CN114591076A - 一种石榴石铁氧体材料及其制备方法 - Google Patents
一种石榴石铁氧体材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 53
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 44
- 239000002223 garnet Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims description 40
- 239000002994 raw material Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000005469 granulation Methods 0.000 claims description 12
- 230000003179 granulation Effects 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 7
- 239000011656 manganese carbonate Substances 0.000 claims description 7
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
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- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 239000011363 dried mixture Substances 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 5
- 229910001679 gibbsite Inorganic materials 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910000831 Steel Inorganic materials 0.000 description 8
- 239000010959 steel Substances 0.000 description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 230000005350 ferromagnetic resonance Effects 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
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- 238000005342 ion exchange Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- -1 oxygen ion Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
本申请提供了一种石榴石铁氧体材料及其制备方法，所述石榴石铁氧体材料的化学式为Y3‑x‑yDyxCayFe5‑y‑z‑aSiyMnzAlaO12，其中，0.01≤x≤0.03，0.01≤y≤0.02，0.02≤z≤0.09，0≤a≤0.05。本申请的石榴石铁氧体材料在制备过程中可以降低烧结温度，提高材料致密度，降低损耗。
Description
技术领域
本申请属于磁性材料技术领域，特别涉及一种石榴石铁氧体材料及其制备方法。
背景技术
随着相控阵雷达技术的飞速发展，对作为解决雷达接收设备和发射设备相互干扰、级间隔离及阻抗匹配等问题的微带环行器的性能提出了更加严苛的要求，在高功率、低损耗、宽频带、高稳定性和高可靠性的严苛要求下，微波铁氧体材料的性能要求也在不断提高。
石榴石铁氧体的氧离子间隙全部被金属阳离子占据，因此铁磁共振线宽、介电损耗相比尖晶石结构要低，通过离子置换能够灵活改变饱和磁化强度及温度稳定性等。微带环行器作为相控阵天线的重要器件之一，对插入损耗、功率、隔离具有要求极高，因此，作为微带环行器核心的铁氧体需要具有低损耗、高功率的特性。
目前石榴石铁氧体的性能依然存在着低功率、高损耗、低致密性等问题。
发明内容
本申请的目的是提供了一种石榴石铁氧体材料，以解决或减轻背景技术中的至少一个问题。
