CN109554562A - High-temperature special material master alloy production technology - Google Patents
High-temperature special material master alloy production technology Download PDFInfo
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- CN109554562A CN109554562A CN201811487770.8A CN201811487770A CN109554562A CN 109554562 A CN109554562 A CN 109554562A CN 201811487770 A CN201811487770 A CN 201811487770A CN 109554562 A CN109554562 A CN 109554562A
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- 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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- 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
- C22C1/023—Alloys based on nickel
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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
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
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Abstract
The invention discloses a kind of high-temperature special material master alloy production technologies, include the following steps: the first step, alumina crucible spray treatment；Second step, pretreatment of raw material；Third step, each raw metal for weighing second step, handling well, are successively put into sequence in the processed crucible of the first step, carry out vacuum melting and obtain high temperature alloy ingot casting；After 4th step, high temperature alloy ingot casting scale removal prepared by step 3, riser；5th step is put into melting in the copper crucible of vacuum magnetic suspension smelting furnace and obtains high-temperature special material master alloy.The present invention forms one layer of calcium hexaluminate high-melting-point separation layer, can significantly improve the erosion-resisting characteristics of crucible, improve the purity of foundry alloy melting process, improve the quality of master alloy by carrying out spray treatment in alumina crucible；Entire production process is simple, and design is rationally and realization is easy, and alloy melt is not polluted in easily operated control, does not need expensive equipment, is suitable for industrialized production.
Description
Technical field
The invention belongs to technical field of metal material, and in particular, to a kind of high-temperature special material master alloy production technology.
Background technique
Master alloy is raw material important in metal industry as a kind of semi-finished product.By each element according to certain technique
It melts and reconfigures, by the adjusting of different element alloyed and ingredients and be poured and solidified required for reaching
The purpose of alloy property, these performances include heat-resisting quantity, stretch-resistance etc..
Master alloy is exactly the alloy of impurity element and silicon, and common master alloy has silicon phosphorus and two kinds of silicon boron, and impurity concentration is
10-2 powers and 10-3 powers.Doping can be made to be easy to control as dopant using master alloy, is more acurrate, and female conjunction
The purpose of gold doping is the impurity concentration for changing donor impurity in silicon melt (such as phosphorus) or acceptor impurity (such as boron), makes its life
The monocrystalline resistivity grown reaches defined requirement.When practical progress master alloy production, silicon material and impurity raw material need to be packed into stone
After English crucible, then it is preheated, fusing (also referred to as melt), crystallize, anneal, cooling down, both can be molten using common vacuum
Furnace is processed, and can also be processed using polycrystalline silicon ingot or purifying furnace.
In modern society, master alloy is widely used, and is in the diesel engine turbocharging hot-end component of ship, naval vessels
Irreplaceable critical material.But existing master alloy is required higher and higher, it is desirable that degree of purity is high, miscellaneous to solid, gas etc.
Will requirement is lower, and for the especially height of hydrogen in materials'use, the crackle generated to fatigue plays a part of decision.Thus can not
Go the diesel engine turbocharging for sufficiently meeting ship, naval vessels to the increasing need of performances such as high temperature resistant, stretch-proof, lasting
It asks, effect is undesirable.
Summary of the invention
The purpose of the present invention is to provide a kind of high-temperature special material master alloy production technologies, by alumina crucible
Spray treatment is carried out, one layer of calcium hexaluminate high-melting-point separation layer is formed, the erosion-resisting characteristics of crucible can be significantly improved, is improved female
The purity of alloy melting process improves the quality of master alloy；Entire production process is simple, and design is rationally and realization is easy,
Easily operated control, does not pollute alloy melt, does not need expensive equipment, is suitable for industrialized production, according to present invention process
The high temperature master alloy of preparation has the advantages that surface is smooth, with high purity.
