CN114180957B - 一种微波介质陶瓷及其制备方法与应用 - Google Patents

一种微波介质陶瓷及其制备方法与应用 Download PDF

Info

Publication number
CN114180957B
CN114180957B CN202111392509.1A CN202111392509A CN114180957B CN 114180957 B CN114180957 B CN 114180957B CN 202111392509 A CN202111392509 A CN 202111392509A CN 114180957 B CN114180957 B CN 114180957B
Authority
CN
China
Prior art keywords
dielectric ceramic
microwave dielectric
crystal phase
equal
preparation
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.)
Active
Application number
CN202111392509.1A
Other languages
English (en)
Other versions
CN114180957A (zh
Inventor
吴纪锐
莫方策
董水友
宋永生
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.)
Guangdong Fenghua Advanced Tech Holding Co Ltd
Original Assignee
Guangdong Fenghua Advanced Tech Holding Co Ltd
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 Guangdong Fenghua Advanced Tech Holding Co Ltd filed Critical Guangdong Fenghua Advanced Tech Holding Co Ltd
Priority to CN202111392509.1A priority Critical patent/CN114180957B/zh
Publication of CN114180957A publication Critical patent/CN114180957A/zh
Application granted granted Critical
Publication of CN114180957B publication Critical patent/CN114180957B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

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
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
    • 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
    • C04B2235/3206—Magnesium 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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
    • 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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • 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
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
    • C04B2235/3267—MnO2
    • 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
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3279—Nickel oxides, nickalates, 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
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • 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
    • C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
    • 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
    • C04B2235/02—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
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/608—Green bodies or pre-forms with well-defined density
    • 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
    • C04B2235/6567—Treatment time
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

本发明公开了一种微波介质陶瓷及其制备方法与应用。微波介质陶瓷包括主晶相，组成表达式为aMgTiO3‑bCaTiO3‑cMg2SiO4，0.4≤a≤0.6，0≤c≤0.06，0≤b≤0.053，且b和c不同时为零，a、b和c为化学计量数。微波介质陶瓷主晶相稳定可控，性能稳定；晶粒细小、均匀、致密，活性高，无杂相生成，制造的元件性能稳定，符合通讯电子类产品要求；微波介质陶瓷性能可通过控制晶相成分进行调整；一次性配料即可直接达到晶相设计要求；制备工艺简单，降低了预烧温度、烧结温度和保温时间，节约能源；制备方法为成熟的量产工艺，解决了镁钛钙体系微波陶瓷粉量产应用过程中生坯密度不足的问题。

