CN105777100A - Intermediate-temperature sintering high-frequency dielectric ceramic capacitor material - Google Patents

Intermediate-temperature sintering high-frequency dielectric ceramic capacitor material Download PDF

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Publication number
CN105777100A
CN105777100A CN201610098246.6A CN201610098246A CN105777100A CN 105777100 A CN105777100 A CN 105777100A CN 201610098246 A CN201610098246 A CN 201610098246A CN 105777100 A CN105777100 A CN 105777100A
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ceramic capacitor
dielectric ceramic
sintering temperature
frequency dielectric
powder
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李玲霞
张帅
吕笑松
孙正
张宁
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Tianjin University
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Tianjin University
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/447Shaped 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 phosphates, e.g. hydroxyapatite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/002Details
    • H01G4/018Dielectrics
    • H01G4/06Solid dielectrics
    • H01G4/08Inorganic dielectrics
    • H01G4/12Ceramic dielectrics
    • H01G4/1209Ceramic dielectrics characterised by the ceramic dielectric material
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206Magnesium oxides or oxide-forming salts thereof
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Ceramic Capacitors (AREA)

Abstract

The invention discloses an intermediate-temperature sintering high-frequency dielectric ceramic capacitor material.The chemical formula of the material is Mg3P2O8.Firstly, raw materials MgO and (NH4)H2PO4 are weighed and mixed according to the chemical formula, the raw materials are calcined at the temperature of 850 DEG C after ball-milling, drying and screening, polyvinyl alcohol with the mass percentage of 5% is added, and after ball-milling, drying and screening, a green body is formed; the green body is sintered at the temperature of 1,000-1,075 DEG C, and the intermediate-temperature sintering high-frequency dielectric ceramic capacitor material is prepared.The material has the low sintering temperature (1.000-1,075 DEG C), low dielectric constant (5.4-6.2), small loss value (15*10-4 to 20*10-4) and small capacitance temperature coefficient (40*10-6/DEG C to 170*10-6/DEG C, and the vacancy of low-dielectric-constant capacitors on the market is further filled up.

