CN113307638A - Method for sintering ceramic and ceramic - Google Patents
Method for sintering ceramic and ceramic Download PDFInfo
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- CN113307638A CN113307638A CN202110700207.XA CN202110700207A CN113307638A CN 113307638 A CN113307638 A CN 113307638A CN 202110700207 A CN202110700207 A CN 202110700207A CN 113307638 A CN113307638 A CN 113307638A
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- ceramic
- green body
- ceramic green
- sintering
- power supply
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- 239000000919 ceramic Substances 0.000 title claims abstract description 131
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000005245 sintering Methods 0.000 title claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 239000007772 electrode material Substances 0.000 claims 1
- 238000010304 firing Methods 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 210000000988 bone and bone Anatomy 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005467 ceramic manufacturing process Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
Abstract
The invention provides a sintering method of ceramics, which comprises the following steps: providing a ceramic green body, and dripping liquid drops on the surface of the ceramic green body; connecting two ends of the ceramic green body dropwise added with the liquid drops with a power supply; communicating the power source to apply a voltage to the ceramic green body; and raising the voltage to a preset voltage value to enable the ceramic green body to generate surface discharge or internal discharge, enabling the current flowing through the ceramic green body to reach a preset current value, and cutting off the power supply after maintaining for a preset time period to obtain the ceramic. The sintering method of the ceramic provided by the invention can generate flash firing at room temperature and can rapidly densify. The invention also provides a ceramic sintered by applying the sintering method of the ceramic.
Description
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a ceramic sintering method and ceramic sintered by applying the ceramic sintering method.
Background
The ceramic material has important application in daily life, industrial manufacturing and other industries. Currently, the manufacture of ceramic materials requires high temperatures for a long time to sinter an otherwise loose green body to full density. This means that the conventional ceramic manufacturing process requires a large amount of energy consumption and a long time.
The flash firing technology can reduce energy consumption in the ceramic sintering process, and is a novel electric field auxiliary sintering process, namely, the ceramic is rapidly densified at a lower furnace temperature by applying appropriate electric fields at two ends of a ceramic green body and utilizing mechanisms such as thermal runaway and the like. The flash firing technology can reduce the furnace temperature required by ceramic sintering by hundreds of degrees centigrade compared with the traditional sintering mode, and simultaneously, the time is greatly reduced. However, the devices and steps required for flash-firing are complicated.
Disclosure of Invention
In view of the above, the present invention provides a rapid and convenient sintering method of ceramics, thereby solving the above problems.
In addition, the invention also provides a ceramic sintered by the sintering method of the ceramic.
The invention provides a sintering method of ceramics, which comprises the following steps:
providing a ceramic green body, and dripping liquid drops on the surface of the ceramic green body;
connecting two ends of the ceramic green body dropwise added with the liquid drops with a power supply;
communicating the power source to apply a voltage to the ceramic green body; and
and raising the voltage to a preset voltage value to enable the ceramic green body to generate surface discharge or internal discharge, enabling the current flowing through the ceramic green body to reach a preset current value, and cutting off the power supply after maintaining for a preset time period to obtain the ceramic.
The invention also provides a ceramic sintered by applying the sintering method of the ceramic, wherein the compactness of the ceramic is more than 90%.
According to the sintering method of the ceramic, quantitative liquid drops are dripped on the surface of the ceramic green body, so that the ceramic green body is subjected to flash combustion at room temperature, the densification is rapid, different ions can be doped in the sintered ceramic by dripping liquid drops containing different ions, and the process and the operation are simple. The density of the ceramic sintered by the ceramic sintering method is more than 90%, and no obvious defects such as cracks and the like occur.
Drawings
FIG. 1 is a flow chart of the preparation of the ceramic according to the preferred embodiment of the present invention.
Fig. 2 is a schematic structural diagram of an apparatus for sintering ceramic by dropping droplets manually according to a preferred embodiment of the present invention.
FIG. 3 is a schematic structural diagram of an apparatus for sintering ceramic by automatically dropping droplets according to a preferred embodiment of the present invention.
Description of the main elements
Ceramic green body 10
Electrode 11
Automatic sample adding device 30
Second sample injector 301
Switch 302
Display 303
Conducting wire 50
Fixing bracket 60
The following detailed description will further illustrate the invention in conjunction with the above-described figures.
Detailed Description
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.
Referring to fig. 1, a preferred embodiment of the present invention provides a method for sintering a ceramic, comprising the following steps:
in step S11, referring to fig. 2, a ceramic green body 10 is provided, and a droplet is dropped on the surface of the ceramic green body 10.
Specifically, ceramic powder is put into a mold for compression molding to obtain a ceramic green body 10, and electrodes 11 are respectively formed at two ends of the ceramic green body 10 by a method of spraying gold or coating conductive silver paste.
In some embodiments, the droplets may be manually applied by the first applicator 20. In particular, the first sample injector 20 may be a syringe.
