CN109279882A - A kind of strontium silicate copper system media ceramic of temperature coefficient adjustable and its preparation method and application - Google Patents

A kind of strontium silicate copper system media ceramic of temperature coefficient adjustable and its preparation method and application Download PDF

Info

Publication number
CN109279882A
CN109279882A CN201710602160.7A CN201710602160A CN109279882A CN 109279882 A CN109279882 A CN 109279882A CN 201710602160 A CN201710602160 A CN 201710602160A CN 109279882 A CN109279882 A CN 109279882A
Authority
CN
China
Prior art keywords
temperature coefficient
copper system
media ceramic
system media
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710602160.7A
Other languages
Chinese (zh)
Inventor
张平
廖建文
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin University
Original Assignee
Tianjin University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tianjin University filed Critical Tianjin University
Priority to CN201710602160.7A priority Critical patent/CN109279882A/en
Publication of CN109279882A publication Critical patent/CN109279882A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C04B35/16—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 silicates other than clay
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • 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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3213—Strontium oxides or oxide-forming salts thereof
    • 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
    • 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
    • C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O

Abstract

The invention discloses strontium silicate copper system media ceramics of a kind of temperature coefficient adjustable and its preparation method and application, are with SrCuSi4O10Based on media ceramic, its sintering temperature is successfully down to 900 DEG C by 1100 DEG C by additional 0.5~2.0% LiF sintering aid, and preparing dielectric constant is 5.88, dielectric loss 1.6 × 10‑3The microwave-medium ceramics that (1MHz), temperature coefficient of permittivity are 119.90ppm/ DEG C.With SrCuSi4O10Based on -1.0%LiF media ceramic, additional 15.0~24.0% TiO2Temperature coefficient regulator, is successfully realized SrCuSi4O10The controllability of media ceramic temperature coefficient.Preparation cost of the invention is low, and simple process, process is pollution-free, prepares a kind of up-and-coming LTCC medium substrate material.

Description

A kind of strontium silicate copper system media ceramic of temperature coefficient adjustable and preparation method thereof and Using
Technical field
The present invention relates to ceramic composition technical fields, are situated between more particularly to a kind of strontium silicate copper system of temperature coefficient adjustable Matter ceramics and its preparation method and application.
Background technique
Fast development of the hyundai electronics information technology to high frequency, high stable, low-loss direction, to critical electronic element material More stringent requirements are proposed for material-media ceramic performance.In order to meet this requirement, low-k, low-loss, nearly zero temperature Degree coefficient, inexpensive dielectric ceramic material become the hot spot direction studied now.With low-temperature co-fired ceramics (low- Temperature co-fired ceramic, LTCC) multi-layer structure design based on technology can effectively reduce device volume, It is to realize component to miniaturization, integrated and modular important channel.LTCC technology requires dielectric material that can lead with height (961 DEG C) realization cofirings of electric rate and cheap silver electrode.It is therefore desirable to for using the dielectric material on microwave device Sintering temperature will be at 950 DEG C or less.
SrCuSi4O10It is a kind of novel medium substrate material with superior dielectric properties, raw material inexpensively can be substantially Cost is reduced, and there is lower dielectric constant (4.0) and dielectric loss (1.0 × 10-3), but sintering temperature is 1100 DEG C, and there is biggish temperature coefficient of permittivity.Its higher sintering temperature causes it that cannot apply in LTCC technology, Biggish temperature coefficient of permittivity also limits it in the application in high-stability requirement field.
Summary of the invention
The purpose of the present invention is be to overcome SrCuSi4O10It is that media ceramic sintering temperature is excessively high, temperature coefficient of permittivity It is too high, the disadvantage in LTCC technology cannot be applied to, provide one kind with SrCO3、CuO、SiO2For primary raw material, additional LiF, TiO2As sintering aid, cooperate SrCO3、CuO、SiO2Raw material, sintering temperature is successfully down to 900 DEG C, dielectric by 1100 DEG C The adjustable strontium silicate copper system media ceramic of constant temperature coefficient, while the dielectric properties for keeping its excellent.
The technical solution adopted to achieve the purpose of the present invention is:
A kind of preparation method of the strontium silicate copper system media ceramic of temperature coefficient adjustable of the invention, comprising the following steps:
(1) by SrCO3、CuO、SiO2Raw material, by chemical formula SrCuSi4O10Carry out ingredient, i.e. SrCO3、CuO、SiO2Rub Than being 1:1:4 by raw material, deionized water, abrading-ball, ball milling in polyester tank is added in you；
(2) raw material after step (1) ball milling is placed in drying box, is dried in 80~130 DEG C, 20-40 mesh is crossed after drying Sieve, obtains evengranular powder；
(3) powder that step (2) are uniformly mixed is warming up to from 20-25 DEG C of room temperature with 3 DEG C -5 DEG C of speed per minute 950-975 DEG C pre-burning 4-5 hours, furnace cooling after calcining；
(4) ceramic powder after pre-burning that step (3) obtains is put into polyester tank, additional mass percent 0.5~ 2.0% LiF (i.e. the mass ratio of LiF and the ceramic powder is (0.005~0.02): 1) and mass percent 0%~ 24.0% TiO2(i.e. TiO2It is (0~0.24) with the mass ratio of the ceramic powder: 1) is mixed with calcined powder, ball Mill, is granulated drying, crosses 60-80 mesh, then be shaped to green body with powder compressing machine；
(5) by the green body of step (4) in being warming up to 825~925 from 20-25 DEG C of room temperature with 3 DEG C -5 DEG C of speed per minute DEG C sintering, keep the temperature 4~8 hours, then furnace cooling, be made strontium silicate copper system media ceramic.
Preferably, the mass percent of LiF is 1.0%, TiO in the step (4)2Mass percent be 15.0%~ 24.0%.
Preferably, raw material in the step (1): deionized water: the mass ratio of abrading-ball is 1:(15-17): (14-16), ball Time consuming is 4~8 hours.
Preferably, it is added deionized water and zirconia ball in the step (4) when ball milling, ball milling 4~8 hours, granulation Specific steps are as follows: the paraffin that added weight percentage is 8~10% in ceramic powder is granulated as adhesive.
Preferably, the operating pressure of the tablet press machine of the step (4) be 4-5MPa, green body specification be Φ (14-16) mm × The cylindrical body of (0.5-1.5) mm.
Another aspect of the present invention further includes TiO2On the adjustable strontium silicate copper system media ceramic of preparation temperature coefficient Using.
Another aspect of the present invention further includes a kind of strontium silicate copper system media ceramic prepared according to the method described above, wherein SrCuSi4O10With LiF, TiO2Mass ratio be 1:(0.005~0.02): (0~0.24), i.e. ceramic powder and LiF, TiO2's Mass ratio is 1:(0.005~0.02): (0~0.24).
Preferably, SrCuSi in the strontium silicate copper system media ceramic4O10With LiF, TiO2Mass ratio be 1:0.01: (0.15~0.24), i.e. ceramic powder and LiF, TiO2Mass ratio be 1:0.01:(0.15~0.24).
Preferably, the dielectric constant of the strontium silicate copper system media ceramic is 5.28-6.32, and temperature coefficient of permittivity is 112.86-137.48ppm/ DEG C, dielectric loss is 1.6 × 10-3-230.0×10-3(1MHz)。
Preferably, the dielectric constant 6.42-6.85 of the strontium silicate copper system media ceramic, temperature coefficient of permittivity be- 15.4-38.6ppm/ DEG C, dielectric loss is 2.7 × 10-3-5.4×10-3(1MHz)。
Another aspect of the present invention further includes TiO2On the adjustable strontium silicate copper system media ceramic of preparation temperature coefficient Using.
Another aspect of the present invention further includes application of the strontium silicate copper system media ceramic on microwave device.
Compared with prior art, the beneficial effects of the present invention are:
Beneficial effects of the present invention are with SrCuSi4O10Based on media ceramic, additional 0.5~2.0% LiF sintering Its sintering temperature is successfully down to 900 DEG C by 1100 DEG C by auxiliary agent, and preparing dielectric constant is 5.88, dielectric loss 1.6 × 10-3 The microwave-medium ceramics that (1MHz), temperature coefficient of permittivity are 119.90ppm/ DEG C.With SrCuSi4O10- 1.0%LiF medium Based on ceramics, additional 15.0~24.0% TiO2Temperature coefficient regulator, is successfully realized SrCuSi4O10Medium pottery The controllability of porcelain temperature coefficient.Under conditions of 900 DEG C of sintering temperature, sintering time 6 hours, preparing dielectric constant is 6.73, dielectric loss 3.7 × 10-3The microwave-medium ceramics that (1MHz), temperature coefficient of permittivity are 1.80ppm/ DEG C.The present invention Preparation cost it is low, simple process, process is pollution-free, is a kind of up-and-coming LTCC medium substrate material.
Detailed description of the invention
Fig. 1 show the SEM figure of strontium silicate copper system media ceramic of the invention
Wherein: a is the SEM figure of strontium silicate copper system media ceramic made from embodiment 1；
B is the SEM figure of strontium silicate copper system media ceramic made from embodiment 2；
C is the SEM figure of strontium silicate copper system media ceramic made from embodiment 3；
D is the SEM figure of strontium silicate copper system media ceramic made from embodiment 4.
Specific embodiment
The present invention is described in further detail below in conjunction with the drawings and specific embodiments.It should be appreciated that described herein Specific embodiment be only used to explain the present invention, be not intended to limit the present invention.
The present invention is greater than 99.0% chemical raw material: SrCO using purity3、CuO、SiO2, prepare SrCuSi4O10Medium pottery Porcelain.
The present invention is by SrCO3、CuO、SiO2Raw material presses chemical formula SrCuSi4O10Carry out ingredient, raw material: deionized water: abrading-ball Quality be 1:16:15, be added polyester tank in, ball milling 4~8 hours；Again by the raw material after ball milling be placed in infrared drying oven in 80~130 DEG C of drying, cross 40 meshes, calcine 4 hours then at 900~1000 DEG C；Calcined ceramic powder is put into ball milling again In tank, the LiF sintering aid that additional mass percent is 0.5~2.0% is added in calcined powder, and zirconium oxide is then added Ball and deionized water ball milling 4~8 hours；The paraffin that added weight percentage is 8~10% in ceramic powder after drying again is viscous Mixture is granulated, cross 80 meshes after, with powder compressing machine under the pressure of 4MPa by powder be pressed into diameter be 15mm, with a thickness of The green compact of 1mm；Green compact are sintered at 825~950 DEG C, 4~8 hours is kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made. Finally by capacity measuring set and the dielectric properties of dependence test fixture test article.
On the basis of adding LiF sintering aid acquisition best sintering character, calcined ceramic powder is put into ball milling In tank, the LiF sintering aid that additional mass percent is 1.0% is added in calcined powder, adds 15.0~24.0% TiO2, zirconia ball and deionized water ball milling 4~8 hours are then added；Added weight hundred in ceramic powder after drying again Divide than being granulated for 8~10% paraffin wax binder, after crossing 80 meshes, with powder compressing machine by powder under the pressure of 4MPa Being pressed into diameter is 15mm, the green compact with a thickness of 1mm；Green compact are sintered at 850~925 DEG C, keep the temperature 4~8 hours, low temperature is made and burns The strontium silicate copper system media ceramic of knot, temperature coefficient adjustable.Finally by capacity measuring set and dependence test fixture test article Dielectric properties.
The specific embodiment of the invention is as follows.
Embodiment 1
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weighs LiF-0.1000g that mass percent is 0.5% and forge Powder mixing after burning, is added zirconia ball and deionized water secondary ball milling 6 hours, dries after discharging, cross 40 meshes；Then again The paraffin that additional mass percent is 8% is granulated as adhesive, and crosses 80 meshes；Again with powder compressing machine with 4MPa's It is 15mm, the green body with a thickness of 1mm that pressure, which is pressed into diameter,；
5. green body is sintered in 900 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 2
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weighs LiF-0.2000g that mass percent is 1.0% and forge Powder mixing after burning, is added zirconia ball and deionized water secondary ball milling 6 hours, dries after discharging, cross 40 meshes；Then again The paraffin that additional mass percent is 8% is granulated as adhesive, and crosses 80 meshes；Again with powder compressing machine with 4MPa's It is 15mm, the green body with a thickness of 1mm that pressure, which is pressed into diameter,；
5. green body is sintered in 900 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 3
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weighs LiF-0.3000g that mass percent is 1.5% and forge Powder mixing after burning, is added zirconia ball and deionized water secondary ball milling 6 hours, dries after discharging, cross 40 meshes；Then again The paraffin that additional mass percent is 8% is granulated as adhesive, and crosses 80 meshes；Again with powder compressing machine with 4MPa's It is 15mm, the green body with a thickness of 1mm that pressure, which is pressed into diameter,；
5. green body is sintered in 900 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 4
