CN106498236B - A kind of glass fibre production alloy crucible and preparation method thereof - Google Patents

A kind of glass fibre production alloy crucible and preparation method thereof Download PDF

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CN106498236B
CN106498236B CN201610947614.XA CN201610947614A CN106498236B CN 106498236 B CN106498236 B CN 106498236B CN 201610947614 A CN201610947614 A CN 201610947614A CN 106498236 B CN106498236 B CN 106498236B
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alloy
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crucible
electrode bar
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CN106498236A (en
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苏风格
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Jining Beichen machinery processing Co., Ltd.
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Beichen Jining Metal Material Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/08—Bushings, e.g. construction, bushing reinforcement means; Spinnerettes; Nozzles; Nozzle plates
    • C03B37/0805—Manufacturing, repairing, or other treatment of bushings, nozzles or bushing nozzle plates
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/08—Bushings, e.g. construction, bushing reinforcement means; Spinnerettes; Nozzles; Nozzle plates
    • C03B37/095—Use of materials therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/06—Alloys based on chromium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/11—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of chromium or alloys based thereon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Physics & Mathematics (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a kind of glass fibre production alloy crucible and preparation method thereof, its chemical component weight ratio is：C：0.02 0.1%, Cr：20 50%, Ni：35 70%, Hf：5 13.8%, Cu：0.8 2.4%, Ce：0.1 1.0%, Al：0.28 1.5%, pretreated metal is smelting, casting, turning obtain electrode bar, then smelted through vacuum consumable, diffusion annealing, forging obtain alloy blank, last machined to obtain alloy crucible；Compared with prior art, the beneficial effects of the invention are as follows：Using Cr and Ni as alloy material main component, the existing platinum crucible using platinum as main component is substituted, greatly reduces cost, effectively remove contained gaseous impurity etc. in molten steel, improve the degree of purity of product, improve the intensity and heat-resisting quantity of alloy crucible.

Description

A kind of glass fibre production alloy crucible and preparation method thereof
Technical field
The invention belongs to glass fibre manufacture equipment technical field, more particularly relates to a kind of glass fibre production alloy Crucible and preparation method thereof.
Background technology
Glass fibre is indispensable important industrial products in industrial production, has good insulating, heat resistance strong, anti- The advantages that corrosivity is good, high mechanical strength, it is many to be widely used in electrically insulating material, heat-insulating material and circuit substrate etc. Field.
Glass fibre is drawn in a manner of mechanical wire drawing frequently with by melten glass ball platinum alloy plate, all the time glass The manufacture of glass fiber mainly has two kinds of techniques of fire clay bushing and platinum crucible, and the former pollutes environment, waste of resource, low production efficiency Under, poor product quality, it is the production technology that superseded backwardness is give stricted orders by country；The latter's product quality is high, but its raw material platinum Price is high, high processing costs.
The application for a patent for invention of Application No. 200910028338.7 discloses a kind of ultra-fine continuous glass fiber production and used Crucible, along crucible center line its both sides set two pieces of tabulars draw electrode, its bushing using platinum-rhodium alloy making, crucible remaining Part uses refractory material laying, reduces the dosage of platinum alloy, reduces production cost to a certain extent.
But it is still very high as the crucible cost that main raw material produce using platinum or platinum, therefore urgently find a kind of product Quality is high, lower-cost with high temperature resistant, the alloy crucible material of corrosion resistance.
The content of the invention
In order to solve the problems, such as that existing production glass fibre crucible converted products is of poor quality, cost is high, the present invention provides A kind of glass fibre production alloy crucible and preparation method thereof, the crucible material have very strong heat-resisting quantity and corrosion-resistant Property, the product quality processed is high, and cost is only 1/10th of existing platinum crucible.
