[go: up one dir, main page]

CN110845226A - Microwave dielectric ceramic material SrGa2O4And method for preparing the same - Google Patents

Microwave dielectric ceramic material SrGa2O4And method for preparing the same Download PDF

Info

Publication number
CN110845226A
CN110845226A CN201911198610.6A CN201911198610A CN110845226A CN 110845226 A CN110845226 A CN 110845226A CN 201911198610 A CN201911198610 A CN 201911198610A CN 110845226 A CN110845226 A CN 110845226A
Authority
CN
China
Prior art keywords
srga
ceramic material
microwave dielectric
dielectric ceramic
sintering
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
CN201911198610.6A
Other languages
Chinese (zh)
Inventor
刘兵
黄玉辉
吴施熠徽
宋开新
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.)
Hangzhou Electronic Science and Technology University
Original Assignee
Hangzhou Electronic Science and Technology 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 Hangzhou Electronic Science and Technology University filed Critical Hangzhou Electronic Science and Technology University
Priority to CN201911198610.6A priority Critical patent/CN110845226A/en
Publication of CN110845226A publication Critical patent/CN110845226A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • 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
    • 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
    • C04B2235/3213Strontium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5427Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
    • 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
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding
    • 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
    • C04B2235/65Aspects 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
    • 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
    • C04B2235/65Aspects 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
    • C04B2235/6562Heating rate
    • 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
    • C04B2235/65Aspects 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
    • C04B2235/6565Cooling rate
    • 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
    • C04B2235/65Aspects 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
    • C04B2235/6567Treatment time

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Insulating Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

本发明属于陶瓷材料技术领域,具体涉及一种具有低介电常数和高品质因数的微波介质陶瓷材料SrGa2O4及其制备方法,主要原料为SrCO3、Ga2O3高纯粉末,制备方法主要包括:配料、一次球磨、预烧、二次球磨、造粒压片、烧结。通过调控制备工艺和烧结温度获得具有优异微波介电性能的低介电常数微波介质陶瓷材料SrGa2O4,在未来毫米波段无线通讯技术领域有极大的应用价值。

Figure 201911198610

The invention belongs to the technical field of ceramic materials, and in particular relates to a microwave dielectric ceramic material SrGa 2 O 4 with low dielectric constant and high quality factor and a preparation method thereof. The main raw materials are SrCO 3 and Ga 2 O 3 high-purity powder. The method mainly includes: batching, primary ball milling, pre-sintering, secondary ball milling, granulation and tableting, and sintering. The low dielectric constant microwave dielectric ceramic material SrGa 2 O 4 with excellent microwave dielectric properties can be obtained by adjusting the preparation process and sintering temperature, which has great application value in the field of future millimeter wave band wireless communication technology.

Figure 201911198610

Description

一种微波介质陶瓷材料SrGa2O4及其制备方法A kind of microwave dielectric ceramic material SrGa2O4 and preparation method thereof

技术领域technical field

本发明属于陶瓷材料技术领域,具体涉及一种具有低介电常数和高品质因数的微波介质陶瓷材料SrGa2O4及其制备方法。The invention belongs to the technical field of ceramic materials, in particular to a microwave dielectric ceramic material SrGa 2 O 4 with low dielectric constant and high quality factor and a preparation method thereof.

背景技术Background technique

随着无线通讯技术如手机通信、WIFI、卫星与雷达通信等逐渐朝亚毫米波-毫米波段方向发展,无线通讯系统中作为滤波器、谐振器、振荡器等关键元器件的微波陶瓷材料成为面向毫米波通信发展的关键材料。不同于2G/3G/4G通讯工作在6GHz频段以下,未来亚毫米波(24GHz-30GHz)与毫米波段(60GHz-78GHz)通讯为保证极快的信号传播速度,要求信号延迟时间低于1毫秒。因此,在毫米波通讯元器件中便要求微波介质陶瓷具有尽可能低的介电常数(εr<10)以提高微波器件信号响应、降低微波信号传输的延迟;同时,微波陶瓷需要具备高Qf值(Qf>20000GHz)以增强器件的选频特性与降低能量传递损耗。近年来,随着5G通讯研究与产业布局的推进,(亚)毫米波通信电路中高端元器件的需求量急剧增大。为了促进信息技术的发展,开发出信号传输、响应速度快,温度稳定性强,信号传输质量高、传输损耗小、频率选择性好的低介电常数微波介质陶瓷,已经成为各国通讯领域研究的重要课题。With the gradual development of wireless communication technologies such as mobile phone communication, WIFI, satellite and radar communication, etc. towards the sub-millimeter wave-millimeter wave band, microwave ceramic materials as key components such as filters, resonators, and oscillators in wireless communication systems have become a Key materials for the development of millimeter-wave communications. Different from 2G/3G/4G communication working in the frequency band below 6GHz, in the future submillimeter wave (24GHz-30GHz) and millimeter wave band (60GHz-78GHz) communication, in order to ensure extremely fast signal propagation speed, the signal delay time is required to be less than 1 millisecond. Therefore, microwave dielectric ceramics are required to have the lowest possible dielectric constant ( εr <10) in millimeter-wave communication components to improve the signal response of microwave devices and reduce the delay of microwave signal transmission; at the same time, microwave ceramics need to have high Qf value (Qf>20000GHz) to enhance the frequency selection characteristics of the device and reduce the energy transfer loss. In recent years, with the advancement of 5G communication research and industrial layout, the demand for high-end components in (sub)millimeter wave communication circuits has increased dramatically. In order to promote the development of information technology, the development of low dielectric constant microwave dielectric ceramics with high signal transmission, fast response speed, strong temperature stability, high signal transmission quality, low transmission loss and good frequency selectivity has become a research topic in the field of communication in various countries. important topic.

因此,本领域亟需开发一种新的微波介质陶瓷材料,以丰富(亚)毫米波段无源器件的材料需求。Therefore, there is an urgent need in the art to develop a new microwave dielectric ceramic material to enrich the material requirements of passive devices in the (sub) millimeter waveband.

发明内容SUMMARY OF THE INVENTION

针对现有信息通信技术领域向亚毫米波-毫米波高频通讯方向发展的需要,本发明提供一种具有低介电常数和高品质因数的微波介质陶瓷材料SrGa2O4及其制备方法。Aiming at the needs of the existing information communication technology field developing towards submillimeter wave-millimeter wave high-frequency communication, the present invention provides a microwave dielectric ceramic material SrGa 2 O 4 with low dielectric constant and high quality factor and a preparation method thereof.