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weighs LiF-0.4000g that mass percent is 2.0% and forge Powder mixing after burning, is added zirconia ball and deionized water secondary ball milling 6 hours, dries after discharging, cross 40 meshes；Then again The paraffin that additional mass percent is 8% is granulated as adhesive, and crosses 80 meshes；Again with powder compressing machine with 4MPa's It is 15mm, the green body with a thickness of 1mm that pressure, which is pressed into diameter,；
5. green body is sintered in 875 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 5
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weighs LiF-0.2000g that mass percent is 1.0% and forge Powder mixing after burning, is added zirconia ball and deionized water secondary ball milling 6 hours, dries after discharging, cross 40 meshes；Then again The paraffin that additional mass percent is 8% is granulated as adhesive, and crosses 80 meshes；Again with powder compressing machine with 4MPa's It is 15mm, the green body with a thickness of 1mm that pressure, which is pressed into diameter,；
5. green body is sintered in 825 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 6
1. according to microwave-medium ceramics component SrCuSi4O10, claim SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weighs LiF-0.2000g that mass percent is 1.0% and forge Powder mixing after burning, is added zirconia ball and deionized water secondary ball milling 6 hours, dries after discharging, cross 40 meshes；Then again The paraffin that additional mass percent is 8% is granulated as adhesive, and crosses 80 meshes；Again with powder compressing machine with 4MPa's It is 15mm, the green body with a thickness of 1mm that pressure, which is pressed into diameter,；
5. green body is sintered in 850 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 7
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weighs LiF-0.2000g that mass percent is 1.0% and forge Powder mixing after burning, is added zirconia ball and deionized water secondary ball milling 6 hours, dries after discharging, cross 40 meshes；Then again The paraffin that additional mass percent is 8% is granulated as adhesive, and crosses 80 meshes；Again with powder compressing machine with 4MPa's It is 15mm, the green body with a thickness of 1mm that pressure, which is pressed into diameter,；
5. green body is sintered in 875 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 8
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weighs LiF-0.2000g that mass percent is 1.0% and forge Powder mixing after burning, is added zirconia ball and deionized water secondary ball milling 6 hours, dries after discharging, cross 40 meshes；Then again The paraffin that additional mass percent is 8% is granulated as adhesive, and crosses 80 meshes；Again with powder compressing machine with 4MPa's It is 15mm, the green body with a thickness of 1mm that pressure, which is pressed into diameter,；
5. green body is sintered in 925 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
See Table 1 for details for the every key parameter and its dielectric properties testing result of some embodiments of the present invention.
Table 1
In table: τεIt is dielectric loss for temperature coefficient of permittivity, tan δ.
Embodiment 9
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weigh LiF-0.2000g and matter that mass percent is 1.0% Measure the TiO that percentage is 15.0%2- 3.0000g is mixed with calcined powder, and zirconia ball and deionized water secondary ball is added Mill 6 hours, is dried after discharging, crosses 40 meshes；Then the paraffin that additional mass percent is 8% again is made as adhesive Grain, and cross 80 meshes；Again with powder compressing machine with the pressure of 4MPa be pressed into diameter for 15mm, with a thickness of the green body of 1mm；
5. green body is sintered in 900 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 10
1. according to microwave-medium ceramics component SrCuSi4O10, claim SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weigh LiF-0.2000g and matter that mass percent is 1.0% Measure the TiO that percentage is 18.0%2- 3.6000g is mixed with calcined powder, and zirconia ball and deionized water secondary ball is added Mill 6 hours, is dried after discharging, crosses 40 meshes；Then the paraffin that additional mass percent is 8% again is made as adhesive Grain, and cross 80 meshes；Again with powder compressing machine with the pressure of 4MPa be pressed into diameter for 15mm, with a thickness of the green body of 1mm；
5. green body is sintered in 900 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 11
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weigh LiF-0.2000g and matter that mass percent is 1.0% Measure the TiO that percentage is 21.0%2- 4.2000g is mixed with calcined powder, and zirconia ball and deionized water secondary ball is added Mill 6 hours, is dried after discharging, crosses 40 meshes；Then the paraffin that additional mass percent is 8% again is made as adhesive Grain, and cross 80 meshes；Again with powder compressing machine with the pressure of 4MPa be pressed into diameter for 15mm, with a thickness of the green body of 1mm；
5. green body is sintered in 900 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
Embodiment 12
1. according to microwave-medium ceramics component SrCuSi4O10, weigh SrCO3-6.3157g、CuO-3.4028g、SiO2- 10.2815g ingredient, total 20.0000g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, Ball milling 6 hours on planetary ball mill, drum's speed of rotation are 1000 revs/min；
2. the raw material after ball milling is placed in drying box, 40 meshes are dried and crossed in 120 DEG C, obtain evengranular powder Material；
3. evengranular powder is calcined 4 hours in 975 DEG C；
4. calcined powder is put into polyester tank, then weigh LiF-0.2000g and matter that mass percent is 1.0% Measure the TiO that percentage is 24.0%2- 4.8000g is mixed with calcined powder, and zirconia ball and deionized water secondary ball is added Mill 6 hours, is dried after discharging, crosses 40 meshes；Then the paraffin that additional mass percent is 8% again is made as adhesive Grain, and cross 80 meshes；Again with powder compressing machine with the pressure of 4MPa be pressed into diameter for 15mm, with a thickness of the green body of 1mm；
