CN106938920A - A kind of low-dielectric loss alumina ceramic material - Google Patents

A kind of low-dielectric loss alumina ceramic material Download PDF

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CN106938920A
CN106938920A CN201710192403.4A CN201710192403A CN106938920A CN 106938920 A CN106938920 A CN 106938920A CN 201710192403 A CN201710192403 A CN 201710192403A CN 106938920 A CN106938920 A CN 106938920A
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ceramic material
dielectric loss
low
catio
ball
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李蔚
胡家驹
程玉晶
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East China University of Science and Technology
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    • 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
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Abstract

The present invention discloses a kind of low-dielectric loss Al2O3Ceramic material and its manufacture method.It is characterized in high-purity alumina powder（Alumina content>99.95%）CaTiO is added for major ingredient3Dopant（Per 100gAl2O3CaTiO in powder material3Doping be 0.1 ~ 0.5g）, ball milling utilizes dry-pressing formed obtained ceramic green after mixing, is then placed in electric furnace, 1,550 1650 DEG C of 2 4h of sintering, you can obtain the dielectric loss very low alumina ceramic material of densification（Dielectric constant：9.81 9.87, Q ×fValue：176000‑226000GHz）.The present invention selects CaTiO3Adulterate to reduce Al2O3The dielectric loss of ceramic material, and MgO, TiO2Compared Deng doping, CaTiO3It is the Ca ions of one+divalent and the Ti ions of+4 valencys during doping while solid solution enters Al2O3In lattice, its average valence is+trivalent, with Al3+Valence state is identical, therefore is not easily formed vacancy defect, it is to avoid the problems such as dielectric loss increase and unstable properties occur.

Description

A kind of low-dielectric loss alumina ceramic material
Technical field
The present invention relates to a kind of low-dielectric loss Al2O3Ceramic material, is a kind of environmentally friendly microwave dielectric ceramic material Material, available for fields such as microwave communications.
Background technology
Al2O3Ceramics are a kind of important dielectric materials, with electrical insulation capability is good, dielectric constant is low, dielectric loss is low, Thermal conductivity is higher, mechanical strength is higher, and high temperature resistant, it is wear-resisting and resistant to chemical etching the features such as, it is and cheap, technique into It is ripe, there is extensive purposes in fields such as electronics, communication, electrovacuums.But, with the high speed development of the technologies such as communication, to material The requirement of material is increasingly harsh, Al2O3The deficiency of ceramic material is more and more obvious.Most one of distinct issues are exactly that dielectric loss is inclined Greatly.Although theoretically seeing, Al is improved2O3Purity can just reduce Al2O3The dielectric loss of ceramic material, but in reality In, high-purity Al2O3Powder might not can guarantee that high Q ×fValue or low-dielectric loss, the preparation process of material It is more important.Because：Al2O3Dielectric loss in ceramic material is by intrinsic loss（intrinsic loss）With it is extrinsic Loss（extrinsic loss）Two parts are constituted.Cause Al2O3The big principal element of the total dielectric loss of ceramic material is extrinsic The fault of construction produced in loss, rather than intrinsic loss and material preparation process for example impurity, crystal boundary, room, stomata, micro-crack and Crystal grain orientation etc. is closely related.Therefore, optimize preparation technology to reduce Al2O3The dielectric loss of ceramic material is just increasingly subject to close Note.And " doping " technique therein, i.e., in Al2O3Upper appropriate compound is added in ceramic material, more because its controllability is good, behaviour The property made turns into by force the focus researched and developed both at home and abroad.Such as, N.M.Alord et al. passes through in Al2O3Added in ceramic material 0.5wt%TiO2, make tan δ by 2.7 × 10-5It is down to 2.0 × 10-5（Q ×fValue reaches 452790GHz）.C.L.Huang et al. is adopted With high-purity nanometer Al2O3Powder is raw material and adds 0.5wt%TiO2, by Q ×fValue is further improved to 680000GHz （Under 14GHz）.At home, the Zhang Juxian of research institute of electronics technology group company the 12nd is in Al2O3Mixed in ceramic material a small amount of MgO, reduces bulk porosity using double sintering, tan δ is greatly reduced to 1 × 10-5（Under 9503MHz）.But, MgO, TiO2Although doping is common, has one disadvantage in that, be exactly Mg2+、Ti4+With Al3+Valence state is different, as MgO, TiO2Doping is solidly soluted into Al2O3When in lattice, vacancy defect is easily formed, causes dielectric loss to increase, unstable properties.
The content of the invention
Present invention aims at provide a kind of low-dielectric loss Al2O3Ceramic material, solves Al in the prior art2O3Ceramics Dielectric loss（tanδ）Higher the problem of, 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 Al2O3Powder（>99.95%） As raw material, from CaTiO3As dopant, after wet ball grinding mixing, dry at a certain temperature, then it is ground, sieve To mixed powder.By gained mixed powder it is dry-pressing formed after, be positioned in electric furnace be warming up to predetermined temperature insulation the regular hour, The Al of densification is just obtained after cooling2O3Ceramic material sample
The formula of above-mentioned technical proposal is：Per 100gAl2O3CaTiO in powder material3Doping be 0.1 ~ 0.5g.
The hybrid technique parameter of above-mentioned technical proposal is：Ball-milling Time is 12-24h, and ball-milling medium is deionized water and oxygen Change zirconium ball, material：Water：Ball=1:2:3.
The Drying Technology Parameter of above-mentioned technical proposal is：Drying temperature is 100-120 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 1550-1650 DEG C, soaking time is 2-4h, and programming rate is natural cooling after the completion of 2-5 degree per minute, sintering, you can To fine and close Al2O3Ceramic material sample.
The Al prepared in a manner described2O3Ceramic material has excellent microwave dielectric property, and its dielectric constant is 9.81- 9.87, and Q ×fValue is up to 176000-226000GHz（Wherein, CaTiO is worked as3Doping when being 0.4wt%, last gained Al2O3The Q of ceramic material ×fValue reaches up to 226000GHz, about pure Al2O32 times of ceramic material）.
With MgO, TiO2Compared Deng doping, CaTiO3It is the Ca ions of one+divalent and the Ti ions of+4 valencys during doping Solid solution simultaneously enters Al2O3In lattice, its average valence is+trivalent, with Al3+Valence state is identical, therefore is not easily formed vacancy defect, The problems such as avoiding the occurrence of dielectric loss increase and unstable properties.Operating method of the present invention is simple, and production procedure is short, required Process equipment is also very simple, is adapted to large-scale production.
Brief description of the drawings
Fig. 1 is CaTiO3Adulterate Al2O3The Q of ceramic material ×fValue is with CaTiO3The change curve of doping.
With reference to Fig. 1 and embodiment, the present invention is further illustrated.
Embodiment
Embodiment 1：A kind of pure Al2O3Ceramic material, it, which is prepared by the following method, forms：Take high-purity Al2O3Powder （>99.95%）, appropriate binding agent is added, columnar samples of the dry-pressing into diameter about 16mm, height about 12mm under 100MPa pressure Product, are placed in silicon molybdenum rod furnace and are incubated 4h at 1600 DEG C.
The sample baked was placed after some hours, dielectric properties test is carried out, as a result shows：The pure alumina of gained Ceramic material sample dielectric constant be 9.86, Q ×fIt is worth for 1,14000GHz（f=10.38GHz)。
Embodiment 2：A kind of low-dielectric loss Al2O3Ceramic material, it, which is prepared by the following method, forms：Weigh height Pure Al2O3Powder（>99.95%）100g and CaTiO3Powder 0.1g adds the two in ball grinder as raw material, plus deionized water Wet ball grinding mixing is carried out with zirconium oxide balls（Material：Water：Ball=1:2:3）, Ball-milling Time is 24h.Water is leached out afterwards, will Compound sieves after being dried in 100 DEG C of baking oven, obtains uniform mixed powder.Appropriate bond is added in mixed powder Agent, silicon molybdenum rod furnace is placed under 100MPa pressure by powder dry-pressing into diameter about 16mm, height about 12mm cylindrical sample In be incubated 4h at 1600 DEG C.
The sample baked was placed after some hours, dielectric properties test is carried out, as a result shows：Gained CaTiO3Doping The dielectric constant of alumina ceramic material be 9.85, Q ×fIt is worth for 176000GHz（f=10.41GHz), than pure in example 1 The Q of alumina ceramic material ×fValue improves 54%.
Embodiment 3：A kind of low-dielectric loss Al2O3Ceramic material, it, which is prepared by the following method, forms：Weigh height Pure Al2O3Powder（>99.95%）100g and CaTiO3Powder 0.2g adds the two in ball grinder as raw material, plus deionized water Wet ball grinding mixing is carried out with zirconium oxide balls（Material：Water：Ball=1:2:3）, Ball-milling Time is 24h.Water is leached out afterwards, will Compound sieves after being dried in 100 DEG C of baking oven, obtains uniform mixed powder.Appropriate bond is added in mixed powder Agent, silicon molybdenum rod furnace is placed under 100MPa pressure by powder dry-pressing into diameter about 16mm, height about 12mm cylindrical sample In be incubated 4h at 1600 DEG C.
The sample baked was placed after some hours, dielectric properties test is carried out, as a result shows：Gained CaTiO3Doping The dielectric constant of alumina ceramic material be 9.87, Q ×fIt is worth for 194000GHz（f=10.40GHz), than pure in example 1 The Q of alumina ceramic material ×fValue improves 70%.
Embodiment 4：A kind of low-dielectric loss Al2O3Ceramic material, it, which is prepared by the following method, forms：Weigh height Pure Al2O3Powder（>99.95%）100g and CaTiO3Powder 0.3g adds the two in ball grinder as raw material, plus deionized water Wet ball grinding mixing is carried out with zirconium oxide balls（Material：Water：Ball=1:2:3）, Ball-milling Time is 24h.Water is leached out afterwards, will Compound sieves after being dried in 100 DEG C of baking oven, obtains uniform mixed powder.Appropriate bond is added in mixed powder Agent, silicon molybdenum rod furnace is placed under 100MPa pressure by powder dry-pressing into diameter about 16mm, height about 12mm cylindrical sample In be incubated 4h at 1600 DEG C.
The sample baked was placed after some hours, dielectric properties test is carried out, as a result shows：Gained CaTiO3Doping Alumina ceramic material dielectric constant be 9.84, Q ×fIt is worth for 210000GHz（f=10.39GHz), than the pure oxygen in example 1 The Q of change aluminium ceramic material ×fValue improves 84%.
Embodiment 5：A kind of low-dielectric loss Al2O3Ceramic material, it, which is prepared by the following method, forms：Weigh height Pure Al2O3Powder（>99.95%）100g and CaTiO3Powder 0.4g adds the two in ball grinder as raw material, plus deionized water Wet ball grinding mixing is carried out with zirconium oxide balls（Material：Water：Ball=1:2:3）, Ball-milling Time is 24h.Water is leached out afterwards, will Compound sieves after being dried in 80 DEG C of baking oven, obtains uniform mixed powder.Appropriate binding agent is added in mixed powder, Powder dry-pressing is placed in silicon molybdenum rod furnace into diameter about 16mm, height about 12mm cylindrical sample under 100MPa pressure 4h is incubated at 1600 DEG C.
The sample baked was placed after some hours, dielectric properties test is carried out, as a result shows：Gained CaTiO3Doping The dielectric constant of alumina ceramic material be 9.81, Q ×fIt is worth for 226000GHz（f=10.39GHz), than pure in example 1 The Q of alumina ceramic material ×fValue improves 98%.
Embodiment 6：A kind of low-dielectric loss Al2O3Ceramic material, it, which is prepared by the following method, forms：Weigh height Pure Al2O3Powder（>99.95%）100g and CaTiO3Powder 0.5g adds the two in ball grinder as raw material, plus deionized water Wet ball grinding mixing is carried out with zirconium oxide balls（Material：Water：Ball=1:2:3）, Ball-milling Time is 24h.Water is leached out afterwards, will Compound sieves after being dried in 100 DEG C of baking oven, obtains uniform mixed powder.Appropriate bond is added in mixed powder Agent, silicon molybdenum rod furnace is placed under 100MPa pressure by powder dry-pressing into diameter about 16mm, height about 12mm cylindrical sample In be incubated 4h at 1600 DEG C.
The sample baked was placed after some hours, dielectric properties test is carried out, as a result shows：Gained CaTiO3Doping The dielectric constant of alumina ceramic material be 9.85, Q ×fIt is worth for 207000GHz（f=10.42GHz), than pure in example 1 The Q of alumina ceramic material ×fValue improves 82%.