为了达到上述发明目的,本发明采用以下技术方案:In order to achieve the above-mentioned purpose of the invention, the present invention adopts the following technical solutions:

一种微波介质陶瓷材料SrGa2O4的制备方法,包括以下步骤:A preparation method of microwave dielectric ceramic material SrGa 2 O 4 , comprising the following steps:

(1)配料:将原料SrCO3、Ga2O3按照SrGa2O4的化学计量比1:1进行配比;(1) batching: the raw materials SrCO 3 and Ga 2 O 3 are proportioned according to the stoichiometric ratio of SrGa 2 O 4 1:1;

(2)混料:将配料得到的物料、球磨珠、无水乙醇按照1:4:2.5的质量比置于球磨机中进行湿法球磨,球磨时间为6h,得到泥浆状原料;(2) mixing: the material, ball milling beads and dehydrated alcohol obtained by batching are placed in a ball mill according to the mass ratio of 1:4:2.5 to carry out wet ball milling, and the ball milling time is 6h to obtain mud-like raw materials;

(3)烘干:将步骤(2)的泥浆状原料置入烘箱中烘干至恒重,得到干燥的混合料;(3) drying: the slurry-like raw material of step (2) is placed in an oven and dried to constant weight to obtain a dry mixture;

(4)预烧:将步骤(3)的混合料过筛分散,然后置入高温炉中预烧3h,预烧温度为1000~1100℃,制得SrGa2O4粉体;(4) Pre-sintering: the mixture in step (3) is sieved and dispersed, and then placed in a high-temperature furnace for pre-sintering for 3 hours, and the pre-sintering temperature is 1000-1100° C. to obtain SrGa 2 O 4 powder;

(5)球磨:将步骤(4)的SrGa2O4粉体加入无水乙醇,置于球磨机中研磨6h,形成SrGa2O4浆料;(5) Ball milling: adding the SrGa 2 O 4 powder of step (4) to absolute ethanol, and placing it in a ball mill to grind for 6 hours to form SrGa 2 O 4 slurry;

(6)烘干:将步骤(5)的SrGa2O4浆料置于烘箱中烘干至恒重,得到SrGa2O4化合物粉末;(6) drying: the SrGa 2 O 4 slurry of step (5) is placed in an oven and dried to constant weight to obtain SrGa 2 O 4 compound powder;

(7)造粒:将步骤(6)的SrGa2O4化合物粉末过100目标准筛,取筛下料加入聚乙烯醇溶液,混合均匀后将粉料颗粒过60目标准筛,取筛下料压制成圆柱体生坯;(7) Granulation: pass the SrGa 2 O 4 compound powder of step (6) through a 100-mesh standard sieve, take the sieve material and add it to the polyvinyl alcohol solution, after mixing evenly, pass the powder particles through a 60-mesh standard sieve, take out the sieve The material is pressed into a cylindrical green body;

(8)排胶:将圆柱体生坯置于高温炉中以5℃/min的速度升温至650℃,保温2h;(8) Debinding: place the green cylindrical body in a high-temperature furnace to heat up to 650°C at a rate of 5°C/min, and keep the temperature for 2h;

(9)烧结:将排胶处理后的圆柱体生坯进行烧结处理,得到微波介质陶瓷材料SrGa2O4(9) Sintering: sintering the green cylindrical body after the debinding treatment to obtain the microwave dielectric ceramic material SrGa 2 O 4 .

作为优选方案,所述烧结处理的工艺包括:以5℃/min的速度将温度升至1200~1300℃烧结3h,然后以1℃/min的速度降温至1100℃,最后自然降温。As a preferred solution, the sintering process includes: raising the temperature to 1200-1300°C for 3 hours at a rate of 5°C/min, then cooling to 1100°C at a rate of 1°C/min, and finally cooling down naturally.

作为优选方案,所述聚乙烯醇溶液的添加量为SrGa2O4化合物粉末质量的4~6wt%。As a preferred solution, the addition amount of the polyvinyl alcohol solution is 4-6 wt % of the mass of the SrGa 2 O 4 compound powder.

作为优选方案,在配料前,原料分别放入球磨机连续球磨6h以上;其中,原料、氧化锆球磨介质、无水乙醇的质量比为1:4:2.5。As a preferred solution, before batching, the raw materials are respectively put into a ball mill for continuous ball milling for more than 6 hours; wherein, the mass ratio of raw materials, zirconia ball milling medium, and anhydrous ethanol is 1:4:2.5.

作为优选方案,所述步骤(9)之后还包括以下步骤:As a preferred version, the step (9) also includes the following steps after:

(10)后期机械加工:将烧结好的微波介质陶瓷材料SrGa2O4进行研磨抛光。(10) Post-processing: grinding and polishing the sintered microwave dielectric ceramic material SrGa 2 O 4 .

作为优选方案,所述SrCO3的纯度为99.99%,所述Ga2O3的纯度为99.99%。As a preferred solution, the purity of the SrCO 3 is 99.99%, and the purity of the Ga 2 O 3 is 99.99%.

作为优选方案,所述球磨机为行星式球磨机,转速为180r/min。As a preferred solution, the ball mill is a planetary ball mill, and the rotational speed is 180 r/min.

作为优选方案,所述步骤(4)中的预烧温度为1100℃。As a preferred solution, the calcination temperature in the step (4) is 1100°C.

作为优选方案,所述圆柱体生坯的直径为12mm,高度为5mm。As a preferred solution, the cylindrical green body has a diameter of 12 mm and a height of 5 mm.

本发明还提供如上任一方案所述的制备方法制得的微波介质陶瓷材料SrGa2O4,介电常数εr范围为8.97~9.22,品质因数Qf的范围为26136~66000GHz,谐振频率温度系数τf范围为-79.7~-85.6ppm/℃。The invention also provides the microwave dielectric ceramic material SrGa 2 O 4 prepared by the preparation method according to any one of the above schemes, the dielectric constant εr is in the range of 8.97-9.22, the quality factor Qf is in the range of 26136-66000GHz, and the resonant frequency temperature coefficient is in the range of 8.97-9.22. The range of τ f is -79.7~-85.6ppm/°C.

本发明与现有技术相比,有益效果是:Compared with the prior art, the present invention has the following beneficial effects:

本发明的微波介质陶瓷材料SrGa2O4的制备方法为标准的固态反应法,制备方法简单,生产成本较低。The preparation method of the microwave dielectric ceramic material SrGa 2 O 4 of the present invention is a standard solid-state reaction method, the preparation method is simple, and the production cost is low.

