料放入所需形状的模具，用压机压制成型为相应的压坯坯件，压制成型的压力为1600kg/cm2，得到压坯。
烧结：将坯件装入匣钵中，放入钟罩炉中在空气气氛中烧结，烧结温度1395℃，时间5h，得到石榴石铁氧体材料。
具体性能参数如表1所示。
表1实施例1～5石榴石铁氧体材料的电磁性能
Figure BDA0002744212680000071
注：剩磁比的测试外场为20Oe，达到15Hc～20Hc，确保磁化充分。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定，对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动，这里无法对所有的实施方式予以穷举，凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之列。

Claims (10)

1.一种高功率和高剩磁比的石榴石铁氧体材料，其特征在于，所述石榴石铁氧体材料为单相石榴石结构，其化学式为Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中0≤a≤1.5，0.01≤b≤0.1，0≤c≤0.3，0≤d≤0.3，0≤e≤0.3，0≤f≤0.15，0≤g≤0.5，0≤δ≤0.3，且a和b不同时为0，δ为工艺缺铁量。
2.一种如权利要求1所述的石榴石铁氧体材料的制备方法，其特征在于，包括以下步骤：
配料：按化学式为Y3-a-b-(c+d)GdaDybCa(c+d)GecZrdIneMnfAlgFe5-c-d-e-f-g-δO12，其中0≤a≤1.5，0.01≤b≤0.1，0≤c≤0.3，0≤d≤0.3，0≤e≤0.3，0≤f≤0.15，0≤g≤0.5，0≤δ≤0.3，且a和b不同时为0，δ为工艺缺铁量，计算并称取各种原料，所述原料为Y2O3、Gd2O3、Dy2O3、CaCO3、GeO2、ZrO2、In2O3、Al2O3、MnCO3、Fe2O3；
一次球磨：将各原料、钢球和弥散剂放入球磨机，进行一次球磨，得到一次浆料；
一次烘干：将一次浆料烘干去除弥散剂，得到一次粉料；
预烧：将一次粉料进行预烧，得到预烧后的粉料；
二次球磨：将预烧后的粉料、钢球和弥散剂进行二次球磨，得到二次浆料；
二次烘干：将二次浆料烘干去除弥散剂，得到二次粉料；
造粒：在二次粉料中加入粘合剂进行造粒，得到粒料；
成型：将粒料进行压制成型，得到坯件；
烧结：将坯件进行烧结，得到石榴石铁氧体材料。
3.根据权利要求2所述的制备方法，其特征在于，所述一次球磨中各原料的总质量、钢球和弥散剂的质量比为1:2～4:0.9～1.5；优选的，所述一次球磨的时间为22h～35h。
4.根据权利要求2所述的制备方法，其特征在于，所述预烧中预烧的温度为1180℃～1250℃，时间为4h～6h。
5.根据权利要求2所述的制备方法，其特征在于，所述二次球磨中预烧后的粉料、钢球和弥散剂的质量比1:2～4:0.8～1.2；，优选的，所述二次球磨的时间为22h～35h。
6.根据权利要求3或5所述的制备方法，其特征在于，所述弥散剂为水，优选的为去离子水或蒸馏水。
7.根据权利要求2所述的制备方法，其特征在于，所述造粒中粘合剂为聚乙烯醇的水溶液。
8.根据权利要求7所述的制备方法，其特征在于，所述粘合剂的添加量为二次粉料重量的10wt％～18wt％。
9.根据权利要求2所述的制备方法，其特征在于，所述成型中压制成型的压力为1000kg/cm2～1600kg/cm2。
10.根据权利要求2所述的制备方法，其特征在于，所述烧结中烧结的温度为1400℃～1460℃，时间为4h～6h。
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