CN105509488B - A kind of immersion ceramic resistor inner heating device - Google Patents

A kind of immersion ceramic resistor inner heating device Download PDF

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Publication number
CN105509488B
CN105509488B CN201510975416.XA CN201510975416A CN105509488B CN 105509488 B CN105509488 B CN 105509488B CN 201510975416 A CN201510975416 A CN 201510975416A CN 105509488 B CN105509488 B CN 105509488B
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resistance tube
electrode
biscuit
heating device
molten metal
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CN105509488A (en
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杨万利
代丽娜
赵松
彭志刚
冯婧
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Chaoma Science & Technology Co Ltd Xian
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Chaoma Science & Technology Co Ltd Xian
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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
    • C—CHEMISTRY; METALLURGY
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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
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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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
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • 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
    • 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
    • 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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    • C04B2235/00—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
    • C04B2235/40—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
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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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Resistance Heating (AREA)

Abstract

The invention provides a kind of immersion ceramic resistor inner heating device, including transformer and molten bath, resistance tube and first electrode are inserted with the molten bath, the upper end open lower end closed of the resistance tube, molten metal is loaded with the molten bath and resistance tube, second electrode is inserted with the resistance tube, the bottom of the first electrode and second electrode is immersed in molten metal, the top of the first electrode and second electrode is connected by wire with transformer, and deposition has coat of silicon carbide on the inner and outer wall of resistance tube.Resistance tube, electrode, molten metal and transformer are constituted safety return circuit by the present invention, and the energy needed for the heating and thermal insulation of molten metal is provided by resistance tube self-heating, can be prevented effectively from the electric discharge failure of resistance tube interface.Existing interior heating technique is compared to, the present invention has the bulk properties of structure function one, while having higher safety and operation stability.

Description

A kind of immersion ceramic resistor inner heating device
Technical field
The invention belongs to heater technical field, and in particular to a kind of immersion ceramic resistor inner heating device.
Background technology
In recent years, with the implementation of national Eleventh Five-Year Plan energy saving policy, using new material, new technology to non-ferrous metal metallurgy Common recognition of the reducing energy consumption as industry development is carried out Deng high energy-consuming industry.Wherein, heating technique is at home and abroad obtained in molten metal Extensive accreditation was obtained, its general principle is that the internal heater with spontaneous thermal source is inserted directly into metal bath, and passed through isolation Sheath transfers heat to molten metal, then by the heat transfer and convection current of itself reaches thermal balance by molten metal, and then right The technology that liquation is heated, is incubated.(crucible is heated " external heat " mode that contrast industry is generally used at present or upper radiation adds Heat), the technology has the advantages such as the thermal efficiency high, resource loss small, workpiece quality is high, energy-conserving and environment-protective, is that one kind has business very much The new technology of industry promotion prospect.
At present, most internal heaters of engineering staff's design thermal source built in, additional protection sleeve pipe isolation Mode is implemented, the internal heater skill of built-in electric heating element, additional composite ceramic protective sleeve as described in CN101765255A patents Art, and built-in gas heating component described in CN102506429A patents internal heater technology.However, prior art but faces Problem of both：First, the internal heater life-span depends on the life-span of outer protective sleeve, sheath, which is damaged, certainly will cause internal heater Global failure；Second, the internal heater failure fire that easily causes that liquation is powered or liquid level is leapt up interior in short-term, forms potential safety hazard, and then limit The popularization and application of interior heating technique are made.Therefore, immersion ceramic resistor inner heating device turns into a kind of feasible solution, Its principle is that spontaneous thermal source and insulated jacket integrate, and is constituted " heater resistance pipe ", by being applied to heater resistance pipe Plus the safe load of low-voltage and high-current directly contacts and heats molten metal, it can effectively solve sheath and fail to form safe hidden The problems such as suffering from, its technological core applies to molten metal, the preparation of the internal heater resistance tube of resistance adaptation.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of immersion ceramics for above-mentioned the deficiencies in the prior art Resistance inner heating device.Resistance tube, electrode, molten metal and transformer are constituted safety return circuit by the device, by resistance tube certainly Body generates heat to providing the energy needed for the heating and thermal insulation of molten metal, and the coat of silicon carbide of resistance pipe surface can be prevented effectively from electricity Resistance pipe discharges with molten metal interface to fail.Existing interior heating technique is compared to, the present invention has the bulk properties of structure function one, There is higher safety and operation stability simultaneously.
