CN108147810A - A kind of preparation method of middle low temperature MLCC capacitance ceramics - Google Patents

A kind of preparation method of middle low temperature MLCC capacitance ceramics Download PDF

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CN108147810A
CN108147810A CN201711361153.9A CN201711361153A CN108147810A CN 108147810 A CN108147810 A CN 108147810A CN 201711361153 A CN201711361153 A CN 201711361153A CN 108147810 A CN108147810 A CN 108147810A
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ceramics
glass
preparation
low temperature
ball
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仪凯
张庆猛
唐群
杨志民
杨剑
毛昌辉
杜军
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Beijing General Research Institute for Non Ferrous Metals
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

The invention belongs to technical field of ceramic material, and in particular to a kind of preparation method of middle low temperature MLCC capacitance ceramics.The preparation method processing step:Glass ceramics raw material is uniformly mixed, high-temperature fusion, stirring form uniform glass precursor solution;Melten glass liquid is quickly poured into deionized water, obtains glass disintegrating slag;After glass disintegrating slag ball milling, drying, powder is made;By powder sintering, MLCC capacitance ceramics are made.MLCC capacitance ceramics preparation method of the present invention, short preparation period is simple for process, and sintering temperature is low, and obtained powder constituents are uniform.

Description

A kind of preparation method of middle low temperature MLCC capacitance ceramics
Technical field
The invention belongs to technical field of ceramic material, and in particular to a kind of preparation method of middle low temperature MLCC capacitance ceramics.
Background technology
Electronic component is the foundation stone of electronics and information industry, with the high speed development of electronic information technology, electronic component Industry is also grown rapidly therewith, and multilayer ceramic capacitor (Multilayer Ceramic Capacitor, abbreviation MLCC) is should With widest a kind of electronic component.Multilayer ceramic capacitor is alternately stacked simultaneously by ceramic dielectric and metal inner electrode Cofiring forms, and two adjacent interior electrodes form a capacity plate antenna, and a MLCC is equivalent to several such tablet electricity Container is in parallel.By casting technique prepare MLCC production procedure include slurry preparation, curtain coating, silk-screen printing, lamination, cutting, Dumping, sintering, chamfering, burning end and test and etc..
Since the 1990s, the global MLCC market demands constantly increase, since MLCC is compared to other capacitance utensils Have the advantages that small, price is low, equivalent series resistance is small, high frequency characteristics is good, have become at present most main in capacitor market The product of stream, while MLCC also becomes clear day by day to the substitution effect of other kinds of capacitor.
Following MLCC constantly develops to micromation, high capacity, high reliability and inexpensive direction.Miniaturization, large capacity Growth requirement cause the medium number of plies while being continuously increased, the thickness of dielectric layer is also constantly being thinned.At present in the world most Thin MLCC dielectric layers have reached 1um or so.In addition, MLCC capacitances also develop towards inexpensive direction, more inexpensive is low-priced Metal electrode is rapidly developed, and this requires sintering temperatures when reducing preparation media ceramics to match cheap metal electrode, Realize low temperature sintering.
The development of MLCC technically proposes ceramic powder the requirement of high pure and ultra-fine, while to meet relatively low sintering Temperature.The preparation method of barium carbonate powder mainly has solid-phase synthesis, liquid phase synthesizing method etc. at present.Most common master in solid phase method If high-temperature calcination synthetic method, synthesis calcination temperature is high, can generate that grain size is big and distribution is wide, serious powder of reuniting; And there are the shortcomings of chemical composition is uneven, impurity content is high due to the uneven powder that can cause of ball milling mixing; In addition longer Ball-milling Time and higher calcination temperature, time consumption and energy consumption are also very serious.Liquid phase method is most common mainly to be included Three kinds of sol-gel method, hydro-thermal method and the precipitation method.Hydro-thermal method is by the Ba (OH) containing titanium source2Aqueous solution carries out hydro-thermal process, To be formed, crystallinity is high, purity is high and the powder of even size distribution, the powder that this method obtains are handled without high-temperature calcination, kept away Exempted from crystal grain grow up, the formation of defect and the introducing of impurity, there is higher sintering activity;The precipitation method be usually adjust it is organic before The pH value of liquid solution is driven, is precipitated under alkaline environment, carrying out Low Temperature Heat Treatment to precipitation obtains required powder;Colloidal sol-solidifying Glue rule is to hydrolyze to form colloidal sol by using the organic alkoxide of titanium, further forms barium titanate aqueous precursor gel after heating, so Dried dry gel powder be can obtain into barium carbonate powder in certain temperature calcination processing afterwards.Although obtained powder has Topographic profile is uniform, reactivity is high and the advantages that narrow particle size distribution, but the requirement of its technology is higher, and synthesis condition is more severe It carves.
Invention content
The purpose of the invention is to meet the needs of MLCC micromations, high capacity, high reliability and low cost, so as to A kind of preparation method of the middle low temperature MLCC capacitance ceramics proposed, specific implementation step:
(1) ceramic raw material prepared is put into overturning batch mixer, mixes 2~7h, be sufficiently mixed it;