Referring to fig. 3, in other embodiments, the liquid drop can also be automatically dropped by the automatic loading device 30. Specifically, the automatic sample adding device 30 includes a second sample adding device 301, a controller (not shown), a switch 302, a display 303, and the like. In particular, the second injector 301 may be a syringe. The controller is configured to control the volume of the liquid drops applied by the second applicator 301. The switch 302 is connected between the controller and the second sampler 301, and the switch 302 is used for connecting the controller and the second sampler 301. The display screen 303 is electrically connected to the controller, and thus can be used to display the volume of the liquid drops dropped by the second sample injector 301. More specifically, the controller is further electrically connected to a user interface (not shown), and when dripping is required, the dripping rate and the dripping amount of the automatic sample adding device 30 can be set through the user interface, so that a certain amount of liquid drops are dripped on the surface of the ceramic green body 10.
The ceramic green body 10 is at least one of cylindrical, rectangular and dog-bone shaped. It is understood that the shape of the ceramic green body 10 may be other regular shapes. In the present embodiment, the ceramic green sheet 10 has a dog bone shape. The ceramic green body 10 may be made of zinc oxide.
In some embodiments, the droplets may be water, an acid solution, a base solution, and a salt solution. In other embodiments, the droplets may be an organic liquid. Wherein, the organic liquid can be methanol and ethanol. The dripped liquid drops enable the ceramic green body to be subjected to flash firing at room temperature subsequently, rapid densification is achieved, and different ions can be doped in the sintered ceramic by dripping liquid drops containing different ions, so that the multifunctional ceramic can be prepared.
The volume of the droplets accounts for less than or equal to 50% of the volume of the ceramic green body.
And step S12, connecting the two ends of the ceramic green body 10 dripped with the liquid drops with a power supply 40.
Specifically, a wire 50 may be wound around each of the two electrodes 11, and the wire 50 may be connected to the power source 40, so that each of the two electrodes 11 is connected to the power source 40. The electrode 11 is made of gold or conductive silver paste.
The wire 50 is a metal wire with a high melting point. Specifically, the metal wire may include a platinum wire. In the present embodiment, the power supply 40 is a high voltage power supply. The power source 40 may be a dc power source or an ac power source. Preferably, the power source 40 is an alternating current power source. The ceramic crystal grains obtained by final sintering have better uniformity by using an alternating current power supply. It will be appreciated that the power source 40 may also be a square wave, pulsed or other various forms of power source.
In the present embodiment, when the ceramic green sheet 10 is connected to the power source 40, the ceramic green sheet 10 is suspended. Specifically, the lead 50 is fixed to the upper ends of two fixing brackets 60 so that the ceramic green sheet 10 can be suspended between the two fixing brackets 60, both ends of the ceramic green sheet 10 are connected to the power source 40 through the lead 50, and the ceramic green sheet 10 and the power source 40 form a closed loop through the lead 50. In other embodiments, the ceramic green body 10 may also be placed on a dielectric ceramic plate. In some embodiments, the automatic sample adding device 30 can be fixed on the upper end of one of the fixing brackets 60.
Step S13, the power source 40 is connected to apply a voltage to the ceramic green body 10.
Step S14, raising the voltage to a predetermined voltage value, causing creeping discharge or internal discharge to occur in the ceramic green sheet 10, causing the current flowing through the ceramic green sheet 10 to a predetermined current value, and cutting off the power supply 40 after maintaining the current value for a predetermined period of time, thereby obtaining the ceramic.
In particular, the voltage is raised to the predetermined voltage value at a rate of 0.1-5 kV/s. Wherein the density of the obtained ceramic is more than 90%.
When the current flowing through the ceramic green sheet 10 suddenly increases and the voltage across the ceramic green sheet 10 drops suddenly, it is judged that the ceramic green sheet 10 has creeping discharge or internal discharge.
Wherein the density of the predetermined current value is 10-200mA/mm2。
According to the sintering method of the ceramic, quantitative liquid drops are dripped on the surface of the ceramic green body 10, so that the ceramic green body 10 is subjected to flash combustion at room temperature, the densification is rapid, different ions can be doped in the sintered ceramic by dripping liquid drops containing different ions, and the process and the operation are simple.
The invention also provides a ceramic sintered by applying the sintering method of the ceramic, wherein the density of the ceramic is more than 90%, and obvious defects such as cracks and the like do not appear.
The present invention will be specifically described below with reference to examples.
Example 1
In the first step, 50. mu.L of water was manually dropped on a green zinc oxide ceramic blank having a dog bone shape using a syringe. Wherein the middle part of the dog bone shaped ceramic green body has a thickness of 1.7mm, a length of 21mm and a width of 3.3 mm.
And secondly, winding wires at two ends of the zinc ceramic green body, connecting the wires with an alternating current power supply, and fixing the wires on a fixed support to suspend the ceramic green body.
And thirdly, switching on a power supply, then rapidly increasing the voltage at the rate of 1kV/s until the voltage at two ends of the ceramic green body is suddenly reduced and the current passing through the ceramic green body is suddenly increased, keeping the voltage and the current unchanged, and switching off the power supply after 1 minute to finish sintering.
Example 2
The difference from example 1 is: in the first step, 100 mu L of sodium chloride solution with the mass fraction of 20 percent is dripped by using an automatic sample feeding device at the flow rate of 5 mu L/s; the ceramic green body had a cylindrical shape with a diameter of 3mm and a length of 22 mm. In the second step, the DC power supply is connected.
The ceramics sintered in examples 1 to 2 were each subjected to a density test by the archimedes drainage method. The results show that the density of the sintered ceramic of example 1 is 95% and that of the sintered ceramic of example 2 is 92%.
The density of the ceramic sintered by the sintering method of the ceramic provided by the invention can reach more than 90%, and the defects such as cracks and the like do not occur.
According to the sintering method of the ceramic, quantitative liquid drops are dripped on the surface of the ceramic green body 10, so that the ceramic green body 10 is subjected to flash combustion at room temperature, the densification is rapid, different ions can be doped in the sintered ceramic by dripping liquid drops containing different ions, and the process and the operation are simple. The density of the ceramic sintered by the ceramic sintering method is more than 90%, and no obvious defects such as cracks and the like occur.
In addition, the invention greatly reduces the environmental temperature required for sintering the ceramic by sintering the ceramic at room temperature, thereby reducing a large amount of energy consumption. Meanwhile, the sintering method of the ceramic is simple in process flow, and compared with a common flash-firing process, an additional heating device is not needed.
Although the embodiments of the present invention have been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the embodiments of the present invention.
Claims (10)
1. A method of sintering a ceramic, comprising the steps of:
providing a ceramic green body, and dripping liquid drops on the surface of the ceramic green body;
connecting two ends of the ceramic green body dropwise added with the liquid drops with a power supply;
communicating the power source to apply a voltage to the ceramic green body; and
and raising the voltage to a preset voltage value to enable the ceramic green body to generate surface discharge or internal discharge, enabling the current flowing through the ceramic green body to reach a preset current value, and cutting off the power supply after maintaining for a preset time period to obtain the ceramic.
2. The method of sintering a ceramic of claim 1 wherein the droplets comprise at least one of water, an acid solution, an alkali solution, a salt solution, methanol, and ethanol.
3. The method of sintering a ceramic according to claim 1, wherein the volume of the droplets accounts for less than or equal to 50% of the volume of the ceramic green body.
4. The method for sintering ceramics according to claim 1, wherein the rate of raising the voltage to the predetermined voltage value is 0.1 to 5kV/s, and the density of the predetermined current value is 10 to 200mA/mm2。
5. The method of sintering a ceramic of claim 1 wherein the ceramic green body has a shape of at least one of a cylinder, a cuboid, and a dog-bone shape.
6. The method for sintering a ceramic according to claim 1, wherein the liquid droplets are dropped by a sample applicator.
7. The method of sintering a ceramic of claim 1, wherein prior to dropping droplets on the surface of the ceramic green body, the method of sintering a ceramic further comprises:
putting the ceramic powder into a mould for compression molding to obtain the ceramic green body; and
forming electrodes at two ends of the ceramic green body respectively;
connecting both ends of the ceramic green compact to which the droplet is added with the power supply comprises:
and connecting the two electrodes with the power supply respectively by using leads.
8. The method of claim 7, wherein the electrode material comprises gold or conductive silver paste, and the wire comprises platinum wire.
9. The method of claim 1, wherein the power source is a dc power source or an ac power source.
10. A ceramic sintered using the method of sintering a ceramic according to any one of claims 1 to 9, said ceramic having a density of greater than 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110700207.XA CN113307638A (en) | 2021-06-23 | 2021-06-23 | Method for sintering ceramic and ceramic |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110700207.XA CN113307638A (en) | 2021-06-23 | 2021-06-23 | Method for sintering ceramic and ceramic |
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| CN113307638A true CN113307638A (en) | 2021-08-27 |
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| CN202110700207.XA Pending CN113307638A (en) | 2021-06-23 | 2021-06-23 | Method for sintering ceramic and ceramic |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362707A (en) * | 2020-04-03 | 2020-07-03 | 清华大学深圳国际研究生院 | Room temperature ceramic sintering method and ceramic |
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- 2021-06-23 CN CN202110700207.XA patent/CN113307638A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362707A (en) * | 2020-04-03 | 2020-07-03 | 清华大学深圳国际研究生院 | Room temperature ceramic sintering method and ceramic |
Non-Patent Citations (3)
| Title |
|---|
| JIEMING LIU等: "Mechanism of flash sintering with high electric field: In the view of electric discharge and breakdown", 《SCRIPTA MATERIALIA》 * |
| JIUYUAN NIE等: "Water-assisted flash sintering: Flashing ZnO at room temperature to achieve ~98% density in seconds", 《SCRIPTA MATERIALIA》 * |
| 毛正文等: "《重点疑点难点学习手册 化学 初三》", 30 September 1996, 东北师范大学出版社 * |
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Application publication date: 20210827 |
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