CN110105067A - A kind of high dielectric X7R ceramic medium material and preparation method thereof - Google Patents
A kind of high dielectric X7R ceramic medium material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to ceramic medium material field, specifically a kind of high dielectric X7R ceramic medium material and preparation method thereof.It is the Nd for being 5-25% by mass percent2O3With the Ca of 75-95%0.95La0.05Cu2.55Zn0.5Ti4O12Composition.High dielectric X7R ceramic medium material provided by the present invention, Ca0.95La0.05Cu2.55Zn0.5Ti4O12It is that have moderate sintering temperature generally in 1130 DEG C or so, dielectric constant with higher, adjustable temperature coefficient of capacity and lower loss be a kind of medium ceramic material haveing excellent performance to media ceramic.The present invention selects Ca0.95La0.05Cu2.55Zn0.5Ti4O12System takes addition Nd2O3For the method for doping vario-property, while so that it is met performance X7R standard, have that dielectric constant is high, dielectric loss is low, leadless environment-friendly advantage.
Description
Technical field
The present invention relates to ceramic medium material field, specifically a kind of high dielectric X7R ceramic medium material and its preparation side
Method.
Background technique
Multiple stratification, chip type, the integrated and multifunction of informational function ceramic components become the mainstream of development.Electronics
Integrated, micromation and the Intelligent Developing Trends of information technology, push electronic component to generate in assembling and operational mode
New variation, that is, insert to surface-assembled, it is simulated to digitlization, it is fixed to mobile, separate type to integrated transformation.
Sheet capacitor, chip inductor and plate resistor are three big passive elements being most widely used, and have developed into the production of scale
Industry group.The different electronic element of other function for example chip driver, chip transformation group, piece type antenna, sheet type sensor and
The development such as chip energy converter are also very rapid.
Capacitor is a kind of important passive electronic, is device indispensable in electronics, communication and information industry
Part can play storage charge, partition direct current, ac filter, provide tuning and concussion etc..According to material is constituted, pottery can be divided into
Porcelain capacitor, alminium electrolytic condenser, tantalum capacitor, plastic film capacitor etc..Chip multilayer ceramic capacitor (MLCC) belongs to ceramic condenser class,
With small in size, capacitance is big, cheap, stability is high and the characteristics such as suitable mass production, pursued in electronics and IT products
Under the promotion of miniaturization, the development trend of lightness and surface mounting technology, development prospect is very wide.
Currently, X7R type MLCC device has been widely applied on various electric terminal equipments, the device -55 DEG C~
There is high dielectric constant and good temperature stability in 125 DEG C of temperature ranges.With advances in technology, tantalum electricity is gradually replaced
The trend of electrolysis condenser.The relatively common dielectric ceramic system with X7R characteristic has tungsten-bronzes structure ceramic system, lead base
Relaxation ferroelectric ceramic system and BaTiO3Base ferroelectric ceramics system.Although the X7R ceramic medium material reported at present is many kinds of,
But these ceramic materials are there are sintering temperature height, dielectric constant is low and the problems such as higher is lost.
Summary of the invention
The present invention is intended to provide a kind of high dielectric X7R ceramic medium material and preparation method thereof, and the dielectric material is normal
Number is high, dielectric loss is low, leadless environment-friendly, and the sintering temperature of its method is low.
The present invention is achieved by the following technical solutions: a kind of high dielectric X7R ceramic medium material, is by quality percentage
Than the Nd for 5-25%2O3With the Ca of 75-95%0.95La0.05Cu2.55Zn0.5Ti4O12Composition.
Invention further provides a kind of preparation methods of high dielectric X7R ceramic medium material, comprising the following steps:
(1) by raw materials of Ca CO3、La2O3、CuO、ZnO、TiO2With press general formula Ca0.95La0.05Cu2.55Zn0.5Ti4O12, carry out
Ingredient ball milling is warming up to 1000 DEG C, keeps the temperature 2-4 hours, and frit A is made；
(2) according to mass percent by the Nd of 5-25%2O3Second batch is carried out with the frit A of 75-95%, obtains ingredient
B；
(3) by ingredient B ball milling, the binder for being incorporated as the 5-8wt% of ingredient B is granulated, is pressed into green compact, is warming up to 400-
500 DEG C are warming up to 1120 DEG C -1150 DEG C again and keep the temperature 1 hour, and high dielectric X7R ceramic medium material is made after cooling.
As the further improvement of preparation method technical solution of the present invention, in the step (1), it is warming up to 1000 DEG C of liter
Warm rate is 9-12 DEG C/min.
As the further improvement of preparation method technical solution of the present invention, in the step (1), it is warming up to 1000 DEG C of liter
Warm rate is 10 DEG C/min.
