WO2021098243A1 - 一种移动谷点提高MnZn功率铁氧体材料Bs的方法 - Google Patents

一种移动谷点提高MnZn功率铁氧体材料Bs的方法 Download PDF

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WO2021098243A1
WO2021098243A1 PCT/CN2020/101991 CN2020101991W WO2021098243A1 WO 2021098243 A1 WO2021098243 A1 WO 2021098243A1 CN 2020101991 W CN2020101991 W CN 2020101991W WO 2021098243 A1 WO2021098243 A1 WO 2021098243A1
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increase
power ferrite
mnzn power
ferrite material
sanding
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PCT/CN2020/101991
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French (fr)
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吕东华
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横店集团东磁股份有限公司
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Priority to US17/778,430 priority Critical patent/US20220411335A1/en
Priority to EP20889372.7A priority patent/EP4063338A4/en
Publication of WO2021098243A1 publication Critical patent/WO2021098243A1/zh

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Definitions

  • the invention relates to the field of preparation of MnZn power ferrite materials, in particular to a method for moving valley points to increase the Bs of MnZn power ferrite materials.
  • Existing MnZn power ferrite materials move valley points. It is generally considered that the loss valley points with high Fe 2 O 3 content in the main formula move to low temperature, and the loss valley points with low Fe 2 O 3 content move to high temperature, or by controlling Fe The content of 2 O 3 and ZnO shifts the valley point, reducing the content of ZnO and increasing the Bs of the MnZn power ferrite material.
  • the existing technology relies on the high and low content of Fe 2 O 3 to move valley points, which will increase high temperature loss or decrease Bs. With high Fe 2 O 3 content, valley points will move to low temperature, and high temperature, especially after 100 °C, will increase and decrease loss. The content of Fe 2 O 3 will reduce the Bs of the material.
  • a method for controlling the valley point of a manganese-zinc ferrite powder with a wide temperature and a low temperature coefficient is disclosed in Chinese patent literature, its announcement number CN107935579A, which discloses a product development and mass production Method for accurately controlling the valley point of manganese-zinc ferrite powder with wide temperature and low temperature coefficient.
  • this invention uses the Fe 2 O 3 and ZnO content in the main formula to control the valley point, and does not involve the problems of how to reduce the loss and increase the Bs, and controlling the valley point by this method will also increase the loss of the material.
  • the present invention is to overcome the current technology of controlling the content of Fe 2 O 3 and ZnO in the main formula to move valley points, reducing the content of ZnO and increasing the Bs of MnZn power ferrite materials, which will increase the loss of the material, and proposes a The method of moving the valley point to increase the power of MnZn ferrite material Bs.
  • a method for moving valley points to increase MnZn power ferrite material Bs includes the following steps:
  • the additive in step 3) includes the following components and the mass percentage of the pre-burned material is: 0.03-0.08wt% CaCO 3 , 0.015-0.04wt% ZrO 2 , 0.43-0.52wt% Co 2 O 3 , 0.05- 0.2wt% SnO 2 .
  • the valley point is moved toward the high temperature direction, and the Bs is increased while reducing high temperature loss.
  • the principle of the present invention is that the valley point of the material is affected by the relationship between the magnetocrystalline anisotropy constant K1 and the temperature, and the valley point of the material is where K1 is 0.
  • the ratio of Fe 2 O 3 , MnO and ZnO should be controlled within a certain range. This is because when the content of Fe 2 O 3 in the main formula exceeds 53.3 mol%, the eddy current loss of the material will increase. , Less than 52.9 mol%, it cannot cooperate with Co 2 O 3 to effectively reduce the magnetocrystalline anisotropy constant K1 of the material.
  • the Co 2 O 3 content of the present invention must be 0.43%-0.52%; this is because when the Co 2 O 3 content is less than 0.43%, increasing the Fe 2 O 3 content will cause The valley point moves towards the low temperature direction, when it is higher than 0.52%, the loss of the material will be worse, mainly because the excessive Co 2 O 3 will increase the magnetocrystalline anisotropy constant K2 of the material, resulting in increased loss.
