CN106927810A - Low temperature sintering high-dielectric constant dielectric material and its manufacture method - Google Patents

Low temperature sintering high-dielectric constant dielectric material and its manufacture method Download PDF

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CN106927810A
CN106927810A CN201710136590.4A CN201710136590A CN106927810A CN 106927810 A CN106927810 A CN 106927810A CN 201710136590 A CN201710136590 A CN 201710136590A CN 106927810 A CN106927810 A CN 106927810A
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dielectric constant
low temperature
dielectric material
temperature sintering
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李启云
刘超莲
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Hunan Yun Ping Environmental Protection Technology Co Ltd
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    • 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
    • C04B35/453—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
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    • H01G4/12—Ceramic dielectrics
    • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
    • H01G4/1254—Ceramic dielectrics characterised by the ceramic dielectric material based on niobium or tungsteen, tantalum oxides or niobates, tantalates
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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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • 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
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The present invention discloses a kind of manufacture method of low temperature sintering high-dielectric constant dielectric material.Comprise the following steps：By Bi2O3、ZnO、MgO、Nb2O5、Ta2O5In molar ratio 20：18：2：15：5 dispensings, add alcohol mixing and ball milling 8 10 hours, and slurry is dried；The powder that step S1 is obtained is calcined 35 hours under the conditions of 720 780 DEG C, forms principal crystalline phase；The AEO and alcohol mixing and ball milling 20 30 hours of 0.5wt% are added in powder after firing, and slurry is dried；Powder pressing prepared by step 3 is shaped to base substrate, and by base substrate in sintering at 950 DEG C~1000 DEG C, and 4~6 hours are incubated, furnace cooling.The low temperature sintering high-dielectric constant dielectric material preparation method that the present invention is provided, the capacitor material that realization is obtained under lower sintering temperature equally has dielectric constant higher.The present invention also provides a kind of low temperature sintering high-dielectric constant dielectric material obtained by manufacture method manufacture.