The present invention is that technical scheme is used by solving its technical problem：A kind of glass fibre production alloy crucible Preparation method, it is characterised in that the chemical component weight ratio of alloy crucible is：C：0.02-0.1%, Cr：20-50%, Ni：35- 70%, Hf：5-13.8%, Cu：0.8-2.4%, Ce：0.1-1.0%, Al：0.28-1.5%；The preparation method of alloy crucible include with Lower step：
（1）Pretreatment：Pure Ni, Cr are respectively charged into small charging basket, loaded in heating furnace, is warming up to 200 DEG C, is incubated 24 hours Take out afterwards and be air-cooled to room temperature；
（2）Melting：The C of Cr, Hf, Ni, Cu, 1/2 amount is sequentially loaded into vacuum drying oven, the C of Al, Ce and 1/2 amount is filled respectively Enter in small hopper, close vacuum stove top case；Start mechanical pump after 5 minutes, start lobe pump, when vacuum reaches 0.2Pa, open Dynamic melting power supply carries out melting, control fusing power 18kW；Control fusing power 25kW, vacuum 0.4Pa after 10 minutes；Again 10 minutes control fusing power 50kW are crossed, are kept for 10 minutes；Argon gas is filled with into vacuum drying oven, adds Al, is controlled after 10 minutes molten Ce is added when changing power 40kW, the C of 1/2 amount is added after melting down, is kept for 10 minutes；Adjustment control melts power 20kW, is kept for 5 points Clock；
（3）Cool conjunctiva：Melting power supply is disconnected, carries out cooling conjunctiva, is kept for 15 minutes, goes out liquation under power 20kW；
（4）Ingot casting：Liquation is injected in alloy ingot mould, pouring temperature is 1400-1480 DEG C；
（5）Cooling：After liquation stops 10 minutes in alloy ingot mould, vacuum breaker, will when temperature is dropped to below 200 DEG C Alloy pig takes out from alloy ingot mould；
（6）Turning：Melted alloy pig is placed on engine lathe, alloy ingot surface car is gone into unilateral 5mm, car is in line Spend the electrode bar for 0-2mm；
（7）Consutrode welds：The vacuum of consumable electrode vacuum furnace is 0.8Pa, voltage 22V, electric current 2.5kA, carries out electrode The welding of rod and transition electrode；
（8）Vacuum consumable is smelted：After the normal starting the arc 5 minutes, adjustment consumable electrode vacuum furnace voltage is 24V, electric current 3.8kA, Melting speed control is at 80 kgs/hour；
（9）Bind：Molten electrode bar length to primary electrode rod length 1/5 when, adjust voltage and current, make melting speed control At 40 kgs/hour；
（10）Diffusion annealing：The alloy pig of vacuum consumable is put into cabinet-type electric furnace and is diffused annealing, charging temperature is 690-700 DEG C, programming rate 2.5-4.0mm/ minutes, 1220 DEG C are warming up to, are incubated 24 hours, take out air cooling；
（11）One-time forging：The good electrode bar of DIFFUSION TREATMENT is reloaded in cabinet-type electric furnace, charging temperature 690- 700 DEG C, programming rate 2.5mm/ minutes, 1180 DEG C are warming up to, are incubated 2 hours, electrode bar are quickly put on 3 tons of pneumatic hammers, Aforesaid operations control is completed within half a minute, and electrode bar one end is clamped with manipulator, and whole process was controlled within one minute, the One fiery deformation amount controlling is 50%, and time control is in 3 minutes；
（12）Second fire forging：Electrode bar after One-time forging is reloaded in electric furnace immediately, and it is small that 1 is incubated at 1180 DEG C When, electrode bar is quickly put on 3 tons of pneumatic hammers, aforesaid operations control is completed within half a minute, and electrode bar is clamped with manipulator One end, whole process were controlled within one minute, and the second fiery deformation amount controlling is 30%, and time control is in 2 minutes, by forging Air cooling；
（13）Machining：The blank that will have been forged, according to crucible size, with wire cutting blanking, and descended material is shifted To machining center, machining center programming, produces alloy crucible according to layout design.
It is further preferred that the step（7）The bonding area of middle electrode bar and transition electrode accumulates not less than electrode sections 2/3.