  • the Co 2 O 3 content is controlled at 0.43%-0.52% relative to the total weight of the main formula, which can make the valley point Move in the high temperature direction to reduce high temperature loss and increase the Bs of the material.
  • K1 is a 0 whereas the prior art by controlling the level of Fe 2 O 3 content of ZnO or control relationship between the ratio of K1 to control the temperature of the Fe 2 O 3, i.e., by adjusting the height of the content of Fe 2 O 3 or Fe 2 control
  • the ratio of O 3 and ZnO to move the valley points it cannot take into account the movement valley points at the same time, reduce the loss and increase the Bs of the material; although the existing technology will also consider the use of Co 2 O 3 in terms of moving valley points.
  • the prior art believes that adding Co 2 O 3 to the valley point will definitely move to the low temperature direction. Therefore, in the prior art, Co 2 O 3 is generally considered to be helpful for the valley point to move to the low temperature direction and help reduce room temperature loss.
  • the amount of Co 2 O 3 added will not be too much, generally controlled below 0.35wt% of the total weight of the pre-fired material. It does not take into account that when the amount of Co 2 O 3 is within a certain range, the valley points will be reversed. The movement of, that is , the increase of Fe 2 O 3 content, causes the valley point to move to high temperature.
  • the ball water ratio of the primary sanding and the secondary sanding is 1:5-7:0.4-0.6, and the sanding time is 0.5-1.5h.
  • step 2) glue with a total mass of 10% of the pre-fired material and a mass fraction of 7.5% is added.
  • the pre-firing in step 2) is pre-firing in a rotary kiln at 900-1000°C.
  • step 3 glue with a total mass of 10% of the secondary sanding material and a mass fraction of 7.5% is added.
  • the pressing pressure in step 4) is 6-8Mpa.
  • the present invention has the following beneficial effects: the present invention controls and moves valley points by controlling the content of Fe 2 O 3 and the content of Co 2 O 3 , while reducing the loss, increasing the Bs of the material, and solving the problem that the prior art cannot simultaneously take care of
  • the problem of moving valley points can reduce the loss and increase the Bs of the material, and the method of the present invention is relatively simple and suitable for industrialization.
  • Embodiment 1 A method for moving valley points to increase MnZn power ferrite material Bs, including the following steps:
  • Glue with 10% of the total mass of the secondary abrasive and 7.5% by mass is added to the secondary abrasive, spray granulation, and sinter after 6Mpa compression into a standard ring.
  • Embodiment 2 A method for moving valley points to increase MnZn power ferrite material Bs, including the following steps:
  • Embodiment 3 A method for moving valley points to increase MnZn power ferrite material Bs, including the following steps:
  • Glue with 10% of the total mass of the secondary abrasive and 7.5% by mass is added to the secondary abrasive, spray granulation, and press the 7Mpa into a standard ring before sintering.
  • Comparative Example 1 A method for moving valley points to increase MnZn power ferrite material Bs, including the following steps:
  • Add additives including the following components to the calcined material and the mass percentage of the calcined material is: CaCO 3 is 0.03%, ZrO 2 is 0.04%, Co 2 O 3 is 0.44%, SnO 2 is 0.05%, Afterwards, the ball water ratio is 1:5:0.4 for the second time sanding for 1.5 hours;
  • Glue with 10% of the total mass of the secondary abrasive and 7.5% by mass is added to the secondary abrasive, spray granulation, and sinter after 6Mpa compression into a standard ring.
  • Comparative Example 2 A method for moving valley points to increase MnZn power ferrite material Bs, including the following steps:
  • Comparative Example 3 A method for moving valley points to increase MnZn power ferrite material Bs, including the following steps:
  • Add additives including the following components to the calcined material and the mass percentage of the calcined material is: CaCO 3 is 0.03%, ZrO 2 is 0.04%, Co 2 O 3 is 0.52%, SnO 2 is 0.05%, Afterwards, the ball water ratio is 1:6:0.5 for the second time of sanding for 1h;
  • Table 1 Example and comparative example test data table.