It is the liter by 2 DEG C/min in the step (3) as the further improvement of preparation method technical solution of the present invention
Warm rate is heated to 400-500 DEG C, then is heated to 1120 DEG C -1150 DEG C by the heating rate of 10 DEG C/min.
As the further improvement of preparation method technical solution of the present invention, the binder is polyvinyl alcohol or paraffin.
Material as the further improvement of preparation method technical solution of the present invention, after the ball milling of the step (1) and (3)
Needed the hole 120-250/cm2Sub-sieve.
High dielectric X7R ceramic medium material provided by the present invention, Ca0.95La0.05Cu2.55Zn0.5Ti4O12It is media ceramic
With moderate sintering temperature, generally 1130 DEG C or so, dielectric constant with higher, adjustable temperature coefficient of capacity and compared with
Low loss is a kind of medium ceramic material haveing excellent performance.The present invention selects Ca0.95La0.05Cu2.55Zn0.5Ti4O12System,
Take addition Nd2O3For the method for doping vario-property, its crystal grain can be made to reduce, to meet performance with the lattice energy of activation system
While X7R standard, with dielectric constant is high, dielectric loss is low, leadless environment-friendly advantage.The preparation method through the invention
The ceramic medium material of acquisition, dielectric constant is between 4550-4700, and dielectric loss is between 0.01-0.02.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the temperature coefficient for the ceramic medium material that embodiment 1, embodiment 2, embodiment 3 and embodiment 4 prepare
The test result figure of TCC.As seen from the figure: as temperature increases, temperature coefficient is all presented slow ascendant trend, but temperature
Coefficient has reached X7R standard, temperature stability with higher all in ± 15%.
Fig. 2 is the SEM figure for the ceramic medium material that the present invention prepares.As seen from the figure: grain growth is better
Good, morphological rules is uniform in size, and average grain diameter is 1.8 μm, and consistency is high.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
A kind of high dielectric X7R ceramic medium material is the Nd for being 5-25% by mass percent2O3With 75-95%'s
Ca0.95La0.05Cu2.55Zn0.5Ti4O12Composition.
A kind of preparation method of high dielectric X7R ceramic medium material, comprising the following steps:
(1) by raw materials of Ca CO3、La2O3、CuO、ZnO、TiO2With press general formula Ca0.95La0.05Cu2.55Zn0.5Ti4O12, carry out
Ingredient ball milling is warming up to 1000 DEG C, keeps the temperature 2-4 hours, and frit A is made；
(2) according to mass percent by the Nd of 5-25%2O3Second batch is carried out with the frit A of 75-95%, obtains ingredient
B；
(3) by ingredient B ball milling, the binder for being incorporated as the 5-8wt% of ingredient B is granulated, is pressed into green compact, is warming up to 400-
500 DEG C are warming up to 1120 DEG C -1150 DEG C again and keep the temperature 1 hour, and high dielectric X7R ceramic medium material is made after cooling.
In the present invention, the binder that step (3) is added can vapor away in subsequent temperature-rise period, and of the invention
The sintering process of step (3) is primarily to make ceramic medium material achieve the purpose that densification.
In the present invention, it is preferred to, in the step (1), the heating rate for being warming up to 1000 DEG C is 9-12 DEG C/min.
In the present invention, it is preferred to, in the step (1), the heating rate for being warming up to 1000 DEG C is 10 DEG C/min.
In the present invention, it is preferred to, it is to be heated to 400-500 DEG C by the heating rate of 2 DEG C/min in the step (3),
1120 DEG C -1150 DEG C are heated to by the heating rate of 10 DEG C/min again.
In the present invention, it is preferred to, the binder is polyvinyl alcohol or paraffin.
In the present invention, it is preferred to, the material after the ball milling of the step (1) and (3) needed the hole 120-250/cm2Divide sample
Sieve.When it is implemented, the medium of the ball milling is the zirconia ball of diameter 1mm.
Test method and detection device used in the present invention are as follows:
1, the test of permittivity ε and loss tan δ
Using HEWLETT PACKARD 4278A capacitance measuring tester, capacitance C and dielectric loss the tan δ of test capacitors
(test frequency 1KHz), and permittivity ε is calculated by following formula:
Wherein: the capacitance of C- print, unit pF；The thickness of d- print, unit cm；The sintered diameter of D- print, it is single
Position cm.
2, the test (- 55 DEG C~125 DEG C) of temperature coefficient TCC
Utilize 6425 type WAYKERR electric bridges, GZ-ESPEC MC-710F high-low temperature chamber and HM27002 type capacitor C-T/V
Characteristic dedicated tester measures the capacitance variation with temperature situation of sample, so as to find out the capacitance temperature factor of capacitor
(test frequency 1KHz), calculation formula are as follows:
Wherein: fiducial temperature chooses 25 DEG C, C0For 25 DEG C of capacity of temperature, C1For temperature t1Capacity.
