CN105869887B - A kind of X9R high-temperature stables multilayer ceramic capacitor porcelain slurry and its device preparation method - Google Patents
A kind of X9R high-temperature stables multilayer ceramic capacitor porcelain slurry and its device preparation method Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 57
- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 41
- 230000000087 stabilizing effect Effects 0.000 title claims abstract description 32
- 239000002002 slurry Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 16
- 239000004014 plasticizer Substances 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000003989 dielectric material Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000003475 lamination Methods 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 11
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 239000002019 doping agent Substances 0.000 claims description 7
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 7
- 239000007858 starting material Substances 0.000 claims description 7
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 5
- 238000009766 low-temperature sintering Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000007772 electrode material Substances 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical group CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 4
- 229910002113 barium titanate Inorganic materials 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 125000003944 tolyl group Chemical group 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 238000009472 formulation Methods 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 16
- 239000003990 capacitor Substances 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 7
- 238000007639 printing Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- 206010011376 Crepitations Diseases 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000007766 curtain coating Methods 0.000 description 1
- 125000002243 cyclohexanonyl group Chemical group *C1(*)C(=O)C(*)(*)C(*)(*)C(*)(*)C1(*)* 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
- C04B35/465—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
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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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
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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
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
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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
- C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
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Abstract
The present invention relates to a kind of X9R high-temperature stables multilayer ceramic capacitor porcelain slurry and its device preparation methods, its raw material composition includes X9R high-temperature stables medium material for multilayer ceramic capacitors and organic solvent, dispersant, binding agent, plasticizer, antifoaming agent, levelling agent, and the weight ratio of each component and X9R high-temperature stable medium material for multilayer ceramic capacitors is respectively：Organic solvent 46%~55%, dispersant 1.0%~2.0%, binding agent 3.0%~6.0%, plasticizer 3.0%~6.0%, antifoaming agent 0.2%~0.4%, levelling agent 0.1%~0.4%.It can obtain high stability in wide temperature range, function admirable, X9R high-temperature stable multilayer ceramic capacitor products simple for process using formula and preparation method thereof of the present invention, product upper limit temperature in use is up to+200 DEG C, meet temperature coefficient of capacitance≤± 15% in 55~+200 DEG C of temperature ranges, with high reliability, high temperature multilayer ceramic capacitor field can be efficiently applied to.
Description
Technical field
It is main to apply the present invention relates to a kind of X9R high-temperature stables multilayer ceramic capacitor porcelain slurry and its device preparation method
In electronic component field.
Background technology
Chip multilayer ceramic capacitor (MLCC) is the novel first device of one kind indispensable in electronics, communication and information industry
Part, has that small, capacitance is big, cheap, stability is high and the characteristics such as suitable mass production, therefore is largely used to lead to
In the surface mount of the consumer electronics complete machine such as news, computer, household electrical appliance.Global surface mounting technique is sent out rapidly in recent years
Exhibition, MLCC demands constantly rise, and properties of product requirement is also higher and higher.For example automotive ignition system and sensor-based system, oil field are surveyed
Reinforcement in terms of the electronic control of the intensification of depth sounding degree and the shock resistance system of aircraft etc., will because its working environment is harsh
Multilayer ceramic capacitor upper limit operating temperature is asked to be increased to 200 DEG C.Nowadays it is widely used general operating temperature range only
Be limited to -55 DEG C~+125 DEG C, -55 DEG C~+150 DEG C X7R-MLCC, X8R-MLCC can not meet the requirement of this respect, therefore
For the research of -55 DEG C~+200 DEG C of X9R-MLCC and prepared by the hot spot become in industry, and have to more wide temperature range
It hopes in the electronic system being used in high-temperature severe environment.