5. green body is sintered in 900 DEG C, 6 hours are kept the temperature, low-temperature sintering strontium silicate copper system media ceramic is made；
Finally, testing the dielectric property of resulting product by capacity measuring set and dependence test fixture.
See Table 2 for details for the every key parameter and its dielectric properties testing result of some embodiments of the present invention.
Table 2
As seen from the above table, when the additive amount of LiF is 1.0wt%, TiO2When additive amount is 15.0~24.0wt%, temperature system Number can be adjusted between -15.4~38.6.
The detection method of the embodiment of the present invention is as follows:
1. the diameter and thickness of product is measured using micrometer.
2. parallel using starting to rob by Agilent E4981A 120Hz/1KHz/1MHz Capacitance Meter Plate method measures the dielectric constant of prepared cylindrical ceramic material, and test fixture is put into ESPEC MC-710F type high/low temperature and is followed Circumstance temperature case carries out the measurement of temperature coefficient of permittivity, and temperature range is that 25-85 DEG C of test frequency is 1MHz.
3. measuring prepared cylinder using Agilent E4981A 120Hz/1KHz/1MHz Capacitance Meter The dielectric loss of shape ceramic.
The SEM figure of the strontium silicate copper system media ceramic of embodiment 1-4 preparation is as shown in Figure 1, as seen from the figure, prepared by the present invention Strontium silicate copper system media ceramic microstructure it is good.
The above is only a preferred embodiment of the present invention, it is noted that for the common skill of the art For art personnel, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications Also it should be regarded as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of the strontium silicate copper system media ceramic of temperature coefficient adjustable, which comprises the following steps:
(1) by SrCO3、CuO、SiO2Raw material, by chemical formula SrCuSi4O10Ingredient is carried out, by raw material, deionized water, abrading-ball, is added Enter ball milling in polyester tank；
(2) raw material after step (1) ball milling is placed in drying box, is dried in 80~130 DEG C, 20-40 mesh is crossed after drying, is obtained Obtain evengranular powder；
(3) powder that step (2) are uniformly mixed is warming up to 950-975 from 20-25 DEG C of room temperature with 3 DEG C -5 DEG C of speed per minute DEG C pre-burning 4-5 hours, furnace cooling after calcining；
(4) ceramic powder after pre-burning that step (3) obtains is put into polyester tank, additional mass percent 0.5~2.0% The TiO of LiF and mass percent 0%~24.0%2It is mixed with calcined powder, ball milling, drying, granulation, crosses 60-80 mesh Sieve, then green body is shaped to powder compressing machine；
(5) by the green body of step (4) in being warming up to 825~925 DEG C of burnings from 20-25 DEG C of room temperature with 3 DEG C -5 DEG C of speed per minute Knot keeps the temperature 4~8 hours, and strontium silicate copper system media ceramic is made in then furnace cooling.
2. a kind of preparation method of the strontium silicate copper system media ceramic of temperature coefficient adjustable as described in claim 1, feature It is, the mass percent of LiF is 1.0%, TiO in the step (4)2Mass percent be 15.0%~24.0%.
3. a kind of preparation method of the strontium silicate copper system media ceramic of temperature coefficient adjustable as described in claim 1, feature Be, raw material in the step (1): deionized water: the mass ratio of abrading-ball be 1:(15-17): (14-16), Ball-milling Time be 4~ 8 hours；It is added deionized water and zirconia ball in the step (4) when ball milling, ball milling 4~8 hours, the specific steps of granulation Are as follows: the paraffin that added weight percentage is 8~10% in ceramic powder is granulated as adhesive.
4. a kind of preparation method of the strontium silicate copper system media ceramic of temperature coefficient adjustable as described in claim 1, feature It is, the operating pressure of the tablet press machine of the step (4) is 4-5MPa, and green body specification is Φ (14-16) mm × (0.5-1.5) mm Cylindrical body.
5.TiO2Application on the adjustable strontium silicate copper system media ceramic of preparation temperature coefficient.
6. a kind of strontium silicate copper system media ceramic of the temperature coefficient adjustable of method preparation as described in claim 1, feature exist In SrCuSi4O10With LiF, TiO2Mass ratio be 1:(0.005~0.02): (0~0.24).
7. a kind of strontium silicate copper system media ceramic of temperature coefficient adjustable as claimed in claim 6, which is characterized in that SrCuSi4O10With LiF, TiO2Mass ratio be 1:0.01:(0.15~0.24).
8. a kind of strontium silicate copper system media ceramic of temperature coefficient adjustable as claimed in claim 6, which is characterized in that the silicon The dielectric constant of sour strontium copper system media ceramic is 5.28-6.32, and temperature coefficient of permittivity is 112.86-137.48ppm/ DEG C, Dielectric loss is 1.6 × 10-3-230.0×10-3(1MHz)。
9. a kind of strontium silicate copper system media ceramic of temperature coefficient adjustable as claimed in claim 7, which is characterized in that the silicon The dielectric constant 6.42-6.85 of sour strontium copper system media ceramic, temperature coefficient of permittivity are -15.4-38.6ppm/ DEG C, dielectric damage Consumption is 2.7 × 10-3-5.4×10-3(1MHz)。
10. application of the strontium silicate copper system media ceramic of temperature coefficient adjustable as claimed in claim 6 on microwave device.
CN201710602160.7A 2017-07-21 2017-07-21 A kind of strontium silicate copper system media ceramic of temperature coefficient adjustable and its preparation method and application Pending CN109279882A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710602160.7A CN109279882A (en) 2017-07-21 2017-07-21 A kind of strontium silicate copper system media ceramic of temperature coefficient adjustable and its preparation method and application