通过设计陶瓷的烧结温度,能够稳定得到具有低介电常数(8.97~9.22),高品质因数(26136~66000GHz)的微波介质陶瓷材料SrGa2O4,其谐振频率温度系数τf的范围为-79.7~-85.6ppm/℃。By designing the sintering temperature of the ceramic, the microwave dielectric ceramic material SrGa 2 O 4 with low dielectric constant (8.97~9.22) and high quality factor (26136~66000GHz) can be stably obtained, and the range of its resonant frequency temperature coefficient τ f is - 79.7~-85.6ppm/℃.

附图说明Description of drawings

图1为本发明实施例1制备得到的微波介质陶瓷材料SrGa2O4的XRD图谱;Fig. 1 is the XRD pattern of the microwave dielectric ceramic material SrGa 2 O 4 prepared in Example 1 of the present invention;

图2为本发明实施例1~5制备得到的微波介质陶瓷材料SrGa2O4的介电常数随烧结温度变化曲线图;Fig. 2 is a graph showing the variation of dielectric constant with sintering temperature of the microwave dielectric ceramic material SrGa 2 O 4 prepared in Examples 1-5 of the present invention;

图3为本发明实施例1~5制备得到的微波介质陶瓷材料SrGa2O4的品质因数随烧结温度变化曲线图;FIG. 3 is a graph showing the variation of quality factor with sintering temperature of the microwave dielectric ceramic material SrGa 2 O 4 prepared in Examples 1-5 of the present invention;

图4为本发明实施例1~5制备得到的微波介质陶瓷材料SrGa2O4的谐振频率温度系数随烧结温度变化曲线图。4 is a graph showing the variation of the temperature coefficient of resonance frequency with the sintering temperature of the microwave dielectric ceramic material SrGa 2 O 4 prepared in Examples 1 to 5 of the present invention.

具体实施方式Detailed ways

下面通过具体实施例对本发明的技术方案作进一步描述说明。The technical solutions of the present invention will be further described and illustrated below through specific embodiments.

实施例1:Example 1:

本实施例的微波介质陶瓷材料SrGa2O4的制备方法,包括以下步骤:The preparation method of the microwave dielectric ceramic material SrGa 2 O 4 in this embodiment includes the following steps:

(1)配料:SrCO3(纯度99.99%)、Ga2O3(纯度99.99%)按照SrGa2O4的化学计量1:1进行配比;具体为依次称取10.1492g SrCO3、12.8812g Ga2O3原料。(1) Ingredients: SrCO 3 (purity 99.99%) and Ga 2 O 3 (purity 99.99%) were proportioned according to the stoichiometric 1:1 of SrGa 2 O 4 ; specifically, 10.1492g SrCO 3 and 12.8812g Ga were weighed in turn. 2 O 3 raw material.

(2)混料:将上述混合料倒入球磨机中,按1:4:2.5的质量比分别加入球磨介质和无水乙醇,置于行星式球磨机中,以180r/min的转速球磨6h,得到浆料;(2) Mixing: Pour the above mixture into a ball mill, add ball milling medium and dehydrated ethanol in a mass ratio of 1:4:2.5, place it in a planetary ball mill, and mill it at a rotational speed of 180 r/min for 6 hours to obtain slurry;

(3)烘干:将球磨后的浆料倒出,置入烘箱中于70℃下干燥至恒重,得到干燥的混合料;(3) drying: pour out the ball-milled slurry, put it in an oven and dry to constant weight at 70°C to obtain a dry mixture;

(4)预烧:将上一步得到的干燥混合料在研钵中研磨然后过100目标准筛,分散混合料后,置入高温炉中预烧3h,预烧温度为1100℃,升温速度为5℃/min,使混合料初步反应合成SrGa2O4化合物;(4) Pre-sintering: grind the dry mixture obtained in the previous step in a mortar and then pass through a 100-mesh standard sieve. After dispersing the mixture, put it into a high-temperature furnace for pre-sintering for 3 hours. The pre-sintering temperature is 1100°C, and the heating rate is 5 ℃/min, make the mixture preliminarily react to synthesize SrGa 2 O 4 compound;

(5)球磨:将初步合成的SrGa2O4化合物加入50g无水乙醇置于球磨机中以180r/min的转速研磨6h,形成粒径细化的SrGa2O4化合物;(5) Ball milling: adding 50 g of dehydrated alcohol to the preliminarily synthesized SrGa 2 O 4 compound and placing it in a ball mill to grind for 6 hours at a rotational speed of 180 r/min to form a SrGa 2 O 4 compound with a refined particle size;

(6)烘干:将SrGa2O4化合物浆料取出,置于烘箱中70℃下干燥至恒重,得到初步合成的SrGa2O4化合物;(6) drying: take out the SrGa 2 O 4 compound slurry, and place it in an oven to dry to constant weight at 70° C. to obtain a preliminary synthesized SrGa 2 O 4 compound;

(7)造粒:将上一步得到的恒重SrGa2O4化合物过60目标准筛使颗粒分散均匀,之后按照SrGa2O4化合物的6wt%质量百分比加入聚乙烯醇溶液(PVA)作为粘合剂,混合均匀后,将粉料置于模具中于200Mpa压力下压制成直径为12mm、厚度约为5mm的圆柱体生坯;(7) Granulation: pass the constant weight SrGa 2 O 4 compound obtained in the previous step through a 60-mesh standard sieve to disperse the particles uniformly, and then add a polyvinyl alcohol solution (PVA) as a viscous solution according to the 6wt% mass percentage of the SrGa 2 O 4 compound. Mixture, after mixing evenly, the powder is placed in a mold and pressed into a cylindrical green body with a diameter of 12mm and a thickness of about 5mm under a pressure of 200Mpa;

(8)排胶:将压成的圆柱体置于高温炉中以5℃/min的速度升温至650℃,保温2h以排除圆柱体中的PVA;(8) Debinding: place the pressed cylinder in a high temperature furnace and heat it up to 650°C at a rate of 5°C/min, and keep it for 2 hours to remove PVA in the cylinder;

(9)烧结:烧结:排胶后以5℃/min的速度将温度升至1200℃烧结3h,然后以1℃/min的速度降温至1100℃,最后设置为自然降温;(9) Sintering: Sintering: after debinding, the temperature was raised to 1200°C for 3 hours at a rate of 5°C/min, then cooled to 1100°C at a rate of 1°C/min, and finally set to natural cooling;

(10)后期机械加工:将烧结好的SrGa2O4陶瓷进行研磨抛光,得到表面平整光滑的陶瓷成品。(10) Post-processing: grinding and polishing the sintered SrGa 2 O 4 ceramic to obtain a finished ceramic product with a smooth surface.

如图1为本实施例的微波介质陶瓷材料SrGa2O4的XRD图谱,说明微波介质陶瓷材料为SrGa2O4。以下实施例的XRD图谱同本实施例。As shown in FIG. 1 , the XRD pattern of the microwave dielectric ceramic material SrGa 2 O 4 of the present embodiment indicates that the microwave dielectric ceramic material is SrGa 2 O 4 . The XRD patterns of the following examples are the same as those in this example.

实施例2:Example 2:

本实施例的微波介质陶瓷材料SrGa2O4的制备方法,包括以下步骤:The preparation method of the microwave dielectric ceramic material SrGa 2 O 4 in this embodiment includes the following steps:

(1)配料:SrCO3(纯度99.99%)、Ga2O3(纯度99.99%)按照SrGa2O4的化学计量1:1进行配比;具体为依次称取10.1492g SrCO3、12.8812g Ga2O3原料。(1) Ingredients: SrCO 3 (purity 99.99%) and Ga 2 O 3 (purity 99.99%) were proportioned according to the stoichiometric 1:1 of SrGa 2 O 4 ; specifically, 10.1492g SrCO 3 and 12.8812g Ga were weighed in turn. 2 O 3 raw material.

(2)混料:将上述混合料倒入球磨机中,按1:4:2.5的质量比分别加入球磨介质和无水乙醇,置于行星式球磨机中,以180r/min的转速球磨6h,得到浆料;(2) Mixing: Pour the above mixture into a ball mill, add ball milling medium and dehydrated ethanol in a mass ratio of 1:4:2.5, place it in a planetary ball mill, and mill it at a rotational speed of 180 r/min for 6 hours to obtain slurry;

(3)烘干:将球磨后的浆料倒出,置入烘箱中于70℃下干燥至恒重,得到干燥的混合料;(3) drying: pour out the ball-milled slurry, put it in an oven and dry to constant weight at 70°C to obtain a dry mixture;

(4)预烧:将上一步得到的干燥混合料在研钵中研磨然后过100目标准筛,分散混合料后,置入高温炉中预烧3h,预烧温度为1100℃,升温速度为5℃/min,使混合料初步反应合成SrGa2O4化合物;(4) Pre-sintering: grind the dry mixture obtained in the previous step in a mortar and then pass through a 100-mesh standard sieve. After dispersing the mixture, put it into a high-temperature furnace for pre-sintering for 3 hours. The pre-sintering temperature is 1100°C, and the heating rate is 5 ℃/min, make the mixture preliminarily react to synthesize SrGa 2 O 4 compound;

(5)球磨:将初步合成的SrGa2O4化合物加入50g无水乙醇置于球磨机中以180r/min的转速研磨6h,形成粒径细化的SrGa2O4化合物;(5) Ball milling: adding 50 g of dehydrated alcohol to the preliminarily synthesized SrGa 2 O 4 compound and placing it in a ball mill to grind for 6 hours at a rotational speed of 180 r/min to form a SrGa 2 O 4 compound with a refined particle size;

(6)烘干:将SrGa2O4化合物浆料取出,置于烘箱中70℃下干燥至恒重,得到初步合成的SrGa2O4化合物;(6) drying: take out the SrGa 2 O 4 compound slurry, and place it in an oven to dry to constant weight at 70° C. to obtain a preliminary synthesized SrGa 2 O 4 compound;

(7)造粒:将上一步得到的恒重SrGa2O4化合物过60目标准筛使颗粒分散均匀,按照SrGa2O4化合物的6wt%质量百分比加入聚乙烯醇溶液(PVA)作为粘合剂,混合均匀后,将粉料置于模具中于200Mpa压力下压制成直径为12mm、厚度约为5mm的圆柱体生坯;(7) Granulation: pass the constant weight SrGa 2 O 4 compound obtained in the previous step through a 60-mesh standard sieve to disperse the particles uniformly, and add a polyvinyl alcohol solution (PVA) as a binding agent according to the 6wt% mass percentage of the SrGa 2 O 4 compound. After mixing uniformly, the powder is placed in a mold and pressed into a cylindrical green body with a diameter of 12mm and a thickness of about 5mm under a pressure of 200Mpa;

(8)排胶:将压成的圆柱体置于高温炉中以5℃/min的速度升温至650℃,保温2h以排除圆柱体中的PVA;(8) Debinding: place the pressed cylinder in a high temperature furnace and heat it up to 650°C at a rate of 5°C/min, and keep it for 2 hours to remove PVA in the cylinder;

(9)烧结:烧结:排胶后以5℃/min的速度将温度升至1225℃烧结3h,然后以1℃/min的速度降温至1100℃,最后设置为自然降温;(9) Sintering: Sintering: after debinding, the temperature is raised to 1225°C for 3 hours at a rate of 5°C/min, then cooled to 1100°C at a rate of 1°C/min, and finally set to natural cooling;

(10)后期机械加工:将烧结好的SrGa2O4陶瓷进行研磨抛光,得到表面平整光滑的陶瓷成品。(10) Post-processing: grinding and polishing the sintered SrGa 2 O 4 ceramic to obtain a finished ceramic product with a smooth surface.

实施例3:Example 3:

本实施例的微波介质陶瓷材料SrGa2O4的制备方法,包括以下步骤:The preparation method of the microwave dielectric ceramic material SrGa 2 O 4 in this embodiment includes the following steps:

(1)配料:SrCO3(纯度99.99%)、Ga2O3(纯度99.99%)按照SrGa2O4的化学计量1:1进行配比;具体为依次称取10.1492g SrCO3、12.8812g Ga2O3原料。(1) Ingredients: SrCO 3 (purity 99.99%) and Ga 2 O 3 (purity 99.99%) were proportioned according to the stoichiometric 1:1 of SrGa 2 O 4 ; specifically, 10.1492g SrCO 3 and 12.8812g Ga were weighed in turn. 2 O 3 raw material.

(2)混料:将上述混合料倒入球磨机中,按1:4:2.5的质量比分别加入球磨介质和无水乙醇,置于行星式球磨机中,以180r/min的转速球磨6h,得到浆料;(2) Mixing: Pour the above mixture into a ball mill, add ball milling medium and dehydrated ethanol in a mass ratio of 1:4:2.5, place it in a planetary ball mill, and mill it at a rotational speed of 180 r/min for 6 hours to obtain slurry;

(3)烘干:将球磨后的浆料倒出,置入烘箱中于70℃下干燥至恒重,得到干燥的混合料;(3) drying: pour out the ball-milled slurry, put it in an oven and dry to constant weight at 70°C to obtain a dry mixture;

(4)预烧:将上一步得到的干燥混合料在研钵中研磨然后过100目标准筛,分散混合料后,置入高温炉中预烧3h,预烧温度为1100℃,升温速度为5℃/min,使混合料初步反应合成SrGa2O4化合物;(4) Pre-sintering: grind the dry mixture obtained in the previous step in a mortar and then pass through a 100-mesh standard sieve. After dispersing the mixture, put it into a high-temperature furnace for pre-sintering for 3 hours. The pre-sintering temperature is 1100°C, and the heating rate is 5 ℃/min, make the mixture preliminarily react to synthesize SrGa 2 O 4 compound;

(5)球磨:将初步合成的SrGa2O4化合物加入50g无水乙醇置于球磨机中以180r/min的转速研磨6h,形成粒径细化的SrGa2O4化合物;(5) Ball milling: adding 50 g of dehydrated alcohol to the preliminarily synthesized SrGa 2 O 4 compound and placing it in a ball mill to grind for 6 hours at a rotational speed of 180 r/min to form a SrGa 2 O 4 compound with a refined particle size;

(6)烘干:将SrGa2O4化合物浆料取出,置于烘箱中70℃下干燥至恒重,得到初步合成的SrGa2O4化合物;(6) drying: take out the SrGa 2 O 4 compound slurry, and place it in an oven to dry to constant weight at 70° C. to obtain a preliminary synthesized SrGa 2 O 4 compound;

(7)造粒:将上一步得到的恒重SrGa2O4化合物过60目标准筛使颗粒分散均匀,按照SrGa2O4化合物的6wt%质量百分比加入聚乙烯醇溶液(PVA)作为粘合剂,混合均匀后,将粉料置于模具中于200Mpa压力下压制成直径为12mm、厚度约为5mm的圆柱体生坯;(7) Granulation: pass the constant weight SrGa 2 O 4 compound obtained in the previous step through a 60-mesh standard sieve to disperse the particles uniformly, and add a polyvinyl alcohol solution (PVA) as a binding agent according to the 6wt% mass percentage of the SrGa 2 O 4 compound. After mixing uniformly, the powder is placed in a mold and pressed into a cylindrical green body with a diameter of 12mm and a thickness of about 5mm under a pressure of 200Mpa;

(8)排胶:将压成的圆柱体置于高温炉中以5℃/min的速度升温至650℃,保温2h以排除圆柱体中的PVA;(8) Debinding: place the pressed cylinder in a high temperature furnace and heat it up to 650°C at a rate of 5°C/min, and keep it for 2 hours to remove PVA in the cylinder;

(9)烧结:烧结:排胶后以5℃/min的速度将温度升至1250℃烧结3h,然后以1℃/min的速度降温至1100℃,最后设置为自然降温;(9) Sintering: Sintering: after debinding, the temperature was raised to 1250°C for 3 hours at a rate of 5°C/min, then cooled to 1100°C at a rate of 1°C/min, and finally set to natural cooling;

(10)后期机械加工:将烧结好的SrGa2O4陶瓷进行研磨抛光,得到表面平整光滑的陶瓷成品。(10) Post-processing: grinding and polishing the sintered SrGa 2 O 4 ceramic to obtain a finished ceramic product with a smooth surface.

实施例4:Example 4:

本实施例的微波介质陶瓷材料SrGa2O4的制备方法,包括以下步骤:The preparation method of the microwave dielectric ceramic material SrGa 2 O 4 in this embodiment includes the following steps:

(1)配料:SrCO3(纯度99.99%)、Ga2O3(纯度99.99%)按照SrGa2O4的化学计量1:1进行配比;具体为依次称取10.1492g SrCO3、12.8812g Ga2O3原料。(1) Ingredients: SrCO 3 (purity 99.99%) and Ga 2 O 3 (purity 99.99%) were proportioned according to the stoichiometric 1:1 of SrGa 2 O 4 ; specifically, 10.1492g SrCO 3 and 12.8812g Ga were weighed in turn. 2 O 3 raw material.

(2)混料:将上述混合料倒入球磨机中,按1:4:2.5的质量比分别加入球磨介质和无水乙醇,置于行星式球磨机中,以180r/min的转速球磨6h,得到浆料;(2) Mixing: Pour the above mixture into a ball mill, add ball milling medium and dehydrated ethanol in a mass ratio of 1:4:2.5, place it in a planetary ball mill, and mill it at a rotational speed of 180 r/min for 6 hours to obtain slurry;

(3)烘干:将球磨后的浆料倒出,置入烘箱中于70℃下干燥至恒重,得到干燥的混合料;(3) drying: pour out the ball-milled slurry, put it in an oven and dry to constant weight at 70°C to obtain a dry mixture;

(4)预烧:将上一步得到的干燥混合料在研钵中研磨然后过100目标准筛,分散混合料后,置入高温炉中预烧3h,预烧温度为1100℃,升温速度为5℃/min,使混合料初步反应合成SrGa2O4化合物;(4) Pre-sintering: grind the dry mixture obtained in the previous step in a mortar and then pass through a 100-mesh standard sieve. After dispersing the mixture, put it into a high-temperature furnace for pre-sintering for 3 hours. The pre-sintering temperature is 1100°C, and the heating rate is 5 ℃/min, make the mixture preliminarily react to synthesize SrGa 2 O 4 compound;

(5)球磨:将初步合成的SrGa2O4化合物加入50g无水乙醇置于球磨机中以180r/min的转速研磨6h,形成粒径细化的SrGa2O4化合物;(5) Ball milling: adding 50 g of dehydrated alcohol to the preliminarily synthesized SrGa 2 O 4 compound and placing it in a ball mill to grind for 6 hours at a rotational speed of 180 r/min to form a SrGa 2 O 4 compound with a refined particle size;

(6)烘干:将SrGa2O4化合物浆料取出,置于烘箱中70℃下干燥至恒重,得到初步合成的SrGa2O4化合物;(6) drying: take out the SrGa 2 O 4 compound slurry, and place it in an oven to dry to constant weight at 70° C. to obtain a preliminary synthesized SrGa 2 O 4 compound;

(7)造粒:将上一步得到的恒重SrGa2O4化合物过60目标准筛使颗粒分散均匀,按照SrGa2O4化合物的6wt%质量百分比加入聚乙烯醇溶液(PVA)作为粘合剂,混合均匀后,将粉料置于模具中于200Mpa压力下压制成直径为12mm、厚度约为5mm的圆柱体生坯;(7) Granulation: pass the constant weight SrGa 2 O 4 compound obtained in the previous step through a 60-mesh standard sieve to disperse the particles uniformly, and add a polyvinyl alcohol solution (PVA) as a binding agent according to the 6wt% mass percentage of the SrGa 2 O 4 compound. After mixing uniformly, the powder is placed in a mold and pressed into a cylindrical green body with a diameter of 12mm and a thickness of about 5mm under a pressure of 200Mpa;