首先，本申请提供了一种石榴石铁氧体材料，所述石榴石铁氧体材料的化学式为Y3-x-yDyxCayFe5-y-z-aSiyMnzAlaO12，其中，0.01≤x≤0.03，0.01 ≤y≤0.02，0.02≤z≤0.09，0≤a≤0.05。
进一步的，所述石榴石铁氧体材料的制备原材料包括Y2O3、Dy2O3、 CaCO3、Fe2O3、SiO2、MnCO3，Al(OH)3，纯度不低于99wt％。
另外，本申请中提供了一种制备如上的石榴石铁氧体材料的制备方法，所述制备方法包括：
1)根据石榴石铁氧体材料的化学式计算并称取所需原材料的重量；
2)将原材料放入球磨机中进行一次球磨，球磨后烘干；
3)将烘干后的混合物放入烧结炉内预烧，并保温若干小时；
4)将预烧后的烧结物放入球磨机中进行二次球磨，球磨后烘干；
5)将二次球磨后的混合物中加入聚乙烯醇水溶液造粒；
6)将造粒后得到的颗粒在模具内压制得到生坯件；
7)将压制生坯件放入烧结炉内烧结，保温若干时间后得到所述石榴石铁氧体材料。
进一步的，一次球磨和二次球磨时，采用蒸馏水作为浸没原料。
进一步的，二次球磨后的混合物中加入的聚乙烯醇水溶液质量比为 (4～8)％，重量比为(6～8)wt％。
最后，本申请中提高了一种环形器，所述环形器应用于如上任一项所述的石榴石铁氧体材料。
具体实施方式
为使本申请实施的目的、技术方案和优点更加清楚，下面将结合本申请具体的实施例，对本申请的技术方案进行更加详细的描述。
实施例1：
本实施例中提供了一种石榴石铁氧体材料，该实施例中的石榴石铁氧体材料的化学式为Y3-x-yDyxCayFe5-y-z-aSiyMnzAlaO12，其中，x＝0.02， y＝0.02，z＝0.02，a＝0.05。
制备上述实施例成分的石榴石铁氧体材料的的制备方法包括如下具体步骤：
1)根据化学式Y3-x-yDyxCayFe5-y-z-aSiyMnzAlaO12，其中，x＝0.02、y＝0.02、 z＝0.02、a＝0.05计算并称取所需原材料，所需原材料为Y2O3、Dy2O3、 CaCO3、Fe2O3、SiO2、MnCO3和Al(OH)3；
2)将上述原材料放入球磨机中进行一次球磨24小时后烘干，球磨时料、钢球、蒸馏水的比例为1:2.5:1；
3)将烘干后的混合物放入烧结炉内1200℃预烧，保温5小时；
4)将预烧后的烧结体放入球磨机中进行二次球磨后烘干，球磨时间 22小时，球磨时料、钢球、蒸馏水的比例为1:3:0.6；
5)将二次球磨后的混合物加入质量比为4％、重量比8Wt％的聚乙烯醇水溶液造粒；
6)将造粒后得到的颗粒在模具内压制制得生坯件；
7)将压制生坯件放入烧结炉内1500℃烧结，保温8小时，从而得到该实施例成分的石榴石铁氧体材料。
实施例2：
本实施例中提供了一种石榴石铁氧体材料，该实施例中的石榴石铁氧体材料的化学式为Y3-x-yDyxCayFe5-y-z-aSiyMnzAlaO12，其中，x＝0.03， y＝0.015，z＝0.09，a＝0。
制备上述实施例成分的石榴石铁氧体材料的的制备方法包括如下具体步骤：
1)根据化学式Y3-x-yDyxCayFe5-y-z-aSiyMnzAlaO12，其中x＝0.03，y＝0.015， z＝0.09，a＝0计算并称取所需原材料，所需原材料为Y2O3、Dy2O3、CaCO3、 Fe2O3、SiO2、MnCO3，Al(OH)3；
2)将原材料放入球磨机中进行一次球磨24小时后烘干，球磨时料、钢球、蒸馏水的比例为1:2.5:0.7；
3)将烘干后的混合物放入烧结炉内1150℃预烧，保温6小时；
4)将预烧后的烧结物放入球磨机中进行二次球磨后烘干，球磨时间 22小时，球磨时料、钢球、蒸馏水的比例为1:2.5:1；
5)将二次球磨后的组分加入质量比为8％、重量比6Wt％的聚乙烯醇水溶液造粒；
6)将造粒后得到的颗粒在模具内压制制得生坯件；
7)将压制生坯件放入烧结炉内1450℃烧结，保温6小时，从而得到该实施例成分的石榴石铁氧体材料。
实施例3：
本实施例中提供了一种石榴石铁氧体材料，该实施例中的石榴石铁氧体材料的化学式为Y3-x-yDyxCayFe5-y-z-aSiyMnzAlaO12，其中，x＝0.01， y＝0.01，z＝0.05，a＝0.025。
制备上述实施例成分的石榴石铁氧体材料的的制备方法包括如下具体步骤：
1)根据化学式Y3-x-yDyxCayFe5-y-z-aSiyMnzAlaO12，其中，x＝0.01，y＝0.01， z＝0.05，a＝0.025计算并称取所需原材料，所需原材料为Y2O3、Dy2O3、 CaCO3、Fe2O3、SiO2、MnCO3，Al(OH)3；