(2) by uniformly mixed raw material high-temperature fusion into glass metal, and a molten liquid is stirred at interval of half an hour;
(3) it is poured into what high-temperature fusion liquid uniformly dispersed in 25 DEG C of deionized water, obtains glass disintegrating slag;
(4) glass disintegrating slag is dried;
(5) glass disintegrating slag, ethyl alcohol are put into togerther ball milling in ball grinder;
(6) ball grinder in 70 DEG C of baking oven is dried into 12~18h, then abrasive material is crossed to the sieve of 200 mesh, required powder is made Body;
(7) by powder sintering, ceramics print is made.
In step (2), the melting temperature of raw material is 1300~1450 DEG C, and soaking time is 2~5h.
In step (4), drying temperature is 110~120 DEG C, and the time is 12~16h.
In step (5), ball milling speed is 50~200r/min, Ball-milling Time for 8~for 24 hours.
In step (5), ball milling method uses planetary ball mill or high-energy ball milling, and glass powder granularity is 1~5 μ after ball milling m。
In step (5), the mass ratio of ball, glass disintegrating slag and ethyl alcohol is ball during ball milling:Glass dregs:Ethyl alcohol=0.95:0.3: 0.2。
In step (7), it is niobates phase or titanate phase that ceramic phase, which is precipitated, in the ceramics sample of sintering, and remaining glass is mutually two Silica glass phase or boric oxide glass phase.
Beneficial effects of the present invention:Ceramic powder is prepared, short preparation period is simple for process, and sintering temperature is low, obtains powder Ingredient is uniform.
Description of the drawings
Fig. 1:The stereoscan photograph of 1 gained powder of embodiment.
Fig. 2:The stereoscan photograph of 2 gained powder of embodiment.
Fig. 3:The Capacitance Shift Rate of 1100 DEG C of sintering potsherds in embodiment 1.
Fig. 4:The Capacitance Shift Rate of 1100 DEG C of sintering potsherds in embodiment 2.
Specific embodiment
The present invention proposes a kind of preparation method of middle low temperature MLCC capacitance ceramics, with reference to specific embodiment with it is attached Figure is described further it.
Embodiment 1
1) dispensing, raw material is uniformly mixed
To analyze pure BaCO3、SiO2、Nb2O5、PbO、TiO2、SrCO3It is 0.2 according to molar ratio for raw material:1:1.2: 0.6:0.5:1 carries out dispensing, using overturning batch mixer mixing 3h.
2) by raw material high-temperature fusion, water quenching into glass dregs
Uniformly mixed raw material is kept the temperature into 3h at a high temperature of 1450 DEG C, is stirred at interval of half an hour once, by molten liquid Homodisperse pouring into carries out water quenching in deionized water, glass disintegrating slag is made.
3) by glass dregs ball milling, drying
In 110 DEG C of baking oven, glass disintegrating slag, time 8h are dried;Glass disintegrating slag is crushed by ball-milling technology.Ball milling The rotating speed of machine is 200r/min, Ball-milling Time 8h, during ball milling the quality of ball, glass disintegrating slag and ethyl alcohol be respectively 950g, 300g, 200g.Then slurry after ball milling is dried into 12h in 70 DEG C of baking oven, with the sieve of 200 mesh, required powder is made.Pass through Scanning electron microscope (Hitachi S4800, amplification factor are 1K times), observes powder microscopic appearance, as shown in Figure 1, sample crystal grain ruler It is very little to be distributed in 1~5um.
4) powder is sintered, prepares sample
The powder prepared is pressed into diameter by granulation, uniaxial compression, isostatic cool pressing (pressing pressure 200MPa) For 20mm, thickness is the sample of 2mm, in air atmosphere, selects 1050 DEG C, 1075 DEG C, 1100 DEG C, 1125 DEG C of sintering 1h, In sintering process, the densification of sample and precipitation ceramic phase are successively completed, and ceramics sample is made.
The ceramic disks upper and lower surface of firing is silver-colored, silver electrode is fired, tests its dielectric properties, as shown in table 1.
The dielectric properties of the made ceramic disks of the different sintering temperatures of table 1
Its capacitance-temperature curve is tested to the ceramic disks of 1100 DEG C of sintering, as shown in figure 3, in -40 DEG C~80 DEG C temperature In the range of degree, △ C/C≤17%.
Embodiment 2
1) dispensing, raw material is uniformly mixed
With the commercially available pure SiO of analysis2、Nb2O5、PbSi、NaCO3、SrCO3、Gd2O3It is 1 according to molar ratio for raw material: 0.9:0.25:0.5:0.3:0.06 carries out dispensing, using overturning batch mixer mixing 3h.
2) by raw material high-temperature fusion, water quenching into glass dregs
Uniformly mixed raw material is kept the temperature into 3h at a high temperature of 1420 DEG C, is stirred at interval of half an hour once, by molten liquid Homodisperse pouring into carries out water quenching in deionized water, glass disintegrating slag is made.
3) by glass dregs ball milling, drying
In 110 DEG C of baking oven, glass disintegrating slag, time 8h are dried;Glass disintegrating slag is crushed by ball-milling technology.Ball milling The rotating speed of machine is 200r/min, Ball-milling Time 8h, during ball milling the quality of ball, glass disintegrating slag and ethyl alcohol be respectively 950g, 300g, 200g.Then slurry after ball milling is dried into 12h in 70 DEG C of baking oven, with the sieve of 200 mesh, required powder is made.Pass through Scanning electron microscope (HitachiS4800, amplification factor are 1K times), observes powder microscopic appearance, as shown in Fig. 2, sample crystallite dimension It is distributed in 1~5um.
4) powder is sintered, prepares sample
The powder prepared is pressed into diameter by granulation, uniaxial compression, isostatic cool pressing (pressing pressure 200MPa) For 20mm, thickness is the sample of 2mm, in air atmosphere, selects 1050 DEG C, 1075 DEG C, 1100 DEG C, 1125 DEG C of sintering 1h, is made Ceramics sample.
The ceramic disks upper and lower surface of firing is silver-colored, silver electrode is fired, tests its dielectric properties, as shown in table 2.
The dielectric properties of the made ceramic disks of the different sintering temperatures of table 2
Its capacitance-temperature curve is tested to the ceramic disks of 1100 DEG C of sintering, as shown in figure 4, in -40 DEG C~80 DEG C temperature In the range of degree, △ C/C≤5%.

