CN113527082A - Electronic functional ceramic and manufacturing method and application thereof - Google Patents

Electronic functional ceramic and manufacturing method and application thereof Download PDF

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CN113527082A
CN113527082A CN202110730234.1A CN202110730234A CN113527082A CN 113527082 A CN113527082 A CN 113527082A CN 202110730234 A CN202110730234 A CN 202110730234A CN 113527082 A CN113527082 A CN 113527082A
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organic acid
acid salt
powder
electronic functional
sintering
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CN113527082B (en
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郭靖
司明明
李晓萌
付长利
薛仙
汪宏
郝建宇
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Xian Jiaotong University
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41—Preparation of salts of carboxylic acids
    • C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
    • C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene

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Abstract

The invention discloses an organic acid salt electronic functional ceramic and a manufacturing method and application thereof. Sintering by adopting single organic acid salt powder, wherein the pressure load during sintering is 150-350 MPa, the sintering temperature is 20-300 ℃, the heating rate is 10-15 ℃/min, the sintering time is 40-150min, and the organic acid salt electronic functional ceramic with the density of more than or equal to 95 percent is obtained after sintering. The organic acid salt electronic functional ceramic is applied to piezoresistors, microwave dielectric ceramics and magneto-dielectric coupling ceramics. On the premise of reducing the process difficulty and the cost, the electronic functional ceramic with remarkable direct current voltage-sensitive characteristic or excellent microwave dielectric property is obtained.

Description

Electronic functional ceramic and manufacturing method and application thereof
Technical Field
The invention belongs to the field of power electronics and electronic information application, and relates to electronic functional ceramic and a manufacturing method and application thereof.
Background
The electronic functional ceramics have physical properties of themselves, such as: the sensor has acoustic, optical, thermal, electrical, magnetic and mechanical properties, and is widely applied to the fields of electronic information, microelectronics and internet of things sensors. The traditional electronic functional ceramic is prepared from one inorganic compound or is a compact composite ceramic material prepared from a plurality of inorganic compounds through different processing technologies.
In order to improve the physical properties of the conventional electronic functional ceramics by doping organic polymer materials, a low-temperature sintering technology is adopted to dope the organic polymer materials into inorganic compound matrixes to form the composite ceramic materials. Although the mode can realize inorganic-organic compounding, the method has the disadvantages of multiple component types, and difficult accurate regulation and control of formula proportion in industrial production, so that the final ceramic product has poor performance uniformity and low yield. Secondly, the inorganic compounds and organic polymer materials used in part are expensive, which is not favorable for cost control in industry.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an electronic functional ceramic, a manufacturing method and application thereof, and the electronic functional ceramic with remarkable direct current voltage-sensitive characteristic, microwave dielectric characteristic and magnetism is obtained on the premise of reducing process difficulty and cost.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a manufacturing method of electronic functional ceramics adopts single organic acid salt powder to sinter, the pressure load during sintering is 150MPa-350MPa, the sintering temperature is 20-300 ℃, the heating rate is 10-15 ℃/min, the sintering time is 40-150min, and the electronic functional ceramics are obtained after sintering.
Preferably, the organic acid salt powder includes oxalic acid series organic acid salt powder, glutamic acid series organic acid salt powder, citric acid series organic acid salt powder, formic acid series organic acid salt powder, acetic acid series organic acid salt powder or gluconic acid series organic acid salt powder.
Preferably, the organic acid salt powder is subjected to wet ball milling for at least 8 hours before sintering, and the product after wet ball milling is dried for 18 to 24 hours at the temperature of between 50 and 80 ℃.
Preferably, the organic acid salt powder is ground for 10 to 20 minutes before sintering until the powder particles are in a flour form.
Preferably, before sintering, the organic acid salt powder is ground for 10-20 minutes, and in the grinding process, 1.2-1.5mol/L acetic acid aqueous solution is added successively until the powder is in a wet state.
Preferably, before sintering, the organic acid salt powder is ground for 10-20 minutes, and deionized water is added in the grinding process until the powder is in a wet state.
An electronic functional ceramic comprises a single organic acid salt.
