CN104860682B - Cofired ceramic heating member preparation technology - Google Patents
Cofired ceramic heating member preparation technology Download PDFInfo
- Publication number
- CN104860682B CN104860682B CN201410066362.0A CN201410066362A CN104860682B CN 104860682 B CN104860682 B CN 104860682B CN 201410066362 A CN201410066362 A CN 201410066362A CN 104860682 B CN104860682 B CN 104860682B
- Authority
- CN
- China
- Prior art keywords
- sintering
- heating body
- ceramic heating
- ceramic
- mass percent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Ceramic Products (AREA)
- Resistance Heating (AREA)
Abstract
The invention relates to the technical field of heating member preparation and especially relates to a cofired ceramic heating member preparation technology. The cofired ceramic heating member preparation technology orderly comprises material blending, ball milling, drainage, molding and drying, printing, lamination, sintering and electrode connection. The cofired ceramic heating member preparation technology has simple processes. A blank is sintered under normal pressure in a tunnel kiln-combined reduction sintering atmosphere so that continuous production is realized, production efficiency is high, a liquid sintering method is used, a sintering temperature is low, a production cost is low and large scale production is realized.
Description
Technical field
The present invention relates to the fabricating technology field of calandria, more particularly, to a kind of ceramic heating body of cofired materials
Preparation technology.
Background technology
Silicon nitride heating plate is that one kind is sent out with reference to high-performance silicon nitride ceramics matrix and long-life powerful high-temperature metal
The device of heated filament, it has small volume, and power is big and the features such as the thermal efficiency is high, is also demonstrate,proved by silicon nitride heating plate heat production simultaneously
Bright is a kind of safe and reliable heating system.
, as a kind of covalent key compound, diffusion coefficient is little, does not have fusing point for silicon nitride, about decomposes ammonification and silicon in 2173K,
It is difficult to sinter.At present, traditional silicon nitride ceramics heating plate is tungsten filament to be embedded in alpha-silicon nitride powders be molded into plates hot pressing
Sintering forms, and due to being limited by technique, tungsten filament is difficult to positioning to the heater of this technique productions, causes position inclined in forming process
Move, cause heater integrally to conduct heat inequality, simultaneously because tungsten filament and beta-silicon nitride powder have obvious interface, be difficult to after sintering become
Integrally, tungsten filament and ceramic contact surface form space, form selective oxidation, reduce the service life of fever tablet in heating process.Mesh
The sintering of front silicon nitride ceramics heating plate also has using reaction-sintered and hot pressed sintering, but reaction-sintered low density, mechanics
Poor performance, although hot pressed sintering density is high, mechanical property is good, relatively costly it is difficult to large-scale production.Therefore, the above
Problems demand solves.
Content of the invention
Present invention aims to the deficiencies in the prior art, provide a kind of high, sharp beneficial to continuous production, production efficiency
Preparation technology in large-scale production, the ceramic heating body of the cofired materials of low production cost.
The present invention is achieved through the following technical solutions.
A kind of preparation technology of the ceramic heating body of cofired materials, comprises the following steps that：
A, batch mixing：Weigh the Si of 65-98% by mass percentage3N4, 0.1-10% MgO, 0.1-5% Y2O3、0.1-5%
Al2O3, the SiO of 0.1-5%2, the La of 0.1-5%2O3, the BN of 0.1-5% mixing and stirring, make ceramic substrate powder；
B, ball milling：The ceramic substrate powder that step a is obtained adds mill ball, solvent and adhesive and puts in ball grinder
Carry out wet ball grinding, the time of wet ball grinding is 8-24h；Wet ball grinding can improve mill efficiency, so that diameter of particle is reduced, compare table
Area increases, increased activity.
C, deaeration：Compound after wet ball grinding in step b is carried out under vacuum deaeration；
D, molding and drying：Compound casting machine in step c is cast and makes ceramic substrate or set using rolling film
Standby be rolled into ceramic substrate, and ceramic substrate is dried；
E, printing：By silk-screen printing technique, resistance slurry is printed through ceramic substrate surface dried in step d, electricity
Resistance paste forms the heating circuit of reciprocal inflection structure on the surface of ceramic substrate；
F, laminate：The ceramic substrate that the ceramic substrate that a piece of step d is obtained is printed with heating circuit with a piece of step e is folded
It is pressed into base substrate；
G, sintering：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, then uses case
The base substrate being embedded in insulating powder is sintered by formula stove or tunnel cave at ambient pressure, and sintering atmosphere is nitrogen and hydrogen mixed gas
Body, blank sintering is obtained ceramic heating body semi-finished product；Reductive sintered atmosphere is combined in normal pressure-sintered base substrate using tunnel cave, can
Realize continuous production, yield is changed into daily 48 batches from original daily 1 batch, and production efficiency improves 48 times, and continuous metaplasia
Produce and be beneficial to energy-conservation, substantially reduce production cost, accomplish scale production beneficial to enterprise；Simultaneously because hydrogen atom radius very little, easily
Be conducive to, in diffusion, hole elimination of holding one's breath, the oxonium ion in aluminium oxide lattice can also be made in a hydrogen atmosphere relatively easily to lose
Go, form room, accelerate oxonium ion diffusion, therefore can be effectively facilitated sintering in a hydrogen atmosphere, so that ceramic is obtained
Consistency well.
H, receiving electrode：The two ends of ceramic heating body semi-finished product or sidepiece are carried out plating nickel on surface process, at nickel plating
Position after reason carries out soldering extraction electrode, prepared ceramic heating body finished product.
