CN110066172A - 一种正温度系数陶瓷介质材料及其制备方法 - Google Patents
一种正温度系数陶瓷介质材料及其制备方法 Download PDFInfo
- Publication number
- CN110066172A CN110066172A CN201910483934.8A CN201910483934A CN110066172A CN 110066172 A CN110066172 A CN 110066172A CN 201910483934 A CN201910483934 A CN 201910483934A CN 110066172 A CN110066172 A CN 110066172A
- Authority
- CN
- China
- Prior art keywords
- temperature coefficient
- ceramic dielectric
- positive temperature
- dielectric material
- heating rate
- 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.)
- Granted
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 41
- 239000003989 dielectric material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000000498 ball milling Methods 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 239000004615 ingredient Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 15
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 abstract description 7
- 239000006104 solid solution Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 12
- 239000003990 capacitor Substances 0.000 description 5
- 238000010304 firing Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000010295 mobile communication Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 206010037660 Pyrexia Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- 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
-
- 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
- H01G4/1236—Ceramic dielectrics characterised by the ceramic dielectric material based on zirconium oxides or zirconates
-
- 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
-
- 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
- C04B2235/3201—Alkali metal 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
-
- 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
- C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
-
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
-
- 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
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
-
- 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
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects 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
-
- 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
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects 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
- C04B2235/6562—Heating rate
-
- 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
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects 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
- C04B2235/6567—Treatment time
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Composite Materials (AREA)
- Inorganic Insulating Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明属陶瓷介质材料技术领域，为解决目前陶瓷介质材料的电容温度系数在‑55℃～150℃范围内有正有负，不断变化的问题，提供一种正温度系数陶瓷介质材料及其制备方法，由质量百分比为80‑90％的Na0.2Bi0.6ZrO3和10‑20％的Yb2O3组成。具备介电常数高、介电损耗低、正温度系数的特征。Na0.2Bi0.6ZrO3材料具有钙钛矿结构，它在‑55℃～150℃范围内没有居里峰，掺入Yb2O3能够使Na+和Bi3+稳定固溶，使其在‑55℃～150℃范围内具有正电容温度系数。
Description
技术领域
本发明属于陶瓷介质材料技术领域，具体涉及一种正温度系数陶瓷介质材料及其制备方法。
背景技术
片式多层陶瓷电容器(MLCC)是三大无源电子元器件之一，它与片式电感器、片式电阻器构成了电子信息产业中不可或缺的基础被动元件。MLCC具有结构紧凑、比容高、体积小、损耗低、价格低廉等优点，除大量应用在移动通信、广播电视、家用电器、家用计算机、医疗设备、测量仪器等民用电子设备中外，在航空航天、军用移动通讯、坦克电子、军事信号监控和武器弹头控制等军用电子设备以及石油勘探等行业中都具有广泛应用。
近年来，超高温环境下电子元器件及相关材料的制造及检测技术正随着电子学的发展而快速发展。在汽车控制领域里，发动机舱内安装的防抱死系统(ABS)、发动机电子控制单元(ECU)、曲柄角传感模块、空气/燃料比控制模块、燃料喷射程序控制(PGMFI)模块等，都要求MLCC在高温下的工作温度范围达到150℃附近。同时航空电子学、环境检测学、自动电子学等很多领域都要求电子系统在极其苛刻的环境下能够工作。电子系统应用在各种恶劣环境中。电子元件的可靠性决定了电子系统总体的可靠性，因此对MLCC可靠性的要求也越来越高。
虽然目前报道的陶瓷介质材料种类繁多，但这些陶瓷材料的电容温度系数在-55℃～150℃范围内有正有负，不断变化。本发明提供一种正电容温度系数高介电材料，它可以作为温度补偿材料和功能器件材料使用，它的发明有助于丰富此类产品的需求。另外，由于电容器在使用过程中在电压的作用下，产生功率损耗并引起发热使电容器温度升高，此种温升决定于外加交流电压，频率的高低电容量及损耗的大小，同时也受散热系数和散热面积的影响。此种温升导致实际电容量降低或升高。研制正温度系数陶瓷介质材料也是为了防止电容器在使用过程中由于温升或其他因素造成的电容量降低，从而提高可靠性，具有重要的意义。
发明内容
本发明为了解决目前陶瓷介质材料的电容温度系数在-55℃～150℃范围内有正有负，不断变化的问题，提供了一种正温度系数陶瓷介质材料及其制备方法，该陶瓷介质材料的介电常数高、介电损耗低、同时具有正电容温度系数。
本发明由如下技术方案实现的：一种正温度系数陶瓷介质材料，由质量百分比为80-90％的Na0.2Bi0.6ZrO3和10-20％的Yb2O3组成。
制备所述的一种正温度系数陶瓷介质材料的方法，步骤如下：
(1)将原料Na2CO3、Bi2O3和ZrO2按通式Na0.2Bi0.6ZrO3，进行配料球磨，在3.3kw的普通烘箱中于100℃干燥4-5小时，过120-250孔/cm2分样筛，升温至800℃，保温2-4小时，制得熔块A；
(2)按照质量百分比将10-20％的Yb2O3和80-90％的熔块A进行二次配料，获得配料B；
(3)将配料B加去离子水70ml在转速为400r/min球磨机上球磨8小时，120℃干燥4-5小时，过120-250孔/cm2分样筛，加入质量百分比为配料B的5-8％的黏合剂造粒，压制成生坯压强为8MPa，先按照2℃/min的升温速率升温至400-500℃，然后再按10℃/min的升温速率升温至1100-1150℃保温1小时，冷却后制得陶瓷介质。
步骤(1)中球磨时间为4-6小时；步骤(1)中升温速率为5-10℃/min。优选步骤(1)中升温速率为7℃/min。
步骤(3)中升温速率为按2℃/min的升温速率升温至450℃，再按10℃/min的升温速率加热至1100-1150℃保温1小时。步骤(3)中的黏合剂为聚乙烯醇或者石蜡。
Na0.2Bi0.6ZrO3介质陶瓷具有适中的烧结温度，一般在1200℃左右、具有高的介电常数、可调的容量温度系数和较低的损耗，是一种性能优异的介质陶瓷材料。本发明选择Na0.2Bi0.6ZrO3介质陶瓷，采取添加Yb2O3改性的方法，具备介电常数高、介电损耗低、正温度系数的特征。其主要机理：Na0.2Bi0.6ZrO3材料具有钙钛矿结构，它在-55℃～150℃范围内没有居里峰，掺入Yb2O3能够使Na+和Bi3+稳定固溶，使其在-55℃～150℃范围内具有正电容温度系数。
