CN1719560A - Method for mfg. crystal boundary layer ceramic medium material and substrate for single layer capacitor and substrate thereof - Google Patents

Method for mfg. crystal boundary layer ceramic medium material and substrate for single layer capacitor and substrate thereof Download PDF

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Publication number
CN1719560A
CN1719560A CN 200510034827 CN200510034827A CN1719560A CN 1719560 A CN1719560 A CN 1719560A CN 200510034827 CN200510034827 CN 200510034827 CN 200510034827 A CN200510034827 A CN 200510034827A CN 1719560 A CN1719560 A CN 1719560A
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ceramics
layer capacitor
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substrate
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CN100418167C (en
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庄严
朱卓雄
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Guangzhou Tianji Electronic Technology Co.,Ltd.
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GUANGZHOU XIANGYU MICROELECTRONICS CO Ltd
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Abstract

This invention relates to a medium porcelain of a grain boundary layer ceramics of a single layer condenser, the composition and weight portion of which is: SrCO3 64.66~65.95, TiO2 34.99~35.69, Nb2O5 0.20~0.45 a modified additive 0.5~1.5 including one or several kinds of SiO2, Al2O3, MnO2 CaCO3 and CuO. This invention also relates to a preparation method for a chip applying said porcelain and the chip. The modified additive of this medium ceramics increase the mechanical and electric performance of the grain boundary and limits the over growing of grains. This method manufactures smooth and clean chips and applies an oxidizer, the additive of which enables it to form a grain boundary of good performance after penetrating into the ceramic chip under 1050~1250deg.C.

