CN106116578A - Titanium alloy melts casting electric smelting yttrium oxide ceramic crucible and preparation method thereof - Google Patents
Titanium alloy melts casting electric smelting yttrium oxide ceramic crucible and preparation method thereof Download PDFInfo
- Publication number
- CN106116578A CN106116578A CN201610593898.7A CN201610593898A CN106116578A CN 106116578 A CN106116578 A CN 106116578A CN 201610593898 A CN201610593898 A CN 201610593898A CN 106116578 A CN106116578 A CN 106116578A
- Authority
- CN
- China
- Prior art keywords
- titanium alloy
- crucible
- yttrium oxide
- granule
- electric smelting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
- C04B35/505—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds based on yttrium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/653—Processes involving a melting step
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3241—Chromium oxides, chromates, or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to oxide ceramics application, particularly relate to a kind of melt the titanium alloy of casting for titanium alloy and melt casting electric smelting yttrium oxide ceramic crucible and preparation method thereof, percentages with oxide weight, adding up to 100%, it has following chemical composition: Y2O3:70% 99.5%；Zro2:30% 0.5%；It is not more than other trace impurity of 0.5%, other trace impurity is oxide, by high-frequency heating fusion crust method, high-purity crystallized body raw material is prepared in yttrium oxide molten mass magnetic agitation melting, broken and the granularity of yittrium oxide crystalline solid is equipped with and molding, the steps such as the sintering of yttrium crucible, it has and is not adhered, do not infiltrate, the characteristics such as good thermal shock resistance properties and the service life of superelevation, safe handling temperature less than 2300 degree, effectively avoid that crucible life that chemical reaction that is big with titanium alloy metallic solution at high temperature activity and that cause causes is low and reacted peeling and the lower degradation problem of titanium alloy degree of purity that causes.
Description
Technical field
The present invention relates to oxide ceramics application, particularly relate to a kind of for titanium alloy melt casting titanium alloy melt
Melt casting electric smelting yttrium oxide ceramic crucible and preparation method thereof.
Background technology
Titanium alloy is a kind of important structural metal grown up the 1950's, titanium alloy because of have intensity high,
Good corrosion resistance, thermostability high and be widely used in every field.Many countries all recognize titanium alloy material in the world
The importance of material, in succession researchs and develops it, and is applied, and mainly develops the high temperature of aero-engine
Titanium alloy and the structural titanium alloy of body, since the eighties, corrosion resistant Ti alloy and high-strength titanium alloy are further developed, main
It is used for making aircraft engine pressure steam turbine parts, is secondly the structural member of rocket, guided missile and high-speed aircraft, many states in the world
Family all recognizes the importance of titanium alloy material, in succession researchs and develops it, and is applied.
But titanium or titanium alloy major limitation is poor in the chemical reactivity of high temperature Yu other material, titanium or titanium alloy is a kind of
High chemically active metal, in the molten state, almost can be with all conventional material generation chemical reactions generate fragility chemical combination
Thing, thus cause titanium alloy metallic surface of poor quality and mechanical properties decrease, see to a certain extent, titanium alloy metal quality
The development that promotes seek the evolution of process material of high chemical stability exactly, this character forces titanium alloy and general tradition
Refine, melted different with foundry engieering, even often result in the decline of titanium alloy quality as a result, make high-quality high-purity titanium
It is sufficiently expensive that the price of alloy becomes.Therefore they have just started mostly to be used in aircaft configuration, airborne vehicle, and are used in oil and change
Learn the high-technology industries such as industry.But due to the prosperity of space science and technology, the lifting of people's living standard, so titanium alloy is the most gradually
Ground is used for making people's livelihood articles for use, the life brought benefit to the people, and simply these product prices are the most higher, belong to higher-priced product more
Product, this is the maximum mortal wound that titanium alloy cannot be developed, and is the most effectively reduced by the titanium alloy of high-purity high-quality
Production cost, the performance boost of institute's contact material and the use of applicable new material during titanium alloy smelting to be depended on,
The cost of titanium alloy smelting and casting is greatly decreased with this.
Summary of the invention
It is an object of the invention to overcome deficiency of the prior art, and provide a kind of titanium alloy to melt casting electric smelting three
Y 2 O ceramic crucible and preparation method thereof, this high pure oxide ceramic crucible compared with zirconium oxide/calcium oxide/magnesium oxide
The contact of titanium alloy motlten metal has be not adhered, do not infiltrate, the characteristic such as service life of good thermal shock resistance properties and superelevation,
Safe handling temperature less than 2300 degree, effectively avoids chemistry that is big with titanium alloy metallic solution at high temperature activity and that cause
The crucible life that causes of reaction is low and reacted peeling and the lower degradation problem of titanium alloy degree of purity that causes.
The technical solution adopted in the present invention:
A kind of titanium alloy melts casting electric smelting yttrium oxide ceramic crucible, with the percentages of oxide weight, adds up to
100%, it has a following chemical composition:
Y2O3:70%-99.5%；
Zro2:30%-0.5%；
Being not more than other trace impurity of 0.5%, other trace impurity is oxide.
Other trace impurity described is oxide, including Fe2O3、Cr2O3、TiO2、CaO、K2O、SiO2、Al2O3、MgO、
Na2O。
A kind of above-mentioned titanium alloy melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, including following step
Rapid:
A, by high-frequency heating fusion crust method, high-purity crystallized body raw material is prepared in yttrium oxide molten mass magnetic agitation melting
It is the yttrium oxide of 99.999% by material purity, at a temperature of 2500 DEG C-2800 DEG C, carries out melting, use water-cooled
Copper-cold crucible crystallization electromagnetic induction heating mode；Yttrium oxide raw material loads in cold crucible, can also be uniformly blended into oxygen simultaneously
Change zirconium, put into metal zirconium sheet or cubic crystal zirconium powder at cold crucible center, switch on power, carry out high-frequency heating；Treat central area
The metal zirconium sheet thrown in or cubic crystal zirconium powder start thermal source diffusion, and raw material starts to melt, and is now passed through cold water in copper tube and follows
Ring cools down, and takes away heat, makes outer layer powder not melt, and forms cold crucible fusion crust, and in treating cold crucible, raw material 75-83% zone melt reaches
During to molten condition, the magnetic agitation effect that high-frequency induction is had starts to play a role, and makes melt solution present uniformly fusion
State, also makes solution obtain the consistent degree of superheat simultaneously, after melt is maintained molten condition 60-120 minute, stops merit
Rate, stops heating, and allows molten mass Temperature fall, along with melt temperature declines, starts gradually because cooling produces supersaturation concentration
Solidification is to lenticular, after melt crystallization is cooled to room temperature, takes out yittrium oxide crystalline solid.