Preferably, the organic acid salt includes oxalic acid organic acid salt, glutamic acid organic acid salt, citric acid organic acid salt, formic acid organic acid salt, acetic acid organic acid salt or gluconic acid organic acid salt.
Preferably, the density of the ceramic is equal to or more than 95%, the nonlinear coefficient of current and voltage is more than 10, the electric breakdown field strength is more than 1000V/mm, the quality factor of the microwave dielectric property is more than 1000GHz, and the dielectric constant is 4-10.
An application of the electronic functional ceramic in piezoresistors, microwave dielectric ceramics and magneto-dielectric coupling ceramics.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts a cold sintering mode, obtains the electronic functional ceramic with remarkable direct current voltage-sensitive characteristic on the premise of reducing the process difficulty and the cost, and the organic acid salt multifunctional electronic ceramic can form a grain boundary layer among crystal grains in the sintering process, and the existence of the grain boundary layer causes a Schottky barrier to be formed among the crystal grains. The schottky barrier hinders the movement of charges, thereby causing the breakdown field strength of the electronic functional ceramic to be significantly increased and causing the current to exhibit a nonlinear relationship with the voltage. The organic acid salt multifunctional electronic ceramic adopts a cold sintering preparation process, so that the ceramic does not have phase change in the sintering process, the final densified ceramic is ensured to be kept in a single-phase state, and the nonlinear electrical property of the ceramic is further improved. The prepared ceramic has remarkable multifunctional electronic performance, direct-current pressure-sensitive characteristic and microwave dielectric property, and the organic acid salt ceramic prepared by cold sintering has compact structure and few internal defects, so that the dielectric loss is small, and the good microwave dielectric property is ensured. Meanwhile, part of the organic acid salt electronic functional ceramic has microwave dielectric property and magnetism and can be used as a magnetic dielectric coupling material. The organic acid salt powder has low price, mature industrial production and rich raw materials, is suitable for industrial large-scale production of the organic acid salt electronic functional ceramics, and has low production cost.
Drawings
FIG. 1 shows an SnC of the present invention2O4The transmission electron micrograph of the grain boundary of (1).
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
the electronic functional ceramic comprises a single organic acid salt in chemical composition.
The organic acid salt includes oxalic acid organic acid salt, glutamic acid organic acid salt, citric acid organic acid salt, formic acid organic acid salt, acetic acid organic acid salt or gluconic acid organic acid salt.
Therefore, the electronic functional ceramics according to the present embodiment relates to six types of electronic functional ceramics, each of which is an oxalic acid-based electronic functional ceramic, and includes: li2C2O4(lithium oxalate) electronic functional ceramics, K2C2O4(Potassium oxalate) electronic function ceramic, Na2C2O4(sodium oxalate) electronic functional ceramics, CaC2O4(calcium oxalate) electronic functional ceramics, CoC2O4(cobalt oxalate) electronic functional ceramics, FeC2O4(II) (ferrous oxalate) electronic functional ceramic, MnC2O4(manganese oxalate) electronic functional ceramics, SnC2O4(II) (tin oxalate) electronic functional ceramics. A glutamic acid-based electronically functional ceramic comprising: c5H8NNaO4(sodium glutamate) electronic functional ceramics, C5H8KNO4(Potassium glutamate) electronic functional ceramics, C10H16O8N2Ca (calcium glutamate) electronic functional ceramics, C5H7MgNO4(magnesium glutamate) electronic functional ceramics. A citric acid-based electronically functional ceramic comprising: c6H5Li3O7(lithium citrate) electronic functional ceramics, C6H5Na3O7(sodium citrate) electronic functional ceramics, C6H5K3O7(Potassium citrate) electric powerSubfunctional ceramics, Zn3(C6H5O7)2(Zinc citrate) electronic functional ceramics, C12H10Ca3O14(calcium citrate) electronic functional ceramics. Formic acid electronic functional ceramics, comprising: CHO2Li (lithium formate) electronic functional ceramics, CHO2Na (sodium formate) electronic functional ceramic, CHO2K (potassium formate) electronic functional ceramic, C2H2O4Ca (calcium formate) electronic functional ceramic, C2H6MgO6(magnesium formate) electronic functional ceramic. An acetic acid electronically functional ceramic comprising: c2H3LiO2(lithium acetate) electronic functional ceramics, C2H3NaO2(sodium acetate) electronic functional ceramics, C2H3KO2(Potassium acetate) electronic functional ceramics. Gluconic acid electronic functional ceramic: c6H11LiO7(lithium gluconate) electronic functional ceramics, C6H11NaO7(sodium gluconate) electronic functional ceramic, C6H11KO7(Potassium gluconate) electronic functional ceramics.