It is further preferred that the step（8）Middle arcing voltage is 23.0V, electric current 4.0kA.
Compared with prior art, the beneficial effects of the invention are as follows：
1. using Cr and Ni as alloy material main component, the existing platinum crucible using platinum as main component is substituted, greatly Reduce cost greatly；
2. with the addition of Cr, Ni, Hf element in the alloy material, be advantageous to improve alloy crucible elevated temperature strength and corrosion resistance Energy；
3. smelting process is smelted using vacuum consumable, contained gaseous impurity etc. in liquation can be effectively removed, improves product Degree of purity；
4. the strict temperature of forging process and empty hammer dynamics and speed control, be advantageous to improve the carbon of alloy crucible material Compound is uniformly distributed and resistance to elevated temperatures.
Embodiment
The present invention is described in further detail with reference to specific embodiment, so that the public preferably grasps the present invention's Implementation.
Embodiment 1
A kind of glass fibre production alloy crucible, its chemical component weight ratio are as follows：
C：0.02%, Cr：50%, Ni：35%, Hf：13.8%, Cu：0.8%, Ce：0.1%, Al：0.28%.
Its preparation method comprises the following steps：
（1）Pretreatment：Pure Ni, Cr are respectively charged into small charging basket, loaded in heating furnace, is warming up to 200 DEG C, is incubated 24 hours Take out afterwards and be air-cooled to room temperature；
（2）Melting：The C of Cr, Hf, Ni, Cu, 1/2 amount is sequentially loaded into vacuum drying oven, the C of Al, Ce and 1/2 amount is filled respectively Enter in small hopper, close vacuum stove top case；Start mechanical pump after 5 minutes, start lobe pump, when vacuum reaches 0.2Pa, open Dynamic melting power supply carries out melting, control fusing power 18kW；Control fusing power 25kW, vacuum 0.4Pa after 10 minutes；Again 10 minutes control fusing power 50kW are crossed, are kept for 10 minutes；Argon gas is filled with into vacuum drying oven, adds Al, is controlled after 10 minutes molten Ce is added when changing 40 kW of power, the C of 1/2 amount is added after melting down, is kept for 10 minutes；Adjustment control melts power 20kW, keeps 5 Minute；
（3）Cool conjunctiva：Melting power supply is disconnected, carries out cooling conjunctiva, is kept for 15 minutes, goes out liquation under power 20kW；
（4）Ingot casting：Liquation is injected in alloy ingot mould, pouring temperature is 1400 DEG C；
（5）Cooling：After liquation stops 10 minutes in alloy ingot mould, vacuum breaker, will when temperature is dropped to below 200 DEG C Alloy pig takes out from alloy ingot mould；
（6）Turning：Melted alloy pig is placed on engine lathe, alloy ingot surface car is gone into unilateral 5mm, car is in line Spend the electrode bar for 0-2mm；
（7）Consutrode welds：The vacuum of consumable electrode vacuum furnace is 0.8Pa, voltage 22V, electric current 2.5kA, carries out electrode The welding of rod and transition electrode；
（8）Vacuum consumable is smelted：After the normal starting the arc 5 minutes, adjustment consumable electrode vacuum furnace voltage is 24V, electric current 3.8kA, Melting speed control is at 80 kgs/hour；
（9）Bind：Molten electrode bar length to primary electrode rod length 1/5 when, adjust voltage and current, make melting speed control At 40 kgs/hour；
（10）Diffusion annealing：The alloy pig of vacuum consumable is put into cabinet-type electric furnace and is diffused annealing, charging temperature 690 DEG C, programming rate 2.5mm/ minutes, 1250 DEG C are warming up to, are incubated 24 hours, take out air cooling；
（11）One-time forging：The good electrode bar of DIFFUSION TREATMENT is reloaded in cabinet-type electric furnace, 690 DEG C of charging temperature, Programming rate 2.5mm/ minutes, 1180 DEG C are warming up to, are incubated 2 hours, electrode bar are quickly put on 3 tons of pneumatic hammers, above-mentioned behaviour Control and completed within half a minute, electrode bar one end is clamped with manipulator, whole process was controlled within one minute, and the first fire becomes The control of shape amount is 50%, and time control is in 3 minutes；
（12）Second fire forging：Electrode bar after One-time forging is reloaded in electric furnace immediately, and it is small that 1 is incubated at 1180 DEG C When, electrode bar is quickly put on 3 tons of pneumatic hammers, aforesaid operations control is completed within half a minute, and electrode bar is clamped with manipulator One end, whole process were controlled within one minute, and the second fiery deformation amount controlling is 30%, and time control is in 2 minutes, by forging Air cooling；
（13）Machining：The blank that will have been forged, according to crucible size, with wire cutting blanking, and descended material is shifted To machining center, machining center programming, produces alloy crucible according to layout design.