  • Example 1 and Comparative Example 1 are only different in Fe 2 O 3 content, and both have the same Co 2 O 3 content.
  • the Fe 2 O 3 content is high, but the valley points move to the high temperature direction.
  • ratio 1 the Fe 2 O 3 content is low, but the valley points move toward the low temperature. These are all caused by the addition of a certain amount of Co 2 O 3.
  • the content of Fe 2 O 3 is high, the Bs is also high.
  • Example 2 and Comparative Example 2 except a different content of Co 2 O 3, in Comparative Example 2 Co 2 O 3 content are not within the scope of the present invention, so long valley point moves toward the lower temperature the content of Fe 2 O 3.
  • Comparing Example 3 with Comparative Example 3 the content of Fe 2 O 3 and ZnO in Comparative Example 3 is beyond the scope of the present invention, and the loss is relatively high.

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Abstract

一种移动谷点提高MnZn功率铁氧体材料Bs的方法，涉及MnZn功率铁氧体材料制备领域，包括以下步骤：1）将Fe2O3、MnO和ZnO混合，进行一次砂磨；2）加入胶水，并进行喷雾造粒，随后进行预烧，得到预烧料；3）在预烧料中加入添加剂，进行二次砂磨；4）在二次砂磨料中加入胶水，喷雾造粒，压制成标环后烧结，通过控制Fe2O3含量与Co2O3含量来控制和移动谷点，降低损耗的同时，提高材料的Bs，解决了现有技术中无法同时兼顾移动谷点，降低损耗和提高材料的Bs的问题，且方法较为简便，适合工业化。

Description

一种移动谷点提高MnZn功率铁氧体材料Bs的方法 技术领域
本发明涉及MnZn功率铁氧体材料制备领域，尤其涉及一种移动谷点提高MnZn功率铁氧体材料Bs的方法。
背景技术
现有的MnZn功率铁氧体材料移动谷点，通常认为主配方中Fe 2O 3含量高的损耗谷点往低温移动，Fe 2O 3含量低的损耗谷点往高温移动，或者通过控制Fe 2O 3和ZnO含量移动谷点，减少ZnO含量提高MnZn功率铁氧体材料的Bs。现有的技术，依靠Fe 2O 3含量高低移动谷点，会使高温损耗增加或Bs降低，Fe 2O 3含量高，谷点往低温移动，高温特别是100℃之后的损耗会增加，降低Fe 2O 3含量，会使材料的Bs降低。通过控制Fe 2O 3和ZnO含量移动谷点，减少ZnO含量提高MnZn功率铁氧体材料的Bs的技术，会使材料的损耗增加。因此现有的技术条件下，提高Bs、降低损耗和移动谷点之间有一定的矛盾，无法兼顾，因为其本质还是通过Fe 2O 3和ZnO含量控制谷点的移动。
