CN107021748A - A kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet - Google Patents

A kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet Download PDF

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CN107021748A
CN107021748A CN201710248752.3A CN201710248752A CN107021748A CN 107021748 A CN107021748 A CN 107021748A CN 201710248752 A CN201710248752 A CN 201710248752A CN 107021748 A CN107021748 A CN 107021748A
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mixed powder
burning
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ball milling
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徐庆宇
薛丰铧
黄菊
李天睿
王子凡
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Southeast University
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2675—Other ferrites containing rare earth metals, e.g. rare earth ferrite garnets
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof

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Abstract

The invention provides a kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet, by adding surfactant cetyl trimethyl ammonium (CTAB) in the raw material for preparing yttrium iron garnet (YIG), 1050 DEG C effectively will be dropped into phase temperature from 1200 DEG C, reduce the damping factors of the YIG Spin precessions prepared simultaneously, numeric ratio does not add the small magnitude of YIG of CTAB preparations.Present invention could apply to YIG industrialized production, reaction temperature is reduced, reduces energy consumption, while improving the performance of product.

Description

A kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet
Technical field
The present invention relates to a kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet, belong to microwave ferrite material technology neck Domain.
Background technology
Yttrium iron garnet (Y3Fe5O12, abbreviation YIG) and it is a kind of ferrimagnetism material, with body-centered cubic structure.YIG works Working frequency is in microwave band, therefore is referred to as microwave ferrite material.YIG ferromagnetic resonance line width is very narrow, with excellent Gyromagnet characteristic and high resistivity.Have in fields such as radar, microwave communication, guided missile, artificial satellite, microwave heating and Medical Devices It is widely applied.In recent years, with the rapid development of electronic technology, YIG materials and device are in mobile communication, radar system Using expanding day by day.Especially various YIG ferrite phase shifters on phased-array radar using after succeeding, major states all YIG materials are classified as military project security information.
With continuing to bring out for electronic message unit Large and middle scale IC and portable communications instrument, microwave ferrite Device develops to miniaturization, miniaturization, chip type even integrated direction, it is therefore desirable to microwave ferrite and common electrode Low temperature co-fired, reducing ferritic sintering temperature turns into a key issue.
The content of the invention
Technical problem：It is an object of the invention to provide a kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet, this method drop The sintering temperature of low YIG materials, reduces production cost, improves properties of product, is easy to large-scale production.
Technical scheme：The invention provides a kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet, this method includes following Step：
1) according to mol ratio 5:3 weigh raw material yittrium oxide and iron oxide, mixing after obtain compound；
2) it will be dried in vacuo after the compound ball milling, obtain dry mixed powder I；Afterwards by dry mixed powder I is put into batch-type furnace, is warming up to 700 DEG C~1000 DEG C, is incubated 1~24h, and furnace cooling afterwards obtains the sample of first time pre-burning Product；
3) vacuum drying after cetyl trimethyl ammonium, ball milling is added in the sample of first time pre-burning and obtains mixed powder Dry mixed powder II, is put into batch-type furnace by material II afterwards, is warming up to 700 DEG C~1000 DEG C, is incubated 1h~24h, afterwards Furnace cooling, obtains the sample of second of pre-burning, the wherein quality of cetyl trimethyl ammonium is that yittrium oxide and iron oxide are total The 0.1%~10% of quality,；
4) sample of second of pre-burning is put into batch-type furnace, furnace temperature rises to 900 DEG C~1400 DEG C, is incubated 3~24h, it Furnace cooling afterwards, obtains yttrium iron garnet.
Wherein：
Step 2) described in will after the compound ball milling vacuum drying refer to compound being put into ball grinder, in rotating speed Under conditions of 200~800rpm, ball grinder is integrally put into vacuum drying chamber by 3~24h of ball milling afterwards, is 30 in temperature DEG C~80 DEG C under the conditions of, dry 1~10h, obtain dry mixed powder I.
Step 3) described in ball milling after vacuum drying obtain mixed powder II, refer in the sample of first time pre-burning add After cetyl trimethyl ammonium, ball grinder is placed in ball mill, under conditions of rotating speed is 200rpm~800rpm, ball milling Ball grinder, is integrally put into vacuum drying chamber by 3~24h afterwards, under the conditions of 30 DEG C~80 DEG C of temperature, dries 1~10h, obtains To dry mixed powder II.
Described yittrium oxide, iron oxide and cetyl trimethyl ammonium is that analysis is pure.
Beneficial effect：Compared with prior art, the present invention has advantages below：
By adding surfactant cetyl trimethyl ammonium (CTAB) in the feed, solid phase is effectively reduced anti- Answer method prepare YIG into phase temperature, 1050 DEG C will be dropped into phase temperature from 1200 DEG C, energy consumption is reduced, reduce and be produced into This, and the damping factor of Spin precession is reduce further, the quality of product is improved, is easy to large-scale production；In raw material In without addition CTAB, the YIG prepared in 1200 DEG C of sintering, the damping factor of its Spin precession is 0.018, and addition CTAB exists The damping factor of YIG prepared by 1050 DEG C of sintering Spin precession is 0.0051, and adds what CTAB was prepared in 1100 DEG C of sintering The damping factor of YIG Spin precession is even more to be reduced to 0.0014.
Brief description of the drawings
Fig. 1 is addition CTAB and the comparison diagram that yttrium iron garnet is prepared without CTAB.
Embodiment
Embodiment 1：
1) according to mol ratio 5:3 weigh raw material yittrium oxide and iron oxide, mixing after obtain compound；
