CN104860683A - All-in-one ceramic heating member and preparation technology thereof - Google Patents
All-in-one ceramic heating member and preparation technology thereof Download PDFInfo
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Abstract
The invention relates to the technical field of ceramic heating member preparation technologies and especially relates to an all-in-one ceramic heating member and a preparation technology thereof. The all-in-one ceramic heating member comprises 50-95% of a ceramic raw material and 5-50% of a heating raw material. The ceramic raw material comprises 50-95% of Si3N4, 0.1-10% of MgO, 0.1-5% of Y2O3, 0.1-5% of Al2O3, 0.1-5% of SiO2, 0.1-5% of La2O3 and 0.1-5% of BN. The heating raw material comprises one or two of MoSi2 and TiC. The preparation technology comprises material blending, ball milling, drainage, molding, pre-sintering, sintering, polishing processing 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 ceramic heating member has a long service life, stable power and high heating efficiency.
Description
Technical field
The present invention relates to the fabricating technology field of ceramic heating body, particularly relate to a kind of integrated ceramic heating body and preparation technology thereof.
Background technology
At present, the electrical heating element of traditional hair dryer forms with nichrome wire coiling, be contained in the air outlet place of hair dryer, the wind that electric motor is discharged by electric-heating-wire-heating at air outlet, becomes hot blast and sends, traditional hair dryer is owing to being heat with heating wire, not only radiation is large, and nichrome wire contacts with air in heat-processed, more oxidizable, the power-off that is repeatedly energized there will be heating wire and blows, and the life-span is short.
Warm-air drier is a kind of forced convection formula heating installation, and traditional warm-air drier ptc heater heats, and utilizes blower fan blow air to flow through PTC electrical heating element forced convection, as main heat exchange method.But PTC electrical heating element is leaded, during use, rush current is large, and power is decayed gradually along with the lengthening of duration of service, and thermo-efficiency is low.
For this reason, people have developed a kind of novel well heater-silicon nitride heating sheet, and current silicon nitride heating sheet generally adopts and directly added in beta-silicon nitride powder by the tungsten filament being used for generating heat, and then form through firing.But because tungsten filament and beta-silicon nitride powder have obvious interface, be difficult to into and be integrated after sintering, in the production process of product, tungsten filament is easily short splits, or resistance value changes in sintering process, cause product performance unstable, yield rate is lower; And at high temperature, the oxygen in tungsten and silicon nitride composite ceramics matrix and nitrogen can react, cause the resistance value of heating piece unstable, work-ing life is not good enough, and heat conductivility needs to be improved further simultaneously; Therefore, existing silicon nitride heating sheet is still difficult to solve the problem of oxidation of heating wire heating and the problem of PTC electrical heating element power attenuation.In addition; the manufacture method of current silicon nitride heating sheet is based on high-temperature high-pressure craft; energy consumption is very big; and High Temperature High Pressure stove is independent body of heater; continuous seepage cannot be realized; the low one side of production efficiency cannot meet the powerful demand in market, also limits the reduction of large-scale production and cost on the other hand in itself.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 a kind of and be beneficial to the preparation technology that continuous seepage, production efficiency are high, be beneficial to 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 integrated ceramic heating body, it is made up of the raw material of following mass percent:
Ceramic raw material 50-95%
Heating material 5-50%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
470-96%
MgO 0.1-9%
Y
2O
30.1-5%
Al
2O
30.1-5%
SiO
2 0.1-5%
La
2O
30.1-3%
BN 0.1-3%；
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, a kind of integrated ceramic heating body, it is made up of the raw material of following mass percent:
Ceramic raw material 60-80%
Heating material 20-40%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
480-90%
MgO 2-6%
Y
2O
32-4%
Al
2O
32-4%
SiO
2 2-4%
La
2O
31-2.5%
BN 1-2.5%；
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, a kind of integrated ceramic heating body, it is made up of the raw material of following mass percent:
Ceramic raw material 70%
Heating material 30%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
485%
MgO 3%
Y
2O
33%
Al
2O
33%
SiO
2 3%
La
2O
31.5%
BN 1.5%；
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 integrated ceramic heating body, comprises following processing step:
A, batch mixing: first by the Si of formula ratio
3n
4, MgO, Y
2o
3, Al
2o
3, SiO
2, La
2o
3, BN mixing and stirring makes ceramic raw material, then by heating material MoSi
2, TiC, MoSi
2with the one in the mixture of TiC and ceramic raw material mixing and stirring, make powder;
B, ball milling: powder, mill ball, water or alcohol that step a is obtained are put into ball grinder and carries out wet ball grinding, the time of wet ball grinding is 8-24h; Wet ball grinding can improve mill efficiency, and diameter of particle is reduced, and specific surface area increases, increased activity.
C, to be filtered dry: solid-liquid separation is carried out to the slurry after wet ball grinding in step b, the powder after being separated is carried out drying and processing;
D, shaping: the powder after drying and processing in step c is shaping according to the one in following forming method: hot die-casting molding, dry-pressing formed, extrusion moulding, isostatic pressing, flow casting molding and injection moulding, the shaping obtained base substrate of powder;
E, pre-burning: the base substrate that steps d is obtained carries out pre-burning, and the temperature of pre-burning is 350-1250 DEG C; Through molding procedure be prepared from base substrate in containing the tackiness agent such as paraffin, adopt pre-burning operation that base substrate can be made first to be removed by tackiness agent before sintering, the excessive velocities that when avoiding base substrate direct sintering, temperature raises, non-uniform temperature produces thermal stresses and causes blank deformation or cracking, in addition, the calcined temperature of 350-1250 DEG C is beneficial to and is fully removed by the tackiness agent in base substrate.
F, sintering: the base substrate after step e pre-burning 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, 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.
G, polished finish: ceramic heating body work in-process are carried out surface finish process; This operation makes ceramic surface finer and close, smooth, greatly can improve the use properties of ceramic heating body.
H, receiving electrode: by half-finished for ceramic heating body surface-treated in step g 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 f sintering is specially: the base substrate after step e pre-burning 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 f sintering is specially: the base substrate after step e pre-burning is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, 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 f 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, during steps d is shaping, described hot die-casting molding is: powder is added paraffin wax and stirring of heating, stir formation slip, slip added thermocompressor die cast;
Described be dry-pressing formedly: powder is added tackiness agent and mix and blend, mixes formation powder, powder is loaded oil press dry-pressing formed;
Described extrusion moulding is: powder is added tackiness agent and mix and blend, mixes formation powder, powder is loaded extruder for shaping;
Described isostatic pressing is: powder is added tackiness agent and mix and blend, mixes formation powder, is first loaded in rubber mold by powder, then loads isostatic pressing in isostatic pressing machine in the lump.Tackiness agent can be polyvinyl alcohol, paraffin etc., and powder adds tackiness agent before being shaped, and makes powder and tackiness agent homogenizing, is beneficial to and improves the forming property of powder and the intensity of base substrate.
Wherein, step h receiving electrode is specially: by half-finished for ceramic heating body surface-treated in step g 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, obtained ceramic heating body is a kind of shape in cellular, lattice-shaped, pole shape, tabular.Ceramic honeycomb heating is arranged in hair dryer, and during work, the air-supply of motor driving fan blade is heated through ceramic heating body air, and hot blast is sent from air outlet, reaches the object adding warm air; Lattice-shaped ceramic heating body is arranged in warm-air drier and air-conditioning, and during work, the air-supply of motor driving fan blade is heated through ceramic heater air, reaches the object of heating installation; Pole shape ceramic heating body is applied on automotive oxygen sensor, is to detect motor vehicle exhaust order, prevents gasoline combustion insufficient; Tabular ceramic heating body should in mold heated, as the heating of the field such as boiler, foot bath.
Beneficial effect of the present invention is: ceramic heating body of the present invention is burnt till altogether by ceramic raw material and metal heating material and integrally forms, due to whole ceramic heating body is sintered into one, heating element and external insulation, antioxidant property is good, power is not easily decayed, long service life; And operationally ceramic heating body entirety heating, there is the significant advantages such as heat-up rate is fast, thermo-efficiency is high, heat balance.Therefore, ceramic heating body of the present invention overcomes the defect of oxidation that existing heating member heats as heating wire and PTC power attenuation, and long service life, power stability, heating efficiency are high.
The preparation technology of ceramic heating body of the present invention sequentially by batch mixing, ball milling, be filtered dry, shaping, pre-burning, sintering, polished finish and receiving electrode operation; whole manufacturing process is simple; adopt tunnel furnace in conjunction with reductive sintered atmosphere at normal pressure-sintered base substrate; be beneficial to continuous seepage, production efficiency is high; the product good compactness of sintering, 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 integrated ceramic heating body of the present embodiment, comprises following processing step:
A, batch mixing: first by the Si of mass percent 70%
3n
4, the MgO of 9%, the Y of 5%
2o
3, 5% Al
2o
3, 5% SiO
2, 3% La
2o
3, 3% BN mixing and stirring make ceramic raw material, then by the ceramic raw material of 50% and 50% heating material MoSi
2mixing and stirring, makes powder;
B, ball milling: powder, mill ball, water or alcohol that step a is obtained are put into ball grinder and carries out wet ball grinding, the time of wet ball grinding is 8h;
C, to be filtered dry: solid-liquid separation is carried out to the slurry after wet ball grinding in step b, the powder after being separated is carried out drying and processing;
D, hot die-casting molding: the powder after drying and processing in step c is added paraffin wax and stirring of heating, stir formation slip, slip added thermocompressor die cast, the shaping obtained base substrate of powder;
E, pre-burning: the base substrate that steps d is obtained carries out pre-burning, and the temperature of pre-burning is 350 DEG C;
F, sintering: the base substrate after step e pre-burning is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, 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,
G, polished finish: ceramic heating body work in-process are carried out surface finish process;
H, receiving electrode: by half-finished for ceramic heating body surface-treated in step g 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 integrated ceramic heating body of the present embodiment, comprises following processing step:
A, batch mixing: be first the Si of 96% by mass percent
3n
4, the MgO of 1%, the Y of 1%
2o
3, 0.5% Al
2o
3, 0.5% SiO
2, 0.5% La
2o
3, 0.5% BN mixing and stirring make ceramic raw material, then by the ceramic raw material of 95% and 5% heating material TiC mixing and stirring, make powder;
B, ball milling: powder, mill ball, water or alcohol that step a is obtained are put into ball grinder and carries out wet ball grinding, the time of wet ball grinding is 11h;
C, to be filtered dry: solid-liquid separation is carried out to the slurry after wet ball grinding in step b, the powder after being separated is carried out drying and processing;
D, dry-pressing formed: the powder after drying and processing in step c to be added tackiness agent and mix and blend, mixes formation powder, powder is loaded oil press dry-pressing formed, the shaping obtained base substrate of powder;
E, pre-burning: the base substrate that steps d is obtained carries out pre-burning, and the temperature of pre-burning is 500 DEG C;
F, sintering: the base substrate after step e pre-burning is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, 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,
G, polished finish: ceramic heating body work in-process are carried out surface finish process;
H, receiving electrode: by half-finished for ceramic heating body surface-treated in step g 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 integrated ceramic heating body of the present embodiment, comprises following processing step:
A, batch mixing: be first the Si of 80% by mass percent
3n
4, the MgO of 6%, the Y of 4%
2o
3, 4% Al
2o
3, 4% SiO
2, 1% La
2o
3, 1% BN mixing and stirring make ceramic raw material, then by the ceramic raw material of 60% and the heating material TiC of 20%, the heating material MoSi of 20%
2mixing and stirring, makes powder;
B, ball milling: powder, mill ball, water or alcohol that step a is obtained are put into ball grinder and carries out wet ball grinding, the time of wet ball grinding is 14h;
C, to be filtered dry: solid-liquid separation is carried out to the slurry after wet ball grinding in step b, the powder after being separated is carried out drying and processing;
D, extrusion moulding: the powder after drying and processing in step c is added tackiness agent and mix and blend, mix formation powder, powder loaded extruder for shaping, the shaping obtained base substrate of powder;
E, pre-burning: the base substrate that steps d is obtained carries out pre-burning, and the temperature of pre-burning is 650 DEG C;
F, sintering: the base substrate after step e pre-burning is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, 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,
G, polished finish: ceramic heating body work in-process are carried out surface finish process;
H, receiving electrode: by half-finished for ceramic heating body surface-treated in step g 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 integrated ceramic heating body of the present embodiment, comprises following processing step:
A, batch mixing: be first the Si of 90% by mass percent
3n
4, the MgO of 2%, the Y of 2%
2o
3, 2% Al
2o
3, 2% SiO
2, 1% La
2o
3, 1% BN mixing and stirring make ceramic raw material, then by the ceramic raw material of 80% and 16% heating material MoSi
2, 4% heating material TiC mixing and stirring, make powder;
B, ball milling: powder, mill ball, water or alcohol that step a is obtained are put into ball grinder and carries out wet ball grinding, the time of wet ball grinding is 18h;
C, to be filtered dry: solid-liquid separation is carried out to the slurry after wet ball grinding in step b, the powder after being separated is carried out drying and processing;
D, isostatic pressing: the powder after drying and processing in step c is added tackiness agent and mix and blend, mix formation powder, first loaded in rubber mold by powder, then load isostatic pressing in isostatic pressing machine in the lump;
E, pre-burning: the base substrate that steps d is obtained carries out pre-burning, and the temperature of pre-burning is 800 DEG C;
F, sintering: the base substrate after step e pre-burning is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, 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,
G, polished finish: ceramic heating body work in-process are carried out surface finish process;
H, receiving electrode: by half-finished for ceramic heating body surface-treated in step g two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 950 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 integrated ceramic heating body of the present embodiment, comprises following processing step:
A, batch mixing: be first the Si of 85% by mass percent
3n
4, the MgO of 3%, the Y of 3%
2o
3, 3% Al
2o
3, 3% SiO
2, 1.5% La
2o
3, 1.5% BN mixing and stirring make ceramic raw material, then by the ceramic raw material of 70% and 21% heating material MoSi
2, 9% heating material TiC mixing and stirring, make powder;
B, ball milling: powder, mill ball, water or alcohol that step a is obtained are put into ball grinder and carries out wet ball grinding, the time of wet ball grinding is 22h;
C, to be filtered dry: solid-liquid separation is carried out to the slurry after wet ball grinding in step b, the powder after being separated is carried out drying and processing;
D, flow casting molding: by the powder flow casting molding after drying and processing in step c, the shaping obtained base substrate of powder;
E, pre-burning: the base substrate that steps d is obtained carries out pre-burning, and the temperature of pre-burning is 1000 DEG C;
F, sintering: the base substrate after step e pre-burning is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, 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,
G, polished finish: ceramic heating body work in-process are carried out surface finish process;
H, receiving electrode: by half-finished for ceramic heating body surface-treated in step g 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 integrated ceramic heating body of the present embodiment, comprises following processing step:
A, batch mixing: be first the Si of 75% by mass percent
3n
4, the MgO of 7%, the Y of 3%
2o
3, 5% Al
2o
3, 5% SiO
2, 2% La
2o
3, 3% BN mixing and stirring make ceramic raw material, then by the ceramic raw material of 90% and 9% heating material MoSi
2, 1% heating material TiC mixing and stirring, make powder;
B, ball milling: powder, mill ball, water or alcohol that step a is obtained are put into ball grinder and carries out wet ball grinding, the time of wet ball grinding is 24h;
C, to be filtered dry: solid-liquid separation is carried out to the slurry after wet ball grinding in step b, the powder after being separated is carried out drying and processing;
D, injection moulding: by the powder injection moulding after drying and processing in step c, the shaping obtained base substrate of powder;
E, pre-burning: the base substrate that steps d is obtained carries out pre-burning, and the temperature of pre-burning is 1250 DEG C;
F, sintering: the base substrate after step e pre-burning is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, 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,
G, polished finish: ceramic heating body work in-process are carried out surface finish process;
H, receiving electrode: by half-finished for ceramic heating body surface-treated in step g two ends or sidepiece printing electrocondution slurry, electrocondution slurry makes electrode through the sintering of 1200 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 integrated 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 integrated 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 (10)
1. an integrated ceramic heating body, is characterized in that: it is made up of the raw material of following mass percent:
Ceramic raw material 50-95%
Heating material 5-50%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
470-96%
MgO 0.1-9%
Y
2O
30.1-5%
Al
2O
30.1-5%
SiO
2 0.1-5%
La
2O
30.1-3%
BN 0.1-3%；
Wherein, heating material is MoSi
2, one or both mixture in TiC.
2. the integrated ceramic heating body of one according to claim 1, is characterized in that: it is made up of the raw material of following mass percent:
Ceramic raw material 60-80%
Heating material 20-40%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
480-90%
MgO 2-6%
Y
2O
32-4%
Al
2O
32-4%
SiO
2 2-4%
La
2O
31-2.5%
BN 1-2.5%；
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. the integrated ceramic heating body of one according to claim 1, is characterized in that: it is made up of the raw material of following mass percent:
Ceramic raw material 70%
Heating material 30%;
Wherein, ceramic raw material is made up of the raw material of following mass percent:
Si
3N
485%
MgO 3%
Y
2O
33%
Al
2O
33%
SiO
2 3%
La
2O
31.5%
BN 1.5%；
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 integrated ceramic heating body described in claims 1 to 3 any one, is characterized in that: comprise following processing step:
A, batch mixing: first by the Si of formula ratio
3n
4, MgO, Y
2o
3, Al
2o
3, SiO
2, La
2o
3, BN mixing and stirring makes ceramic raw material, then by heating material MoSi
2, TiC, MoSi
2with the one in the mixture of TiC and ceramic raw material mixing and stirring, make powder;
B, ball milling: powder, mill ball, water or alcohol that step a is obtained are put into ball grinder and carries out wet ball grinding, the time of wet ball grinding is 8-24h;
C, to be filtered dry: solid-liquid separation is carried out to the slurry after wet ball grinding in step b, the powder after being separated is carried out drying and processing;
D, shaping: the powder after drying and processing in step c is shaping according to the one in following forming method: hot die-casting molding, dry-pressing formed, extrusion moulding, isostatic pressing, flow casting molding and injection moulding, the shaping obtained base substrate of powder;
E, pre-burning: the base substrate that steps d is obtained carries out pre-burning, and the temperature of pre-burning is 350-1250 DEG C;
F, sintering: sintering: 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, and blank sintering obtains ceramic heating body work in-process;
G, polished finish: ceramic heating body work in-process are carried out surface finish process;
H, receiving electrode: by half-finished for ceramic heating body surface-treated in step g 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 integrated ceramic heating body according to claim 4, it is characterized in that: step f sintering is specially: the base substrate after step e pre-burning 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 integrated ceramic heating body according to claim 4, is characterized in that: step f sintering is specially: the base substrate after step e pre-burning is placed in plumbago crucible or molybdenum crucible, and imbeds insulating powder, 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 integrated ceramic heating body according to claim 4, it is characterized in that: step f 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 integrated ceramic heating body according to claim 4, it is characterized in that: during steps d is shaping, described hot die-casting molding is: powder is added paraffin wax and stirring of heating, stir formation slip, slip added thermocompressor die cast;
Described be dry-pressing formedly: powder is added tackiness agent and mix and blend, mixes formation powder, powder is loaded oil press dry-pressing formed;
Described extrusion moulding is: powder is added tackiness agent and mix and blend, mixes formation powder, powder is loaded extruder for shaping;
Described isostatic pressing is: powder is added tackiness agent and mix and blend, mixes formation powder, is first loaded in rubber mold by powder, then loads isostatic pressing in isostatic pressing machine in the lump.
9. the preparation technology of a kind of integrated ceramic heating body according to claim 4, it is characterized in that: step h receiving electrode is specially: by half-finished for ceramic heating body surface-treated in step g 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.
10. the preparation technology of a kind of integrated ceramic heating body according to claim 4, is characterized in that: obtained ceramic heating body is a kind of shape in cellular, lattice-shaped, pole shape, tabular.
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| CN105523766A (en) * | 2016-03-03 | 2016-04-27 | 刘佩佩 | Silicon nitride and tantalum silicide composite ceramic material and preparation method thereof |
| CN106376107A (en) * | 2016-11-24 | 2017-02-01 | 常德科锐新材料科技有限公司 | Large-power silicon nitride ceramic heating plate and inner-soft outer-hard manufacturing method thereof |
| CN106747463A (en) * | 2016-12-14 | 2017-05-31 | 宜兴市华井科技有限公司 | A kind of anticorrosive special cermacis and preparation method thereof |
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| CN1314448A (en) * | 2001-04-26 | 2001-09-26 | 中国科学院上海硅酸盐研究所 | Molybdenum silicide base composite exothermic body and preparing method |
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| CN102595665A (en) * | 2012-02-28 | 2012-07-18 | 威海兴泰金属制造有限公司 | Silicon nitride heating sheet and manufacturing method thereof |
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| CN106376107B (en) * | 2016-11-24 | 2020-03-20 | 常德科锐新材料科技有限公司 | High-power silicon nitride ceramic heating plate and manufacturing method of high-power silicon nitride ceramic heating plate with soft inside and hard outside |
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| WO2019119612A1 (en) * | 2017-12-21 | 2019-06-27 | 深圳市卓力能电子有限公司 | Preparation process for novel porous ceramic heating body |
| CN108059479A (en) * | 2017-12-21 | 2018-05-22 | 深圳市卓力能电子有限公司 | A kind of preparation process of novel porous ceramic heating body |
| 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 |
| CN108492951A (en) * | 2018-03-11 | 2018-09-04 | 南京科敏电子有限公司 | SMD power-types NTC thermistor and its preparation process |
| CN109080238A (en) * | 2018-07-30 | 2018-12-25 | 福建闽航电子有限公司 | A kind of manufacturing method of ceramic heating plate |
| US20210269368A1 (en) * | 2018-08-17 | 2021-09-02 | Zone Infinity Co., Ltd. | Method for manufacturing active metal-brazed nitride ceramic substrate with excellent joining strength |
| US11964919B2 (en) * | 2018-08-17 | 2024-04-23 | Zone Infinityco., Ltd. | Method for manufacturing active metal-brazed nitride ceramic substrate with excellent joining strength |
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| CN115611637A (en) * | 2022-08-19 | 2023-01-17 | 江苏方达正塬电子材料科技有限公司 | Isolation powder and preparation method thereof |
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