Claims (7)

  1. A kind of 1. preparation method of middle low temperature MLCC capacitance ceramics, which is characterized in that specific steps:
    (1) ceramic raw material prepared is put into overturning batch mixer, mixes 2~7h, be sufficiently mixed it;
    (2) by uniformly mixed raw material high-temperature fusion into glass metal, and a molten liquid is stirred at interval of half an hour;
    (3) it is poured into what high-temperature fusion liquid uniformly dispersed in 25 DEG C of deionized water, obtains glass disintegrating slag;
    (4) glass disintegrating slag is dried;
    (5) glass disintegrating slag, ethyl alcohol are put into togerther ball milling in ball grinder;
    (6) ball grinder in 70 DEG C of baking oven is dried into 12~18h, then abrasive material is crossed to the sieve of 200 mesh, required powder is made;
    (7) by powder sintering, ceramics print is made.
  2. 2. a kind of preparation method of middle low temperature MLCC capacitance ceramics as described in claim 1, which is characterized in that in step (2), The melting temperature of raw material is 1300~1450 DEG C, and soaking time is 2~5h.
  3. 3. a kind of preparation method of middle low temperature MLCC capacitance ceramics as described in claim 1, which is characterized in that in step (4), Drying temperature is 110~120 DEG C, and the time is 12~16h.
  4. 4. a kind of preparation method of middle low temperature MLCC capacitance ceramics as described in claim 1, which is characterized in that in step (5), Ball milling speed is 50~200r/min, Ball-milling Time for 8~for 24 hours.
  5. 5. a kind of preparation method of middle low temperature MLCC capacitance ceramics as described in claim 1, which is characterized in that in step (5), Ball milling method uses planetary ball mill or high-energy ball milling, and glass powder granularity is 1~5 μm after ball milling.
  6. 6. a kind of preparation method of middle low temperature MLCC capacitance ceramics as described in claim 1, which is characterized in that in step (5), The mass ratio of ball, glass disintegrating slag and ethyl alcohol is ball during ball milling:Glass dregs:Ethyl alcohol=0.95:0.3:0.2.
  7. 7. a kind of preparation method of middle low temperature MLCC capacitance ceramics as described in claim 1, which is characterized in that in step (7), It is niobates phase or titanate phase that ceramic phase, which is precipitated, in the ceramics sample of sintering, and remaining glass is mutually silica glass phase or oxidation Boron glass phase.
CN201711361153.9A 2017-12-18 2017-12-18 A kind of preparation method of middle low temperature MLCC capacitance ceramics Pending CN108147810A (en)

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