Description

A kind of intermediate sintering temperature high-frequency dielectric ceramic capacitor material
Technical field
The invention belongs to a kind of ceramic composition being characterized with composition, particularly to a kind of Novel medium temperature sintered high-frequency dielectric pottery Ceramic material and preparation method.
Background technology
Along with advancing by leaps and bounds of electronic information technology, electronic product is just towards the side of light weight slimming, high-performance and multifunction To development.Since entering 21 century, the most in recent years, the integrated level of super large-scale integration device is more and more higher.When When i.e. integrated level improves constantly when the characteristic size of device is gradually reduced, resistance-capacitance (RC) can be caused to postpone to rise, thus The series of problems such as the enhancing of signal transmission delay, noise jamming and power attenuation increase occur, this will greatly limit the height of device Speed performance.Reducing RC and postpone there are two approach with power attenuation, one is to reduce conductor resistance R, and another one is also more simultaneously It is important that reduce parasitic capacitance C that dielectric layer brings.Owing to electric capacity C is proportional to DIELECTRIC CONSTANT εr, so being accomplished by exploitation Novel, low cost and there is the advanced low-k materials of superperformance.
Mg3P2O8Launch research as a kind of photoelectric material before binary system always, then thus do not have people reported its Dielectric properties under high frequency or even microwave frequency band.Through experimental studies have found that this system have sintering temperature low (~1050 DEG C), Low-k (~6), low (≤2x10 is lost-3), and its free dielectric constant temperature coefficient is relatively low.But, this system Sintering temperature can not be applied to the preparation of LTCC (LTCC), for satisfied actual application, reduce system further Sintering temperature, be substantially reduced the cost of multilayer device, become researcher make great efforts direction.
Summary of the invention
The purpose of the present invention, is to prepare a kind of high frequency low-k ceramic condenser, meets the market demand, it is provided that Yi Zhongxin Type intermediate sintering temperature high-frequency dielectric ceramic capacitor and preparation method thereof.
The present invention is achieved by following technical solution.
. a kind of intermediate sintering temperature high-frequency dielectric ceramic capacitor material, its chemical formula is Mg3P2O8
The preparation method of above-mentioned intermediate sintering temperature high-frequency dielectric ceramic capacitor material, has following steps:
(1) by raw material MgO, (NH4)H2PO4By Mg3P2O8Chemical formula weighs dispensing;
(2) powder that step (1) is prepared is put in ball grinder, add zirconia ball and deionized water, ball milling 4 hours;Will Raw material after ball milling is placed in infrared drying oven drying, crosses 40 mesh sieves, it is thus achieved that evengranular powder after drying;
(3) powder after step (2) being processed is calcined 4 hours at 850 DEG C, synthesizes principal crystalline phase;
(4) in the powder after step (3) synthesis principal crystalline phase, additional mass percent is the polyvinyl alcohol of 5%, puts into ball grinder In, add zirconia ball and deionized water, ball milling 12 hours, after drying, cross 80 mesh sieves, then with powder compressing machine with 4MPa Pressure forming be base substrate;
(5) by the base substrate after step (4) molding in 1000~1075 DEG C of sintering, it is incubated 4 hours, makes intermediate sintering temperature high frequency and be situated between Ceramics.
The drying temperature of described step (2) and step (4) is 100 DEG C.
The ceramic powder of described step (2) and step (4) is 1: 1: 2 with zirconia ball, the mass ratio of deionized water.
The base substrate of described step (4) is the disk of Φ 10mm × 1mm.
Briquetting pressure 4Mpa of the powder compressing machine of described step (4).
The sintering temperature of described step (5) is 1050 DEG C, and temperature retention time is 4h.
Beneficial effects of the present invention is as follows:
Provide a kind of Novel medium temperature sintered high-frequency dielectric ceramic material, prepared Mg3P2O8Material, has relatively low sintering Temperature (1000~1075 DEG C), relatively low-k (5.4~6.2), relatively low loss-value (15~20 × 10-4), less electric capacity Amount temperature coefficient (40 × 10-6/ DEG C~170 × 10-6/ DEG C), further compensate for the vacancy of low-k capacitor on market.
Detailed description of the invention
Below by specific embodiment, the invention will be further described, raw materials used in example is commercially available analytical reagent, Specific embodiment is as follows.
Embodiment 1
(1) by raw material MgO, (NH4)H2PO4By Mg3P2O8Chemical formula weighs dispensing;
(2) powder of above-mentioned preparation is put in ball grinder, adds zirconia ball and deionized water, ball milling 4 hours, powder body with Zirconia ball, the mass ratio of deionized water are 1: 1: 2;Raw material after ball milling is placed in infrared drying oven at 100 DEG C baking Dry, cross 40 mesh sieves after drying, it is thus achieved that evengranular powder;
(3) powder of above-mentioned mix homogeneously is calcined 4 hours at 850 DEG C, synthesize principal crystalline phase;
(4) in the powder after synthesis principal crystalline phase, additional mass percent is the polyvinyl alcohol of 5%, puts in ball grinder, adds Zirconia ball and deionized water, powder body is 1: 1: 2 with zirconia ball, the mass ratio of deionized water, and ball milling 12 hours dries Cross 80 mesh sieves after Gan, then be pressed into the base substrate of Φ 10mm × 1mm with powder compressing machine with the pressure of 4MPa;
(5) by the base substrate after above-mentioned molding in 1050 DEG C of sintering, it is incubated 4 hours, makes high-frequency dielectric ceramic capacitor material;
(6) Agilent 4278A electric impedance analyzer is used to test its dielectric properties, under 1MHz, εr=5.83, tan δ=16.3 TCC=78 × 10-6/℃。
Embodiment 2-4
The related process parameters of embodiment 2-4 and dielectric properties refer to table 1, and remaining preparation process is identical with embodiment 1.
Table 1
The present invention is not limited to above-described embodiment, and the change of some details is possible, but the most therefore this run counter to the present invention's Scope and spirit.