Alloy crucible material is taken, 25*25*3 square, test specimen is used as after polishing, while takes the NS333 alloy blocks of same specification Test specimen as a comparison：
（1）It is test knot in 15% middle alkali glass solution by the alkali content that two kinds of materials are respectively put into c-glass marble Fruit is shown in Table 1.1；
（2）Two kinds of materials are respectively put into progress cool-hot fatigue test, test result in cold-hot fatigue testing machine to be shown in Table 1.2；
（3）Two kinds of materials are tested into its tensile strength respectively according to GB/T 28487-2012, test result is shown in Table 1.3；
（4）Two kinds of materials are respectively placed in into progress high-temperature oxidation test, test result under 1200 DEG C of high temperature to be shown in Table 1.4。
The corrosion resistance of the alloy crucible of table 1.1 and NS333 alloys contrasts
Test material Test temperature/DEG C Test period/h Quality/g before experiment Quality/g after experiment The proportion of goods damageds/%
NS333 1180 2520 15 11 26.67
Alloy crucible 1180 2520 15 14.1 6.00
The cool-hot fatigue of the alloy crucible of table 1.2 and NS333 alloys contrasts
Test material State Test temperature Recycle ratio Crack length/mm
NS333 Hot rolling 1150 10 0.52
Alloy crucible Hot forging 1150 15 0.39
The tensile strength of the alloy crucible of table 1.3 and NS333 alloys contrasts
Test material State Test temperature/DEG C Tensile strength/MPa
NS333 Hot rolling 1200 480
Alloy crucible Hot forging 1200 617
The high-temperature oxidation of the alloy crucible of table 1.4 and NS333 alloys contrasts
Test material State Test temperature/DEG C Soaking time/h Rate of body weight gain/%
NS333 Hot rolling 1200 300 0.259
Alloy crucible Hot forging 1200 300 0.083
Embodiment 2
A kind of glass fibre production alloy crucible, its chemical component weight ratio are as follows：
C：0.05%, Cr：30%, Ni：60%, Hf：8%, Cu：1.2%, Ce：0.2%, Al：0.55%.