Description

Low temperature sintering high-dielectric constant dielectric material and its manufacture method
【Technical field】
The present invention relates to technical field of electronic materials, and in particular to a kind of low temperature sintering high-dielectric constant dielectric material and its Manufacture method.
【Background technology】
With the development of electronic product, electronic component is increasingly minimized, integration degree more and more higher.Realize micro- The miniaturization of wave device, high reliability and cheapness, it is necessary to develop the novel medium material with more superiority.Electronics unit The size of device, into negative correlation, will realize the miniaturization of microwave equipment with the dielectric constant of medium, must just develop more Gao Jie The material of electric constant, but high-k has bigger dielectric loss, seeks high-k, low dielectric loss all the time All it is the target of research and development.
In correlation technique, high-k is obtained, the ceramic material of low-dielectric loss is needed in sintering temperature bar higher Carried out under part, make energy consumption in the ceramic material manufacturing process, production cost high, be unfavorable for high-dielectric-constant ceramics electric capacity equipment The application of material and development.
Therefore, it is necessary to providing a kind of new technique solves above-mentioned technical problem.
【The content of the invention】
The purpose of the present invention is to overcome above-mentioned technical problem, there is provided a kind of system of low temperature sintering high-dielectric constant dielectric material Method is made, the capacitor material that realization is obtained under lower sintering temperature equally has dielectric constant higher.
The technical scheme is that：
A kind of manufacture method of low temperature sintering high-dielectric constant dielectric material, comprises the following steps：
Step S1：By Bi2O3、ZnO、MgO、Nb2O5、Ta2O5In molar ratio 20：18：2：15：5 dispensings, add alcohol mixing Ball milling 8-10 hours, slurry is dried；
Step S2：The powder that step S1 is obtained is calcined 3-5 hours under the conditions of 720-780 DEG C, forms principal crystalline phase；
Step S3：The AEO and alcohol mixing and ball milling 20- of 0.5wt% are added in powder after firing 30 hours, and slurry is dried；
Step S4：Powder pressing prepared by step 3 is shaped to base substrate, and by base substrate in sintering at 950 DEG C~1000 DEG C, And 4~6 hours are incubated, furnace cooling obtains described kind of low temperature sintering high-dielectric constant dielectric material.
Preferably, in step S1, S3, stoving process uses infrared drying, and drying temperature is 60-80 DEG C.
Preferably, in the step S3, will be dried after slurries filtration, filter screen aperture is 200-320 mesh.
The present invention also provides a kind of low temperature sintering high-dielectric constant dielectric material, is situated between by the low temperature sintering high-dielectric constant The manufacture method manufacture of material is obtained.
Preferably, the permittivity ε of the low temperature sintering high-dielectric constant dielectric materialrIt is under 1MHz test conditions 180-200, temperature coefficient of capacitance is -27 × 10 under the conditions of 0 DEG C-6/ DEG C~-20 × 10-6/℃。
Compared with correlation technique, the manufacture method of the low temperature sintering high-dielectric constant dielectric material that the present invention is provided is beneficial Effect is：There is provided a kind of Bi, Zn atom doped Bi2O3-ZnO-Nb2O5Ternary system ceramics medium, and by optimizing manufacture work Skill step, making to sinter at a lower temperature the capacitor material for obtaining has the advantages that dielectric constant is high, dielectric loss is low.Through inspection Survey, the manufacture method of the low temperature sintering high-dielectric constant dielectric material provided using the present invention, the capacitor material that manufacture is obtained Permittivity εrIt is 180-200 under 1MHz test conditions, temperature coefficient of capacitance is -27 × 10 under the conditions of 0 DEG C-6/ DEG C~- 20×10-6/℃。
【Specific embodiment】
Below will the invention will be further described by specific embodiment.
Embodiment 1
A kind of manufacture method of low temperature sintering high-dielectric constant dielectric material, comprises the following steps：
Step S1：By Bi2O3、ZnO、MgO、Nb2O5、Ta2O5In molar ratio 20：18：2：15：5 dispensings, add alcohol mixing Ball milling 8-10 hours, slurry is dried；
Wherein, using infrared drying technique, drying temperature is 60 DEG C；
Step S2：The powder that step S1 is obtained is calcined 3-5 hours under the conditions of 720 DEG C, forms principal crystalline phase；
Step S3：The AEO and alcohol mixing and ball milling 20- of 0.5wt% are added in powder after firing 30 hours, slurry is dried after 200 mesh sieve；Stoving process is infrared drying, and drying temperature is 60 DEG C；
Step S4：Powder pressing prepared by step 3 is shaped to base substrate, and by base substrate in sintering at 950 DEG C, and it is incubated 4 ~6 hours, furnace cooling obtained described kind of low temperature sintering high-dielectric constant dielectric material.
Embodiment 2
A kind of manufacture method of low temperature sintering high-dielectric constant dielectric material, comprises the following steps：
Step S1：By Bi2O3、ZnO、MgO、Nb2O5、Ta2O5In molar ratio 20：18：2：15：5 dispensings, add alcohol mixing Ball milling 8-10 hours, slurry is dried；
Wherein, using infrared drying technique, drying temperature is 70 DEG C；
Step S2：The powder that step S1 is obtained is calcined 3-5 hours under the conditions of 750 DEG C, forms principal crystalline phase；