例如，一种在中国专利文献上公开的“一种控制宽温低温度系数锰锌铁氧体粉料谷点的方法”，其公告号CN107935579A，其公开了一种在产品研发及产品批量生产中精确控制宽温低温度系数锰锌铁氧体粉料谷点的方法。所述锰锌铁氧体粉料包括主成分和添加剂；所述主成分由Fe 2O 3、ZnO和Mn 3O 4组成；所述ZnO占主成分的重量百分比为4～9wt％；所述Fe 2O 3占主成分的重量百分比根据公式Fe 2O 3(wt％)＝72.88A*ZnO(wt％)计算；其中控制谷点为80℃时，A值为0.2278；其中控制谷点为90℃时，A值为0.2313；其中控制谷点为100℃时，A值为0.2358。然而，该发明通过主配方中的Fe 2O 3和ZnO含量来控制谷点，未涉及如何降低损耗，提高Bs等问题，且通过该方法控制谷点也会使材料的损耗增加。
发明内容
本发明是为了克服目前通过主配方中控制Fe 2O 3和ZnO含量移动谷点，减少ZnO含量提高MnZn功率铁氧体材料的Bs的技术，会使材料的损耗增加等问题，提出了一种移动谷点提高MnZn功率铁氧体材料Bs的方法。
为了实现上述目的，本发明采用以下技术方案：
一种移动谷点提高MnZn功率铁氧体材料Bs的方法，包括以下步骤：
1)将Fe 2O 3、MnO和ZnO混合，进行一次砂磨；
2)加入胶水，并进行喷雾造粒，随后进行预烧，得到预烧料；
3)在预烧料中加入添加剂，进行二次砂磨；
4)在二次砂磨料中加入胶水，喷雾造粒，压制成标环后烧结。
作为优选，步骤1)中各组分配比：Fe 2O 3为52.9-53.3mol％，MnO为38.3-39.08mol％，ZnO为7.62-8.8mol％。
作为优选，步骤3)中添加剂包括以下组分且占预烧料的质量百分比为：0.03-0.08wt％CaCO 3，0.015-0.04wt％ZrO 2，0.43-0.52wt％Co 2O 3，0.05-0.2wt％SnO 2。
本发明通过调整Fe 2O 3含量与Co 2O 3含量配比，使谷点往高温方向移动，提高Bs的同时，降低高温损耗。
本发明的原理在于，材料的谷点是受磁晶各向异性常数K1与温度的关系的影响，在K1为0处，就是材料的谷点处。在本发明的主配方中，即Fe 2O 3、MnO和ZnO的配比要控制在一定的范围，这是由于当主配方中Fe 2O 3含量超过53.3mol％，会使材料的涡流损耗增加，低于52.9mol％，则不能与Co 2O 3协同有效降低材料的磁晶各向异性常数K1。其次，相对于主配方的总重量而言，本发明Co 2O 3含量必须在0.43％-0.52％；这是由于Co 2O 3含量低于0.43％时，增加Fe 2O 3含量，会使谷点往低温方向移动，高于0.52％时，会使材料的损耗变差，主要是因为过量的Co 2O 3，会使材料的磁晶各向异性常数K2变大，导致损耗增加。因此，在原配方的基础上，包括添加剂，通过提高原配方的Fe 2O 3含量，将Co 2O 3含量控制在相对于主配方的总重量的0.43％--0.52％，可以使谷点往高温方向移动，来降低高温损耗，提高材料的Bs。而这与现有技术中通常认为的提高Fe 2O 3含量谷点往低温移动，降低Fe 2O 3含量谷点往高温移动是相违背的。
而现有技术K1为0是通过控制Fe 2O 3含量的高低或控制Fe 2O 3与ZnO的配比来控制K1与温度的关系，即通过调整Fe 2O 3含量的高低或控制Fe 2O 3和ZnO的配比来移动谷点，其并不能同时兼顾移动谷点，降低损耗和提高材料的Bs；虽然，现有的技术在移动谷点方面，也会考虑到用Co 2O 3来调整，但现有技术认为，加入Co 2O 3谷点就肯定往低温方向移动，因此现有技术中Co 2O 3通常是认为对谷点往低温方向移动有帮助，有利于降低室温损耗，所以Co 2O 3的添加量也不会多，一般控制在预烧料总重量的0.35wt％以下，其并没有考虑到Co 2O 3的量在一定范围内时，谷点会出现相反的移动，即Fe 2O 3含量的增加，导致谷点往高温移动。
作为优选，所述一次砂磨和二次砂磨的料球水比例为1:5-7:0.4-0.6，砂磨时间为0.5-1.5h。
在该条件配比下，砂磨更加均匀。
作为优选，步骤2)中加入预烧料总质量10％、质量分数为7.5％的胶水。
作为优选，步骤2)中所述预烧为在回转窑中900-1000℃下预烧。
作为优选，步骤3)中加入二次砂磨料总质量10％、质量分数为7.5％的胶水。
作为优选，步骤4)中所述压制的压力为6-8Mpa。
因此，本发明具有如下有益效果：本发明通过控制Fe 2O 3含量与Co 2O 3含量来控制和移动谷点，降低损耗的同时，提高材料的Bs，解决了现有技术中无法同时兼顾移动谷点，降低损耗和提高材料的Bs的问题，且本发明方法较为简便，适合工业化。