Description

一种微波介质陶瓷及其制备方法与应用
技术领域
本发明涉及微波介质陶瓷技术领域，尤其涉及一种微波介质陶瓷及其制备方法与应用。
背景技术
微波介质陶瓷是指应用于特定微波频段(主要在300MHz～30GHz)电路中的电介质材料，具有低损耗、高温度稳定性的特点，被广泛应用于个人便携式移动电话、微波基站、车载电话、卫星通讯、军用雷达等众多领域，是用作谐振器、滤波器介质导波回路等重要元器件的关键材料。但现有的微波介质陶瓷大部分采用较高的烧结温度，且谐振频率温度系数不近零，或者采用贵重的金属元素，大大增加了生产成本，限制了移动通信等领域的微波介质器件的开发利用。
镁钛系微波介质陶瓷是近年来开发的新型微波介质陶瓷，以偏钛酸镁为主晶相，抑制杂相的生成，可实现近零的温度系数的产品的制备，易实现大批量稳定生产，具有较好的微波介电性能、稳定性和成本优势，应用前景广泛。
专利CN108033786A的微波介质陶瓷以MgTiO3与Mg2TiO4为基础，采用不同比例的MgTiO3与Mg2TiO4进行复合，其中，0.48MgTiO3-0.52Mg2TiO4陶瓷在1360℃烧结时得到了微波介电性能最佳的陶瓷：相对介电常数为16.43，Q×f值为219423GHz，谐振频率温度系数为-49.2ppm/℃。此方案的谐振频率温度系数偏离0过多，且直接配比氧化镁和二氧化钛无法精确控制生成MgTiO3（偏钛酸镁）与Mg2TiO4（正钛酸镁）的晶相比例，电性能无法稳定，无法应用于工业生产。CN103641469A和CN103319166A公开了以钛酸镁、硅酸镁、钛酸钙为主晶相的微波介质陶瓷材料，有良好的介电性能，近零的谐振频率温度系数，但是在工业生产应用时，存在干压成型低压条件下生坯密度不足的问题，无法满足微波元器件的成型要求。
发明内容
本发明的首要目的在于克服现有技术的缺点与不足，提供一种微波介质陶瓷。
本发明的另一目的在于提供上述微波介质陶瓷的制备方法。
本发明的再一目的在于提供上述微波介质陶瓷的应用。
本发明的目的通过下述技术方案实现：一种微波介质陶瓷，包括主晶相，所述主晶相的组成表达式为aMgTiO3-bCaTiO3-cMg2SiO4,0.4≤a≤0.6，0≤b≤0.053，0≤c≤0.06，且b和c不同时为零，a、b和c为化学计量数。
优选地，所述主晶相组成表达式为0.58MgTiO3-0.046CaTiO3-0.026MgSiO4。
优选地，所述微波介质陶瓷的组分中还包括改性剂、分散剂、粘合剂、润滑剂。
优选地，所述改性剂、分散剂、粘合剂、润滑剂的用量按其占主晶相的质量百分比计，分别为：0.4%-5%、0.1-1%、1%-3.5%、0.1-1%。
优选地，所述改性剂为MnO2、Al2O3、Nb2O5、Ni2O3、CeO2中一种或几种；更优选地，为MnO2与Ni2O3中至少一种。
优选地，所述分散剂为聚乙烯醇。
优选地，所述粘合剂为聚乙烯醇树脂、甲基纤维素和聚丙烯酸树脂中至少一种；更优选地，为聚乙烯醇树脂和聚丙烯酸树脂。
优选地，所述润滑剂为聚乙烯羧酸。
上述微波介质陶瓷的制备方法，包括以下步骤：
（1）按照组成表达式中的化学计量数称取氧化镁、碳酸钙、二氧化钛、二氧化硅，与改性剂、分散剂混合，球磨，砂磨，烘干，过筛，得到粉料；
（2）对步骤（1）所述粉料进行1000℃-1200℃预烧1-3h，冷却后再进行二次球磨和砂磨，使得浆料的固含量达到45%-65%，粒度和比表面积分别达到1.2µm-1.5µm、2m²/g-4m²/g；
（3）将粘合剂与步骤（2）所述浆料搅拌，再与润滑剂搅拌，干燥，得到造粒粉；所述造粒粉含水率为0.30%-0.50%，松装密度为1.10-1.30g/cm3，安息角为26°-29°，中位粒径为50-80μm；
（4）将步骤（3）所述造粒粉干压成型，350-500℃保持2-3h，1250-1400℃烧结2-4小时，得到微波介质陶瓷。
优选地，步骤（1）所述球磨为湿法球磨。
优选地，步骤（1）所述砂磨为砂磨至粒度D50为0.4µm-0.6µm。
优选地，步骤（1）所述打粉过筛的目数为40-60目。
优选地，步骤（2）所述预烧的升温速率为3-6℃/min。
优选地，步骤（3）所述搅拌均为采用搅拌机，30Hz电机转速下搅拌0.5-3h；更优选地，为30Hz电机转速下搅拌1h。
优选地，步骤（3）所述干燥为离心雾化干燥。
优选地，步骤（4）所述干压成型采用的压力为8-12Mpa。
优选地，步骤（4）所述烧结的温度为1350℃。
上述微波介质陶瓷在制备微波元器件中的应用。
与现有技术相比，本发明具有以下有益效果：
（1）本发明通过一次性配料即可以直接达到晶相设计要求，不需要二次配料。晶粒细小、均匀、致密，活性高，无杂相生成，该材料所制造的元件性能稳定，符合通讯电子类产品要求。
（2）本发明的制备工艺简单，与现有技术比较，进一步降低了预烧温度、烧结温度和保温时间，可以在大量生产时缩短生产周期，节约能源。
（3）本发明采用的原料为常见的电子材料，无贵金属无环境有害物质参与，绿色环保。
（4）本发明的微波介质陶瓷主晶相稳定可控，没有额外的相生成，性能稳定，介电常数为19-22，品质因数>55000GHz，谐振频率温度系数为（25℃-85℃）-10-+10ppm/℃。
（5）本发明的微波介质陶瓷性能可通过控制晶相成分进行调整。
（6）本发明的制备方法为成熟的量产工艺，解决了镁钛钙体系微波陶瓷粉量产应用过程中存在的生坯密度不足的问题。
附图说明
图1为实施例1微波介质陶瓷的X射线衍射图谱。
图2为实施例1微波介质陶瓷的扫描电子显微镜图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1-10
1）按组成表达式aMgTiO3-bCaTiO3-cMgSiO4的化学计量数称量纯度为99.8%的氧化镁、碳酸钙、二氧化钛、二氧化硅，加入改性剂（MnO2、Ni2O3的混合物，二者摩尔比为1:1）和分散剂聚乙烯醇，湿法球磨，得到一次球磨后的原料，再进行一次砂磨，控制粒度D50为0.5µm；
2）将一次砂磨后的原料烘干并过60目筛，得到粉料；
3）对粉料进行预烧处理，温度为1100℃，时间为2h，升温速率为5℃/min，得到预烧后的粉料；
4）对预烧后的粉料进行二次球磨，然后进行二次砂磨，得到粒度为1.2µm、比表面为3m²/g的浆料，其固含量为50%；
5）按重量称取粘合剂，与二次砂磨后的浆料在搅拌机（30Hz）中搅拌1小时，再加入润滑剂搅拌1h；
6）在离心雾化干燥器干燥，得到造粒粉（含水率为0.50%，松装密度为1.2g/cm3，安息角为28°，中位粒径为60μm）。
7）将造粒粉在10MPa压力下干压成型成圆柱状块体，在400℃下保温3h，然后在1300～1380℃下烧结2h，得到微波介质陶瓷。
8）将所得微波介质陶瓷采用网络分析仪(Agilent 5071C)及相关配套夹具测试其微波介电性能。实施例1的X射线衍射（XRD）图谱和扫描电子显微镜（SEM）图见图1和图2。
表1实施例1-10中各物质及用量、材料性能
如表1所示，实施例1-10得到的微波介质陶瓷的介电常数（Er）为19-22，品质因数（Qf）大于50000GHz，谐振频率温度系数（TE）在-10至10ppm/℃之间。图1和图2可以看出，材料晶体细小、均匀、致密、活性高、无杂相。
对比例
将实施例1中的粘合剂、润滑剂替换为其他种类，生坯密度见表2。
表2
如表2所示，实施例1中加入分散剂、粘合剂、润滑剂，进行生坯密度的调整，发现聚乙烯醇作为分散剂，聚丙烯树脂+聚乙烯醇树脂为粘合剂，聚乙烯羧酸为润湿剂为最优组合。
以上所述是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也视为本发明的保护范围。

