CN110981549A - Production process of alumina ceramic - Google Patents
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5133—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the refractory metals
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
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Abstract
The invention relates to an alumina ceramic production process, which comprises the following steps: ceramic pretreatment: cleaning the surface of the area to be metallized of the ceramic; and (3) slurry treatment: mixing molybdenum powder, aluminum oxide and silicon dioxide according to a certain proportion to obtain molybdenum slurry, and placing the molybdenum slurry in a binder to be fully and uniformly stirred; screen printing: uniformly coating molybdenum slurry on the upper and lower silk-screen surfaces of the ceramic; metallization and sintering: forming a metallized layer on the surface of the ceramic to prepare metallized ceramic; hot-pressing and sealing: and sealing the metallized ceramic and the inner and outer nickel rings. The metallized ceramic prepared by the alumina ceramic production process can stably run for a long time in a high-temperature molten salt corrosion environment at 270-350 ℃, is suitable for sodium salt batteries, and meets the working and using requirements of the sodium salt batteries.
Description
Technical Field
The present invention relates to the field of ceramics.
Background
The sodium-nickel battery and the sodium-sulfur battery are all of a full-sealing structure and comprise three sealing technologies, namely α -alumina ceramic and β' -alumina ceramic, α -alumina ceramic and metal, and metal are sealed, wherein the α -reliability of the sealing of the alumina ceramic and the metal is directly related to the performance, the service life and the safety reliability of the battery, so the battery is extremely important.
Disclosure of Invention
In order to solve the technical problem, the invention provides an alumina ceramic production process, which comprises the following steps: ceramic pretreatment: cleaning the surface of the area to be metallized of the ceramic; and (3) slurry treatment: mixing metal powder comprising molybdenum powder, aluminum oxide, silicon dioxide and titanium dioxide according to a certain proportion to obtain molybdenum slurry, and placing the molybdenum slurry in a binder to be fully and uniformly stirred; screen printing: uniformly coating molybdenum slurry on the upper and lower silk-screen surfaces of the ceramic; metallization and sintering: forming a metallized layer on the surface of the ceramic to prepare metallized ceramic; hot-pressing and sealing: and sealing the metallized ceramic and the inner and outer nickel rings.
Further, the slurry is processed, and the mass ratio of molybdenum powder to alumina to silicon dioxide is x: y: 1-x-y, wherein x is 65-80, y is 0-5, and Z is 0-10; metal powder: binder 80: 20, the binder is prepared by mixing ethylene glycol monobutyl ether: the ethylene glycol monobutyl ether acetate is prepared by mixing in a weight ratio of 5:15, and before the screen printing is used, the slurry is fully rolled for 48-72 hours at a rotating speed of 20 rpm.
Further, in the silk-screen printing, molybdenum slurry is uniformly coated on the upper and lower silk-screen printing surfaces of the ceramic, and is dried at a high temperature of 250 ℃, wherein the thickness of the slurry is 22-52 mu m.
Further, the metallized sintering: the sintering time is 15 minutes, and a uniform and compact metalized layer with the thickness of 15-35 mu m is obtained.
Further, the hot-press sealing is carried out on the metallized ceramic and the inner and outer nickel rings under the high temperature and protective atmosphere.
Furthermore, the alumina ceramic adopts a CaO-Al2O3-SiO2 ternary system, wherein the content of alumina is 94-96%, and the mass ratio of SiO2/CaO is less than 1.3.
The metallized ceramic prepared by the alumina ceramic production process can stably run for a long time in a high-temperature molten salt corrosion environment at 270-350 ℃, is suitable for sodium salt batteries, and meets the working and using requirements of the sodium salt batteries.
Detailed Description
The invention is further described with reference to specific examples.
The alumina ceramic adopts a CaO-Al2O3-SiO2 ternary system, wherein the content of alumina is 94-96%, the mass ratio of SiO2/CaO is less than 1.3, the alumina ceramic is sintered at high temperature by a dry pressing process, the density of the ceramic is controlled to be about 3.7g/cm3, and the grain size is 6-10 mu m. The invention relates to an alumina ceramic production process, which comprises the following steps:
ceramic pretreatment: cleaning the surface of the area to be metallized of the ceramic;
and (3) slurry treatment: the preparation method comprises the steps of mixing metalized powder comprising molybdenum powder, alumina, silicon dioxide and titanium dioxide according to a certain proportion, and placing the mixture into a binder to be fully and uniformly stirred. The mass ratio of the molybdenum powder to the aluminum oxide to the silicon dioxide is x: y: 1-x-y, wherein x is 65-80, y is 0-5, and Z is 0-10; the purity of the molybdenum powder is required to be 99.5%, the particle size is 2-3 mu m, and other components are analytically pure raw materials; metal powder: binder 80: 20, the binder is prepared by mixing ethylene glycol monobutyl ether: the screen printing paste is prepared by mixing ethylene glycol monobutyl ether acetate in a weight ratio of 5:15, sealing and storing the mixture in a clean environment with certain temperature and humidity, and fully rolling the paste at a rotating speed of 20rpm for 48-72 hours before screen printing;
and (2) screen printing, namely selecting a stainless steel screen with a proper mesh number for plate making, designing special printing tooling trays, putting 8 multiplied by 8 α -alumina ceramics on each tray, selecting a scraper material with proper hardness according to the characteristics of the slurry, controlling the tension of the screen to be 25-40N/cm, uniformly coating the molybdenum slurry on the upper and lower screen printing surfaces of the ceramics by adjusting parameters such as the speed of a scraper, the angle of the scraper, the pressure of the scraper, the distance between screens and the like of a screen printing machine, and drying at a high temperature of 250 ℃, wherein the thickness of the slurry is controlled to be 22-52 mu m.
Metallization and sintering: the single-furnace-door tunnel-type atmosphere protection boat pushing furnace is used, the atmosphere of the whole hearth is wet hydrogen, namely, a nitrogen-hydrogen mixed gas is firstly brought into a certain amount of water vapor through a wet hydrogen water tank and then enters the hearth, the wet hydrogen water tank is placed in a constant-temperature water bath, the temperature of the water bath is controlled to be 15-30 ℃, the sintering temperature is controlled to be 1500-1565 ℃, the sintering time is 15 minutes, and a uniform and compact metalized layer with the thickness of 15-35 mu m is obtained.
Hot-pressing and sealing: and assembling the metallized ceramic and the inner and outer nickel rings by a tool clamp, applying pressure, and obtaining the TCB structural component with ideal sealing strength and airtightness requirements under high temperature and protective atmosphere.
Example 1:
the method comprises the following steps:
(1) the ceramic components require 95.3 percent of alumina, 1.12 percent of SiO2/CaO, 3.69g/cm3 of density and 7.2 mu m of grain size, the ceramic A is cleaned at high temperature of 1200 ℃, and then is put in a specially designed printing tool tray, 8 multiplied by 8 to 64 ceramic plates are put in each plate, the direction of the inner square step is upward, and seven plates are stacked in total;
(2) rolling the prepared pure molybdenum slurry continuously at the rotating speed of 20rpm for 72 hours;
(3) selecting a 105-mesh imported stainless steel wire screen, wherein a screen frame is made of hollow aluminum, the screen distance is 4mm, the scraper pressure is 3kg, the scraper angle is 70 degrees, the scraper speed is 150mm/s, firstly, screen printing is carried out on a first surface, then, baking is carried out at the high temperature of 250 ℃ for 15 minutes, then, the first surface is overturned through an overturning mechanism, the second surface is placed upwards, after the ceramic is cooled to the room temperature, screen printing is carried out on the second surface, and high-temperature baking is carried out at the temperature of 250 ℃, so that metalized slurry with the screen printing drying thickness of about 35 mu m is obtained;
(4) suspending the silk-screened ceramic string in a molybdenum boat, carrying out metallization sintering in a single-furnace-door tunnel-type atmosphere protection boat pushing furnace, wherein the whole atmosphere of a hearth is wet hydrogen, and the hydrogen in the nitrogen-hydrogen mixed gas accounts for 13%, namely, the nitrogen-hydrogen mixed gas is firstly brought into certain water vapor through a water tank and then enters the hearth, the water tank is placed in a constant-temperature water bath, the water bath temperature is 20 ℃, the sintering temperature is 1520 ℃, the boat pushing speed is 14.48mm/min, and the cycle period is 15min, so that the metallization ceramic with the metallization layer thickness of about 20 mu m is obtained;
(5) assembling a certain amount of metallized ceramics and nickel rings with two specifications through a TZM rod and a ceramic gasket, and carrying out hot-pressing diffusion sealing in a bell jar furnace protected by nitrogen-hydrogen mixed atmosphere.
Example 2:
the method comprises the following steps:
(1) the ceramic components require 95.3 percent of alumina, 1.12 percent of SiO2/CaO, 3.69g/cm3 of density and 7.2 mu m of grain size, the ceramic A is cleaned at high temperature of 1200 ℃, and then is put in a specially designed printing tool tray, 8 multiplied by 8 to 64 ceramic plates are put in each plate, the direction of the inner square step is upward, and seven plates are stacked in total;
(2) rolling the prepared pure molybdenum slurry continuously at the rotating speed of 20rpm for 72 hours;
(3) selecting a 105-mesh imported stainless steel wire screen, wherein a screen frame is made of hollow aluminum, the screen distance is 4mm, the scraper pressure is 3kg, the scraper angle is 70 degrees, the scraper speed is 150mm/s, firstly, screen printing is carried out on a first surface, then, baking is carried out at the high temperature of 250 ℃ for 15 minutes, then, the first surface is overturned through an overturning mechanism, the second surface is placed upwards, after the ceramic is cooled to the room temperature, screen printing is carried out on the second surface, and high-temperature baking is carried out at the temperature of 250 ℃, so that metalized slurry with the screen printing drying thickness of about 35 mu m is obtained;
(4) suspending the silk-screened ceramic string in a molybdenum boat, and carrying out metallized sintering in a single-furnace-door tunnel atmosphere protection pushed slab kiln, wherein the whole atmosphere of a hearth is wet hydrogen, and the hydrogen in the nitrogen-hydrogen mixed gas accounts for 13%, namely, the nitrogen-hydrogen mixed gas is firstly brought into certain water vapor through a water tank and then enters the hearth, the water tank is placed in a constant-temperature water bath, the water bath temperature is 20 ℃, the sintering temperature is 1535 ℃, the pushing speed is 14.48mm/min, the cycle period is 15min, and the metallized ceramic with the metallized layer thickness of about 20 mu m is obtained;
(5) assembling a certain amount of metallized ceramics and nickel rings with two specifications through a TZM rod and a ceramic gasket, and carrying out hot-pressing diffusion sealing in a bell jar furnace protected by nitrogen-hydrogen mixed atmosphere.
Example 3:
the method comprises the following steps:
(1) the ceramic components require 95.3 percent of alumina, 1.12 percent of SiO2/CaO, 3.69g/cm3 of density and 7.2 mu m of grain size, the ceramic A is cleaned at high temperature of 1200 ℃, and then is put in a specially designed printing tool tray, 8 multiplied by 8 to 64 ceramic plates are put in each plate, the direction of the inner square step is upward, and seven plates are stacked in total;
(2) rolling the prepared pure molybdenum slurry continuously at the rotating speed of 20rpm for 72 hours;
(3) selecting a stainless steel wire mesh screen printing plate with 105 meshes, wherein a screen frame is made of hollow aluminum, the screen distance is 4.5mm, the scraper pressure is 3.2kg, the scraper angle is 60 degrees, and the scraper speed is 150mm/s, firstly carrying out screen printing on a first surface, then baking for 15 minutes at the high temperature of 250 ℃, then overturning the first surface through an overturning mechanism to enable a second surface to be placed upwards, carrying out screen printing on the second surface after the ceramic is cooled to the room temperature, and baking at the high temperature of 250 ℃ to obtain metalized slurry with the screen printing drying thickness of about 35 mu m;
(4) the ceramic rings after silk printing are strung and suspended in a molybdenum boat, and are subjected to metalized sintering through a single-furnace-door tunnel atmosphere protection pushed slab kiln, the whole atmosphere of a hearth is wet hydrogen, and the hydrogen in a nitrogen-hydrogen mixed gas accounts for 13 percent, namely, the nitrogen-hydrogen mixed gas is firstly brought into certain water vapor through a water tank and then enters the hearth, the water tank is placed in a constant-temperature water bath, the water bath temperature is 15 ℃, the sintering temperature is 1550 ℃, the pushing speed is 14.48mm/min, the cycle period is 15min, and the metalized ceramic with the metalized layer thickness of about 20 mu m is obtained;
(5) assembling a certain amount of metallized ceramics and nickel rings with two specifications through a TZM loading rod and a ceramic gasket, and carrying out hot-pressing diffusion sealing in a bell jar furnace protected by nitrogen-hydrogen mixed atmosphere.
Example 4:
the method comprises the following steps:
(1) the ceramic components require that the alumina content is 94.5 percent, the SiO2/CaO is 1.28, the density is 3.74g/cm3, the grain size is 8.9 mu m, the ceramic B is cleaned at high temperature of 1200 ℃, and then is put in a specially designed printing tool tray, 8 multiplied by 8 is 64 in each tray, the direction of the inner square step is upward, and seven trays are stacked in total;
(2) rolling the pure molybdenum slurry at the rotating speed of 20rpm for 72 hours;
(3) selecting a stainless steel wire mesh screen printing plate with 105 meshes, wherein a screen frame is made of hollow aluminum, the screen distance is 4mm, the scraper pressure is 3kg, the scraper angle is 70 degrees, the scraper speed is 150mm/s, firstly, screen printing is carried out on a first surface, then, baking is carried out at the high temperature of 250 ℃ for 15 minutes, then, the first surface is overturned through an overturning mechanism, the second surface is placed upwards, and after the ceramic is cooled to the room temperature, screen printing is carried out on the second surface, and high-temperature baking is carried out at the temperature of 250 ℃, so that metalized slurry with the screen printing drying thickness of about 35 mu m is obtained;
(4) the ceramic rings after silk printing are strung and suspended in a molybdenum boat, and are subjected to metalized sintering through a single-furnace-door tunnel atmosphere protection pushed slab kiln, the whole atmosphere of a hearth is wet hydrogen, and the hydrogen in a nitrogen-hydrogen mixed gas accounts for 13 percent, namely, the nitrogen-hydrogen mixed gas is firstly brought into certain water vapor through a water tank and then enters the hearth, the water tank is placed in a constant-temperature water bath, the water bath temperature is 25 ℃, the sintering temperature is 1550 ℃, the pushing speed is 14.48mm/min, the cycle period is 15min, and the metalized ceramic with the metalized layer thickness of about 20 mu m is obtained;
(5) assembling a certain amount of metallized ceramics and nickel rings with two specifications through a TZM rod and a ceramic gasket, and carrying out hot-pressing diffusion sealing in a bell jar furnace protected by nitrogen-hydrogen mixed atmosphere.
Example 5:
the method comprises the following steps:
(1) the ceramic components require that the alumina content is 94.5 percent, the SiO2/CaO is 1.28, the density is 3.74g/cm3, the grain size is 8.9 mu m, the ceramic B is cleaned at high temperature of 1200 ℃, and then is put in a specially designed printing tool tray, 8 multiplied by 8 is 64 in each tray, the direction of the inner square step is upward, and seven trays are stacked in total;
(2) rolling the pure molybdenum slurry at the rotating speed of 20rpm for 72 hours;
(3) selecting a stainless steel wire mesh screen printing plate with 105 meshes, wherein a screen frame is made of hollow aluminum, the screen distance is 4.5mm, the scraper pressure is 3.2kg, the scraper angle is 60 degrees, and the scraper speed is 150mm/s, firstly carrying out screen printing on a first surface, then baking for 15 minutes at the high temperature of 250 ℃, then overturning the first surface through an overturning mechanism to enable a second surface to be placed upwards, carrying out screen printing on the second surface after the ceramic is cooled to the room temperature, and baking at the high temperature of 250 ℃ to obtain metalized slurry with the screen printing drying thickness of about 35 mu m;
(4) the silk-screen ceramic rings are strung and suspended in a molybdenum boat, and are subjected to metallization sintering through a single-furnace-door tunnel atmosphere protection pushed slab kiln, the whole atmosphere of a hearth is wet hydrogen, and the hydrogen in a nitrogen-hydrogen mixed gas accounts for 13 percent, namely, the nitrogen-hydrogen mixed gas is firstly brought into certain water vapor through a water tank and then enters the hearth, the water tank is placed in a constant-temperature water bath, the water bath temperature is 15 ℃, the sintering temperature is 1565 ℃, the pushing speed is 14.48mm/min, the cycle period is 15min, and the metallization layer thickness of the metallization layer is about 20 mu m;
(5) assembling a certain amount of metallized ceramics and nickel rings with two specifications through a TZM rod and a ceramic gasket, and carrying out hot-pressing diffusion sealing in a bell jar furnace protected by nitrogen-hydrogen mixed atmosphere;
the metallized production process of the alumina ceramic comprises the steps of ceramic pretreatment, slurry treatment, screen printing, metallized sintering, hot-press sealing and the like, wherein the metallized ceramic is sealed with metal and then is subjected to glass sealing with an β -Al2O3 ceramic tube, and then a battery cell is assembled, so that the metallized ceramic can stably run in a high-temperature molten salt corrosion environment at 270-350 ℃ for a long time, is suitable for a sodium salt battery, and meets the working and using requirements of the sodium salt battery.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (6)
1. The production process of the alumina ceramic is characterized by comprising the following steps: ceramic pretreatment: cleaning the surface of the area to be metallized of the ceramic; and (3) slurry treatment: mixing molybdenum powder, aluminum oxide and silicon dioxide according to a certain proportion to obtain molybdenum slurry, and placing the molybdenum slurry in a binder to be fully and uniformly stirred; screen printing: uniformly coating molybdenum slurry on the upper and lower silk-screen surfaces of the ceramic; metallization and sintering: forming a metallized layer on the surface of the ceramic to prepare metallized ceramic; hot-pressing and sealing: and sealing the metallized ceramic and the inner and outer nickel rings.
2. The alumina ceramic production process according to claim 1, wherein the slurry is processed, and the mass ratio of molybdenum powder, alumina and silica is x: y: 1-x-y, wherein x is 65-80, y is 0-5, and Z is 0-10; metal powder: binder 80: 20, the binder is prepared by mixing ethylene glycol monobutyl ether: the ethylene glycol monobutyl ether acetate is prepared by mixing in a weight ratio of 5:15, and before the screen printing is used, the slurry is fully rolled for 48-72 hours at a rotating speed of 20 rpm.
3. The alumina ceramic production process as claimed in claim 1 or 2, wherein the molybdenum paste is uniformly coated on the upper and lower silk-screen surfaces of the ceramic by silk-screen printing, and is dried at a high temperature of 250 ℃ to form paste with a thickness of 22-52 μm.
4. The alumina ceramic production process of claim 3, wherein the metallized sintering: the sintering time is 15 minutes, and a uniform and compact metalized layer with the thickness of 15-35 mu m is obtained.
5. The alumina ceramic production process according to claim 4, wherein the hot press sealing is carried out by hot press sealing the metallized ceramic and the inner and outer nickel rings at high temperature under a protective atmosphere.
6. The alumina ceramic production process according to claim 1, wherein the alumina ceramic adopts a CaO-Al2O3-SiO2 ternary system, wherein the alumina content is 94-96%, and the SiO2/CaO mass ratio is less than 1.3.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111634132A (en) * | 2020-04-25 | 2020-09-08 | 湖南省美程陶瓷科技有限公司 | Magnetron ceramic metallization coating control method and application system thereof |
| CN111662096A (en) * | 2020-05-13 | 2020-09-15 | 江苏大学 | Sealing method of ceramic capacitor pressure sensor chip |
| CN117377210A (en) * | 2023-10-09 | 2024-01-09 | 南通威斯派尔半导体技术有限公司 | Manufacturing process suitable for Si3N4 ceramic aluminum-coated substrate |
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