The purpose of the present invention can be achieved through the following technical solutions:
High-temperature special material master alloy production technology, includes the following steps:
The first step, alumina crucible spray treatment: spraying a layer thickness in the inner surface of alumina crucible is 45-55 μm
Coating；
Second step, pretreatment of raw material: according to following parts by weight: 40-50 parts of nickel, 10-20 parts of chromium, 3-6 parts of iron, ferro-niobium 15-
18 parts, 4-6 parts of molybdenum-iron, 1-2 parts of titanium weigh raw metal, by each raw material metal successively mass fraction be 6% hydrochloric acid water
30-40min is impregnated in solution, the NaOH aqueous solution that mass fraction is 5%, oxide on surface is removed, by the gold after immersion treatment
Belong to raw material to pull out, be put into dehydrated alcohol, room temperature ultrasound 10-20min, then each raw metal is placed in electric furnace dryer respectively
It is toasted, baking temperature is 400-420 DEG C, and baking time 150-180min removes the moisture of raw metal；
Third step, each raw metal that second step is weighed, is handled well, according to nickel → chromium → ferro-niobium → molybdenum → iron → titanium
Sequence is successively put into the processed crucible of the first step, specifically, nickel and chromium are put into the bottom of crucible, ferro-niobium is placed in crucible
Bottom and middle part, molybdenum and iron are placed in the middle part and top of crucible, and titanium, which is placed in, is packed into the small of vacuum intermediate-frequency induction melting furnace
In hopper, carries out vacuum melting and obtain high temperature alloy ingot casting；
After 4th step, high temperature alloy ingot casting scale removal prepared by step 3, riser, high temperature alloy fine fodder is obtained；
High temperature alloy fine fodder prepared by step 4 is put into melting in the copper crucible of vacuum magnetic suspension smelting furnace and obtained by the 5th step
To high-temperature special material master alloy.
Further, the detailed process of the first step are as follows:
1) coating spraying liquid is prepared: a calcium aluminate powder being mixed with dehydrated alcohol according to mass ratio 1:6-8, ball milling is put into
Ball milling 25-30min in machine is further continued for ultrasonic disperse 20-30min, obtains coating spraying liquid；
2) crucible cleans: alumina crucible being put into acetone and impregnates 20-25min, is taken out, rinses 2-3 with dehydrated alcohol
It is secondary, then dry 3-4h is placed in 80-90 DEG C of baking oven；
3) it sprays: coating spraying liquid being placed in spray gun, by the interior table of coating spraying liquid even application to magnesia crucible
Face；
4) dry: the magnesia crucible that spraying is completed being put into 85 DEG C of vacuum ovens and dries 150min, is then transferred to
22h is dried in 115 DEG C of baking ovens, completes crucible spraying processing.
Further, the specific steps of vacuum melting described in third step are as follows:
1) 5 × 10 are evacuated to-1Pa-5×10-3Pa carries out melting, dissolved clarification end, and material temperature reaches 1580 DEG C, metal
The interior fusing of frequency induction melting furnace obtains molten steel to raw material in a vacuum；
2) continue to refine 26-28min, refining temperature is maintained at 1540-1560 DEG C, after concise, closes vacuum intermediate-frequency
Induction melting furnace, by freezing mask in the molten steel after refining in a vacuum frequency induction melting furnace；
3) when freezing mask temperature is down to 1520 DEG C, slowly the Ti in small hopper is added in crucible, 150KW is increased to smelting furnace
Grate 5-6 times after power further removes gas, deslagging, until aluminium alloy is poured into punching block after being completely melt again, obtains
High temperature alloy ingot casting.
Further, melting step described in the 5th step are as follows:
1) 5 × 10 are evacuated to-3Pa is then charged with high-purity argon gas to 0.01Pa, and the step is in triplicate to clean vacuum
Room；
2) it is melted, fusion temperature is 1350-1450 DEG C, soaking time 10-20min；
3) it is quickly solidified in such a way that water flowing is cooling.