附图说明
图1为实施例1、2、3和4所制备的正温度系数陶瓷介质材料的温度系数的测试结果图。
具体实施方式
下面结合具体实施例进一步说明本发明的技术方案。
实施例1：一种正温度系数陶瓷介质材料，由质量百分比为10％的Yb2O3和90％的Na0.2Bi0.6ZrO3组成。
制备所述的正温度系数陶瓷介质材料的方法，步骤如下：将原料Na2CO3、Bi2O3和ZrO2按通式Na0.2Bi0.6ZrO3，进行配料，在转速为400r/min的球磨机上球磨6小时，在3.3kw的普通烘箱中于100℃干燥4小时，过250孔/cm2分样筛，以5℃/min升温至800℃，并在800℃下保温3小时，得到熔块A。
进行二次配料，按照90％熔块A和10％Yb2O3的质量关系均匀混合，加去离子水70ml在转速为400r/min球磨机上球磨8小时，于120℃干燥4小时，过250孔/cm2分样筛，加入8wt％石蜡造粒，压制成生坯压强8MPa，先按2℃/min的升温速率加热至450℃，再按10℃/min的升温速率加热至1100℃烧成，保温1小时，冷却后制得陶瓷介质。所制备的正温度系数陶瓷介质材料的介电性能的测试结果(测试频率为1MHz)见表1和图1。对于实施例1，由图中可以看出，在-55℃～150℃温度范围内，随着温度的升高，介电常数逐渐升高。试样具有正温度系数特征。由表可知，室温下，试样介电常数高，损耗低。
实施例2：一种正温度系数陶瓷介质材料，由质量百分比为15％的Yb2O3和85％的Na0.2Bi0.6ZrO3组成。
制备所述的正温度系数陶瓷介质材料的方法，步骤如下：将原料Na2CO3、Bi2O3和ZrO2按通式Na0.2Bi0.6ZrO3，进行配料，在转速为400r/min的球磨机上球磨5小时，在3.3kw的普通烘箱中于100℃干燥5小时，过200孔/cm2分样筛，以7℃/min升温至800℃，并在800℃下保温2小时，得到熔块A。
进行二次配料，按照85％熔块A和15％Yb2O3的质量关系均匀混合，加去离子水70ml在转速为400r/min球磨机上球磨8小时，于120℃干燥4小时，过200孔/cm2分样筛，加入7wt％石蜡造粒，压制成生坯压强为8MPa，先按2℃/min的升温速率加热至500℃，再按10℃/min的升温速率加热至1110℃烧成，保温1小时，冷却后制得陶瓷介质。所制备的正温度系数陶瓷介质材料的介电性能的测试结果(测试频率为1MHz)见表1和图1。对于实施例2，由图中可以看出，在-55℃～150℃温度范围内，随着温度的升高，介电常数逐渐升高。试样具有正温度系数特征。由表可知，室温下，试样介电常数高，损耗低。
实施例3：一种正温度系数陶瓷介质材料，由重量百分比为20％的Yb2O3和80％的Na0.2Bi0.6ZrO3组成。
制备所述的正温度系数陶瓷介质材料的方法，步骤如下：将原料Na2CO3、Bi2O3和ZrO2按通式Na0.2Bi0.6ZrO3，进行配料，在转速为400r/min的球磨机上球磨4小时，在3.3kw的普通烘箱中于100℃干燥5小时，过120孔/cm2分样筛，以10℃/min升温至800℃，并在800℃下保温4小时，得到熔块A。
进行二次配料，按照80％熔块A和20％Yb2O3的质量关系均匀混合，加去离子水70ml在转速为400r/min球磨机上球磨8小时，于120℃干燥5小时，过120孔/cm2分样筛，加入5wt％石蜡造粒，压制成生坯压强8MPa，先按2℃/min的升温速率加热至400℃，再按10℃/min的升温速率加热至1120℃烧成，保温1小时，冷却后制得陶瓷介质。所制备的正温度系数陶瓷介质材料的介电性能的测试结果(测试频率为1MHz)见表1和图1。对于实施例3，由图中可以看出，在-55℃～150℃温度范围内，随着温度的升高，介电常数逐渐升高。试样具有正温度系数特征。由表可知，室温下，试样介电常数高，介电损耗低。
实施例4：一种正温度系数陶瓷介质材料，由重量百分比为11％的Yb2O3和89％的Na0.2Bi0.6ZrO3组成。
制备所述的正温度系数陶瓷介质材料的方法，步骤如下：将原料Na2CO3、Bi2O3和ZrO2按通式Na0.2Bi0.6ZrO3，进行配料，在转速为400r/min的球磨机上球磨6小时，在3.3kw的普通烘箱中于100℃干燥5小时，过250孔/cm2分样筛，以5℃/min升温至800℃，并在800℃下保温3小时，得到熔块A。
进行二次配料，按照89％熔块A和11％Yb2O33的质量关系均匀混合，加去离子水70ml在转速为400r/min球磨机上球磨8小时，于120℃干燥5小时，过250孔/cm2分样筛，加入8wt％石蜡造粒，压制成生坯压强8MPa，先按2℃/min的升温速率加热至450℃，再按10℃/min的升温速率加热至1150℃烧成，保温1小时，冷却后制得陶瓷介质。所制备的正温度系数陶瓷介质材料的介电性能的测试结果(测试频率为1MHz)见表1和图1。对于实施例4，由图中可以看出，在-55℃～150℃温度范围内，随着温度的升高，介电常数逐渐升高。试样具有正温度系数特征。由表可知，室温下，试样介电常数高，介电损耗低。
表1
综合四个实施例，由表1和图1看出，在-55℃～150℃温度范围内，试样的介电常数都随温度的升高而增加，具有正温度系数特征，主要是由于Na0.2Bi0.6ZrO3具有正电容温度系数，掺杂Yb2O3不仅使Na0.2Bi0.6ZrO3系统的电容温度系数为正，并且使介电常数都较高，介电损耗小。
本发明中使用的测试方法和检测设备如下：