Technical solution of the present invention is described in detail with reference to the accompanying drawing.
Embodiment 1
By raw materials of Ca CO3、La2O3、CuO、ZnO、TiO2With press general formula Ca0.95La0.05Cu2.55Zn0.5Ti4O12, matched
Material, in 100 DEG C of dryings in a conventional oven of 3.3kw, crosses 250 ball milling 6 hours on the ball mill that revolving speed is 400r/min
Hole/cm2Sub-sieve is warming up to 1000 DEG C with 9 DEG C/min, and keeps the temperature 3 hours at 1000 DEG C, obtains frit A.
Second batch is carried out, according to 95% frit A and 5%Nd2O3Relationship between quality uniformly mix, add deionized water turn
Speed is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill2Sub-sieve is added 8wt% paraffin and makes
Grain, is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then be heated to by the heating rate of 10 DEG C/min
1120 DEG C of firings, keep the temperature 1 hour, and ceramic medium material is made after cooling.
See Table 1 for details and figure for the test result (test frequency 1KHz) of the dielectric properties of above-described embodiment ceramic medium material
1。
Table 1
| Project | Firing temperature (DEG C) | Soaking time (h) | Permittivity ε | Tan δ is lost |
| Embodiment 1 | 1120 | 1 | 4600 | 0.016 |
Embodiment 2
By raw materials of Ca CO3、La2O3、CuO、ZnO、TiO2With press general formula Ca0.95La0.05Cu2.55Zn0.5Ti4O12, matched
Material, in 100 DEG C of dryings in a conventional oven of 3.3kw, crosses 250 ball milling 6 hours on the ball mill that revolving speed is 400r/min
Hole/cm2Sub-sieve is warming up to 1000 DEG C with 10 DEG C/min, and keeps the temperature 3 hours at 1000 DEG C, obtains frit A.
Second batch is carried out, according to 90% frit A and 10%Nd2O3Relationship between quality uniformly mix, add deionized water turn
Speed is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill2Sub-sieve is added 8wt% paraffin and makes
Grain, is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then be heated to by the heating rate of 10 DEG C/min
1130 DEG C of firings, keep the temperature 1 hour, and ceramic medium material is made after cooling.
See Table 2 for details and Fig. 1 for the test result (test frequency 1KHz) of above-described embodiment dielectric properties.
Table 2
| Project | Firing temperature (DEG C) | Soaking time (h) | Permittivity ε | Tan δ is lost |
| Embodiment 2 | 1130 | 1 | 4670 | 0.013 |
Embodiment 3
By raw materials of Ca CO3、La2O3、CuO、ZnO、TiO2With press general formula Ca0.95La0.05Cu2.55Zn0.5Ti4O12, matched
Material, in 100 DEG C of dryings in a conventional oven of 3.3kw, crosses 250 ball milling 6 hours on the ball mill that revolving speed is 400r/min
Hole/cm2Sub-sieve is warming up to 1000 DEG C with 10 DEG C/mm, and keeps the temperature 3 hours at 1000 DEG C, obtains frit A.
Second batch is carried out, according to 85% frit A and 15%Nd2O3Relationship between quality uniformly mix, add deionized water turn
Speed is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill2Sub-sieve is added 8wt% paraffin and makes
Grain, is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then be heated to by the heating rate of 10 DEG C/min
1140 DEG C of firings, keep the temperature 1 hour, and ceramic medium material is made after cooling.
See Table 3 for details and Fig. 1 for the test result (test frequency 1KHz) of above-described embodiment dielectric properties.
Table 3
| Project | Firing temperature (DEG C) | Soaking time (h) | Permittivity ε | Tan δ is lost |
| Embodiment 3 | 1140 | 1 | 4700 | 0.0191 |
Embodiment 4
By raw materials of Ca CO3、La2O3、CuO、ZnO、TiO2With press general formula Ca0.95La0.05Cu2.55Zn0.5Ti4O12, matched
Material, in 100 DEG C of dryings in a conventional oven of 3.3kw, crosses 250 ball milling 6 hours on the ball mill that revolving speed is 400r/min
Hole/cm2Sub-sieve is warming up to 1000 DEG C with 12 DEG C/min, and keeps the temperature 3 hours at 1000 DEG C, obtains frit A.
