CN101200367A - Method for preparing yttrium iron garnet ferrite material - Google Patents

Method for preparing yttrium iron garnet ferrite material Download PDF

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Publication number
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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China
Prior art keywords
ferrite material
iron garnet
yttrium iron
sintering
garnet ferrite
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CNA2007100503439A
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Inventor
杨青慧
张怀武
文岐业
刘颖力
李元勋
张朝坤
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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Priority to CNA2007100503439A priority Critical patent/CN101200367A/en
Publication of CN101200367A publication Critical patent/CN101200367A/en
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Abstract

The invention relates to yttrium iron garnet ferrite preparation method, belonging to a field of electronic material. The invention comprises the following steps: 1 the proportion of the required materials Fe2O3 and Y2O3 is calculated according to the chemical formula Y3Fe5O12; 2. According to the proportion calculated in the step 1, the Fe2O3 and Y2O3 are mixed and milled; 3. Drying and crushing; 4, the dried and crushed powder is sintered by microwave; 5. Granulation; 6. Pressing formation. The invention has the advantages of: 1. Density structure; 2. excellent magnetic energy; 3 large dielectric constant and small dielectric loss; 4. Small electromagnetic loss.

Description

Method for preparing yttrium iron garnet ferrite material
Technical field
The present invention relates to field of electronic materials, particularly the technology of preparing of microwave ferrite material.
Background technology
Microwave heating is a kind of type of heating of whole heatable substance, has characteristics such as efficient, energy-conservation, pollution-free, more and more is subjected to everybody attention now.Though the microwave sintering technology also has much immature, incomplete place, but, it has the incomparable advantage of routine techniques: at first, as a kind ofly save time, energy-conservation, save work, free of contamination technology, microwave sintering can satisfy current save energy, protection environment requirement; Secondly, the characteristics of the activated sintering that it had help obtaining good microstructure, thereby improve material property; Once more, microwave and material coupled characteristics have determined can carry out the selectivity heating with microwave, thereby can make the structured material with particular tissues, as function-graded material.These advantages make microwave sintering have broad prospects at high-performance ceramics and ceramic-metal composite preparation field.
In the prior art, the resistance furnace sintering method that the preparation of yttrium iron garnet gyromagnetic ferrite material is at present main still conventional, i.e. solid state reaction sintering method, its technology mainly contains: batching-ball milling-oven dry-pre-burning-ball milling-oven dry-granulation-moulding-sintering, this method is consuming time, power consumption.
Summary of the invention
Technical problem to be solved by this invention is, a kind of new method for preparing yttrium iron garnet ferrite material is provided, and prepared yttrium iron garnet gyromagnetic ferrite material can provide the yttrium iron garnet gyromagnetic ferrite material than prior art for preparing to have the better properties parameter.
The technical scheme that the present invention solve the technical problem employing is that method for preparing yttrium iron garnet ferrite material may further comprise the steps:
1) according to the chemical formula Y of yttrium iron garnet 3Fe 5O 12Calculate needed raw material Fe 2O 3And Y 2O 3Ratio;
2) ratio of calculating according to step 1) is with Fe 2O 3And Y 2O 3Mix ball milling;
3) oven dry is pulverized;
4) powder after oven dry, the pulverizing is carried out microwave sintering,
5) granulation;
6) compression moulding.
Described step 2) in, adopts the steel ball ball milling, and take a certain amount of iron deficiency prescription.
In the described step 5), the Ferrite Material behind ball milling oven dry is sieved, add 10% tackiness agent again and carry out granulation, compacting then.
Described raw material is that purity is 99.99% analytical pure Fe 2O 3With purity be 99.99% analytical pure Y 2O 3
In the described step 1), in weight unit, Y 2O 3Be 45.8996 units; Adopt the prescription of iron deficiency 3%, Fe 2O 3Be 51.1004 units.
Compare with ordinary method agglomerating yttrium iron garnet ferrite material, the present invention has the following advantages:
(1) compact structure: most of grain-size of the powder of normal sintering is about 3.0-5.0 μ m, and the powder grain size of microwave sintering is between 0.5-1.5 μ m.The result can find that also the powder crystal grain after crystal grain through the powder of microwave sintering is than normal sintering is much smaller in other raw materials of microwave sintering.So, preferentially improve the densification process of material in the microwave sintering process, but do not impel grain growing.
(2) magnetic property excellence: the saturation magnetization Mc of the sample behind microwave sintering is 14.49emu/g, and the value of coercivity H is 31.94Oe.
(3) specific inductivity is big, dielectric loss is little: this is because the treatment technology of microwave sintering has improved the microtexture of material and can obtain better close grain micro-, microwave sintering sample gas boring ratio is less, caused the minimizing of the low-k phase that causes by pore, density has also increased simultaneously, the dielectric coefficient that has caused the microwave sintering sample is greater than the normal sintering sample, and its dielectric loss is less than the normal sintering sample.
(4) the magnetoelectricity loss is little.
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the microwave agglomerating furnace schematic internal view.Wherein, infrared measurement of temperature hole 1, quartz crucible 2 with a lid waits to burn material 3, carborundum powder 4, corundum crucible 5, microwave oven exocoel 6, refractory brick 7.
Fig. 3 is the microwave sintering curve.
Fig. 4 is the XRD figure of microwave sintering powder.
Fig. 5 be the microwave sintering powder the SEM photo (900 ℃, 20min).
Fig. 6 is the B-H hysteresis curve (example weight 1 gram) of normal sintering and microwave sintering material, and wherein, " A " is the normal sintering sample, and " B " is the microwave sintering sample.
Fig. 7 is the dielectric loss curve of normal sintering and microwave sintering sample, and wherein, " A " is the normal sintering sample, and " B " is the microwave sintering sample.
Fig. 8 is the magnetoelectricity damage curve of normal sintering and microwave sintering sample, and wherein, " A " is the normal sintering sample, and " B " is the microwave sintering sample.
Embodiment
The yttrium iron garnet iron gyromagnetic ferrite material of the microwave sintering that the present invention proposes, its processing unit as shown in Figure 2, adopt the NL75 microwave agglomerating furnace to carry out the material crystallization, device comprises infrared measurement of temperature hole 1, and quartz crucible 2 with a lid waits to burn material 3, carborundum powder 4, corundum crucible 5, microwave oven exocoel 6, refractory brick 7.
A kind of microwave sintering yttrium iron garnet microwave ferrite material provided by the invention is mainly made by five steps once:
Step 1: batching
Use purity is 99.99% analytical pure Fe 2O 3With purity be 99.99% analytical pure Y 2O 3As raw material, according to the chemical formula (Y of pure yttrium iron garnet 3Fe 5O 12) calculate needed material rate.
For example: about the about 100g of required yttrium iron garnet ferrite material, historical facts or anecdotes is tested with 100g and is calculated material rate, and the result is: Y 2O 3Need 45.8996g; Use the steel ball ball milling when considering ball milling, adopt the prescription of iron deficiency 3%, Fe 2O 3Need 51.1004g, compensate with the iron of sneaking into to ball milling.
Step 2: ball milling
In the experiment, the ball milling time be 10h (hour), and adopt deionized water as disperse means.
Step 3: oven dry, granulation
Ball milling Ferrite Material oven dry is later sieved, add 10% tackiness agent again and carry out granulation. scalping 40 orders, dusting cover 100 orders.
Step 4: microwave sintering
Be easy to cause produce thermograde with microwave field density is inhomogeneous owing to heat-up rate is very fast in the microwave sintering process, thereby cause sintered products crackle to occur in sample interior.So sintering again after can not be device in the experiment molded, device can split at last like that, does not have use value.Adopt a powder for preparing to carry out earlier being pressed again after the microwave sintering processing in the experiment.In the microwave sintering process, the material that crushes is packed in the quartz crucible with a lid, imbed in the carborundum powder, open microwave oven then and transfer to the 400W preheating, improve power after 3 minutes to 500W, temperature rise rate is slack-off gradually in this process, after 10 minutes, again hoisting power to 600W to sintering temperature point, turn the about 20W of power down, make it in temperature spot annex insulation, then power is transferred to 0, take out after being cooled to room temperature.
Step 5: granulation, compacting
After granulation was finished, device was suppressed in weighing, pressed a part of sheet and ring-type device respectively.Pressure uses 50MPa.
By Fig. 3-8 as can be known, microwave sintering has the following advantages compared to normal sintering: 1) compact structure 2) the magnetic property excellence; 3) specific inductivity is big, and dielectric loss is little; 4) the magnetoelectricity loss is little; 5) save time, energy-conservation.

Claims (7)

1. method for preparing yttrium iron garnet ferrite material is characterized in that, may further comprise the steps:
1) according to the chemical formula Y of yttrium iron garnet 3Fe 5O 12Calculate needed raw material Fe 2O 3And Y 2O 3Ratio;
2) ratio of calculating according to step 1) is with Fe 2O 3And Y 2O 3Mix ball milling;
3) oven dry is pulverized;
4) powder after oven dry, the pulverizing is carried out microwave sintering;
5) granulation;
6) compression moulding.
2. method for preparing yttrium iron garnet ferrite material as claimed in claim 1 is characterized in that, described step 2) in, adopt the steel ball ball milling, and take a certain amount of iron deficiency prescription.
3. the described method for preparing yttrium iron garnet ferrite material of claim 1 is characterized in that, in the described step 4), adopts the method for microwave heating to carry out sintering;
4. method for preparing yttrium iron garnet ferrite material as claimed in claim 1 is characterized in that, in the described step 5), the Ferrite Material behind the sintering is added 10% tackiness agent and carries out granulation, compacting then.
5. method for preparing yttrium iron garnet ferrite material as claimed in claim 1 is characterized in that, described step 2) in, adopt deionized water as disperse means in the mechanical milling process.
6. method for preparing yttrium iron garnet ferrite material as claimed in claim 1 is characterized in that, described raw material is that purity is 99.99% analytical pure Fe 2O 3With purity be 99.99% analytical pure Y 2O 3
7. method for preparing yttrium iron garnet ferrite material as claimed in claim 1 is characterized in that, in the described step 1), and in weight unit, Y 2O 3Be 45.8996 units; Adopt the prescription of iron deficiency 3%, Fe 2O 3Be 51.1004 units.
CNA2007100503439A 2007-10-29 2007-10-29 Method for preparing yttrium iron garnet ferrite material Pending CN101200367A (en)

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101942695A (en) * 2010-10-20 2011-01-12 福州大学 Method for growing pure and doped yttrium iron garnet crystals by guided mold pulling method
CN102267810A (en) * 2011-08-09 2011-12-07 中国科学院宁波材料技术与工程研究所 Preparation method of high-density ferrite-carbon nanotube composite block material
CN102503393A (en) * 2011-10-25 2012-06-20 安徽理工大学 Method for preparing high-performance ferrite material with microwave sintering method
CN102850045A (en) * 2012-09-24 2013-01-02 陕西科技大学 Ferrite composite material with giant dielectric constant and high magnetic intensity and preparation method of ferrite composite material
CN102976729A (en) * 2012-11-14 2013-03-20 东阳富仕特磁业有限公司 Garnet microwave ferrite with narrow line width and high dielectric constant
CN102976726A (en) * 2012-08-07 2013-03-20 横店集团东磁股份有限公司 Method for preparing ultrathin type ferrite sheet by using microwave sintering
CN104848690A (en) * 2015-05-11 2015-08-19 深圳振华富电子有限公司 Sintering mould
CN105669181A (en) * 2016-01-13 2016-06-15 杭州电子科技大学 Preparation method of compact small-grain YIG ceramic
CN105777097A (en) * 2016-03-13 2016-07-20 浙江展邦电子科技有限公司 Preparation method for improving purity and saturation magnetization of YIG target
CN107021748A (en) * 2017-04-17 2017-08-08 东南大学 A kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet
CN108530058A (en) * 2018-05-17 2018-09-14 合肥工业大学 A kind of preparation method with negative permittivity barium titanate/yttrium iron garnet composite ceramics
CN111960815A (en) * 2020-08-24 2020-11-20 上海阖煦微波技术有限公司 Microwave gyromagnetic ferrite material and preparation process and application thereof
CN112846182A (en) * 2021-01-13 2021-05-28 内蒙古科技大学 Method for microwave in-situ synthesis of iron-based metal ceramic and iron-based metal ceramic
CN112851348A (en) * 2021-01-11 2021-05-28 西南科技大学 Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body
CN114907107A (en) * 2021-09-24 2022-08-16 浙江凯文磁钢有限公司 Method for manufacturing yttrium aluminum garnet ferrite material
CN115385680A (en) * 2022-09-14 2022-11-25 电子科技大学 High-dielectric-width and low-linewidth microwave gyromagnetic ferrite material and preparation method thereof

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101942695A (en) * 2010-10-20 2011-01-12 福州大学 Method for growing pure and doped yttrium iron garnet crystals by guided mold pulling method
CN102267810A (en) * 2011-08-09 2011-12-07 中国科学院宁波材料技术与工程研究所 Preparation method of high-density ferrite-carbon nanotube composite block material
CN102503393A (en) * 2011-10-25 2012-06-20 安徽理工大学 Method for preparing high-performance ferrite material with microwave sintering method
CN102503393B (en) * 2011-10-25 2013-07-10 安徽理工大学 Method for preparing high-performance ferrite material with microwave sintering method
CN102976726A (en) * 2012-08-07 2013-03-20 横店集团东磁股份有限公司 Method for preparing ultrathin type ferrite sheet by using microwave sintering
CN102850045A (en) * 2012-09-24 2013-01-02 陕西科技大学 Ferrite composite material with giant dielectric constant and high magnetic intensity and preparation method of ferrite composite material
CN102976729A (en) * 2012-11-14 2013-03-20 东阳富仕特磁业有限公司 Garnet microwave ferrite with narrow line width and high dielectric constant
CN104848690A (en) * 2015-05-11 2015-08-19 深圳振华富电子有限公司 Sintering mould
CN105669181A (en) * 2016-01-13 2016-06-15 杭州电子科技大学 Preparation method of compact small-grain YIG ceramic
CN105669181B (en) * 2016-01-13 2018-02-16 杭州电子科技大学 A kind of preparation method of fine and close small-grain Y IG ceramics
CN105777097A (en) * 2016-03-13 2016-07-20 浙江展邦电子科技有限公司 Preparation method for improving purity and saturation magnetization of YIG target
CN107021748A (en) * 2017-04-17 2017-08-08 东南大学 A kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet
CN108530058A (en) * 2018-05-17 2018-09-14 合肥工业大学 A kind of preparation method with negative permittivity barium titanate/yttrium iron garnet composite ceramics
CN111960815A (en) * 2020-08-24 2020-11-20 上海阖煦微波技术有限公司 Microwave gyromagnetic ferrite material and preparation process and application thereof
CN112851348A (en) * 2021-01-11 2021-05-28 西南科技大学 Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body
CN112846182A (en) * 2021-01-13 2021-05-28 内蒙古科技大学 Method for microwave in-situ synthesis of iron-based metal ceramic and iron-based metal ceramic
CN114907107A (en) * 2021-09-24 2022-08-16 浙江凯文磁钢有限公司 Method for manufacturing yttrium aluminum garnet ferrite material
CN115385680A (en) * 2022-09-14 2022-11-25 电子科技大学 High-dielectric-width and low-linewidth microwave gyromagnetic ferrite material and preparation method thereof

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Application publication date: 20080618