2)将原材料放入球磨机中进行一次球磨20小时后烘干，球磨时料、钢球、蒸馏水的比例为1:3:0.6；
3)将烘干后的混合物放入烧结炉内1100℃预烧，保温4小时；
4)将预烧后的烧结物放入球磨机中进行二次球磨后烘干，球磨时间 20小时，球磨时料、钢球、蒸馏水的比例为1:3:1；
5)将二次球磨后的组分加入质量比为6％、重量比6Wt％的聚乙烯醇水溶液造粒；
6)将造粒后得到的颗粒在模具内压制制得生坯件；
7)将压制生坯件放入烧结炉内1490℃烧结，保温6小时，从而得到该实施例成分的石榴石铁氧体材料。
实施例4：
本实施例中提供了一种石榴石铁氧体材料，该实施例中的石榴石铁氧体材料的化学式为Y3-x-yDyxCayFe5-y-z-aSiyMnzAlaO12，其中，x＝0.02， y＝0.015，z＝0.06，a＝0.04。
制备上述石榴石铁氧体材料的的制备方法包括如下具体步骤：
1)根据化学式Y3-x-yDyxCayFe5-y-z-aSiyMnzAlaO12，其中，x＝0.02， y＝0.015，z＝0.06，a＝0.04计算并称取所需原材料，所需原材料为Y2O3、 Dy2O3、CaCO3、Fe2O3、SiO2、MnCO3，Al(OH)3；
2)将原材料放入球磨机中进行一次球磨24小时后烘干，球磨时料、钢球、蒸馏水的比例为1:2.5:0.75；
3)将烘干后的混合物放入烧结炉内1150℃预烧，保温5小时；
4)将预烧后的烧结物放入球磨机中进行二次球磨后烘干，球磨时间22小时，球磨时料、钢球、蒸馏水的比例为1:2.5:0.9；
5)将二次球磨后的组分加入质量比为5％、重量比7.5Wt％的聚乙烯醇水溶液造粒；
6)将造粒后得到的颗粒在模具内压制制得生坯件；
7)将压制生坯件放入烧结炉内1470℃烧结，保温6小时，从而得到该实施例成分的石榴石铁氧体材料。
用振动样品磁强计测量饱和磁化强度，用排水法测量密度，按 GB/T9633《微波频率应用的旋磁材料性能测量方法》测试上述实施例中制的的石榴石铁氧体材料的铁磁共振线宽、介电常数和介电损耗，检测结果参见表1所示：
表1
本申请的石榴石铁氧体材料中采用SiO2降低烧结温度，提高材料致密度，降低损耗，采用Dy2O3提高材料功率容量，采用MnCO3和Al(OH)3降低损耗。利用本申请的方法制备的微带环行器用石榴石铁氧体具有高功率、低损耗、高致密性等优异性能。
以上所述，仅为本申请的具体实施方式，但本申请的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本申请揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本申请的保护范围之内。因此，本申请的保护范围应以所述权利要求的保护范围为准。
Claims (6)
1.一种石榴石铁氧体材料，其特征在于，所述石榴石铁氧体材料的化学式为Y3-x- yDyxCayFe5-y-z-aSiyMnzAlaO12，其中，0.01≤x≤0.03，0.01≤y≤0.02，0.02≤z≤0.09，0≤a≤0.05。
2.如权利要求1所述的石榴石铁氧体材料，其特征在于，所述石榴石铁氧体材料的制备原材料包括Y2O3、Dy2O3、CaCO3、Fe2O3、SiO2、MnCO3，Al(OH)3，纯度不低于99wt％。
3.一种制备如权利要求1至2任一所述石榴石铁氧体材料的制备方法，其特征在于，所述制备方法包括：
1)根据石榴石铁氧体材料的化学式计算并称取所需原材料的重量；
2)将原材料放入球磨机中进行一次球磨，球磨后烘干；
3)将烘干后的混合物放入烧结炉内预烧，并保温若干小时；
4)将预烧后的烧结物放入球磨机中进行二次球磨，球磨后烘干；
5)将二次球磨后的混合物中加入聚乙烯醇水溶液造粒；
6)将造粒后得到的颗粒在模具内压制得到生坯件；
7)将压制生坯件放入烧结炉内烧结，保温若干时间后得到所述石榴石铁氧体材料。
4.如权利要求3所述的制备方法，其特征在于，一次球磨和二次球磨时，采用蒸馏水作为浸没原料。
5.如权利要求3所述的制备方法，其特征在于，二次球磨后的混合物中加入的聚乙烯醇水溶液质量比为(4～8)％，重量比为(6～8)wt％。
6.一种环形器，所述环形器应用于如权利要求或2任一项所述的石榴石铁氧体材料。
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