Claims (5)

1.一种微波介质陶瓷的制备方法，其特征在于，包括以下步骤：
（1）按照微波介质陶瓷主晶相的组成表达式中的化学计量数称取氧化镁、碳酸钙、二氧化钛、二氧化硅，与改性剂、分散剂混合，球磨，砂磨，烘干，过筛，得到粉料；
（2）对步骤（1）所述粉料进行1000℃-1200℃预烧1-3h，冷却后再进行二次球磨和砂磨，使得浆料的固含量达到45%-65%，粒度和比表面积分别达到1.2µm-1.5µm、2m²/g-4m²/g；
（3）将粘合剂与步骤（2）所述浆料搅拌，再与润滑剂搅拌，干燥，得到造粒粉；所述造粒粉含水率为0.30%-0.50%，松装密度为1.10-1.30g/cm3，安息角为26°-29°，中位粒径为50-80μm；
（4）将步骤（3）所述造粒粉干压成型，350-500℃保持2-3h，1250-1400℃烧结2-4小时，得到微波介质陶瓷；
所述微波介质陶瓷的主晶相的组成表达式为aMgTiO3-bCaTiO3-cMg2SiO4,0.4≤a≤0.6，0≤b≤0.053，0≤c≤0.06，且b和c不同时为零，a、b和c为化学计量数；
所述改性剂为MnO2与Ni2O3的混合物；
所述分散剂为聚乙烯醇；
所述粘合剂为聚乙烯醇树脂和聚丙烯酸树脂的混合物；
所述润滑剂为聚乙烯羧酸。
2.根据权利要求1所述微波介质陶瓷的制备方法，其特征在于，所述主晶相的组成表达式为0.58MgTiO3-0.046CaTiO3-0.026MgSiO4。
3.根据权利要求1所述微波介质陶瓷的制备方法，其特征在于，所述改性剂、分散剂、粘合剂、润滑剂的用量按其占主晶相的质量百分比计，分别为：0.4%-5%、0.1-1%、1%-3.5%、0.1-1%。
4.根据权利要求1所述微波介质陶瓷的制备方法，其特征在于，
步骤（1）所述砂磨为砂磨至粒度D50为0.4µm-0.6µm；
步骤（1）所述过筛的目数为40-60目；
步骤（4）所述干压成型采用的压力为8-12Mpa；
步骤（4）所述烧结的温度为1350℃。
5.根据权利要求1所述微波介质陶瓷的制备方法，其特征在于，
步骤（1）所述球磨为湿法球磨；
步骤（2）所述预烧的升温速率为3-6℃/min；
步骤（3）所述搅拌均为采用搅拌机，30Hz电机转速下搅拌0.5-3h；
步骤（3）所述干燥为离心雾化干燥。
CN202111392509.1A 2021-11-23 2021-11-23 一种微波介质陶瓷及其制备方法与应用 Active CN114180957B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111392509.1A CN114180957B (zh) 2021-11-23 2021-11-23 一种微波介质陶瓷及其制备方法与应用

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111392509.1A CN114180957B (zh) 2021-11-23 2021-11-23 一种微波介质陶瓷及其制备方法与应用

Publications (2)

Publication Number Publication Date
CN114180957A CN114180957A (zh) 2022-03-15
CN114180957B true CN114180957B (zh) 2023-05-09

Family

ID=80541218

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111392509.1A Active CN114180957B (zh) 2021-11-23 2021-11-23 一种微波介质陶瓷及其制备方法与应用

Country Status (1)

Country Link
CN (1) CN114180957B (zh)

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1212442A (zh) * 1997-09-19 1999-03-31 广东肇庆风华电子工程开发有限公司 中温烧结多层陶瓷电容器用低介微波介质材料
JP4004046B2 (ja) * 2003-03-17 2007-11-07 Ｔｄｋ株式会社 誘電体磁器組成物及びそれを用いた誘電体共振器
CN103319166A (zh) * 2013-05-28 2013-09-25 电子科技大学 一种微波陶瓷介质材料及其制备方法
CN103641469B (zh) * 2013-12-02 2015-11-25 电子科技大学 一种低损耗微波介质陶瓷材料及其制备方法
TWI592384B (zh) * 2016-05-17 2017-07-21 Low temperature co-fired microwave dielectric ceramic material and its preparation method

Also Published As

Publication number Publication date
CN114180957A (zh) 2022-03-15

Similar Documents

Publication Publication Date Title
CN107010942B (zh) 一种高q值通信用陶瓷介质谐振器
CN104310980A (zh) 一种微波介质陶瓷材料及其制备方法
CN111763083B (zh) 一种低温烧结型超低损耗微波介电陶瓷及其制备方法和应用
CN111099892A (zh) 一种钛酸钡基两相复合微波介质陶瓷材料及其制备方法
CN111592348A (zh) 一种具有优异温度稳定性的低介电常数微波介质陶瓷及其制备方法
CN110423117A (zh) 一种高q值微波介质陶瓷材料及其制备方法
CN107188557B (zh) 一种微波介质陶瓷材料及其制备方法
CN113105231B (zh) 一种微波介质陶瓷材料及其制备方法
CN114394827B (zh) 一种低介电常数硅酸盐微波介质陶瓷及其制备方法
CN105254293A (zh) 一种微波介质陶瓷材料及其制备方法
CN111004030B (zh) 一种MgTiO3基微波介质陶瓷及其制备方法
WO2019126969A1 (zh) 一种介质陶瓷材料及其制备方法
CN111925207B (zh) 一种Mg3B2O6-Ba3(VO4)2复合陶瓷材料及制备方法
CN113336539A (zh) 微波介质陶瓷材料、制备方法及应用
CN114180956A (zh) 高介电常数5g波导用微波介质陶瓷及其制备方法和应用
CN103467084B (zh) 一种高介电常数锂铌钛系低温烧结陶瓷及其制备方法
CN114180957B (zh) 一种微波介质陶瓷及其制备方法与应用
CN107253856A (zh) 一种近零谐振频率温度系数的微波介质材料及其制备方法
CN110845226A (zh) 一种微波介质陶瓷材料SrGa2O4及其制备方法
CN111908897A (zh) MgO基微波陶瓷介质材料及其制备方法
CN111018524B (zh) 一种低损耗三方晶系钨酸盐基微波介质陶瓷及其制备方法
CN110734284A (zh) 一种中介高q微波介质陶瓷材料及其制备方法
CN114736012B (zh) 具有超高q值的低介微波介质陶瓷及其ltcc材料
CN113387695A (zh) 一种5g通信用低介高品质微波介质陶瓷及其制备方法
CN105294103B (zh) 一种钒基温度稳定型微波介质陶瓷及其制备方法

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