In order to solve the above technical problems, the technical solution adopted by the present invention is：Heating dress in a kind of immersion ceramic resistor Put, it is characterised in that including transformer and molten bath, resistance tube and first electrode are inserted with the molten bath, the resistance tube It is loaded with upper end open lower end closed, the molten bath and resistance tube in molten metal, the resistance tube and is inserted with the second electricity Pole, the bottom of the first electrode and second electrode is immersed in molten metal, the first electrode and second electrode it is upper Portion is connected by wire with transformer, and the material of the resistance tube is carbide composite ceramic, the inner and outer wall of resistance tube On deposition have coat of silicon carbide.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterised in that be provided with the top of the resistance tube The breather pipe for being passed through protective gas into resistance tube is provided with insulation cover plate, the insulation cover plate.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterised in that the molten metal is Zn liquations, Al In liquation, Mg liquations and Sn liquations any one or it is two or more.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterised in that the first electrode and second electrode It is graphite electrode.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterised in that the transformer is adjustable variable-pressure Device, the adjustable range of the output voltage of the adjustable variable-pressure device is 0V~36V.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterised in that the first heat is inserted with the molten bath The second thermocouple is inserted with galvanic couple, the resistance tube, the thermometric end of first thermocouple and the second thermocouple is immersed in In molten metal, protection pipe is set with outside first thermocouple and the second thermocouple, the material of the protection pipe is Si3N4、 AlN or Sialon ceramics.
A kind of above-mentioned immersion ceramic resistor inner heating device, it is characterised in that the preparation method bag of the resistance tube Include following steps：
Step 1: weighing each raw material of following mass percent：SiC 45%~75%, graphite 15%~35%, Y2O31.5%~3%；Al2O31%~2%；Ni 2.5%~5%；Mo 2.5%~5%, TiC 2.5%~5%；
Step 2: each raw material ball milling weighed in step one is well mixed, basic powder is obtained, then by the basis It is compressing after granulation for powders, biscuit is obtained after drying；
Step 3: the ethanol solution of phenolic resin is placed in pressurized tank, biscuit described in step 2 is then immersed into phenol In the ethanol solution of urea formaldehyde, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 1MPa~ 20min~60min is impregnated to biscuit under conditions of 2MPa, then the biscuit after dipping is placed in vacuum drying chamber, in temperature To dry 8h~14h under conditions of 80 DEG C~100 DEG C；The ethanol solution of the phenolic resin is pressed by phenolic resin and absolute ethyl alcohol Mass ratio (1~2): 1 well mixed forms；
Step 4: the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after being impregnated in step 3 is immersed In the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 1MPa~ 20min~60min is impregnated to biscuit under conditions of 2MPa, then the biscuit after dipping is placed in vacuum drying chamber, in temperature To dry 8h~14h under conditions of 80 DEG C~100 DEG C；The aqueous solution of the butyl titanate presses quality by butyl titanate and distilled water Than (2~4): 1 well mixed forms；
Step 5: repeat step three and step 4, untill the constant mass of biscuit, then put the biscuit after dipping In high temperature sintering furnace, in nitrogen atmosphere, temperature is sintering 1h~4h under conditions of 1650 DEG C~1750 DEG C, obtains resistance tube.
Above-mentioned a kind of immersion ceramic resistor inner heating device, it is characterised in that ball milling described in step 2 is high energy Ball milling, the rotating speed of the high-energy ball milling is 1000r/min~2000r/min, and the time of the high-energy ball milling is 2h~4h, described The temperature of drying is 100 DEG C~150 DEG C, and time of the drying is 4h~8h, it is described it is compressing be isostatic cool pressing, it is described cold The pressure of isostatic pressed is 150MPa~200MPa.
A kind of above-mentioned immersion ceramic resistor inner heating device, it is characterised in that the preparation side of the coat of silicon carbide Method is：Resistance tube is placed in chemical vapor deposition stove, using CH3SiCl3As raw material, hydrogen is as carrier gas, and argon gas is as dilute Outgassing body, is 200mL/min~400mL/min in hydrogen flowing quantity, argon flow amount is 100mL/min~150mL/min, and temperature is 2h~6h is deposited under conditions of 1000 DEG C~1200 DEG C, coat of silicon carbide is obtained on the inner and outer wall of resistance tube.
The present invention has advantages below compared with prior art：
1st, resistance tube, electrode, molten metal and transformer are constituted safety return circuit by the present invention, pass through resistance tube self-heating To provide the energy needed for the heating and thermal insulation of molten metal.Existing interior heating technique is compared to, the present invention has structure function One bulk properties, while having higher safety and operation stability.
2nd, resistance tube of the present invention is preferably the heater resistance pipe of SiC composite ceramics materials, and it has significant anti- Liquation infiltration, anticorrosive, anti-thermal shock performance, in molten metal can it is cold plug and will not ftracture.
3rd, immersion ceramic resistor inner heating device of the present invention, its technological core applies to molten metal, electricity The internal heater resistance tube of adaptation is hindered, using the SiC composite ceramics materials with good conductive characteristic, low-voltage can be matched big The high power consumption operating mode of electric current, service life is long.
4th, present invention interface electric discharge under the conditions of SiC dense coatings prepared by resistance pipe surface can effectively suppress high current is existing As, it is to avoid the overload failure of resistance tube matrix.
The present invention is described in further detail with reference to the accompanying drawings and examples.
Brief description of the drawings
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；
The thermocouples of 5-1-first；The thermocouples of 5-2-second；6-1-first electrode；
6-2-second electrode；7-transformer；8-molten metal；
9-molten bath.
Embodiment
Embodiment 1
As shown in figure 1, the present embodiment immersion ceramic resistor inner heating device includes transformer 7 and molten bath 9, the molten bath Resistance tube 1 and first electrode 6-1, the upper end open lower end closed of the resistance tube 1, the molten bath 9 and resistance tube are inserted with 9 It is loaded with 1 in molten metal 8, the resistance tube 1 and is inserted with second electrode 6-2, the first electrode 6-1 and the second electricity Pole 6-2 bottom is dipped in molten metal 8, and the top of the first electrode 6-1 and second electrode 6-2 pass through wire and change Depressor 7 is connected, and deposition has coat of silicon carbide on the inner and outer wall of resistance tube 1.
It is used for as shown in figure 1, the top of the resistance tube 1 is provided with to be provided with insulation cover plate 3, the insulation cover plate 3 The breather pipe 4 of protective gas is passed through into resistance tube 1, by being passed through the protective gas such as nitrogen, argon gas into resistance tube 1, is used to Prevent that the over oxidation of molten metal 8 influences the service life of device in resistance tube.The insulation cover plate 3 using polytetrafluoroethylene (PTFE) or The exotic materials such as bakelite are made.
In the present embodiment, the molten metal 8 be Zn liquations, Al liquations, Mg liquations and Sn liquations in any one or It is two or more.
In the present embodiment, the first electrode 6-1 and second electrode 6-2 are graphite electrode.
In the present embodiment, the transformer 7 is adjustable variable-pressure device, the regulation of the output voltage of the adjustable variable-pressure device Scope is 0V~36V, and output voltage is adjustable, the safe operation to ensure heater.
The second thermoelectricity is inserted with as shown in figure 1, being inserted with the molten bath 9 in first thermocouple 5-1, the resistance tube 1 Even 5-2, the first thermocouple 5-1 and the second thermocouple 5-2 thermometric end are dipped in molten metal 8.Due to molten metal 8 Corrosivity, be arranged with protection pipe outside the first thermocouple 5-1 and the second thermocouple 5-2 and protected, the material of the protection pipe Matter is Si3N4, AlN or Sialon insulating ceramicses.
In the present embodiment, the preparation method of the coat of silicon carbide is：Resistance tube 1 is placed in chemical vapor deposition stove, Using CH3SiCl3As raw material, hydrogen, as diluent gas, is 300mL/min, argon gas in hydrogen flowing quantity as carrier gas, argon gas Flow is 120mL/min, and temperature is carbonized to deposit 4h under conditions of 1000 DEG C on the inner and outer wall of resistance tube 1 Silicon coating.
In the present embodiment, the material of the resistance tube 1 is carbide composite ceramic, the preparation method bag of the resistance tube 1 Include following steps：
Step 1: weighing each raw material of following mass percent：SiC 55%, graphite 25%, Y2O33%；Al2O32%； Ni 5%；Mo 5%, TiC 5%；Each raw material is powder, and graphite is preferably Nano graphite powder；
Step 2: each raw material ball milling weighed in step one is well mixed, basic powder is obtained, then by the basis It is compressing after granulation for powders, biscuit is obtained after drying；The ball milling is high-energy ball milling, and the rotating speed of the high-energy ball milling is 1500r/min, the time of the high-energy ball milling is 3h, and the temperature of the drying is 120 DEG C, and the time of the drying is 6h, institute It is isostatic cool pressing to state compressing, and the pressure of the isostatic cool pressing is 180MPa；
Step 3: the ethanol solution of phenolic resin is placed in pressurized tank, biscuit described in step 2 is then immersed into phenol In the ethanol solution of urea formaldehyde, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 2MPa bar 30min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, is done under conditions of temperature is 90 DEG C Dry 10h；The ethanol solution of the phenolic resin is formed by phenolic resin and absolute ethyl alcohol in mass ratio 1.5: 1 are well mixed；
Step 4: the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after being impregnated in step 3 is immersed In the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 2MPa bar 50min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, is done under conditions of temperature is 90 DEG C Dry 12h；The aqueous solution of the butyl titanate is formed by butyl titanate and distilled water in mass ratio 3: 1 are well mixed；
Step 5: repeat step three and step 4, untill the constant mass of biscuit, then put the biscuit after dipping In high temperature sintering furnace, in nitrogen atmosphere, temperature obtains resistance tube 1 to sinter 3h under conditions of 1700 DEG C.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is shown in Table 1.
The performance data of the coat of silicon carbide of 1 embodiment of the present invention of table 1 and resistance tube 1
As shown in Table 1, resistance tube 1 has relatively low porosity, and intensity and thermal shock performance can meet the length in liquation Phase uses, under 36V voltages, and its limit can also reach more than 20kW using power, is adapted to the demand of liquation heating and thermal insulation.Coating Thickness reaches 37 μm, and interface bond strength is higher.
The application method of the present embodiment immersion ceramic resistor inner heating device is：It is exported by adjusting transformer 7 The electric current of safe load, electric current sequentially pass through second electrode 6-2, resistance tube 1, the molten metal 8 in resistance tube 1, in molten bath 9 Molten metal and first electrode 6-1, to transformer 7 constitute safety return circuit, using resistance tube 1 in galvanization self-heating So as to be heated to molten metal 8.
Embodiment 2
The present embodiment immersion ceramic resistor inner heating device is same as Example 1, and it the difference is that only：Carborundum The preparation method of coating and resistance tube 1 is different.Wherein, the preparation method of the coat of silicon carbide is：By being placed in of resistance tube 1 Learn in gaseous phase deposition stove, using CH3SiCl3As raw material, hydrogen is in hydrogen flowing quantity as diluent gas as carrier gas, argon gas 400mL/min, argon flow amount is 150mL/min, and temperature is to deposit 6h under conditions of 1000 DEG C, in the inwall of resistance tube 1 and outer Coat of silicon carbide is obtained on wall.The preparation method of the resistance tube 1 comprises the following steps：
Step 1: weighing each raw material of following mass percent：SiC 50%, graphite 33%, Y2O33%；Al2O32%； Ni 4%；Mo 4%, TiC 4%；Each raw material is powder, and graphite is preferably Nano graphite powder；
Step 2: each raw material ball milling weighed in step one is well mixed, basic powder is obtained, then by the basis It is compressing after granulation for powders, biscuit is obtained after drying；The ball milling is high-energy ball milling, and the rotating speed of the high-energy ball milling is 1000r/min, the time of the high-energy ball milling is 4h, and the temperature of the drying is 150 DEG C, and the time of the drying is 8h, institute It is isostatic cool pressing to state compressing, and the pressure of the isostatic cool pressing is 200MPa；
Step 3: the ethanol solution of phenolic resin is placed in pressurized tank, biscuit described in step 2 is then immersed into phenol In the ethanol solution of urea formaldehyde, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 2MPa bar 20min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, under conditions of temperature is 100 DEG C Dry 8h；The ethanol solution of the phenolic resin is formed by phenolic resin and absolute ethyl alcohol in mass ratio 1: 1 are well mixed；
Step 4: the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after being impregnated in step 3 is immersed In the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 1MPa bar 60min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, is done under conditions of temperature is 80 DEG C Dry 14h；The aqueous solution of the butyl titanate is formed by butyl titanate and distilled water in mass ratio 4: 1 are well mixed；
Step 5: repeat step three and step 4, untill the constant mass of biscuit, then put the biscuit after dipping In high temperature sintering furnace, in nitrogen atmosphere, temperature obtains resistance tube 1 to sinter 4h under conditions of 1750 DEG C.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is shown in Table 2.
The performance data of the coat of silicon carbide of 2 embodiment of the present invention of table 2 and resistance tube 1
As shown in Table 2, resistance tube 1 have low porosity, bending strength be more than 50MPa, Critical thermal shock temperature difference also greater than 500 DEG C, the requirement of the long-term use in liquation is substantially met, under the operating mode of the maximum safe voltages of 36V, its limit uses work( Rate is more than 20kW, it is adaptable to the heating and thermal insulation demand of molten metal；Coating layer thickness reaches 32 μm, and interface bond strength is higher.
The application method of the present embodiment immersion ceramic resistor inner heating device is：It is exported by adjusting transformer 7 The electric current of safe load, electric current sequentially pass through second electrode 6-2, resistance tube 1, the molten metal 8 in resistance tube 1, in molten bath 9 Molten metal and first electrode 6-1, to transformer 7 constitute safety return circuit, using resistance tube 1 in galvanization self-heating So as to be heated to molten metal 8.
Embodiment 3
The present embodiment immersion ceramic resistor inner heating device is same as Example 1, and it the difference is that only：Carborundum The preparation method of coating and resistance tube 1 is different.Wherein, the preparation method of the coat of silicon carbide is：By being placed in of resistance tube 1 Learn in gaseous phase deposition stove, using CH3SiCl3As raw material, hydrogen is in hydrogen flowing quantity as diluent gas as carrier gas, argon gas 200mL/min, argon flow amount is 100mL/min, and temperature is to deposit 2h under conditions of 1200 DEG C, in the inwall of resistance tube 1 and outer Coat of silicon carbide is obtained on wall.The preparation method of the resistance tube 1 comprises the following steps：
Step 1: weighing each raw material of following mass percent：SiC 60%, graphite 28%, Y2O31.5%； Al2O31.5%；Ni 3%；Mo 3%, TiC 3%；Each raw material is powder, and graphite is preferably Nano graphite powder；
Step 2: each raw material ball milling weighed in step one is well mixed, basic powder is obtained, then by the basis It is compressing after granulation for powders, biscuit is obtained after drying；The ball milling is high-energy ball milling, and the rotating speed of the high-energy ball milling is 1000r/min, the time of the high-energy ball milling is 4h, and the temperature of the drying is 150 DEG C, and the time of the drying is 8h, institute It is isostatic cool pressing to state compressing, and the pressure of the isostatic cool pressing is 200MPa；
Step 3: the ethanol solution of phenolic resin is placed in pressurized tank, biscuit described in step 2 is then immersed into phenol In the ethanol solution of urea formaldehyde, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 2MPa bar 60min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, is done under conditions of temperature is 80 DEG C Dry 14h；The ethanol solution of the phenolic resin is formed by phenolic resin and absolute ethyl alcohol in mass ratio 1.5: 1 are well mixed；
Step 4: the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after being impregnated in step 3 is immersed In the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 2MPa bar 20min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, is done under conditions of temperature is 80 DEG C Dry 14h；The aqueous solution of the butyl titanate is formed by butyl titanate and distilled water in mass ratio 3: 1 are well mixed；
Step 5: repeat step three and step 4, untill the constant mass of biscuit, then put the biscuit after dipping In high temperature sintering furnace, in nitrogen atmosphere, temperature obtains resistance tube 1 to sinter 3h under conditions of 1700 DEG C.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is shown in Table 3.
The performance data of the coat of silicon carbide of 3 embodiment of the present invention of table 3 and resistance tube 1
As shown in Table 3, resistance tube 1 has low porosity, bending strength close to 60MPa, Critical thermal shock temperature difference also greater than 500 DEG C, the requirement of the long-term use in liquation is substantially met, under the operating mode of the maximum safe voltages of 36V, its limit uses work( Rate is more than 20kW, it is adaptable to the heating and thermal insulation demand of molten metal；Coating layer thickness reaches 25 μm, and interface bond strength is higher.
The application method of the present embodiment immersion ceramic resistor inner heating device is：It is exported by adjusting transformer 7 The electric current of safe load, electric current sequentially pass through second electrode 6-2, resistance tube 1, the molten metal 8 in resistance tube 1, in molten bath 9 Molten metal and first electrode 6-1, to transformer 7 constitute safety return circuit, using resistance tube 1 in galvanization self-heating So as to be heated to molten metal 8.
Embodiment 4
The present embodiment immersion ceramic resistor inner heating device is same as Example 1, and it the difference is that only：Carborundum The preparation method of coating and resistance tube 1 is different.Wherein, the preparation method of the coat of silicon carbide is：By being placed in of resistance tube 1 Learn in gaseous phase deposition stove, using CH3SiCl3As raw material, hydrogen is in hydrogen flowing quantity as diluent gas as carrier gas, argon gas 400mL/min, argon flow amount is 150mL/min, and temperature is to deposit 2h under conditions of 1000 DEG C, in the inwall of resistance tube 1 and outer Coat of silicon carbide is obtained on wall.The preparation method of the resistance tube 1 comprises the following steps：
Step 1: weighing each raw material of following mass percent：SiC 62%, graphite 25%, Y2O32%；Al2O32%； Ni 3%；Mo 3%, TiC 3%；Each raw material is powder, and graphite is preferably Nano graphite powder；
Step 2: each raw material ball milling weighed in step one is well mixed, basic powder is obtained, then by the basis It is compressing after granulation for powders, biscuit is obtained after drying；The ball milling is high-energy ball milling, and the rotating speed of the high-energy ball milling is 1000r/min, the time of the high-energy ball milling is 2h, and the temperature of the drying is 100 DEG C, and the time of the drying is 4h, institute It is isostatic cool pressing to state compressing, and the pressure of the isostatic cool pressing is 150MPa；
Step 3: the ethanol solution of phenolic resin is placed in pressurized tank, biscuit described in step 2 is then immersed into phenol In the ethanol solution of urea formaldehyde, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 1MPa bar 60min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, is done under conditions of temperature is 80 DEG C Dry 8h；The ethanol solution of the phenolic resin is formed by phenolic resin and absolute ethyl alcohol in mass ratio 1.5: 1 are well mixed；
Step 4: the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after being impregnated in step 3 is immersed In the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 1MPa bar 60min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, under conditions of temperature is 100 DEG C Dry 14h；The aqueous solution of the butyl titanate is formed by butyl titanate and distilled water in mass ratio 4: 1 are well mixed；
Step 5: repeat step three and step 4, untill the constant mass of biscuit, then put the biscuit after dipping In high temperature sintering furnace, in nitrogen atmosphere, temperature obtains resistance tube 1 to sinter 1h under conditions of 1750 DEG C.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is shown in Table 4.
The performance data of the coat of silicon carbide of 4 embodiment of the present invention of table 4 and resistance tube 1
As shown in Table 4, resistance tube 1 have low porosity, bending strength be more than 60MPa, Critical thermal shock temperature difference also greater than 470 DEG C, the requirement of the long-term use in liquation is substantially met, under the operating mode of the maximum safe voltages of 36V, its limit uses work( Rate is more than 20kW, it is adaptable to the heating and thermal insulation demand of molten metal；Coating layer thickness reaches 24 μm, and interface bond strength is higher.
The application method of the present embodiment immersion ceramic resistor inner heating device is：It is exported by adjusting transformer 7 The electric current of safe load, electric current sequentially pass through second electrode 6-2, resistance tube 1, the molten metal 8 in resistance tube 1, in molten bath 9 Molten metal and first electrode 6-1, to transformer 7 constitute safety return circuit, using resistance tube 1 in galvanization self-heating So as to be heated to molten metal 8.
Embodiment 5
The present embodiment immersion ceramic resistor inner heating device is same as Example 1, and it the difference is that only：Carborundum The preparation method of coating and resistance tube 1 is different.Wherein, the preparation method of the coat of silicon carbide is：By being placed in of resistance tube 1 Learn in gaseous phase deposition stove, using CH3SiCl3As raw material, hydrogen is in hydrogen flowing quantity as diluent gas as carrier gas, argon gas 200mL/min, argon flow amount is 150mL/min, and temperature is to deposit 6h under conditions of 1000 DEG C, in the inwall of resistance tube 1 and outer Coat of silicon carbide is obtained on wall.The preparation method of the resistance tube 1 comprises the following steps：
Step 1: weighing each raw material of following mass percent：SiC 66%, graphite 20%, Y2O32%； Al2O31.5%；Ni 3.5%；Mo 3.5%, TiC 3.5%；Each raw material is powder, and graphite is preferably Nano graphite powder；
Step 2: each raw material ball milling weighed in step one is well mixed, basic powder is obtained, then by the basis It is compressing after granulation for powders, biscuit is obtained after drying；The ball milling is high-energy ball milling, and the rotating speed of the high-energy ball milling is 1000r/min, the time of the high-energy ball milling is 4h, and the temperature of the drying is 150 DEG C, and the time of the drying is 8h, institute It is isostatic cool pressing to state compressing, and the pressure of the isostatic cool pressing is 200MPa；
Step 3: the ethanol solution of phenolic resin is placed in pressurized tank, biscuit described in step 2 is then immersed into phenol In the ethanol solution of urea formaldehyde, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 1MPa bar 60min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, under conditions of temperature is 100 DEG C Dry 14h；The ethanol solution of the phenolic resin is formed by phenolic resin and absolute ethyl alcohol in mass ratio 2: 1 are well mixed；
Step 4: the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after being impregnated in step 3 is immersed In the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 2MPa bar 60min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, under conditions of temperature is 100 DEG C Dry 14h；The aqueous solution of the butyl titanate is formed by butyl titanate and distilled water in mass ratio 3: 1 are well mixed；
Step 5: repeat step three and step 4, untill the constant mass of biscuit, then put the biscuit after dipping In high temperature sintering furnace, in nitrogen atmosphere, temperature obtains resistance tube 1 to sinter 4h under conditions of 1650 DEG C.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is shown in Table 5.
The performance data of the coat of silicon carbide of 5 embodiment of the present invention of table 5 and resistance tube 1
As shown in Table 5, resistance tube 1 has low porosity, and bending strength is more than 60MPa, and Critical thermal shock temperature difference is more than 450 DEG C, the requirement of the long-term use in liquation is met, under the operating mode of the maximum safe voltages of 36V, its limit is exceeded using power 20kW, it is adaptable to the heating and thermal insulation demand of molten metal；Coating layer thickness reaches 35 μm, and interface bond strength is higher.
The application method of the present embodiment immersion ceramic resistor inner heating device is：It is exported by adjusting transformer 7 The electric current of safe load, electric current sequentially pass through second electrode 6-2, resistance tube 1, the molten metal 8 in resistance tube 1, in molten bath 9 Molten metal and first electrode 6-1, to transformer 7 constitute safety return circuit, using resistance tube 1 in galvanization self-heating So as to be heated to molten metal 8.
Embodiment 6
The present embodiment immersion ceramic resistor inner heating device is same as Example 1, and it the difference is that only：Carborundum The preparation method of coating and resistance tube 1 is different.Wherein, the preparation method of the coat of silicon carbide is：By being placed in of resistance tube 1 Learn in gaseous phase deposition stove, using CH3SiCl3As raw material, hydrogen is in hydrogen flowing quantity as diluent gas as carrier gas, argon gas 400mL/min, argon flow amount is 100mL/min, and temperature is to deposit 6h under conditions of 1000 DEG C, in the inwall of resistance tube 1 and outer Coat of silicon carbide is obtained on wall.The preparation method of the resistance tube 1 comprises the following steps：
Step 1: weighing each raw material of following mass percent：SiC 45%, graphite 35%, Y2O33%；Al2O32%； Ni 5%；Mo 5%, TiC 5%；Each raw material is powder, and graphite is preferably Nano graphite powder；
Step 2: each raw material ball milling weighed in step one is well mixed, basic powder is obtained, then by the basis It is compressing after granulation for powders, biscuit is obtained after drying；The ball milling is high-energy ball milling, and the rotating speed of the high-energy ball milling is 2000r/min, the time of the high-energy ball milling is 4h, and the temperature of the drying is 150 DEG C, and the time of the drying is 8h, institute It is isostatic cool pressing to state compressing, and the pressure of the isostatic cool pressing is 150MPa；
Step 3: the ethanol solution of phenolic resin is placed in pressurized tank, biscuit described in step 2 is then immersed into phenol In the ethanol solution of urea formaldehyde, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 2MPa bar 60min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, is done under conditions of temperature is 80 DEG C Dry 14h；The ethanol solution of the phenolic resin is formed by phenolic resin and absolute ethyl alcohol in mass ratio 1: 1 are well mixed；
Step 4: the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after being impregnated in step 3 is immersed In the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 2MPa bar 60min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, under conditions of temperature is 100 DEG C Dry 8h；The aqueous solution of the butyl titanate is formed by butyl titanate and distilled water in mass ratio 4: 1 are well mixed；
Step 5: repeat step three and step 4, untill the constant mass of biscuit, then put the biscuit after dipping In high temperature sintering furnace, in nitrogen atmosphere, temperature obtains resistance tube 1 to sinter 4h under conditions of 1750 DEG C.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is shown in Table 6.
The performance data of the coat of silicon carbide of 6 embodiment of the present invention of table 6 and resistance tube 1
As shown in Table 6, resistance tube 1 have low porosity, bending strength be more than 50MPa, Critical thermal shock temperature difference also greater than 500 DEG C, the requirement of the long-term use in liquation is substantially met, under the operating mode of the maximum safe voltages of 36V, its limit uses work( Rate is more than 20kW, it is adaptable to the heating and thermal insulation demand of molten metal；Coating layer thickness reaches 27 μm, and interface bond strength is higher.
The application method of the present embodiment immersion ceramic resistor inner heating device is：It is exported by adjusting transformer 7 The electric current of safe load, electric current sequentially pass through second electrode 6-2, resistance tube 1, the molten metal 8 in resistance tube 1, in molten bath 9 Molten metal and first electrode 6-1, to transformer 7 constitute safety return circuit, using resistance tube 1 in galvanization self-heating So as to be heated to molten metal 8.
Embodiment 7
The present embodiment immersion ceramic resistor inner heating device is same as Example 1, and it the difference is that only：Carborundum The preparation method of coating and resistance tube 1 is different.Wherein, the preparation method of the coat of silicon carbide is：By being placed in of resistance tube 1 Learn in gaseous phase deposition stove, using CH3SiCl3As raw material, hydrogen is in hydrogen flowing quantity as diluent gas as carrier gas, argon gas 400mL/min, argon flow amount is 100mL/min, and temperature is to deposit 6h under conditions of 1200 DEG C, in the inwall of resistance tube 1 and outer Coat of silicon carbide is obtained on wall.The preparation method of the resistance tube 1 comprises the following steps：
Step 1: weighing each raw material of following mass percent：SiC 75%, graphite 15%, Y2O31.5%； Al2O31%；Ni 2.5%；Mo 2.5%, TiC 2.5%；Each raw material is powder, and graphite is preferably Nano graphite powder；
Step 2: each raw material ball milling weighed in step one is well mixed, basic powder is obtained, then by the basis It is compressing after granulation for powders, biscuit is obtained after drying；The ball milling is high-energy ball milling, and the rotating speed of the high-energy ball milling is 2000r/min, the time of the high-energy ball milling is 4h, and the temperature of the drying is 100 DEG C, and the time of the drying is 8h, institute It is isostatic cool pressing to state compressing, and the pressure of the isostatic cool pressing is 200MPa；
Step 3: the ethanol solution of phenolic resin is placed in pressurized tank, biscuit described in step 2 is then immersed into phenol In the ethanol solution of urea formaldehyde, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 1MPa bar 60min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, under conditions of temperature is 100 DEG C Dry 8h；The ethanol solution of the phenolic resin is formed by phenolic resin and absolute ethyl alcohol in mass ratio 1: 1 are well mixed；
Step 4: the aqueous solution of butyl titanate is placed in pressurized tank, then the biscuit after being impregnated in step 3 is immersed In the aqueous solution of butyl titanate, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank be 2MPa bar 20min is impregnated to biscuit under part, then the biscuit after dipping is placed in vacuum drying chamber, under conditions of temperature is 100 DEG C Dry 8h；The aqueous solution of the butyl titanate is formed by butyl titanate and distilled water in mass ratio 2: 1 are well mixed；
Step 5: repeat step three and step 4, untill the constant mass of biscuit, then put the biscuit after dipping In high temperature sintering furnace, in nitrogen atmosphere, temperature obtains resistance tube 1 to sinter 4h under conditions of 1650 DEG C.
The performance data of the present embodiment coat of silicon carbide and resistance tube 1 is shown in Table 7.
The performance data of the coat of silicon carbide of 7 embodiment of the present invention of table 7 and resistance tube 1
As shown in Table 7, resistance tube 1 have low porosity, bending strength be more than 70MPa, Critical thermal shock temperature difference also greater than 450 DEG C, the requirement of the long-term use in liquation is met, under the operating mode of the maximum safe voltages of 36V, its limit is super using power Cross 20kW, it is adaptable to the heating and thermal insulation demand of molten metal；Coating layer thickness reaches 34 μm, and interface bond strength is high.
The application method of the present embodiment immersion ceramic resistor inner heating device is：It is exported by adjusting transformer 7 The electric current of safe load, electric current sequentially pass through second electrode 6-2, resistance tube 1, the molten metal 8 in resistance tube 1, in molten bath 9 Molten metal and first electrode 6-1, to transformer 7 constitute safety return circuit, using resistance tube 1 in galvanization self-heating So as to be heated to molten metal 8.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions.It is every according to invention skill Any simple modification, change and equivalence change that art is substantially made to above example, still fall within technical solution of the present invention Protection domain in.

Claims (8)

1. a kind of immersion ceramic resistor inner heating device, it is characterised in that including transformer (7) and molten bath (9), the molten bath (9) resistance tube (1) and first electrode (6-1), the upper end open lower end closed of the resistance tube (1), the molten bath are inserted with (9) and in resistance tube (1) it is loaded with molten metal (8), is inserted with second electrode (6-2) in the resistance tube (1), described the The bottom of one electrode (6-1) and second electrode (6-2) is immersed in molten metal (8), the first electrode (6-1) and second The top of electrode (6-2) is connected by wire with transformer (7), and the material of the resistance tube (1) is carbide composite ceramic, Deposition has coat of silicon carbide on the inner and outer wall of resistance tube (1)；
The preparation method of the resistance tube (1) comprises the following steps：
Step 1: weighing each raw material of following mass percent：SiC 45%~75%, graphite 15%~35%, Y2O31.5% ~3%；Al2O31%~2%；Ni 2.5%~5%；Mo 2.5%~5%, TiC 2.5%~5%；
Step 2: each raw material ball milling weighed in step one is well mixed, basic powder is obtained, then by the basic powder It is compressing after granulation, biscuit is obtained after drying；
Step 3: the ethanol solution of phenolic resin is placed in pressurized tank, biscuit described in step 2 is then immersed into phenolic aldehyde tree In the ethanol solution of fat, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank is 1MPa~2MPa Under the conditions of to biscuit impregnate 20min~60min, then the biscuit after dipping is placed in vacuum drying chamber, temperature be 80 DEG C 8h~14h is dried under conditions of~100 DEG C；The ethanol solution of the phenolic resin by phenolic resin and absolute ethyl alcohol in mass ratio (1~2): 1 well mixed forms；
Step 4: the aqueous solution of butyl titanate is placed in pressurized tank, the biscuit after being impregnated in step 3 is then immersed into metatitanic acid In the aqueous solution of butyl ester, backward pressurized tank in be filled with compressed air, the gas pressure in pressurized tank is 1MPa~2MPa Under the conditions of to biscuit impregnate 20min~60min, then the biscuit after dipping is placed in vacuum drying chamber, temperature be 80 DEG C 8h~14h is dried under conditions of~100 DEG C；The aqueous solution of the butyl titanate by butyl titanate and distilled water in mass ratio (2~ 4): 1 well mixed forms；
Step 5: repeat step three and step 4, untill the constant mass of biscuit, are then placed in height by the biscuit after dipping In warm sintering furnace, in nitrogen atmosphere, temperature is sintering 1h~4h under conditions of 1650 DEG C~1750 DEG C, obtains resistance tube (1).
2. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterised in that the resistance tube (1) it is provided with insulation cover plate (3), the insulation cover plate (3) and is provided with for being passed through protection gas into resistance tube (1) at the top of The breather pipe (4) of body.
3. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterised in that the molten metal (8) it is any one in Zn liquations, Al liquations, Mg liquations and Sn liquations or two or more.
4. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterised in that the first electrode (6-1) and second electrode (6-2) are graphite electrode.
5. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterised in that the transformer (7) it is adjustable variable-pressure device, the adjustable range of the output voltage of the adjustable variable-pressure device is 0V~36V.
6. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterised in that the molten bath (9) Inside it is inserted with the first thermocouple (5-1), the resistance tube (1) and is inserted with the second thermocouple (5-2), first thermocouple The thermometric end of (5-1) and the second thermocouple (5-2) is immersed in molten metal (8), first thermocouple (5-1) and second Thermocouple (5-2) is set with protection pipe outside, and the material of the protection pipe is Si3N4, AlN or Sialon ceramics.
7. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterised in that described in step 2 Ball milling is high-energy ball milling, and the rotating speed of the high-energy ball milling is 1000r/min~2000r/min, and the time of the high-energy ball milling is 2h~4h, the temperature of the drying is 100 DEG C~150 DEG C, and the time of the drying is 4h~8h, described compressing to be cold etc. Static pressure, the pressure of the isostatic cool pressing is 150MPa~200MPa.
8. a kind of immersion ceramic resistor inner heating device according to claim 1, it is characterised in that the carborundum is applied Layer preparation method be：Resistance tube (1) is placed in chemical vapor deposition stove, using CH3SiCl3As raw material, hydrogen is used as load Gas, argon gas is 200mL/min~400mL/min in hydrogen flowing quantity as diluent gas, argon flow amount be 100mL/min~ 150mL/min, temperature is deposition 2h~6h under conditions of 1000 DEG C~1200 DEG C, on the inner and outer wall of resistance tube (1) Obtain coat of silicon carbide.
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