Its preparation method comprises the following steps：
（1）Pretreatment：Pure Ni, Cr are respectively charged into small charging basket, loaded in heating furnace, is warming up to 200 DEG C, is incubated 24 hours Take out afterwards and be air-cooled to room temperature；
（2）Melting：The C of Cr, Hf, Ni, Cu, 1/2 amount is sequentially loaded into vacuum drying oven, the C of Al, Ce and 1/2 amount is filled respectively Enter in small hopper, close vacuum stove top case；Start mechanical pump after 5 minutes, start lobe pump, when vacuum reaches 0.2Pa, open Dynamic melting power supply carries out melting, control fusing power 18kW；Control fusing power 25kW, vacuum 0.4Pa after 10 minutes；Again 10 minutes control fusing power 50kW are crossed, are kept for 10 minutes；Argon gas is filled with into vacuum drying oven, adds Al, is controlled after 10 minutes molten Ce is added when changing 40 kW of power, the C of 1/2 amount is added after melting down, is kept for 10 minutes；Adjustment control melts power 20kW, keeps 5 Minute；
（3）Cool conjunctiva：Melting power supply is disconnected, carries out cooling conjunctiva, is kept for 15 minutes, goes out liquation under power 20kW；
（4）Ingot casting：Liquation is injected in alloy ingot mould, pouring temperature is 1440 DEG C；
（5）Cooling：After liquation stops 10 minutes in alloy ingot mould, vacuum breaker, will when temperature is dropped to below 200 DEG C Alloy pig takes out from alloy ingot mould；
（6）Turning：Melted alloy pig is placed on engine lathe, alloy ingot surface car is gone into unilateral 5mm, car is in line Spend the electrode bar for 0-2mm；
（7）Consutrode welds：The vacuum of consumable electrode vacuum furnace is 0.8Pa, voltage 22V, electric current 2.5kA, carries out electrode The welding of rod and transition electrode；
（8）Vacuum consumable is smelted：After the normal starting the arc 5 minutes, adjustment consumable electrode vacuum furnace voltage is 24V, electric current 3.8kA, Melting speed control is at 80 kgs/hour；
（9）Bind：Molten electrode bar length to primary electrode rod length 1/5 when, adjust voltage and current, make melting speed control At 40 kgs/hour；
（10）Diffusion annealing：The alloy pig of vacuum consumable is put into cabinet-type electric furnace and is diffused annealing, charging temperature 695 DEG C, programming rate 3.0mm/ minutes, 1250 DEG C are warming up to, are incubated 24 hours, take out air cooling；
（11）One-time forging：The good electrode bar of DIFFUSION TREATMENT is reloaded in cabinet-type electric furnace, 695 DEG C of charging temperature, Programming rate 2.5mm/ minutes, 1180 DEG C are warming up to, are incubated 2 hours, electrode bar are quickly put on 3 tons of pneumatic hammers, above-mentioned behaviour Control and completed within half a minute, electrode bar one end is clamped with manipulator, whole process was controlled within one minute, and the first fire becomes The control of shape amount is 50%, and time control is in 3 minutes；
（12）Second fire forging：Electrode bar after One-time forging is reloaded in electric furnace immediately, and it is small that 1 is incubated at 1180 DEG C When, electrode bar is quickly put on 3 tons of pneumatic hammers, aforesaid operations control is completed within half a minute, and electrode bar is clamped with manipulator One end, whole process were controlled within one minute, and the second fiery deformation amount controlling is 30%, and time control is in 2 minutes, by forging Air cooling；
（13）Machining：The blank that will have been forged, according to crucible size, with wire cutting blanking, and descended material is shifted To machining center, machining center programming, produces alloy crucible according to layout design.
Alloy crucible material is taken, 25*25*3 square, test specimen is used as after polishing, while takes the NS333 alloy blocks of same specification Test specimen as a comparison：
（1）It is test knot in 15% middle alkali glass solution by the alkali content that two kinds of materials are respectively put into c-glass marble Fruit is shown in Table 2.1；
（2）Two kinds of materials are respectively put into progress cool-hot fatigue test, test result in cold-hot fatigue testing machine to be shown in Table 2.2；
（3）Two kinds of materials are tested into its tensile strength respectively according to GB/T 28487-2012, test result is shown in Table 2.3；
（4）Two kinds of materials are respectively placed in into progress high-temperature oxidation test, test result under 1200 DEG C of high temperature to be shown in Table 2.4。
The corrosion resistance of the alloy crucible of table 2.1 and NS333 alloys contrasts
Test material Test temperature/DEG C Test period/h Quality/g before experiment Quality/g after experiment The proportion of goods damageds/%
NS333 1180 2520 15 11 26.67
Alloy crucible 1180 2520 14.6 13.6 6.85
The cool-hot fatigue of the alloy crucible of table 2.2 and NS333 alloys contrasts
Test material State Test temperature Recycle ratio Crack length/mm
NS333 Hot rolling 1150 10 0.52
Alloy crucible Hot forging 1150 15 0.38
The tensile strength of the alloy crucible of table 2.3 and NS333 alloys contrasts
Test material State Test temperature/DEG C Tensile strength/MPa
NS333 Hot rolling 1200 480
Alloy crucible Hot forging 1200 620
The high-temperature oxidation of the alloy crucible of table 2.4 and NS333 alloys contrasts
Test material State Test temperature/DEG C Soaking time/h Rate of body weight gain/%
NS333 Hot rolling 1200 300 0.259
Alloy crucible Hot forging 1200 300 0.087
Embodiment 3
A kind of glass fibre production alloy crucible, its chemical component weight ratio are as follows：
C：0.1%, Cr：20%, Ni：70%, Hf：5%, Cu：2.4%, Ce：1.0%, Al：1.5%.
Its preparation method comprises the following steps：
（1）Pretreatment：Pure Ni, Cr are respectively charged into small charging basket, loaded in heating furnace, is warming up to 200 DEG C, is incubated 24 hours Take out afterwards and be air-cooled to room temperature；
（2）Melting：The C of Cr, Hf, Ni, Cu, 1/2 amount is sequentially loaded into vacuum drying oven, the C of Al, Ce and 1/2 amount is filled respectively Enter in small hopper, close vacuum stove top case；Start mechanical pump after 5 minutes, start lobe pump, when vacuum reaches 0.2Pa, open Dynamic melting power supply carries out melting, control fusing power 18kW；Control fusing power 25kW, vacuum 0.4Pa after 10 minutes；Again 10 minutes control fusing power 50kW are crossed, are kept for 10 minutes；Argon gas is filled with into vacuum drying oven, adds Al, is controlled after 10 minutes molten Ce is added when changing 40 kW of power, the C of 1/2 amount is added after melting down, is kept for 10 minutes；Adjustment control melts power 20kW, keeps 5 Minute；
（3）Cool conjunctiva：Melting power supply is disconnected, carries out cooling conjunctiva, is kept for 15 minutes, goes out liquation under power 20kW；
（4）Ingot casting：Liquation is injected in alloy ingot mould, pouring temperature is 1480 DEG C；
（5）Cooling：After liquation stops 10 minutes in alloy ingot mould, vacuum breaker, will when temperature is dropped to below 200 DEG C Alloy pig takes out from alloy ingot mould；
（6）Turning：Melted alloy pig is placed on engine lathe, alloy ingot surface car is gone into unilateral 5mm, car is in line Spend the electrode bar for 0-2mm；
（7）Consutrode welds：The vacuum of consumable electrode vacuum furnace is 0.8Pa, voltage 22V, electric current 2.5kA, carries out electrode The welding of rod and transition electrode；
（8）Vacuum consumable is smelted：After the normal starting the arc 5 minutes, adjustment consumable electrode vacuum furnace voltage is 24V, electric current 3.8kA, Melting speed control is at 80 kgs/hour；
（9）Bind：Molten electrode bar length to primary electrode rod length 1/5 when, adjust voltage and current, make melting speed control At 40 kgs/hour；
（10）Diffusion annealing：The alloy pig of vacuum consumable is put into cabinet-type electric furnace and is diffused annealing, charging temperature 700 DEG C, programming rate 4.0mm/ minutes, 1250 DEG C are warming up to, are incubated 24 hours, take out air cooling；
（11）One-time forging：The good electrode bar of DIFFUSION TREATMENT is reloaded in cabinet-type electric furnace, 700 DEG C of charging temperature, Programming rate 2.5mm/ minutes, 1180 DEG C are warming up to, are incubated 2 hours, electrode bar are quickly put on 3 tons of pneumatic hammers, above-mentioned behaviour Control and completed within half a minute, electrode bar one end is clamped with manipulator, whole process was controlled within one minute, and the first fire becomes The control of shape amount is 50%, and time control is in 3 minutes；
（12）Second fire forging：Electrode bar after One-time forging is reloaded in electric furnace immediately, and it is small that 1 is incubated at 1180 DEG C When, electrode bar is quickly put on 3 tons of pneumatic hammers, aforesaid operations control is completed within half a minute, and electrode bar is clamped with manipulator One end, whole process were controlled within one minute, and the second fiery deformation amount controlling is 30%, and time control is in 2 minutes, by forging Air cooling；
（13）Machining：The blank that will have been forged, according to crucible size, with wire cutting blanking, and descended material is shifted To machining center, machining center programming, produces alloy crucible according to layout design.