Claims (5)

1. a kind of low-dielectric loss Al2O3Ceramic material and its manufacture method, it is characterised in that：
With high-purity alumina powder（Alumina content>99.95%）For major ingredient, add and add appropriate CaTiO3 Dopant.
2. by step（1）In major ingredient and dopant added water in ball mill ball milling, sieving obtains mixed powder after drying：
By step（2）Obtained mixed powder is dry-pressing formed, fires, you can obtain required ceramic material sample.
3. low-dielectric loss Al according to claim 12O3Ceramic material and its manufacture method, it is characterised in that：Step（1）、 （2）In, the proportioning of major ingredient and sintering aid is 100：（0.1~0.5）（Percentage by weight）, the Ball-milling Time is 12 ~ 24h, ball Grinding media is zirconium oxide balls and deionized water, material：Water：Ball=1：2：3, drying temperature is 100-120 DEG C.
4. low-dielectric loss Al according to claim 12O3Ceramic material and its manufacture method, it is characterised in that：Step（3） In, described dry-pressing pressure is 50-150MPa, and sample sintering temperature is 1550 ~ 1650 DEG C, and programming rate is 2 ~ 5 DEG C/min, is protected The warm time is 2 ~ 5h.
5. the low-dielectric loss Al according to claim 1,2,3,42O3Ceramic material and its manufacture method, it is characterised in that：Will The sample baked was placed after some hours, is carried out performance test, is as a result shown：This low sintering alumina ceramic material Dielectric properties are good, and its dielectric constant is 9.81-9.87, and Q × fValue is up to 176000-226000GHz.
CN201710192403.4A 2017-03-28 2017-03-28 A kind of low-dielectric loss alumina ceramic material Pending CN106938920A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62229711A (en) * 1986-03-31 1987-10-08 日本特殊陶業株式会社 Alumina porcelain compound
US20030107455A1 (en) * 2001-10-23 2003-06-12 Yoshihiko Imanaka Integrated ceramic module and microwave dielectric composition
CN101925557A (en) * 2008-01-21 2010-12-22 住友化学株式会社 Aluminum magnesium titanate - alumina composite ceramic
CN105985102A (en) * 2015-01-30 2016-10-05 上海光线新材料科技有限公司 Microwave dielectric ceramic material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62229711A (en) * 1986-03-31 1987-10-08 日本特殊陶業株式会社 Alumina porcelain compound
US20030107455A1 (en) * 2001-10-23 2003-06-12 Yoshihiko Imanaka Integrated ceramic module and microwave dielectric composition
CN101925557A (en) * 2008-01-21 2010-12-22 住友化学株式会社 Aluminum magnesium titanate - alumina composite ceramic
CN105985102A (en) * 2015-01-30 2016-10-05 上海光线新材料科技有限公司 Microwave dielectric ceramic material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张康等: "CaTiO_3添加剂对氧化铝陶瓷烧结、显微结构及微波介电性能的影响", 《硅酸盐通报》 *

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