Wherein, step g sintering is specially：By step f be obtained base substrate be placed in graphite crucible or molybdenum crucible, and imbed every
From powder, then with batch-type furnace or tunnel cave, the base substrate being embedded in insulating powder is sintered at ambient pressure, sintering atmosphere is nitrogen
And hydrogen gas mixture, percent by volume in mixed gas for the hydrogen is 5-29%, volume basis in mixed gas for the nitrogen
Than for 71%-95%, blank sintering is obtained ceramic heating body semi-finished product.The percent by volume of hydrogen is more than 1% it is ensured that gaseous mixture
Restitutive protection's effect of body, simultaneously because hydrogen belongs to flammable explosive gas, therefore makes the percent by volume of hydrogen be less than
40%, reduce potential safety hazard, the percent by volume of therefore hydrogen 1-40% make mixed gas can simultaneously work as reproducibility protection and
Explosion-proof effect；Hydrogen in the present invention is to decompose by ammonia to make, higher with respect to the nitrogen cost of outsourcing, therefore mixed
The percent by volume making nitrogen in conjunction gas is 60%-99%, higher than the percent by volume of the 1-40% of hydrogen, can save further
Production cost.
Wherein, step g sintering is specially：By step f be obtained base substrate be placed in graphite crucible or molybdenum crucible, and imbed every
From powder, the insulating powder burying burning is Si3N4With the mixture of BN, then the base substrate in insulating powder will be embedded in batch-type furnace or tunnel cave
It is sintered at ambient pressure, sintering atmosphere is nitrogen and hydrogen gas mixture, percent by volume in mixed gas for the hydrogen is
10-25%, percent by volume in mixed gas for the nitrogen is 75%-90%, controls the dew point temperature of water vapour in mixed gas low
In 50 DEG C, blank sintering is obtained ceramic heating body semi-finished product.
Wherein, tunnel cave used by step g sintering is divided into dumping area, sintering zone and the cooling zone being sequentially connected, dumping area, burning
The temperature of interface and cooling zone is respectively 300-1300 DEG C, 1600-1850 DEG C, 1850-25 DEG C, and base substrate is respectively in dumping area, burning
The sintering time of interface and cooling zone is 3-8h, 1-3h, 8-12h.Replace traditional batch-type furnace, because tunnel cave be divided into dumping area,
Sintering zone and cooling zone, make base substrate can realize the operation of dumping, high temperature sintering and cooling successively, the blank sintering of last batch is complete
Bi Shi, tunnel cave need not experience long intensification again, and the base substrate that again can put into next batch immediately is sintered, and eliminates
The operation that batch-type furnace need to repeatedly heat up, cool down in the multiple batches of base substrate of continuous sintering, can achieve continuous circulation using tunnel cave
Metaplasia is produced, and yield is changed into daily 48 batches from original daily 1 batch, and production efficiency improves 48 times, and production efficiency greatly improves,
And more conducively energy-conservation, substantially reduce production cost；What 1600-1850 DEG C of sintering temperature ensured ceramic heating body fires effect
Good, avoid the hydrogen explosion that high temperature causes simultaneously.
Resistance slurry in step e is made up of the raw material of following mass percent：
Solid formation 70-90%
Carrier 10-30%；
Wherein, solid formation is made up of the raw material of following mass percent：
Conductive phase 60-99%
Glass phase 1-40%；
Conductive phase is the mixture of one or more of tungsten, manganese, molybdenum；
Glass is made up of the raw material of following mass percent：
Si3N465-98%
MgO 0.1-10%
Y2O30.1-5%
Al2O30.1-5%
SiO20.1-5%
La2O30.1-5%
BN 0.1-5%；
Wherein, carrier is made up of the raw material of following mass percent：
Terpineol 50-80%
Tributyl citrate 8-30%
Butyl carbitol amyl acetate 8-30%
Oleum Ricini 0.1-2%
Ethyl cellulose 3-10%
Lecithin 0.3-1.5%
Span 85 0.5-3%.
In resistance slurry, conductive phase plays the effect of conduction；Glass phase be sintering when from grill thoroughly anti-reflection layer and cementation；
Carrier is mainly provides conductive phase effect mutually scattered with glass, in the constitutive material of carrier, terpineol and butyl carbitol
All as solvent, as plasticiser, as thixotropic agent, ethyl cellulose is thickening agent to Oleum Ricini to tributyl citrate to amyl acetate,
, all as surfactant, carrier makes resistance slurry have by materialization effect to be applied to silk screen printing for lecithin and Span 85
The rheological property of viscosity, thixotropy etc. is so that silk screen printing can obtain printing precision and the effect of needs.
Terpineol colourless liquid or low melting point clear crystals body, have Flos Caryophylli taste, and its molecular formula is C10H18O, molecular weight is
154.2516, relative density is 0.9337 (20/4 DEG C), and solidification point is 2 DEG C.Optical rotation is [α] -0 ° of 10'～+0 ° 10 ', boiling range
For 214～224 DEG C, it is refracted as nD (20 DEG C) 1.4825～1.4850.1 part of terpineol can be dissolved in 2 parts（Volume）70% ethanol is molten
In liquid, it is slightly soluble in water and glycerol, can be used as senior solvent.
The chemical name of citric acid be 3- hydroxyl -3- carboxyl 1,3-propanedicarboxylic acid tributyl, be a kind of ester type compound, be colourless or
Weak yellow liquid, its molecular formula is C18H32O7, molal weight is 360 44 g/mol, can be with acetone, CCl4, mineral oil, vinegar
Acid, Oleum Ricini, alcohol and its solvent phase are mixed；Water insoluble, nonpoisonous and tasteless, volatility is little, heat-resisting fast light water-fast, with vinyl tree
The compatibilitys such as fat, cellulose acetate, acetoxybutanoic acid cellulose, ethyl cellulose, benzylcellulose are good, are that plasticising efficiency is preferable
Plasticizer；Antibacterium of also having does not grow antibacterial, nonirritant, anti-flammability and degradability again.
Also known as butyl acetate, its molecular formula is C to butyl carbitol amyl acetate10H20O4, molecular weight is
204.26, boiling point is 246.4 DEG C（0.101mpa）, flash-point is 116 DEG C, is slightly soluble in water, can and most of immiscible organic solvents.Fourth
Base carbitol amyl acetate due to having higher boiling point, beneficial to high temperature sintering.
Oleum Ricini is colourless or micro- yellowy clarification thick liquid, the light then micro-pungent of abnormal smells from the patient, and Oleum Ricini is easy in ethanol
Molten, can arbitrarily mix with dehydrated alcohol, chloroform, ether or glacial acetic acid；Relative density（d20℃4℃）：0.9550-0.9700, folding
Optical index（n20℃D) ：1.4765-1.4819, (E020 DEG C of viscosity）More than 14, freezing point（℃）：- 10, burning-point（℃）：
322, iodine number (g iodine/100g oil）：82-86, saponification number（MgKOH/g oil）：176-187, thiocyanogen value：81-82, total fatty acids contain
Amount（%) about 96, fatty acid mean molecule quantity is 290-300.Oleum Ricini is fine to celluloid, ethyl cellulose, acetate butyrate
Dimension element, polyamide, fourth tripolycyanamide (or carbamide) formaldehyde resin, Colophonium, Lac etc. have good intermiscibility, as
Thixotropic agent can increase the viscosity of resistance slurry, and makes it have thixotropy.
Also known as cellulosic ether, its softening point is 135 ~ 155 DEG C to ethyl cellulose, and fusing point is 165 ~ 185 DEG C, apparent specific gravity (gd)
0.3 ~ 0.4 gram/cc, 1.07 ~ 1.18 grams/cc of relative density, it dissolves in more organic solvent, in resistance slurry
Play the effect of thickening agent in material.
Lecithin belongs to a kind of mixture, is one group of filemot oils and fats being present among animal vegetable tissue and yolk
Property material, its constituent includes phosphoric acid, choline, fatty acid, glycerol, glycolipid, triglyceride and phospholipid（As phosphatidyl gallbladder
Alkali, PHOSPHATIDYL ETHANOLAMINE and phosphatidylinositols）, dissolubility in water for the lecithin is relatively low.In aqueous, according to different water
Close（Hydration, aquation）And temperature conditionss, its phospholipid can form liposome, lipid bilayer, micelle（micelles）
Or plate layer structure, therefore lecithin has both sexes for one kind（amphoteric）The surfactant of feature.
The molecular formula of Span 85 is C60H108O8, its molecular weight is 957.51, and its amber oily liquids has fat note,
It is dissolved in dimethylbenzene, mineral oil, Oleum Gossypii semen and acetone, relative density is 0.92～0.98, and fusing point is 10 DEG C, hydrophilic and oleophilic value
（HLB）For 1.8, viscosity about 200mPa s（25℃）.Span 85 has fixing hydrophilic lipophilic group, fixed in the surface energy of solution
To arrangement, monolayer can be formed in liquid surface, and significantly decrease interfacial tension between two kinds of liquid, and surface tension can be made
It is remarkably decreased.
Preferably, the resistance slurry in step e is made up of the raw material of following mass percent：
Solid formation 75-85%
Carrier 15-25%；
Wherein, solid formation is made up of the raw material of following mass percent：
Conductive phase 70-90%
Glass phase 10-30%；
Conductive phase is the mixture of one or more of tungsten, manganese, molybdenum；
Glass is made up of the raw material of following mass percent：
Si3N475-90%
MgO 4-8%
Y2O32-4%
Al2O32-4%
SiO22-4%
La2O32-4%
BN 2-4%；
Wherein, carrier is made up of the raw material of following mass percent：
Terpineol 60-70%
Tributyl citrate 12-25%
Butyl carbitol amyl acetate 12-25%
Oleum Ricini 0.5-1.5%
Ethyl cellulose 4-8%
Lecithin 0.5-1.2%
Span 85 1-2.5%.
It is more highly preferred to, the resistance slurry in step e is made up of the raw material of following mass percent：
Solid formation 80%
Carrier 20%；
Wherein, solid formation is made up of the raw material of following mass percent：
Conductive phase 80%
Glass phase 20%；
Conductive phase is the mixture of one or more of tungsten, manganese, molybdenum；
Glass is made up of the raw material of following mass percent：
Si3N480%
MgO 7%
Y2O33%
Al2O32%
SiO23%
La2O32%
BN 3%；
Wherein, carrier is made up of the raw material of following mass percent：
Terpineol 65%
Tributyl citrate 14%
Butyl carbitol amyl acetate 12%
Oleum Ricini 1%
Ethyl cellulose 5%
Lecithin 1%
Span 85 2%.
Wherein, prepared ceramic heating body is in one of tabular, pole shape, circular tube shaped, and pole shape or circular tube shaped are made pottery
Porcelain calandria is rolled by tabular ceramic heating body and forms.
Beneficial effects of the present invention are：The preparation technology of the ceramic heating body of the cofired materials of the present invention sequentially passes through mixed
Material, ball milling, it is filtered dry, molding and drying, prints, laminate, sintering and receiving electrode operation, whole manufacturing process is simple, using tunnel
Kiln combines reductive sintered atmosphere in normal pressure-sintered base substrate, beneficial to continuous production, production efficiency height, and is sintered to liquid-phase sintering,
Sintering temperature is low, low production cost, beneficial to accomplishing scale production；And, the heating layer of the ceramic heating body of the present invention is served as reasons
The heating circuit of resistance slurry printing, in the base substrate that ceramic substrate is overrided to form, the position of heating layer is placed in the middle, and radiating is all
Even, internal combustion is fine and close, long service life.
Specific embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1.