The MLCC prepared at present often uses base-metal inner-electrode slurry, but since nickel electrode is burnt under air conditions
Cheng Shi, it is oxidizable and cannot be conductive, therefore need to be burnt under reducing atmosphere, but when it is sintered in reducing atmosphere, sintering process is different
It is often cumbersome and also very high to equipment requirement, easily cause the reduction of oxide in porcelain body, so as to destroy the dielectric of porcelain body spy
Property.In addition, the ceramic dielectric system for preparing Ni-MLCC is needed with resistance to reduction, therefore the making difficulty of raw material and cost
Time is longer.To sum up, working efficiency is relatively low when prepared by Ni-MLCC, energy consumption is also higher.
The country is nowadays in the Preliminary study stage to the research and development of X9R multilayer ceramic capacitors, the design of MLCC and
Still there is very big gap in process manufacturing technology, and domestic manufacturer not yet forms the X9R multilayers pottery of seriation with foreign countries
The production catalogue of porcelain condenser.Therefore the technique technology of preparing of X9R-MLCC is for study with solving.Patent No.
The patent of invention of CN101908415A discloses a kind of X8R property slice type multilayer ceramic capacitors, -55 DEG C of temperature range~
Meet temperature coefficient of capacitance Δ C/C≤± 15% in+150 DEG C, but it cannot be applied under 200 DEG C of hot environment.
Invention content
The technical problems to be solved by the invention be for the above-mentioned prior art in deficiency, and provide a kind of X9R high temperature
Stablize multilayer ceramic capacitor porcelain slurry and its device preparation method, inner electrode uses Ag/Pd materials, dumping, sintering and burning
End process can carry out in air, and simple for process and working efficiency is high；And used ceramic dielectric material meets institute X9R's
It is required that the capacitor prepared also meets the requirement of X9R capacitors.
The used to solve above-mentioned technical problem technical solution of the present invention is：
A kind of X9R high-temperature stables multilayer ceramic capacitor porcelain slurry, raw material composition include X9R high-temperature stables multi-layer ceramics electricity
Vessel media material (i.e. porcelain powder) and organic solvent, dispersant, binding agent, plasticizer, antifoaming agent, levelling agent, each component and porcelain
The weight ratio of powder is respectively：Organic solvent 46%~55%, dispersant 1.0%~2.0%, binding agent 3.0%~6.0% increase
Mould agent 3.0%~6.0%, antifoaming agent 0.2%~0.4%, levelling agent 0.1%~0.4%.
The preparation method of above-mentioned X9R high-temperature stables multilayer ceramic capacitor porcelain slurry, includes the following steps：
(a) each raw material is weighed by said ratio；
(b) organic solvent, dispersion are added in the X9R high-temperature stables medium material for multilayer ceramic capacitors (i.e. porcelain powder)
After agent, ball milling 4~8 hours makes dielectric material fully dispersed and is uniformly mixed, obtains premix；
(c) premix obtained by step (b) with binding agent, plasticizer is mixed, it is abundant adds antifoaming agent, levelling agent ball milling
Mixing is starched to get to X9R high-temperature stable multilayer ceramic capacitors porcelain.Wherein, Ball-milling Time preferably 12~24 hours.
By said program, the organic solvent is toluene and the mixed solvent of ethyl alcohol, it is preferable that weight ratio during two kinds of mixing
For toluene：Ethyl alcohol=(1.5-2.5):1.
By said program, the dispersant is triethyl phosphate.
By said program, the binding agent is polyvinyl butyral (PVB).
By said program, the plasticizer is dibutyl phthalate (DBP).
By said program, the antifoaming agent is n-butanol and the mixed solvent of ethylene glycol, it is preferable that weight during two kinds of mixing
Than for n-butanol：Ethylene glycol=(0.5-1.5):1.
By said program, the levelling agent is cyclohexanone.