具体实施方式
下面结合具体实施方式对本发明做进一步的描述。
实施例1：一种移动谷点提高MnZn功率铁氧体材料Bs的方法，包括以下步骤：
1)将52.9mol％的Fe 2O 3、38.3mol％的MnO和8.8mol％的ZnO混合，在料球水比例为1:5:0.4下一次砂磨1.5h；
2)加入预烧料总质量10％、质量分数为7.5％的胶水，并进行喷雾造粒，随后在回转窑中900℃下预烧，得到预烧料；
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为：CaCO 3为0.03％、ZrO 2为0.04％，Co 2O 3为0.44％，SnO 2为0.05％，随后在料球水比例为1:5:0.4下二次砂磨1.5h；
4)在二次砂磨料中加入二次砂磨料总质量10％、质量分数为7.5％的胶水，喷雾造粒，在6Mpa压制成标环后烧结。
实施例2：一种移动谷点提高MnZn功率铁氧体材料Bs的方法，包括以下步骤：
1)将53.3mol％的Fe 2O 3、39.08mol％的MnO和7.62mol％的ZnO混合，在料球水比例为1:7:0.6下一次砂磨0.5h；
2)加入预烧料总质量10％、质量分数为7.5％的胶水，并进行喷雾造粒，随后在回转窑中1000℃下预烧，得到预烧料；
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为：CaCO 3为0.03％、ZrO 2为0.04％，Co 2O 3为0.48％，SnO 2为0.05％，随后在料球水比例为1:7:0.6下二次砂磨0.5h；
4)在二次砂磨料中加入二次砂磨料总质量10％、质量分数为7.5％的胶水，喷雾造粒，在8Mpa压制成标环后烧结。
实施例3：一种移动谷点提高MnZn功率铁氧体材料Bs的方法，包括以下步骤：
1)将53.1mol％的Fe 2O 3、38.5mol％的MnO和8.4mol％的ZnO混合，在料球水比例为1:6:0.5下一次砂磨1h；
2)加入预烧料总质量10％、质量分数为7.5％的胶水，并进行喷雾造粒，随后在回转窑中950℃下预烧，得到预烧料；
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为：CaCO 3为0.03％、ZrO 2为0.04％，Co 2O 3为0.52％，SnO 2为0.05％，随后在料球水比例为1:6:0.5下二次砂磨1h；
4)在二次砂磨料中加入二次砂磨料总质量10％、质量分数为7.5％的胶水，喷雾造粒，在7Mpa压制成标环后烧结。
对比例1：一种移动谷点提高MnZn功率铁氧体材料Bs的方法，包括以下步骤：
1)将52.6mol％的Fe 2O 3、38.6mol％的MnO和8.8mol％的ZnO混合，在料球水比例为1:5:0.4下一次砂磨1.5h；
2)加入预烧料总质量10％、质量分数为7.5％的胶水，并进行喷雾造粒，随后在回转窑中900℃下预烧，得到预烧料；
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为：CaCO 3为0.03％、ZrO 2为0.04％，Co 2O 3为0.44％，SnO 2为0.05％，随后在料球水比例为1:5:0.4下二次砂磨1.5h；
4)在二次砂磨料中加入二次砂磨料总质量10％、质量分数为7.5％的胶水，喷雾造粒，在6Mpa压制成标环后烧结。
对比例2：一种移动谷点提高MnZn功率铁氧体材料Bs的方法，包括以下步骤：
1)将53.3mol％的Fe 2O 3、39.08mol％的MnO和7.62mol％的ZnO混合，在料球水比例为1:7:0.6下一次砂磨0.5h；
2)加入预烧料总质量10％、质量分数为7.5％的胶水，并进行喷雾造粒，随后在回转窑中1000℃下预烧，得到预烧料；
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为：CaCO 3为0.03％、ZrO 2为0.04％，Co 2O 3为0.35％，SnO 2为0.05％，随后在料球水比例为1:7:0.6下二次砂磨0.5h；
