CN105509488A - Internal heating device with immersive ceramic resistor - Google Patents
Internal heating device with immersive ceramic resistor Download PDFInfo
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- CN105509488A CN105509488A CN201510975416.XA CN201510975416A CN105509488A CN 105509488 A CN105509488 A CN 105509488A CN 201510975416 A CN201510975416 A CN 201510975416A CN 105509488 A CN105509488 A CN 105509488A
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- resistance tube
- biscuit
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- molten metal
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D11/00—Arrangement of elements for electric heating in or on furnaces
- F27D11/02—Ohmic resistance heating
- F27D11/04—Ohmic resistance heating with direct passage of current through the material being heated
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D99/00—Subject matter not provided for in other groups of this subclass
- F27D99/0001—Heating elements or systems
- F27D99/0006—Electric heating elements or system
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/148—Silicon, e.g. silicon carbide, magnesium silicide, heating transistors or diodes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3839—Refractory metal carbides
- C04B2235/3843—Titanium carbides
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/40—Metallic constituents or additives not added as binding phase
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D99/00—Subject matter not provided for in other groups of this subclass
- F27D99/0001—Heating elements or systems
- F27D99/0006—Electric heating elements or system
- F27D2099/0008—Resistor heating
- F27D2099/0011—The resistor heats a radiant tube or surface
- F27D2099/0013—The resistor heats a radiant tube or surface immersed in the charge
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27M—INDEXING SCHEME RELATING TO ASPECTS OF THE CHARGES OR FURNACES, KILNS, OVENS OR RETORTS
- F27M2001/00—Composition, conformation or state of the charge
- F27M2001/01—Charges containing mainly non-ferrous metals
Abstract
The invention provides an internal heating device with an immersive ceramic resistor. The internal heating device comprises a transformer and a molten pool, wherein a resistance tube and a first electrode are inserted into the molten pool; the upper end of the resistance tube is opened, and the lower end of the resistance tube is closed; both the molten pool and the resistance tube are filled with molten metal; a second electrode is inserted into the resistance tube; the lower parts of both the first electrode and the second electrode are immersed to the molten metal, and the upper parts of both the first electrode and the second electrode are connected with the transformer through conducting wires; and a silicon carbide coating is deposited on each of the inner and outer walls of the resistance tube. According to the internal heating device, the resistance tube, the electrodes, the molten metal and the transformer form a safety circuit, and energy required by the heating and heat preservation of the molten metal is provided by heat generated by the resistance tube, so that discharge failure on an interface of the resistance tube can be effectively avoided. Compared with the existing internal heating technology, the internal heating device has the characteristic of structure and function integration and also has higher safety and operation stability.
Description
Technical field
The invention belongs to heater technical field, be specifically related to a kind of immersion ceramic resistor inner heating device.
Background technology
In recent years, along with the enforcement of national Eleventh Five-Year Plan energy saving policy, employing new material, new technology carry out to high energy-consuming industries such as non-ferrous metal metallurgies the common recognition that reducing energy consumption becomes industry development.Wherein, in molten metal, heating technique at home and abroad obtains and approves widely, its general principle is that the internal heater with spontaneous thermal source is directly inserted metal bath, molten metal is transferred heat to by insulated jacket, thermal balance is reached by self heat transfer and convection current again by molten metal, and then technology liquation being heated, is incubated." external heat " mode (crucible heating or upper radiation heating) that contrast industry generally adopts at present, this technology has the advantages such as the thermal efficiency is high, resource loss is little, workpiece quality is high, energy-conserving and environment-protective, is a kind of new technology very with business promotion prospect.
At present; most internal heaters of engineering staff's design all adopt built-in thermal source; the mode of additional protective casing isolation is implemented; the internal heater technology of built-in electric heating element, additional composite ceramic protective sleeve as described in CN101765255A patent, and the internal heater technology of built-in gas heating assembly described in CN102506429A patent.But prior art is but faced with the problem of two aspects: one, the internal heater life-span depends on life-span of outer protective sleeve, and sheath damages certainly will cause internal heater global failure; Its two, internal heater lost efficacy and easily to cause the charged or liquid level of liquation to leap up fire in short-term, formed potential safety hazard, and then limited applying of interior heating technique.Therefore, immersion ceramic resistor inner heating device becomes a kind of feasible solution, its principle is integrated at spontaneous thermal source and insulated jacket, form " heater resistance pipe ", directly contacted and heating of metal liquation by safe load heater resistance pipe being applied to low-voltage and high-current, effectively can solve sheath to lose efficacy and form the problem such as potential safety hazard, its technological core is the preparation of internal heater resistance tube being applicable to molten metal, resistance adaptation.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of immersion ceramic resistor inner heating device.Resistance tube, electrode, molten metal and transformer are formed safety return circuit by this device, thered is provided the energy needed for heating and thermal insulation of molten metal by resistance tube self-heating, the coat of silicon carbide on resistance tube surface can effectively be avoided resistance tube and molten metal interface to discharge losing efficacy.Be compared to existing interior heating technique, the present invention has structure function one bulk properties, has higher safety and operation stability simultaneously.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of immersion ceramic resistor inner heating device, it is characterized in that, comprise transformer and molten bath, resistance tube and the first electrode is inserted with in described molten bath, the upper end open lower end closed of described resistance tube, all molten metal is loaded with in described molten bath and resistance tube, the second electrode is inserted with in described resistance tube, the bottom of described first electrode and the second electrode is all immersed in molten metal, described first electrode is all connected with transformer by wire with the top of the second electrode, the material of described resistance tube is carbide composite ceramic, the inner and outer wall of resistance tube all deposits coat of silicon carbide.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterized in that, the top of described resistance tube is provided with insulation cover plate, described insulation cover plate is provided with the breather pipe for passing into protective gas in resistance tube.
Above-mentioned a kind of immersion ceramic resistor inner heating device, is characterized in that, described molten metal be in Zn liquation, Al liquation, Mg liquation and Sn liquation any one or two or more.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterized in that, described first electrode and the second electrode are graphite electrode.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterized in that, described transformer is adjustable variable-pressure device, and the adjustable range of the output voltage of described adjustable variable-pressure device is 0V ~ 36V.
Above-mentioned a kind of immersion ceramic resistor inner heating device; it is characterized in that; the first thermocouple is inserted with in described molten bath; the second thermocouple is inserted with in described resistance tube; the thermometric end of described first thermocouple and the second thermocouple is all immersed in molten metal; described first thermocouple and the second thermocouple are all set with protection tube outward, and the material of described protection tube is Si
3n
4, AlN or Sialon pottery.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterized in that, the preparation method of described resistance tube comprises the following steps:
Step one, take each raw material of following mass percent: SiC45% ~ 75%, graphite 15% ~ 35%, Y
2o
31.5% ~ 3%; Al
2o
31% ~ 2%; Ni2.5% ~ 5%; Mo2.5% ~ 5%, TiC2.5% ~ 5%;
Step 2, each raw material ball milling taken in step one to be mixed, obtain basic powder, then by compressing after described basic granulation for powders, after oven dry, obtain biscuit;
Step 3, the ethanolic solution of phenolic resins is placed in pressurized tank, then biscuit described in step 2 is immersed in the ethanolic solution of phenolic resins, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 20min ~ 60min under the condition of 1MPa ~ 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 8h ~ 14h under the condition of 80 DEG C ~ 100 DEG C in temperature; The ethanolic solution of described phenolic resins is by phenolic resins and absolute ethyl alcohol in mass ratio (1 ~ 2): 1 mixes and forms;
Step 4, the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after dipping in step 3 is immersed in the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 20min ~ 60min under the condition of 1MPa ~ 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 8h ~ 14h under the condition of 80 DEG C ~ 100 DEG C in temperature; The aqueous solution of described butyl titanate is by butyl titanate and distilled water in mass ratio (2 ~ 4): 1 mixes and forms;
Step 5, repetition step 3 and step 4, till the constant mass of biscuit, then the biscuit after dipping is placed in high temperature sintering furnace, at nitrogen atmosphere, temperature is sinter 1h ~ 4h under the condition of 1650 DEG C ~ 1750 DEG C, obtains resistance tube.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterized in that, ball milling described in step 2 is high-energy ball milling, the rotating speed of described high-energy ball milling is 1000r/min ~ 2000r/min, the time of described high-energy ball milling is 2h ~ 4h, and the temperature of described oven dry is 100 DEG C ~ 150 DEG C, and the time of described oven dry is 4h ~ 8h, described compressing be isostatic cool pressing, the pressure of described isostatic cool pressing is 150MPa ~ 200MPa.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterized in that, the preparation method of described coat of silicon carbide is: resistance tube is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, argon gas is as diluent gas, be 200mL/min ~ 400mL/min at hydrogen flowing quantity, argon flow amount is 100mL/min ~ 150mL/min, temperature is deposit 2h ~ 6h under the condition of 1000 DEG C ~ 1200 DEG C, and the inner and outer wall of resistance tube all obtains coat of silicon carbide.
The present invention compared with prior art has the following advantages:
1, resistance tube, electrode, molten metal and transformer are formed safety return circuit by the present invention, are provided the energy needed for heating and thermal insulation of molten metal by resistance tube self-heating.Be compared to existing interior heating technique, the present invention has structure function one bulk properties, has higher safety and operation stability simultaneously.
2, resistance tube of the present invention is preferably the heater resistance pipe of SiC composite ceramics material, and it has the performance of the infiltration of significant anti-liquation, anticorrosive, anti-thermal shock, can cold plug and unlikely cracking in molten metal.
3, immersion ceramic resistor inner heating device of the present invention, its technological core is the internal heater resistance tube being applicable to molten metal, resistance adaptation, adopt the SiC composite ceramics material with good conductive characteristic, the high power consumption operating mode of low-voltage and high-current can be mated, long service life.
4, the present invention's interface electric discharge phenomena under the SiC dense coating of resistance tube surface preparation effectively can suppress big current condition, avoid resistance tube matrix to transship and lost efficacy.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the structural representation of immersion ceramic resistor inner heating device of the present invention.
Description of reference numerals:
1-resistance tube; 3-insulation cover plate; 4-breather pipe;
5-1-the first thermocouple; 5-2-the second thermocouple; 6-1-the first electrode;
6-2-the second electrode; 7-transformer; 8-molten metal;
9-molten bath.
Detailed description of the invention
Embodiment 1
As shown in Figure 1, the present embodiment immersion ceramic resistor inner heating device comprises transformer 7 and molten bath 9, resistance tube 1 and the first electrode 6-1 is inserted with in described molten bath 9, the upper end open lower end closed of described resistance tube 1, molten metal 8 is all loaded with in described molten bath 9 and resistance tube 1, the second electrode 6-2 is inserted with in described resistance tube 1, described first electrode 6-1, all be dipped in molten metal 8 with the bottom of the second electrode 6-2, described first electrode 6-1 is all connected with transformer 7 by wire with the top of the second electrode 6-2, the inner and outer wall of resistance tube 1 all deposits coat of silicon carbide.
As shown in Figure 1; the top of described resistance tube 1 is provided with insulation cover plate 3; described insulation cover plate 3 is provided with the breather pipe 4 for passing into protective gas in resistance tube 1; by passing into the protective gas such as nitrogen, argon gas in resistance tube 1, affect the service life of device in order to prevent molten metal 8 over oxidation in resistance tube.Described insulation cover plate 3 adopts the exotic material such as polytetrafluoroethylene (PTFE) or bakelite to make.
In the present embodiment, described molten metal 8 be in Zn liquation, Al liquation, Mg liquation and Sn liquation any one or two or more.
In the present embodiment, described first electrode 6-1 and the second electrode 6-2 is graphite electrode.
In the present embodiment, described transformer 7 is adjustable variable-pressure device, and the adjustable range of the output voltage of described adjustable variable-pressure device is 0V ~ 36V, and output voltage is adjustable, in order to ensure the safe operation of heater.
As shown in Figure 1, be inserted with the first thermocouple 5-1 in described molten bath 9, be inserted with the second thermocouple 5-2 in described resistance tube 1, the thermometric end of described first thermocouple 5-1 and the second thermocouple 5-2 is all dipped in molten metal 8.Due to the corrosivity of molten metal 8, the first thermocouple 5-1 and the second thermocouple 5-2 is all arranged with protection tube protection outward, and the material of described protection tube is Si
3n
4, AlN or Sialon insulating ceramics.
In the present embodiment, the preparation method of described coat of silicon carbide is: resistance tube 1 is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 300mL/min at hydrogen flowing quantity, and argon flow amount is 120mL/min, and temperature is deposit 4h under the condition of 1000 DEG C, and the inner and outer wall of resistance tube 1 all obtains coat of silicon carbide.
In the present embodiment, the material of described resistance tube 1 is carbide composite ceramic, and the preparation method of described resistance tube 1 comprises the following steps:
Step one, take each raw material of following mass percent: SiC55%, graphite 25%, Y
2o
33%; Al
2o
32%; Ni5%; Mo5%, TiC5%; Each raw material is powder, and graphite is preferably Nano graphite powder;
Step 2, each raw material ball milling taken in step one to be mixed, obtain basic powder, then by compressing after described basic granulation for powders, after oven dry, obtain biscuit; Described ball milling is high-energy ball milling, and the rotating speed of described high-energy ball milling is 1500r/min, and the time of described high-energy ball milling is 3h, the temperature of described oven dry is 120 DEG C, the time of described oven dry is 6h, described compressing be isostatic cool pressing, the pressure of described isostatic cool pressing is 180MPa;
Step 3, the ethanolic solution of phenolic resins is placed in pressurized tank, then biscuit described in step 2 is immersed in the ethanolic solution of phenolic resins, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 30min under the condition of 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 10h under the condition of 90 DEG C in temperature; The ethanolic solution of described phenolic resins in mass ratio by phenolic resins and absolute ethyl alcohol is mixed forms at 1.5: 1;
Step 4, the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after dipping in step 3 is immersed in the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 50min under the condition of 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 12h under the condition of 90 DEG C in temperature; The aqueous solution of described butyl titanate in mass ratio by butyl titanate and distilled water is mixed forms at 3: 1;
Step 5, repetition step 3 and step 4, till the constant mass of biscuit, then the biscuit after dipping is placed in high temperature sintering furnace, at nitrogen atmosphere, temperature is sinter 3h under the condition of 1700 DEG C, obtains resistance tube 1.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is in table 1.
The performance data of table 1 embodiment of the present invention 1 coat of silicon carbide and resistance tube 1
As shown in Table 1, resistance tube 1 has lower porosity, and intensity and thermal shock performance all can meet the Long-Time Service in liquation, and under 36V voltage, its limit uses power also can reach more than 20kW, is applicable to the demand of liquation heating and thermal insulation.Coating layer thickness reaches 37 μm, and interface bond strength is higher.
The using method of the present embodiment immersion ceramic resistor inner heating device is: by the electric current regulating transformer 7 to make its output safety load, electric current is the molten metal 8 in the second electrode 6-2, resistance tube 1, resistance tube 1, the molten metal in molten bath 9 and the first electrode 6-1 successively, form safety return circuit to transformer 7, utilize resistance tube 1 self-heating thus molten metal 8 is heated in galvanization.
Embodiment 2
The present embodiment immersion ceramic resistor inner heating device is identical with embodiment 1, and its difference is only: the preparation method of coat of silicon carbide and resistance tube 1 is different.Wherein, the preparation method of described coat of silicon carbide is: resistance tube 1 is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 400mL/min at hydrogen flowing quantity, and argon flow amount is 150mL/min, and temperature is deposit 6h under the condition of 1000 DEG C, and the inner and outer wall of resistance tube 1 all obtains coat of silicon carbide.The preparation method of described resistance tube 1 comprises the following steps:
Step one, take each raw material of following mass percent: SiC50%, graphite 33%, Y
2o
33%; Al
2o
32%; Ni4%; Mo4%, TiC4%; Each raw material is powder, and graphite is preferably Nano graphite powder;
Step 2, each raw material ball milling taken in step one to be mixed, obtain basic powder, then by compressing after described basic granulation for powders, after oven dry, obtain biscuit; Described ball milling is high-energy ball milling, and the rotating speed of described high-energy ball milling is 1000r/min, and the time of described high-energy ball milling is 4h, the temperature of described oven dry is 150 DEG C, the time of described oven dry is 8h, described compressing be isostatic cool pressing, the pressure of described isostatic cool pressing is 200MPa;
Step 3, the ethanolic solution of phenolic resins is placed in pressurized tank, then biscuit described in step 2 is immersed in the ethanolic solution of phenolic resins, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 20min under the condition of 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 8h under the condition of 100 DEG C in temperature; The ethanolic solution of described phenolic resins in mass ratio by phenolic resins and absolute ethyl alcohol is mixed forms at 1: 1;
Step 4, the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after dipping in step 3 is immersed in the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 60min under the condition of 1MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 14h under the condition of 80 DEG C in temperature; The aqueous solution of described butyl titanate in mass ratio by butyl titanate and distilled water is mixed forms at 4: 1;
Step 5, repetition step 3 and step 4, till the constant mass of biscuit, then the biscuit after dipping is placed in high temperature sintering furnace, at nitrogen atmosphere, temperature is sinter 4h under the condition of 1750 DEG C, obtains resistance tube 1.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is in table 2.
The performance data of table 2 embodiment of the present invention 2 coat of silicon carbide and resistance tube 1
As shown in Table 2, resistance tube 1 has low porosity, bending strength is greater than 50MPa, Critical thermal shock temperature difference is also greater than 500 DEG C, substantially the requirement of the Long-Time Service in liquation is met, under the operating mode of the maximum safe voltage of 36V, its limit uses power more than 20kW, is applicable to the heating and thermal insulation demand of molten metal; Coating layer thickness reaches 32 μm, and interface bond strength is higher.
The using method of the present embodiment immersion ceramic resistor inner heating device is: by the electric current regulating transformer 7 to make its output safety load, electric current is the molten metal 8 in the second electrode 6-2, resistance tube 1, resistance tube 1, the molten metal in molten bath 9 and the first electrode 6-1 successively, form safety return circuit to transformer 7, utilize resistance tube 1 self-heating thus molten metal 8 is heated in galvanization.
Embodiment 3
The present embodiment immersion ceramic resistor inner heating device is identical with embodiment 1, and its difference is only: the preparation method of coat of silicon carbide and resistance tube 1 is different.Wherein, the preparation method of described coat of silicon carbide is: resistance tube 1 is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 200mL/min at hydrogen flowing quantity, and argon flow amount is 100mL/min, and temperature is deposit 2h under the condition of 1200 DEG C, and the inner and outer wall of resistance tube 1 all obtains coat of silicon carbide.The preparation method of described resistance tube 1 comprises the following steps:
Step one, take each raw material of following mass percent: SiC60%, graphite 28%, Y
2o
31.5%; Al
2o
31.5%; Ni3%; Mo3%, TiC3%; Each raw material is powder, and graphite is preferably Nano graphite powder;
Step 2, each raw material ball milling taken in step one to be mixed, obtain basic powder, then by compressing after described basic granulation for powders, after oven dry, obtain biscuit; Described ball milling is high-energy ball milling, and the rotating speed of described high-energy ball milling is 1000r/min, and the time of described high-energy ball milling is 4h, the temperature of described oven dry is 150 DEG C, the time of described oven dry is 8h, described compressing be isostatic cool pressing, the pressure of described isostatic cool pressing is 200MPa;
Step 3, the ethanolic solution of phenolic resins is placed in pressurized tank, then biscuit described in step 2 is immersed in the ethanolic solution of phenolic resins, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 60min under the condition of 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 14h under the condition of 80 DEG C in temperature; The ethanolic solution of described phenolic resins in mass ratio by phenolic resins and absolute ethyl alcohol is mixed forms at 1.5: 1;
Step 4, the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after dipping in step 3 is immersed in the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 20min under the condition of 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 14h under the condition of 80 DEG C in temperature; The aqueous solution of described butyl titanate in mass ratio by butyl titanate and distilled water is mixed forms at 3: 1;
Step 5, repetition step 3 and step 4, till the constant mass of biscuit, then the biscuit after dipping is placed in high temperature sintering furnace, at nitrogen atmosphere, temperature is sinter 3h under the condition of 1700 DEG C, obtains resistance tube 1.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is in table 3.
The performance data of table 3 embodiment of the present invention 3 coat of silicon carbide and resistance tube 1
As shown in Table 3, resistance tube 1 has low porosity, bending strength is close to 60MPa, Critical thermal shock temperature difference is also greater than 500 DEG C, substantially the requirement of the Long-Time Service in liquation is met, under the operating mode of the maximum safe voltage of 36V, its limit uses power more than 20kW, is applicable to the heating and thermal insulation demand of molten metal; Coating layer thickness reaches 25 μm, and interface bond strength is higher.
The using method of the present embodiment immersion ceramic resistor inner heating device is: by the electric current regulating transformer 7 to make its output safety load, electric current is the molten metal 8 in the second electrode 6-2, resistance tube 1, resistance tube 1, the molten metal in molten bath 9 and the first electrode 6-1 successively, form safety return circuit to transformer 7, utilize resistance tube 1 self-heating thus molten metal 8 is heated in galvanization.
Embodiment 4
The present embodiment immersion ceramic resistor inner heating device is identical with embodiment 1, and its difference is only: the preparation method of coat of silicon carbide and resistance tube 1 is different.Wherein, the preparation method of described coat of silicon carbide is: resistance tube 1 is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 400mL/min at hydrogen flowing quantity, and argon flow amount is 150mL/min, and temperature is deposit 2h under the condition of 1000 DEG C, and the inner and outer wall of resistance tube 1 all obtains coat of silicon carbide.The preparation method of described resistance tube 1 comprises the following steps:
Step one, take each raw material of following mass percent: SiC62%, graphite 25%, Y
2o
32%; Al
2o
32%; Ni3%; Mo3%, TiC3%; Each raw material is powder, and graphite is preferably Nano graphite powder;
Step 2, each raw material ball milling taken in step one to be mixed, obtain basic powder, then by compressing after described basic granulation for powders, after oven dry, obtain biscuit; Described ball milling is high-energy ball milling, and the rotating speed of described high-energy ball milling is 1000r/min, and the time of described high-energy ball milling is 2h, the temperature of described oven dry is 100 DEG C, the time of described oven dry is 4h, described compressing be isostatic cool pressing, the pressure of described isostatic cool pressing is 150MPa;
Step 3, the ethanolic solution of phenolic resins is placed in pressurized tank, then biscuit described in step 2 is immersed in the ethanolic solution of phenolic resins, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 60min under the condition of 1MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 8h under the condition of 80 DEG C in temperature; The ethanolic solution of described phenolic resins in mass ratio by phenolic resins and absolute ethyl alcohol is mixed forms at 1.5: 1;
Step 4, the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after dipping in step 3 is immersed in the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 60min under the condition of 1MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 14h under the condition of 100 DEG C in temperature; The aqueous solution of described butyl titanate in mass ratio by butyl titanate and distilled water is mixed forms at 4: 1;
Step 5, repetition step 3 and step 4, till the constant mass of biscuit, then the biscuit after dipping is placed in high temperature sintering furnace, at nitrogen atmosphere, temperature is sinter 1h under the condition of 1750 DEG C, obtains resistance tube 1.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is in table 4.
The performance data of table 4 embodiment of the present invention 4 coat of silicon carbide and resistance tube 1
As shown in Table 4, resistance tube 1 has low porosity, bending strength is greater than 60MPa, Critical thermal shock temperature difference is also greater than 470 DEG C, substantially the requirement of the Long-Time Service in liquation is met, under the operating mode of the maximum safe voltage of 36V, its limit uses power more than 20kW, is applicable to the heating and thermal insulation demand of molten metal; Coating layer thickness reaches 24 μm, and interface bond strength is higher.
The using method of the present embodiment immersion ceramic resistor inner heating device is: by the electric current regulating transformer 7 to make its output safety load, electric current is the molten metal 8 in the second electrode 6-2, resistance tube 1, resistance tube 1, the molten metal in molten bath 9 and the first electrode 6-1 successively, form safety return circuit to transformer 7, utilize resistance tube 1 self-heating thus molten metal 8 is heated in galvanization.
Embodiment 5
The present embodiment immersion ceramic resistor inner heating device is identical with embodiment 1, and its difference is only: the preparation method of coat of silicon carbide and resistance tube 1 is different.Wherein, the preparation method of described coat of silicon carbide is: resistance tube 1 is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 200mL/min at hydrogen flowing quantity, and argon flow amount is 150mL/min, and temperature is deposit 6h under the condition of 1000 DEG C, and the inner and outer wall of resistance tube 1 all obtains coat of silicon carbide.The preparation method of described resistance tube 1 comprises the following steps:
Step one, take each raw material of following mass percent: SiC66%, graphite 20%, Y
2o
32%; Al
2o
31.5%; Ni3.5%; Mo3.5%, TiC3.5%; Each raw material is powder, and graphite is preferably Nano graphite powder;
Step 2, each raw material ball milling taken in step one to be mixed, obtain basic powder, then by compressing after described basic granulation for powders, after oven dry, obtain biscuit; Described ball milling is high-energy ball milling, and the rotating speed of described high-energy ball milling is 1000r/min, and the time of described high-energy ball milling is 4h, the temperature of described oven dry is 150 DEG C, the time of described oven dry is 8h, described compressing be isostatic cool pressing, the pressure of described isostatic cool pressing is 200MPa;
Step 3, the ethanolic solution of phenolic resins is placed in pressurized tank, then biscuit described in step 2 is immersed in the ethanolic solution of phenolic resins, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 60min under the condition of 1MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 14h under the condition of 100 DEG C in temperature; The ethanolic solution of described phenolic resins in mass ratio by phenolic resins and absolute ethyl alcohol is mixed forms at 2: 1;
Step 4, the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after dipping in step 3 is immersed in the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 60min under the condition of 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 14h under the condition of 100 DEG C in temperature; The aqueous solution of described butyl titanate in mass ratio by butyl titanate and distilled water is mixed forms at 3: 1;
Step 5, repetition step 3 and step 4, till the constant mass of biscuit, then the biscuit after dipping is placed in high temperature sintering furnace, at nitrogen atmosphere, temperature is sinter 4h under the condition of 1650 DEG C, obtains resistance tube 1.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is in table 5.
The performance data of table 5 embodiment of the present invention 5 coat of silicon carbide and resistance tube 1
As shown in Table 5, resistance tube 1 has low porosity, bending strength is greater than 60MPa, Critical thermal shock temperature difference is greater than 450 DEG C, meet the requirement of the Long-Time Service in liquation, under the operating mode of the maximum safe voltage of 36V, its limit uses power more than 20kW, is applicable to the heating and thermal insulation demand of molten metal; Coating layer thickness reaches 35 μm, and interface bond strength is higher.
The using method of the present embodiment immersion ceramic resistor inner heating device is: by the electric current regulating transformer 7 to make its output safety load, electric current is the molten metal 8 in the second electrode 6-2, resistance tube 1, resistance tube 1, the molten metal in molten bath 9 and the first electrode 6-1 successively, form safety return circuit to transformer 7, utilize resistance tube 1 self-heating thus molten metal 8 is heated in galvanization.
Embodiment 6
The present embodiment immersion ceramic resistor inner heating device is identical with embodiment 1, and its difference is only: the preparation method of coat of silicon carbide and resistance tube 1 is different.Wherein, the preparation method of described coat of silicon carbide is: resistance tube 1 is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 400mL/min at hydrogen flowing quantity, and argon flow amount is 100mL/min, and temperature is deposit 6h under the condition of 1000 DEG C, and the inner and outer wall of resistance tube 1 all obtains coat of silicon carbide.The preparation method of described resistance tube 1 comprises the following steps:
Step one, take each raw material of following mass percent: SiC45%, graphite 35%, Y
2o
33%; Al
2o
32%; Ni5%; Mo5%, TiC5%; Each raw material is powder, and graphite is preferably Nano graphite powder;
Step 2, each raw material ball milling taken in step one to be mixed, obtain basic powder, then by compressing after described basic granulation for powders, after oven dry, obtain biscuit; Described ball milling is high-energy ball milling, and the rotating speed of described high-energy ball milling is 2000r/min, and the time of described high-energy ball milling is 4h, the temperature of described oven dry is 150 DEG C, the time of described oven dry is 8h, described compressing be isostatic cool pressing, the pressure of described isostatic cool pressing is 150MPa;
Step 3, the ethanolic solution of phenolic resins is placed in pressurized tank, then biscuit described in step 2 is immersed in the ethanolic solution of phenolic resins, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 60min under the condition of 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 14h under the condition of 80 DEG C in temperature; The ethanolic solution of described phenolic resins in mass ratio by phenolic resins and absolute ethyl alcohol is mixed forms at 1: 1;
Step 4, the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after dipping in step 3 is immersed in the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 60min under the condition of 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 8h under the condition of 100 DEG C in temperature; The aqueous solution of described butyl titanate in mass ratio by butyl titanate and distilled water is mixed forms at 4: 1;
Step 5, repetition step 3 and step 4, till the constant mass of biscuit, then the biscuit after dipping is placed in high temperature sintering furnace, at nitrogen atmosphere, temperature is sinter 4h under the condition of 1750 DEG C, obtains resistance tube 1.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is in table 6.
The performance data of table 6 embodiment of the present invention 6 coat of silicon carbide and resistance tube 1
As shown in Table 6, resistance tube 1 has low porosity, bending strength is greater than 50MPa, Critical thermal shock temperature difference is also greater than 500 DEG C, substantially the requirement of the Long-Time Service in liquation is met, under the operating mode of the maximum safe voltage of 36V, its limit uses power more than 20kW, is applicable to the heating and thermal insulation demand of molten metal; Coating layer thickness reaches 27 μm, and interface bond strength is higher.
The using method of the present embodiment immersion ceramic resistor inner heating device is: by the electric current regulating transformer 7 to make its output safety load, electric current is the molten metal 8 in the second electrode 6-2, resistance tube 1, resistance tube 1, the molten metal in molten bath 9 and the first electrode 6-1 successively, form safety return circuit to transformer 7, utilize resistance tube 1 self-heating thus molten metal 8 is heated in galvanization.
Embodiment 7
The present embodiment immersion ceramic resistor inner heating device is identical with embodiment 1, and its difference is only: the preparation method of coat of silicon carbide and resistance tube 1 is different.Wherein, the preparation method of described coat of silicon carbide is: resistance tube 1 is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 400mL/min at hydrogen flowing quantity, and argon flow amount is 100mL/min, and temperature is deposit 6h under the condition of 1200 DEG C, and the inner and outer wall of resistance tube 1 all obtains coat of silicon carbide.The preparation method of described resistance tube 1 comprises the following steps:
Step one, take each raw material of following mass percent: SiC75%, graphite 15%, Y
2o
31.5%; Al
2o
31%; Ni2.5%; Mo2.5%, TiC2.5%; Each raw material is powder, and graphite is preferably Nano graphite powder;
Step 2, each raw material ball milling taken in step one to be mixed, obtain basic powder, then by compressing after described basic granulation for powders, after oven dry, obtain biscuit; Described ball milling is high-energy ball milling, and the rotating speed of described high-energy ball milling is 2000r/min, and the time of described high-energy ball milling is 4h, the temperature of described oven dry is 100 DEG C, the time of described oven dry is 8h, described compressing be isostatic cool pressing, the pressure of described isostatic cool pressing is 200MPa;
Step 3, the ethanolic solution of phenolic resins is placed in pressurized tank, then biscuit described in step 2 is immersed in the ethanolic solution of phenolic resins, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 60min under the condition of 1MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 8h under the condition of 100 DEG C in temperature; The ethanolic solution of described phenolic resins in mass ratio by phenolic resins and absolute ethyl alcohol is mixed forms at 1: 1;
Step 4, the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after dipping in step 3 is immersed in the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 20min under the condition of 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 8h under the condition of 100 DEG C in temperature; The aqueous solution of described butyl titanate in mass ratio by butyl titanate and distilled water is mixed forms at 2: 1;
Step 5, repetition step 3 and step 4, till the constant mass of biscuit, then the biscuit after dipping is placed in high temperature sintering furnace, at nitrogen atmosphere, temperature is sinter 4h under the condition of 1650 DEG C, obtains resistance tube 1.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is in table 7.
The performance data of table 7 embodiment of the present invention 7 coat of silicon carbide and resistance tube 1
As shown in Table 7, resistance tube 1 has low porosity, bending strength is greater than 70MPa, Critical thermal shock temperature difference is also greater than 450 DEG C, meet the requirement of the Long-Time Service in liquation, under the operating mode of the maximum safe voltage of 36V, its limit uses power more than 20kW, is applicable to the heating and thermal insulation demand of molten metal; Coating layer thickness reaches 34 μm, and interface bond strength is high.
The using method of the present embodiment immersion ceramic resistor inner heating device is: by the electric current regulating transformer 7 to make its output safety load, electric current is the molten metal 8 in the second electrode 6-2, resistance tube 1, resistance tube 1, the molten metal in molten bath 9 and the first electrode 6-1 successively, form safety return circuit to transformer 7, utilize resistance tube 1 self-heating thus molten metal 8 is heated in galvanization.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (9)
1. an immersion ceramic resistor inner heating device, it is characterized in that, comprise transformer (7) and molten bath (9), resistance tube (1) and the first electrode (6-1) is inserted with in described molten bath (9), the upper end open lower end closed of described resistance tube (1), molten metal (8) is all loaded with in described molten bath (9) and resistance tube (1), the second electrode (6-2) is inserted with in described resistance tube (1), the bottom of described first electrode (6-1) and the second electrode (6-2) is all immersed in molten metal (8), described first electrode (6-1) is all connected with transformer (7) by wire with the top of the second electrode (6-2), the material of described resistance tube (1) is carbide composite ceramic, the inner and outer wall of resistance tube (1) all deposits coat of silicon carbide.
2. a kind of immersion ceramic resistor inner heating device according to claim 1; it is characterized in that; the top of described resistance tube (1) is provided with insulation cover plate (3), described insulation cover plate (3) is provided with the breather pipe (4) for passing into protective gas in resistance tube (1).
3. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterized in that, described molten metal (8) is Zn liquation, in Al liquation, Mg liquation and Sn liquation any one or two or more.
4. a kind of immersion ceramic resistor inner heating device according to claim 1, is characterized in that, described first electrode (6-1) and the second electrode (6-2) are graphite electrode.
5. a kind of immersion ceramic resistor inner heating device according to claim 1, is characterized in that, described transformer (7) is adjustable variable-pressure device, and the adjustable range of the output voltage of described adjustable variable-pressure device is 0V ~ 36V.
6. a kind of immersion ceramic resistor inner heating device according to claim 1; it is characterized in that; the first thermocouple (5-1) is inserted with in described molten bath (9); the second thermocouple (5-2) is inserted with in described resistance tube (1); the thermometric end of described first thermocouple (5-1) and the second thermocouple (5-2) is all immersed in molten metal (8); described first thermocouple (5-1) and the second thermocouple (5-2) are all set with protection tube outward, and the material of described protection tube is Si
3n
4, AlN or Sialon pottery.
7. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterized in that, the preparation method of described resistance tube (1) comprises the following steps:
Step one, take each raw material of following mass percent: SiC45% ~ 75%, graphite 15% ~ 35%, Y
2o
31.5% ~ 3%; Al
2o
31% ~ 2%; Ni2.5% ~ 5%; Mo2.5% ~ 5%, TiC2.5% ~ 5%;
Step 2, each raw material ball milling taken in step one to be mixed, obtain basic powder, then by compressing after described basic granulation for powders, after oven dry, obtain biscuit;
Step 3, the ethanolic solution of phenolic resins is placed in pressurized tank, then biscuit described in step 2 is immersed in the ethanolic solution of phenolic resins, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 20min ~ 60min under the condition of 1MPa ~ 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 8h ~ 14h under the condition of 80 DEG C ~ 100 DEG C in temperature; The ethanolic solution of described phenolic resins is by phenolic resins and absolute ethyl alcohol in mass ratio (1 ~ 2): 1 mixes and forms;
Step 4, the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after dipping in step 3 is immersed in the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, gas pressure in pressurized tank is to biscuit dipping 20min ~ 60min under the condition of 1MPa ~ 2MPa, then the biscuit after dipping being placed in vacuum drying chamber, is dry 8h ~ 14h under the condition of 80 DEG C ~ 100 DEG C in temperature; The aqueous solution of described butyl titanate is by butyl titanate and distilled water in mass ratio (2 ~ 4): 1 mixes and forms;
Step 5, repetition step 3 and step 4, till the constant mass of biscuit, then the biscuit after dipping is placed in high temperature sintering furnace, at nitrogen atmosphere, temperature is sinter 1h ~ 4h under the condition of 1650 DEG C ~ 1750 DEG C, obtains resistance tube (1).
8. a kind of immersion ceramic resistor inner heating device according to claim 7, it is characterized in that, ball milling described in step 2 is high-energy ball milling, the rotating speed of described high-energy ball milling is 1000r/min ~ 2000r/min, the time of described high-energy ball milling is 2h ~ 4h, and the temperature of described oven dry is 100 DEG C ~ 150 DEG C, and the time of described oven dry is 4h ~ 8h, described compressing be isostatic cool pressing, the pressure of described isostatic cool pressing is 150MPa ~ 200MPa.
9. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterized in that, the preparation method of described coat of silicon carbide is: resistance tube (1) is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, argon gas is as diluent gas, be 200mL/min ~ 400mL/min at hydrogen flowing quantity, argon flow amount is 100mL/min ~ 150mL/min, temperature is deposit 2h ~ 6h under the condition of 1000 DEG C ~ 1200 DEG C, and the inner and outer wall of resistance tube (1) all obtains coat of silicon carbide.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106083066A (en) * | 2016-06-12 | 2016-11-09 | 辽宁伊菲科技股份有限公司 | Silicon nitride adds the manufacture method of heat pipe |
| CN111279791A (en) * | 2017-10-31 | 2020-06-12 | 日本特殊陶业株式会社 | Ceramic heater for heating fluid |
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| EP0602680A1 (en) * | 1992-12-18 | 1994-06-22 | Praxair S.T. Technology, Inc. | Potassium silicate-containing sealant |
| WO1996009738A1 (en) * | 1994-09-20 | 1996-03-28 | Negawatt Gmbh | Electric heating element |
| CN2443005Y (en) * | 2000-09-07 | 2001-08-15 | 吴金盛 | Hot-dip equipment for wire straight-line moving into it through fusion pot |
| CN201390777Y (en) * | 2008-08-01 | 2010-01-27 | 王青松 | Heating rod of internal heating type hot-dip galvanized device |
| CN101765255A (en) * | 2010-02-02 | 2010-06-30 | 西安交通大学 | Immersion type hot-dip plating composite ceramic protecting pipe and preparation method thereof |
| CN102506429A (en) * | 2011-11-07 | 2012-06-20 | 西安交通大学 | Immersed gas ceramic inner heater sleeve and preparation method thereof |
| CN103406503A (en) * | 2013-07-16 | 2013-11-27 | 辽宁科技大学 | Method for producing high-quality large steel ingot and device thereof |
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| CN106083066A (en) * | 2016-06-12 | 2016-11-09 | 辽宁伊菲科技股份有限公司 | Silicon nitride adds the manufacture method of heat pipe |
| CN111279791A (en) * | 2017-10-31 | 2020-06-12 | 日本特殊陶业株式会社 | Ceramic heater for heating fluid |
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