By said program, the X9R high-temperature stables medium material for multilayer ceramic capacitors, including matrix components and doping group
Point, the matrix components are (1-x) BaTiO3-xBi(Znl/2Til/2)O3(0.10≤x≤0.25)；The doping component is
Nb2O5, in terms of mass fraction, doping quality is 0.5wt.%~2.5wt.% of matrix components., preparation method, including as follows
Step：
(1) according to the expression formula of matrix components (1-x) BaTiO3-xBi(Znl/2Til/2)O3It is golden in (0.10≤x≤0.25)
Belong to atomic stoichionmtry than choosing BaTiO3、ZnO、Bi2O3、TiO2As base starting material；And weigh Nb2O5As dopant, mix
Impurity level is 0.5wt.%~2.5wt.% of matrix total amount；
(2) it is the base starting material and dopant ball milling mixing that have been weighed in step (1) is uniform, it is warming up to 900 after drying~
1050 DEG C of pre-burnings 2~3 hours；Wherein heating rate is 2~3 DEG C/min；
(3) it by the powder ball milling after step (2) pre-burning, dries and porcelain powder, as X9R high-temperature stables multi-layer ceramic capacitance is made
Device dielectric material.
It is a further object of the present invention to provide a kind of preparation method of X9R high-temperature stables multilayer ceramic capacitor, i.e.,：It will be upper
It states X9R high-temperature stable multilayer ceramic capacitors porcelain slurry and is cut by making electrode and dielectric layer, lamination in medium diaphragm, alternately double exposure
It cuts, dumping, sintering, sealing end and burn the processes such as end X9R high-temperature stable multilayer ceramic capacitors are prepared.
By said program, the making medium diaphragm step is：By casting technique make dry diaphragm thickness for 100 μm~
160 μm of medium diaphragm.
By said program, electrode and dielectric layer step are in the alternately double exposure：Using the printing technology being staggered front to back, borrow
Dislocation block is helped to complete to misplace, prints bar block that high printing quality, high aligning accuracy are made after the dielectric film lamination of electrode.
By said program, the lamination, which is cut into, to be laminated an above-mentioned bar block, isostatic pressed and cuts into raw cook.Lamination
Condition with isostatic pressed can be depending on actual conditions, and the condition in the present invention preferably is：Pressure during lamination for 40MPa~
46MPa, temperature are 40 DEG C~50 DEG C；Pressure during isostatic pressed is 20MPa~35MPa, and the dwell time is 25min~40min.
By said program, the temperature of the dumping is 600 DEG C~650 DEG C, and soaking time is 2~4 hours.Wherein, dumping
Heating rate is 0.1~0.5 DEG C/min.
By said program, the sintering is preferably divided into low-temperature sintering stage (0 DEG C~400 DEG C), intermediate sintering temperature stage (400
DEG C~1000 DEG C) and the high temperature sintering stage (1000 DEG C~1150 DEG C).Wherein, the heating rate in the low-temperature sintering stage is
0.2~1 DEG C/min, the heating rate of medium temperature heating sintering stage is 0.2~0.5 DEG C/min, and sintering stage is completed in soak
Heating rate for 0.5~1 DEG C/min, soaking time is 2~4 hours.
By said program, in the printing, sealing end and burning end step, termination electrode material is silver-colored termination electrode material, is
Common commercial product, when printing, adopt inner electrode using Ag/Pd materials；It burns end to carry out in air furnace, burns the end highest temperature
It is 500~600 DEG C to spend, 15~30min of soaking time.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, X9R high-temperature stables medium material for multilayer ceramic capacitors of the present invention meets the wide hot operation range of X9R,
High-temperature stability is good.The present invention, which is added in using this ceramic dielectric material after suitable organic additive, prepares porcelain slurry, this porcelain slurry
The ceramic diaphragm thickness that is cast out uniformly, without surface quality problems such as apparent pin hole, bubble and crackles.
2nd, in method of preparing capacitor provided by the present invention, sintering temperature is low, and the requirement to process equipment is simple, and
Working efficiency is high.The MLCC devices of gained of the invention dielectric constant within the temperature range of -55 DEG C~+200 DEG C is about 800~
1100, dielectric loss is low to be met (<0.40%), dielectric loss is gradually reduced with the raising of temperature, and capacitance temperature changes
Rate (Δ C/C25℃≤ ± 15%), meet the performance requirement of high temperature X 9R-MLCC.