B, the broken and granularity of yittrium oxide crystalline solid are equipped with and molding
The yittrium oxide monocrystalline block crossed through electromagnetic induction melting obtained in step a carrying out broken and granularity be equipped with, preparing should
For product molding；To crush in solid solution that is rear and that be equipped with granularity is placed in rustless steel V-type batch mixer or three-dimensional material mixer
Row is blended, and the time being blended is not less than 4 hours, after granule to be combined and powder are sufficiently mixed uniformly, is placed on rustless steel
In blender, and adding vinyl alcohol water-soluble binding agents, be stirred, mixing time is not less than 2 hours, treats water-soluble binding agents
After being thoroughly mixed uniformly with raw material, drying in being placed on drying baker, the hard being placed on molding after drying closes
In gold mold cavity, extrusion forming, obtain required shape and sized products green compact；Obtained product green compact are placed in high temperature
Dry in drying baker, after drying, be naturally cooling to room temperature；
C, the sintering of yttrium crucible
Product green compact use computer programming to control sintering process and are sintered:
Sintering, uses the closed kiln of electrical heating to be sintered green compact, after having sintered, makes kiln be naturally cooling to room temperature,
Then take out yttrium crucible.
Further, in described a step, the yttrium oxide D50 granularity that feeds intake is 1um-3um.
Further, the operating frequency of the high-frequency induction generator described in described a step is 800 kHz～1 MHz,
Power is at 500 kW.
Further, the broken and granularity described in step b is equipped with, and concrete broken yittrium oxide electric smelting crystal size is 325
Mesh, 100 mesh, φ 0-0.5mm granule, φ 0.5-1mm granule, φ 1-2mm granule, φ 2-3mm granule, totally 6 ranks；After Po Sui
Grain size proportion be: 325 mesh account for the 28-33% of gross mass, and 100 mesh account for the 17-22% of gross mass, φ 0-0.5mm granule and account for total matter
9-11%, the φ 0.5-1mm granule of amount accounts for 8-11%, the φ 1-2mm granule of gross mass and accounts for the 19-23%, φ 2-3mm of gross mass
Grain accounts for the 8-12% of gross mass.
Further, the amount adding vinyl alcohol water-soluble binding agents in described step b is the yittrium oxide gross mass after crushing
5%-6%。
Further, drying in raw material is released in described step b drying baker, drying temperature is 30 DEG C-80 DEG C, dries
Time is 8-12 hour, raw aqueous weight ＜ 2% after drying.
Further, dry in product green compact are placed in high temperature drying baker by described step b, dry curve be 0 DEG C-
200 DEG C even all heats up 6 hours, then keeps 200 DEG C of constant temperature 8-12 hour.
Further, in described step c, sintering temperature is 1750 ± 3 DEG C, and sintering temperature curve is from the beginning of 0 DEG C, with per hour
The uniform programming rate of 30 DEG C rises to 1750 DEG C；After reaching 1750 DEG C, constant temperature closes heating power after maintaining 18-24 hour.
Beneficial effects of the present invention:
The present invention high-purity yttrium oxide material is through clean electric smelting PROCESS FOR TREATMENT, and for single crystalline phase, high temperature does not has activity, purity
High, use the higher lifting of degree of purity to titanium alloy compared with other oxide materials, safe handling temperature 2300 degree with
Lower higher with the smelting temperature of titanium alloy metallic solution, it is to avoid titanium alloy Metal Materials At High Temperature chemical reaction causes adhesion and invades profit
Etc. problem, it it is 3-5 times of the life-span that other oxide materials use；To the stability of titanium alloy metallic solution and degree of purity significantly
Promoting, be significantly increased service life, use cost declines to a great extent, and will replace the use of other oxide materials comprehensively.
Detailed description of the invention
Embodiment 1
A kind of titanium alloy melts casting electric smelting yttrium oxide ceramic crucible, with the percentages of oxide weight, adds up to
100%, it is by following chemical composition: the Y2O3 of 98%, be not more than 0.5% other trace impurity, remaining be Zro2, other trace
Impurity is oxide, including Fe2O3、Cr2O3、TiO2、CaO、K2O、SiO2、Al2O3、MgO、Na2O。
A kind of above-mentioned titanium alloy melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, including following step
Rapid:
A, by high-frequency heating fusion crust method, high-purity crystallized body raw material is prepared in yttrium oxide molten mass magnetic agitation melting
It is the yttrium oxide of 99.999% by material purity, at a temperature of 2500 DEG C-2800 DEG C, carries out melting, use water-cooled
Copper-cold crucible crystallization electromagnetic induction heating mode；It is 99.999% by purity, three oxidations two that D50 feeds intake that granularity is 1um-3um
Yttrium raw material loads in cold crucible, and cold crucible selects the diameter cold crucible (in the cup-shaped bucket that copper tube surrounds) more than 1000 mm,
Yttrium oxide charge is 500kg, is uniformly blended into zirconium oxide 8kg simultaneously, cold crucible center put into 4-6g metal zirconium sheet or
1kg cubic crystal zirconium powder is used for drawing heat, switches on power, and carries out high-frequency heating, and the operating frequency of high-frequency induction generator is 800
KHz～1 MHz, power is at 500 kW；Treating that the thermit powder that draws that central area is thrown in starts thermal source diffusion, raw material starts to melt, this
Time copper tube in be passed through circulating chilled water cooling, take away heat, make outer layer powder not melt, formed cold crucible fusion crust, in treating cold crucible
When raw material 75-83% zone melt reaches molten condition, the magnetic agitation effect that high-frequency induction is had starts to play a role, and makes
Melt solution presents uniform Fusion Strain, also makes solution obtain the consistent degree of superheat simultaneously；Melt is maintained molten condition
After 60-120 minute, stop power, stop heating, allow molten mass Temperature fall, along with melt temperature declines, because cooling produced
Saturated concentration and start gradually to solidify to lenticular, after melt crystallization is cooled to room temperature, take out pure yittrium oxide crystalline solid
Product；
Do not bring incorporating of other materials during this into, be effectively guaranteed purity and the cleanliness factor of yittrium oxide crystal, and adopt
With magnetic force, solution is stirred, is not only able to enable solution the most even, also make the yittrium oxide after cooling for completely
Monocrystalline block.
B, the broken and granularity of yittrium oxide crystalline solid are equipped with and molding
The yittrium oxide monocrystalline block crossed through electromagnetic induction melting obtained in step a carrying out broken and granularity be equipped with, preparing should
For product molding；Concrete broken yittrium oxide electric smelting crystal size is 325 mesh, 100 mesh, φ 0-0.5mm granule, φ 0.5-
1mm granule, φ 1-2mm granule, φ 2-3mm granule, totally 6 ranks；Grain size proportion after Po Sui is: 325 mesh account for gross mass
28-33%, 100 mesh account for the 17-22% of gross mass, φ 0-0.5mm granule and account for 9-11%, the φ 0.5-1mm granule of gross mass and account for total matter
8-11%, the φ 1-2mm granule of amount accounts for 19-23%, the φ 2-3mm granule of gross mass and accounts for the 8-12% of gross mass；To be equipped with after crushing
The solid solution of good granularity is placed in rustless steel V-type batch mixer or three-dimensional material mixer is blended, and the time being blended is not less than 4 hours,
After granule and powder are sufficiently mixed uniformly, more mixed granule and powder are placed in rustless steel blender, and add second
Enol water-soluble binding agents, adds the 5%-6% that amount is the yittrium oxide gross mass after crushing of vinyl alcohol water-soluble binding agents, then
Being sufficiently stirred for, the time of stirring is not less than 2 hours, after water-soluble binding agents and raw material are sufficiently mixed uniformly, by raw material
Drying in being placed in drying baker, drying temperature is 30 DEG C-80 DEG C, and drying time is 8-12 hour, the raw aqueous after drying
Weight ＜ 2%, is placed in raw material the sintered-carbide die intracavity of molding, extrusion forming, obtains required shape and chi after drying
Very little product green compact；Drying in obtained product green compact are placed in high temperature drying baker, drying temperature curve is 0 DEG C-200 DEG C
Even all intensifications 6 hours, then keep 200 DEG C of constant temperature 4-8 hour, then green compact are naturally cooling to room temperature；
C, the sintering of yttrium crucible
Product green compact use computer programming to control sintering process and are sintered:
Sintering, uses the closed kiln of electrical heating to be sintered green compact, and sintering temperature 1750 ± 3 DEG C, sintering temperature curve is from 0
DEG C start, be warming up to 1750 DEG C with the uniform programming rate of per hour 30 DEG C；After reaching 1750 DEG C, constant temperature maintains 18-24 hour
Rear closedown heating power, makes kiln take out yttrium crucible after being naturally cooling to room temperature.
Crucible prepared in this embodiment actual heated after reach 98% ratio, phase due to its component Y2O3 when using
Based on the life-span using uninterrupted molten titanium alloy, the ceramic crucible that this component proportion obtains is difficult to and titanium alloy solution most
Sticking together and invade profit, within cooling of the most repeatedly heating uses 12 hours, crucible will not stick together with titanium alloy solution, even
Continuous cooling of repeatedly heating uses more than 12 hours, and crucible material just would tend to occur catabiosis and is susceptible to bulk material stripping
Fall to being mixed in titanium alloy solution.
Embodiment 2
A kind of titanium alloy melts casting electric smelting yttrium oxide ceramic crucible, with the percentages of oxide weight, adds up to
100%, it is by following chemical composition: the Y2O3 of 95%, be not more than 0.5% other trace impurity, remaining be Zro2, other trace
Impurity is oxide, including Fe2O3、Cr2O3、TiO2、CaO、K2O、SiO2、Al2O3、MgO、Na2O。
A kind of above-mentioned titanium alloy melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, including following step
Rapid:
A, by high-frequency heating fusion crust method, high-purity crystallized body raw material is prepared in yttrium oxide molten mass magnetic agitation melting
It is the yttrium oxide of 99.999% by material purity, at a temperature of 2500 DEG C-2800 DEG C, carries out melting, use water-cooled
Copper-cold crucible crystallization electromagnetic induction heating mode；It is 99.999% by purity, three oxidations two that D50 feeds intake that granularity is 1um-3um
Yttrium raw material loads in cold crucible, and cold crucible selects the diameter cold crucible (in the cup-shaped bucket that copper tube surrounds) more than 1000 mm,
Yttrium oxide charge is 500kg, is uniformly blended into zirconium oxide 24kg simultaneously, cold crucible center put into 4-6g metal zirconium sheet or
1kg cubic crystal zirconium powder is used for drawing heat, switches on power, and carries out high-frequency heating, and the operating frequency of high-frequency induction generator is 800
KHz～1 MHz, power is at 500 kW；Treating that the thermit powder that draws that central area is thrown in starts thermal source diffusion, raw material starts to melt, this
Time copper tube in be passed through circulating chilled water cooling, take away heat, make outer layer powder not melt, formed cold crucible fusion crust, in treating cold crucible
When raw material 75-83% zone melt reaches molten condition, the magnetic agitation effect that high-frequency induction is had starts to play a role, and makes
Melt solution presents uniform Fusion Strain, also makes solution obtain the consistent degree of superheat simultaneously；Melt is maintained molten condition
After 60-120 minute, stop power, stop heating, allow molten mass Temperature fall, along with melt temperature declines, because cooling produced
Saturated concentration and start gradually to solidify to lenticular, after melt crystallization is cooled to room temperature, take out pure yittrium oxide crystalline solid
Product；
Do not bring incorporating of other materials during this into, be effectively guaranteed purity and the cleanliness factor of yittrium oxide crystal, and adopt
With magnetic force, solution is stirred, is not only able to enable solution the most even, also make the yittrium oxide after cooling for completely
Monocrystalline block.
B, the broken and granularity of yittrium oxide crystalline solid are equipped with and molding
The yittrium oxide monocrystalline block crossed through electromagnetic induction melting obtained in step a carrying out broken and granularity be equipped with, preparing should
For product molding；Concrete broken yittrium oxide electric smelting crystal size is 325 mesh, 100 mesh, φ 0-0.5mm granule, φ 0.5-
1mm granule, φ 1-2mm granule, φ 2-3mm granule, totally 6 ranks；Grain size proportion after Po Sui is: 325 mesh account for gross mass
28-33%, 100 mesh account for the 17-22% of gross mass, φ 0-0.5mm granule and account for 9-11%, the φ 0.5-1mm granule of gross mass and account for total matter
8-11%, the φ 1-2mm granule of amount accounts for 19-23%, the φ 2-3mm granule of gross mass and accounts for the 8-12% of gross mass；To be equipped with after crushing
The solid solution of good granularity is placed in rustless steel V-type batch mixer or three-dimensional material mixer is blended, and the time being blended is not less than 4 hours,
After granule and powder are sufficiently mixed uniformly, more mixed granule and powder are placed in rustless steel blender, and add second
Enol water-soluble binding agents, adds the 5%-6% that amount is the yittrium oxide gross mass after crushing of vinyl alcohol water-soluble binding agents, then
Being sufficiently stirred for, the time of stirring is not less than 2 hours, after water-soluble binding agents and raw material are sufficiently mixed uniformly, by raw material
Drying in being placed in drying baker, drying temperature is 30 DEG C-80 DEG C, and drying time is 8-12 hour, the raw aqueous after drying
Weight ＜ 2%, is placed in raw material the sintered-carbide die intracavity of molding, extrusion forming, obtains required shape and chi after drying
Very little product green compact；Drying in obtained product green compact are placed in high temperature drying baker, drying temperature curve is 0 DEG C-200 DEG C
Even all intensifications 6 hours, then keep 200 DEG C of constant temperature 4-8 hour, then green compact are naturally cooling to room temperature；
C, the sintering of yttrium crucible
Product green compact use computer programming to control sintering process and are sintered:
Sintering, uses the closed kiln of electrical heating to be sintered green compact, and sintering temperature 1750 ± 3 DEG C, sintering temperature curve is from 0
DEG C start, be warming up to 1750 DEG C with the uniform programming rate of per hour 30 DEG C；After reaching 1750 DEG C, constant temperature maintains 18-24 hour
Rear closedown heating power, makes kiln take out yttrium crucible after being naturally cooling to room temperature.
The crucible prepared in this embodiment actual heated after reach 95% ratio, phase due to its component Y2O3 when using
Based on the life-span using uninterrupted molten titanium alloy, the ratio that the ceramic crucible that this component proportion obtains exists because of zirconium oxide
Titanium alloy solution adhesion occurring and invades time of profit and be about 7-8 hour, i.e. in the present embodiment, crucible is adding temperature drop continuously repeatedly
Temperature uses more than 7-8 hour, and crucible material the most easily occurs that catabiosis is susceptible to bulk material peeling and is mixed into titanium alloy
In solution, using 7-8 hour in cooling of the most repeatedly heating continuously, will not there is the phenomenon of adhesion with titanium alloy solution in crucible.
Embodiment 3
A kind of titanium alloy melts casting electric smelting yttrium oxide ceramic crucible, with the percentages of oxide weight, adds up to
100%, it is by following chemical composition: the Y2O3 of 90%, be not more than 0.5% other trace impurity, remaining be Zro2, other trace
Impurity is oxide, including Fe2O3、Cr2O3、TiO2、CaO、K2O、SiO2、Al2O3、MgO、Na2O。
A kind of above-mentioned titanium alloy melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, including following step
Rapid:
A, by high-frequency heating fusion crust method, high-purity crystallized body raw material is prepared in yttrium oxide molten mass magnetic agitation melting
It is the yttrium oxide of 99.999% by material purity, at a temperature of 2500 DEG C-2800 DEG C, carries out melting, use water-cooled
Copper-cold crucible crystallization electromagnetic induction heating mode；It is 99.999% by purity, three oxidations two that D50 feeds intake that granularity is 1um-3um
Yttrium raw material loads in cold crucible, and cold crucible selects the diameter cold crucible (in the cup-shaped bucket that copper tube surrounds) more than 1000 mm,
Yttrium oxide charge is 500kg, is uniformly blended into zirconium oxide 54kg simultaneously, cold crucible center put into 4-6g metal zirconium sheet or
1kg cubic crystal zirconium powder is used for drawing heat, switches on power, and carries out high-frequency heating, and the operating frequency of high-frequency induction generator is 800
KHz～1 MHz, power is at 500 kW；Treating that the thermit powder that draws that central area is thrown in starts thermal source diffusion, raw material starts to melt, this
Time copper tube in be passed through circulating chilled water cooling, take away heat, make outer layer powder not melt, formed cold crucible fusion crust, in treating cold crucible
When raw material 75-83% zone melt reaches molten condition, the magnetic agitation effect that high-frequency induction is had starts to play a role, and makes
Melt solution presents uniform Fusion Strain, also makes solution obtain the consistent degree of superheat simultaneously；Melt is maintained molten condition
After 60-120 minute, stop power, stop heating, allow molten mass Temperature fall, along with melt temperature declines, because cooling produced
Saturated concentration and start gradually to solidify to lenticular, after melt crystallization is cooled to room temperature, take out pure yittrium oxide crystalline solid
Product；
Do not bring incorporating of other materials during this into, be effectively guaranteed purity and the cleanliness factor of yittrium oxide crystal, and adopt
With magnetic force, solution is stirred, is not only able to enable solution the most even, also make the yittrium oxide after cooling for completely
Monocrystalline block.
B, the broken and granularity of yittrium oxide crystalline solid are equipped with and molding
The yittrium oxide monocrystalline block crossed through electromagnetic induction melting obtained in step a carrying out broken and granularity be equipped with, preparing should
For product molding；Concrete broken yittrium oxide electric smelting crystal size is 325 mesh, 100 mesh, φ 0-0.5mm granule, φ 0.5-
1mm granule, φ 1-2mm granule, φ 2-3mm granule, totally 6 ranks；Grain size proportion after Po Sui is: 325 mesh account for gross mass
28-33%, 100 mesh account for the 17-22% of gross mass, φ 0-0.5mm granule and account for 9-11%, the φ 0.5-1mm granule of gross mass and account for total matter
8-11%, the φ 1-2mm granule of amount accounts for 19-23%, the φ 2-3mm granule of gross mass and accounts for the 8-12% of gross mass；To be equipped with after crushing
The solid solution of good granularity is placed in rustless steel V-type batch mixer or three-dimensional material mixer is blended, and the time being blended is not less than 4 hours,
After granule and powder are sufficiently mixed uniformly, more mixed granule and powder are placed in rustless steel blender, and add second
Enol water-soluble binding agents, adds the 5%-6% that amount is the yittrium oxide gross mass after crushing of vinyl alcohol water-soluble binding agents, then
Being sufficiently stirred for, the time of stirring is not less than 2 hours, after water-soluble binding agents and raw material are sufficiently mixed uniformly, by raw material
Drying in being placed in drying baker, drying temperature is 30 DEG C-80 DEG C, and drying time is 8-12 hour, the raw aqueous after drying
Weight ＜ 2%, is placed in raw material the sintered-carbide die intracavity of molding, extrusion forming, obtains required shape and chi after drying
Very little product green compact；Drying in obtained product green compact are placed in high temperature drying baker, drying temperature curve is 0 DEG C-200 DEG C
Even all intensifications 6 hours, then keep 200 DEG C of constant temperature 4-8 hour, then green compact are naturally cooling to room temperature；
C, the sintering of yttrium crucible
Product green compact use computer programming to control sintering process and are sintered:
Sintering, uses the closed kiln of electrical heating to be sintered green compact, and sintering temperature 1750 ± 3 DEG C, sintering temperature curve is from 0
DEG C start, be warming up to 1750 DEG C with the uniform programming rate of per hour 30 DEG C；After reaching 1750 DEG C, constant temperature maintains 18-24 hour
Rear closedown heating power, makes kiln take out yttrium crucible after being naturally cooling to room temperature.
The crucible prepared in this embodiment actual heated after reach 90% ratio, phase due to its component Y2O3 when using
Based on the life-span using uninterrupted molten titanium alloy, the ratio that the ceramic crucible that this component proportion obtains exists because of zirconium oxide
Titanium alloy solution adhesion occurring and invades time of profit and be about 6-7 hour, i.e. in the present embodiment, crucible is adding temperature drop continuously repeatedly
Temperature uses more than 6-7 hour, and crucible material the most easily occurs that catabiosis is susceptible to bulk material peeling and is mixed into titanium alloy
In solution, using 6-7 hour in cooling of the most repeatedly heating continuously, will not there is the phenomenon of adhesion with titanium alloy solution in crucible.
Embodiment 4
A kind of titanium alloy melts casting electric smelting yttrium oxide ceramic crucible, with the percentages of oxide weight, adds up to
100%, it is by following chemical composition: the Y2O3 of 80%, be not more than 0.5% other trace impurity, remaining be Zro2, other trace
Impurity is oxide, including Fe2O3、Cr2O3、TiO2、CaO、K2O、SiO2、Al2O3、MgO、Na2O。
A kind of above-mentioned titanium alloy melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, including following step
Rapid:
A, by high-frequency heating fusion crust method, high-purity crystallized body raw material is prepared in yttrium oxide molten mass magnetic agitation melting
It is the yttrium oxide of 99.999% by material purity, at a temperature of 2500 DEG C-2800 DEG C, carries out melting, use water-cooled
Copper-cold crucible crystallization electromagnetic induction heating mode；It is 99.999% by purity, three oxidations two that D50 feeds intake that granularity is 1um-3um
Yttrium raw material loads in cold crucible, and cold crucible selects the diameter cold crucible (in the cup-shaped bucket that copper tube surrounds) more than 1000 mm,
Yttrium oxide charge is 500kg, is uniformly blended into zirconium oxide 123kg simultaneously, puts into 4-6g metal zirconium sheet at cold crucible center
Or 1kg cubic crystal zirconium powder is used for drawing heat, switching on power, carry out high-frequency heating, the operating frequency of high-frequency induction generator is
800 kHz～1 MHz, power is at 500 kW；Treating that the thermit powder that draws that central area is thrown in starts thermal source diffusion, raw material starts to melt
Change, copper tube is now passed through circulating chilled water cooling, takes away heat, make outer layer powder not melt, form cold crucible fusion crust, treat cold earthenware
When in crucible, raw material 75-83% zone melt reaches molten condition, the magnetic agitation effect that high-frequency induction is had starts to play and makees
With, make melt solution present uniform Fusion Strain, also make solution obtain the consistent degree of superheat simultaneously；Melt is maintained melted
After state 60-120 minute, stop power, stop heating, allow molten mass Temperature fall, along with melt temperature declines, because cooling is produced
Give birth to supersaturation concentration and start gradually to solidify to lenticular, after melt crystallization is cooled to room temperature, take out pure yittrium oxide knot
Crystal product；
Do not bring incorporating of other materials during this into, be effectively guaranteed purity and the cleanliness factor of yittrium oxide crystal, and adopt
With magnetic force, solution is stirred, is not only able to enable solution the most even, also make the yittrium oxide after cooling for completely
Monocrystalline block.
B, the broken and granularity of yittrium oxide crystalline solid are equipped with and molding
The yittrium oxide monocrystalline block crossed through electromagnetic induction melting obtained in step a carrying out broken and granularity be equipped with, preparing should
For product molding；Concrete broken yittrium oxide electric smelting crystal size is 325 mesh, 100 mesh, φ 0-0.5mm granule, φ 0.5-
1mm granule, φ 1-2mm granule, φ 2-3mm granule, totally 6 ranks；Grain size proportion after Po Sui is: 325 mesh account for gross mass
28-33%, 100 mesh account for the 17-22% of gross mass, φ 0-0.5mm granule and account for 9-11%, the φ 0.5-1mm granule of gross mass and account for total matter
8-11%, the φ 1-2mm granule of amount accounts for 19-23%, the φ 2-3mm granule of gross mass and accounts for the 8-12% of gross mass；To be equipped with after crushing
The solid solution of good granularity is placed in rustless steel V-type batch mixer or three-dimensional material mixer is blended, and the time being blended is not less than 4 hours,
After granule and powder are sufficiently mixed uniformly, more mixed granule and powder are placed in rustless steel blender, and add second
Enol water-soluble binding agents, adds the 5%-6% that amount is the yittrium oxide gross mass after crushing of vinyl alcohol water-soluble binding agents, then
Being sufficiently stirred for, the time of stirring is not less than 2 hours, after water-soluble binding agents and raw material are sufficiently mixed uniformly, by raw material
Drying in being placed in drying baker, drying temperature is 30 DEG C-80 DEG C, and drying time is 8-12 hour, the raw aqueous after drying
Weight ＜ 2%, is placed in raw material the sintered-carbide die intracavity of molding, extrusion forming, obtains required shape and chi after drying
Very little product green compact；Drying in obtained product green compact are placed in high temperature drying baker, drying temperature curve is 0 DEG C-200 DEG C
Even all intensifications 6 hours, then keep 200 DEG C of constant temperature 4-8 hour, then green compact are naturally cooling to room temperature；
C, the sintering of yttrium crucible
Product green compact use computer programming to control sintering process and are sintered:
Sintering, uses the closed kiln of electrical heating to be sintered green compact, and sintering temperature 1750 ± 3 DEG C, sintering temperature curve is from 0
DEG C start, be warming up to 1750 DEG C with the uniform programming rate of per hour 30 DEG C；After reaching 1750 DEG C, constant temperature maintains 18-24 hour
Rear closedown heating power, makes kiln take out yttrium crucible after being naturally cooling to room temperature.
The crucible prepared in this embodiment actual heated after reach 80% ratio, phase due to its component Y2O3 when using
Based on the life-span using uninterrupted molten titanium alloy, the ratio that the ceramic crucible that this component proportion obtains exists because of zirconium oxide
Titanium alloy solution adhesion occurring and invades time of profit and be about 5-6 hour, i.e. in the present embodiment, crucible is adding temperature drop continuously repeatedly
Temperature uses more than 5-6 hour, and crucible material the most easily occurs that catabiosis is susceptible to bulk material peeling and is mixed into titanium alloy
In solution, using 5-6 hour in cooling of the most repeatedly heating continuously, will not there is the phenomenon of adhesion with titanium alloy solution in crucible.
Embodiment 5
A kind of titanium alloy melts casting electric smelting yttrium oxide ceramic crucible, with the percentages of oxide weight, adds up to
100%, it is by following chemical composition: the Y2O3 of 70%, be not more than 0.5% other trace impurity, remaining be Zro2, other trace
Impurity is oxide, including Fe2O3、Cr2O3、TiO2、CaO、K2O、SiO2、Al2O3、MgO、Na2O。
A kind of above-mentioned titanium alloy melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, including following step
Rapid:
A, by high-frequency heating fusion crust method, high-purity crystallized body raw material is prepared in yttrium oxide molten mass magnetic agitation melting
It is the yttrium oxide of 99.999% by material purity, at a temperature of 2500 DEG C-2800 DEG C, carries out melting, use water-cooled
Copper-cold crucible crystallization electromagnetic induction heating mode；It is 99.999% by purity, three oxidations two that D50 feeds intake that granularity is 1um-3um
Yttrium raw material loads in cold crucible, and cold crucible selects the diameter cold crucible (in the cup-shaped bucket that copper tube surrounds) more than 1000 mm,
Yttrium oxide charge is 500kg, is uniformly blended into zirconium oxide 212kg simultaneously, puts into 4-6g metal zirconium sheet at cold crucible center
Or 1kg cubic crystal zirconium powder is used for drawing heat, switching on power, carry out high-frequency heating, the operating frequency of high-frequency induction generator is
800 kHz～1 MHz, power is at 500 kW；Treating that the thermit powder that draws that central area is thrown in starts thermal source diffusion, raw material starts to melt
Change, copper tube is now passed through circulating chilled water cooling, takes away heat, make outer layer powder not melt, form cold crucible fusion crust, treat cold earthenware
When in crucible, raw material 75-83% zone melt reaches molten condition, the magnetic agitation effect that high-frequency induction is had starts to play and makees
With, make melt solution present uniform Fusion Strain, also make solution obtain the consistent degree of superheat simultaneously；Melt is maintained melted
After state 60-120 minute, stop power, stop heating, allow molten mass Temperature fall, along with melt temperature declines, because cooling is produced
Give birth to supersaturation concentration and start gradually to solidify to lenticular, after melt crystallization is cooled to room temperature, take out pure yittrium oxide knot
Crystal product；
Do not bring incorporating of other materials during this into, be effectively guaranteed purity and the cleanliness factor of yittrium oxide crystal, and adopt
With magnetic force, solution is stirred, is not only able to enable solution the most even, also make the yittrium oxide after cooling for completely
Monocrystalline block.
B, the broken and granularity of yittrium oxide crystalline solid are equipped with and molding
The yittrium oxide monocrystalline block crossed through electromagnetic induction melting obtained in step a carrying out broken and granularity be equipped with, preparing should
For product molding；Concrete broken yittrium oxide electric smelting crystal size is 325 mesh, 100 mesh, φ 0-0.5mm granule, φ 0.5-
1mm granule, φ 1-2mm granule, φ 2-3mm granule, totally 6 ranks；Grain size proportion after Po Sui is: 325 mesh account for gross mass
28-33%, 100 mesh account for the 17-22% of gross mass, φ 0-0.5mm granule and account for 9-11%, the φ 0.5-1mm granule of gross mass and account for total matter
8-11%, the φ 1-2mm granule of amount accounts for 19-23%, the φ 2-3mm granule of gross mass and accounts for the 8-12% of gross mass；To be equipped with after crushing
The solid solution of good granularity is placed in rustless steel V-type batch mixer or three-dimensional material mixer is blended, and the time being blended is not less than 4 hours,
After granule and powder are sufficiently mixed uniformly, more mixed granule and powder are placed in rustless steel blender, and add second
Enol water-soluble binding agents, adds the 5%-6% that amount is the yittrium oxide gross mass after crushing of vinyl alcohol water-soluble binding agents, then
Being sufficiently stirred for, the time of stirring is not less than 2 hours, after water-soluble binding agents and raw material are sufficiently mixed uniformly, by raw material
Drying in being placed in drying baker, drying temperature is 30 DEG C-80 DEG C, and drying time is 8-12 hour, the raw aqueous after drying
Weight ＜ 2%, is placed in raw material the sintered-carbide die intracavity of molding, extrusion forming, obtains required shape and chi after drying
Very little product green compact；Drying in obtained product green compact are placed in high temperature drying baker, drying temperature curve is 0 DEG C-200 DEG C
Even all intensifications 6 hours, then keep 200 DEG C of constant temperature 4-8 hour, then green compact are naturally cooling to room temperature；
C, the sintering of yttrium crucible
Product green compact use computer programming to control sintering process and are sintered:
Sintering, uses the closed kiln of electrical heating to be sintered green compact, and sintering temperature 1750 ± 3 DEG C, sintering temperature curve is from 0
DEG C start, be warming up to 1750 DEG C with the uniform programming rate of per hour 30 DEG C；After reaching 1750 DEG C, constant temperature maintains 18-24 hour
Rear closedown heating power, makes kiln take out yttrium crucible after being naturally cooling to room temperature.
The crucible prepared in this embodiment actual heated after only reach 70% ratio due to its component Y2O3 when using,
Based on the life-span of relative usage uninterrupted molten titanium alloy, the ratio that the ceramic crucible that this component proportion obtains exists because of zirconium oxide
Example generation titanium alloy solution adhesion and invade time of profit and be about 4-5 hour, i.e. in the present embodiment, crucible is being heated continuously repeatedly
Cooling uses more than 4-5 hour, and crucible material the most easily occurs that catabiosis is susceptible to bulk material peeling and is mixed into titanium conjunction
In gold solution, using 4-5 hour in cooling of the most repeatedly heating continuously, will not there is the phenomenon of adhesion with titanium alloy solution in crucible.
By to crucible generation titanium alloy solution adhesion prepared in the various embodiments described above and invade time of profit and carry out
Test and contrast, it can be seen that in embodiment 1, ceramic crucible is least susceptible to titanium alloy solution adhesion and invades profit, and its component is
Optimum proportion scheme.
Claims (10)
1. a titanium alloy melts casting electric smelting yttrium oxide ceramic crucible, it is characterised in that: with the hundred of oxide weight
Proportion by subtraction meter, adds up to 100%, and it has a following chemical composition:
Y2O3:70%-99.5%；
Zro2:0.5%-30%；
Being not more than other trace impurity of 0.5%, other trace impurity is oxide.
Titanium alloy the most according to claim 1 melts casting electric smelting yttrium oxide ceramic crucible, it is characterised in that: institute
Stating other trace impurity is oxide, including Fe2O3、Cr2O3、TiO2、CaO、K2O、SiO2、Al2O3、MgO、Na2O。
3. titanium alloy as claimed in claim 1 melts a preparation method for casting electric smelting yttrium oxide ceramic crucible,
Comprise the following steps:
A, by high-frequency heating fusion crust method, high-purity crystallized body raw material is prepared in yttrium oxide molten mass magnetic agitation melting
It is the yttrium oxide of 99.999% by material purity, at a temperature of 2500 DEG C-2800 DEG C, carries out melting, use water-cooled
Copper-cold crucible crystallization electromagnetic induction heating mode；Yttrium oxide raw material loads in cold crucible, can also be uniformly blended into oxygen simultaneously
Change zirconium, put into metal zirconium sheet or cubic crystal zirconium powder at cold crucible center, switch on power, carry out high-frequency heating；Treat central area
The metal zirconium sheet thrown in or cubic crystal zirconium powder start thermal source diffusion, and raw material starts to melt, and is now passed through cold water in copper tube and follows
Ring cools down, and takes away heat, makes outer layer powder not melt, and forms cold crucible fusion crust, and in treating cold crucible, raw material 75-83% zone melt reaches
During to molten condition, the magnetic agitation effect that high-frequency induction is had starts to play a role, and makes melt solution present uniformly fusion
State, also makes solution obtain the consistent degree of superheat simultaneously, after melt is maintained molten condition 60-120 minute, stops merit
Rate, stops heating, and allows molten mass Temperature fall, along with melt temperature declines, starts gradually because cooling produces supersaturation concentration
Solidification is to lenticular, after melt crystallization is cooled to room temperature, takes out yittrium oxide crystalline solid；
B, the broken and granularity of yittrium oxide crystalline solid are equipped with and molding
The yittrium oxide monocrystalline block crossed through electromagnetic induction melting obtained in step a carrying out broken and granularity be equipped with, preparing should
For product molding；To crush in solid solution that is rear and that be equipped with granularity is placed in rustless steel V-type batch mixer or three-dimensional material mixer
Row is blended, and the time being blended is not less than 4 hours, after granule to be combined and powder are sufficiently mixed uniformly, is placed on rustless steel
In blender, and adding vinyl alcohol water-soluble binding agents, be stirred, mixing time is not less than 2 hours, treats water-soluble binding agents
After being thoroughly mixed uniformly with raw material, drying in being placed on drying baker, the hard being placed on molding after drying closes
In gold mold cavity, extrusion forming, obtain required shape and sized products green compact；Obtained product green compact are placed in high temperature
Dry in drying baker, after drying, be naturally cooling to room temperature；
C, the sintering of yttrium crucible
Product green compact use computer programming to control sintering process and are sintered:
Sintering, uses the closed kiln of electrical heating to be sintered green compact, after having sintered, makes kiln be naturally cooling to room temperature,
Then take out yttrium crucible.
Titanium alloy the most according to claim 3 melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, its
It is characterised by: in described a step, the yttrium oxide D50 granularity that feeds intake is 1um-3um.
Titanium alloy the most according to claim 3 melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, its
It is characterised by: the operating frequency of the high-frequency induction generator described in described a step is 800 kHz～1 MHz, and power exists
500 kW。
Titanium alloy the most according to claim 3 melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, its
Be characterised by: the broken and granularity described in step b is equipped with, concrete broken yittrium oxide electric smelting crystal size be 325 mesh, 100
Mesh, φ 0-0.5mm granule, φ 0.5-1mm granule, φ 1-2mm granule, φ 2-3mm granule, totally 6 ranks；Granularity after Po Sui
Proportioning is: 325 mesh account for the 28-33% of gross mass, and 100 mesh account for the 17-22% of gross mass, φ 0-0.5mm granule and account for the 9-of gross mass
11%, φ 0.5-1mm granule accounts for 8-11%, the φ 1-2mm granule of gross mass and accounts for 19-23%, the φ 2-3mm granule of gross mass and account for always
The 8-12% of quality.
Titanium alloy the most according to claim 3 melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, its
It is characterised by: described step b adds the 5%-6% that amount is the yittrium oxide gross mass after crushing of vinyl alcohol water-soluble binding agents.
Titanium alloy the most according to claim 3 melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, its
Being characterised by: dry in raw material is released in described step b drying baker, drying temperature is 30 DEG C-80 DEG C, and drying time is
4-6 hour, raw aqueous weight ＜ 6% after drying.
Titanium alloy the most according to claim 3 melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, its
Be characterised by: dry in product green compact are placed in high temperature drying baker by described step b, dry curve be 0 DEG C-200 DEG C even
All heat up 6 hours, then keep 200 DEG C of constant temperature 4-8 hour.
Titanium alloy the most according to claim 3 melts the preparation method of casting electric smelting yttrium oxide ceramic crucible, its
Being characterised by: in described step c, sintering temperature is 1750 ± 3 DEG C, and sintering temperature curve is from the beginning of 0 DEG C, with per hour 30 DEG C
Uniformly programming rate rises to 1750 DEG C；After reaching 1750 DEG C, constant temperature closes heating power after maintaining 18-24 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610593898.7A CN106116578B (en) | 2016-07-26 | 2016-07-26 | Titanium alloy melts casting electric smelting yttria ceramic crucible and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610593898.7A CN106116578B (en) | 2016-07-26 | 2016-07-26 | Titanium alloy melts casting electric smelting yttria ceramic crucible and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106116578A true CN106116578A (en) | 2016-11-16 |
| CN106116578B CN106116578B (en) | 2019-02-12 |
Family
ID=57290438
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610593898.7A Active CN106116578B (en) | 2016-07-26 | 2016-07-26 | Titanium alloy melts casting electric smelting yttria ceramic crucible and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106116578B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108623315A (en) * | 2018-05-03 | 2018-10-09 | 苏州卫优知识产权运营有限公司 | A kind of preparation process of titanium alloy smelting oxidation yttrium powder |
| CN109928754A (en) * | 2019-04-22 | 2019-06-25 | 郑州振中电熔新材料有限公司 | A kind of manufacturing method of modified oxidized yttrium |
| CN112225543A (en) * | 2020-10-12 | 2021-01-15 | 郑州方铭高温陶瓷新材料有限公司 | Fusion-cast formed cylindrical ceramic tile applied to glass kiln regenerator and preparation method thereof |
| CN112695375A (en) * | 2021-01-06 | 2021-04-23 | 上海应用技术大学 | Preparation method of zirconia crystal |
| CN115403392A (en) * | 2022-08-24 | 2022-11-29 | 广东省科学院资源利用与稀土开发研究所 | Crucible base body for smelting titanium-based gold storage alloy and preparation method and application thereof |
| RU2791771C1 (en) * | 2022-08-12 | 2023-03-13 | Общество с ограниченной ответственностью Научно-производственная фирма "ЭКСИТОН" | Method for producing high-temperature ceramics based on yttrium oxide |
| CN116675536A (en) * | 2023-05-11 | 2023-09-01 | 武汉科技大学 | Yttria ceramic crucible for smelting titanium alloy and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381242A (en) * | 2008-10-10 | 2009-03-11 | 东北大学 | Method for preparing crucible for smelting titanium and titanium alloys |
| CN103224396A (en) * | 2013-04-11 | 2013-07-31 | 哈尔滨工业大学 | Composite crucible liner for vacuum anti-gravity casting of titanium and titanium alloys, and manufacturing method thereof |
-
2016
- 2016-07-26 CN CN201610593898.7A patent/CN106116578B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381242A (en) * | 2008-10-10 | 2009-03-11 | 东北大学 | Method for preparing crucible for smelting titanium and titanium alloys |
| CN103224396A (en) * | 2013-04-11 | 2013-07-31 | 哈尔滨工业大学 | Composite crucible liner for vacuum anti-gravity casting of titanium and titanium alloys, and manufacturing method thereof |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108623315A (en) * | 2018-05-03 | 2018-10-09 | 苏州卫优知识产权运营有限公司 | A kind of preparation process of titanium alloy smelting oxidation yttrium powder |
| CN109928754A (en) * | 2019-04-22 | 2019-06-25 | 郑州振中电熔新材料有限公司 | A kind of manufacturing method of modified oxidized yttrium |
| CN109928754B (en) * | 2019-04-22 | 2021-07-06 | 郑州振中电熔新材料有限公司 | Method for preparing modified yttrium oxide |
| CN112225543A (en) * | 2020-10-12 | 2021-01-15 | 郑州方铭高温陶瓷新材料有限公司 | Fusion-cast formed cylindrical ceramic tile applied to glass kiln regenerator and preparation method thereof |
| CN112695375A (en) * | 2021-01-06 | 2021-04-23 | 上海应用技术大学 | Preparation method of zirconia crystal |
| RU2791771C1 (en) * | 2022-08-12 | 2023-03-13 | Общество с ограниченной ответственностью Научно-производственная фирма "ЭКСИТОН" | Method for producing high-temperature ceramics based on yttrium oxide |
| CN115403392A (en) * | 2022-08-24 | 2022-11-29 | 广东省科学院资源利用与稀土开发研究所 | Crucible base body for smelting titanium-based gold storage alloy and preparation method and application thereof |
| CN115403392B (en) * | 2022-08-24 | 2023-06-20 | 广东省科学院资源利用与稀土开发研究所 | Crucible substrate for smelting titanium-based hydrogen storage alloy, and preparation method and application thereof |
| CN116675536A (en) * | 2023-05-11 | 2023-09-01 | 武汉科技大学 | Yttria ceramic crucible for smelting titanium alloy and preparation method thereof |
| CN116675536B (en) * | 2023-05-11 | 2024-04-30 | 武汉科技大学 | Yttria ceramic crucible for smelting titanium alloy and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106116578B (en) | 2019-02-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106116578A (en) | Titanium alloy melts casting electric smelting yttrium oxide ceramic crucible and preparation method thereof | |
| CN103276253B (en) | A kind of Low-cost Al-Ti-B refiner and preparation method thereof | |
| CN106319236B (en) | A kind of preparation method of Ti2AlNb alloy materials | |
| CN102863151A (en) | High-strength heat-resistant glassware | |
| CN103866168A (en) | Preparation method of nano-particle reinforcement magnesium-based biocomposite material | |
| CN105948739A (en) | Yttria-zirconia sosoloid ceramics for temperature field of ultrahigh-temperature crystal growing furnace and preparation method for yttria-zirconia sosoloid ceramics | |
| CN112011704B (en) | Preparation method of rare earth aluminum titanium boron grain refiner | |
| CN103233146A (en) | High-efficiency clean Al-Ti-B refiner and preparation method thereof | |
| CN101397613B (en) | Method for preparing molybdenum-silicium-boron alloy | |
| CN108484140A (en) | The ceramic layered core of two-component | |
| CN102392168A (en) | Vanadium aluminum titanium intermediate alloy used for manufacturing high vanadium titanium alloy material and preparation method thereof | |
| CN102965556B (en) | Multi-element Mg-Zn-Al based magnesium alloy and preparation method thereof | |
| CN100398686C (en) | CrB2-FeNiCr composite material, its preparation method and aluminothermy-quick solidification apparatus | |
| CN103866155A (en) | Beryllium-copper alloy production and ingot casting process | |
| CN103060565A (en) | Preparation of vanadium-aluminum alloy material | |
| CN103484701B (en) | Method for refining cast titanium alloy crystalline grains | |
| CN109053194A (en) | Directional solidification niobium silicon-base alloy hollow turbine vane ceramic core preparation method | |
| CN112247156A (en) | Titanium alloy powder of endogenous nano TiC particles and preparation method and application thereof | |
| CN102815940A (en) | Calcium oxide and zirconium oxide composite ceramic core for niobium-silicon based alloy investment casting | |
| CN107058845B (en) | A kind of preparation method of aluminium vanadium zirconium molybdenum chromium quinary alloy | |
| CN113860896A (en) | High-temperature precision casting low-creep corundum mullite and manufacturing method thereof | |
| CN102910918A (en) | Magnesium-calcium-zirconium composite material | |
| CN111910092A (en) | Preparation method of aluminum-niobium-boron intermediate alloy and aluminum-niobium-boron intermediate alloy | |
| CN100445406C (en) | Compounded material for smelting flat 3104 aluminium alloy ingot and its material throwing process | |
| CN101942618A (en) | Magnesium-based block metal glass composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |