CN112011149A - A kind of high dielectric quasicrystal composite material substrate and preparation method thereof - Google Patents
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- 239000013079 quasicrystal Substances 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 239000000758 substrate Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 11
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910002115 bismuth titanate Inorganic materials 0.000 claims abstract description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000005011 phenolic resin Substances 0.000 claims abstract description 6
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 6
- 229910001702 icosahedrite Inorganic materials 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 17
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 230000003014 reinforcing effect Effects 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims 1
- 238000004146 energy storage Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000003990 capacitor Substances 0.000 abstract description 3
- 239000003792 electrolyte Substances 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 230000002547 anomalous effect Effects 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- WEUCVIBPSSMHJG-UHFFFAOYSA-N calcium titanate Chemical compound [O-2].[O-2].[O-2].[Ca+2].[Ti+4] WEUCVIBPSSMHJG-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000005676 thermoelectric effect Effects 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及一种复合材料基板及其制备方法，特别是涉及一种高介电准晶体复合材料基板及其制备方法。The invention relates to a composite material substrate and a preparation method thereof, in particular to a high dielectric quasi-crystal composite material substrate and a preparation method thereof.
背景技术Background technique
准晶体亦称为“准晶”或“拟晶”，是一种介于晶体和非晶体之间的固体结构，具有与晶体相似的长程有序的原子排列，但是准晶体不具备晶体的平移对称性，可以具有晶体所不允许的宏观对称性。准晶体属性独特，坚硬又有弹性，与大多数金属不同的是其导电、导热性很差；具有良好的热电效应，能将电能转化为热能，可以制备理想的热电材料。2000年以前发现的所有几百种准晶体中至少含有3种金属元素，如Al65Cu23Fe12，Al70Pd21Mn9等，但最近发现仅2种金属元素也可形成准晶体，如Cd57Yb10。Quasicrystals, also known as "quasicrystals" or "pseudocrystals", are solid structures between crystals and amorphous crystals, with long-range ordered atomic arrangements similar to crystals, but quasicrystals do not have the translation of crystals Symmetry, which can have macroscopic symmetries that are not allowed by crystals. Quasicrystals have unique properties, are hard and elastic, and are different from most metals in that they have poor electrical and thermal conductivity; they have good thermoelectric effect, can convert electrical energy into thermal energy, and can prepare ideal thermoelectric materials. All the hundreds of quasicrystals discovered before 2000 contain at least 3 kinds of metal elements, such as Al65Cu23Fe12, Al70Pd21Mn9, etc., but recently it was found that only 2 kinds of metal elements can also form quasicrystals, such as Cd57Yb10.
钙钛矿材料是一类有着与钛酸钙(CaTiO3)相同晶体结构的材料，钙钛矿材料结构式一般为ABX3，A、B为阳离子，X为阴离子，这种奇特的晶体结构使其具备了很多独特的理化性质，比如吸光性、电催化性等等。《Scientific Reports》期刊2015年第5卷12699页的论文Origin of anomalous giant dielectric performance in novel perovskite：Bi0.5-xLaxNa0.5-xLixTi1-yMyO3(M＝Mg2+，Ga3+)报道了对钙钛矿结构的Bi0.5Na0.5TiO3陶瓷进行A/B位共掺杂改性设计，获得了具有异常高的介电常数的一类新材料，大大拓展了钙钛矿材料概念的外延，并在高温储能电容器、化学传感器以及新型固态离子电解质等领域具有很大的应用潜力。Perovskite materials are a class of materials with the same crystal structure as calcium titanate (CaTiO3). The structural formula of perovskite materials is generally ABX3, A and B are cations, and X is an anion. Many unique physicochemical properties, such as light absorption, electrocatalysis, etc. The paper Origin of anomalous giant dielectric performance in novel perovskite: Bi0.5-xLaxNa0.5-xLixTi1-yMyO3 (M=Mg2+, Ga3+) reported on the perovskite structure A/B site co-doping modification design of Bi0.5Na0.5TiO3 ceramics has obtained a new class of materials with unusually high dielectric constants, which greatly expands the epitaxy of the concept of perovskite materials, and is widely used in high-temperature energy storage capacitors. , chemical sensors and new solid-state ionic electrolytes have great application potential.
授权公告号为CN103382240B的中国发明专利公开了一种高介电常数的钛酸钡/聚合物复合材料及其制备方法；所述复合材料包括如下体积百分含量的各组分：单核1～60％，内壳3～30％，外壳20～80％，所述单核为钛酸钡陶瓷颗粒，所述内壳为具有高介电常数的聚酰胺，所述外壳为介电常数较低的聚甲基丙烯酸甲酯。本发明还涉及前述的复合材料的制备方法，本发明复合材料中的单核先用氨基硅烷作表面处理，引入有机官能团，然后依次分散到不同单体溶液中，得到核-壳-壳之间共价键连接结构的复合材料，所述复合材料具有高的介电常数，低的介电损耗，无机颗粒均匀分布的特征。The Chinese invention patent with the authorization announcement number CN103382240B discloses a high dielectric constant barium titanate/polymer composite material and a preparation method thereof; the composite material includes the following components in volume percentage: mononuclear 1～ 60%, inner shell 3-30%, outer shell 20-80%, the single core is barium titanate ceramic particles, the inner shell is polyamide with high dielectric constant, and the outer shell is low dielectric constant of polymethyl methacrylate. The invention also relates to the preparation method of the aforementioned composite material. The single core in the composite material of the invention is first treated with aminosilane for surface treatment, and organic functional groups are introduced, and then dispersed into different monomer solutions in turn to obtain a core-shell-shell structure. A composite material with a covalent bond structure, the composite material has the characteristics of high dielectric constant, low dielectric loss, and uniform distribution of inorganic particles.
现有的高介电复合材料基板存在以下问题：(1)易碎、加工困难、机械性能差；(2)耐热性不足、高温下剥离强度低；(3)制备条件严格，对设备、工艺和操作环境的要求都很高。The existing high-dielectric composite material substrates have the following problems: (1) fragile, difficult to process, and poor in mechanical properties; (2) insufficient heat resistance and low peel strength at high temperatures; (3) strict preparation conditions, poor equipment, Both the process and the operating environment are demanding.
发明内容SUMMARY OF THE INVENTION
为解决现有技术的不足，本发明提供一种既可作高温储能电容器，也可作化学传感器以及新型固态离子电解质的高介电准晶体复合材料及其的制备方法。In order to solve the deficiencies of the prior art, the present invention provides a high-dielectric quasi-crystal composite material which can be used not only as a high-temperature energy storage capacitor, but also as a chemical sensor and a novel solid-state ionic electrolyte, and a preparation method thereof.
为了实现本发明的目的，采用了如下技术方案：一种高介电准晶体复合材料基板，由准晶体材料、复合型钙钛矿材料和树脂复合而成，其特征在于准晶体材料作为增强相，复合型钙钛矿材料作为功能相，树脂作为基体材料，准晶体材料占质量百分数5～10％，复合型钙钛矿材料占质量百分数5～10％，树脂占质量百分数80～90％，基板的孔隙率小于3％，所述的准晶体为Al65Cu23Fe12、Al70Pd21Mn9、Cd57Yb10、Al63Cu24Fe13中的一种，所述的复合型钙钛矿为钛酸铋钠，所述的树脂为液体石墨烯酚醛树脂，其中石墨烯含量为质量百分比的0.5％～5％。In order to achieve the purpose of the present invention, the following technical scheme is adopted: a high-dielectric quasi-crystal composite material substrate, which is composed of a quasi-crystal material, a composite perovskite material and a resin, and is characterized in that the quasi-crystal material is used as a reinforcing phase , the composite perovskite material is used as the functional phase, and the resin is used as the matrix material. The porosity of the substrate is less than 3%, the quasi-crystal is one of Al65Cu23Fe12, Al70Pd21Mn9, Cd57Yb10, Al63Cu24Fe13, the composite perovskite is sodium bismuth titanate, and the resin is liquid graphene phenolic resin , wherein the graphene content is 0.5% to 5% by mass.
该高介电准晶体复合材料制备方法，其特征在于包括如下顺序的步骤：The method for preparing the high-dielectric quasi-crystal composite material is characterized in that it comprises the steps of the following sequence:
(1)将含有质量分数为50～55％的Cu、Fe或者质量分数为55～60％的Pd、Mn的Al金属熔体或者含有质量分数为20～25％的Yb的Cd金属熔体急冷，一步转化为介稳的准晶体，充分粉碎研磨后得到平均粒径小于100nm准晶体粉末；(1) Quenching the Al metal melt containing 50-55% Cu, Fe or 55-60% Pd, Mn or the Cd metal melt containing 20-25% Yb by mass fraction , converted into metastable quasi-crystal in one step, fully pulverized and ground to obtain quasi-crystal powder with an average particle size of less than 100 nm;
(2)将复合型钙钛矿结构的钛酸铋钠充分粉碎研磨后得到平均粒径小于100nm钙钛矿粉末；(2) fully pulverizing and grinding the sodium bismuth titanate of the composite perovskite structure to obtain perovskite powder with an average particle size of less than 100 nm;
(3)将准晶体粉末、钙钛矿粉末以及树脂按质量比例充分均匀混合，得到混合物浆料；(3) fully and uniformly mixing the quasicrystal powder, the perovskite powder and the resin according to the mass ratio to obtain a mixture slurry;
(4)将混合物浆料在模具中浇注，在真空烘箱中烘干固化，保温后随炉冷却至室温，得到准晶体复合材料。(4) pouring the mixture slurry in a mold, drying and solidifying in a vacuum oven, and cooling to room temperature with the furnace after heat preservation to obtain a quasi-crystal composite material.
具体实施方式Detailed ways
下面结合具体实施例，进一步阐述本发明，应理解这些实施例仅用于说明本发明而不是用于限制本发明的范围，在阅读了本发明之后，本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定。The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention rather than to limit the scope of the present invention. Modifications of form all fall within the meaning of the appended claims of this application.
实施例1Example 1
一种高介电准晶体复合材料基板，其中Al65Cu23Fe12准晶体占质量百分数5％、复合型钙钛矿材料占质量百分数5％，石墨烯酚醛树脂占质量百分数90％，孔隙率为1％，石墨烯酚醛中石墨烯含量为1％。该高介电准晶体复合材料制备方法如下：A high-dielectric quasicrystal composite material substrate, wherein Al65Cu23Fe12 quasicrystal accounts for 5% by mass, composite perovskite material accounts for 5% by mass, graphene phenolic resin accounts for 90% by mass, porosity is 1%, graphite The graphene content in the alkenol is 1%. The preparation method of the high dielectric quasicrystal composite material is as follows:
(1)将含有50％Cu、Fe的Al金属熔体急冷，一步转化为介稳的准晶体，充分粉碎研磨后得到平均粒径小于100nm准晶体粉末；(1) The Al metal melt containing 50% Cu and Fe is quenched, converted into a metastable quasicrystal in one step, and fully pulverized and ground to obtain a quasicrystal powder with an average particle size of less than 100 nm;
(2)将复合型钙钛矿结构的钛酸铋钠充分粉碎研磨，平均粒径80nm；(2) The composite perovskite structure sodium bismuth titanate is fully pulverized and ground, with an average particle size of 80 nm;
(3)将准晶体粉末、钙钛矿粉末以及树脂按质量比例充分均匀混合，得到混合物浆料；(3) fully and uniformly mixing the quasicrystal powder, the perovskite powder and the resin according to the mass ratio to obtain a mixture slurry;
(4)将混合物浆料在模具中浇注，在真空烘箱中烘干固化，保温后随炉冷却至室温，得到准晶体复合材料。(4) pouring the mixture slurry in a mold, drying and solidifying in a vacuum oven, and cooling to room temperature with the furnace after heat preservation to obtain a quasi-crystal composite material.
经过测试，该复合基板常温下的介电常数落于2300～5200之间，且随温度和频率变化的程度小，优于目前公开文献报道的数据，具有显著的新颖性和实用性。After testing, the dielectric constant of the composite substrate at room temperature falls between 2300 and 5200, and the degree of change with temperature and frequency is small, which is better than the data reported in the current public literature, and has remarkable novelty and practicability.
实施例2Example 2
一种高介电准晶体复合材料基板，其中Al70Pd21Mn9准晶体占质量百分数8％、复合型钙钛矿材料占质量百分数5％，石墨烯酚醛树脂占质量百分数87％，孔隙率为1％，石墨烯酚醛中石墨烯含量为1％。该高介电准晶体复合材料制备方法如下：A high-dielectric quasicrystal composite material substrate, wherein Al70Pd21Mn9 quasicrystal accounts for 8% by mass, composite perovskite material accounts for 5% by mass, graphene phenolic resin accounts for 87% by mass, porosity is 1%, graphite The graphene content in the alkenol is 1%. The preparation method of the high dielectric quasicrystal composite material is as follows:
(1)将含有60wt％Pd、Mn的Al金属熔体急冷，一步转化为介稳的准晶体，充分粉碎研磨后得到平均粒径小于100nm准晶体粉末；(1) The Al metal melt containing 60wt% Pd and Mn is quenched, converted into a metastable quasicrystal in one step, and fully pulverized and ground to obtain a quasicrystal powder with an average particle size of less than 100nm;
(2)将复合型钙钛矿结构的钛酸铋钠充分粉碎研磨，平均粒径80nm；(2) The composite perovskite structure sodium bismuth titanate is fully pulverized and ground, with an average particle size of 80 nm;
(3)将准晶体粉末、钙钛矿粉末以及树脂按质量比例充分均匀混合，得到混合物浆料；(3) fully and uniformly mixing the quasicrystal powder, the perovskite powder and the resin according to the mass ratio to obtain a mixture slurry;
(4)将混合物浆料在模具中浇注，在真空烘箱中烘干固化，保温后随炉冷却至室温，得到准晶体复合材料。(4) pouring the mixture slurry in a mold, drying and solidifying in a vacuum oven, and cooling to room temperature with the furnace after heat preservation to obtain a quasi-crystal composite material.
经过测试，该复合基板常温下的介电常数落于2500～6000之间，且随温度和频率变化的程度小，优于目前公开文献报道的数据，具有显著的新颖性和实用性。After testing, the dielectric constant of the composite substrate at room temperature falls between 2500 and 6000, and the degree of variation with temperature and frequency is small, which is better than the data reported in the current public literature, and has remarkable novelty and practicability.
实施例3Example 3
一种高介电准晶体复合材料基板，其中Cd57Yb10准晶体占质量百分数10％、复合型钙钛矿材料占质量百分数10％，石墨烯酚醛树脂占质量百分数80％，孔隙率为2％，石墨烯酚醛中石墨烯含量为2％。该高介电准晶体复合材料制备方法如下：A high dielectric quasicrystal composite material substrate, wherein Cd57Yb10 quasicrystal accounts for 10% by mass, composite perovskite material accounts for 10% by mass, graphene phenolic resin accounts for 80% by mass, porosity is 2%, graphite The graphene content in the alkenol is 2%. The preparation method of the high dielectric quasicrystal composite material is as follows:
(1)将含有20wt％Pd、Mn的Al金属熔体急冷，一步转化为介稳的准晶体，充分粉碎研磨后得到平均粒径小于70nm准晶体粉末；(1) The Al metal melt containing 20wt% Pd and Mn is quenched, converted into a metastable quasicrystal in one step, and fully pulverized and ground to obtain a quasicrystal powder with an average particle size of less than 70nm;
(2)将复合型钙钛矿结构的钛酸铋钠Bi0.5Na0.5TiO3充分粉碎研磨，平均粒径60nm；(2) The composite perovskite structure sodium bismuth titanate Bi0.5Na0.5TiO3 is fully pulverized and ground, with an average particle size of 60 nm;
(3)将准晶体粉末、钙钛矿粉末以及树脂按质量比例充分均匀混合，得到混合物浆料；(3) fully and uniformly mixing the quasicrystal powder, the perovskite powder and the resin according to the mass ratio to obtain a mixture slurry;
(4)将混合物浆料在模具中浇注，在真空烘箱中烘干固化，保温后随炉冷却至室温，得到准晶体复合材料。(4) pouring the mixture slurry in a mold, drying and solidifying in a vacuum oven, and cooling to room temperature with the furnace after heat preservation to obtain a quasi-crystal composite material.
经过测试，该复合基板常温下的介电常数落于3000～6000之间，且随温度和频率变化的程度小，优于目前公开文献报道的数据，具有显著的新颖性和实用性。After testing, the dielectric constant of the composite substrate at room temperature falls between 3000 and 6000, and the degree of change with temperature and frequency is small, which is better than the data reported in the current public literature, and has remarkable novelty and practicability.
上述仅为本发明的三个具体实施方式，但是本发明的设计构思并不局限于此，凡利用此构思对本发明进行非实质性的改动，均应属于侵犯本发明保护的范围的行为。凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所做的任何形式的简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。The above are only three specific embodiments of the present invention, but the design concept of the present invention is not limited to this, and any non-substantial changes to the present invention by using this concept should all belong to the act of infringing the protection scope of the present invention. Any form of simple modification, equivalent change and modification made to the above embodiment according to the technical essence of the present invention without departing from the content of the technical solution of the present invention still belongs to the protection scope of the technical solution of the present invention.
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