Description of the drawings
Fig. 1 is the preparation technology flow chart of chip multilayer ceramic capacitor.
Fig. 2 is the cross-sectional view of the structure of X9R multilayer ceramic capacitors.
Fig. 3 is the XRD spectrum of capacitor dielectric material prepared by embodiment 1.
Fig. 4 be embodiment 1 prepare capacitor dielectric material under 1kHz, 10kHz, 100kHz frequency dielectric constant with temperature
The relation curve of degree.
Fig. 5 is that capacitor dielectric material prepared by embodiment 1 relationship of temperature coefficient of capacitance and temperature under 1kHz frequencies is bent
Line.
Fig. 6 be embodiment 1 prepare chip multilayer ceramic capacitor under 1kHz, 10kHz, 100kHz frequency dielectric constant
With the relation curve of temperature.
Fig. 7 is that chip multilayer ceramic capacitor prepared by embodiment 1 holds temperature variation under 1kHz, 10kHz, 100kHz frequency
The relation curve of rate and temperature.
Specific embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
1st, a kind of X9R high-temperature stables medium material for multilayer ceramic capacitors, including matrix components and doping component, the base
Matter component is 0.80BaTiO3-0.20Bi(Znl/2Til/2)O3, further include dopant Nb2O5, doping is matrix in mass
The 1.5wt.% of composition quality score.
Above-mentioned X9R high-temperature stables medium material for multilayer ceramic capacitors, includes the following steps：
(1) according to matrix components expression formula 0.80BaTiO3-0.20Bi(Znl/2Til/2)O3Middle metallic atom stoichiometric ratio
Choose BaTiO3、ZnO、Bi2O3、TiO2As base starting material；And weigh Nb2O5As dopant, doping quality is base starting material
The 1.5wt.% of total amount；
(2) it is the base starting material and dopant ball milling mixing that have been weighed in step (1) is uniform, 900 DEG C are warming up to after drying
Pre-burning 2 hours；Wherein heating rate is 3 DEG C/min；
(3) it by the powder ball milling after step (2) pre-burning, dries and ceramic powders, as X9R high-temperature stables multi-layer ceramics is made
Capacitor dielectric material.
(4) to the test of gained X9R high-temperature stable medium material for multilayer ceramic capacitors dielectric material performances, by binding agent
PVA (5%) is added in ceramic powders obtained by step (3) and is uniformly mixed, and is then sieved, tabletting；The ceramic disks liter that will be pressed into
Temperature keeps the temperature 2 hours to 600 DEG C, then heats at 1120 DEG C and is sintered, keeps the temperature 2 hours, and then test its dielectric properties.
The ceramic medium material that 1 step of embodiment (4) obtains does material phase analysis after polishing, polishing with X-ray diffractometer；
Upper silver paste tests its dielectric properties, as shown in Fig. 3, Fig. 4, Fig. 5.As can be seen from Figure 3, pure perovskite can be formed in x=0.2
Phase；From Fig. 4,5 it is found that during as x=0.2, the dielectric constant under room temperature is 1165, dielectric loss 0.015, and dielectric loss
It is gradually reduced with the raising of temperature, temperature range of the temperature coefficient of capacitance without departing from ± 15%：- 55 DEG C~+200 DEG C, have super
The characteristics of wide operating temperature, high stability, meets the requirement of X9R type high temperature multi-layer capacitor dielectric materials.
2nd, a kind of X9R high-temperature stables multilayer ceramic capacitor porcelain slurry, raw material composition include X9R high-temperature stable multi-layer ceramics
Capacitor dielectric material (i.e. porcelain powder) and organic solvent, dispersant, binding agent, plasticizer, antifoaming agent, levelling agent, each component with
The weight ratio of porcelain powder is respectively：Organic solvent 48%, dispersant TEP (triethyl phosphate) 1.4%, binding agent PVB (polyvinyl alcohol
Butyral) 4.0%, Plasticizer DBP (dibutyl phthalate) 4.0%, antifoaming agent 0.3%, levelling agent cyclohexanone 0.15%.
