CN107129281A - A kind of magnesium titanate doped aluminium microwave-medium ceramics - Google Patents

A kind of magnesium titanate doped aluminium microwave-medium ceramics Download PDF

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CN107129281A
CN107129281A CN201710292933.6A CN201710292933A CN107129281A CN 107129281 A CN107129281 A CN 107129281A CN 201710292933 A CN201710292933 A CN 201710292933A CN 107129281 A CN107129281 A CN 107129281A
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magnesium titanate
microwave
aluminium
ball
ceramics
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李蔚
胡家驹
刘会娇
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East China University of Science and Technology
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East China University of Science and Technology
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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
    • C04B35/10—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 aluminium oxide
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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
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • C04B2235/3234—Titanates, not containing zirconia
    • C04B2235/3236—Alkaline earth titanates
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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Abstract

The present invention discloses a kind of magnesium titanate doped aluminium microwave-medium ceramics.It is characterized in high-purity alumina powder（Alumina content>99.95%）Magnesium titanate dopant is added for major ingredient（The doping of magnesium titanate is 0.2 ~ 0.4 gram in every 100 grams of alumina powder raw materials）, after ball milling mixing, dry-pressing formed obtained ceramic green, sintered 24 hours after 1,580 1620 DEG C, you can obtain the magnesium titanate doped aluminium ceramics of densification, this aluminium oxide ceramics has the characteristics of dielectric loss is low（Dielectric constant：9.98 10.05, Q ×fValue：1878900‑199550GHz）.The present invention is used as dopant from magnesium titanate, it is not easy to form vacancy defect, it is to avoid the problems such as dielectric loss increase and unstable performance occur.Present invention process method is simple, and production procedure is short, and equipment requirement is relatively low, is adapted to large-scale production.

Description

A kind of magnesium titanate doped aluminium microwave-medium ceramics
Technical field
It is a kind of environment-friendly low-dielectric loss microwave-medium the present invention relates to a kind of magnesium titanate doped aluminium ceramics Material, available for fields such as microwave communication, electrovacuums.
Background technology
Aluminium oxide ceramics is a kind of important dielectric material, not only electrical insulation capability is good, dielectric loss is low, thermal conductivity is high, High temperature resistant and chemical attack, and cheap, technical maturity, therefore be widely used in fields such as electronics, communication, electrovacuums.But Be, due to the high speed development of information technology, the requirement more and more higher to dielectric material, aluminium oxide ceramics it is not enough increasingly apparent, Wherein most prominent is exactly that dielectric loss is bigger than normal, and Q ×fValue is relatively low.In order to reduce the dielectric loss of aluminium oxide ceramics, its Q is improved ×fValue, most common and effective method is exactly to adulterate.Such as, N.M.Alord et al. in alumina ceramic material by adding 0.5wt% titanium oxide, makes dielectric loss decline to a great extent, and Q ×fValue rises to 452790GHz.C.L.Huang et al. is received using high-purity Rice alumina powder is raw material and adds 0.5wt% titanium oxide, by Q ×fValue is further improved to 680000GHz（Under 14GHz）. At home, open huge first pass through and small amounts magnesium is mixed in aluminium oxide ceramics, and utilize double sintering technique, obtain material Q ×fValue reaches 950000GHz, reaches sapphire level.But, magnesia, titania addition are although common, but have one to lack Point, is exactly magnesium ion（+ divalent）, titanium ion（+ 4 valencys）With aluminium ion（+ trivalent）Valence state is different, when magnesia or titania addition are solid When in the molten lattice to aluminum oxide, vacancy defect is easily formed, causes dielectric loss to increase, performance is unstable.
The content of the invention
Present invention aims at provide a kind of magnesium titanate doped aluminium microwave-medium ceramics, this aluminum oxide microwave-medium Ceramics have the characteristics of dielectric loss is relatively low, while not allowing to be also easy to produce vacancy defect during dopant solid solution.
In order to realize foregoing invention purpose, the technical solution adopted by the present invention is as follows：With high purity aluminium oxide（Al2O3）Powder （>99.95%）As raw material, with magnesium titanate（MgTiO3）As dopant, after wet ball grinding mixing, then through drying, grinding, mistake Sieve obtains mixed powder.By gained powder it is dry-pressing formed after, be placed in electric furnace, be warming up to predetermined temperature insulation the regular hour, The magnesium titanate doped aluminium ceramics sample of densification is just obtained after cooling.
The formula of above-mentioned technical proposal is：The doping of magnesium titanate is 0.2 ~ 0.4 in every 100 grams of alumina powder raw materials Gram.
The hybrid technique parameter of above-mentioned technical proposal is：Ball-milling Time is 24 hours, and ball-milling medium is deionized water and oxygen Change zirconium ball, material：Water：Ball=1:2:3, drum's speed of rotation is 30-50 revs/min.
The Drying Technology Parameter of above-mentioned technical proposal is：Drying temperature is 100-150 DEG C.
The technological parameter of shaping and sintering in above-mentioned technical proposal is：The pressure of shaping is 50 ~ 150MPa, sintering temperature For 1580-1620 DEG C, soaking time is 3-5 hours, and programming rate is natural cooling after the completion of 2-5 degree per minute, sintering, i.e., It can obtain the magnesium titanate doped aluminium ceramics sample of densification.
The aluminium oxide ceramics prepared in a manner described has excellent microwave dielectric property.With Hakii- Coleman media Post the resonance method measure, its dielectric constant be 9.99-10.05, Q ×fValue is up to 1878900-199550GHz（Wherein, metatitanic acid is worked as When the doping of magnesium is 0.3wt%, the Q of the aluminium oxide ceramics of last gained ×fValue reaches up to 199550GHz）.
Compared with the doping such as magnesia or titanium oxide, be the magnesium ion and+4 valencys of one+divalent during metatitanic acid mg-doped Titanium ion solid solution simultaneously enters in aluminum oxide lattice, and its average valence is+trivalent, identical with aluminium ion valence state, therefore is not easily formed Vacancy defect, it is to avoid the problems such as dielectric loss increase and unstable performance occur.Present invention process route is simple, production procedure Short, equipment requirement is relatively low, is adapted to large-scale production.
Brief description of the drawings
Fig. 1 be magnesium titanate doped aluminium ceramics Q ×fIt is worth the change curve with metatitanic acid doped amount of magnesium.From Fig. 1 It can be seen that, when metatitanic acid doped amount of magnesium be 0.2-0.4 grams in every hectogram alumina amount, the Q of gained aluminium oxide ceramics ×f Value is higher, and when metatitanic acid doped amount of magnesium is too low or too high, Q ×fValue can be all decreased obviously.
With reference to Fig. 1 and embodiment, the present invention is further illustrated.
Embodiment
Embodiment 1：A kind of magnesium titanate doped aluminium ceramics, it, which is prepared by the following method, forms：Weigh high-purity Alumina powder（>99.95%）100 grams and 0.1 gram of magnesium titanate powder are as raw material, by the two addition ball grinder, plus deionization Water and zirconium oxide balls carry out wet ball grinding mixing（Material：Water：Ball=1:2:3）, Ball-milling Time is 24 hours, and drum's speed of rotation is 40 revs/min.Water is leached out afterwards, compound is dried in 120 DEG C of baking oven, sieved, uniform mixed powder is obtained. Appropriate binding agent is added in mixed powder, by powder dry-pressing into diameter about 16mm's, highly about 12mm under 100MPa pressure Cylindrical sample, is placed in silicon molybdenum rod furnace at 1600 DEG C and is incubated 4 hours.
The sample baked was placed after some hours, dielectricity is measured with Hakii- Coleman dielectric posts the resonance method Energy.As a result show：Gained magnesium titanate doped aluminium ceramics dielectric constant for 9.91, Q ×fIt is worth for 123300GHz（f= 10.51GHz)。
Embodiment 2：A kind of magnesium titanate doped aluminium ceramics, it, which is prepared by the following method, forms：Weigh high-purity Alumina powder（>99.95%）100 grams and 0.2 gram of magnesium titanate powder are as raw material, by the two addition ball grinder, plus deionization Water and zirconium oxide balls carry out wet ball grinding mixing（Material：Water：Ball=1:2:3）, Ball-milling Time is 24 hours, and drum's speed of rotation is 40 revs/min.Water is leached out afterwards, is sieved after compound is dried in 120 DEG C of baking oven, obtains uniform mixed powder. Appropriate binding agent is added in mixed powder, under 100MPa pressure by powder dry-pressing into diameter about 16mm, height about 12mm Cylindrical sample, be placed in silicon molybdenum rod furnace at 1600 DEG C be incubated 4 hours.
The sample baked was placed after some hours, dielectricity is measured with Hakii- Coleman dielectric posts the resonance method Energy.As a result show：Gained magnesium titanate doped aluminium ceramics dielectric constant for 9.99, Q ×fIt is worth for 187890GHz（f= 10.41GHz), than the aluminium oxide ceramics in example 1 Q ×fValue improves 52%.
Embodiment 3：A kind of magnesium titanate doped aluminium ceramics, it, which is prepared by the following method, forms：Weigh high-purity Alumina powder（>99.95%）100 grams and 0.3 gram of magnesium titanate powder are as raw material, by the two addition ball grinder, plus deionization Water and zirconium oxide balls carry out wet ball grinding mixing（Material：Water：Ball=1:2:3）, Ball-milling Time is 24 hours, and drum's speed of rotation is 40 revs/min.Water is leached out afterwards, is sieved after compound is dried in 120 DEG C of baking oven, obtains uniform mixed powder. Appropriate binding agent is added in mixed powder, under 100MPa pressure by powder dry-pressing into diameter about 16mm, height about 12mm Cylindrical sample, be placed in silicon molybdenum rod furnace at 1600 DEG C be incubated 4 hours.
The sample baked was placed after some hours, dielectricity is measured with Hakii- Coleman dielectric posts the resonance method Energy.As a result show：Gained magnesium titanate doped aluminium ceramic dielectric constant be 9.98, Q ×fIt is worth for 199550GHz（f= 10.43GHz), than the aluminium oxide ceramics in example 1 Q ×fValue improves 62%.
Embodiment 4：A kind of magnesium titanate doped aluminium ceramics, it, which is prepared by the following method, forms：Weigh high-purity Alumina powder（>99.95%）100 grams and 0.4 gram of magnesium titanate powder are as raw material, by the two addition ball grinder, plus deionization Water and zirconium oxide balls carry out wet ball grinding mixing（Material：Water：Ball=1:2:3）, Ball-milling Time is 24 hours, and drum's speed of rotation is 40 revs/min.Water is leached out afterwards, is sieved after compound is dried in 120 DEG C of baking oven, obtains uniform mixed powder. Appropriate binding agent is added in mixed powder, under 100MPa pressure by powder dry-pressing into diameter about 16mm, height about 12mm Cylindrical sample, be placed in silicon molybdenum rod furnace at 1600 DEG C be incubated 4 hours.
The sample baked was placed after some hours, dielectricity is measured with Hakii- Coleman dielectric posts the resonance method Energy.As a result show：Gained magnesium titanate doped aluminium ceramics dielectric constant for 10.05, Q ×fIt is worth for 191530GHz（f= 10.42GHz), than the aluminium oxide ceramics in example 1 Q ×fValue improves 55%.
Embodiment 5：A kind of magnesium titanate doped aluminium ceramics, it, which is prepared by the following method, forms：Weigh high-purity Alumina powder（>99.95%）100 grams and 0.5 gram of magnesium titanate powder are as raw material, by the two addition ball grinder, plus deionization Water and zirconium oxide balls carry out wet ball grinding mixing（Material：Water：Ball=1:2:3）, Ball-milling Time is 24 hours, and drum's speed of rotation is 40 revs/min.Water is leached out afterwards, is sieved after compound is dried in 120 DEG C of baking oven, obtains uniform mixed powder. Appropriate binding agent is added in mixed powder, under 100MPa pressure by powder dry-pressing into diameter about 16mm, height about 12mm Cylindrical sample, be placed in silicon molybdenum rod furnace at 1600 DEG C be incubated 4 hours.
The sample baked was placed after some hours, dielectricity is measured with Hakii- Coleman dielectric posts the resonance method Energy.As a result show：Gained magnesium titanate doped aluminium ceramics dielectric constant for 9.90, Q ×fIt is worth for 137440GHz（f= 10.48GHz), have dropped to Q only than the aluminium oxide ceramics in example 1 ×fValue is substantially suitable（It is only high by 11%）Level.

Claims (4)

1. a kind of magnesium titanate doped aluminium microwave-medium ceramics, it is characterised in that：
（1）With high-purity alumina powder（Alumina content>99.95%）For major ingredient, appropriate magnesium titanate dopant is added；
（2）By step（1）In major ingredient and dopant added water in ball mill ball milling, sieving obtains mixed powder after drying；
（3）By step（2）Obtained mixed powder is dry-pressing formed, fires, you can obtain required ceramics sample.
2. a kind of magnesium titanate doped aluminium microwave-medium ceramics according to claim 1, it is characterised in that：Step（2）In, The proportioning of major ingredient and sintering aid is 100：（0.2~0.4）（Percentage by weight）, the Ball-milling Time is 24 hours, ball-milling medium For zirconium oxide balls and deionized water, material：Water：Ball=1：2：3, drum's speed of rotation is 30-50 revs/min, and drying temperature is 100- 150℃。
3. a kind of magnesium titanate doped aluminium microwave-medium ceramics according to claim 1, it is characterised in that：Step（3）In, Described dry-pressing pressure is 50-150MPa, and sintering temperature is 1580-1620 DEG C, and soaking time is 3-5 hours, and programming rate is Natural cooling after the completion of 2-5 degree per minute, sintering.
4. a kind of magnesium titanate doped aluminium microwave-medium ceramics according to claim 1,2,3, it is characterised in that this oxygen Change aluminium microwave-medium ceramics have low-dielectric loss, high Q × fThe characteristics of value, with Hakii- Coleman dielectric posts the resonance methods Measurement, dielectric constant is 9.98-10.05, Q ×fIt is worth for 1878900- 199550GHz.
CN201710292933.6A 2017-04-28 2017-04-28 A kind of magnesium titanate doped aluminium microwave-medium ceramics Pending CN107129281A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116004012A (en) * 2022-12-24 2023-04-25 北京创盈光电医疗科技有限公司 Flexible heat storage phase change composite material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR960012727B1 (en) * 1994-05-23 1996-09-24 삼화콘덴서공업 주식회사 Dielectric composition and production thereof
CN1727303A (en) * 2005-06-29 2006-02-01 上海大学 Method for fabricating Mg, Ti adulterated Al2O3 crystalline material, and transparent laser ceramics
CN101962287A (en) * 2010-09-14 2011-02-02 石家庄铁道大学 Processable aluminium oxide base composite ceramic material and preparation method thereof
CN105084873A (en) * 2015-07-23 2015-11-25 华北理工大学 Preparation method for alumina-based microwave ceramic

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR960012727B1 (en) * 1994-05-23 1996-09-24 삼화콘덴서공업 주식회사 Dielectric composition and production thereof
CN1727303A (en) * 2005-06-29 2006-02-01 上海大学 Method for fabricating Mg, Ti adulterated Al2O3 crystalline material, and transparent laser ceramics
CN101962287A (en) * 2010-09-14 2011-02-02 石家庄铁道大学 Processable aluminium oxide base composite ceramic material and preparation method thereof
CN105084873A (en) * 2015-07-23 2015-11-25 华北理工大学 Preparation method for alumina-based microwave ceramic

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116004012A (en) * 2022-12-24 2023-04-25 北京创盈光电医疗科技有限公司 Flexible heat storage phase change composite material and preparation method thereof
CN116004012B (en) * 2022-12-24 2024-03-22 北京创盈光电医疗科技有限公司 Flexible heat storage phase change composite material and preparation method thereof

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Application publication date: 20170905