The original powder related to the six types of electronic functional ceramics comprises MC2O4·xH2O (wherein M is Li, K, Na, Ca, Co, Fe (II), Sn; x is 1, 2, 3, 4); c5H8NNaO4·xH2O (wherein x ═ 1, 2, 3, 4); c5H8KNO4·xH2O (wherein x ═ 1, 2, 3, 4); c10H16O8N2Ca·xH2O (wherein x is 1, 2, 3, 4), C5H7MgNO4·xH2O (wherein x ═ 1, 2, 3, 4); c6H5M3O7·xH2O (where M is Li, K, Na; x ═ 1, 2, 3, 4), Zn3(C6H5O7)2·xH2O (wherein x is 1, 2, 3, 4), C12H10Ca3O14·xH2O (wherein x ═ 1, 2, 3, 4); CHO2M·xH2O (wherein M is Li, K, Na,；x＝1，2，3，4)，C2H2O4Ca·xH2o (wherein x is 1, 2, 3, 4), C2H6MgO6·xH2O (wherein x ═ 1, 2, 3, 4); c2H3MO2·xH2O (wherein M is Li, K, Na; x is 1, 2, 3, 4); c6H11LiO7·xH2O (wherein M is Li, K, Na; x is 1, 2, 3, 4); c6H11MO7·xH2O (where x ═ 1, 2, 3, 4). The purity of all the original powder raw materials is higher than 95 percent;
the manufacturing method of the electronic functional ceramic comprises the following steps:
the method comprises the following steps: carrying out wet ball milling on the original powder respectively, wherein the wet ball milling medium is acetone;
step two: after wet ball milling for at least 8h, respectively placing the original powder in an oven at 50-80 ℃ for drying for 18-24 h;
step three: taking the dried sample in the step two for grinding pretreatment; the pretreatment method has three types, respectively,
(1) no liquid phase auxiliary pretreatment. And (4) grinding the various dried powder in the step two for 10-20 minutes until powder particles are in a flour shape, so as to ensure the uniformity of particle size and facilitate subsequent sintering preparation.
(2) And (3) carrying out auxiliary pretreatment on the acetic acid aqueous solution. And (3) taking the various dried powder in the step two, grinding the powder respectively for 10-20 minutes, and adding 1.2-1.5mol/L acetic acid aqueous solution in the grinding process until the powder is dark in color and is in a wet state, so that the particles and the acetic acid aqueous solution are uniformly mixed, and the subsequent sintering preparation is facilitated.
(3) And (5) auxiliary pretreatment of deionized water. And (3) grinding the various dried powder in the second step for 10-20 minutes, and adding deionized water in the grinding process until the powder is deepened and is in a wet state, so that the particles and the acetic acid aqueous solution are uniformly mixed, and the subsequent sintering preparation is facilitated.
Step four: and (4) respectively transferring the powder pretreated in the third step into metal molds, and placing the metal molds into a hot press for pressing. The pressure load is 150MPa-350MPa, the sintering temperature is 20-300 ℃, the heating rate is 10-15 ℃/min, and the sintering time is 40-150 min.
And step five, demolding, polishing, trimming and deburring the products prepared in the step four, and storing the products in a drying vessel.
The invention adopts cold sintering to prepare the organic acid salt powder into a compact ceramic block material, so that the material can be applied to the fields of power electronic devices, communication and dielectrics.
The prepared organic acid salt electronic functional ceramic has remarkable direct current voltage-sensitive characteristic, and the nonlinear coefficients of current and voltage are all more than 10 and can be more than 400 (MnC)2O4). The ultra-high electric breakdown field strengths are all over 1000V/mm and can be over 10000V/mm (CaC) at most2O4). In addition, the organic acid salt electronic functional ceramic containing Fe, Co and Mn elements has certain magnetism. The prepared organic acid salt has certain microwave dielectric property, wherein Qxf exceeds 1000GHz, and can reach over 30000GHz (C) at most2H3LiO2). The dielectric constant of the prepared organic acid salt electronic functional ceramic is 4-10.
The first embodiment is as follows:
MC2O4·H2o (wherein M is Li, K, Na, Ca, Co, Fe (II) and Sn); c5H8NNaO4·H2O；C5H8KNO4·H2O；C10H16O8N2Ca·H2O，C5H7MgNO4·H2O；C6H5M3O7·H2O (wherein M is Li, K, Na, respectively), Zn3(C6H5O7)2·H2O，C12H10Ca3O14·H2O；CHO2M·H2O (wherein M is Li, K, Na, respectively), C2H2O4Ca·H2O，C2H6MgO6·H2O；C2H3MO2·H2O (wherein M is Li, K, Na, respectively); c6H11LiO7·H2O (wherein M is Li, K, Na respectively).
The method comprises the following steps: respectively carrying out acetone wet ball milling on the original split bodies;
step two: after wet ball milling for 8h, respectively placing the original powder in an oven at 50 ℃ for drying for 18 h;
step three: taking the dried sample in the step two for grinding pretreatment;
no liquid phase auxiliary pretreatment. And (4) respectively grinding the various dried powder in the step two for 10 minutes until powder particles are in a flour shape, so as to ensure the uniformity of particle size and facilitate subsequent sintering preparation.
Step four: and (4) respectively transferring the powder pretreated in the third step into metal molds, and placing the metal molds into a hot press for pressing. The pressure load is 150MPa, the sintering temperature is 20 ℃, the heating rate is 10 ℃/min, and the sintering time is 40 min.
And step five, demolding, polishing, trimming and deburring the products prepared in the step four, and storing the products in a drying vessel.
Example two:
MC2O4·4H2o (wherein M is Li, K, Na, Ca, Co, Fe (II) and Sn); c5H8NNaO4·4H2O；C5H8KNO4·4H2O；C10H16O8N2Ca·H2O，C5H7MgNO4·H2O；C6H5M3O7·4H2O (wherein M is Li, K, Na, respectively), Zn3(C6H5O7)2·4H2O，C12H10Ca3O14·4H2O；CHO2M·4H2O (wherein M is Li, K, Na, respectively), C2H2O4Ca·4H2O，C2H6MgO6·4H2O；C2H3MO2·4H2O (wherein M is Li, K, Na, respectively); c6H11LiO7·4H2O (wherein M is Li, K, Na respectively).
The method comprises the following steps: respectively carrying out acetone wet ball milling on the original split bodies;
step two: after wet ball milling for 8h, respectively placing the original powder in an oven at 80 ℃ for drying for 24 h;
step three: and D, grinding the dried sample in the step two for pretreatment.
And (3) carrying out auxiliary pretreatment on the acetic acid aqueous solution. And (3) taking the various dried powder in the second step, grinding the powder for 20 minutes, and adding 1.5mol/L acetic acid aqueous solution in the grinding process until the color of the powder is deepened, so as to ensure that the particles and the acetic acid aqueous solution are uniformly mixed, and the subsequent sintering preparation is facilitated.
Step four: and (4) respectively transferring the powder pretreated in the third step into metal molds, and placing the metal molds into a hot press for pressing. The pressure load is 350MPa, the sintering temperature is 300 ℃, the heating rate is 15 ℃/min, and the sintering time is 150 min.
And step five, demolding, polishing, trimming and deburring the products prepared in the step four, and storing the products in a drying vessel.
Example three:
MC2O4·2H2o (wherein M is Li, K, Na, Ca, Co, Fe (II) and Sn); c5H8NNaO4·2H2O；C5H8KNO4·2H2O；C10H16O8N2Ca·2H2O，C5H7MgNO4·2H2O；C6H5M3O7·2H2O (wherein M is Li, K, Na, respectively), Zn3(C6H5O7)2·2H2O，C12H10Ca3O14·2H2O；CHO2M·2H2O (wherein M is Li, K, Na, respectively), C2H2O4Ca·2H2O，C2H6MgO6·2H2O；C2H3MO2·2H2O (wherein M is Li, K, Na, respectively); c6H11LiO7·2H2O (wherein M is Li, K, Na respectively).
Step two: after wet ball milling for 8h, respectively placing the original powder in an oven at 70 ℃ for drying for 20 h;
step three: taking the dried sample in the step two for grinding pretreatment; and (5) auxiliary pretreatment of deionized water. And (3) grinding the various dried powder in the second step for 15 minutes, and adding deionized water in the grinding process until the color of the powder is deepened, so that the particles and the acetic acid aqueous solution are uniformly mixed, and the subsequent sintering preparation is facilitated.
Step four: and (4) respectively transferring the powder pretreated in the third step into metal molds, and placing the metal molds into a hot press for pressing. The pressure load is 218MPa, the sintering temperature is 145 ℃, the heating rate is 12 ℃/min, and the sintering time is 90 min.
And step five, demolding, polishing, trimming and deburring the products prepared in the step four, and storing the products in a drying vessel.
Shown in the figure is SnC2O4The transmission electron micrograph of the grain boundary of (1). SnC2O4The transmission electron microscope clearly shows that2O4A grain boundary layer with a thickness of 1nm-6nm is formed between crystal grains, and the structure of the grain boundary layer enables SnC2O4Has excellent electric breakdown field strength and voltage-current nonlinear coefficient.
Examples one to three main properties of the finally produced electronic functional ceramics are shown in tables 1 to 3;
TABLE 1 Main electrical Properties of example I
Figure BDA0003139021380000091
Figure BDA0003139021380000101
TABLE 2 Main electrical Properties of example two
Figure BDA0003139021380000102
Figure BDA0003139021380000111
TABLE 3 Main electrical Properties of example III
Figure BDA0003139021380000112
Figure BDA0003139021380000121
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (10)

1. A manufacturing method of electronic functional ceramics is characterized in that single organic acid salt powder is adopted for sintering, the pressure load during sintering is 150MPa-350MPa, the sintering temperature is 20-300 ℃, the heating rate is 10-15 ℃/min, the sintering time is 40-150min, and the electronic functional ceramics are obtained after sintering.
2. The method for producing an electronic functional ceramic according to claim 1, wherein the organic acid salt powder comprises oxalic acid-based organic acid salt powder, glutamic acid-based organic acid salt powder, citric acid-based organic acid salt powder, formic acid-based organic acid salt powder, acetic acid-based organic acid salt powder, or mono-organic acid salt of gluconic acid-based organic acid salt powder.
3. The method of claim 1, wherein the organic acid salt powder is wet ball milled for at least 8 hours before sintering, and the wet ball milled product is dried at a temperature of 50 ℃ to 80 ℃ for 18 hours to 24 hours.
4. The method of claim 1, wherein the organic acid salt powder is ground for 10 to 20 minutes before sintering until the powder particles are in a flour form.
5. The method of claim 1, wherein the organic acid salt powder is ground for 10-20 minutes before sintering, and 1.2-1.5mol/L acetic acid aqueous solution is added during grinding until the powder is wet.
6. The method of claim 1, wherein the organic acid salt powder is ground for 10-20 minutes before sintering, and deionized water is added during grinding until the powder is in a wet state.
7. An electronic functional ceramic is characterized in that the chemical composition comprises a single organic acid salt.
8. The electronically functional ceramic of claim 1, wherein the organic acid salt comprises a single organic acid salt in the oxalate series, the glutamate series, the citrate series, the formate series, the acetate series, or the gluconate series.
9. The electronic functional ceramic according to claim 1, wherein the ceramic has a density of 95% or more, a nonlinear current-voltage coefficient of 10 or more, an electrical breakdown field strength of 1000V/mm or more, a microwave dielectric property quality factor of 1000GHz or more, and a dielectric constant of 4-10.
10. Use of an electronically functional ceramic according to any one of claims 7 to 9 in a varistor, a microwave dielectric ceramic and a magneto-dielectric coupling ceramic.
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