Wherein organic solvent is toluene and ethyl alcohol by weight 1:2 mix；Antifoaming agent is that n-butanol is by weight with ethylene glycol
1:1 mixes.
The preparation method of above-mentioned X9R high-temperature stables multilayer ceramic capacitor porcelain slurry, includes the following steps：
(a) each raw material is weighed by said ratio；
(b) organic solvent, dispersion are added in the X9R high-temperature stables medium material for multilayer ceramic capacitors (i.e. porcelain powder)
After agent, ball milling 4 hours makes dielectric material fully dispersed and is uniformly mixed, obtains premix；
(c) premix obtained by step (b) with binding agent, plasticizer is mixed, adds antifoaming agent, levelling agent in horizontal ball
Porcelain slurry is formed after ball milling is sufficiently mixed for 24 hours on grinding machine to starch to get to X9R high-temperature stable multilayer ceramic capacitors porcelain.
3rd, a kind of preparation method of X9R high-temperature stables multilayer ceramic capacitor, i.e.,：Above-mentioned X9R high-temperature stables multilayer is made pottery
Porcelain condenser porcelain slurry by make medium diaphragm, alternately electrode and dielectric layer in double exposure, lamination cutting, dumping, sintering, sealing end and
It burns the processes such as end and X9R high-temperature stable multilayer ceramic capacitors is prepared, be as follows：
(1) medium diaphragm is made：It is starched purer porcelain is obtained after above-mentioned porcelain slurry vacuum filtration, using film casting technology
Preparation media diaphragm is carried with the PET film of 38 μ m thicks as matrix, and the porcelain slurry of preparation is poured into curtain coating box, is passed through simultaneously
The setting of edge height is cast, certain thickness ceramic porcelain is starched into even application in PET film, and be dried to through being cast drying tunnel
For ceramic diaphragm, the ceramic dielectric diaphragm being cast out is 100 μm；
(2) electrode and dielectric layer in alternating double exposure：Using the printing technology being staggered front to back, inner electrode is using commercial
Ag70-Pd30 inner electrodes are completed to misplace by dislocation block, and height is made after printing 26 layers of the dielectric film lamination of electrode
Bar block of printing quality, high aligning accuracy；
(3) lamination cutting：An above-mentioned bar block is laminated and cuts into raw cook, wherein, pressure during lamination is
45MPa, temperature are 45 DEG C.Pressure during isostatic pressed is 35MPa, dwell time 30min；
(4) dumping, sintering：It will be sintered in conventional, electric-resistance stove after raw cook progress dumping, obtain sintered capacitance
Device.Wherein, the temperature of dumping is 600 DEG C, and soaking time is 2 hours, and dumping heating rate is 0.2 DEG C/min；Low-temperature sintering rank
The heating rate of section (0 DEG C~400 DEG C) is 0.2 DEG C/min, the heating rate of medium temperature heating sintering stage (400 DEG C~1000 DEG C)
For 0.5 DEG C/min, heating rate that sintering stage (1000 DEG C~1150 DEG C) is completed in soak is 1 DEG C/min, soaking time
It is 2 hours；
(5) it blocks and burns end：Silver electrode is coated at the both ends of above-mentioned capacitor, chip multilayer is obtained after applying end silver ink firing
Ceramic capacitor.Wherein, the temperature for applying end silver ink firing is 600 DEG C, soaking time 15min.
The chip multilayer ceramic capacitor that embodiment 1 obtains tests its dielectric properties, respectively as shown in Figure 6, Figure 7.From figure
6 it is found that when frequency is 1kHz, and at 35 DEG C or so, there are one Jie Wen Feng；During less than 35 DEG C, dielectric constant is continuously increased；Work as temperature
When degree is higher than 35 DEG C, dielectric constant is gradually reduced；Dielectric loss is in ever-reduced trend with the raising of temperature.Room temperature (25
DEG C) under dielectric constant for 1015, the slightly below dielectric constant (1165) of potsherd；Dielectric loss is (0.85%), than ceramics
The dielectric loss (1.5%) of piece is low.It will be seen in fig. 7 that when frequency is 1kHz, the warm curve that is situated between becomes flat, -55 DEG C~
+ 200 DEG C of temperature coefficient of capacitance requirements for meeting X9R capacitors.