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710602160.7A CN109279882A (en) 2017-07-21 2017-07-21 A kind of strontium silicate copper system media ceramic of temperature coefficient adjustable and its preparation method and application

Publications (1)

Publication Number Publication Date
CN109279882A true CN109279882A (en) 2019-01-29

Family

ID=65185761

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710602160.7A Pending CN109279882A (en) 2017-07-21 2017-07-21 A kind of strontium silicate copper system media ceramic of temperature coefficient adjustable and its preparation method and application

Country Status (1)

Country Link
CN (1) CN109279882A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111848150A (en) * 2020-07-09 2020-10-30 上海交通大学医学院附属第九人民医院 SrCuSi4O10－Ca3(PO4)2Composite bioceramic, bone scaffold and application thereof
CN113242844A (en) * 2019-02-27 2021-08-10 费罗公司 LTCC dielectric compositions and devices with high Q
CN115947587A (en) * 2022-09-30 2023-04-11 郴州功田电子陶瓷技术有限公司 Microwave dielectric ceramic with low dielectric constant, and preparation method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106478083A (en) * 2016-10-13 2017-03-08 天津大学 A kind of low sintering preparation method of strontium silicate copper system microwave-medium ceramics

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106478083A (en) * 2016-10-13 2017-03-08 天津大学 A kind of low sintering preparation method of strontium silicate copper system microwave-medium ceramics

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
JIANLI MA ET AL.: "Low-fired Mg2SiO4-based dielectric ceramics with temperature stable for LTCC applications", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
PING ZHANG ET AL.: "Microstructures and dielectric properties of low permittivity SrCuSi4O10-Bi2O3 ceramics for LTCC applications", 《J MATER SCI: MATER ELECTRON》 *
ZHIFEN FU ET AL.: "Microwave dielectricpropertiesoflow-fired Li2MnO3 ceramics co-doped with LiF–TiO2", 《CERAMICS INTERNATIONAL》 *
杨桃: "低温烧结硅酸镁陶瓷及其微波介电性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113242844A (en) * 2019-02-27 2021-08-10 费罗公司 LTCC dielectric compositions and devices with high Q
CN113242844B (en) * 2019-02-27 2023-08-08 费罗公司 LTCC dielectric compositions and devices having high Q values
CN111848150A (en) * 2020-07-09 2020-10-30 上海交通大学医学院附属第九人民医院 SrCuSi4O10－Ca3(PO4)2Composite bioceramic, bone scaffold and application thereof
CN111848150B (en) * 2020-07-09 2022-05-24 上海交通大学医学院附属第九人民医院 SrCuSi4O10－Ca3(PO4)2Composite bioceramic, bone scaffold and application thereof
CN115947587A (en) * 2022-09-30 2023-04-11 郴州功田电子陶瓷技术有限公司 Microwave dielectric ceramic with low dielectric constant, and preparation method and application thereof
CN115947587B (en) * 2022-09-30 2024-02-02 郴州功田电子陶瓷技术有限公司 Microwave dielectric ceramic and preparation method thereof

Similar Documents

Publication Publication Date Title
CN100456393C (en) High-dielectric constant microwave dielectric ceramic and producing method thereof
CN106587987B (en) The preparation method of C0G microwave dielectric material and preparation method and ceramic material
CN105565799B (en) A kind of low-loss temperature-stabilized high-frequency dielectric ceramic
CN105254293B (en) A kind of microwave dielectric ceramic materials and preparation method thereof
CN109279882A (en) A kind of strontium silicate copper system media ceramic of temperature coefficient adjustable and its preparation method and application
CN106699150A (en) Low temperature sintering low dielectric constant C0G microwave dielectric material and preparation method thereof
CN110183227A (en) A kind of Li2MoO4-Mg2SiO4Base composite ceramic microwave material and preparation method thereof
CN107162583A (en) The method that barium titanate based ceramic dielectric-temperature stability is improved based on component gradient
CN104860672A (en) High dielectric microwave ceramic dielectric material and preparation method thereof
CN105801104B (en) A kind of high dielectric constant temperature-stable ceramic capacitor dielectric material
CN109231985A (en) A kind of preparation method of low-loss X8R type dielectric substance
CN107235711A (en) Temperature-stable metaantimmonic acid magnesium lithium-based microwave medium composite ceramics and preparation method thereof
CN106478083A (en) A kind of low sintering preparation method of strontium silicate copper system microwave-medium ceramics
CN104692800B (en) A kind of temperature-stable unleaded huge dielectric constant ceramic material
CN104310986A (en) High dielectric constant stable-temperature ceramic capacitor dielectric material
CN104803681B (en) A kind of new type low temperature sinters low dielectric constant microwave dielectric ceramic material
CN105859289A (en) Low-temperature sintering low-loss magnesium-lithium-niobate-series microwave dielectric ceramic
CN109437887A (en) A kind of anion substitution low temperature sintering lithium magnesium titanium series microwave dielectric ceramic
CN101030478B (en) High-dielectric metal-electric medium composite ceramic capacitance and its production
CN101215159A (en) Low-temperature sintering low-loss high frequency medium ceramic and preparing method thereof
CN112408977A (en) High-quality ceramic dielectric material and preparation method thereof
CN1971783A (en) Barium titanate based metal-dielectric composite ceramic capacitor medium and its preparing method
CN107500756A (en) A kind of high-k low-loss SrTiO3Based dielectric material and preparation method thereof
CN105859281B (en) A kind of low Jie's ceramics as low-loss microwave medium and preparation method
CN105272192B (en) A kind of low-k AG characteristic multilayer ceramic capacitor porcelains and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190129