Step S3：The AEO and alcohol mixing and ball milling 20- of 0.5wt% are added in powder after firing 30 hours, slurry is dried after 320 mesh sieve；Stoving process is infrared drying, and drying temperature is 70 DEG C；
Step S4：Powder pressing prepared by step 3 is shaped to base substrate, and by base substrate in sintering at 980 DEG C, and it is incubated 4 ~6 hours, furnace cooling obtained described kind of low temperature sintering high-dielectric constant dielectric material.
Embodiment 3
A kind of manufacture method of low temperature sintering high-dielectric constant dielectric material, comprises the following steps：
Step S1：By Bi2O3、ZnO、MgO、Nb2O5、Ta2O5In molar ratio 20：18：2：15：5 dispensings, add alcohol mixing Ball milling 8-10 hours, slurry is dried；
Wherein, using infrared drying technique, drying temperature is 80 DEG C；
Step S2：The powder that step S1 is obtained is calcined 3-5 hours under the conditions of 780 DEG C, forms principal crystalline phase；
Step S3：The AEO and alcohol mixing and ball milling 20- of 0.5wt% are added in powder after firing 30 hours, slurry is dried after 200 mesh sieve；Stoving process is infrared drying, and drying temperature is 80 DEG C；
Step S4：Powder pressing prepared by step 3 is shaped to base substrate, and by base substrate in sintering at 1000 DEG C, and it is incubated 4 ~6 hours, furnace cooling obtained described kind of low temperature sintering high-dielectric constant dielectric material.
Embodiment 4
A kind of manufacture method of low temperature sintering high-dielectric constant dielectric material, comprises the following steps：
Step S1：By Bi2O3、ZnO、MgO、Nb2O5、Ta2O5In molar ratio 20：18：2：15：5 dispensings, add alcohol mixing Ball milling 8-10 hours, slurry is dried；
Wherein, using infrared drying technique, drying temperature is 68 DEG C；
Step S2：The powder that step S1 is obtained is calcined 3-5 hours under the conditions of 760 DEG C, forms principal crystalline phase；
Step S3：The AEO and alcohol mixing and ball milling 20- of 0.5wt% are added in powder after firing 30 hours, slurry is dried after 320 mesh sieve；Stoving process is infrared drying, and drying temperature is 68 DEG C；
Step S4：Powder pressing prepared by step 3 is shaped to base substrate, and by base substrate in sintering at 960 DEG C, and it is incubated 4 ~6 hours, furnace cooling obtained described kind of low temperature sintering high-dielectric constant dielectric material.
Embodiment 5
A kind of manufacture method of low temperature sintering high-dielectric constant dielectric material, comprises the following steps：
Step S1：By Bi2O3、ZnO、MgO、Nb2O5、Ta2O5In molar ratio 20：18：2：15：5 dispensings, add alcohol mixing Ball milling 8-10 hours, slurry is dried；
Wherein, using infrared drying technique, drying temperature is 72 DEG C；
Step S2：The powder that step S1 is obtained is calcined 3-5 hours under the conditions of 740 DEG C, forms principal crystalline phase；
Step S3：The AEO and alcohol mixing and ball milling 20- of 0.5wt% are added in powder after firing 30 hours, slurry is dried after 320 mesh sieve；Stoving process is infrared drying, and drying temperature is 72 DEG C；
Step S4：Powder pressing prepared by step 3 is shaped to base substrate, and by base substrate in sintering at 990 DEG C, and it is incubated 4 ~6 hours, furnace cooling obtained described kind of low temperature sintering high-dielectric constant dielectric material.
Embodiment 6
A kind of manufacture method of low temperature sintering high-dielectric constant dielectric material, comprises the following steps：
Step S1：By Bi2O3、ZnO、MgO、Nb2O5、Ta2O5In molar ratio 20：18：2：15：5 dispensings, add alcohol mixing Ball milling 8-10 hours, slurry is dried；
Wherein, using infrared drying technique, drying temperature is 68 DEG C；
Step S2：The powder that step S1 is obtained is calcined 3-5 hours under the conditions of 740 DEG C, forms principal crystalline phase；
Step S3：The AEO and alcohol mixing and ball milling 20- of 0.5wt% are added in powder after firing 30 hours, slurry is dried after 200 mesh sieve；Stoving process is infrared drying, and drying temperature is 68 DEG C；
Step S4：Powder pressing prepared by step 3 is shaped to base substrate, and by base substrate in sintering at 970 DEG C, and it is incubated 4 ~6 hours, furnace cooling obtained described kind of low temperature sintering high-dielectric constant dielectric material.
The ceramic material that the manufacture method manufacture of the low temperature sintering high-dielectric constant dielectric material described in embodiment 1-6 is obtained Material carries out performance detection, and testing result is as follows：
Compared with correlation technique, the manufacture method of the low temperature sintering high-dielectric constant dielectric material that the present invention is provided is beneficial Effect is：There is provided a kind of Bi, Zn atom doped Bi2O3-ZnO-Nb2O5Ternary system ceramics medium, and by optimizing manufacture work Skill step, making to sinter at a lower temperature the capacitor material for obtaining has the advantages that dielectric constant is high, dielectric loss is low.Through inspection Survey, the manufacture method of the low temperature sintering high-dielectric constant dielectric material provided using the present invention, the capacitor material that manufacture is obtained Permittivity εrIt is 180-200 under 1MHz test conditions, temperature coefficient of capacitance is -27 × 10 under the conditions of 0 DEG C-6/ DEG C~- 20×10-6/℃。
Above-described is only embodiments of the present invention, it should be noted here that for one of ordinary skill in the art For, without departing from the concept of the premise of the invention, improvement can also be made, but these belong to protection model of the invention Enclose.

Claims (5)

1. a kind of manufacture method of low temperature sintering high-dielectric constant dielectric material, it is characterised in that comprise the following steps：
Step S1：By Bi2O3、ZnO、MgO、Nb2O5、Ta2O5In molar ratio 20：18：2：15：5 dispensings, add alcohol mixing and ball milling 8-10 hours, slurry is dried；
Step S2：The powder that step S1 is obtained is calcined 3-5 hours under the conditions of 720-780 DEG C, forms principal crystalline phase；
Step S3：Add the AEO and alcohol mixing and ball milling 20-30 of 0.5wt% small in powder after firing When, and slurry is dried；
Step S4：Powder pressing prepared by step 3 is shaped to base substrate, and by base substrate in sintering at 950 DEG C~1000 DEG C, and protect Temperature 4~6 hours, furnace cooling obtains described kind of low temperature sintering high-dielectric constant dielectric material.
2. the manufacture method of low temperature sintering high-dielectric constant dielectric material according to claim 1, it is characterised in that described In step S1, S3, stoving process uses infrared drying, and drying temperature is 60-80 DEG C.
3. the manufacture method of low temperature sintering high-dielectric constant dielectric material according to claim 1, it is characterised in that described In step S3, will be dried after slurries filtration, filter screen aperture is 200-320 mesh.
4. a kind of low temperature sintering high-dielectric constant dielectric material, it is characterised in that low as any one of claim 1-3 The manufacture method manufacture of warm sintering high-dielectric constant dielectric material is obtained.
5. low temperature sintering high-dielectric constant dielectric material according to claim 4, it is characterised in that the low-temperature sintering is high The permittivity ε of dielectric constant dielectric materialrIt is 180-200, temperature coefficient of capacitance under the conditions of 0 DEG C under 1MHz test conditions It is -27 × 10-6/ DEG C~-20 × 10-6/℃。
CN201710136590.4A 2017-03-08 2017-03-08 Low temperature sintering high-dielectric constant dielectric material and its manufacture method Pending CN106927810A (en)

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Publication number Priority date Publication date Assignee Title
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CN105777106A (en) * 2016-03-04 2016-07-20 天津大学 Low-temperature-sintered low-loss ceramic capacitor dielectric material
CN105801104A (en) * 2016-02-23 2016-07-27 天津大学 High dielectric constant temperature stable type ceramic capacitor dielectric material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105565799A (en) * 2015-12-18 2016-05-11 天津大学 Low-loss temperature-stable high-frequency dielectric ceramic
CN105801104A (en) * 2016-02-23 2016-07-27 天津大学 High dielectric constant temperature stable type ceramic capacitor dielectric material
CN105777106A (en) * 2016-03-04 2016-07-20 天津大学 Low-temperature-sintered low-loss ceramic capacitor dielectric material

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Title
V.P.SIROTINKIN ETAL.: "Preraration and Dielectric or Bi1.5MNb1.5O7(M=Cu,Mg,Mn,Ni,Zn)Pyrochlore Oxides", 《INORGANIC MATERIALS》 *
彭小松等: "Ta2O5掺杂Bi2O3–ZnO–Nb2O5 陶瓷的晶体结构、结晶化学及介电性能", 《硅酸盐学报》 *

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