Second batch is carried out, according to 75% frit A and 25%Nd2O3Relationship between quality uniformly mix, add deionized water turn
Speed is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill2Sub-sieve is added 8wt% paraffin and makes
Grain, is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then be heated to by the heating rate of 10 DEG C/min
1150 DEG C of firings, keep the temperature 1 hour, and ceramic medium material is made after cooling.
See Table 4 for details and Fig. 1 for the test result (test frequency 1KHz) of above-described embodiment dielectric properties.
Table 4
| Project | Firing temperature (DEG C) | Soaking time (h) | Permittivity ε | Tan δ is lost |
| Embodiment 4 | 1150 | 1 | 4650 | 0.0181 |
Embodiment 5
By raw materials of Ca CO3、La2O3、CuO、ZnO、TiO2With press general formula Ca0.95La0.05Cu2.55Zn0.5Ti4O12, matched
Material, in 100 DEG C of dryings in a conventional oven of 3.3kw, crosses 250 ball milling 6 hours on the ball mill that revolving speed is 400r/min
Hole/cm2Sub-sieve is warming up to 1000 DEG C with 9 DEG C/min, and keeps the temperature 2 hours at 1000 DEG C, obtains frit A.
Second batch is carried out, according to 80% frit A and 20%Nd2O3Relationship between quality uniformly mix, add deionized water turn
Speed is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill2Sub-sieve is added 8wt% paraffin and makes
Grain, is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then be heated to by the heating rate of 10 DEG C/min
1120 DEG C of firings, keep the temperature 1 hour, and ceramic medium material is made after cooling.
Embodiment 6
By raw materials of Ca CO3、La2O3、CuO、ZnO、TiO2With press general formula Ca0.95La0.05Cu2.55Zn0.5Ti4O12, matched
Material, in 100 DEG C of dryings in a conventional oven of 3.3kw, crosses 250 ball milling 6 hours on the ball mill that revolving speed is 400r/min
Hole/cm2Sub-sieve is warming up to 1000 DEG C with 11 DEG C/min, and keeps the temperature 4 hours at 1000 DEG C, obtains frit A.
Second batch is carried out, according to 80% frit A and 20%Nd2O3Relationship between quality uniformly mix, add deionized water turn
Speed is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill2Sub-sieve is added 8wt% paraffin and makes
Grain, is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then be heated to by the heating rate of 10 DEG C/min
1150 DEG C of firings, keep the temperature 1 hour, and ceramic medium material is made after cooling.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (7)
1. a kind of high dielectric X7R ceramic medium material, which is characterized in that be the Nd for being 5-25% by mass percent2O3And 75-
95% Ca0.95La0.05Cu2.55Zn0.5Ti4O12Composition.
2. a kind of preparation method of high dielectric X7R ceramic medium material described in claim 1, which is characterized in that including following
Step:
(1) by raw materials of Ca CO3、La2O3、CuO、ZnO、TiO2With press general formula Ca0.95La0.05Cu2.55Zn0.5Ti4O12, carry out with pellet
Mill is warming up to 1000 DEG C, keeps the temperature 2-4 hours, and frit A is made；
(2) according to mass percent by the Nd of 5-25%2O3Second batch is carried out with the frit A of 75-95%, obtains ingredient B；
(3) by ingredient B ball milling, the binder for being incorporated as the 5-8wt% of ingredient B is granulated, is pressed into green compact, is warming up to 400-500
It DEG C is warming up to 1120 DEG C -1150 DEG C again and keeps the temperature 1 hour, high dielectric X7R ceramic medium material is made after cooling.
3. a kind of preparation method of high dielectric X7R ceramic medium material according to claim 2, which is characterized in that described
In step (1), the heating rate for being warming up to 1000 DEG C is 9-12 DEG C/min.
4. a kind of preparation method of high dielectric X7R ceramic medium material according to claim 3, which is characterized in that described
In step (1), the heating rate for being warming up to 1000 DEG C is 10 DEG C/min.
5. a kind of preparation method of high dielectric X7R ceramic medium material according to claim 2, which is characterized in that described
It is 400-500 DEG C to be heated to by the heating rate of 2 DEG C/min, then be heated to by the heating rate of 10 DEG C/min in step (3)
1120℃-1150℃。
6. a kind of preparation method of high dielectric X7R ceramic medium material, feature according to Claims 2 or 3 or 4 or 5
It is, the binder is polyvinyl alcohol or paraffin.
7. a kind of preparation method of high dielectric X7R ceramic medium material according to claim 6, which is characterized in that described
Material after the ball milling of step (1) and (3) needed the hole 120-250/cm2Sub-sieve.
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| CN114507071A (en) * | 2022-03-05 | 2022-05-17 | 太原理工大学 | High-strength ceramic dielectric material and preparation method thereof |
Citations (6)
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