(8)排胶:将压成的圆柱体置于高温炉中以5℃/min的速度升温至650℃,保温2h以排除圆柱体中的PVA;(8) Debinding: place the pressed cylinder in a high temperature furnace and heat it up to 650°C at a rate of 5°C/min, and keep it for 2 hours to remove PVA in the cylinder;

(9)烧结:烧结:排胶后以5℃/min的速度将温度升至1275℃烧结3h,然后以1℃/min的速度降温至1100℃,最后设置为自然降温;(9) Sintering: Sintering: after debinding, the temperature was raised to 1275°C for 3 hours at a rate of 5°C/min, then cooled to 1100°C at a rate of 1°C/min, and finally set to natural cooling;

(10)后期机械加工:将烧结好的SrGa2O4陶瓷进行研磨抛光,得到表面平整光滑的陶瓷成品。(10) Post-processing machining: grinding and polishing the sintered SrGa 2 O 4 ceramic to obtain a finished ceramic product with a smooth surface.

实施例5:Example 5:

本实施例的微波介质陶瓷材料SrGa2O4的制备方法,包括以下步骤:The preparation method of the microwave dielectric ceramic material SrGa 2 O 4 in this embodiment includes the following steps:

(1)配料:SrCO3(纯度99.99%)、Ga2O3(纯度99.99%)按照SrGa2O4的化学计量1:1进行配比;具体为依次称取10.1492g SrCO3、12.8812g Ga2O3原料。(1) Ingredients: SrCO 3 (purity 99.99%) and Ga 2 O 3 (purity 99.99%) were proportioned according to the stoichiometric 1:1 of SrGa 2 O 4 ; specifically, 10.1492g SrCO 3 and 12.8812g Ga were weighed in turn. 2 O 3 raw material.

(2)混料:将上述混合料倒入球磨机中,按1:4:2.5的质量比分别加入球磨介质和无水乙醇,置于行星式球磨机中,以180r/min的转速球磨6h,得到浆料;(2) Mixing: Pour the above mixture into a ball mill, add ball milling medium and dehydrated ethanol in a mass ratio of 1:4:2.5, place it in a planetary ball mill, and mill it at a rotational speed of 180 r/min for 6 hours to obtain slurry;

(3)烘干:将球磨后的浆料倒出,置入烘箱中于70℃下干燥至恒重,得到干燥的混合料;(3) drying: pour out the ball-milled slurry, put it in an oven and dry to constant weight at 70°C to obtain a dry mixture;

(4)预烧:将上一步得到的干燥混合料在研钵中研磨然后过100目标准筛,分散混合料后,置入高温炉中预烧3h,预烧温度为1100℃,升温速度为5℃/min,使混合料初步反应合成SrGa2O4化合物;(4) Pre-sintering: grind the dry mixture obtained in the previous step in a mortar and then pass through a 100-mesh standard sieve. After dispersing the mixture, put it into a high-temperature furnace for pre-sintering for 3 hours. The pre-sintering temperature is 1100°C, and the heating rate is 5 ℃/min, make the mixture preliminarily react to synthesize SrGa 2 O 4 compound;

(5)球磨:将初步合成的SrGa2O4化合物加入50g无水乙醇置于球磨机中以180r/min的转速研磨6h,形成粒径细化的SrGa2O4化合物;(5) Ball milling: adding 50 g of dehydrated alcohol to the preliminarily synthesized SrGa 2 O 4 compound and placing it in a ball mill to grind for 6 hours at a rotational speed of 180 r/min to form a SrGa 2 O 4 compound with a refined particle size;

(6)烘干:将SrGa2O4化合物浆料取出,置于烘箱中70℃下干燥至恒重,得到初步合成的SrGa2O4化合物;(6) drying: take out the SrGa 2 O 4 compound slurry, and place it in an oven to dry to constant weight at 70° C. to obtain a preliminary synthesized SrGa 2 O 4 compound;

(7)造粒:将上一步得到的恒重SrGa2O4化合物过60目标准筛使颗粒分散均匀,按照SrGa2O4化合物的6wt%质量百分比加入聚乙烯醇溶液(PVA)作为粘合剂,混合均匀后,将粉料置于模具中于200Mpa压力下压制成直径为12mm、厚度约为5mm的圆柱体生坯;(7) Granulation: pass the constant weight SrGa 2 O 4 compound obtained in the previous step through a 60-mesh standard sieve to disperse the particles uniformly, and add a polyvinyl alcohol solution (PVA) as a binding agent according to the 6wt% mass percentage of the SrGa 2 O 4 compound. After mixing uniformly, the powder is placed in a mold and pressed into a cylindrical green body with a diameter of 12mm and a thickness of about 5mm under a pressure of 200Mpa;

(8)排胶:将压成的圆柱体置于高温炉中以5℃/min的速度升温至650℃,保温2h以排除圆柱体中的PVA;(8) Debinding: place the pressed cylinder in a high temperature furnace and heat it up to 650°C at a rate of 5°C/min, and keep it for 2 hours to remove PVA in the cylinder;

(9)烧结:烧结:排胶后以5℃/min的速度将温度升至1300℃烧结3h,然后以1℃/min的速度降温至1100℃,最后设置为自然降温;(9) Sintering: Sintering: after debinding, the temperature was raised to 1300°C for 3 hours at a rate of 5°C/min, then cooled to 1100°C at a rate of 1°C/min, and finally set to natural cooling;

(10)后期机械加工:将烧结好的SrGa2O4陶瓷进行研磨抛光,得到表面平整光滑的陶瓷成品。(10) Post-processing: grinding and polishing the sintered SrGa 2 O 4 ceramic to obtain a finished ceramic product with a smooth surface.

采用Hakki-Coleman提出的介质谐振腔法测试圆柱体陶瓷谐振频率下的微波介电性能,具体的性能参数见图2-4。上述的5个实施例中,实施例1的微波介质陶瓷材料SrGa2O4的介电常数最低,介电常数值为8.97;实施例4微波介质陶瓷材料SrGa2O4的品质因数最高,为66000GHz;实施例1的微波介质陶瓷材料SrGa2O4的谐振频率温度系数为-79.7ppm/℃,稳定性最好。The dielectric resonant cavity method proposed by Hakki-Coleman is used to test the microwave dielectric properties of the cylindrical ceramic at the resonant frequency. The specific performance parameters are shown in Figure 2-4. Among the above five embodiments, the dielectric constant of the microwave dielectric ceramic material SrGa 2 O 4 in Example 1 is the lowest, and the dielectric constant value is 8.97; the quality factor of the microwave dielectric ceramic material SrGa 2 O 4 in Example 4 is the highest, which is 66000GHz; the temperature coefficient of resonance frequency of the microwave dielectric ceramic material SrGa 2 O 4 in Example 1 is -79.7ppm/°C, and the stability is the best.

在上述实施例及其替代方案中,预烧温度还可以为1000℃、1020℃、1050℃、1080℃等。In the above embodiment and its alternatives, the pre-burning temperature can also be 1000°C, 1020°C, 1050°C, 1080°C, and the like.

在上述实施例及其替代方案中,步骤(3)中烘干的温度还可以为60℃、65℃、75℃、80℃等。In the above embodiment and its alternatives, the drying temperature in step (3) can also be 60°C, 65°C, 75°C, 80°C, and the like.

在上述实施例及其替代方案中,步骤(6)中烘干的温度还可以为60℃、65℃、75℃、80℃等。In the above embodiment and its alternatives, the drying temperature in step (6) can also be 60°C, 65°C, 75°C, 80°C, and the like.

在上述实施例及其替代方案中,步骤(7)中的聚乙烯醇溶液(PVA)的添加量占SrGa2O4化合物的质量百分比还可以为4wt%、4.5wt%、5wt%、5.5wt%等。In the above embodiment and its alternatives, the addition amount of the polyvinyl alcohol solution (PVA) in step (7 ) can also be 4wt%, 4.5wt%, 5wt%, 5.5wt% in the mass percentage of the SrGa2O4 compound %Wait.

在上述实施例及其替代方案中,步骤(7)中的压制的压力还可以为100Mpa、120Mpa、150Mpa、160Mpa、180Mpa等。In the above embodiment and its alternatives, the pressing pressure in step (7) can also be 100Mpa, 120Mpa, 150Mpa, 160Mpa, 180Mpa and the like.

在上述实施例及其替代方案中,在配料前,原料分别放入球磨机连续球磨6h以上;其中,原料、氧化锆球磨介质、无水乙醇的质量比为1:4:2.5,保证原料颗粒的均匀性。In the above embodiment and its alternatives, before batching, the raw materials are put into a ball mill for continuous ball milling for more than 6 hours; wherein, the mass ratio of raw materials, zirconia ball milling media, and absolute ethanol is 1:4:2.5, which ensures that the raw material particles are uniformity.

以上实施例的说明只是用于帮助理解本发明方法及其核心思想。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,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求保护范围内。The descriptions of the above embodiments are only used to help understand the method and the core idea of the present invention. It should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and modifications can also be made to the present invention, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.

Claims (10)

1. Microwave dielectric ceramic material SrGa2O4The preparation method is characterized by comprising the following steps:
(1) preparing materials: raw material SrCO3、Ga2O3According to SrGa2O41: 1, proportioning;
(2) mixing materials: mixing the materials obtained by the ingredients, ball milling beads and absolute ethyl alcohol according to the proportion of 1: 4: 2.5, putting the mixture into a ball mill for wet ball milling for 6 hours to obtain slurry raw materials;
(3) drying: putting the slurry raw material in the step (2) into an oven to be dried to constant weight to obtain a dry mixture;
(4) pre-burning: sieving and dispersing the mixture obtained in the step (3), and then placing the mixture into a high-temperature furnace for presintering for 3 hours, wherein the presintering temperature is 1000-1100 ℃, so as to prepare SrGa2O4Powder;
(5) ball milling: SrGa obtained in the step (4)2O4Adding absolute ethyl alcohol into the powder, and placing the powder in a ball mill for grinding for 6 hours to form SrGa2O4Sizing agent;
(6) drying: SrGa obtained in the step (5)2O4The slurry is placed in an oven to be dried to constant weight to obtain SrGa2O4A compound powder;
(7) and (3) granulation: SrGa obtained in the step (6)2O4Sieving compound powder with a 100-mesh standard sieve, adding the sieved powder into a polyvinyl alcohol solution, uniformly mixing, sieving powder particles with a 60-mesh standard sieve, and pressing the sieved powder into a cylindrical green body;
(8) rubber discharging: placing the cylindrical green body in a high-temperature furnace, heating to 650 ℃ at the speed of 5 ℃/min, and preserving heat for 2 h;
(9) and (3) sintering: sintering the cylindrical green body subjected to the binder removal treatment to obtain the microwave dielectric ceramic material SrGa2O4
2. A microwave dielectric ceramic material SrGa as claimed in claim 12O4The preparation method is characterized in that the sintering treatment process comprises the following steps: and (3) increasing the temperature to 1200-1300 ℃ at the speed of 5 ℃/min, sintering for 3h, then reducing the temperature to 1100 ℃ at the speed of 1 ℃/min, and finally naturally reducing the temperature.
3. A microwave dielectric ceramic material SrGa as claimed in claim 12O4The method for producing (1) is characterized in that the polyvinyl alcohol solution is added in an amount of SrGa2O44-6 wt% of the compound powder.
4. A microwave dielectric ceramic material SrGa as claimed in claim 12O4The preparation method is characterized in that before the burdening, the raw materials are respectively put into a ball mill to be continuously ball-milled for more than 6 hours; wherein the mass ratio of the raw materials, the zirconia ball-milling medium and the absolute ethyl alcohol is 1: 4: 2.5.
5. a microwave dielectric ceramic material SrGa as claimed in claim 12O4The method for preparing (5) is characterized by further comprising the following steps after the step (9):
(10) and (3) later-stage mechanical processing: sintering the microwave dielectric ceramic material SrGa2O4And grinding and polishing.
6. A microwave dielectric ceramic material SrGa as claimed in claim 12O4Characterized in that the SrCO is3Has a purity of 99.99%, the Ga being2O3The purity of (2) was 99.99%.
7. A microwave dielectric ceramic material SrGa as claimed in claim 12O4The preparation method is characterized in that the ball mill is a planetary ball mill, and the rotating speed is 180 r/min.
8. A microwave dielectric ceramic material SrGa as claimed in claim 12O4The production method of (4), wherein the pre-firing temperature in the step (4) is 1100 ℃.
9. A microwave dielectric ceramic material SrGa as claimed in claim 12O4The method for preparing (1), wherein the diameter of the cylindrical green compact is 12mm, and the height is 5 mm.
10. SrGa microwave dielectric ceramic material prepared by the preparation method of any one of claims 1 to 92O4Characterized by a dielectric constant εrThe range is 8.97-9.22, the quality factor Qf is 26136-66000 GHz, and the temperature coefficient of resonance frequency taufThe range is-79.7 to-85.6 ppm/DEG C.
CN201911198610.6A 2019-11-29 2019-11-29 Microwave dielectric ceramic material SrGa2O4And method for preparing the same Pending CN110845226A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911198610.6A CN110845226A (en) 2019-11-29 2019-11-29 Microwave dielectric ceramic material SrGa2O4And method for preparing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911198610.6A CN110845226A (en) 2019-11-29 2019-11-29 Microwave dielectric ceramic material SrGa2O4And method for preparing the same

