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 PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000011521 glass Substances 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 31
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 239000002893 slag Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000004927 fusion Effects 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000003082 abrasive agent Substances 0.000 claims description 2
- 238000000713 high-energy ball milling Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 239000002241 glass-ceramic Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000010791 quenching Methods 0.000 description 4
- 230000000171 quenching effect Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000003985 ceramic capacitor Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910011255 B2O3 Inorganic materials 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000007766 curtain coating Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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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
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)
- 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. 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. 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. 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. 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. 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. 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.
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