Alloy crucible material is taken, 25*25*3 square, test specimen is used as after polishing, while takes the NS333 alloy blocks of same specification Test specimen as a comparison：
（1）It is test knot in 15% middle alkali glass solution by the alkali content that two kinds of materials are respectively put into c-glass marble Fruit is shown in Table 3.1；
（2）Two kinds of materials are respectively put into progress cool-hot fatigue test, test result in cold-hot fatigue testing machine to be shown in Table 3.2；
（3）Two kinds of materials are tested into its tensile strength respectively according to GB/T 28487-2012, test result is shown in Table 3.3；
（4）Two kinds of materials are respectively placed in into progress high-temperature oxidation test, test result under 1200 DEG C of high temperature to be shown in Table 3.4。
The corrosion resistance of the alloy crucible of table 3.1 and NS333 alloys contrasts
Test material Test temperature/DEG C Test period/h Quality/g before experiment Quality/g after experiment The proportion of goods damageds/%
NS333 1180 2520 15 11 26.67
Alloy crucible 1180 2520 14.8 13.8 6.76
The cool-hot fatigue of the alloy crucible of table 3.2 and NS333 alloys contrasts
Test material State Test temperature Recycle ratio Crack length/mm
NS333 Hot rolling 1150 10 0.52
Alloy crucible Hot forging 1150 15 0.35
The tensile strength of the alloy crucible of table 3.3 and NS333 alloys contrasts
Test material State Test temperature/DEG C Tensile strength/MPa
NS333 Hot rolling 1200 480
Alloy crucible Hot forging 1200 625
The high-temperature oxidation of the alloy crucible of table 3.4 and NS333 alloys contrasts
Test material State Test temperature/DEG C Soaking time/h Rate of body weight gain/%
NS333 Hot rolling 1200 300 0.259
Alloy crucible Hot forging 1200 300 0.088
The beneficial effects of the invention are as follows：
1. using Cr and Ni as alloy material main component, the existing platinum crucible using platinum as main component is substituted, greatly Reduce cost greatly；
2. with the addition of Cr, Ni, Hf element in the alloy material, be advantageous to improve the heat-resisting quantity of alloy crucible and corrosion-resistant Property, it can be used continuously 165 days under 1200 DEG C of high temperature；
3. smelting process is smelted using vacuum consumable, contained gaseous impurity etc. in liquation can be effectively removed, improves product Degree of purity；
4. the strict temperature of forging process and empty hammer dynamics and speed control, be advantageous to improve the carbonization of alloy crucible material Thing is uniformly distributed, and improves the high-temperature behavior of material.
Above example is merely to illustrate the present invention rather than limits the scope of the present invention, for those skilled in the art For member, any change for being made within the scope of the present invention, modification or directly implemented using the equal conditions in embodiment Example, it is understood to the covering scope in the present invention.