1.介电常数ε和损耗tanδ的测试：采用HEWLETT PACKARD 4278A电容测试仪，测试电容器的电容量C和介电损耗tanδ(测试频率为1MHz)，并通过下面的公式计算介电常数ε：
其中：C-样片的电容量，单位pF；d-样片的厚度，单位cm；D-样片烧结后的直径，单位cm。
2.电容温度系数αc(-55℃～150℃)计算公式：
其中：基准温度t0选取25℃，αc的单位为10-6/℃。
以上对本发明做了示例性的描述，应该说明的是，在不脱离本发明的核心的情况下，任何简单的变形、修改或者其他本领域技术人员能够不花费创造性劳动的等同替换均落入本发明的保护范围。
Claims (6)
1.一种正温度系数陶瓷介质材料，其特征在于：由质量百分比为80-90％的Na0.2Bi0.6ZrO3和10-20％的Yb2O3组成。
2.制备权利要求1所述的一种正温度系数陶瓷介质材料的方法，其特征在于：步骤如下：
(1)将原料Na2CO3、Bi2O3和ZrO2按通式Na0.2Bi0.6ZrO3，进行配料球磨，在3.3kw的普通烘箱中于100℃干燥4-5小时，过120-250孔/cm2分样筛，升温至800℃，保温2-4小时，制得熔块A；
(2)按照质量百分比将10-20％的Yb2O3和80-90％的熔块A进行二次配料，获得配料B；
(3)将配料B加去离子水70ml在转速为400r/min球磨机上球磨8小时，120℃干燥4-5小时，过120-250孔/cm2分样筛，加入质量百分比为配料B的5-8％的黏合剂造粒，压制成生坯压强为8MPa，先按照2℃/min的升温速率升温至400-500℃，然后再按10℃/min的升温速率升温至1100-1150℃保温1小时，冷却后制得陶瓷介质。
3.根据权利要求2所述的制备正温度系数陶瓷介质材料的方法，其特征在于：步骤(1)中在转速为400r/min的球磨机上球磨4-6小时；步骤(1)中升温速率为5-10℃/min。
4.根据权利要求3所述的制备正温度系数陶瓷介质材料的方法，其特征在于：步骤(1)中升温速率为7℃/min。
5.根据权利要求2所述的制备正温度系数陶瓷介质材料的方法，其特征在于：步骤(3)中升温速率为按2℃/min的升温速率升温至450℃，再按10℃/min的升温速率加热至1100-1150℃保温1小时。
6.根据权利要求2所述的制备正温度系数陶瓷介质材料的方法，其特征在于：步骤(3)中的黏合剂为聚乙烯醇或者石蜡。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910483934.8A CN110066172B (zh) | 2019-05-31 | 2019-05-31 | 一种正温度系数陶瓷介质材料及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910483934.8A CN110066172B (zh) | 2019-05-31 | 2019-05-31 | 一种正温度系数陶瓷介质材料及其制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110066172A true CN110066172A (zh) | 2019-07-30 |
| CN110066172B CN110066172B (zh) | 2021-09-03 |
Family
ID=67372570
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910483934.8A Expired - Fee Related CN110066172B (zh) | 2019-05-31 | 2019-05-31 | 一种正温度系数陶瓷介质材料及其制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110066172B (zh) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007031219A (ja) * | 2005-07-28 | 2007-02-08 | Toyota Motor Corp | チタン酸ビスマスナトリウム−ジルコニウムチタン酸バリウム系無鉛圧電セラミック及びその製造方法 |
| CN101595074A (zh) * | 2007-01-29 | 2009-12-02 | 京瓷株式会社 | 电介体瓷器及电容器 |
| CN102245537A (zh) * | 2008-12-12 | 2011-11-16 | 株式会社村田制作所 | 半导体陶瓷以及正特性热敏电阻 |
| CN102992756A (zh) * | 2012-12-11 | 2013-03-27 | 武汉理工大学 | 一种高介电常数x8r型电容器陶瓷材料及其制备方法 |
| US20150353430A1 (en) * | 2013-03-28 | 2015-12-10 | Tdk Corporation | Ceramic composition |
| CN109437896A (zh) * | 2018-11-15 | 2019-03-08 | 太原师范学院 | 一种正温度系数x7r陶瓷介质材料及其制备方法 |
-
2019
- 2019-05-31 CN CN201910483934.8A patent/CN110066172B/zh not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007031219A (ja) * | 2005-07-28 | 2007-02-08 | Toyota Motor Corp | チタン酸ビスマスナトリウム−ジルコニウムチタン酸バリウム系無鉛圧電セラミック及びその製造方法 |
| CN101595074A (zh) * | 2007-01-29 | 2009-12-02 | 京瓷株式会社 | 电介体瓷器及电容器 |
| CN102245537A (zh) * | 2008-12-12 | 2011-11-16 | 株式会社村田制作所 | 半导体陶瓷以及正特性热敏电阻 |
| CN102992756A (zh) * | 2012-12-11 | 2013-03-27 | 武汉理工大学 | 一种高介电常数x8r型电容器陶瓷材料及其制备方法 |
| US20150353430A1 (en) * | 2013-03-28 | 2015-12-10 | Tdk Corporation | Ceramic composition |
| CN109437896A (zh) * | 2018-11-15 | 2019-03-08 | 太原师范学院 | 一种正温度系数x7r陶瓷介质材料及其制备方法 |
Non-Patent Citations (4)
| Title |
|---|
| LILY ET AL.: "Dielectric and impedance study of lead-free ceramic: (Na0.5Bi0.5)ZrO3", 《JOURNAL OF MATERIALS SCIENCE》 * |
| PANUPONG JAIBAN ET AL.: "Fabrication of Bi0.5Na0.5ZrO3 Powder by Mixed Oxide Method", 《MATERIALS SCIENCE FORUM》 * |
| 任少凯等: "阻抗谱研究Yb3+ 掺杂( Bi0.5 Na0.5", 《电子元件与材料》 * |
| 赵旭梅: "元素非计量比对Na0.5Bi0.5TiO3基无铅陶瓷结构与电学性能的影响", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110066172B (zh) | 2021-09-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102199035B (zh) | X9r型陶瓷电容器介质材料及其制备方法 | |
| CN101781115B (zh) | X8r型多层陶瓷电容器介质材料及制备方法 | |
| CN106699150B (zh) | 一种低温烧结低介c0g微波介质材料及其制备方法 | |
| CN111943666A (zh) | 一种温度稳定型陶瓷介质材料及其制备方法 | |
| CN106892659A (zh) | 一种抗还原巨介电常数多层陶瓷电容器介质材料 | |
| CN107512906A (zh) | 一种抗还原x9r型陶瓷电容器介质材料及其制备方法 | |
| CN103408301A (zh) | 一种超高压陶瓷电容器介质及其制备方法 | |
| CN105732020A (zh) | 一种巨介电、低损耗二氧化钛基复合陶瓷的制备方法 | |
| CN105565799A (zh) | 一种低损耗温度稳定型高频介质陶瓷 | |
| CN100359612C (zh) | 一种中低温烧结高压陶瓷电容器介质 | |
| CN103408302A (zh) | 一种高介高温度稳定陶瓷电容器介质及其制备方法 | |
| CN109626999A (zh) | 一种负温度系数陶瓷介质材料及其制备方法 | |
| CN103113100B (zh) | 一种高温度稳定陶瓷电容器介质 | |
| CN104310986A (zh) | 一种高介电常数温度稳定型陶瓷电容器介质材料 | |
| CN106747417A (zh) | 一种ltcc低频介质陶瓷电容器材料及其制备方法 | |
| CN101030478B (zh) | 一种高介金属-电介质复合陶瓷电容器介质及其制备方法 | |
| CN109437896A (zh) | 一种正温度系数x7r陶瓷介质材料及其制备方法 | |
| CN109081693A (zh) | 一种高介电x8r陶瓷介质材料及其制备方法 | |
| CN110066172A (zh) | 一种正温度系数陶瓷介质材料及其制备方法 | |
| CN115784741B (zh) | 一种具有超宽温度稳定性的铌酸钾钠基介质陶瓷材料及其制备方法 | |
| CN101908415B (zh) | X8r特性片式多层陶瓷电容器的制备方法 | |
| CN100434394C (zh) | B位先驱体掺杂改性的钛酸钡基金属复合陶瓷及制备方法 | |
| CN109987930A (zh) | 低温烧结微波介质材料 | |
| CN106145932B (zh) | 一种高介电常数的多层陶瓷电容器介质材料及其制备方法 | |
| CN110078495A (zh) | 介电常数可调的宽温域介质陶瓷材料 |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210903 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |