CN108752009B - Sintering method of electronic ceramic - Google Patents
Sintering method of electronic ceramic Download PDFInfo
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- CN108752009B CN108752009B CN201810394690.1A CN201810394690A CN108752009B CN 108752009 B CN108752009 B CN 108752009B CN 201810394690 A CN201810394690 A CN 201810394690A CN 108752009 B CN108752009 B CN 108752009B
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- 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
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
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Abstract
The invention discloses a sintering method of electronic ceramics, wherein after a blank formed by dry die casting is dried and frozen, the blank is more stable, the solubility of polyvinyl alcohol is increased after the polyvinyl alcohol is heated, the concentration is improved, and the adhesiveness is stronger; the frozen blank is heated to the inner layer one by one, the outer layer is heated firstly, so that the water loss is fast, the structure of the inner layer is in a stable state to play a supporting role, when the outer layer is heated and the water is lost, the outer layer begins to harden to form a fine channel, the inner layer is heated gradually, and the outer layer plays a supporting role; the blank is placed with the gasket of the same material with the technology because of the end when sintering, and in the in-process of high temperature sintering, because the tiny passageway that produces when getting rid of polyvinyl alcohol before can be filled by electronic ceramic material, consequently the blank can reduce when sintering, and the blank is comparatively the same with the gasket because of same material and technology, and the shrinkage factor is comparatively the same, and the blank bottom produces the displacement less or can be neglected, and the blank can not produce the deformation because of directly contacting with the casket bowl because of the friction.
Description
Technical Field
The invention relates to the field of electronic ceramic manufacturing, in particular to a sintering method of electronic ceramic.
Background
The electronic ceramic is formed by dry die casting, and generally a polyvinyl alcohol solution with volume ratio is added to act as an adhesive, so that organic matters in a blank body are removed by a heating method before sintering, namely, preheating and volatilization are carried out. At this stage, the green body is softened by heating, the strength is low, deformation is easy to occur, and the heating rate is directly controlled by the temperature; on the other hand, in this period, no pore channel is formed in the green body, and the volatilized small molecules can generate higher pressure in the green body due to the incapability of being eliminated, so that various defects such as bubbling, swelling, cracking, layering, deformation and the like are generated in the green body, thereby not only reducing the yield of the whole process, but also further influencing the perfect sintering of the green body. When present electronic ceramic product blank sintering, directly arrange the casket-like bowl in, because product blank lower surface and casket-like bowl bottom surface direct contact lead to having the friction between product blank and the casket-like bowl, in the sintering process, the product blank need contract, because friction action, the lower part shrink degree of product blank is less than upper portion, leads to the product deformation after the shaping.
Disclosure of Invention
The present invention is directed to a method for sintering electronic ceramics to solve the above problems in the prior art. In order to achieve the purpose, the invention provides the following technical scheme:
a sintering method of electronic ceramics comprises the following steps:
the first step is as follows: obtaining a dry electronic ceramic blank to be fired by dry pressing molding, slurry dipping, sand spraying and drying; manufacturing a sintered gasket by the same process;
the second step is that: placing the first-step sintering gasket into a sintering sagger, and placing a blank to be sintered on a ceramic sintering gasket;
the third step: putting the sagger obtained in the second step into a freezing chamber, wherein the temperature of the freezing chamber is set to be minus 10 to minus 5 ℃, the freezing chamber is decreased at the speed of minus 5 ℃ per hour, and the freezing time is 2 to 3 hours;
the fourth step: quickly putting the sagger obtained in the third step into a high-pressure carbon dioxide preheating chamber for preheating, wherein the transfer time is 5-15 seconds, the preheating temperature is 75-90 ℃, the air pressure is 0.5-1 MPa, and the preheating time is 10-30 minutes;
the fifth step: putting the sagger obtained in the fourth step into a carbon dioxide heating furnace, heating to 700-900 ℃ at the heating rate of 100-300 ℃ per hour, and preserving heat for 1-2 hours; the heating furnace is provided with an air inlet and an air outlet, the air inlet is connected with a carbon dioxide storage device through a pipeline, an air inlet fan is arranged on the pipeline, and the air outlet is connected with a cooling device through a pipeline;
and a sixth step: and transferring the sagger obtained in the fifth step into a sintering furnace, and sintering for 6-8 hours at 1200-1700 ℃.
As a further improvement of the technical scheme:
the sintering gasket is slightly larger than the bottom of the blank to be sintered, the bottom of the blank to be sintered is completely covered when the sintering gasket is placed, all transfer processes are stable, and the sintering gasket and the bottom of the blank to be sintered do not displace.
The temperature of the freezing chamber is set to be-5 ℃, and the freezing time is 3 hours.
The temperature of the preheating chamber is set to be 75 ℃, the air pressure is 0.5MPa, and the time is 20 minutes.
And during the work of the heating furnace, the carbon dioxide enters the carbon dioxide storage device through the cooling circulation of the air outlet.
The temperature of the sintering furnace is set to 1600 ℃, the sintering time is 6 hours, and the sintered product is naturally cooled to 100 ℃ and discharged.
Advantageous effects
According to the invention, after the dry die-casting molded blank is dried and frozen, the blank is relatively stable, and water is further dried and frozen out of the blank in the freezing process; the temperature of the preheating chamber is slightly higher than the optimal solubility of the polyvinyl alcohol under normal pressure, the bonding strength is higher, the melting point of the polyvinyl alcohol can be increased due to pressurization, the bonding stability of the polyvinyl alcohol is ensured in the preheating chamber, and the chemical structure of the polyvinyl alcohol is not damaged; the polyvinyl alcohol solution is frozen, so that the polyvinyl alcohol on the periphery of the blank is heated strongly to form a small channel, and the polyvinyl alcohol is melted and flows out through the small channel in the front after the inner layer of the blank is heated; compared with the condition that the preheating is not performed by freezing or heating at a higher speed, a fine channel is not formed in the blank, and small molecules with interior too high temperature or too fast volatilization can generate higher pressure in the blank because of being incapable of being discharged in time, so that the blank generates bubbles, swelling, cracking, layering, deformation and other defects, the yield of the whole process can be reduced, and the perfect sintering of the blank can be further influenced. After the blank is transferred into the heating furnace, the discharged polyvinyl alcohol is volatilized when the temperature reaches 700-900 ℃, and the discharged polyvinyl alcohol is absorbed by the liquid cooling device through carbon dioxide gas circulation cooling, so that the influence of the discharged polyvinyl alcohol on the blank is small. The blank is placed with the gasket of the same material with the technology because of the end when sintering, and in the in-process of high temperature sintering, because the tiny passageway that produces when getting rid of polyvinyl alcohol before can be filled by electronic ceramic material, consequently the blank can reduce when sintering, and the blank is comparatively the same with the gasket because of same material and technology, and the shrinkage factor is comparatively the same, and the blank bottom produces the displacement less or can be neglected, and the blank can not produce the deformation because of directly contacting with the casket bowl because of the friction.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the preheating chamber of the present invention;
FIG. 3 is a schematic view of the structure of the heating furnace of the present invention;
FIG. 4 is a schematic view of the construction of a sintering furnace according to the present invention;
FIG. 5 is a schematic view of the construction of a carbon dioxide storage unit and a cooling unit according to the present invention;
FIG. 6 is a schematic view of the structure of the freezing chamber and the air cooling device of the present invention;
FIG. 7 is a schematic view of the structure of the sagger and the gasket of the present invention;
FIG. 8 is a side view of the present sagger;
in the reference symbols: 1. a preheating chamber; 101. a first air inlet; 102. a pressurizing machine; 103. an air pressure detector; 104. a first heater; 105. a first guide rail; 106. a first temperature detector; 107. a first gate; 2. heating furnace; 201. a second gate; 202. a second guide rail; 203. a second air inlet; 204. a second heater; 205. a fan; 206. a first air outlet; 207. a second temperature detector; 208. a third gate; 3. sintering furnace; 301. a third heater; 302. a fourth gate; 303. a third guide rail; 304. a third temperature detector; 401. a second air outlet; 402. a third air outlet; 403. a third air inlet; 404. a cooling device; 405. a wide mouth; 406. a collection port; 407. a fourth air inlet; 408. a carbon dioxide storage device; 5. a freezing chamber; 501. an air cooling device; 502. a fifth air inlet; 503. a fifth gate; 504. a fourth temperature detector; 601. a trapezoidal groove; 602. a first half cylinder; 603. an inner groove; 604. an outer protrusion; 605. a second semi-cylinder; 606. and (7) a gasket.
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.
As shown in fig. 1 to 8, the sintering method of the electronic ceramic of the present invention is implemented by a sintering system, which includes a preheating chamber 1, a heating furnace 2, a sintering furnace 3, a liquid cooling device 404, a carbon dioxide storage device 408, a freezing chamber 5, an air cooling device 501, and a sagger 6;
the air cooling device 501 is connected with the freezing chamber 5 through a fifth air inlet 502 by a duct, the fifth air inlet 502 is arranged on the freezing chamber 5, and a fifth shutter 503 and a fourth temperature detector 504 are arranged on the freezing chamber 5;
the preheating chamber 1 is connected with the heating furnace 2, the preheating chamber 1 and the heating furnace 2 are respectively provided with a first gate 107 and a second gate 201, and the first gate 107 and the second gate 201 are identical in size and position and are overlapped;
the heating furnace 2 is connected with the sintering furnace 3, the heating furnace 2 and the sintering furnace 3 are respectively provided with a third gate 208 and a fourth gate 302, and the third gate 208 and the fourth gate 302 are overlapped;
the heating furnace 2 is connected with the liquid cooling device 404 through a first air outlet 206 by a conduit;
the liquid cooling device 404 is connected to a carbon dioxide storage device 408 through a conduit via a collection port 406;
the carbon dioxide storage device 408 is connected with the preheating chamber 1 through a second air outlet 401 by a conduit; the carbon dioxide storage device 408 is connected to the heating furnace 2 through the third outlet port 402.
The fourth temperature detector 504 is connected by data to the air cooling device 501, and the fifth shutter 503 is used as a feed material, sealed and insulated when closed.
The preheating chamber 1 is provided with a first air inlet 101, a pressurizer 102, an air pressure detector 103, a first heater 104, a first guide rail 105, a first temperature detector 106 and a first gate 107, the first air inlet 101 is connected with a second air outlet 401 through a conduit, the pressurizer 102 is arranged in the middle of the conduit, the pressurizer 102 is in data connection with the air pressure detector 103, the first heater 104 is in data connection with the first temperature detector 106, and the first guide rail 105 is arranged on the upper surface of the bottom of the preheating chamber 1.
The heating furnace 2 is provided with a second gate 201, a second guide rail 202, a second air inlet 203, a second heater 204, a fan 205, a first air outlet 206, a second temperature detector 207 and a third gate 208, the second heater 204 is connected with the second temperature detector 207 through data, the second guide rail 202 is arranged on the upper surface of the bottom of the heating furnace 2, the second air inlet 203 is connected with a third air outlet 402 through a conduit, the fan 205 is arranged on the conduit, and the first air outlet 206 is connected with the third air inlet 403.
The sintering furnace 3 is provided with a third heater 301, a fourth gate 302, a third guide rail 303 and a third temperature detector 304, the third heater 301 and the third temperature detector 304 are connected through data, and the third guide rail 303 is arranged on the upper surface of the bottom of the sintering furnace 3.
The liquid cooling device 404 and the carbon dioxide storage device 408 are respectively provided with a second air outlet 401, a third air outlet 402, a third air inlet 403 and a wide mouth 405, a collection port 406 and a fourth air inlet 407, the second air outlet 401 is connected with the first air inlet 101 through a conduit, the middle of the conduit is provided with the pressurizer 102, the third air outlet 402 is connected with the second air inlet 203 through a conduit, the conduit is provided with the fan 205, the third air inlet 403 is connected with the first air outlet 206 through a conduit, the wide mouth 405 is connected with the third air inlet 403 through a conduit, the collection port 406 is arranged at the top of the liquid cooling device 404 and is connected with the fourth air inlet 407 through a conduit.
The first guide rail 105, the second guide rail 202 and the third guide rail 303 are on the same horizontal plane and are in the same straight line, the first gate 107 and the second gate 201, the third gate 208 and the fourth gate 302 are the same and are overlapped in pairs, and the first guide rail 105, the second guide rail 202 and the third guide rail 303 pass through the gates in the same straight line.
The sagger 6 is provided with a trapezoidal groove 601, a first semi-cylinder 602 and an inner groove 603; the sagger comprises an outer protrusion 604, a second semi-cylinder 605 and a gasket 606, wherein the gasket 606 is placed on the inner upper surface of the sagger, trapezoidal grooves 601 and inner grooves 603 matched with the outer protrusion 604 are formed in the four sides of the sagger 6, the first semi-cylinders 602 are uniformly distributed at intervals, and the second semi-cylinder 605 is arranged on the peripheral wall of the outer protrusion 604 at the bottom of the sagger 6; when the inner groove 603 and the outer protrusion 604 are fitted and overlapped, the first semi-cylinder 602 and the second semi-cylinder 605 have the same cross section.
Example 1:
the first step is as follows: obtaining a dry electronic ceramic blank to be fired by adopting dry pressing molding, slurry dipping, sand spraying and drying; manufacturing a sintered gasket by the same process;
the second step is that: placing the first-step sintering gasket into a sintering sagger, and placing a blank to be sintered on a ceramic sintering gasket;
the third step: putting the sagger obtained in the second step into a freezing chamber, wherein the temperature of the freezing chamber is set to be-10 to-5 ℃, the freezing chamber is decreased at the speed of-5 ℃ per hour averagely, and the freezing time is 2 to 3 hours;
the fourth step: quickly putting the sagger obtained in the third step into a high-pressure carbon dioxide preheating chamber for preheating, wherein the transfer time is 5-15 seconds, the preheating temperature is 75-90 ℃, the air pressure is 0.5-1 MPa, and the preheating time is 10-30 minutes;
the fifth step: putting the sagger obtained in the fourth step into a carbon dioxide heating furnace, heating to 700-900 ℃ at the heating rate of 100-300 ℃ per hour, and preserving heat for 1-2 hours; the heating furnace is provided with an air inlet and an air outlet, the air inlet is connected with the carbon dioxide storage device through a pipeline, an air inlet fan is arranged on the pipeline, and the air outlet is connected with the cooling device through a pipeline;
and a sixth step: and transferring the sagger obtained in the fifth step into a sintering furnace, and sintering for 6-8 hours at 1200-1700 ℃.
Example 2:
the first step is as follows: obtaining a dry electronic ceramic blank to be fired by dry pressing molding, slurry dipping, sand spraying and drying; manufacturing a sintered gasket by the same process;
the second step is that: placing the first-step sintering gasket into a sintering sagger, and placing a blank to be sintered on a ceramic sintering gasket;
the third step: putting the sagger obtained in the second step into a freezing chamber, wherein the temperature of the freezing chamber is set to be-10 to DEG C, the temperature of the freezing chamber is reduced at the speed of-5 ℃ per hour on average, and the freezing time is 2 hours;
the fourth step: quickly putting the sagger obtained in the third step into a high-pressure carbon dioxide preheating chamber for preheating, wherein the transfer time is 15 seconds, the preheating temperature is 75 ℃, the air pressure is 1MPa, and the preheating time is 20 minutes;
the fifth step: putting the sagger obtained in the fourth step into a carbon dioxide heating furnace, heating to 900 ℃ at the temperature rising speed of 200 ℃ per hour, and preserving heat for 1-2 hours; the heating furnace is provided with an air inlet and an air outlet, the air inlet is connected with a carbon dioxide storage device through a pipeline, an air inlet fan is arranged on the pipeline, and the air outlet is connected with a cooling device through a pipeline;
and a sixth step: and transferring the sagger obtained in the fifth step into a sintering furnace, and sintering for 6 hours at 1600 ℃.
Example 3:
the first step is as follows: obtaining a dry electronic ceramic blank to be fired by adopting dry pressing molding, slurry dipping, sand spraying and drying; manufacturing a sintered gasket by the same process;
the second step is that: placing the first-step sintering gasket into a sintering sagger, and placing a blank to be sintered on a ceramic sintering gasket;
the third step: putting the sagger obtained in the second step into a freezing chamber, wherein the temperature of the freezing chamber is set to be-5 ℃, the freezing chamber is decreased at the speed of-5 ℃ per hour averagely, and the freezing time is 3 hours;
the fourth step: quickly putting the sagger obtained in the third step into a high-pressure carbon dioxide preheating chamber for preheating, wherein the transfer time is 15 seconds, the preheating temperature is 90 ℃, the air pressure is 0.5MPa, and the preheating time is 30 minutes;
the fifth step: putting the sagger obtained in the fourth step into a carbon dioxide heating furnace, heating to 900 ℃ at the temperature rising speed of 300 ℃ per hour, and preserving heat for 1 hour; the heating furnace is provided with an air inlet and an air outlet, the air inlet is connected with the carbon dioxide storage device through a pipeline, an air inlet fan is arranged on the pipeline, and the air outlet is connected with the cooling device through a pipeline;
and a sixth step: and transferring the sagger obtained in the fifth step into a sintering furnace, and sintering for 6 hours at 1700 ℃.
Example 4:
the first step is as follows: obtaining a dry electronic ceramic blank to be fired by dry pressing molding, slurry dipping, sand spraying and drying; manufacturing a sintered gasket by the same process;
the second step is that: placing the first-step sintering gasket into a sintering sagger, and placing a blank to be sintered on a ceramic sintering gasket;
the third step: putting the sagger obtained in the second step into a freezing chamber, wherein the temperature of the freezing chamber is set to be 8 ℃ below zero, the freezing chamber is decreased at the speed of 5 ℃ below zero per hour, and the freezing time is 3 hours;
the fourth step: quickly putting the sagger obtained in the third step into a high-pressure carbon dioxide preheating chamber for preheating, wherein the transfer time is 12 seconds, the preheating temperature is 80 ℃, the air pressure is 0.8MPa, and the preheating time is 25 minutes;
the fifth step: putting the sagger obtained in the fourth step into a carbon dioxide heating furnace, heating to 700 ℃ at the temperature rising speed of 75 ℃ per hour, and preserving heat for 2 hours; the heating furnace is provided with an air inlet and an air outlet, the air inlet is connected with the carbon dioxide storage device through a pipeline, an air inlet fan is arranged on the pipeline, and the air outlet is connected with the cooling device through a pipeline;
and a sixth step: and transferring the sagger obtained in the fifth step into a sintering furnace, and sintering for 6 hours at 1650 ℃.
The sintered gasket is slightly larger than the bottom of the blank to be sintered, the bottom of the blank to be sintered is completely covered when the sintered gasket is placed, all transfer processes are stable, and the sintered gasket and the bottom of the blank to be sintered do not displace.
The working principle is as follows: after the dry die-casting molded blank is dried and frozen, the blank is relatively stable, and the solubility of polyvinyl alcohol can be reduced after the blank is frozen, so that some water can be discharged; the temperature of the preheating chamber is slightly higher than the melting point of the polyvinyl alcohol, and as the blank discharges some moisture after being frozen, the solubility of the heated polyvinyl alcohol is increased, the concentration is improved, and the adhesiveness is stronger; the blank after being frozen is heated to the inner layer one by one, the outer layer is heated firstly, the water loss is fast, the structure of the inner layer is in a stable state to play a supporting role when the outer layer is heated, when the outer layer is heated and the water is lost, the outer layer begins to be hardened to form a fine channel, the inner layer is gradually heated, and the outer layer plays a supporting role, so that the blank structure is relatively stable in the preheating process, and redundant water can be discharged; compared with the condition of not freezing or heating higher and faster, fine channels are not formed in the green body, and the interior small molecules which are heated too high or volatilized too fast can generate higher pressure in the green body due to being incapable of being removed in time, so that the green body has various defects of bubbling, swelling, cracking, layering, deformation and the like, the yield of the whole process can be reduced, and the perfect sintering of the green body can be further influenced. The high-pressure carbon dioxide can form pressure for the periphery of the blank, so that the bubbles generated by the fact that the volatile micromolecules in the polyvinyl alcohol heating and melting process are not discharged in time are prevented, and the influence on the blank is avoided. After the blank is transferred into a heating furnace, the discharged polyvinyl alcohol can be volatilized when the temperature reaches 700-900 ℃, and the discharged polyvinyl alcohol is discharged out of the system through the circulating cooling of carbon dioxide gas, meanwhile, the carbon dioxide well prevents the polyvinyl alcohol from being burnt under the high-temperature condition, and the influence of the discharged polyvinyl alcohol on the blank is small. The blank is because of the end puts the gasket of same material with the technology when sintering, and at the in-process of high temperature sintering, because produced tiny passageway can be filled by electronic ceramic material when getting rid of polyvinyl alcohol before, consequently the blank can reduce when sintering, and blank and gasket are because of same material and technology, and the shrinkage factor is comparatively the same, and blank bottom and gasket upper surface production displacement are less or can ignore, and the blank can not produce the deformation because of direct and sagger contact because of the friction.
Claims (6)
1. A sintering method of electronic ceramics is characterized by comprising the following steps:
the first step is as follows: obtaining a dry electronic ceramic blank to be fired by adopting dry pressing molding, slurry dipping, sand spraying and drying; manufacturing a sintered gasket by the same process;
the second step is that: placing the first-step sintering gasket into a sintering sagger, and placing a blank to be sintered on a ceramic sintering gasket;
the third step: placing the sagger obtained in the second step into a freezing chamber, wherein the temperature of the freezing chamber is set to be-10 to-5 ℃, the freezing chamber is decreased at the speed of-5 ℃ per hour averagely, and the freezing time is 2 to 3 hours;
the fourth step: quickly putting the sagger obtained in the third step into a high-pressure carbon dioxide preheating chamber for preheating, wherein the transfer time is 5-15 seconds, the preheating temperature is 75-90 ℃, the air pressure is 0.5-1 MPa, and the preheating time is 10-30 minutes;
the fifth step: putting the sagger obtained in the fourth step into a carbon dioxide heating furnace, heating to 700-900 ℃ at the heating rate of 100-300 ℃ per hour, and preserving heat for 1-2 hours; the heating furnace is provided with an air inlet and an air outlet, the air inlet is connected with a carbon dioxide storage device through a pipeline, an air inlet fan is arranged on the pipeline, and the air outlet is connected with a cooling device through a pipeline;
and a sixth step: and transferring the sagger obtained in the fifth step into a sintering furnace, and sintering for 6-8 hours at 1200-1700 ℃.
2. The method for sintering an electronic ceramic according to claim 1, wherein: the sintering gasket is slightly larger than the bottom of the blank to be sintered, the bottom of the blank to be sintered is completely covered when the sintering gasket is placed, all transfer processes are stable, and the sintering gasket and the bottom of the blank to be sintered do not displace.
3. The method for sintering an electronic ceramic according to claim 1, wherein: the temperature of the freezing chamber is set to be-5 ℃, and the freezing time is 3 hours.
4. The method for sintering an electronic ceramic according to claim 1, wherein: the temperature of the preheating chamber is set to be 75 ℃, the air pressure is 0.5MPa, and the time is 20 minutes.
5. The method for sintering an electronic ceramic according to claim 1, wherein: and the carbon dioxide enters the carbon dioxide storage device through the cooling circulation of the air outlet during the work of the heating furnace.
6. The method for sintering an electronic ceramic according to claim 1, wherein: the temperature of the sintering furnace is set to 1600 ℃, the sintering time is 6 hours, and the sintered product is naturally cooled to 100 ℃ and discharged.
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| CN108752009B true CN108752009B (en) | 2023-04-14 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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