Claims (3)

  1. A kind of 1. preparation method of glass fibre production alloy crucible, it is characterised in that the chemical component weight of alloy crucible Than for：C：0.02-0.1%, Cr：20-50%, Ni：35-70%, Hf：5-13.8%, Cu：0.8-2.4%, Ce：0.1-1.0%, Al： 0.28-1.5%；The preparation method of alloy crucible comprises the following steps：
    （1）Pretreatment：Pure Ni, Cr are respectively charged into small charging basket, loaded in heating furnace, is warming up to 200 DEG C, insulation takes after 24 hours Go out to be air-cooled to room temperature；
    （2）Melting：The C of Cr, Hf, Ni, Cu, 1/2 amount is sequentially loaded into vacuum drying oven, the C of Al, Ce and 1/2 amount is respectively charged into small In hopper, vacuum stove top case is closed；Start mechanical pump after 5 minutes, start lobe pump, when vacuum reaches 0.2Pa, start molten Refine power supply and carry out melting, control fusing power 18kW；Control fusing power 25kW, vacuum 0.4Pa after 10 minutes；After 10 Minute control fusing power 50kW, is kept for 10 minutes；Argon gas is filled with into vacuum drying oven, adds Al, control fusing work(after 10 minutes Ce is added during rate 40kW, the C of 1/2 amount is added after melting down, is kept for 10 minutes；Adjustment control melts power 20kW, is kept for 5 minutes；
    （3）Cool conjunctiva：Melting power supply is disconnected, carries out cooling conjunctiva, is kept for 15 minutes, goes out liquation under power 20kW；
    （4）Ingot casting：Liquation is injected in alloy ingot mould, pouring temperature is 1400-1480 DEG C；
    （5）Cooling：After liquation stops 10 minutes in alloy ingot mould, vacuum breaker, when temperature is dropped to below 200 DEG C, by alloy Ingot takes out from alloy ingot mould；
    （6）Turning：Melted alloy pig is placed on engine lathe, alloy ingot surface car is gone into unilateral 5mm, car degree of being in line is 0-2mm electrode bar；
    （7）Consutrode welds：The vacuum of consumable electrode vacuum furnace is 0.8Pa, voltage 22V, electric current 2.5kA, carry out electrode bar with The welding of transition electrode；
    （8）Vacuum consumable is smelted：After the normal starting the arc 5 minutes, adjustment consumable electrode vacuum furnace voltage is 24V, electric current 3.8kA, melts speed Control is at 80 kgs/hour；
    （9）Bind：Molten electrode bar length to primary electrode rod length 1/5 when, adjust voltage and current, make melting speed control 40 Kg/hour；
    （10）Diffusion annealing：The alloy pig of vacuum consumable is put into cabinet-type electric furnace and is diffused annealing, charging temperature 690-700 DEG C, programming rate 2.5-4.0mm/ minutes, 1220 DEG C are warming up to, are incubated 24 hours, take out air cooling；
    （11）One-time forging：The good electrode bar of DIFFUSION TREATMENT is reloaded in cabinet-type electric furnace, charging temperature 690-700 DEG C, programming rate 2.5mm/ minutes, 1180 DEG C are warming up to, are incubated 2 hours, electrode bar are quickly put on 3 tons of pneumatic hammers, it is above-mentioned Operational control is completed within half a minute, and electrode bar one end is clamped with manipulator, and whole process was controlled within one minute, the first fire Deformation amount controlling is 50%, and time control is in 3 minutes；
    （12）Second fire forging：Electrode bar after One-time forging is reloaded in electric furnace immediately, and 1 hour is incubated at 1180 DEG C, Electrode bar is quickly put on 3 tons of pneumatic hammers, aforesaid operations control is completed within half a minute, and electrode bar one is clamped with manipulator End, whole process were controlled within one minute, and for the second fiery deformation amount controlling 30%, time control is empty by forging in 2 minutes It is cold；
    （13）Machining：The blank that will have been forged, according to crucible size, with wire cutting blanking, and descended material is transferred to plus Work center, machining center programming, produce alloy crucible according to layout design.
  2. 2. the preparation method of glass fibre production alloy crucible according to claim 1, it is characterised in that the step （7）The bonding area of middle electrode bar and transition electrode is not less than the 2/3 of electrode sections product.
  3. 3. the preparation method of glass fibre production alloy crucible according to claim 1, it is characterised in that the step （8）Middle arcing voltage is 23.0V, electric current 4.0kA.
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