4)在二次砂磨料中加入二次砂磨料总质量10％、质量分数为7.5％的胶水，喷雾造粒，在8Mpa压制成标环后烧结。
对比例3：一种移动谷点提高MnZn功率铁氧体材料Bs的方法，包括以下步骤：
1)将53.5mol％的Fe 2O 3、38.9mol％的MnO和7.6mol％的ZnO混合，在料球水比例为1:6:0.5下一次砂磨1h；
2)加入预烧料总质量10％、质量分数为7.5％的胶水，并进行喷雾造粒，随后在回转窑中950℃下预烧，得到预烧料；
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为：CaCO 3为0.03％、ZrO 2为0.04％，Co 2O 3为0.52％，SnO 2为0.05％，随后在料球水比例为1:6:0.5下二次砂磨1h；
4)在二次砂磨料中加入二次砂磨料总质量10％、质量分数为7.5％的胶水，喷雾造粒，在7Mpa 压制成标环后烧结。
对实施例和对比例制备得到的MnZn功率铁氧体材料的谷点和Bs进行测试，所得数据如下表所示。
表1：实施例及对比例测试数据表。
Figure PCTCN2020101991-appb-000001
从上表可知，实施例1和对比例1只是Fe 2O 3含量不同，两者的Co 2O 3含量相同，实施例1中Fe 2O 3含量高，谷点却往高温方向移动，对比例1中Fe 2O 3含量低，谷点却往低温方向移动，这些都是因为加入了一定量的Co 2O 3所致。同时Fe 2O 3含量高的，Bs也高。
实施例2和对比例2只是Co 2O 3含量不同，比较例2中的Co 2O 3含量不在本发明范围内，所以Fe 2O 3含量多时，谷点往低温方向移动。
实施例3和对比例3对比，其中对比例3中的Fe 2O 3和ZnO的含量超出了本发明的范围，损耗偏高。

Claims (8)

  1. 一种移动谷点提高MnZn功率铁氧体材料Bs的方法，其特征在于，包括以下步骤：
    1)将Fe 2O 3、MnO和ZnO混合，进行一次砂磨；
    2)加入胶水，并进行喷雾造粒，随后进行预烧，得到预烧料；
    3)在预烧料中加入添加剂，进行二次砂磨；
    4)在二次砂磨料中加入胶水，喷雾造粒，压制成标环后烧结。
  2. 根据权利要求1所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法，其特征在于，步骤1)中各组分配比：Fe 2O 3为52.9-53.3mol％，MnO为38.3-39.08mol％，ZnO为7.62-8.8mol％。
  3. 根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法，其特征在于，步骤3)中添加剂包括以下组分且占预烧料的质量百分比为：0.03-0.08wt％CaCO 3，0.015-0.04wt％ZrO 2，0.43-0.52wt％Co 2O 3，0.05-0.2wt％SnO 2。
  4. 根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法，其特征在于，所述一次砂磨和二次砂磨的料球水比例为1:5-7:0.4-0.6，砂磨时间为0.5-1.5h。
  5. 根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法，其特征在于，步骤2)中加入预烧料总质量10％、质量分数为7.5％的胶水。
  6. 根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法，其特征在于，步骤2)中所述预烧为在回转窑中900-1000℃下预烧。
  7. 根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法，其特征在于，步骤3)中加入二次砂磨料总质量10％、质量分数为7.5％的胶水。
  8. 根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法，其特征在于，步骤4)中所述压制的压力为6-8Mpa。
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