CN104860681A - Cofired ceramic heating member and preparation technology thereof - Google Patents
Cofired ceramic heating member and preparation technology thereof Download PDFInfo
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- CN104860681A CN104860681A CN201410066359.9A CN201410066359A CN104860681A CN 104860681 A CN104860681 A CN 104860681A CN 201410066359 A CN201410066359 A CN 201410066359A CN 104860681 A CN104860681 A CN 104860681A
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Abstract
The invention relates to the technical field of ceramic heating member preparation and especially relates to a cofired ceramic heating member and a preparation technology thereof. The cofired ceramic heating member comprises an inner substrate and two outer substrates. The inner substrate is arranged between the two outer substrates. The inner substrate and the two outer substrates are prepared from a ceramic raw material and a heating raw material. The inner substrate is prepared from 50-70% of the ceramic raw material and 30-50% of the heating raw material. The outer substrate is prepared from 70-99% of the ceramic raw material and 1-30% of the heating raw material. The preparation technology comprises ceramic raw material preparation, inner substrate blank preparation, outer substrate blank preparation, lamination, sintering and electrode connection. The preparation technology has simple processes, is conducive to continuous production, has high production efficiency and a low production cost, and is conducive to large scale production. The cofired ceramic heating member has the advantages of long life, stable power and high heating efficiency.
Description
Technical field
The present invention relates to the preparing technical field of heating member, particularly relate to a kind of laminated type ceramic heating body and preparation technology thereof.
Background technology
Silicon nitride heating plate is a kind of device in conjunction with high-performance silicon nitride ceramics matrix and long lifetime powerful hot metal heating wire, it is little that it has volume, large and the thermo-efficiency high of power, is also proved to be a kind of safe and reliable heating system by silicon nitride heating plate heat production simultaneously.
Silicon nitride is as a kind of covalent linkage compound, and spread coefficient is little, does not have fusing point, decomposes ammonification and silicon about 2173K, is difficult to sintering.At present, traditional silicon nitride ceramics heating piece is embedded in alpha-silicon nitride powders by tungsten filament to be molded into plates hot pressed sintering and to form, the well heater of this explained hereafter is owing to being subject to process technology limit, and tungsten filament is difficult to location, causes position to offset in moulding process, overall heater is caused to conduct heat uneven, simultaneously because tungsten filament and beta-silicon nitride powder have obvious interface, be difficult to into after sintering and be integrated, tungsten filament and ceramic contact surface form space, form selective oxidation in heat-processed, reduce the work-ing life of fever tablet.The sintering of current silicon nitride ceramics heating piece also has employing reaction sintering and hot pressed sintering, but reaction sintering density is poor, poor mechanical property, although hot pressed sintering density is high, mechanical property is good, and cost is higher, is difficult to scale operation.Therefore, the above problems demand solves.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, and provide that a kind of power stability, thermo-efficiency are high, the integrated ceramic heating body of long service life.
Another object of the present invention is to provide the preparation technology that a kind of production efficiency is high, be beneficial to continuous large-scale production, integrated ceramic heating body that production cost is low.
The present invention is achieved through the following technical solutions.
A kind of laminated type ceramic heating body, it comprises inner-layer substrate and two outer substrates, and inner-layer substrate is superimposed between two outer substrates, inner-layer substrate and two outer substrates by ceramic raw material and heating material formulated; Inner-layer substrate is formulated by the heating material of mass percent to be the ceramic raw material of 50-70% and mass percent be 30-50%, and outer substrate is formulated by the heating material of mass percent to be the ceramic raw material of 70-99% and mass percent be 1-30%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
465-98%
MgO 0.1-10%
Y
2O
30.1-5%
Al
2O
30.1-5%
SiO
2 0.1-5%
La
2O
30.1-5%
BN 0.1-5%；
Wherein, heating material is MoSi
2, one or both mixture in TiC.
Si
3n
4chemical name is silicon nitride, its relative molecular mass is 140.28, gray, white or canescence, hexagonal system, its crystal is hexahedron, Mohs' hardness 9 ~ 9.5, Vickers' hardness is about 2200, microhardness is 32630MPa, fusing point is 1900 DEG C, usually 1900 DEG C of decomposition at ambient pressure, specific heat capacity is 0.71J/ (gK), Heat of Formation is-751.57kJ/mol, thermal conductivity is 16.7W/ (mK), linear expansivity is 2.75 × 10-6/ DEG C (20 ~ 1000 DEG C), water insoluble, be dissolved in hydrofluoric acid, it starts the temperature 1300 ~ 1400 DEG C be oxidized in atmosphere, Young's modulus is 28420 ~ 46060MPa, compressive strength is 490MPa.Specific volume resistance: be 1.4 × 105 m 20 DEG C time is 4 × 108 m 500 DEG C time.Si
3n
4be a kind of important structural ceramic material, be a kind of superhard material, itself has oilness, and wear-resistant, for atomic crystal, anti-oxidant during high temperature, and it can also resist thermal shock, be heated to more than 1000 DEG C in atmosphere, quick refrigeration sharply heats again, also can not be cracked.
The chemical name of MgO is magnesium oxide, and be white or pale yellow powder, odorless, tasteless, nontoxic, its water insoluble or ethanol, is slightly soluble in ethylene glycol, fusing point 2852 DEG C, and boiling point 3600 DEG C, magnesium oxide has extremely fireproof insulating property.Can crystal be changed into through more than 1000 DEG C high temperature sinterings, rise to more than 1500 DEG C and then become dead roasting magnesium oxide (namely said magnesia) or sintered magnesia.Magnesium oxide plays skeleton function, and in pottery, effect has been structure fixed action, makes product be not easy distortion.
Y
2o
3chemical name be yttrium oxide, white yellowish powder.Fusing point: 2415 DEG C; Relative density: 5.01; Solvability: water insoluble and alkali, is dissolved in mineral acid.First, Y
2o
3interpolation very large on the impact of ceramic hardness, because the interpolation refinement of ruthenium ion alumina grain, decrease the defects such as Qi Kong ﹑ crackle, it is made to combine tightr, density increases, so doped with yttrium ion not only can improve the intensity of pottery, improve its mechanical property, the hardness of pottery can also be significantly improved.Secondly, Y
2o
3interpolation significantly improve pottery density, Y
2o
3for rare earth oxide, rare earth oxide, due to the singularity in its performance, is good surfactant, can improves Al
2o
3the wettability of matrix material, reduces the fusing point of stupalith, rare earth oxide Y
2o
3al can be promoted
2o
3with SiO
2chemical reaction, be easy to form low melting point liquid phase, add the wicking action between particle, impel intergranular material to fill to hole place, material porosity is reduced, density raising.Therefore, Y
2o
3interpolation significantly improve intensity, hardness and the density of pottery.
Al
2o
3chemical name be aluminum oxide, Al
2o
3be the typical material in structural ceramics, there is the characteristics such as the physical strength Gao ﹑ hardness Gao ﹑ Shi of the Nai Fu ﹑ Sun of Nai Mo ﹑ resistivity great ﹑ Heat stability is good, the environment of the condition harshnesses such as Ji tool Ying Li ﹑ Fu Shi ﹑ Gao Wen ﹑ insulation can be born.Al
2o
3the increase of liquid content in liquid phase sintering can be promoted, can also liquid phase viscosity be reduced, be conducive to Si
3n
4dissolving, diffusion mass transfer, therefore Al in the liquid phase
2o
3interpolation to Si
3n
4normal pressure-sintered densification has important effect.
SiO
2chemical name be silicon-dioxide, it is water insoluble, is insoluble to acid, but is dissolved in hydrofluoric acid and hot strong phosphoric acid.SiO
2a part and Al
2o
3reaction generates netted mullite (3 Al
2o
32 SiO
2) crystal becomes powder skeleton, improves physical strength and the chemical stability of pottery, another part SiO
2exist with free state and also play skeleton function.And Al
2o
3the densification degree of powder can be improved, the bending strength of silicon nitride ceramics is improved.
La
2o
3chemical name be lanthanum trioxide, it is white amorphous powder, is density 6.51g/cm
3.Fusing point is 2217 DEG C, and boiling point is 4200 DEG C, solvability: be dissolved in acid, ethanol, ammonium chloride, water insoluble, ketone.Si
3n
4there are α and β two kinds of crystalline structure, La
2o
3add and be beneficial to β-Si
3n
4the raising of grain axial ratio, also improves β-Si
3n
4the length-to-diameter ratio of column crystal, promotes α-Si simultaneously
3n
4with β-Si
3n
4transformation completely, substantially increase bending strength and the fracture toughness property of silicon nitride ceramic material.
The chemical name of BN is boron nitride, and boron nitride is corrosion-resistant, and electrical insulating property is fine, and ratio resistance is greater than 10-6 Ω .cm; Compressive strength is 170MPa; Thermal expansivity on c-axis direction is 41 × 10-6/ DEG C and for-2.3 × 10-6 on d direction of principal axis; Under oxidizing atmosphere, maximum operation (service) temperature is 900 DEG C, and can reach 2800 DEG C under nonactive reducing atmosphere.The thermotolerance of BN, heat shock resistance and hot strength are all very high, and can be processed into different shape, are therefore widely used as the work material of various molten mass.The powder of boron nitride has good oilness, is used in pottery as high-temp. resistant self-lubricating compound material.
MoSi
2chemical name be molybdenum disilicide, MoSi
2being a kind of mesophase spherule that in Mo-Si binary alloy system, silicon content is the highest, is compound between composition fixing dalton's shaped metal, and having the dual nature of metal and pottery, is a kind of high-temperature material of excellent performance.MoSi
2have fabulous high-temperature oxidation resistance, oxidation resistance temperature is up to more than 1600 DEG C, suitable with SiC; Medium density, density is 6.24g/cm
3; Lower thermal expansivity (8.1 × 10-6K-1); Good electric heating conductivity; Higher brittle-ductile transition temperature 1000 DEG C.MoSi
2there is good high-temperature oxidation resistance and thermal-shock resistance, and stable resistance characteristic, therefore by MoSi
2heating material as ceramic heating body mixes with stupalith, and the ceramic heating body power stability be prepared into, heating efficiency are high.
The chemical name of TiC is titanium carbide, and the relative molecular mass of TiC is 59.91, and density is 4.93g/cm
3, fusing point is 3160 DEG C, and boiling point is 4820 DEG C, and TiC is in light grey, for isometric system, water insoluble, there is very high chemical stability, with hydrochloric acid, sulfuric acid react with hardly, but can be dissolved in chloroazotic acid, nitric acid and hydrofluoric acid, also be dissolved in the solution of basic oxide.TiC has high-melting-point, high rigidity and high elastic coefficient, good heat-shock resistance and chemical stability, carbon TiC has excellent thermal shock resistance simultaneously, special refractory materials is used as in reducing atmosphere, the stupalith adding TiC not only maintains the characteristics such as high strength, high rigidity, wear-resistant, high temperature resistant, anti-oxidant and chemical stability, there is again good metal toughness, the ceramic heating body power stability making to obtain, heating efficiency be high, long service life.
Further, be the MoSi of 50-99.5% by mass percent
2be the heating material of the TiC composition of 0.5-50% with mass percent, there is splendid high-temperature oxidation resistance and thermal-shock resistance, and stable resistance characteristic.The ceramic heating body that this heating material and ceramic raw material are fired into altogether, power stability, heating efficiency are high, long service life.
Preferably, inner-layer substrate is formulated by the heating material of mass percent to be the ceramic raw material of 55-65% and mass percent be 35-45%, and outer substrate is formulated by the heating material of mass percent to be the ceramic raw material of 80-90% and mass percent be 10-20%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
475-90%
MgO 4-8%
Y
2O
32-4%
Al
2O
32-4%
SiO
2 2-4%
La
2O
32-4%
BN 2-4%；
Wherein, heating material is MoSi
2, one or both mixture in TiC, the mixture of two kinds is the MoSi of 50-99.5% by mass percent
2with the TiC composition that mass percent is 0.5-50%.
More preferred, inner-layer substrate by mass percent be 60% ceramic raw material and mass percent be 40% heating material formulated, outer substrate by mass percent be 85% ceramic raw material and mass percent be 15% heating material formulated;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
480%
MgO 7%
Y
2O
33%
Al
2O
32%
SiO
2 3%
La
2O
32%
BN 3%；
Wherein, heating material is MoSi
2, one or both mixture in TiC, the mixture of two kinds is the MoSi of 65-80% by mass percent
2with the TiC composition that mass percent is 20-35%.
The preparation technology of above-mentioned a kind of laminated type ceramic heating body, comprises following processing step:
The preparation of A, ceramic raw material: the Si taking 65-98% by mass percentage
3n
4, 0.1-10% the Y of MgO, 0.1-5%
2o
3, 0.1-5% Al
2o
3, 0.1-5% SiO
2, 0.1-5% La
2o
3, the BN of 0.1-5% mixing and stirring, make ceramic raw material;
The preparation of B, inner-layer substrate green compact:
A), batch mixing: be the ceramic raw material of 50-70% and the heating material MoSi of 30-50% by mass percent
2or TiC or MoSi
2with the mixture mixing and stirring of TiC, make inner-layer substrate powder;
B), ball milling: inner-layer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carry out wet ball grinding, the time of inner-layer substrate powder wet ball grinding is 8-24h, obtained inner-layer substrate compound; Wet ball grinding can improve mill efficiency, and diameter of particle is reduced, and specific surface area increases, increased activity.
C), deaeration: inner-layer substrate compound is carried out deaeration under vacuum;
D), shaping with drying: by step c) in inner-layer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into inner-layer substrate green compact, and inner-layer substrate green compact are carried out drying;
The preparation of C, outer substrate green compact:
A), batch mixing: the ceramic raw material and the 5-30% heating material MoSi that by mass percent are 70-95%
2or TiC mixing and stirring, make outer substrate powder;
B), ball milling: outer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carries out wet ball grinding, the time of outer substrate powder wet ball grinding is 8-24h, obtained outer substrate compound;
C), deaeration: outer substrate compound is carried out deaeration under vacuum;
D), shaping with drying: by step c) in outer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into outer substrate green compact, and outer substrate green compact are carried out drying;
D, lamination: the inner-layer substrate green compact obtained by step B are superimposed between the obtained outer substrate green compact of two step C, and laminate and make base substrate;
E, sintering: the base substrate of step D is placed in plumbago crucible or molybdenum crucible, and imbed insulating powder, then sintered at ambient pressure by the base substrate be embedded in insulating powder with box-type furnace or tunnel furnace, sintering atmosphere is nitrogen and hydrogen gas mixture, and blank sintering obtains ceramic heating body work in-process; Adopt tunnel furnace in conjunction with reductive sintered atmosphere at normal pressure-sintered base substrate, can realize continuous seepage, output becomes every day 48 batches from original every day 1 batch, production efficiency improves 48 times, and continuous prodution is beneficial to energy-conservation, greatly reduces production cost, is beneficial to enterprise and accomplishes scale production; Simultaneously because hydrogen atom radius is very little, be easy to diffusion and the hole elimination that is conducive to holding one's breath, the oxonium ion in aluminum oxide lattice can also be made in a hydrogen atmosphere to lose relatively easily, form room, acceleration oxonium ion spreads, therefore in a hydrogen atmosphere can acceleration of sintering effectively, make ceramic obtain good density.
F, receiving electrode: by half-finished for the ceramic heating body of step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through sintering, finally draws electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
Wherein, step e sintering is specially: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbed insulating powder, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 1-40%, and the volume percent of nitrogen in mixed gas is 60%-99%, and blank sintering obtains ceramic heating body work in-process.The volume percent of hydrogen is greater than 1%, restitutive protection's effect of mixed gas can be ensured, simultaneously because hydrogen belongs to flammable explosive gas, therefore the volume percent of hydrogen is made to be less than 40%, reduce potential safety hazard, therefore the volume percent of hydrogen 1-40% makes mixed gas can play reductibility protection and explosion-proof effect simultaneously; Hydrogen in the present invention is made for being decomposed by ammonia, higher relative to the nitrogen cost of outsourcing, in mixed gas, therefore makes the volume percent of nitrogen be 60%-99%, higher than the volume percent of the 1-40% of hydrogen, can save production cost further.
Wherein, step e sintering is specially: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, and the insulating powder burying burning is Si
3n
4with the mixture of BN, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 5-29%, the volume percent of nitrogen in mixed gas is 71%-95%, control the dew-point temperature of water vapor in mixed gas lower than 50 DEG C, blank sintering obtains ceramic heating body work in-process.
Wherein, step e sinter tunnel furnace used be divided into connect successively binder removal district, sintering zone and cooling zone, the temperature of binder removal district, sintering zone and cooling zone is respectively 300-1300 DEG C, 1600-1850 DEG C, 1850-25 DEG C, base substrate respectively in binder removal district, the sintering time of sintering zone and cooling zone is 3-8h, 1-3h, 8-12h.Replace traditional box-type furnace, because tunnel furnace is divided into binder removal district, sintering zone and cooling zone, make base substrate can realize binder removal successively, the operation of high temperature sintering and cooling, when the blank sintering of last batch is complete, tunnel furnace is without the need to again experiencing long intensification, the base substrate that can drop into again next batch immediately sinters, eliminate box-type furnace need repeatedly heat up when the base substrate that stoking is multiple batches of, the operation of cooling, adopt tunnel furnace can realize continuous circulationization to produce, output becomes every day 48 batches from original every day 1 batch, production efficiency improves 48 times, production efficiency improves greatly, and be more conducive to energy-conservation, greatly reduce production cost, the sintering temperature of 1600-1850 DEG C ensures that firing of ceramic heating body is effective, avoids the hydrogen explosion that high temperature causes simultaneously.
Wherein, step F receiving electrode is specially: by half-finished for the ceramic heating body in step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 500-1300 DEG C, electrode is silver electrode, silver-colored palladium electrode, gold electrode or platinum electrode, distance between electrode is greater than 2mm, finally draw electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
Wherein, inner-layer substrate is superimposed between two outer substrates and forms ceramic heating body body, ceramic heating body body is the one in tabular, pole shape, circular tube shaped, and pole shape or circular tube shaped ceramic heating body body are rolled by tabular ceramic heating body body and form.
Beneficial effect of the present invention is: ceramic heating body of the present invention is made by inner-layer substrate and outer substrate stack technique, and inner-layer substrate or outer substrate burn till one altogether by ceramic raw material and metal heating material forms, inner combination is fine and close, operationally ceramic heating body entirety heating, have that heat-up rate is fast, thermo-efficiency is high, heat balance, heat radiation is even, long service life.
The preparation technology of ceramic heating body of the present invention sequentially by the preparation of the preparation of ceramic raw material, the preparation of inner-layer substrate green compact, outer substrate green compact, laminate, sinter and receiving electrode operation; whole manufacturing process is simple; solve conventional silicon nitride heating piece production technique problem rambunctious; but also adopt tunnel furnace in conjunction with reductive sintered atmosphere at normal pressure-sintered base substrate; be beneficial to continuous seepage, production efficiency is high; and be sintered to liquid phase sintering; sintering temperature is low; production cost is low, is beneficial to and accomplishes scale production.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
embodiment 1.
The preparation technology of a kind of laminated type ceramic heating body of the present embodiment, comprises following processing step:
The preparation of A, ceramic raw material: take the Si of 65% by mass percentage
3n
4, the MgO of 10%, the Y of 5%
2o
3, 5% Al
2o
3, 5% SiO
2, 5% La
2o
3, 5% BN and mixing and stirring, make ceramic raw material;
The preparation of B, inner-layer substrate green compact: a), batch mixing: be ceramic raw material and the 50% heating material MoSi of 50% by mass percent
2mixing and stirring, makes inner-layer substrate powder; B), ball milling: inner-layer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carry out wet ball grinding, the time of inner-layer substrate powder wet ball grinding is 8h, obtained inner-layer substrate compound; C), deaeration: inner-layer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in inner-layer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into inner-layer substrate green compact, and inner-layer substrate green compact are carried out drying;
The preparation of C, outer substrate green compact: a), batch mixing: be ceramic raw material and the 30% heating material MoSi of 70% by mass percent
2mixing and stirring, makes outer substrate powder; B), ball milling: outer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carries out wet ball grinding, the time of outer substrate powder wet ball grinding is 8h, obtained outer substrate compound; C), deaeration: outer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in outer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into outer substrate green compact, and outer substrate green compact are carried out drying;
D, lamination: the inner-layer substrate green compact obtained by step B are superimposed between the obtained outer substrate green compact of two step C, and laminate and make base substrate;
E, sintering: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, and the insulating powder burying burning is Si
3n
4with the mixture of BN, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, tunnel furnace is divided into the binder removal district connected successively, sintering zone and cooling zone, binder removal district, the temperature of sintering zone and cooling zone is respectively 300 DEG C, 1600 DEG C, 25 DEG C, base substrate is respectively in binder removal district, the sintering time of sintering zone and cooling zone is 3h, 1h, 8h, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 1%, the volume percent of nitrogen in mixed gas is 99%, control the dew-point temperature of water vapor in mixed gas lower than 50 DEG C, blank sintering obtains ceramic heating body work in-process,
F, receiving electrode: receiving electrode: by half-finished for the ceramic heating body in step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 500 DEG C, electrode is silver electrode, silver-colored palladium electrode, gold electrode or platinum electrode, distance between electrode is greater than 2mm, finally draw electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
embodiment 2.
The preparation technology of a kind of laminated type ceramic heating body of the present embodiment, comprises following processing step:
The preparation of A, ceramic raw material: take the Si of 98% by mass percentage
3n
4, the MgO of 0.5%, the Y of 0.5%
2o
3, 0.2% Al
2o
3, 0.3% SiO
2, 0.2% La
2o
3, 0.3% BN and mixing and stirring, make ceramic raw material;
The preparation of B, inner-layer substrate green compact: a), batch mixing: be the ceramic raw material of 70% and the heating material MoSi of 24% by mass percent
2, 6% heating material TiC mixing and stirring, make inner-layer substrate powder; B), ball milling: inner-layer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carry out wet ball grinding, the time of inner-layer substrate powder wet ball grinding is 11h, obtained inner-layer substrate compound; C), deaeration: inner-layer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in inner-layer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into inner-layer substrate green compact, and inner-layer substrate green compact are carried out drying;
The preparation of C, outer substrate green compact: a), batch mixing: be ceramic raw material and the 1% heating material TiC mixing and stirring of 99% by mass percent, make outer substrate powder; B), ball milling: outer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carries out wet ball grinding, the time of outer substrate powder wet ball grinding is 12h, obtained outer substrate compound; C), deaeration: outer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in outer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into outer substrate green compact, and outer substrate green compact are carried out drying;
D, lamination: the inner-layer substrate green compact obtained by step B are superimposed between the obtained outer substrate green compact of two step C, and laminate and make base substrate;
E, sintering: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, and the insulating powder burying burning is Si
3n
4with the mixture of BN, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, tunnel furnace is divided into the binder removal district connected successively, sintering zone and cooling zone, binder removal district, the temperature of sintering zone and cooling zone is respectively 500 DEG C, 1650 DEG C, 100 DEG C, base substrate is respectively in binder removal district, the sintering time of sintering zone and cooling zone is 4h, 2h, 9h, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 40%, the volume percent of nitrogen in mixed gas is 60%, control the dew-point temperature of water vapor in mixed gas lower than 45 DEG C, blank sintering obtains ceramic heating body work in-process,
F, receiving electrode: receiving electrode: by half-finished for the ceramic heating body in step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 650 DEG C, electrode is silver electrode, silver-colored palladium electrode, gold electrode or platinum electrode, distance between electrode is greater than 2mm, finally draw electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
embodiment 3.
The preparation technology of a kind of laminated type ceramic heating body of the present embodiment, comprises following processing step:
The preparation of A, ceramic raw material: take the Si of 75% by mass percentage
3n
4, the MgO of 8%, the Y of 4%
2o
3, 4% Al
2o
3, 3% SiO
2, 3% La
2o
3, 3% BN and mixing and stirring, make ceramic raw material;
The preparation of B, inner-layer substrate green compact: a), batch mixing: be the ceramic raw material of 55% and the heating material MoSi of 27% by mass percent
2, 18% heating material TiC mixing and stirring, make inner-layer substrate powder; B), ball milling: inner-layer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carry out wet ball grinding, the time of inner-layer substrate powder wet ball grinding is 14h, obtained inner-layer substrate compound; C), deaeration: inner-layer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in inner-layer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into inner-layer substrate green compact, and inner-layer substrate green compact are carried out drying;
The preparation of C, outer substrate green compact: a), batch mixing: be the ceramic raw material of 75% and the heating material MoSi of 15% by mass percent
2, 10% heating material TiC mixing and stirring, make outer substrate powder; B), ball milling: outer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carries out wet ball grinding, the time of outer substrate powder wet ball grinding is 16h, obtained outer substrate compound; C), deaeration: outer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in outer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into outer substrate green compact, and outer substrate green compact are carried out drying;
D, lamination: the inner-layer substrate green compact obtained by step B are superimposed between the obtained outer substrate green compact of two step C, and laminate and make base substrate;
E, sintering: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, and the insulating powder burying burning is Si
3n
4with the mixture of BN, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, tunnel furnace is divided into the binder removal district connected successively, sintering zone and cooling zone, binder removal district, the temperature of sintering zone and cooling zone is respectively 700 DEG C, 1700 DEG C, 200 DEG C, base substrate is respectively in binder removal district, the sintering time of sintering zone and cooling zone is 5h, 3h, 10h, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 15%, the volume percent of nitrogen in mixed gas is 85%, control the dew-point temperature of water vapor in mixed gas lower than 40 DEG C, blank sintering obtains ceramic heating body work in-process,
F, receiving electrode: receiving electrode: by half-finished for the ceramic heating body in step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 800 DEG C, electrode is silver electrode, silver-colored palladium electrode, gold electrode or platinum electrode, distance between electrode is greater than 2mm, finally draw electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
embodiment 4.
The preparation technology of a kind of laminated type ceramic heating body of the present embodiment, comprises following processing step:
The preparation of A, ceramic raw material: take the Si of 90% by mass percentage
3n
4, the MgO of 4%, the Y of 2%
2o
3, 1% Al
2o
3, 1% SiO
2, 1% La
2o
3, 1% BN and mixing and stirring, make ceramic raw material;
The preparation of B, inner-layer substrate green compact: a), batch mixing: be the ceramic raw material of 60% and the heating material MoSi of 28% by mass percent
2, 12% heating material TiC mixing and stirring, make inner-layer substrate powder; B), ball milling: inner-layer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carry out wet ball grinding, the time of inner-layer substrate powder wet ball grinding is 18h, obtained inner-layer substrate compound; C), deaeration: inner-layer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in inner-layer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into inner-layer substrate green compact, and inner-layer substrate green compact are carried out drying;
The preparation of C, outer substrate green compact: a), batch mixing: be the ceramic raw material of 80% and the heating material MoSi of 10% by mass percent
2, 10% heating material TiC mixing and stirring, make outer substrate powder; B), ball milling: outer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carries out wet ball grinding, the time of outer substrate powder wet ball grinding is 20h, obtained outer substrate compound; C), deaeration: outer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in outer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into outer substrate green compact, and outer substrate green compact are carried out drying;
D, lamination: the inner-layer substrate green compact obtained by step B are superimposed between the obtained outer substrate green compact of two step C, and laminate and make base substrate;
E, sintering: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, and the insulating powder burying burning is Si
3n
4with the mixture of BN, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, tunnel furnace is divided into the binder removal district connected successively, sintering zone and cooling zone, binder removal district, the temperature of sintering zone and cooling zone is respectively 900 DEG C, 1750 DEG C, 300 DEG C, base substrate is respectively in binder removal district, the sintering time of sintering zone and cooling zone is 6h, 3h, 11h, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 20%, the volume percent of nitrogen in mixed gas is 80%, control the dew-point temperature of water vapor in mixed gas lower than 35 DEG C, blank sintering obtains ceramic heating body work in-process,
F, receiving electrode: receiving electrode: by half-finished for the ceramic heating body in step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 900 DEG C, electrode is silver electrode, silver-colored palladium electrode, gold electrode or platinum electrode, distance between electrode is greater than 2mm, finally draw electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
embodiment 5.
The preparation technology of a kind of laminated type ceramic heating body of the present embodiment, comprises following processing step:
The preparation of A, ceramic raw material: take the Si of 80% by mass percentage
3n
4, the MgO of 7%, the Y of 3%
2o
3, 2% Al
2o
3, 3% SiO
2, 2% La
2o
3, 3% BN and mixing and stirring, make ceramic raw material;
The preparation of B, inner-layer substrate green compact: a), batch mixing: be the ceramic raw material of 65% and the heating material MoSi of 28% by mass percent
2, 7% heating material TiC mixing and stirring, make inner-layer substrate powder; B), ball milling: inner-layer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carry out wet ball grinding, the time of inner-layer substrate powder wet ball grinding is 20h, obtained inner-layer substrate compound; C), deaeration: inner-layer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in inner-layer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into inner-layer substrate green compact, and inner-layer substrate green compact are carried out drying;
The preparation of C, outer substrate green compact: a), batch mixing: be ceramic raw material and the 15% heating material MoSi of 85% by mass percent
2mixing and stirring, makes outer substrate powder; B), ball milling: outer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carries out wet ball grinding, the time of outer substrate powder wet ball grinding is 22h, obtained outer substrate compound; C), deaeration: outer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in outer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into outer substrate green compact, and outer substrate green compact are carried out drying;
D, lamination: the inner-layer substrate green compact obtained by step B are superimposed between the obtained outer substrate green compact of two step C, and laminate and make base substrate;
E, sintering: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, and the insulating powder burying burning is Si
3n
4with the mixture of BN, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, tunnel furnace is divided into the binder removal district connected successively, sintering zone and cooling zone, binder removal district, the temperature of sintering zone and cooling zone is respectively 1100 DEG C, 1800 DEG C, 400 DEG C, base substrate is respectively in binder removal district, the sintering time of sintering zone and cooling zone is 7h, 3h, 12h, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 5%, the volume percent of nitrogen in mixed gas is 95%, control the dew-point temperature of water vapor in mixed gas lower than 30 DEG C, blank sintering obtains ceramic heating body work in-process,
F, receiving electrode: by half-finished for the ceramic heating body in step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 1100 DEG C, electrode is silver electrode, silver-colored palladium electrode, gold electrode or platinum electrode, distance between electrode is greater than 2mm, finally draw electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
embodiment 6.
The preparation technology of a kind of laminated type ceramic heating body of the present embodiment, comprises following processing step:
The preparation of A, ceramic raw material: take the Si of 70% by mass percentage
3n
4, the MgO of 9%, the Y of 5%
2o
3, 4% Al
2o
3, 4% SiO
2, 4% La
2o
3, 4% BN and mixing and stirring, make ceramic raw material;
The preparation of B, inner-layer substrate green compact: a), batch mixing: be ceramic raw material and the 32% heating material TiC mixing and stirring of 68% by mass percent, make inner-layer substrate powder; B), ball milling: inner-layer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carry out wet ball grinding, the time of inner-layer substrate powder wet ball grinding is 22h, obtained inner-layer substrate compound; C), deaeration: inner-layer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in inner-layer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into inner-layer substrate green compact, and inner-layer substrate green compact are carried out drying;
The preparation of C, outer substrate green compact: a), batch mixing: be ceramic raw material and the 10% heating material TiC mixing and stirring of 90% by mass percent, make outer substrate powder; B), ball milling: outer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carries out wet ball grinding, the time of outer substrate powder wet ball grinding is 24h, obtained outer substrate compound; C), deaeration: outer substrate compound is carried out deaeration under vacuum; D), shaping with drying: by step c) in outer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into outer substrate green compact, and outer substrate green compact are carried out drying;
D, lamination: the inner-layer substrate green compact obtained by step B are superimposed between the obtained outer substrate green compact of two step C, and laminate and make base substrate;
E, sintering: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, and the insulating powder burying burning is Si
3n
4with the mixture of BN, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, tunnel furnace is divided into the binder removal district connected successively, sintering zone and cooling zone, binder removal district, the temperature of sintering zone and cooling zone is respectively 1300 DEG C, 1850 DEG C, 500 DEG C, base substrate is respectively in binder removal district, the sintering time of sintering zone and cooling zone is 8h, 2h, 12h, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 10%, the volume percent of nitrogen in mixed gas is 90%, control the dew-point temperature of water vapor in mixed gas lower than 25 DEG C, blank sintering obtains ceramic heating body work in-process,
F, receiving electrode: by half-finished for the ceramic heating body in step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 1300 DEG C, electrode is silver electrode, silver-colored palladium electrode, gold electrode or platinum electrode, distance between electrode is greater than 2mm, finally draw electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
The performance testing index of the laminated type ceramic heating body that embodiment 1 ~ embodiment 6 is made is in table 1.
Table 1
。
As can be seen from Table 1, the High anti bending strength of the laminated type ceramic heating body that embodiment 1 ~ embodiment 6 is made, long service life, power stability, heating efficiency are high.
Finally should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention; but not limiting the scope of the invention; although done to explain to the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.
Claims (9)
1. a laminated type ceramic heating body, is characterized in that: it comprises inner-layer substrate and two outer substrates, and inner-layer substrate is superimposed between two outer substrates, inner-layer substrate and two outer substrates by ceramic raw material and heating material formulated; Inner-layer substrate is formulated by the heating material of mass percent to be the ceramic raw material of 50-70% and mass percent be 30-50%, and outer substrate is formulated by the heating material of mass percent to be the ceramic raw material of 70-99% and mass percent be 1-30%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
465-98%
MgO 0.1-10%
Y
2O
30.1-5%
Al
2O
30.1-5%
SiO
2 0.1-5%
La
2O
30.1-5%
BN 0.1-5%；
Wherein, heating material is MoSi
2or the mixture of TiC or two kind.
2. a kind of laminated type ceramic heating body according to claim 1, it is characterized in that: inner-layer substrate is formulated by the heating material of mass percent to be the ceramic raw material of 55-65% and mass percent be 35-45%, outer substrate is formulated by the heating material of mass percent to be the ceramic raw material of 80-90% and mass percent be 10-20%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
475-90%
MgO 4-8%
Y
2O
32-4%
Al
2O
32-4%
SiO
2 2-4%
La
2O
32-4%
BN 2-4%；
Wherein, heating material is MoSi
2, one or both mixture in TiC, the mixture of two kinds is the MoSi of 50-99.5% by mass percent
2with the TiC composition that mass percent is 0.5-50%.
3. a kind of laminated type ceramic heating body according to claim 1, it is characterized in that: inner-layer substrate by mass percent be 60% ceramic raw material and mass percent be 40% heating material formulated, outer substrate by mass percent be 85% ceramic raw material and mass percent be 15% heating material formulated;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
480%
MgO 7%
Y
2O
33%
Al
2O
32%
SiO
2 3%
La
2O
32%
BN 3%；
Wherein, heating material is MoSi
2, one or both mixture in TiC, the mixture of two kinds is the MoSi of 65-80% by mass percent
2with the TiC composition that mass percent is 20-35%.
4. the preparation technology of a kind of laminated type ceramic heating body described in claim 1-3 any one, is characterized in that: comprise following processing step:
The preparation of A, ceramic raw material: the Si taking 65-98% by mass percentage
3n
4, 0.1-10% the Y of MgO, 0.1-5%
2o
3, 0.1-5% Al
2o
3, 0.1-5% SiO
2, 0.1-5% La
2o
3, the BN of 0.1-5% mixing and stirring, make ceramic raw material;
The preparation of B, inner-layer substrate green compact:
A), batch mixing: be the ceramic raw material of 50-70% and the heating material MoSi of 30-50% by mass percent
2or TiC or MoSi
2with the mixture mixing and stirring of TiC, make inner-layer substrate powder;
B), ball milling: inner-layer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carry out wet ball grinding, the time of inner-layer substrate powder wet ball grinding is 8-24h, obtained inner-layer substrate compound;
C), deaeration: inner-layer substrate compound is carried out deaeration under vacuum;
D), shaping with drying: by step c) in inner-layer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into inner-layer substrate green compact, and inner-layer substrate green compact are carried out drying;
The preparation of C, outer substrate green compact:
A), batch mixing: the ceramic raw material and the 5-30% heating material MoSi that by mass percent are 70-95%
2or TiC mixing and stirring, make outer substrate powder;
B), ball milling: outer substrate powder is added mill ball, solvent and tackiness agent and puts into ball grinder and carries out wet ball grinding, the time of outer substrate powder wet ball grinding is 8-24h, obtained outer substrate compound;
C), deaeration: outer substrate compound is carried out deaeration under vacuum;
D), shaping with drying: by step c) in outer substrate compound casting machine curtain coating after deaeration make ceramic substrate or use and roll film device and be rolled into outer substrate green compact, and outer substrate green compact are carried out drying;
D, lamination: the inner-layer substrate green compact obtained by step B are superimposed between the obtained outer substrate green compact of two step C, and laminate and make base substrate;
E, sintering: the base substrate of step D is placed in plumbago crucible or molybdenum crucible, and imbed insulating powder, then sintered at ambient pressure by the base substrate be embedded in insulating powder with box-type furnace or tunnel furnace, sintering atmosphere is nitrogen and hydrogen gas mixture, and blank sintering obtains ceramic heating body work in-process;
F, receiving electrode: by half-finished for the ceramic heating body of step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through sintering, finally draws electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
5. the preparation technology of a kind of laminated type ceramic heating body according to claim 4, it is characterized in that: step e sintering is specially: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbed insulating powder, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 1-40%, the volume percent of nitrogen in mixed gas is 60%-99%, and blank sintering obtains ceramic heating body work in-process.
6. the preparation technology of a kind of laminated type ceramic heating body according to claim 4, is characterized in that: step e sintering is specially: the base substrate that step D is obtained is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, and the insulating powder burying burning is Si
3n
4with the mixture of BN, then with box-type furnace or tunnel furnace, the base substrate be embedded in insulating powder is sintered at ambient pressure, sintering atmosphere is nitrogen and hydrogen gas mixture, the volume percent of hydrogen in mixed gas is 5-29%, the volume percent of nitrogen in mixed gas is 71%-95%, control the dew-point temperature of water vapor in mixed gas lower than 50 DEG C, blank sintering obtains ceramic heating body work in-process.
7. the preparation technology of a kind of laminated type ceramic heating body according to claim 4, it is characterized in that: step e sinter tunnel furnace used be divided into connect successively binder removal district, sintering zone and cooling zone, the temperature of binder removal district, sintering zone and cooling zone is respectively 300-1300 DEG C, 1600-1850 DEG C, 1850-25 DEG C, base substrate respectively in binder removal district, the sintering time of sintering zone and cooling zone is 3-8h, 1-3h, 8-12h.
8. the preparation technology of a kind of laminated type ceramic heating body according to claim 4, it is characterized in that: step F receiving electrode is specially: by half-finished for the ceramic heating body in step e two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 500-1300 DEG C, electrode is silver electrode, silver-colored palladium electrode, gold electrode or platinum electrode, distance between electrode is greater than 2mm, finally draw electrical terminals at the fixed terminal of electrode, obtained ceramic heating body finished product.
9. a kind of laminated type ceramic heating body according to claim 1, it is characterized in that: inner-layer substrate is superimposed between two outer substrates and forms ceramic heating body body, ceramic heating body body is the one in tabular, pole shape, circular tube shaped, and pole shape or circular tube shaped ceramic heating body body are rolled by tabular ceramic heating body body and form.
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