CN101200367A - Preparation method of yttrium iron garnet ferrite material - Google Patents
Preparation method of yttrium iron garnet ferrite material Download PDFInfo
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- CN101200367A CN101200367A CNA2007100503439A CN200710050343A CN101200367A CN 101200367 A CN101200367 A CN 101200367A CN A2007100503439 A CNA2007100503439 A CN A2007100503439A CN 200710050343 A CN200710050343 A CN 200710050343A CN 101200367 A CN101200367 A CN 101200367A
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- 239000000463 material Substances 0.000 title claims abstract description 35
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 23
- 239000002223 garnet Substances 0.000 title claims abstract description 22
- MTRJKZUDDJZTLA-UHFFFAOYSA-N iron yttrium Chemical compound [Fe].[Y] MTRJKZUDDJZTLA-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000009768 microwave sintering Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000005469 granulation Methods 0.000 claims abstract description 9
- 230000003179 granulation Effects 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000000748 compression moulding Methods 0.000 claims abstract 2
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 206010022971 Iron Deficiencies Diseases 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000003701 mechanical milling Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 3
- 230000005291 magnetic effect Effects 0.000 abstract description 3
- 239000012776 electronic material Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 5
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- 239000010453 quartz Substances 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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Abstract
钇铁石榴石铁氧体材料制备方法,涉及电子材料领域,本发明包括以下步骤:1)依据钇铁石榴石的化学式Y3Fe5O12计算出所需要的原料Fe2O3和Y2O3的比例;2)根据步骤1)计算的比例,将Fe2O3和Y2O3混合,球磨;3)烘干,粉碎;4)对烘干、粉碎后的粉料进行微波烧结;5)造粒;6)压制成型。本发明具有以下优点:(1)结构致密;(2)磁性能优异;(3)介电常数大,介电损耗小;(4)磁电损耗小。
The method for preparing yttrium iron garnet ferrite material relates to the field of electronic materials. The invention comprises the following steps: 1) calculating the required raw materials Fe 2 O 3 and Y 2 O according to the chemical formula Y 3 Fe 5 O 12 of yttrium iron garnet 3 ; 2) According to the ratio calculated in step 1), Fe 2 O 3 and Y 2 O 3 were mixed and ball milled; 3) Drying and crushing; 4) Microwave sintering the dried and crushed powder; 5) granulation; 6) compression molding. The invention has the following advantages: (1) compact structure; (2) excellent magnetic performance; (3) large dielectric constant and small dielectric loss; (4) small magnetoelectric loss.
Description
技术领域technical field
本发明涉及电子材料领域,特别涉及微波铁氧体材料的制备技术。The invention relates to the field of electronic materials, in particular to the preparation technology of microwave ferrite materials.
背景技术Background technique
微波加热是一种整体加热物质的加热方式,具有高效、节能、无污染等特点,现在越来越受到大家的重视。微波烧结技术虽然还有很多不成熟、不完善的地方,但是,它具有常规技术无法比拟的优点:首先,作为一种省时、节能、节省劳动、无污染的技术,微波烧结能满足当今节约能源、保护环境的要求;其次,它所具有的活化烧结的特点有利于获得优良的显微组织,从而提高材料性能;再次,微波与材料耦合的特点,决定了用微波可进行选择性加热,从而能制得具有特殊组织的结构材料,如梯度功能材料。这些优势使得微波烧结在高技术陶瓷及金属陶瓷复合材料制备领域具有广阔的前景。Microwave heating is a heating method for heating materials as a whole. It has the characteristics of high efficiency, energy saving, and no pollution. Now it is getting more and more attention. Although microwave sintering technology is still immature and imperfect, it has advantages that conventional technologies cannot match: first, as a time-saving, energy-saving, labor-saving, and pollution-free technology, microwave sintering can meet The requirements of energy and environmental protection; secondly, its activated sintering characteristics are conducive to obtaining excellent microstructures, thereby improving material performance; thirdly, the characteristics of microwave and material coupling determine that microwaves can be used for selective heating. Thus, structural materials with special organization can be prepared, such as gradient functional materials. These advantages make microwave sintering have broad prospects in the field of preparation of high-tech ceramics and metal-ceramic composite materials.
