CN103498063B - A kind of yttrium oxide crucible that utilizes carries out the method for sublimate melting to high-temperature alloy return material - Google Patents
A kind of yttrium oxide crucible that utilizes carries out the method for sublimate melting to high-temperature alloy return material Download PDFInfo
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Abstract
The invention discloses a kind of yttrium oxide crucible that utilizes and the method for sublimate melting is carried out to high-temperature alloy return material, steps of the method are charging → sublimate melting → cast.The inventive method only takes melting once technique, need not repeatedly melting and repeatedly add reductor the O of returns, N content can be reduced to below 5ppm, significantly simplify processing step, reduce energy consumption.The inventive method only adds carbon and carries out deoxidation in the scope that alloying constituent allows, and does not introduce and needs the strict harmful element controlling content, eliminate the impact of harmful element alloy melt while deoxidation denitrogenation.
Description
Technical field
The present invention relates to vacuum induction melting field, more particularly, refer to that a kind of yttrium oxide crucible that utilizes carries out the method for sublimate melting to high-temperature alloy return material.
Background technology
Along with the sustainable development of the industries such as aerospace, petrochemical complex, communications and transportation and electricity power, the usage quantity of superalloy gets more and more, and also more and more high to the specification of quality of its part.In order to the over-all properties requirement of satisfied harshness, add a large amount of rare expensive strategy metal element in superalloy, comprise nickel, chromium, molybdenum, tungsten, cobalt, niobium, titanium, hafnium, rhenium etc.But, the material use efficiency of usual superalloy part is only 20% ~ 30%, some complex shape part even only have 10%, and more than 70% of superalloy turnout all exists with the form of stub bar, running channel, rising head, scrapped parts and chip the like waste and high-temperature alloy return material.The high-temperature alloy return material of annual generation nearly ten thousand tons is not fully used substantially, therefore reclaims and utilize the problem that these returns have become in the urgent need to address.
In high-temperature alloy return material, the content of principal element and virgin material alloy are close to identical, and some trace elements, particularly O, N can increase to some extent.When O residual in alloy, N content are higher, can form oxide compound and nitride inclusion thing, these inclusiones are all often that crackle produces and the vantage point of expansion, affects the creep of superalloy, creep rupture strength, serious reduction alloy plasticity and low cycle fatigue property.Therefore, the main purpose for high-temperature alloy return material sublimate seeks a kind of suitable technique, O, N content in alloy controlled in lower scope.
Melting at present for high-temperature alloy return material mostly adopts process for vacuum induction smelting, and as Chinese invention patent publication number CN101440436A, denomination of invention is " a kind of sublimate smelting technology of high-temperature alloy return material ".This patent content discloses the traditional MgO crucible of application, adopts that two deoxidation is two coldly puts technique, and O, N content in returns are reduced to below 10ppm.It adopts twice melting to add freezing technique, except adding deoxidant element carbon in fusion process, also add strong deoxidant element calcium, and calcium needs the number of times added to reach 3 ~ 6 times.Complicated technique causes smelting time long, and energy consumption increases.And calcium can affect the performance of alloy as harmful element." high temperature alloy " (first volume) the 155th page of Guo Jianting work describes " after reaching the ageing treatment of 3000h at 650 DEG C; calcium reduces the lasting of this alloy and creep fracture time and plasticity strongly; and the speed of remarkable increasing creep subordinate phase, see Fig. 5-17.Therefore, for the high-temperature component of the GH4169 alloy manufacture run time long, calcium is unfavorable as micro alloying element ".Therefore the content of calcium must accurately control, and U.S.'s aerospace material standard " trace element of nickel-base alloy foundry goods controls " (ASM2280B-2006) regulation, in nickel base superalloy foundry goods, calcium constituent can not more than 50ppm.More external factories even also have stricter requirement, as calcium constituent in GE companies ask high-temperature alloy casting can not more than 25ppm.This standard is not only applicable to novel material, is also the sublimate standard that superalloy waste must reach after sublimate process.
In addition, magnesium oxide chemical stability is poor, and magnesia crucible is at 1600 DEG C, and vacuum tightness is under 50Pa condition, just starts to decompose, and cause it to oxygen supply in alloy melt, the effect not only having influence on deoxidation also affects the process of denitrogenation.And when smelting the superalloy containing a large amount of high reactivity element, can react, cause the increase of O in alloy, N content with active element, this is also adopt complicated technique elemental gas content can not be reduced to lower level reason why.
Except magnesia crucible, the crucible material of vacuum induction melting superalloy also has and adopts aluminum oxide and calcium oxide, because lime crucible has higher chemical stability than magnesium oxide and alumina crucible, active element in refractory materials and aluminium alloy can be reduced to react and the oxygen entered in aluminium alloy, lime crucible is increasing for the situation of vacuum induction melting furnace melting in recent years, but lime crucible is easy to aquation in atmosphere, and be easy to slagging with acidic oxide.Come from the first impression in April, 2008, " high temperature alloy " (middle volume) 24-25 page of Guo Jianting work.
Summary of the invention
The object of the invention is to propose a kind of yttrium oxide crucible that utilizes and the method for sublimate melting is carried out to high-temperature alloy return material, steps of the method are charging → sublimate melting → cast.Nitrogen, the oxygen level of the high-temperature alloy return material of employing the inventive method sublimate process are all less than 5ppm.
A kind of yttrium oxide crucible that utilizes of the present invention carries out the method for sublimate melting to high-temperature alloy return material, it is characterized in that the step of this sublimate melting is:
Step 1: the ingot mould of yttrium oxide crucible and fully preheating is arranged in vacuum induction melting furnace, cleaning crucible and ingot mould, and on sprue cup, install aluminum oxide or yttrium filtering net additional;
Ingot mould: by ingot mold or graphite ingot mould, yttrium oxide shuttering after molding flask moulding, put into resistance furnace, be warming up to 600 ~ 900 DEG C, insulation 2 ~ 4h, indoor to treat that the ingot mould of abundant preheating is loaded vacuum induction furnace mold, in order to cast;
Yttrium oxide crucible and ingot mould cleaning: adopt fly-ash separator by yttrium oxide crucible and ingot mould inner wall cleaning clean;
Step 2: first add 1/3rd pretreated high-temperature alloy return material in yttrium oxide crucible after, add carbon, and then add remaining returns, closes vacuum induction melting furnace fire door;
Add carbon amounts: the carbon adding 0.01 ~ 0.2 kilogram in the returns of 100 kilograms, the actual carbon content in the carbon content scope that concrete add-on allows according to alloying constituent and returns and determining;
Step 3: vacuum induction melting furnace is vacuumized, power transmission is started after making vacuum tightness in stove reach 0.05Pa, to be now that 5 ~ 15KW heats 10 ~ 15min with small power, after increasing power to 15 ~ 25KW continues heating 5 ~ 10min, increasing power to 30 ~ 40KW, until furnace charge is all melting down;
Step 4: when being heated to charge-temperature and being 1600 DEG C ~ 2000 DEG C, vacuumize until vacuum tightness≤1Pa in stove, start refining, refining time is 10 ~ 30min;
Step 5: after refining terminates, carry out stokehold composition analysis, when not meeting the scope that revert alloy composition allows, carry out the composition adjustment of respective element, when charge composition is adjusted to alloying constituent allowed band, stop power transmission 2 ~ 5min, then give electricity with power 10 ~ 15KW, when to record charge-temperature be 1400 DEG C ~ 1500 DEG C, carry out casting.
The described yttrium oxide crucible that utilizes carries out the method for sublimate melting to high-temperature alloy return material, and after sublimate melting process, the O of returns, N content are reduced to below 5ppm.
The advantage of sublimate melting high-temperature alloy return material method of the present invention:
1. melting technology process of the present invention is simple, easy operation control, compared with published patent (publication number CN101440436A), only take melting once technique, need not repeatedly melting add freezing and repeatedly add reductor the O of returns, N content can be reduced to below 5ppm, significantly simplify processing step, reduce energy consumption.
2. the present invention only in melting early stage in the scope that alloying constituent allows, add carbon and carry out deoxidation, and in published patent (publication number CN101440436A), except adding deoxidant element carbon, also repeatedly add strong deoxidant element calcium, therefore this patent is compared with publication, while the more excellent sublimate effect of acquisition, do not introduce and need the strict harmful element calcium controlling content, while deoxidation, therefore eliminate the impact of harmful element alloy melt.
3. the yttrium oxide crucible adopted has high stability, and be difficult to react with active metal Al, Ti, Hf, Nb, Ta, Zr, Re, the B in returns and rare earth element etc. at high temperature 1600 ~ 2000 DEG C, therefore yttrium oxide crucible is adopted to carry out sublimate melting to the returns containing alloy with high activity element, decrease the possibility of yttrium oxide crucible to oxygen supply in returns, therefore the present invention can be applicable to the returns that sublimate melting process contains high level active element preferably.