A kind of preparation technology of the ceramic heating body of cofired materials of the present embodiment, it comprises the following steps that：
A, batch mixing：Weigh 65% Si by mass percentage3N4, 10% MgO, 5% Y2O3, 5% Al2O3, 5% SiO2、
5% La2O3, 5% BN and mixing and stirring, make ceramic substrate powder；
B, ball milling：The ceramic substrate powder that step a is obtained adds mill ball, solvent and adhesive and puts in ball grinder
Carry out wet ball grinding, the time of wet ball grinding is 8h；
C, deaeration：Compound after wet ball grinding in step b is carried out under vacuum deaeration；
D, molding and drying：Compound casting machine in step c is cast and makes ceramic substrate or set using rolling film
Standby be rolled into ceramic substrate, and ceramic substrate is dried；
E, printing：By silk-screen printing technique, resistance slurry is printed through ceramic substrate surface dried in step d, electricity
Resistance paste forms the heating circuit of reciprocal inflection structure on the surface of ceramic substrate；Resistance slurry is 70% by mass percent
Solid formation and 30% carrier composition；Tungsten and 40% glass phase composition that solid formation is 60% by mass percent；Glass by
65% Si3N4, 10% MgO, 5% Y2O3, 5% Al2O3, 5% SiO2, 5% La2O3, 5% BN mixing and stirring and
Become；Terpineol that carrier is 50% by mass percent, 30% tributyl citrate, 30% butyl carbitol amyl acetate, 2%
Oleum Ricini, 10% ethyl cellulose, 1.5% lecithin, 3% Span 85 form；
F, laminate：The ceramic substrate that the ceramic substrate that a piece of step d is obtained is printed with heating circuit with a piece of step e is folded
It is pressed into base substrate；
G, sintering：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, bury burning every
It is Si from powder3N4With the mixture of BN, then with batch-type furnace or tunnel cave, the base substrate being embedded in insulating powder is burnt at ambient pressure
Knot, tunnel cave is divided into dumping area, sintering zone and the cooling zone being sequentially connected, and the temperature of dumping area, sintering zone and cooling zone is respectively
For 300 DEG C, 1600 DEG C, 25 DEG C, the sintering time in dumping area, sintering zone and cooling zone is 3h, 1h, 8h to base substrate respectively, sintering
Atmosphere is nitrogen and hydrogen gas mixture, and percent by volume in mixed gas for the hydrogen is 1%, and nitrogen is in mixed gas
Percent by volume is 99%, controls the dew point temperature of water vapour in mixed gas to be less than 50 DEG C, blank sintering is obtained ceramic heating body
Semi-finished product；
H, receiving electrode：The two ends of ceramic heating body semi-finished product or sidepiece are carried out plating nickel on surface process, at nickel plating
Position after reason carries out soldering extraction electrode, prepared ceramic heating body finished product.
Embodiment 2.
A kind of preparation technology of the ceramic heating body of cofired materials of the present embodiment, it comprises the following steps that：
A, batch mixing：Weigh 98% Si by mass percentage3N4, 0.5% MgO, 0.5% Y2O3, 0.2% Al2O3、0.3%
SiO2, 0.2% La2O3, 0.3% BN and mixing and stirring, make ceramic substrate powder；
B, ball milling：The ceramic substrate powder that step a is obtained adds mill ball, solvent and adhesive and puts in ball grinder
Carry out wet ball grinding, the time of wet ball grinding is 11h；
C, deaeration：Compound after wet ball grinding in step b is carried out under vacuum deaeration；
D, molding and drying：Compound casting machine in step c is cast and makes ceramic substrate or set using rolling film
Standby be rolled into ceramic substrate, and ceramic substrate is dried；
E, printing：By silk-screen printing technique, resistance slurry is printed through ceramic substrate surface dried in step d, electricity
Resistance paste forms the heating circuit of reciprocal inflection structure on the surface of ceramic substrate；Resistance slurry is 90% by mass percent
Solid formation and 10% carrier composition；Manganese and 1% glass phase composition that solid formation is 99% by mass percent；Glass is by 98%
Si3N4, 0.5% MgO, 0.5% Y2O3, 0.2% Al2O3, 0.3% SiO2, 0.2% La2O3, 0.3% BN mix and blend
Uniformly form；Terpineol that carrier is 80% by mass percent, 8% tributyl citrate, 8% butyl carbitol amyl acetate,
0. 2% Oleum Ricini, 3% ethyl cellulose, 0.3% lecithin, 0.5% Span 85 form；
F, laminate：The ceramic substrate that the ceramic substrate that a piece of step d is obtained is printed with heating circuit with a piece of step e is folded
It is pressed into base substrate；
G, sintering：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, bury burning every
It is Si from powder3N4With the mixture of BN, then with batch-type furnace or tunnel cave, the base substrate being embedded in insulating powder is burnt at ambient pressure
Knot, tunnel cave is divided into dumping area, sintering zone and the cooling zone being sequentially connected, and the temperature of dumping area, sintering zone and cooling zone is respectively
For 500 DEG C, 1650 DEG C, 100 DEG C, the sintering time in dumping area, sintering zone and cooling zone is 3h, 2h, 9h to base substrate respectively, sintering
Atmosphere is nitrogen and hydrogen gas mixture, and percent by volume in mixed gas for the hydrogen is 40%, and nitrogen is in mixed gas
Percent by volume is 60%, controls the dew point temperature of water vapour in mixed gas to be less than 45 DEG C, blank sintering is obtained ceramic heating body
Semi-finished product；
H, receiving electrode：The two ends of ceramic heating body semi-finished product or sidepiece are carried out plating nickel on surface process, at nickel plating
Position after reason carries out soldering extraction electrode, prepared ceramic heating body finished product.
Embodiment 3.
A kind of preparation technology of the ceramic heating body of cofired materials of the present embodiment, it comprises the following steps that：
A, batch mixing：Weigh 75% Si by mass percentage3N4, 8% MgO, 4% Y2O3, 4% Al2O3, 3% SiO2、
3% La2O3, 3% BN and mixing and stirring, make ceramic substrate powder；
B, ball milling：The ceramic substrate powder that step a is obtained adds mill ball, solvent and adhesive and puts in ball grinder
Carry out wet ball grinding, the time of wet ball grinding is 14h；
C, deaeration：Compound after wet ball grinding in step b is carried out under vacuum deaeration；
D, molding and drying：Compound casting machine in step c is cast and makes ceramic substrate or set using rolling film
Standby be rolled into ceramic substrate, and ceramic substrate is dried；
E, printing：By silk-screen printing technique, resistance slurry is printed through ceramic substrate surface dried in step d, electricity
Resistance paste forms the heating circuit of reciprocal inflection structure on the surface of ceramic substrate；Resistance slurry is 75% by mass percent
Solid formation and 25% carrier composition；Molybdenum and 30% glass phase composition that solid formation is 70% by mass percent；Glass by
75% Si3N4, 8% MgO, 4% Y2O3, 4% Al2O3, 3% SiO2, 3% La2O3, 3% BN mixing and stirring forms；
Terpineol that carrier is 60% by mass percent, 25% tributyl citrate, 25% butyl carbitol amyl acetate, 1.5%
Oleum Ricini, 8% ethyl cellulose, 1.2% lecithin, 2.5% Span 85 form；
F, laminate：The ceramic substrate that the ceramic substrate that a piece of step d is obtained is printed with heating circuit with a piece of step e is folded
It is pressed into base substrate；
G, sintering：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, bury burning every
It is Si from powder3N4With the mixture of BN, then with batch-type furnace or tunnel cave, the base substrate being embedded in insulating powder is burnt at ambient pressure
Knot, tunnel cave is divided into dumping area, sintering zone and the cooling zone being sequentially connected, and the temperature of dumping area, sintering zone and cooling zone is respectively
For 700 DEG C, 1700 DEG C, 200 DEG C, the sintering time in dumping area, sintering zone and cooling zone is 5h, 3h, 10h to base substrate respectively, burns
Stagnation of QI atmosphere is nitrogen and hydrogen gas mixture, and percent by volume in mixed gas for the hydrogen is 15%, and nitrogen is in mixed gas
Percent by volume be 85%, control mixed gas in water vapour dew point temperature be less than 40 DEG C, blank sintering is obtained ceramic heat
Body semi-finished product；
H, receiving electrode：The two ends of ceramic heating body semi-finished product or sidepiece are carried out plating nickel on surface process, at nickel plating
Position after reason carries out soldering extraction electrode, prepared ceramic heating body finished product.
Embodiment 4.
A kind of preparation technology of the ceramic heating body of cofired materials of the present embodiment, it comprises the following steps that：
A, batch mixing：Weigh 90% Si by mass percentage3N4, 4% MgO, 2% Y2O3, 1% Al2O3, 1% SiO2、
1% La2O3, 1% BN and mixing and stirring, make ceramic substrate powder；
B, ball milling：The ceramic substrate powder that step a is obtained adds mill ball, solvent and adhesive and puts in ball grinder
Carry out wet ball grinding, the time of wet ball grinding is 18h；
C, deaeration：Compound after wet ball grinding in step b is carried out under vacuum deaeration；
D, molding and drying：Compound casting machine in step c is cast and makes ceramic substrate or set using rolling film
Standby be rolled into ceramic substrate, and ceramic substrate is dried；
E, printing：By silk-screen printing technique, resistance slurry is printed through ceramic substrate surface dried in step d, electricity
Resistance paste forms the heating circuit of reciprocal inflection structure on the surface of ceramic substrate；Resistance slurry is 85% by mass percent
Solid formation and 15% carrier composition；The glass phase composition of tungsten that solid formation is 30% by mass percent, 60% molybdenum and 10%；Glass
Glass by 90% Si3N4, 4% MgO, 2% Y2O3, 1% Al2O3, 1% SiO2, 1% La2O3, 1% BN mix and blend equal
Even form；Terpineol that carrier is 70% by mass percent, 12% tributyl citrate, 12% butyl carbitol amyl acetate,
0.5% Oleum Ricini, 4% ethyl cellulose, 0.5% lecithin, 1% Span 85 form；
F, laminate：The ceramic substrate that the ceramic substrate that a piece of step d is obtained is printed with heating circuit with a piece of step e is folded
It is pressed into base substrate；
G, sintering：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, bury burning every
It is Si from powder3N4With the mixture of BN, then with batch-type furnace or tunnel cave, the base substrate being embedded in insulating powder is burnt at ambient pressure
Knot, tunnel cave is divided into dumping area, sintering zone and the cooling zone being sequentially connected, and the temperature of dumping area, sintering zone and cooling zone is respectively
For 900 DEG C, 1750 DEG C, 300 DEG C, the sintering time in dumping area, sintering zone and cooling zone is 6h, 3h, 11h to base substrate respectively, burns
Stagnation of QI atmosphere is nitrogen and hydrogen gas mixture, and percent by volume in mixed gas for the hydrogen is 20%, and nitrogen is in mixed gas
Percent by volume be 80%, control mixed gas in water vapour dew point temperature be less than 35 DEG C, blank sintering is obtained ceramic heat
Body semi-finished product；
H, receiving electrode：The two ends of ceramic heating body semi-finished product or sidepiece are carried out plating nickel on surface process, at nickel plating
Position after reason carries out soldering extraction electrode, prepared ceramic heating body finished product.
Embodiment 5.
A kind of preparation technology of the ceramic heating body of cofired materials of the present embodiment, it comprises the following steps that：
A, batch mixing：Weigh 80% Si by mass percentage3N4, 7% MgO, 3% Y2O3, 2% Al2O3, 3% SiO2、
2% La2O3, 3% BN and mixing and stirring, make ceramic substrate powder；
B, ball milling：The ceramic substrate powder that step a is obtained adds mill ball, solvent and adhesive and puts in ball grinder
Carry out wet ball grinding, the time of wet ball grinding is 20h；
C, deaeration：Compound after wet ball grinding in step b is carried out under vacuum deaeration；
D, molding and drying：Compound casting machine in step c is cast and makes ceramic substrate or set using rolling film
Standby be rolled into ceramic substrate, and ceramic substrate is dried；
E, printing：By silk-screen printing technique, resistance slurry is printed through ceramic substrate surface dried in step d, electricity
Resistance paste forms the heating circuit of reciprocal inflection structure on the surface of ceramic substrate；Resistance slurry is 80% by mass percent
Solid formation and 20% carrier composition；The glass phase composition of tungsten that solid formation is 40% by mass percent, 40% manganese and 20%；Glass
Glass by 80% Si3N4, 7% MgO, 3% Y2O3, 2% Al2O3, 3% SiO2, 2% La2O3, 3% BN mix and blend equal
Even form；Terpineol that carrier is 65% by mass percent, 14% tributyl citrate, 12% butyl carbitol amyl acetate,
1% Oleum Ricini, 5% ethyl cellulose, 1% lecithin, 2% Span 85 form；
F, laminate：The ceramic substrate that the ceramic substrate that a piece of step d is obtained is printed with heating circuit with a piece of step e is folded
It is pressed into base substrate；
G, sintering：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, bury burning every
It is Si from powder3N4With the mixture of BN, then with batch-type furnace or tunnel cave, the base substrate being embedded in insulating powder is burnt at ambient pressure
Knot, tunnel cave is divided into dumping area, sintering zone and the cooling zone being sequentially connected, and the temperature of dumping area, sintering zone and cooling zone is respectively
For 1100 DEG C, 1800 DEG C, 400 DEG C, the sintering time in dumping area, sintering zone and cooling zone is 7h, 3h, 12h to base substrate respectively, burns
Stagnation of QI atmosphere is nitrogen and hydrogen gas mixture, and percent by volume in mixed gas for the hydrogen is 5%, and nitrogen is in mixed gas
Percent by volume be 95%, control mixed gas in water vapour dew point temperature be less than 30 DEG C, blank sintering is obtained ceramic heat
Body semi-finished product；
H, receiving electrode：The two ends of ceramic heating body semi-finished product or sidepiece are carried out plating nickel on surface process, at nickel plating
Position after reason carries out soldering extraction electrode, prepared ceramic heating body finished product.
Embodiment 6.
A kind of preparation technology of the ceramic heating body of cofired materials of the present embodiment, it comprises the following steps that：
A, batch mixing：Weigh 70% Si by mass percentage3N4, 9% MgO, 5% Y2O3, 4% Al2O3, 4% SiO2、
4% La2O3, 4% BN and mixing and stirring, make ceramic substrate powder；
B, ball milling：The ceramic substrate powder that step a is obtained adds mill ball, solvent and adhesive and puts in ball grinder
Carry out wet ball grinding, the time of wet ball grinding is 24h；
C, deaeration：Compound after wet ball grinding in step b is carried out under vacuum deaeration；
D, molding and drying：Compound casting machine in step c is cast and makes ceramic substrate or set using rolling film
Standby be rolled into ceramic substrate, and ceramic substrate is dried；
E, printing：By silk-screen printing technique, resistance slurry is printed through ceramic substrate surface dried in step d, electricity
Resistance paste forms the heating circuit of reciprocal inflection structure on the surface of ceramic substrate；Resistance slurry is 80% by mass percent
Solid formation and 20% carrier composition；The glass phase composition of manganese that solid formation is 20% by mass percent, 40% molybdenum and 40%；Glass
Glass by 70% Si3N4, 9% MgO, 5% Y2O3, 4% Al2O3, 4% SiO2, 4% La2O3, 4% BN mix and blend equal
Even form；Terpineol that carrier is 55% by mass percent, 20% tributyl citrate, 20% butyl carbitol amyl acetate,
1% Oleum Ricini, 2% ethyl cellulose, 1% lecithin, 1% Span 85 form；
F, laminate：The ceramic substrate that the ceramic substrate that a piece of step d is obtained is printed with heating circuit with a piece of step e is folded
It is pressed into base substrate；
G, sintering：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, bury burning every
It is Si from powder3N4With the mixture of BN, then with batch-type furnace or tunnel cave, the base substrate being embedded in insulating powder is burnt at ambient pressure
Knot, tunnel cave is divided into dumping area, sintering zone and the cooling zone being sequentially connected, and the temperature of dumping area, sintering zone and cooling zone is respectively
For 1300 DEG C, 1850 DEG C, 500 DEG C, the sintering time in dumping area, sintering zone and cooling zone is 8h, 2h, 12h to base substrate respectively, burns
Stagnation of QI atmosphere is nitrogen and hydrogen gas mixture, and percent by volume in mixed gas for the hydrogen is 10%, and nitrogen is in mixed gas
Percent by volume be 90%, control mixed gas in water vapour dew point temperature be less than 25 DEG C, blank sintering is obtained ceramic heat
Body semi-finished product；
H, receiving electrode：The two ends of ceramic heating body semi-finished product or sidepiece are carried out plating nickel on surface process, at nickel plating
Position after reason carries out soldering extraction electrode, prepared ceramic heating body finished product.
The performance testing index of the ceramic heating body that embodiment 1 ~ embodiment 6 is made is shown in Table 1.
Table 1
.
As it can be seen from table 1 the High anti bending strength of ceramic heating body that embodiment 1 ~ embodiment 6 is made, long service life,
Power stability, the efficiency of heating surface are high.
Finally it should be noted that above example is only in order to illustrating technical scheme, rather than the present invention is protected
The restriction of shield scope, although having made to explain to the present invention with reference to preferred embodiment, those of ordinary skill in the art should
Work as understanding, technical scheme can be modified or equivalent, without deviating from the reality of technical solution of the present invention
Matter and scope.
Claims (7)
1. a kind of preparation technology of the ceramic heating body of cofired materials it is characterised in that：Comprise the following steps that：
A, batch mixing：Weigh the Si of 65-98% by mass percentage3N4, 0.1-10% MgO, 0.1-5% Y2O3, 0.1-5%
Al2O3, the SiO of 0.1-5%2, the La of 0.1-5%2O3, the BN of 0.1-5% mixing and stirring, make ceramic substrate powder；
B, ball milling：The ceramic substrate powder that step a is obtained adds mill ball, solvent and adhesive putting in ball grinder to carry out
Wet ball grinding, the time of wet ball grinding is 8-24h；
C, deaeration：Compound after wet ball grinding in step b is carried out under vacuum deaeration；
D, molding and drying：Compound casting machine in step c is cast and makes ceramic substrate or rolled using rolling film device
Make ceramic substrate, and ceramic substrate is dried；
E, printing：By silk-screen printing technique, resistance slurry is printed through ceramic substrate surface dried in step d, resistance is starched
Material forms the heating circuit of reciprocal inflection structure on the surface of ceramic substrate；
F, laminate：The ceramic substrate that the ceramic substrate that a piece of step d is obtained is printed with heating circuit with a piece of step e laminates system
Become base substrate；
G, sintering：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, then uses batch-type furnace
Or the base substrate being embedded in insulating powder is sintered by tunnel cave at ambient pressure, sintering atmosphere is nitrogen and hydrogen gas mixture, base
Body sintering is obtained ceramic heating body semi-finished product；
H, receiving electrode：The two ends of ceramic heating body semi-finished product or sidepiece are carried out plating nickel on surface process, after Nickel Plating Treatment
Position carry out soldering extraction electrode, prepared ceramic heating body finished product；
Resistance slurry in step e is made up of the raw material of following mass percent：
Solid formation 70-90%
Carrier 10-30%；
Wherein, solid formation is made up of the raw material of following mass percent：
Conductive phase 60-99%
Glass phase 1-40%；
Conductive phase is the mixture of one or more of tungsten, manganese, molybdenum；
Glass is made up of the raw material of following mass percent：
Si3N465-98%
MgO 0.1-10%
Y2O30.1-5%
Al2O30.1-5%
SiO20.1-5%
La2O30.1-5%
BN 0.1-5%；
Wherein, carrier is made up of the raw material of following mass percent：
Terpineol 50-80%
Tributyl citrate 8-30%
Butyl carbitol amyl acetate 8-30%
Oleum Ricini 0.1-2%
Ethyl cellulose 3-10%
Lecithin 0.3-1.5%
Span 85 0.5-3%.
2. a kind of ceramic heating body of cofired materials according to claim 1 preparation technology it is characterised in that：Step g
Sintering is specially：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, then uses batch-type furnace
Or the base substrate being embedded in insulating powder is sintered by tunnel cave at ambient pressure, sintering atmosphere is nitrogen and hydrogen gas mixture, hydrogen
Percent by volume in mixed gas for the gas is 1-40%, and percent by volume in mixed gas for the nitrogen is 60%-99%, base substrate
Sintering is obtained ceramic heating body semi-finished product.
3. a kind of ceramic heating body of cofired materials according to claim 1 preparation technology it is characterised in that：Step g
Sintering is specially：The base substrate that step f is obtained is placed in graphite crucible or molybdenum crucible, and imbeds insulating powder, buries the insulating powder of burning
For Si3N4With the mixture of BN, then with batch-type furnace or tunnel cave, the base substrate being embedded in insulating powder is sintered at ambient pressure,
Sintering atmosphere is nitrogen and hydrogen gas mixture, and percent by volume in mixed gas for the hydrogen is 5-29%, and nitrogen is in gaseous mixture
Percent by volume in body is 71%-95%, and blank sintering is obtained ceramic heating body semi-finished product.
4. a kind of ceramic heating body of cofired materials according to claim 1 preparation technology it is characterised in that：Step g
Tunnel cave used by sintering is divided into dumping area, sintering zone and the cooling zone being sequentially connected, the temperature of dumping area, sintering zone and cooling zone
It is respectively 300-1300 DEG C, 1600-1850 DEG C, 1850-25 DEG C, base substrate is respectively in the sintering of dumping area, sintering zone and cooling zone
Time is 3-8h, 1-3h, 8-12h.
5. a kind of ceramic heating body of cofired materials according to claim 1 preparation technology it is characterised in that：Step e
In resistance slurry be made up of the raw material of following mass percent：
Solid formation 75-85%
Carrier 15-25%；
Wherein, solid formation is made up of the raw material of following mass percent：
Conductive phase 70-90%
Glass phase 10-30%；
Conductive phase is the mixture of one or more of tungsten, manganese, molybdenum；
Glass is made up of the raw material of following mass percent：
Si3N475-90%
MgO 4-8%
Y2O32-4%
Al2O32-4%
SiO22-4%
La2O32-4%
BN 2-4%；
Wherein, carrier is made up of the raw material of following mass percent：
Terpineol 60-70%
Tributyl citrate 12-25%
Butyl carbitol amyl acetate 12-25%
Oleum Ricini 0.5-1.5%
Ethyl cellulose 4-8%
Lecithin 0.5-1.2%
Span 85 1-2.5%.
6. a kind of ceramic heating body of cofired materials according to claim 1 preparation technology it is characterised in that：Step e
In resistance slurry be made up of the raw material of following mass percent：
Solid formation 80%
Carrier 20%；
Wherein, solid formation is made up of the raw material of following mass percent：
Conductive phase 80%
Glass phase 20%；
Conductive phase is the mixture of one or more of tungsten, manganese, molybdenum；
Glass is made up of the raw material of following mass percent：
Si3N480%
MgO 7%
Y2O33%
Al2O32%
SiO23%
La2O32%
BN 3%；
Wherein, carrier is made up of the raw material of following mass percent：
Terpineol 65%
Tributyl citrate 14%
Butyl carbitol amyl acetate 12%
Oleum Ricini 1%
Ethyl cellulose 5%
Lecithin 1%
Span 85 2%.
7. a kind of ceramic heating body of cofired materials according to claim 1 preparation technology it is characterised in that：Prepared
Ceramic heating body is in one of tabular, pole shape, circular tube shaped, and pole shape or circular tube shaped ceramic heating body are by tabular pottery
Calandria rolls and forms.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410066362.0A CN104860682B (en) | 2014-02-26 | 2014-02-26 | Cofired ceramic heating member preparation technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410066362.0A CN104860682B (en) | 2014-02-26 | 2014-02-26 | Cofired ceramic heating member preparation technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104860682A CN104860682A (en) | 2015-08-26 |
| CN104860682B true CN104860682B (en) | 2017-02-15 |
Family
ID=53906924
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410066362.0A Active CN104860682B (en) | 2014-02-26 | 2014-02-26 | Cofired ceramic heating member preparation technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104860682B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046834B (en) * | 2017-12-21 | 2020-12-04 | 深圳市卓力能电子有限公司 | Preparation process of porous ceramic heating body with mosaic structure |
| CN108046833B (en) * | 2017-12-21 | 2020-06-30 | 深圳市卓力能电子有限公司 | Preparation process of ceramic heating body with porous heating film structure |
| CN108059479B (en) * | 2017-12-21 | 2020-09-15 | 深圳市卓力能电子有限公司 | Preparation process of novel porous ceramic heating body |
| CN108503391A (en) * | 2018-04-10 | 2018-09-07 | 珠海惠友电子有限公司 | A kind of manufacturing process of ceramic heating part |
| CN109005608B (en) * | 2018-06-28 | 2021-03-19 | 珠海华宇宏瑞科技有限公司 | Processing method of hollow ceramic heating body |
| CN108882405B (en) * | 2018-06-28 | 2021-05-25 | 珠海华宇宏瑞科技有限公司 | Method for manufacturing ceramic heating element |
| CN112430072A (en) * | 2020-11-24 | 2021-03-02 | 广东国研新材料有限公司 | Co-fired laminated porous ceramic heating body and preparation method thereof |
| CN112568506A (en) * | 2020-12-22 | 2021-03-30 | 深圳顺络电子股份有限公司 | Ceramic heating body and manufacturing method thereof |
| CN112552055A (en) * | 2021-01-14 | 2021-03-26 | 威海圆环先进陶瓷股份有限公司 | Method for high-temperature co-firing of metal and silicon nitride ceramic composite substrate |
| CN114101827B (en) * | 2021-11-22 | 2023-01-06 | 广东国研新材料有限公司 | Ceramic heating element electrode brazing process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1849017A (en) * | 2005-04-05 | 2006-10-18 | 郜长福 | Silicon nitride heating body and its pressureless lower temperature sintering producing method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2530392B2 (en) * | 1991-07-16 | 1996-09-04 | 日立造船株式会社 | Heat resistant ceramics |
-
2014
- 2014-02-26 CN CN201410066362.0A patent/CN104860682B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1849017A (en) * | 2005-04-05 | 2006-10-18 | 郜长福 | Silicon nitride heating body and its pressureless lower temperature sintering producing method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104860682A (en) | 2015-08-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104860682B (en) | Cofired ceramic heating member preparation technology | |
| TWI342568B (en) | Method of manufacture of semiconductor device and conductive compositions used therein | |
| CN103482985B (en) | Low-temperature co-fired ceramic tape casting material and preparing method and application thereof | |
| CN104867537B (en) | Low lead high square resistance silicon solar cell front silver electrode paste and preparation method thereof | |
| TW201144250A (en) | Thick-film pastes containing lead-tellurium-lithium-titanium-oxides, and their use in the manufacture of semiconductor devices | |
| TW201101499A (en) | Conductive paste for solar cell electrode | |
| CN103295659B (en) | Conductive paste for solar cell and preparation method thereof | |
| CN103096529A (en) | Preparation method for silicon nitride heating body with high reliability and safety | |
| JP2018078120A (en) | Thick-film composition containing antimony oxides and their use in manufacture of semiconductor devices | |
| CN107658045B (en) | Back electrode silver paste for lead-free PERC battery and preparation method | |
| JP2015506066A (en) | Conductive silver paste for metal wrap-through silicon solar cells | |
| TW201718422A (en) | Crystalline oxides, preparation thereof and conductive pastes containing the same | |
| TW201202367A (en) | Solar cell and electroconductive paste used to form electrode thereof | |
| TWI568700B (en) | Glass powder material | |
| CN103440901A (en) | Low-cost leadless back silver paste for crystalline silica solar energy battery, and preparation method thereof | |
| CN103922725B (en) | A kind of low-temperature sintering temperature-stabilized microwave medium ceramic material and preparation method thereof | |
| CN103096528B (en) | Preparation method for silicon nitride heating body | |
| CN104751937A (en) | Aluminum conductive paste for solar cell and preparation method thereof | |
| CN106057277A (en) | Silver paste for forming back silver electrode of back passivation solar battery | |
| US20210410234A1 (en) | Ceramic heater and preparation method and use of ceramic heater | |
| CN102432184A (en) | Low melting point phosphate glass powder for silver paste of solar battery and preparation method thereof | |
| CN103680674B (en) | Front Seed Layer silver slurry of crystal-silicon solar cell and preparation method thereof, crystal-silicon solar cell and preparation method thereof | |
| CN107622812A (en) | A kind of two-sided PERC crystal-silicon solar cells aluminium paste of p-type and preparation method thereof | |
| CN103366860B (en) | A kind of conductive paste for solar cell and preparation method thereof, the preparation method of a kind of solar battery sheet | |
| CN103177790A (en) | Solar cell back surface field transition paste and preparation method thereof, preparation method of solar cell piece and solar cell piece |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20211229 Address after: 517000 plant of Guangdong hemi Technology Co., Ltd. in the west of Binjiang Road and in the south of Gaoxin fifth road, high tech Zone, Heyuan City, Guangdong Province Patentee after: GUANGDONG GUOYAN NEW MATERIAL Co.,Ltd. Address before: 523000 Sima Village Industrial Zone, Changping Town, Dongguan City, Guangdong Province Patentee before: Key Material Co.,Ltd. |
|
| TR01 | Transfer of patent right |