现有技术中,钇铁石榴石旋磁铁氧体材料的制备目前主要还是常规的电阻炉烧结方法,即固相反应烧结方法,其工艺主要有:配料-球磨-烘干-预烧-球磨-烘干-造粒-成型-烧结,此方法耗时,耗能。In the prior art, the preparation of yttrium iron garnet gyromagnetic ferrite material is mainly the conventional resistance furnace sintering method, that is, the solid phase reaction sintering method. Drying-granulation-forming-sintering, this method is time-consuming and energy-consuming.
发明内容Contents of the invention
本发明所要解决的技术问题是,提供一种新的钇铁石榴石铁氧体材料制备方法,所制备的钇铁石榴石旋磁铁氧体材料能够提供比现有技术制备的钇铁石榴石旋磁铁氧体材料具有更好的性能参数。The technical problem to be solved by the present invention is to provide a new preparation method of yttrium-iron-garnet ferrite material, the prepared yttrium-iron-garnet gyromagnetic ferrite material can provide better than the yttrium-iron-garnet gyromagnetic ferrite material prepared by the prior art. Ferrite materials have better performance parameters.
本发明解决所述技术问题采用的技术方案是,钇铁石榴石铁氧体材料制备方法,包括以下步骤:The technical solution adopted by the present invention to solve the technical problem is that the preparation method of yttrium iron garnet ferrite material comprises the following steps:
1)依据钇铁石榴石的化学式Y3Fe5O12计算出所需要的原料Fe2O3和Y2O3的比例;1) Calculate the ratio of the required raw materials Fe 2 O 3 and Y 2 O 3 according to the chemical formula Y 3 Fe 5 O 12 of yttrium iron garnet;
2)根据步骤1)计算的比例,将Fe2O3和Y2O3混合,球磨;2) According to the ratio calculated in step 1), Fe 2 O 3 and Y 2 O 3 are mixed and ball milled;
3)烘干,粉碎;3) drying, crushing;
4)对烘干、粉碎后的粉料进行微波烧结,4) Microwave sintering the dried and pulverized powder,
5)造粒;5) Granulation;
6)压制成型。6) Press molding.
所述步骤2)中,采用钢球球磨,并采取一定量的缺铁配方。In the step 2), steel ball milling is used, and a certain amount of iron-deficiency formula is adopted.
所述步骤5)中,将球磨后的铁氧体材料烘干过筛,再加入10%的粘合剂进行造粒,然后压制。In the step 5), the ball-milled ferrite material is dried and sieved, then 10% of binder is added for granulation, and then pressed.
所述原料为纯度为99.99%的分析纯Fe2O3和纯度为99.99%的分析纯Y2O3。The raw materials are analytically pure Fe 2 O 3 with a purity of 99.99% and analytically pure Y 2 O 3 with a purity of 99.99%.
所述步骤1)中,以重量单位计,Y2O3为45.8996单位;采用缺铁3%的配方,Fe2O3为51.1004单位。In the step 1), Y 2 O 3 is 45.8996 units by weight; and Fe 2 O 3 is 51.1004 units in the formula of 3% iron deficiency.
与常规方法烧结的钇铁石榴石铁氧体材料相比,本发明具有以下优点:Compared with the yttrium iron garnet ferrite material sintered by conventional methods, the present invention has the following advantages:
(1)结构致密:常规烧结的粉体的大部分晶粒尺寸在3.0-5.0μm左右,而微波烧结的粉体晶粒尺寸在0.5-1.5μm之间。在用微波烧结其他原料的时候结果也会发现经过微波烧结的粉体的晶粒要比常规烧结后的粉体晶粒小得多。所以,微波烧结过程中优先改善材料的致密化过程,但没有促使晶粒生长。(1) Dense structure: Most of the grain size of conventional sintered powder is about 3.0-5.0 μm, while the grain size of microwave sintered powder is between 0.5-1.5 μm. When other raw materials are sintered by microwave, it is also found that the crystal grains of the microwave sintered powder are much smaller than those of conventional sintered powder. Therefore, the microwave sintering process preferentially improved the densification process of the material, but did not promote the grain growth.
(2)磁性能优异:经微波烧结后的样品的饱和磁化强度Mc为14.49emu/g,矫顽力Hc的值为31.94Oe。(2) Excellent magnetic properties: the saturation magnetization Mc of the sample after microwave sintering is 14.49emu/g, and the value of coercive force Hc is 31.94Oe.
(3)介电常数大,介电损耗小:这是因为微波烧结的处理技术改善了材料的微观结构并能获得更好的细晶粒显微,微波烧结样品气孔比较少,导致了由气孔导致的低介电常数相的减少,同时密度也增加了,导致了微波烧结样品的介电系数大于常规烧结样品,其介电损耗小于常规烧结样品。(3) Large dielectric constant and small dielectric loss: This is because the microwave sintering treatment technology improves the microstructure of the material and can obtain better fine-grained microstructure. Microwave sintering samples have fewer pores, which leads to The resulting reduction of the low dielectric constant phase and the increase in density lead to a larger dielectric coefficient of the microwave sintered sample than that of the conventional sintered sample, and a smaller dielectric loss than the conventional sintered sample.
(4)磁电损耗小。(4) The magnetoelectric loss is small.
以下结合附图和具体实施方式对本发明作进一步的说明。The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.
附图说明Description of drawings
图1为本发明的工艺流程图。Fig. 1 is a process flow diagram of the present invention.
图2为微波烧结炉内部示意图。其中,红外测温孔1,带盖子的石英坩锅2,待烧材料3,碳化硅粉4,刚玉坩锅5,微波炉外腔6,耐火砖7。Figure 2 is a schematic diagram of the interior of the microwave sintering furnace. Among them, an infrared
图3为微波烧结曲线。Figure 3 is the microwave sintering curve.
图4为微波烧结粉体的XRD图。Figure 4 is the XRD pattern of the microwave sintered powder.
图5为微波烧结粉体的SEM照片(900℃,20min)。Figure 5 is the SEM photo of the microwave sintered powder (900°C, 20min).
图6为常规烧结和微波烧结材料的B-H磁滞曲线(样品重量1克),其中,“A”为常规烧结样品,“B”为微波烧结样品。Figure 6 is the B-H hysteresis curves of conventional sintered and microwave sintered materials (sample weight 1 g), where "A" is the conventional sintered sample and "B" is the microwave sintered sample.
图7为常规烧结和微波烧结样品的介电损耗曲线,其中,“A”为常规烧结样品,“B”为微波烧结样品。Figure 7 is the dielectric loss curves of the conventional sintered and microwave sintered samples, where "A" is the conventional sintered sample and "B" is the microwave sintered sample.
图8为常规烧结和微波烧结样品的磁电损耗曲线,其中,“A”为常规烧结样品,“B”为微波烧结样品。Figure 8 is the magnetoelectric loss curves of the conventional sintered and microwave sintered samples, where "A" is the conventional sintered sample and "B" is the microwave sintered sample.
具体实施方式Detailed ways
本发明提出的微波烧结的钇铁石榴石铁旋磁铁氧体材料,其工艺设备如图2所示,采用NL75微波烧结炉进行材料晶化,装置包括红外测温孔1,带盖子的石英坩锅2,待烧材料3,碳化硅粉4,刚玉坩锅5,微波炉外腔6,耐火砖7。The microwave sintered yttrium-iron-garnet ferromagnetic ferrite material proposed by the present invention has its process equipment as shown in Figure 2. The NL75 microwave sintering furnace is used to crystallize the material. The device includes an infrared
本发明提供的一种微波烧结钇铁石榴石微波铁氧体材料主要由一下五个步骤制成:A microwave sintered yttrium iron garnet microwave ferrite material provided by the present invention is mainly made by the following five steps:
步骤一:配料Step 1: Ingredients
使用纯度为99.99%的分析纯Fe2O3和纯度为99.99%的分析纯Y2O3作为原料,根据纯钇铁石榴石的化学式(Y3Fe5O12)计算出所需要的原料比例。Using analytically pure Fe 2 O 3 with a purity of 99.99% and analytically pure Y 2 O 3 with a purity of 99.99% as raw materials, the required ratio of raw materials was calculated according to the chemical formula (Y 3 Fe 5 O 12 ) of pure yttrium iron garnet.
例如:所需钇铁石榴石铁氧体材料约100g左右,故实验以100g来计算原料比例,结果为:Y2O3需要45.8996g;考虑到球磨时使用钢球球磨,采用缺铁3%的配方,Fe2O3需要51.1004g,以对球磨的混入的铁进行补偿。For example: the required yttrium iron garnet ferrite material is about 100g, so the experiment uses 100g to calculate the raw material ratio, and the result is: Y 2 O 3 needs 45.8996g; considering the use of steel balls for ball milling, 3% iron deficiency is used The formula of Fe 2 O 3 needs 51.1004g to compensate for the iron mixed in the ball mill.
步骤二:球磨Step 2: Ball Milling
实验中,球磨时间为10h(小时),且采用去离子水作为弥散剂。In the experiment, the ball milling time was 10h (hour), and deionized water was used as the dispersant.
步骤三:烘干,造粒Step 3: drying, granulation
将球磨过后的铁氧体材料烘干过筛,再加入10%的粘合剂进行造粒.粗筛用40目,细筛用100目。The ball-milled ferrite material is dried and sieved, and then 10% of binder is added for granulation. The coarse sieve is 40 mesh, and the fine sieve is 100 mesh.
步骤四:微波烧结Step 4: Microwave Sintering
微波烧结过程中由于升温速度很快和微波场强不均匀很容易导致在样品内部产生温度梯度,从而导致烧结产品出现裂纹。所以实验中不能把器件压成型之后再烧结,那样器件最后会裂开,没有使用价值。实验中采用把配制好的粉料先进行微波烧结处理之后,再进行压制成型。微波烧结过程中,将粉碎好的料装入带盖子的石英坩锅中,埋入碳化硅粉中,然后开启微波炉调至400W预热,3分钟后提高功率至500W,此过程中升温速率逐渐变慢,10分钟后,再提升功率至600W至烧结温度点后,调小功率约20W,使其在温度点附件保温,然后将功率调至0,降温至室温后取出。During the microwave sintering process, due to the rapid heating rate and uneven microwave field strength, it is easy to generate a temperature gradient inside the sample, resulting in cracks in the sintered product. Therefore, in the experiment, the device cannot be pressed into shape and then sintered, otherwise the device will crack at the end, which is useless. In the experiment, the prepared powder was subjected to microwave sintering treatment, and then pressed into shape. During the microwave sintering process, put the pulverized material into a quartz crucible with a lid, bury it in silicon carbide powder, then turn on the microwave oven and adjust it to 400W for preheating, and increase the power to 500W after 3 minutes. During this process, the heating rate gradually increases. Slow down, after 10 minutes, increase the power to 600W to the sintering temperature point, then reduce the power by about 20W to keep it warm at the temperature point, then adjust the power to 0, cool down to room temperature and take it out.
步骤五:造粒,压制Step 5: Granulation, pressing
造粒完成之后,称料进行压制器件,分别压一部分片状和环状器件。压力使用50MPa。After the granulation is completed, the material is weighed to press the device, and a part of the sheet-shaped and ring-shaped devices are respectively pressed. The pressure is 50MPa.
由图3-8可知,微波烧结相较于常规烧结具有以下优点:1)结构致密2)磁性能优异;3)介电常数大,介电损耗小;4)磁电损耗小;5)省时,节能。It can be seen from Figure 3-8 that microwave sintering has the following advantages compared with conventional sintering: 1) compact structure 2) excellent magnetic properties; 3) large dielectric constant and small dielectric loss; 4) small magnetoelectric loss; 5) saving , energy saving.
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