After the chip multilayer ceramic capacitor test insulation resistance that embodiment 1 obtains, find it in the case where temperature is 25 DEG C
Insulation resistance is 4.70 × 1011Ω(≥1010Ω).RC values are 11900 Ω F at 25 DEG C, and 200 DEG C of whens are 175 Ω F；Insulation resistance
And RC is more than 100G Ω at 25 DEG C and is either more than 10G Ω at 200 DEG C more than 1000 Ω F or more than 100 Ω F, meets
The requirement of EIA.
The chip multilayer ceramic capacitor that embodiment 1 obtains can be expressed as Ag70-Pd30X9R-MLCC products, performance
As shown in table 1.
Table 1
Note：Model specification dissects, 1210 (L of product size：3.20 ± 0.20mm, W：2.50 ± 0.20mm), capacity：
26nF, rated voltage：220V.
Embodiment 2-5
Embodiment 2-5 and embodiment 1 the difference lies in：The formula of porcelain slurry is different, is specifically shown in Table 2.Table 2 is matched for porcelain slurry
Performance of side's (mass ratio of each component and porcelain powder) with tape casting diaphragm.
Table 2
Match when diaphragm comparing result it is found that embodiment 1, embodiment 3 and the proportioning of embodiment 4 are cast from by table 2
The diaphragm performance gone out is more excellent, and the membrane surface that the formula of wherein embodiment 1 is cast out is without apparent bubble, crackle, and distribution is most
To be uniform, performance is the most excellent.
Table 3
Table 3 is to be cast out diaphragm using different formula of size, in same sintering after a series of casting technique processes
At a temperature of the performance of capacitor prepared.From the properties comparing result by table 3 it is found that embodiment 3, embodiment 4 are made
It is more excellent for the capacitor performance gone out, therefore the quality of diaphragm has a significant impact to the performance of later stage capacitor.Although implement
Example 3, embodiment 4 temperature coefficient of capacitance meet the requirement of X9R-MLCC, but their dielectric constant, capacitance and insulation resistance
Below embodiment 1, dielectric loss is higher than embodiment 1, therefore 1 performance of embodiment is the most excellent.
The above is only the preferred embodiment of the present invention, it is noted that those of ordinary skill in the art are come
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to the present invention's
Protection domain.
Claims (8)
1. a kind of X9R high-temperature stables multilayer ceramic capacitor porcelain slurry, it is characterised in that it is more that its raw material composition includes X9R high-temperature stables
Layer ceramic capacitor dielectric material and organic solvent, dispersant, binding agent, plasticizer, antifoaming agent, levelling agent, each component and X9R
The weight ratio of high-temperature stable medium material for multilayer ceramic capacitors is respectively：Organic solvent 46%~55%, dispersant 1.0%~
2.0%, binding agent 3.0%~6.0%, plasticizer 3.0%~6.0%, antifoaming agent 0.2%~0.4%, levelling agent 0.1%~
0.4%；
The preparation method of the X9R high-temperature stables medium material for multilayer ceramic capacitors includes the following steps：
(1) according to the expression formula of matrix components (1-x) BaTiO3-xBi(Znl/2Til/2)O3Metal is former in (0.10≤x≤0.25)
Sub- stoichiometric ratio chooses BaTiO3、ZnO、Bi2O3、TiO2As base starting material；And weigh Nb2O5As dopant, doping
Measure 0.5wt.%~2.5wt.% for matrix total amount；
(2) it is the base starting material and dopant ball milling mixing that have been weighed in step (1) is uniform, 900~1050 are warming up to after drying
DEG C pre-burning 2~3 hours；Wherein heating rate is 2~3 DEG C/min；
(3) it by the powder ball milling after step (2) pre-burning, dries and porcelain powder is made, as X9R high-temperature stables multilayer ceramic capacitor is situated between
Material.
