CN114907102A - Ceramic material and room-temperature ultrafast reactive sintering method thereof - Google Patents

Ceramic material and room-temperature ultrafast reactive sintering method thereof Download PDF

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CN114907102A
CN114907102A CN202210404033.7A CN202210404033A CN114907102A CN 114907102 A CN114907102 A CN 114907102A CN 202210404033 A CN202210404033 A CN 202210404033A CN 114907102 A CN114907102 A CN 114907102A
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ceramic
powder
raw material
powder raw
green body
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晏年平
王希林
蔡木良
李博江
徐碧川
晏子杨
贾志东
张宇
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Jiangxi Electric Power Co Ltd
Shenzhen International Graduate School of Tsinghua University
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Jiangxi Electric Power Co Ltd
Shenzhen International Graduate School of Tsinghua University
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    • 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
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The invention discloses a ceramic material and a room temperature ultrafast reactive sintering method thereof, relating to the technical field of ceramic material preparation. The invention takes one of the powder with high defect concentration as a sintering aid and a reactant to realize the room-temperature ultrafast reactive sintering of various ceramic materials, and the single-phase high-density ceramic is prepared and has universal applicability.

Description

Ceramic material and room-temperature ultrafast reactive sintering method thereof
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a ceramic material and a room-temperature ultrafast reactive sintering method thereof.
Background
The ceramic material has wide application in various fields, such as a zinc oxide arrester valve plate, a zinc aluminate high-frequency microwave ceramic substrate, a zinc titanate lithium cathode battery material, MnZn soft magnetic ferrite and the like. Sintering is a key link for preparing ceramic materials. The ceramic material prepared by high-temperature sintering has the defects of large crystal grains, more energy consumption and the like. Flash firing techniques can achieve rapid densification of ceramic materials at room temperature. In the traditional solid-phase reaction sintering, oxide raw materials are mixed in proportion and then react at high temperature to obtain target powder, and then ceramic green bodies are prepared for high-temperature sintering. Reactive flash firing is a novel sintering technique formed by combining the two methods. The two steps of the traditional solid-phase reaction sintering can be combined into one step, so that the ceramic sintering energy consumption is greatly reduced, the ceramic sintering time is shortened, and the mechanical and electrical properties of the ceramic are improved.
Disclosure of Invention
The invention aims to solve at least one technical problem in the prior art and provides a ceramic material and a room-temperature ultrafast reactive sintering method thereof.
The technical solution of the invention is as follows:
a ceramic material comprising the following raw materials: a powder raw material A having a high defect concentration and at least one powder raw material B which reacts with the powder raw material A.
In a preferred embodiment of the present invention, the high defect concentration is a concentration of oxygen vacancies in which the raw material A has a mole fraction of at least 4%.
In a preferred embodiment of the present invention, the powder raw material a is zinc oxide, and the powder raw material B is one or more of spherical alumina, manganese oxide, iron oxide, titanium oxide, and lithium carbonate. More specifically, A zinc oxide, B manganese oxide and iron oxide are reactively sintered into manganese zinc ferrite at room temperature; or the manganese oxide is replaced by nickel oxide to generate the nickel-zinc ferrite.
Performing reactive sintering on zinc oxide A, titanium oxide B and lithium carbonate at room temperature to obtain a zinc titanate lithium battery material; etc., may be used in many instances, but are not limited to such.
In a preferred embodiment of the present invention, the molar ratio of the powder raw material a to the powder raw material B is determined by a coefficient in the reaction equation.
The invention discloses a room temperature ultrafast reactive sintering method of ceramic materials, which comprises the steps of preparing a green ceramic blank by performing blank preparation on a powder raw material A with high defect concentration and at least one powder raw material B reacting with the powder raw material A, and applying voltage to two ends of the green ceramic blank to form Joule heating sintering to prepare the ceramic materials.
As a preferable scheme of the invention, the method comprises the following steps:
uniformly mixing and drying a powder raw material A and at least one powder raw material B which reacts with the powder raw material A in a planetary ball mill according to a certain proportion to obtain mixed powder, adding a binder into the mixed powder, fully grinding to obtain blank-making powder, pressing the blank-making powder into a dog bone shape by a single-shaft press, and placing the dog bone shape in a muffle furnace to discharge rubber to obtain a ceramic green blank; after room temperature silver paste is evenly smeared at two ends of the ceramic green body, the ceramic green body is connected into a circuit through a platinum wire, voltage is applied to the ceramic green body, the voltage is increased to a target voltage, then the current density flowing through the ceramic green body is maintained within a preset range within a preset time range, and powder in the green body is rapidly sintered while fully reacting to obtain compact ceramic.
In a preferred embodiment of the present invention, the mass ratio of the addition amount of the binder to the mixed powder is 1: 9.5-10.5.
In a preferred embodiment of the present invention, the binder is a PVA solution having a mass concentration of 3 to 7%.
As a preferable mode of the invention, the ball milling pot in the planetary ball mill is filled with absolute ethyl alcohol.
As a preferable mode of the present invention, the voltage is raised to a target voltage at a rate of 0.1 to 5kV/s, and the current density is controlled to 10 to 150mA/mm 2
The invention has the beneficial effects that: the ceramic reaction powder with high defect concentration is used as a sintering aid and a reactant thereof, and A and B with high defect concentration are made into green bodies and connected into a circuit through platinum wires, the high defect concentration indicates that more free electrons exist in the material, the initial conductivity of the material is higher, current is generated under the action of an electric field, joule heat is increased, the conductivity is further increased due to the rapid temperature rise of the sample, the current is rapidly increased until a stable value, and the sample slowly emits light at the moment, which is stage one; when the temperature rises to a temperature at which the reaction proceeds, two or more materials in the sample react with each other to form a single-phase material, and at this time, the electric field promotes the reaction, and the chemical reaction and densification of the green compact occur simultaneously at this stage.
The invention realizes the room-temperature ultrafast reactive sintering of various ceramic materials, prepares single-phase high-density ceramic and has universal applicability.
Drawings
FIG. 1 is a schematic view of a test apparatus embodying the present invention;
FIG. 2 is an XRD pattern of a sample of example 1;
FIG. 3 is a microscopic topography of the sample of example 1;
FIG. 4 is a graph of the results of characterization of the zinc aluminate samples of example 1;
FIG. 5 is a graph showing the results of characterization of the samples of example 2.
Detailed Description
The test method of the invention is as follows: (1) uniformly mixing the A powder with high-concentration defects with other required powder (B, C and the like) according to a certain proportion, and preparing a multiphase composite ceramic raw material after ball milling and granulation; (2) pressing and molding the ceramic raw material by using a die under a uniaxial press; (3) after the formed green body is subjected to glue discharging by a muffle furnace, silver paste is uniformly coated on two ends of the green body, and then the green body is connected into a circuit by a platinum wire; (4) the electric conductivity of the ceramic green body is changed, the voltage is instantly reduced, the current is instantly increased to a fixed value, and then the current value can be changed by adjusting the voltage; (5) the ceramic forms conductive paths within the ceramic, which by joule heating causes the ceramic to begin to glow red, at which stage the ceramic green body begins to react, forming a single phase ceramic and densifying rapidly.
The powder A in the invention is powder with high defect concentration.
The proportion of A and other raw materials (B, C, etc.) in the invention is determined according to the chemical equation coefficient of the single-phase ceramic to be synthesized.
The die used by the ceramic raw material is a dog bone-shaped die, the pressure is 5-6MPa, preferably 5.6MPa, the green body can be broken by overlarge pressure, and the strength of the green body cannot meet the requirement by the overlow pressure, so that the green body is broken by current impact in the sintering process.
The ceramic green body is subjected to glue removal in a muffle furnace, the temperature of the muffle furnace is raised to 400-450 ℃ at the temperature raising rate of 2-3 ℃/min, and the temperature is kept for 2-2.5 h; preferably, the temperature is raised to 400 ℃ at a heating rate of 2 ℃/min, and the temperature is kept for 2h, so as to ensure that the PVA added is completely decomposed and removed.
In the present invention, the voltage is increased at a rate of 0.1 to 5kV/s, and the current density flowing through the ceramic green body is maintained at 10 to 150mA/mm 2 . Too low a current density does not guarantee rapid densification of the ceramic green body, and too high a current may cause the ceramic to shrink sharply, resulting in local overheating and fracture.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The invention provides a room-temperature ultrafast reactive sintering method for a ceramic material by taking high-defect-concentration powder as a sintering aid and a reactant, wherein a device used in a test is shown in a figure 1, specifically, a sample 1 is electrically connected with a high-power resistor 2 with the resistance value of 7k omega, voltage is regulated in a circuit by arranging a transformer 4, a boosting transformer 3 and a capacitive voltage divider 5, and the numerical values of the voltage and the current are specifically displayed in a voltage and voltage combined current measuring device 6. But the specific implementation form is not limited thereto.
The high-concentration defect powder mainly refers to point defects (such as oxygen vacancies and atomic gaps) on a chemical structure, and can be characterized by X-ray photoelectron spectroscopy (XPS), electron paramagnetic spectrum and the like; the powder can be realized by a heat treatment process such as quenching and the like, and can also be directly obtained by adjusting the production process of a manufacturer during production.
Example 1
An ultrafast reactive sintering method of zinc aluminate ceramic comprises the following steps: the method comprises the following steps:
(1) according to the chemical reaction equation of synthesizing zinc aluminate ZnO + Al 2 O 3 =ZnAl 2 O 4 Light yellow zinc oxide powder (having an oxygen vacancy concentration with an oxygen vacancy mole fraction of 4%) and spherical alumina were mixed in a molar ratio of 1: 1, mixing, and fully dissolving the mixture into a ball milling tank by using absolute ethyl alcohol;
(2) placing a ball milling tank in a planetary ball mill, wherein the ball milling tank in the planetary ball mill is filled with absolute ethyl alcohol, and the mass ratio of the absolute ethyl alcohol to the powder is as follows: the absolute ethyl alcohol is 1: 8, the powder is taken out and dried after ball milling for 12 hours, PVA solution is added into the obtained powder, the powder is fully ground and granulated to obtain the raw material, the mass fraction of the added PVA solution is 5 percent, and the mass ratio of the PVA solution to the powder is 1: 10;
(3) 0.75g of the raw material was weighed and placed in a dog bone-shaped mold, and the raw material was placed under a uniaxial press, and pressure was maintained at 5.6MPa for 5 minutes, and then the raw material was taken out to obtain a dog bone-shaped green compact. Wherein the thickness of the middle part is 1.7mm, the length is 21mm, and the width is 3.3 mm;
(4) after silver paste is evenly coated on two ends of the dog-bone-shaped sample, connecting the dog-bone-shaped sample into a circuit, namely the position of the sample shown in figure 1, by using a platinum wire, and keeping a power supply in a power-off state;
(5) turning on a high-voltage alternating-current power supply, uniformly increasing voltage at a rate of 0.2kV/s until the current is increased instantly, decreasing the voltage instantly, and slowly emitting red light from the sample, wherein the voltage is adjusted to stabilize the current density at 50mA/mm 2 Maintaining for 30s, wherein the zinc oxide and the aluminum oxide in the green body react to generate single-phase zinc aluminate;
(6) and (3) observing the microscopic appearance of the sintered sample through SEM (EDS), wherein the apparent density of the sample is mainly observed according to the grain size and the number of air holes in the observation period. The crystal structure of the sintered sample was measured by XRD and it was observed whether a single-phase zinc aluminate spinel structure was formed, referring to fig. 2 to 4.
The experimental results of fig. 2-4 show that zinc aluminate EDS in the finished product shows a Zn to Al ratio of about 1: 2, the compactness can reach 99.5 percent through the Archimedes drainage method, which shows that the sample is basically compact and generates single-phase zinc aluminate ceramic.
Example 2
An ultrafast reactive sintering of zinc titanate ceramic comprising the steps of:
(1) equation 2ZnO + TiO based on the chemical reaction for synthesizing zinc aluminate 2 =Zn 2 TiO 4 Light yellow zinc oxide powder (having an oxygen vacancy concentration with an oxygen vacancy mole fraction of 4%) and spherical alumina were mixed in a molar ratio of 2: 1, mixing, and fully dissolving the mixture into a ball milling tank by using absolute ethyl alcohol;
(2) placing a ball milling tank in a planetary ball mill, wherein the ball milling tank in the planetary ball mill is filled with absolute ethyl alcohol, and the mass ratio of the absolute ethyl alcohol to the powder is as follows: the absolute ethyl alcohol is 1: 9, the powder is taken out and dried after ball milling for 12 hours, PVA solution is added into the obtained powder, the powder is fully ground and granulated to obtain the raw material, the mass fraction of the added PVA solution is 5 percent, and the mass ratio of the PVA solution to the powder is 1: 10;
(3) 0.75g of the raw material was weighed into a dog bone-shaped mold, placed under a uniaxial press, and pressure-maintained at 5.6MPa for 5 minutes, and then taken out to obtain a green dog bone-shaped article. Wherein the thickness of the middle part is 1.7mm, the length is 21mm, and the width is 3.3 mm;
(4) after silver paste is evenly coated on two ends of the dog-bone-shaped sample, connecting the dog-bone-shaped sample into a circuit, namely the position of the sample shown in figure 1, by using a platinum wire, and keeping a power supply in a power-off state;
(5) and (3) turning on a high-voltage alternating-current power supply, uniformly increasing the voltage at the rate of 0.2kV/s until the current is increased instantly, decreasing the voltage instantly, and slowly emitting red light by the sample. At this time, the voltage was adjusted to stabilize the current density at 50mA/mm 2 Maintaining for 30s, wherein the zinc oxide and the titanium dioxide in the green body react to generate single-phase zinc titanate;
(6) and observing the microscopic morphology of the sintered sample through SEM, wherein the grain size and the apparent density of the sample with the number of air holes are mainly observed. The crystal structure of the sample after sintering was measured by XRD, and it was observed whether a single-phase zinc titanate spinel structure was formed, referring to fig. 5.
The experimental result of figure 5 shows that the sample is basically compact and single-phase zinc titanate ceramic is generated, and the compactness of the sample can reach 98.8 percent through the Archimedes drainage method.
The above description is only a preferred embodiment of the present invention, and the technical solutions that achieve the objects of the present invention by substantially the same means are within the protection scope of the present invention.

Claims (10)

1. A ceramic material, characterized by comprising the following raw materials: a powder raw material A having a high defect concentration and at least one powder raw material B which reacts with the powder raw material A.
2. The ceramic material of claim 1 wherein said high defect concentration is such that feedstock a has an oxygen vacancy concentration of at least 4 mole percent.
3. The ceramic material according to claim 1, wherein the powder raw material A is zinc oxide, and the powder raw material B is one or more of spherical alumina, manganese oxide, iron oxide, titanium oxide, and lithium carbonate.
4. The ceramic material according to claim 1, wherein the molar ratio of the powder material A to the powder material B is determined by the coefficient in the reaction equation.
5. A room temperature ultrafast reactive sintering method of ceramic materials is characterized in that a powder raw material A with high defect concentration and at least one powder raw material B reacting with the powder raw material A are subjected to blank making to obtain a ceramic green body, and voltages are applied to two ends of the ceramic green body to form Joule heating sintering to obtain the ceramic materials.
6. A method for ultra-fast reactive sintering at room temperature of a ceramic material according to claim 5, comprising the steps of:
uniformly mixing and drying a powder raw material A and at least one powder raw material B which reacts with the powder raw material A in a planetary ball mill according to a certain proportion to obtain mixed powder, adding a binder into the mixed powder, fully grinding to obtain blank-making powder, pressing the blank-making powder into a dog bone shape by a single-shaft press, and placing the dog bone shape in a muffle furnace to discharge rubber to obtain a ceramic green blank; after room temperature silver paste is evenly smeared at two ends of the ceramic green body, the ceramic green body is connected into a circuit through a platinum wire, voltage is applied to the ceramic green body, the voltage is increased to a target voltage, then the current density flowing through the ceramic green body is maintained within a preset range within a preset time range, and powder in the green body is rapidly sintered while fully reacting to obtain compact ceramic.
7. The method for ultrafast reactive sintering at room temperature of ceramic material as set forth in claim 6, wherein a mass ratio of said binder added to said powder mixture is 1: 9.5-10.5.
8. The method as claimed in claim 6, wherein the binder is PVA solution with a mass concentration of 3-7%.
9. The method for ultrafast reactive sintering at room temperature of ceramic material as set forth in claim 6, wherein a ball milling pot of said planetary ball mill is filled with absolute ethanol.
10. The method of claim 6, wherein the voltage is increased to a target voltage at a rate of 0.1-5kV/s, and the current density is controlled at 10-150mA/mm 2
CN202210404033.7A 2022-04-18 2022-04-18 Ceramic material and room-temperature ultrafast reactive sintering method thereof Pending CN114907102A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN115974560A (en) * 2022-10-10 2023-04-18 国网江西省电力有限公司电力科学研究院 Method for sintering ceramic at room temperature

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CN110357633A (en) * 2019-07-11 2019-10-22 上海交通大学 A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic
CN110606751A (en) * 2019-09-18 2019-12-24 上海交通大学 Method for graphene-assisted room-temperature flash firing of ceramic material
CN112683062A (en) * 2020-12-08 2021-04-20 国网江西省电力有限公司电力科学研究院 Ultrafast sintering method and device for ceramic material
CN113307624A (en) * 2021-05-13 2021-08-27 佛山华骏特瓷科技有限公司 Method for sintering ceramic at room temperature
CN113754435A (en) * 2021-09-08 2021-12-07 郑州航空工业管理学院 Y2O3Preparation method of-MgO infrared transparent ceramic

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110204328A (en) * 2019-06-05 2019-09-06 西南交通大学 A kind of preparation method of high entropy oxide ceramics
CN110357633A (en) * 2019-07-11 2019-10-22 上海交通大学 A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic
CN110606751A (en) * 2019-09-18 2019-12-24 上海交通大学 Method for graphene-assisted room-temperature flash firing of ceramic material
CN112683062A (en) * 2020-12-08 2021-04-20 国网江西省电力有限公司电力科学研究院 Ultrafast sintering method and device for ceramic material
CN113307624A (en) * 2021-05-13 2021-08-27 佛山华骏特瓷科技有限公司 Method for sintering ceramic at room temperature
CN113754435A (en) * 2021-09-08 2021-12-07 郑州航空工业管理学院 Y2O3Preparation method of-MgO infrared transparent ceramic

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115974560A (en) * 2022-10-10 2023-04-18 国网江西省电力有限公司电力科学研究院 Method for sintering ceramic at room temperature
CN115974560B (en) * 2022-10-10 2024-03-12 国网江西省电力有限公司电力科学研究院 Ceramic room temperature sintering method

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Application publication date: 20220816