Claims (6)

1. an intermediate sintering temperature high-frequency dielectric ceramic capacitor material, its chemical formula is Mg3P2O8
The preparation method of above-mentioned intermediate sintering temperature high-frequency dielectric ceramic capacitor material, has following steps:
(1) by raw material MgO, (NH4)H2PO4By Mg3P2O8Chemical formula weighs dispensing;
(2) powder that step (1) is prepared is put in ball grinder, add zirconia ball and deionized water, ball milling 4 hours;Will Raw material after ball milling is placed in infrared drying oven drying, crosses 40 mesh sieves, it is thus achieved that evengranular powder after drying;
(3) powder after step (2) being processed is calcined 4 hours at 850 DEG C, synthesizes principal crystalline phase;
(4) in the powder after step (3) synthesis principal crystalline phase, additional mass percent is the polyvinyl alcohol of 5%, puts into ball grinder In, add zirconia ball and deionized water, ball milling 12 hours, after drying, cross 80 mesh sieves, then with powder compressing machine with 4MPa Pressure forming be base substrate;
(5) by the base substrate after step (4) molding in 1000~1075 DEG C of sintering, it is incubated 4 hours, makes intermediate sintering temperature high frequency and be situated between Ceramics.
A kind of intermediate sintering temperature high-frequency dielectric ceramic capacitor material the most according to claim 1, it is characterised in that described step Suddenly the drying temperature of (2) and step (4) is 100 DEG C.
A kind of intermediate sintering temperature high-frequency dielectric ceramic capacitor material the most according to claim 1, it is characterised in that described step Suddenly the ceramic powder of (2) and step (4) is 1: 1: 2 with zirconia ball, the mass ratio of deionized water.
A kind of intermediate sintering temperature high-frequency dielectric ceramic capacitor material the most according to claim 1, it is characterised in that described step Suddenly the base substrate of (4) is the disk of Φ 10mm × 1mm.
A kind of intermediate sintering temperature high-frequency dielectric ceramic capacitor material the most according to claim 1, it is characterised in that described step Suddenly briquetting pressure 4Mpa of the powder compressing machine of (4).
A kind of intermediate sintering temperature high-frequency dielectric ceramic capacitor material the most according to claim 1, it is characterised in that described step Suddenly the sintering temperature of (5) is 1050 DEG C, and temperature retention time is 4h.
CN201610098246.6A 2016-02-23 2016-02-23 Intermediate-temperature sintering high-frequency dielectric ceramic capacitor material Pending CN105777100A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109851350A (en) * 2019-01-17 2019-06-07 天津大学 A kind of low Jie high Q lithium magnesium phosphorus system dielectric material and preparation method thereof
CN110937889A (en) * 2019-12-10 2020-03-31 武汉科技大学 Zirconium phosphate ceramic material and preparation method thereof
CN116924789A (en) * 2023-07-25 2023-10-24 山东同方鲁颖电子有限公司 Nickel ion doped low-dielectric magnesium phosphate microwave dielectric ceramic and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104973857A (en) * 2015-07-31 2015-10-14 华南理工大学 Low-dielectric-constant polyanion type microwave dielectric ceramic and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104973857A (en) * 2015-07-31 2015-10-14 华南理工大学 Low-dielectric-constant polyanion type microwave dielectric ceramic and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JIAN-JIANG BIAN等: "Microwave Dielectric Properties of A2P2O7 (A = Ca, Sr, Ba; Mg, Zn, Mn)", 《JAPANESE JOURNAL OF APPLIED PHYSICS》 *
ROBERT NEIMAN等: "Setting and thermal reactions of phosphate investments", 《JOURNAL OF DENTAL RESEARCH》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109851350A (en) * 2019-01-17 2019-06-07 天津大学 A kind of low Jie high Q lithium magnesium phosphorus system dielectric material and preparation method thereof
CN110937889A (en) * 2019-12-10 2020-03-31 武汉科技大学 Zirconium phosphate ceramic material and preparation method thereof
CN110937889B (en) * 2019-12-10 2022-03-04 武汉科技大学 Zirconium phosphate ceramic material and preparation method thereof
CN116924789A (en) * 2023-07-25 2023-10-24 山东同方鲁颖电子有限公司 Nickel ion doped low-dielectric magnesium phosphate microwave dielectric ceramic and preparation method thereof
CN116924789B (en) * 2023-07-25 2024-02-27 山东同方鲁颖电子有限公司 Nickel ion doped low-dielectric magnesium phosphate microwave dielectric ceramic and preparation method thereof

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Application publication date: 20160720