2. a kind of X9R high-temperature stables multilayer ceramic capacitor porcelain slurry according to claim 1, it is characterised in that described organic
Solvent is toluene and the mixed solvent of ethyl alcohol；The dispersant is triethyl phosphate；The binding agent is polyvinyl butyral；
The plasticizer is dibutyl phthalate；The antifoaming agent is n-butanol and the mixed solvent of ethylene glycol；The levelling agent
For cyclohexanone.
3. the preparation method that X9R high-temperature stables multilayer ceramic capacitor porcelain described in claim 1 is starched, it is characterised in that including as follows
Step：
(a) it weighs each raw material by proportioning and includes X9R high-temperature stables medium material for multilayer ceramic capacitors and organic solvent, dispersion
Agent, binding agent, plasticizer, antifoaming agent, levelling agent, the weight of each component and X9R high-temperature stable medium material for multilayer ceramic capacitors
Measuring ratio is respectively：Organic solvent 46%~55%, dispersant 1.0%~2.0%, binding agent 3.0%~6.0%, plasticizer
3.0%~6.0%, antifoaming agent 0.2%~0.4%, levelling agent 0.1%~0.4%；
(b) after adding in organic solvent, dispersant in the X9R high-temperature stables medium material for multilayer ceramic capacitors, ball milling 4~
8 hours, make dielectric material fully dispersed and be uniformly mixed, obtain premix；
(c) premix obtained by step (b) with binding agent, plasticizer is mixed, it is fully mixed adds antifoaming agent, levelling agent ball milling
It closes and is starched to get to X9R high-temperature stable multilayer ceramic capacitors porcelain.
4. X9R high-temperature stable multilayer ceramic capacitors prepared by porcelain slurry described in claim 1.
5. the preparation method of the X9R high-temperature stable multilayer ceramic capacitors described in claim 4, it is characterised in that by the X9R
High-temperature stable multilayer ceramic capacitor porcelain slurry is by making electrode and dielectric layer, lamination cutting, row in medium diaphragm, alternately double exposure
X9R high-temperature stable multilayer ceramic capacitors are prepared in glue, sintering, sealing end and burning end process.
6. the preparation method of X9R high-temperature stables multilayer ceramic capacitor according to claim 5, it is characterised in that the system
Making medium diaphragm step is：The medium diaphragm that dry diaphragm thickness is 100 μm~160 μm is made by casting technique；The lamination
Be cut into will alternately a bar block obtained by electrode and dielectric layer step is laminated, isostatic pressed and cuts into raw cook in double exposure, middle level
Pressure during pressure is 40MPa~46MPa, and temperature is 40 DEG C~50 DEG C；Pressure during isostatic pressed is 20MPa~35MPa, during pressurize
Between be 25min~40min.
7. the preparation method of X9R high-temperature stables multilayer ceramic capacitor according to claim 5, it is characterised in that the burning
Knot be divided into 1000 DEG C of 0 DEG C~400 DEG C of low-temperature sintering stage, 400 DEG C~1000 DEG C of intermediate sintering temperature stage and high temperature sintering stage~
1150℃；The heating rate in the low-temperature sintering stage is 0.2~1 DEG C/min, and the heating rate of medium temperature heating sintering stage is
0.2~0.5 DEG C/min, the heating rate in high temperature sintering stage is 0.5~1 DEG C/min, and soaking time is 2~4 hours.
8. the preparation method of X9R high-temperature stables multilayer ceramic capacitor according to claim 5, it is characterised in that described
Alternately in double exposure in electrode and dielectric layer, sealing end and burning end step, termination electrode material is silver-colored termination electrode material, and inner electrode is adopted
With Ag/Pd materials；It burns end to carry out in air furnace, it is 500~600 DEG C to burn end maximum temperature, 15~30min of soaking time.
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