2) compound is put into ball grinder, under conditions of rotating speed is 200rpm, ball milling 3h is overall by ball grinder afterwards It is put into vacuum drying chamber, under the conditions of temperature is 30 DEG C, dries 1h, obtain dry mixed powder I；Dry is mixed afterwards Close powder I to be put into batch-type furnace, be warming up to 700 DEG C, be incubated 1h, furnace cooling afterwards obtains the sample of first time pre-burning；
3) refer to add after cetyl trimethyl ammonium in the sample of first time pre-burning, ball grinder is placed in ball mill In, under conditions of rotating speed is 200rpm, ball grinder is integrally put into vacuum drying chamber by ball milling 3h afterwards, in 30 DEG C of temperature Under the conditions of, 1h is dried, dry mixed powder II is obtained, dry mixed powder II is put into batch-type furnace afterwards, is warming up to 700 DEG C, 1h is incubated, furnace cooling afterwards obtains the sample of second of pre-burning, and the quality of wherein cetyl trimethyl ammonium is The 0.1% of yittrium oxide and iron oxide gross mass,；
4) sample of second of pre-burning is put into batch-type furnace, furnace temperature rises to 900 DEG C, is incubated 3h, furnace cooling afterwards is obtained To yttrium iron garnet.
Embodiment 2：
1) according to mol ratio 5:3 weigh raw material yittrium oxide and iron oxide, mixing after obtain compound；
2) compound is put into ball grinder, under conditions of rotating speed is 800rpm, ball milling 24h is whole by ball grinder afterwards Body is put into vacuum drying chamber, under the conditions of temperature is 80 DEG C, is dried 10h, is obtained dry mixed powder I；Afterwards by drying Mixed powder I be put into batch-type furnace, be warming up to 1000 DEG C, be incubated 24h, furnace cooling afterwards obtains the sample of first time pre-burning Product；
3) refer to add after cetyl trimethyl ammonium in the sample of first time pre-burning, ball grinder is placed in ball mill In, under conditions of rotating speed is 800rpm, ball grinder is integrally put into vacuum drying chamber by ball milling 24h afterwards, in 80 DEG C of temperature Under the conditions of, 10h is dried, dry mixed powder II is obtained, dry mixed powder II is put into batch-type furnace afterwards, is warming up to 1000 DEG C, 24h is incubated, furnace cooling afterwards obtains the quality of the sample of second of pre-burning, wherein cetyl trimethyl ammonium For the 10% of yittrium oxide and iron oxide gross mass,；
4) sample of second of pre-burning is put into batch-type furnace, furnace temperature rises to 1400 DEG C, is incubated 24h, furnace cooling afterwards, Obtain yttrium iron garnet.
Embodiment 3：
1) according to mol ratio 5:3 weigh raw material yittrium oxide and iron oxide, mixing after obtain compound；
2) compound is put into ball grinder, under conditions of rotating speed is 450rpm, ball milling 6h is overall by ball grinder afterwards It is put into vacuum drying chamber, under the conditions of temperature is 50 DEG C, dries 2h, obtain dry mixed powder I；Dry is mixed afterwards Close powder I to be put into batch-type furnace, be warming up to 900 DEG C, be incubated 3h, furnace cooling afterwards obtains the sample of first time pre-burning；
3) refer to add after cetyl trimethyl ammonium in the sample of first time pre-burning, ball grinder is placed in ball mill In, under conditions of rotating speed is 450rpm, ball grinder is integrally put into vacuum drying chamber, in temperature 50 C by ball milling 12h afterwards Under the conditions of, 2h is dried, dry mixed powder II is obtained, dry mixed powder II is put into batch-type furnace afterwards, is warming up to 900 DEG C, 3h is incubated, furnace cooling afterwards obtains the sample of second of pre-burning, and the quality of wherein cetyl trimethyl ammonium is The 1% of yittrium oxide and iron oxide gross mass,；
4) sample of second of pre-burning is put into batch-type furnace, furnace temperature rises to 1050 DEG C, is incubated 3h, furnace cooling afterwards, Obtain yttrium iron garnet.
Embodiment 4：
1) according to mol ratio 5:3 weigh raw material yittrium oxide and iron oxide, mixing after obtain compound；
2) compound is put into ball grinder, under conditions of rotating speed is 550rpm, ball milling 8h is overall by ball grinder afterwards It is put into vacuum drying chamber, under the conditions of temperature is 50 DEG C, dries 4h, obtain dry mixed powder I；Dry is mixed afterwards Close powder I to be put into batch-type furnace, be warming up to 800 DEG C, be incubated 6h, furnace cooling afterwards obtains the sample of first time pre-burning；
3) refer to add after cetyl trimethyl ammonium in the sample of first time pre-burning, ball grinder is placed in ball mill In, under conditions of rotating speed is 550rpm, ball grinder is integrally put into vacuum drying chamber, in temperature 50 C by ball milling 16h afterwards Under the conditions of, 4h is dried, dry mixed powder II is obtained, dry mixed powder II is put into batch-type furnace afterwards, is warming up to 800 DEG C, 6h is incubated, furnace cooling afterwards obtains the sample of second of pre-burning, and the quality of wherein cetyl trimethyl ammonium is The 0.5% of yittrium oxide and iron oxide gross mass,；
4) sample of second of pre-burning is put into batch-type furnace, furnace temperature rises to 1100 DEG C, is incubated 6h, furnace cooling afterwards, Obtain yttrium iron garnet.
Fig. 1 is addition CTAB and the comparison diagram that yttrium iron garnet is prepared without CTAB, is as can be seen from the figure added CTAB and the X-ray diffraction spectrum without the addition CTAB YIG samples sintered at different temperatures using solid reaction process, asterisk mark What is remembered is the diffraction maximum of dephasign.It can be seen that be not added with CTAB, only to 1200 degree of sintering temperatures, YIG phases, and add CTAB, at 1050 degree just substantially completely into phase, to 1100 degree then completely into phase.
Present example provides a kind of effective high-quality YIG low heat temperature solid state reaction preparation technology, the YIG of preparation With excellent structure, magnetic and microwave property, with stronger popularization and application value.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., for example, change CTAB addition, turn of ball mill Speed, the temperature and time of sintering, the modification of the parameter such as dry time should be included in the scope of the protection.

Claims (3)

1. a kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet, it is characterised in that：This method comprises the following steps：
1) according to mol ratio 5:3 weigh raw material yittrium oxide and iron oxide, mixing after obtain compound；
2) it will be dried in vacuo after the compound ball milling, obtain dry mixed powder I；Dry mixed powder I is put afterwards Enter in batch-type furnace, be warming up to 700 DEG C~1000 DEG C, be incubated 1~24h, furnace cooling afterwards obtains the sample of first time pre-burning；
3) vacuum drying after cetyl trimethyl ammonium, ball milling is added in the sample of first time pre-burning and obtains mixed powder II, dry mixed powder II is put into batch-type furnace afterwards, 700 DEG C~1000 DEG C are warming up to, 1h~24h, Zhi Housui is incubated Stove is cooled down, and obtains the sample of second of pre-burning, the wherein quality of cetyl trimethyl ammonium is yittrium oxide and the total matter of iron oxide The 0.1%~10% of amount,；
4) sample of second of pre-burning is put into batch-type furnace, furnace temperature rises to 900 DEG C~1400 DEG C, is incubated 3~24h, Zhi Housui Stove is cooled down, and obtains yttrium iron garnet.
2. a kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet as claimed in claim 1, it is characterised in that：Step 2) it is described Will vacuum drying refer to compound being put into ball grinder after the compound ball milling, in rotating speed for 200rpm~800rpm Under the conditions of, ball grinder is integrally put into vacuum drying chamber by 3~24h of ball milling afterwards, under the conditions of temperature is 30 DEG C~80 DEG C, 1~10h is dried, dry mixed powder I is obtained.
3. a kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet as claimed in claim 1, it is characterised in that：Step 3) it is described Ball milling after vacuum drying obtain mixed powder II, refer in the sample of first time pre-burning add cetyl trimethyl ammonium Afterwards, ball grinder is placed in ball mill, under conditions of rotating speed is 200rpm~800rpm, 3~24h of ball milling, afterwards by ball milling Tank is integrally put into vacuum drying chamber, under the conditions of 30 DEG C~80 DEG C of temperature, is dried 1~10h, is obtained dry mixed powder Ⅱ。
CN201710248752.3A 2017-04-17 2017-04-17 A kind of Low Temperature Solid-Phase preparation method of yttrium iron garnet Pending CN107021748A (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN115537924A (en) * 2022-10-11 2022-12-30 安徽科瑞思创晶体材料有限责任公司 YIG microwave filter crystal and growth method thereof
CN116425206A (en) * 2023-04-06 2023-07-14 中国科学院宁波材料技术与工程研究所 Improve SrFe 12 O 19 Method for magnetic performance of ferrite

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115537924A (en) * 2022-10-11 2022-12-30 安徽科瑞思创晶体材料有限责任公司 YIG microwave filter crystal and growth method thereof
CN116425206A (en) * 2023-04-06 2023-07-14 中国科学院宁波材料技术与工程研究所 Improve SrFe 12 O 19 Method for magnetic performance of ferrite

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Application publication date: 20170808