Publications (1)

Publication Number Publication Date
CN110845226A true CN110845226A (en) 2020-02-28

Family

ID=69606098

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911198610.6A Pending CN110845226A (en) 2019-11-29 2019-11-29 Microwave dielectric ceramic material SrGa2O4And method for preparing the same

Country Status (1)

Country Link
CN (1) CN110845226A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112266232A (en) * 2020-08-03 2021-01-26 杭州电子科技大学 Low-dielectric microwave dielectric ceramic material suitable for 5G millimeter wave communication application and preparation method thereof
CN114988877A (en) * 2022-06-15 2022-09-02 桂林理工大学 A kind of ultra-low loss microwave dielectric ceramic material and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020045532A1 (en) * 2000-05-30 2002-04-18 Yoshihiro Okawa Dielectric ceramics and dielectric resonator
CN101319377A (en) * 2007-06-06 2008-12-10 中国科学院金属研究所 Nano SrAl2O4 material and method for producing the same
CN104449685A (en) * 2013-09-25 2015-03-25 海洋王照明科技股份有限公司 Cerium-doped alkaline earth gallate luminescent material as well as preparation method and application thereof
CN107399966A (en) * 2017-07-28 2017-11-28 江苏大学 Low dielectric microwave dielectric material of a kind of high-performance and preparation method thereof
CN109928753A (en) * 2019-03-14 2019-06-25 杭州电子科技大学 A kind of low-k silicon substrate microwave dielectric ceramic materials and preparation method thereof
CN109942295A (en) * 2019-03-14 2019-06-28 杭州电子科技大学 A kind of microwave dielectric ceramic material used as 5G communication device and preparation method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020045532A1 (en) * 2000-05-30 2002-04-18 Yoshihiro Okawa Dielectric ceramics and dielectric resonator
CN101319377A (en) * 2007-06-06 2008-12-10 中国科学院金属研究所 Nano SrAl2O4 material and method for producing the same
CN104449685A (en) * 2013-09-25 2015-03-25 海洋王照明科技股份有限公司 Cerium-doped alkaline earth gallate luminescent material as well as preparation method and application thereof
CN107399966A (en) * 2017-07-28 2017-11-28 江苏大学 Low dielectric microwave dielectric material of a kind of high-performance and preparation method thereof
CN109928753A (en) * 2019-03-14 2019-06-25 杭州电子科技大学 A kind of low-k silicon substrate microwave dielectric ceramic materials and preparation method thereof
CN109942295A (en) * 2019-03-14 2019-06-28 杭州电子科技大学 A kind of microwave dielectric ceramic material used as 5G communication device and preparation method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
SHUXIN LIU ET AL.: "Exploring crystal-field splittings of Eu3+ ions in γ- and β-SrGa2O4", 《JOURNAL OF LUMINESCENCE》 *
SONGPING WU ET AL.: "Synthesis, characterization and microwave dielectric properties of spinel MgGa2O4 ceramic materials", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
X.Q. LIU ET AL.: "Microwave dielectric characteristics of SrLaGaO4 and SrNdGaO4 ceramics", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112266232A (en) * 2020-08-03 2021-01-26 杭州电子科技大学 Low-dielectric microwave dielectric ceramic material suitable for 5G millimeter wave communication application and preparation method thereof
CN114988877A (en) * 2022-06-15 2022-09-02 桂林理工大学 A kind of ultra-low loss microwave dielectric ceramic material and preparation method thereof
CN114988877B (en) * 2022-06-15 2023-08-29 桂林理工大学 Ultralow-loss microwave dielectric ceramic material and preparation method thereof

Similar Documents

Publication Publication Date Title
CN104310980B (en) A kind of microwave dielectric ceramic materials and preparation method thereof
CN111592348A (en) A low dielectric constant microwave dielectric ceramic with excellent temperature stability and preparation method thereof
CN111943671B (en) A low-loss microwave dielectric ceramic with a wide sintering temperature zone and a preparation method thereof
CN104692795A (en) Ultra-low-loss lithium magnesium titanate microwave dielectric ceramic material and preparation method thereof
CN105693241B (en) High quality factor lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof
CN109928753A (en) A kind of low-k silicon substrate microwave dielectric ceramic materials and preparation method thereof
CN108516826A (en) A kind of intermediary containing Sn microwave dielectric ceramic materials and preparation method thereof
CN112266232A (en) Low-dielectric microwave dielectric ceramic material suitable for 5G millimeter wave communication application and preparation method thereof
CN108569903A (en) A kind of low-temperature sintered LTCC microwave dielectric ceramics and preparation method
CN111170734A (en) Two-phase composite microwave dielectric ceramic material for filter and preparation method thereof
CN110885243B (en) Low-dielectric-constant aluminate microwave dielectric ceramic material and preparation method thereof
CN110845226A (en) Microwave dielectric ceramic material SrGa2O4And method for preparing the same
CN108585850A (en) A kind of ultralow-temperature sintering microwave medium ceramics and preparation method
CN111517771A (en) Microwave dielectric ceramic material and preparation method thereof
CN109942295A (en) A kind of microwave dielectric ceramic material used as 5G communication device and preparation method
CN107010956A (en) A kind of microwave dielectric ceramic materials and preparation method thereof
CN105693220B (en) Positive temperature coefficient silicate microwave dielectric ceramic material and preparation method thereof
CN111925207B (en) A kind of Mg3B2O6-Ba3(VO4)2 composite ceramic material and preparation method
CN112250441B (en) A Microwave Dielectric Ceramic with Adjustable Dielectric Properties at Low Sintering Temperature
CN111908897B (en) MgO-based microwave ceramic dielectric material and preparation method thereof
CN107253856A (en) A kind of microwave dielectric material of near-zero resonance frequency temperature coefficient and preparation method thereof
CN113387695A (en) Low-dielectric high-quality microwave dielectric ceramic for 5G communication and preparation method thereof
CN111499376A (en) Ceramic powder for 5G communication high-dielectric ceramic filter and preparation method thereof
CN111018524B (en) Low-loss trigonal tungstate-based microwave dielectric ceramic and preparation method thereof
CN102358698A (en) Microwave dielectric ceramic material with medium dielectric constant, 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