Beneficial effects of the present invention:
The present invention has carried out coated inside processing before alloy melting, to magnesia crucible, sprays one layer in its inner surface
With a thickness of 45-55 μm of coating；Under high temperature environment, the CA (calcium aluminate) in coating material turns the CA coating of inner surface of crucible
Become CA6(calcium hexaluminate) high-melting-point phase forms one layer of calcium hexaluminate (CA6) etc. high-melting-points separation layer, CA6It is CaO-Al2O3Body
Al in system2O3The highest aluminic acid calcium phase of content has excellent high-temperature behavior, and fusing point is higher than 1875 DEG C, to molten metal and melts
The wetability of slag is relatively low, can significantly improve the erosion-resisting characteristics of crucible；During alloy melting, CA6Separation layer will melt
Fusion gold separates with alumina crucible, reduces and directly contacts, due to CA6Material slag resistance is preferable, CA6Separation layer can be one
Determine to protect alumina ceramic crucible by rapid erosion in degree；Simultaneously as CA6Phase and Al2O3The difference of thermal expansion coefficients of phase is very
It is small, thus two kinds of objects mutually can with the fitting of relative close, more difficult crack of coating and fall off；
Copper crucible can pollution to avoid crucible material under high temperature to alloy melt when vacuum magnetic suspension melting of the present invention；Magnetic
The sufficiently large Lorentz force generated that suspends can promote non-metallic inclusion to float, to effectively remove non-metallic inclusion；
Oxygen, nitrogen content are low, to reduce the non-metallic inclusions such as oxide, the nitride that aluminium alloy is cooling, is formed in process of setting
Quantity；This method utilizes the smelting equipment of existing maturation, easy to operate；
The present invention forms one layer of calcium hexaluminate high-melting-point separation layer, energy by carrying out spray treatment in alumina crucible
The erosion-resisting characteristics of crucible is enough significantly improved, the purity of foundry alloy melting process is improved, improves the quality of master alloy；Entire production
Technical process is simple, and design is rationally and realization is easy, and alloy melt is not polluted in easily operated control, does not need expensive equipment,
It is suitable for industrialized production, has the advantages that surface is smooth, with high purity according to high temperature master alloy prepared by present invention process.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with embodiment, it is clear that described reality
Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff all other embodiment obtained without creative efforts belongs to what the present invention protected
Range.
High-temperature special material master alloy production technology, includes the following steps:
The first step, alumina crucible spray treatment: spraying a layer thickness in the inner surface of alumina crucible is 45-55 μm
Coating；
Detailed process are as follows:
1) coating spraying liquid is prepared: a calcium aluminate powder being mixed with dehydrated alcohol according to mass ratio 1:6-8, ball milling is put into
Ball milling 25-30min in machine is further continued for ultrasonic disperse 20-30min, obtains coating spraying liquid；
2) crucible cleans: alumina crucible being put into acetone and impregnates 20-25min, is taken out, rinses 2-3 with dehydrated alcohol
It is secondary, then dry 3-4h is placed in 80-90 DEG C of baking oven；
3) it sprays: coating spraying liquid being placed in spray gun, by the interior table of coating spraying liquid even application to magnesia crucible
Face；
4) dry: the magnesia crucible that spraying is completed being put into 85 DEG C of vacuum ovens and dries 150min, is then transferred to
22h is dried in 115 DEG C of baking ovens, completes crucible spraying processing；
Under high temperature environment, the CA (calcium aluminate) in coating material is transformed into CA to the CA coating of inner surface of crucible6(six aluminium
Sour calcium) high-melting-point phase, form one layer of calcium hexaluminate (CA6) etc. high-melting-points separation layer, CA6It is CaO-Al2O3Al in system2O3Content
Highest aluminic acid calcium phase has excellent high-temperature behavior, and fusing point is higher than 1875 DEG C, to the wetability of molten metal and slag
It is lower, the erosion-resisting characteristics of crucible can be significantly improved；During alloy melting, CA6Separation layer is by molten alloy and aoxidizes
Aluminium crucible separates, and reduces and directly contacts, due to CA6Material slag resistance is preferable, CA6Separation layer can protect to a certain extent
Alumina ceramic crucible is by rapid erosion；Simultaneously as CA6Phase and Al2O3The difference of thermal expansion coefficients very little of phase, therefore two kinds
Object mutually can with the fitting of relative close, more difficult crack of coating and fall off；
Second step, pretreatment of raw material: according to following parts by weight: 40-50 parts of nickel, 10-20 parts of chromium, 3-6 parts of iron, ferro-niobium 15-
18 parts, 4-6 parts of molybdenum-iron, 1-2 parts of titanium weigh raw metal, by each raw material metal successively mass fraction be 6% hydrochloric acid water
30-40min is impregnated in solution, the NaOH aqueous solution that mass fraction is 5%, oxide on surface is removed, by the gold after immersion treatment
Belong to raw material to pull out, be put into dehydrated alcohol, room temperature ultrasound 10-20min, then each raw metal is placed in electric furnace dryer respectively
It is toasted, baking temperature is 400-420 DEG C, and baking time 150-180min removes the moisture of raw metal；
Third step, each raw metal that second step is weighed, is handled well, according to nickel → chromium → ferro-niobium → molybdenum → iron → titanium
Sequence is successively put into the processed crucible of the first step, specifically, nickel and chromium are put into the bottom of crucible, ferro-niobium is placed in crucible
Bottom and middle part, molybdenum and iron are placed in the middle part and top of crucible, and titanium, which is placed in, is packed into the small of vacuum intermediate-frequency induction melting furnace
In hopper, carries out vacuum melting and obtain high temperature alloy ingot casting；
The specific steps of vacuum melting are as follows:
1) 5 × 10 are evacuated to-1Pa-5×10-3Pa carries out melting, dissolved clarification end, and material temperature reaches 1580 DEG C, metal
The interior fusing of frequency induction melting furnace obtains molten steel to raw material in a vacuum；
2) continue to refine 26-28min, refining temperature is maintained at 1540-1560 DEG C, after concise, closes vacuum intermediate-frequency
Induction melting furnace, by freezing mask in the molten steel after refining in a vacuum frequency induction melting furnace；
3) when freezing mask temperature is down to 1520 DEG C, slowly the Ti in small hopper is added in crucible, 150KW is increased to smelting furnace
Grate 5-6 times after power further removes gas, deslagging, until aluminium alloy is poured into punching block after being completely melt again, obtains
High temperature alloy ingot casting；
After 4th step, high temperature alloy ingot casting scale removal prepared by step 3, riser, high temperature alloy fine fodder is obtained；
High temperature alloy fine fodder prepared by step 4 is put into melting in the copper crucible of vacuum magnetic suspension smelting furnace and obtained by the 5th step
To high-temperature special material master alloy；
Melting step are as follows:
1) 5 × 10 are evacuated to-3Pa is then charged with high-purity argon gas to 0.01Pa, and the step is in triplicate to clean vacuum
Room；
2) it is melted, fusion temperature is 1350-1450 DEG C, soaking time 10-20min；
3) it is quickly solidified in such a way that water flowing is cooling.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (4)
1. high-temperature special material master alloy production technology, which comprises the steps of:
The first step, alumina crucible spray treatment: the painting that a layer thickness is 45-55 μm is sprayed in the inner surface of alumina crucible
Layer；
Second step, pretreatment of raw material: according to following parts by weight: 40-50 parts of nickel, 10-20 parts of chromium, 3-6 parts of iron, 15-18 parts of ferro-niobium,
4-6 parts of molybdenum-iron, 1-2 parts of titanium weigh raw metal, by each raw material metal successively mass fraction be 6% aqueous hydrochloric acid solution,
30-40mi n is impregnated in the NaOH aqueous solution that mass fraction is 5%, removes oxide on surface, the metal after immersion treatment is former
Material is pulled out, is put into dehydrated alcohol, room temperature ultrasound 10-20mi n, then respectively by each raw metal be placed in electric furnace dryer into
Row baking, baking temperature are 400-420 DEG C, and baking time is 150-180mi n, removes the moisture of raw metal；
Third step, each raw metal that second step is weighed, is handled well, according to nickel → chromium → ferro-niobium → molybdenum → iron → titanium sequence
It is successively put into the processed crucible of the first step, specifically, nickel and chromium are put into the bottom of crucible, ferro-niobium is placed in the bottom of crucible
And middle part, molybdenum and iron are placed in the middle part and top of crucible, titanium is placed in the small hopper for being packed into vacuum intermediate-frequency induction melting furnace
It is interior, it carries out vacuum melting and obtains high temperature alloy ingot casting；
After 4th step, high temperature alloy ingot casting scale removal prepared by step 3, riser, high temperature alloy fine fodder is obtained；
High temperature alloy fine fodder prepared by step 4 is put into melting in the copper crucible of vacuum magnetic suspension smelting furnace and obtains height by the 5th step
Warm special material master alloy.
2. according to high-temperature special material master alloy production technology described in ingredient requirement 1, which is characterized in that the specific mistake of the first step
Journey are as follows:
1) coating spraying liquid is prepared: a calcium aluminate powder being mixed with dehydrated alcohol according to mass ratio 1:6-8, is put into ball mill
Ball milling 25-30mi n is further continued for ultrasonic disperse 20-30mi n, obtains coating spraying liquid；
2) crucible cleans: alumina crucible is put into immersion 20-25mi n in acetone, takes out, is rinsed 2-3 times with dehydrated alcohol,
Dry 3-4h is placed in 80-90 DEG C of baking oven again；
3) it sprays: coating spraying liquid being placed in spray gun, by the inner surface of coating spraying liquid even application to magnesia crucible；
4) dry: the magnesia crucible that spraying is completed being put into baking 150mi n in 85 DEG C of vacuum ovens, is then transferred to 115
22h is dried in DEG C baking oven, completes crucible spraying processing.
3. according to high-temperature special material master alloy production technology described in ingredient requirement 1, which is characterized in that true described in third step
The specific steps of empty melting are as follows:
1) 5 × 10 are evacuated to-1Pa-5×10-3Pa carries out melting, dissolved clarification end, and material temperature reaches 1580 DEG C, and raw metal exists
Fusing obtains molten steel in vacuum intermediate-frequency induction melting furnace；
2) continue to refine 26-28mi n, refining temperature is maintained at 1540-1560 DEG C, after concise, closes vacuum intermediate-frequency induction
Smelting furnace, by freezing mask in the molten steel after refining in a vacuum frequency induction melting furnace；
3) when freezing mask temperature is down to 1520 DEG C, slowly the T i in small hopper is added in crucible, 150KW function is increased to smelting furnace
Grate 5-6 times after rate further removes gas, deslagging, until aluminium alloy is poured into punching block after being completely melt again, obtains height
Temperature alloy ingot casting.
4. according to high-temperature special material master alloy production technology described in ingredient requirement 1, which is characterized in that melted described in the 5th step
Refine step are as follows:
1) 5 × 10 are evacuated to-3Pa is then charged with high-purity argon gas to 0.01Pa, and the step is in triplicate with clean vacuum chambers；
2) it is melted, fusion temperature is 1350-1450 DEG C, and soaking time is 10-20mi n；
3) it is quickly solidified in such a way that water flowing is cooling.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113584348A (en) * | 2021-06-15 | 2021-11-02 | 江苏兴达高温合金科技有限公司 | D1802017 mother alloy smelting process |
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| CN104662387A (en) * | 2012-07-27 | 2015-05-27 | 通用电气公司 | Crucible and facecoat compositions and methods for melting titanium and titanium aluminide alloys |
| CN104968451A (en) * | 2013-01-29 | 2015-10-07 | 通用电气公司 | Calcium hexaluminate-containing mold and facecoat compositions and methods for casting titanium and titanium aluminide alloys |
| CN108546834A (en) * | 2018-04-16 | 2018-09-18 | 北京科技大学 | A kind of nickel base superalloy master alloy sublimate method of smelting |
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| CN104662387A (en) * | 2012-07-27 | 2015-05-27 | 通用电气公司 | Crucible and facecoat compositions and methods for melting titanium and titanium aluminide alloys |
| CN104968451A (en) * | 2013-01-29 | 2015-10-07 | 通用电气公司 | Calcium hexaluminate-containing mold and facecoat compositions and methods for casting titanium and titanium aluminide alloys |
| CN103952578A (en) * | 2014-05-04 | 2014-07-30 | 江苏兴达高温合金科技有限公司 | K419 master alloy smelting process |
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| CN113584348A (en) * | 2021-06-15 | 2021-11-02 | 江苏兴达高温合金科技有限公司 | D1802017 mother alloy smelting process |
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