CN108727013A - A kind of ultralow dielectric loss high-dielectric-constant ceramics dielectric material and preparation method thereof - Google Patents
A kind of ultralow dielectric loss high-dielectric-constant ceramics dielectric material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of addition Bi2O3(Eu0.5Nb0.5)0.01Ti0.99O2Ultralow dielectric loss high-dielectric-constant ceramics dielectric material and preparation method thereof, stoichiometric equation xwt%Bi2O3(100-x) wt% (Eu0.5Nb0.5)0.01Ti0.99O2, wherein 0<x≤3.Preparation method is to carry out dispensing by chemical composition, is mixed, and is dried, sieving, pre-burning, secondary wet process ball milling, cold isostatic compaction, sinters porcelain into, and ultra-low loss high-dielectric-constant ceramics dielectric material is made in the techniques such as silver ink firing.Dielectric material dielectric constant prepared by the present invention is more than 25000, and minimum dielectric loss is 0.015, there is good frequency (20Hz-106) and temperature stability (- 150~200 DEG C) Hz.Dielectric material prepared by the present invention is highly practical, can be used for microelectronic industry, especially dynamic random storage and high dielectric ceramic capacitor.
Description
Technical field
The invention belongs to electronic ceramic fields, are applied to electronic component, it is normal to be related to a kind of high dielectric of ultralow dielectric loss
Number ceramic dielectric material and preparation method thereof.
Background technology
With the rapid development of microelectronic industry, increasingly to being miniaturized of ceramic capacitor, integrated, intelligent requirements
It is high.Ceramic capacitor because have many advantages, such as wide use temperature range, long lifespan, dependable performance and be widely used in dynamically with
On machine memory (DRAM).DRAM is the maximum semiconductor memory of dosage on computer.Dielectric with high-k
Material can further enhance the storage density of DRAM, to improve integrated level.It is co-doped with TiO using trivalent and pentavalent ion2?
20-106There is very high dielectric constant in Hz frequencies and -150-200 DEG C of temperature ranges, causes dielectric material area research people
The very big concern of member.But its loss is often both greater than 0.02.It is well known that high dielectric loss often leads to device or circuit
Fever, job insecurity or signal the problems such as decaying, to seriously limit the industrialized production of ceramics.In general,
In practical application, when a kind of loss of dielectric material is less than 0.02, so that it may with by industrialized production.So ensureing dielectric constant
It is most important that dielectric loss is further decreased in the case of constant.
2013 Nian Liu rues seminars report In and Nb and are co-doped with titanium dioxide ceramic with high dielectric constant, low dielectric
Loss and good frequency and temperature stability.Then, scientific research personnel by various methods (such as adulterate, different by different ions
Method preparation etc.) it is expected to obtain better dielectric properties.But unfortunately, these methods obtain dielectric material loss according to
So very it is big (>0.02), it is difficult to meet the requirement of practical application, such as patent 201410705357.X.
Invention content
For problems of the prior art, the present invention provides a kind of ultralow dielectric loss high-dielectric-constant ceramics dielectric
Material and preparation method thereof solves the problems, such as that ceramic dielectric material dielectric loss is larger.
The present invention is to be achieved through the following technical solutions：
A kind of ultralow dielectric loss high-dielectric-constant ceramics dielectric material, stoichiometric equation xwt%Bi2O3-(100-
X) wt% (Eu0.5Nb0.5)0.01Ti0.99O2, wherein 0<x≤3.
Preferably, when frequency is 103-104When Hz, dielectric constant be more than 25000, dielectric loss 0.015-0.017 it
Between.
A kind of preparation method of above-mentioned ultralow dielectric loss high-dielectric-constant ceramics dielectric material, by Bi2O3Powder and
(Eu0.5Nb0.5)0.01Ti0.99O2Ceramic powder mixed ingredients, after ball milling, drying, after pre-burning and molding, at 1350-1500 DEG C
Lower heat preservation 2-6h sinters porcelain into, obtains the ceramic dielectric material of ultralow dielectric loss high-k.
Preferably, (Eu0.5Nb0.5)0.01Ti0.99O2Ceramic powder is made by the following method：According to chemical formula
(Eu0.5Nb0.5)0.01Ti0.99O2, europium oxide, niobium oxide and titanium dioxide are kept the temperature at 1200 DEG C to 2h after ball milling and drying, are made
(Eu0.5Nb0.5)0.01Ti0.99O2Ceramic powder.
Preferably, the temperature of pre-burning is 1100-1200 DEG C, time 2-3h.
Preferably, ball milling is wet ball grinding, and ball-milling medium is absolute ethyl alcohol, and ballstone is zirconium dioxide ballstone.
Preferably, the Ball-milling Time of ball milling is 4-6h.
Preferably, the drying temperature of drying is 40-60 DEG C.
Preferably, molding technique refers to isostatic cool pressing technique.
Compared with prior art, the present invention has technique effect beneficial below：
The present invention is prepared for addition Bi2O3(Eu0.5Nb0.5)0.01Ti0.99O2Ceramic dielectric material, obtained ceramic dielectric
Material is no more than 10 in frequency4Dielectric constant is greater than 25000 when Hz, and minimum dielectric loss is 0.015, is less than 0.02, and have
There are good frequency and temperature stability.Its basic principle is：Theoretical according to electronics pinning disfigurement model, most of trivalents are dilute
Native ion and individual trivalent ions and Nb5+Or Ta5+Excellent dielectric properties can be generated by being co-doped with titanium dioxide, moreover, pentavalent from
Son is conducive to improve dielectric constant, and trivalent ion advantageously reduces dielectric loss.It is co-doped with titanium dioxide with europium ion and niobium ion
Dielectric constant up to 105, but its loss cannot meet industrial requirements 0.1 or so.Therefore it is necessary to reduce its dielectric damage
Consumption.Ceramic capacitor belongs to polycrystal, and crystal grain and crystal boundary generally have different resistance, according to grain boundary layer blocking effect
(IBLC), grain boundary layer is thicker, and the resistance activation energy of grain boundaries is higher, and the conductivity of crystal boundary is smaller, advantageously reduces Jie of material
Electrical loss.Bismuth oxide additive is added into ceramics by the present invention keeps the resistance of its grain boundaries very big, further decreases Jie of material
Electrical loss.Compared with rare earth element, China's bismuth resource rich content accounts for 70% or more of world's gross reserves, is easy to industrialization.Cause
This, the present invention (Eu0.5Nb0.5)0.01Ti0.99O2Middle addition Bi2O3, to obtain the dielectric material for meeting real requirement.
The preparation method of the present invention uses conventional solid-state method, and equipment used is simple, and preparation method is simple, reproducible,
Operation is easy；Accurate instrument is not needed, therefore be at low cost；Easy control of reaction conditions, therefore can be mass-produced；It obtains
Ceramic dielectric material is no more than 10 in frequency4Dielectric constant is greater than 25000 when Hz, and minimum dielectric loss is 0.015, is less than
0.02, and there is good frequency and temperature stability, better than the ceramic capacitor dielectric material being previously reported.Be conducive to electronics
The miniaturization of component and integrated, provides the foundation to prepare high energy storage density ceramic material, disclosure satisfy that practicability requirement,
It can be widely applied to microelectronic industry.
Description of the drawings
Fig. 1 is that present example 4 prepares 2wt%Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramic dielectric constant with
Frequency variation curve figure.
Fig. 2 is that present example 1 and example 4 prepare (Eu respectively0.5Nb0.5)0.01Ti0.99O2Ceramics and 2wt%Bi2O3-
98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramic dielectric is lost with frequency variation curve figure.
Fig. 3 is that present example 4 prepares 2wt%Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramic dielectric constant with
Temperature changing curve diagram.
Fig. 4 is that present example 4 prepares 2wt%Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2The SEM figures of ceramics.
Specific implementation mode
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The present invention is based on the reason for generating huge dielectric constant mechanism to trivalent ion and pentavalent ions doped titanium dioxide
Xie Shang seeks a kind of giant dielectric material disclosure satisfy that the applications such as dynamic random storage and high dielectric capacitor.
Ultralow dielectric loss high-dielectric-constant ceramics dielectric material of the present invention, stoichiometric equation xwt%
Bi2O3(100-x) wt% (Eu0.5Nb0.5)0.01Ti0.99O2, wherein 0<x≤3.
When frequency is 103-104When Hz, dielectric constant is more than 25000, and dielectric loss is between 0.015-0.017.
Preparation method includes the following steps：
(1) according to chemical formula (Eu0.5Nb0.5)0.01Ti0.99O2, by europium oxide, niobium oxide and titanium dioxide through wet ball grinding,
2h is kept the temperature after drying at 1200 DEG C, (Eu is made0.5Nb0.5)0.01Ti0.99O2Ceramic powder.
(2) by Bi2O3Powder and (Eu0.5Nb0.5)0.01Ti0.99O2Ceramic powder according to chemical formula xwt%Bi2O3-
(100-x) wt% (Eu0.5Nb0.5)0.01Ti0.99O2Carry out dispensing, wherein 0<X≤3, after wet ball grinding, drying, through pre-burning and at
After type, heat preservation 2-6h sinters porcelain at 1350-1500 DEG C, obtains the ceramic dielectric material of ultralow dielectric loss high-k
Material.
The ball-milling medium of wet ball grinding is absolute ethyl alcohol in the step (1) and the step (2), and ballstone is zirconium dioxide
Ballstone.
The Ball-milling Time of wet ball grinding is 4-6h hours in the step (1) and the step (2).
The drying temperature dried described in the step (1) and the step (2) is 40-60 DEG C.
Molding technique refers to isostatic cool pressing technique in the step (2).
The temperature of pre-burning is 1100-1200 DEG C in the step (2), time 2-3h.
Specific embodiment is as follows.
(Eu0.5Nb0.5)0.01Ti0.99O2Preparation method such as example 1..
Xwt%Bi2O3(100-x) wt% (Eu0.5Nb0.5)0.01Ti0.99O2Preparation such as example 2-8.
Example 1
With Eu2O3、Nb2O5And TiO2For raw material, according to chemical formula (Eu0.5Nb0.5)0.01Ti0.99O2Carry out dispensing, wet method ball
4h is ground, after 50 DEG C of drying, through 1200 DEG C of pre-burning 2h, (Eu is made after grinding0.5Nb0.5)0.01Ti0.99O2Ceramic powder, then through at
Type obtains (Eu at 1400 DEG C after heat preservation 2h sintering0.5Nb0.5)0.01Ti0.99O2Ceramics are tested by silver.
Example 2
(the Eu of this example0.5Nb0.5)0.01Ti0.99O2The preparation of ceramic powder is identical as example 1.According to chemical formula
0.5wt%Bi2O3- 99.5wt% (Eu0.5Nb0.5)0.01Ti0.99O2Dispensing is carried out, then using alcohol as Media Usage planetary ball mill
Machine carries out wet ball grinding 4h, is dried for 40 DEG C after ball milling, through 1200 DEG C of pre-burning 2.5h, after grinding, and cold isostatic compaction, at 1400 DEG C
Lower sintering 2h obtains 0.5wt%Bi2O3- 99.5wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramics.
Example 3
(1) (the Eu of this example0.5Nb0.5)0.01Ti0.99O2The preparation of ceramic powder is identical as example 1.According to chemical formula
1wt%Bi2O3- 99wt% (Eu0.5Nb0.5)0.01Ti0.99O2Carry out dispensing, then using alcohol as Media Usage planetary ball mill into
Row wet ball grinding 4h, 40 DEG C of drying after ball milling, through 1100 DEG C of pre-burning 3h, after grinding, cold isostatic compaction is sintered at 1400 DEG C
2h obtains 1wt%Bi2O3- 99wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramics.
Example 4
(the Eu of this example0.5Nb0.5)0.01Ti0.99O2The preparation of ceramic powder is identical as example 1.According to chemical formula 2wt%
Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Dispensing is carried out, then carries out wet method by Media Usage planetary ball mill of alcohol
Ball milling 4h, 40 DEG C of drying after ball milling, through 1200 DEG C of pre-burning 3h, after grinding, cold isostatic compaction, at 1400 DEG C being sintered 2h obtains
2wt%Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramics.
Example 5
(the Eu of this example0.5Nb0.5)0.01Ti0.99O2The preparation of ceramic powder is identical as example 1.According to chemical formula 2wt%
Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Dispensing is carried out, then carries out wet method by Media Usage planetary ball mill of alcohol
Ball milling 5h, 50 DEG C of drying after ball milling, through 1200 DEG C of pre-burning 2h, after grinding, cold isostatic compaction, at 1350 DEG C being sintered 6h obtains
2wt%Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramics.
Example 6
(the Eu of this example0.5Nb0.5)0.01Ti0.99O2The preparation of ceramic powder is identical as example 1.According to chemical formula 2wt%
Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Dispensing is carried out, then carries out wet method by Media Usage planetary ball mill of alcohol
Ball milling 4h, 60 DEG C of drying after ball milling, through 1150 DEG C of pre-burning 3h, after grinding, cold isostatic compaction, at 1450 DEG C being sintered 4h obtains
2wt%Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramics.
Example 7
(the Eu of this example0.5Nb0.5)0.01Ti0.99O2The preparation of ceramic powder is identical as example 1.According to chemical formula 2wt%
Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Dispensing is carried out, then carries out wet method by Media Usage planetary ball mill of alcohol
Ball milling 4h, 55 DEG C of drying after ball milling, through 1200 DEG C of pre-burning 3h, after grinding, cold isostatic compaction, at 1500 DEG C being sintered 2h obtains
2wt%Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramics.
Example 8
(the Eu of this example0.5Nb0.5)0.01Ti0.99O2The preparation of ceramic powder is identical as example 1.According to chemical formula 3wt%
Bi2O3- 97wt% (Eu0.5Nb0.5)0.01Ti0.99O2Dispensing is carried out, then carries out wet method by Media Usage planetary ball mill of alcohol
Ball milling 6h, 40 DEG C of drying after ball milling, through 1200 DEG C of pre-burning 2h, after grinding, cold isostatic compaction, at 1400 DEG C being sintered 2h obtains
3wt%Bi2O3- 97wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramics.
It is tested by the sample obtained to each example, it is found that the properties of sample that example 4 obtains is best.Fig. 1 is this
Invention example 4 prepares 2wt%Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramic dielectric constant with frequency variation curve figure,
From the figure, it can be seen that it is about 2.7 × 10 that obtained sample, which has good frequency stability, dielectric constant,4Left and right.Fig. 2 is this
(Eu prepared by invention example 10.5Nb0.5)0.01Ti0.99O22wt%Bi prepared by ceramics and example 42O3- 98wt%
(Eu0.5Nb0.5)0.01Ti0.99O2Ceramic dielectric is lost with frequency variation curve figure, from the figure, it can be seen that (Eu0.5Nb0.5)0.01Ti0.99O2The loss of ceramics is 0.1 or so, as shown in Fig. 2, being unsatisfactory for the requirement of practical application；And 2wt%Bi2O3-
98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramics, when frequency is 104When, dielectric loss 0.015, this is better than being previously reported
CCTO giant dielectric materials.Fig. 3 is that present example 4 prepares 2wt%Bi2O3- 98wt% (Eu0.5Nb0.5)0.01Ti0.99O2Ceramics are situated between
Electric constant varies with temperature curve graph, and as seen from the figure, in -150-200 DEG C of temperature ranges, what dielectric constant become almost without
Change, the sample that illustrated example 4 obtains has good temperature stability.Fig. 4 is that present example 4 prepares 2wt%Bi2O3- 98wt%
(Eu0.5Nb0.5)0.01Ti0.99O2The SEM figures of ceramics.As seen from the figure, the sample consistency that example 4 obtains is high, and crystal particle crystal boundary is clear.
Ceramic capacitor dielectric material provided by the invention has ultralow dielectric loss, high-k, good frequency
With temperature stability, highly practical, it is suitble to industrialized production, the ceramic dielectric material dielectric constant of preparation to be more than 25000, dielectric
Loss is less than 0.02, has good frequency and temperature stability.
Above said content is that a further detailed description of the present invention in conjunction with specific preferred embodiments, is not
Whole or unique embodiment, those of ordinary skill in the art are by reading description of the invention to technical solution of the present invention
Any equivalent transformation taken is that claim of the invention is covered.
Claims (9)
1. a kind of ultralow dielectric loss high-dielectric-constant ceramics dielectric material, which is characterized in that its stoichiometric equation is xwt%
Bi2O3(100-x) wt% (Eu0.5Nb0.5)0.01Ti0.99O2, wherein 0<x≤3.
2. ultralow dielectric loss high-dielectric-constant ceramics dielectric material according to claim 1, which is characterized in that work as frequency
103-104When Hz, dielectric constant is more than 25000, and dielectric loss is between 0.015-0.017.
3. according to the preparation side of the ultralow dielectric loss high-dielectric-constant ceramics dielectric material of claim 1-2 any one of them
Method, which is characterized in that by Bi2O3Powder and (Eu0.5Nb0.5)0.01Ti0.99O2Ceramic powder mixed ingredients, after ball milling, drying,
After pre-burning and molding, heat preservation 2-6h sinters porcelain at 1350-1500 DEG C, obtains the pottery of ultralow dielectric loss high-k
Porcelain dielectric material.
4. the preparation method of ultralow dielectric loss high-dielectric-constant ceramics dielectric material according to claim 3, feature
It is, (Eu0.5Nb0.5)0.01Ti0.99O2Ceramic powder is made by the following method：According to chemical formula (Eu0.5Nb0.5)0.01Ti0.99O2, europium oxide, niobium oxide and titanium dioxide are kept the temperature at 1200 DEG C to 2h after ball milling and drying, are made
(Eu0.5Nb0.5)0.01Ti0.99O2Ceramic powder.
5. the preparation method of ultralow dielectric loss high-dielectric-constant ceramics dielectric material according to claim 3, feature
It is, the temperature of pre-burning is 1100-1200 DEG C, time 2-3h.
6. the preparation method of ultralow dielectric loss high-dielectric-constant ceramics dielectric material according to claim 3, feature
It is, ball milling is wet ball grinding, and ball-milling medium is absolute ethyl alcohol, and ballstone is zirconium dioxide ballstone.
7. the preparation method of ultralow dielectric loss high-dielectric-constant ceramics dielectric material according to claim 3, feature
It is, the Ball-milling Time of ball milling is 4-6h.
8. the preparation method of ultralow dielectric loss high-dielectric-constant ceramics dielectric material according to claim 3, feature
It is, the drying temperature of drying is 40-60 DEG C.
9. the preparation method of ultralow dielectric loss high-dielectric-constant ceramics dielectric material according to claim 3, feature
It is, molding technique refers to isostatic cool pressing technique.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205085A (en) * | 2020-02-03 | 2020-05-29 | 河南理工大学 | Preparation method of titanium dioxide-based ceramic with ultrahigh dielectric constant and low dielectric loss |
| CN113831121A (en) * | 2021-09-25 | 2021-12-24 | 天津理工大学 | Complex phase giant dielectric ceramic material with high breakdown field strength and preparation method thereof |
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| CN113831121A (en) * | 2021-09-25 | 2021-12-24 | 天津理工大学 | Complex phase giant dielectric ceramic material with high breakdown field strength and preparation method thereof |
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