Description

The manufacture method and the substrate thereof of single-layer capacitor boundary ceramics dielectric ceramic composition, substrate
Technical field
The present invention relates to the dielectric ceramic composition that a kind of capacitor is used, relate in particular to the dielectric ceramic composition of a kind of single-layer capacitor with the boundary ceramics substrate; The present invention also relates to a kind of manufacture method that adopts described dielectric ceramic composition to use the boundary ceramics substrate as the single-layer capacitor of raw material; The invention still further relates to the single-layer capacitor boundary ceramics substrate that described method is made.
Background technology
Single-layer capacitor (SLC) is to adapt to the electronic component high frequencyization, highly integrated, microminiaturized, the new ceramics capacitor that the requirement of low-power consumption and high reliability grows up, compare with the MLCC multilayer ceramic capacitor, owing to there is not current circuit between dielectric layer, thereby under high frequency, particularly microwave, have lower equivalent series resistance, higher quality factor and the reliability of Geng Gao.
The grain-boundary layer capacitor porcelain has the dielectric constant height, and the characteristics of temperature characterisitic and microwave frequency characteristic good are introduced into the manufacturing of single-layer capacitor in recent years as a kind of new dielectric material.Existing SrTiO 3The production process of grain-boundary layer capacitor porcelain is to utilize exact chemical doping process and powder process technology, by the reducing atmosphere sintering, generates semiconductive ceramic, utilizes oxidant oxidation crystal boundary selectively then.Is crystal boundary the feature of this porcelain as condenser dielectric.Production process requires stoichiometry accurate, and powder mixes, granularity is suitable and narrow distribution, and the composition of sintering curve and reducing atmosphere, pressure, flow tie in, and oxidant composition and infiltration capacity are suitable; And to make the product of electrical property excellence, then will be to above-mentioned process optimization and ingenious cooperation, should strictly control grain size and distribution, reducing degree, strict again control crystal boundary composition, thickness and degree of oxidation, thereby technical difficulty is quite high, particularly this material grains is bigger, generally more than 20 μ, thereby fragility is big, how yielding liquid phase is during the reduction sintering, oxidant liquefaction is infiltrated in the ceramics during oxidizing thermal treatment, also makes ceramics very easily be out of shape bonding die, and it is very difficult especially with the boundary ceramics substrate to make the big single-layer capacitor of thickness small size to this porcelain.
So far only there are U.S. AVX and Johanson company can utilize the grain boundary layer substrate to make the SLC product in the world, but do not find have pertinent literature to disclose the manufacture method of this substrate and the prescription of respective media porcelain both at home and abroad.
Summary of the invention
First technical problem to be solved by this invention provides a kind of being applicable to and makes the dielectric ceramic composition of single-layer capacitor with the boundary ceramics substrate.
Second technical problem to be solved by this invention provides a kind of manufacture method of making single-layer capacitor with the boundary ceramics substrate.
The 3rd technical problem to be solved by this invention provides the produced single-layer capacitor of a kind of employing said method boundary ceramics substrate.
The present invention solves the technical scheme of first technical problem:
A kind of single-layer capacitor dielectric ceramic composition of boundary ceramics, it is characterized in that: its composition and weight portion are:
SrCO 3 64.66～65.95
TiO 2 34.99～35.69
Nb 2O 5 0.20～0.45
Property-modifying additive 0.5～15;
Described property-modifying additive is SiO 2, Al 2O 3, MnO 2, CaCO 3, any or several among the CuO, its total weight parts is 0.5～15.
The present invention solves the technical scheme of second technical problem:
A kind of single-layer capacitor manufacture method of boundary ceramics substrate, it comprises the steps:
1. with the dielectric ceramic composition batch mixing of claim 1, oven dry is sieved;
2. raw material with synthetic grog ball mill grinding, sieve after synthesizing under 1200～1260 ℃;
3. after chamotte powder adds adhesive, adopt and roll film or casting method moulding diaphragm; Press the die-cut diaphragm of size of product requirement;
4. spray on the diaphragm every the stick slurry; Lamination dress Bowls is in 1100～1200 ℃ of binder removals;
⑤ Zheng Portland packs in the atmosphere furnace, in the hydrogen nitrogen mixed gas atmosphere, burns till under 1350～1500 ℃;
6. carry out ultrasonic cleaning and separate burning whole the folding of ceramics;
7. ceramics is sandwiched in two smooth smooth refractory plates, under 1150～1250 ℃ of temperature, composes flat;
8. oxidant is carried out grinding, sieve, be mixed into oxidizer slurry with adhesive then; On ceramics, print oxidizer slurry with silk screen seal point methods; Ceramics is promptly made single-layer capacitor boundary ceramics substrate in 1050～1250 ℃ of following oxidizing thermal treatment.
4. above-mentioned the go on foot describedly every stick, and it is formed and weight portion is
SrCO 3 60～65
TiO 2 35～40
Every stick property-modifying additive 80～100;
Described is ZrO every the stick property-modifying additive 2, AL 2O 3Or any or multiple in the flour, its total weight parts is 80～100.
Above-mentioned the 4. to go on foot described be described every stick and water modulation every the stick slurry.
8. above-mentioned the go on foot described oxidant, and it is formed and weight portion is:
Pb 3O4 0～52
Bi 2O 3 34～37
B 2O 3 15～18
Oxidant property-modifying additive 5～10;
Described oxidant property-modifying additive is SiO 2, CuO, MnO 2, Ni 2O 3, any or several among the NaF, its total weight parts is 5～10.
The present invention solves the technical scheme of the 3rd technical problem:
The single-layer capacitor boundary ceramics substrate that a kind of said method is made, used dielectric ceramic composition, its composition and weight portion are:
SrCO 3 64.66～65.95
TiO 2 34.99～35.69
Nb 2O 5 0.20～0.45
Property-modifying additive 0.5～15;
Described property-modifying additive is SiO 2, Al 2O 3, MnO 2, CaCO 3, any or several among the CuO.
Beneficial effect of the present invention:
1. dielectric ceramic composition of the present invention, its property-modifying additive have improved the mechanical electric performance of crystal boundary, and the restriction excessive grain is grown up.
2. manufacture method of the present invention utilize curtain coating or roll film, spraying every stick, compose technology such as flat, ultrasonic waves for cleaning, guarantee that thickness is little of 0.1mm, area is greatly to 52 * 52mm 2Ceramics is smooth bright and clean, reaches excellent planar degree, roughness.
3. the present invention has adopted oxidant in manufacturing process, and wherein the oxidant property-modifying additive makes oxidant after 1050～1250 ℃ of infiltration ceramics, forms the good grain boundary layer of electromechanical properties.
The present invention adopt special preparation every stick, make product can fold burning, Non-sticking is suitable for producing in batches.
5. single-layer capacitor of the present invention has big capacitance with the boundary ceramics substrate, low dielectric loss, high resistivity and low variation of capacitance with temperature; Have good flatness and roughness, thickness is from 0.1mm to 0.5mm, and area satisfies the requirement of making the various sizes single-layer capacitor greatly to 50 * 50mm.
Embodiment
Embodiment 1
SrCO with 64.66 weight portions 3, 35.10 weight portions TiO 2, 0.24 weight portion Nb 2O 5, 0.05 weight portion SiO 2, 0.1 weight portion MnO 2, 1 weight portion CaCO 3The dielectric ceramic composition batch mixing, after the oven dry, sieve; Raw material are synthetic down at 1200 ℃; And the pulverizing of the grog after will synthesizing, sieve; The preparation slurry, chamotte powder adds adhesive and makes slurry, casting film-forming repeatedly, gross thickness 0.25mm; Be cut into diaphragm by dimensional requirement then, in the spraying every the stick slurry; Lamination dress Bowls is per hour to heat up 50 ℃ of speed binder removals to 1150 ℃; Cooling Hou Zheng Portland packs in the hydrogen nitrogen mixed gas atmosphere furnace, with 100 ℃ of speed to 1420 ℃ 2 hours sintering of insulation that per hour heat up; Burn that the ceramics that is whole to stack in the ultrasonic wave rinse bath, cleaning up every stick, the while is separated ceramics; Ceramics is sandwiched in two smooth smooth alumina plates, under 1150 ℃ of temperature, composes flat; With the oxidant grinding, sieve, place oxidant powder and adhesive mortar to modulate oxidizer slurry; On ceramics, print oxidizer slurry with method for printing screen; Oxidizing thermal treatment in 1100 ℃ promptly makes single-layer capacitor boundary ceramics substrate.
Form and weight portion is 60 parts of SrCO3,40 parts of TiO2,8O part ZrO every stick in the present embodiment 2
Oxidant composition and weight portion are 49 parts of Pb in the present embodiment 3O 4, 34 parts of Bi 2O 3, 17 parts of B 2O 3, 5 parts of CuO, 2 parts of MnO 2
Embodiment 2-6
Be other several embodiment of the present invention below, the single-layer capacitor that discloses these several embodiment is formed and percentage by weight with the dielectric ceramic composition of boundary ceramics, adopt following every stick composition and composition and the weight portion and the technological parameter of weight portion, oxidant, by the step of manufacturing of single-layer capacitor of the present invention, prepare single-layer capacitor of the present invention boundary ceramics substrate with the boundary ceramics substrate.
Embodiment Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
Dielectric ceramic composition is formed and weight portion SrCO 3 65.95 64.85 65.00 65.20 64.66
TiO 2 34.99 35.69 35.12 35.25 35.43
Nb 2O 5 0.20 0.25 0.38 0.42 0.45
Property-modifying additive 0.1 part SiO 20.3 part Al 2O 30.2 part MnO 25 parts of CaCO 3 0.5 part CuO 2 parts of SiO 211 parts of CaCO 33 parts of CuO 3 parts of SiO 2 0.3 part Al 2O 33.2 part MnO 2
Composition and weight portion every stick SrCO 3 65 63 64 62 60
TiO 2 35 37 36 38 40
Every the stick property-modifying additive 80 parts of ZrO 2 85 parts of Al of 15 parts of flour 2O 3 90 parts of Al 2O 3 25 parts of ZrO of 40 parts of flour 225 parts of Al 2O 3 95 parts of flour
The composition of oxidant and weight portion Pb 3O 4 0 52 48 12 34
Bi 2O 3 37 34 36 35 36
B 2O 3 18 16 15 17 17
The oxidant property-modifying additive 5 parts of SiO 2 3 parts of Ni of 3 parts of CuO 2O 33 parts of MnO 2 4 parts of Ni 2O 33 parts of SiO 20.5 part NaF 3 parts of SiO of 2 parts of CuO 23 parts of Ni 2O 32 parts of MnO 2 6 parts of CuO
Synthesis temperature (℃) 1200 1260 1240 1230 1250
The moulding diaphragm approach (℃) Roll film Curtain coating Curtain coating Roll film Curtain coating
Dump temperature (℃) 1100 1200 1180 1160 1130
Sintering temperature (℃) 1350 1500 1400 1380 1450
Compose flat temperature (℃) 1250 1150 1200 1230 1170
Oxidizing temperature (℃) 1250 1050 1100 1150 1180
With the boundary ceramics substrate sampling of the single-layer capacitor of the foregoing description preparation, splash-proofing sputtering metal electrode; Ceramics through sputtering electrode is cut into 2 * 2mm 2Small pieces; Measure the mechanical electric performance of small pieces.
Press K=11.3Ct/S, ρ=RS/t calculates its performance dielectric constant and dc resistivity (t and s are respectively ceramics thickness and electrode area) respectively, draws the performance table of embodiment thus.
Substrate performance table
Embodiment 25 ℃ of following electric properties Mechanical performance
K tgδ (×10 -4) ρ 50V(× 10 10Ω cm) Temperature characterisitic Δ C/C (%) (25～+ 125 ℃) Puncture voltage V/mm (DC) Rough surface Ra (um) Flatness (mm) Size (mm) (L * B * T)
1 2.6 ten thousand ≤50 ≥100 ≤12 ≥1000 ≤2.0 ≤0.4 52×52× 0.22
2 2.3 ten thousand ≤40 ≥150 ≤7.5 ≥1300 ≤1.8 ≤0.25 38×38× 0.50
3 4.8 ten thousand ≤60 ≥80 ≤22 ≥800 ≤1.7 ≤0.2 26×26× 0.10
4 2.0 ten thousand ≤35 ≥150 ≤3.0 ≥1500 ≤1.7 ≤0.2 26×26× 0.10
5 3.0 ten thousand ≤30 ≥100 ≤12 ≥1000 ≤1.8 ≤0.3 38×38× 0.38
6 3.3 ten thousand ≤45 ≥100 ≤10 ≥1000 ≤1.9 ≤0.2 38×38× 0.17

Claims (6)

1. a single-layer capacitor is with the dielectric ceramic composition of boundary ceramics, and it is characterized in that: its composition and weight portion are:
SrCO 3 64.66～65.95
TiO 2 34.99～35.69
Nb 2O 5 0.20～0.45
Property-modifying additive 0.5～15;
Described property-modifying additive is SiO 2, Al 2O 3, MnO 2, CaCO 3, any or several among the CuO.
2. the manufacture method of a single-layer capacitor usefulness boundary ceramics substrate is characterized in that it comprises the steps:
1. with the dielectric ceramic composition batch mixing of claim 1, oven dry is sieved;
2. raw material synthesize down and with synthetic grog ball mill grinding, sieve at 1200～1260 ℃;
3. after chamotte powder adds adhesive, adopt and roll film or casting method moulding diaphragm; Press the die-cut diaphragm of size of product requirement;
4. spray on the diaphragm every the stick slurry; Lamination dress Bowls is in 1100～1200 ℃ of binder removals;
⑤ Zheng Portland packs in the atmosphere furnace, in the hydrogen nitrogen mixed gas atmosphere, burns till under 1350～1500 ℃;
6. carry out ultrasonic cleaning and separate burning whole the folding of ceramics;
7. ceramics is sandwiched in two smooth smooth refractory plates, under 1150～1250 ℃ of temperature, composes flat;
8. oxidant is carried out grinding, sieves, be mixed into oxidizer slurry with adhesive then; On ceramics, print oxidizer slurry with method for printing screen; Ceramics is promptly made single-layer capacitor boundary ceramics substrate in 1050～1250 ℃ of following oxidizing thermal treatment.
3. manufacture method according to claim 2 is characterized in that: 4. the go on foot describedly every stick, and it is formed and weight portion is
SrCO 3 60～65
TiO 2 35～40
Every stick property-modifying additive 80～100;
Described is ZrO every the stick property-modifying additive 2, AL 2O 3Or it is any or multiple in the flour.
4. according to claim 2 or 3 described manufacture methods, it is characterized in that: described the 4. the step be describedly to modulate every the stick slurry every stick and water.
5. manufacture method according to claim 2 is characterized in that: 8. described the go on foot described oxidant, and it is formed and weight portion is:
Pb 3O 4 0～52
Bi 2O 3 34～37
B 2O 3 15～18
Oxidant property-modifying additive 5～10;
Described oxidant property-modifying additive is SiO 2, CuO, MnO 2, Ni 2O 3, any or several among the NaF.
6. the single-layer capacitor boundary ceramics substrate of any one manufacture method manufacturing of claim 2-5, it is characterized in that: its dielectric ceramic composition is the described dielectric ceramic composition of claim 1.
CNB2005100348275A 2005-05-31 2005-05-31 Method for mfg. crystal boundary layer ceramic medium material and substrate for single layer capacitor and substrate thereof Active CN100418167C (en)

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CN101295635B (en) * 2007-04-29 2010-05-19 中芯国际集成电路制造(上海)有限公司 Method and device for improving capacity of MIM capacitance
CN1975943B (en) * 2006-12-20 2010-11-03 天津大学 Doped copper titanium oxide capacitor ceramic dielectric and producing method thereof
CN102013320A (en) * 2010-10-22 2011-04-13 广东风华高新科技股份有限公司 Single-layer capacitor and preparation method thereof
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CN105777112A (en) * 2016-04-12 2016-07-20 武汉理工大学 Ti-bit donor-acceptor co-doping SrTiO3 base high-dielectric ceramic and preparation method thereof
CN108439975A (en) * 2018-05-18 2018-08-24 武汉理工大学 It is a kind of have stablize strontium titanates calcium base energy storage ceramic of defect sturcture and preparation method thereof
CN113072376A (en) * 2021-04-12 2021-07-06 中国振华集团云科电子有限公司 Oxidizing agent for grain boundary layer semiconductor ceramic substrate and coating method thereof
CN115974547A (en) * 2023-02-01 2023-04-18 中国振华集团云科电子有限公司 SrTiO for grain boundary layer capacitor 3 Method for preparing base ceramic substrate

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CN1063732C (en) * 1994-05-06 2001-03-28 清华大学 Method for making strontium titanate base grain-boundary layer capacitor material
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CN101295635B (en) * 2007-04-29 2010-05-19 中芯国际集成电路制造(上海)有限公司 Method and device for improving capacity of MIM capacitance
CN102013320A (en) * 2010-10-22 2011-04-13 广东风华高新科技股份有限公司 Single-layer capacitor and preparation method thereof
CN102013320B (en) * 2010-10-22 2012-09-05 广东风华高新科技股份有限公司 Single-layer capacitor and preparation method thereof
CN102853669A (en) * 2011-06-30 2013-01-02 史祖法 Box pot for sintering ceramic homocentric sphere
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Patentee after: Aurora Technologies Co., Ltd.

Address before: 510300 Haizhuqu District hi tech innovation science park, 89 Dun Road, Guangdong, Guangzhou

Patentee before: Guangzhou Xiangyu Microelectronics Co., Ltd.

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Address after: 511453 No.6, Changli Road, Dongyong Town, Nansha District, Guangzhou City, Guangdong Province

Patentee after: Guangzhou Tianji Electronic Technology Co.,Ltd.

Address before: Room 601 6th floor building 10 No 5 Industrial Zone South China West Enterprise Group Company daganwei Haizhu District Guangzhou

Patentee before: AURORA TECHNOLOGIES Co.,Ltd.

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