4. the yttrium oxide crucible adopted can carry out sublimate melting to returns under high temperature high vacuum condition, and its use temperature can reach 1600 ~ 2000 DEG C.So high vacuum induction melting temperature contributes to the activity improving carbon, impels the volatilization with low melting point element that removes of the elemental gas such as oxygen, nitrogen, thus purification aluminium alloy, and eliminate Structure Heredity by high-temperature fusant process.
5. by melting technology of the present invention, not only effectively can realize the super low loading of high-temperature alloy return material O, N element after sublimate, and there is de-C effect preferably, after sublimate process, in returns, C content is all in the allowed band of the former alloying constituent of returns.
6. the superalloy obtained after adopting yttrium oxide crucible and melting technology disclosed by the invention to carry out sublimate process to returns, the level of the alloy virgin material that can reach a high temperature completely, can be aircraft industry and provides high-quality superalloy mother alloy.Improve the utilization ratio of resource, as strategic resources such as nickel, cobalt, niobium, chromium, molybdenum, tungsten, titanium, hafnium, rheniums.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
In the present invention, to the melting application yttrium oxide crucible of high-temperature alloy return material, and vacuum induction melting method is adopted.Described high-temperature alloy return material can be stub bar, running channel, rising head, scrapped parts and chip waste material.
A kind of yttrium oxide crucible that utilizes of the present invention carries out the method for sublimate melting to high-temperature alloy return material, steps of the method are charging → sublimate melting → casting.Particularly:
Step 1: the ingot mould of yttrium oxide crucible and fully preheating is arranged in vacuum induction melting furnace, cleaning crucible and ingot mould, and on sprue cup, install aluminum oxide or yttrium filtering net additional;
Ingot mould: by ingot mold or graphite ingot mould, yttrium oxide shuttering after molding flask moulding, puts into resistance furnace when being warming up to 600 ~ 900 DEG C, insulation 2 ~ 4h, indoor to treat that the ingot mould of abundant preheating is loaded vacuum induction furnace mold, in order to cast; Yttrium oxide crucible and ingot mould cleaning: adopt fly-ash separator by yttrium oxide crucible and ingot mould inner wall cleaning clean;
Step 2: first add 1/3rd pretreated high-temperature alloy return material in yttrium oxide crucible after, add carbon, then add remaining returns, closes vacuum induction melting furnace fire door;
Returns pre-treatment: after returns carry out blast or polishing, utilize industrial ultrasonic cleaning agent or acetone under frequency is the condition of 30 ~ 50KHz, ultrasonic cleaning 5 ~ 10min, be put in after cleaning in baking oven and dry 10 ~ 30min under 80 ~ 120 DEG C of conditions, obtain pretreated high-temperature alloy return material.
Add carbon amounts: the carbon adding 0.01 ~ 0.2 kilogram in the returns of 100 kilograms, the actual carbon content in the carbon content scope that concrete add-on allows according to alloying constituent and returns and determining, the total amount that add-on and former content are added is at the Near The Upper Limit of alloying constituent; Described carbon adds with carbon or returns-carbon master alloy form;
Step 3: vacuum induction melting furnace is vacuumized, power transmission is started after making vacuum tightness in stove reach 0.05Pa, will be now that 5 ~ 15KW heats 10 ~ 15min with small power, after increasing power to 15 ~ 25KW continues heating 5 ~ 10min, increasing power to 30 ~ 40KW be until furnace charge is all melting down;
Step 4: when being heated to charge-temperature and being 1600 DEG C ~ 2000 DEG C, vacuumize until vacuum tightness≤1Pa in stove, start refining, refining time is 10 ~ 30min;
Step 5: after refining terminates, carry out stokehold composition analysis, when not meeting the scope that revert alloy composition allows, carry out the composition adjustment of respective element, when charge composition is adjusted to alloying constituent allowed band, stop power transmission 3 ~ 5min, then give electricity with power 10 ~ 15KW, when to record charge-temperature be 1400 DEG C ~ 1500 DEG C, carry out casting.
In the present invention, after step 4 refining, with published sublimate Technical comparing (patent publication No. CN101440436A), repeatedly melting-freezing-melting-freezing treatment need not be carried out, also final deoxygenation element calcium need not repeatedly be added in the process that alloy melts again after a freezing treatment, significantly simplify processing step, reduce energy consumption.And utilize technique of the present invention, effectively realize denitrogenation and deoxidation, while the more excellent sublimate effect of acquisition, do not introduce and need the strict harmful element calcium controlling content, while deoxidation, therefore eliminate the impact of harmful element alloy melt.
Melting high-temperature alloy return material of the present invention is mainly the stub bar, running channel, rising head, scrapped parts etc. that produce in production process, and the alloy nomenclature of concrete high-temperature alloy return material is shown in Table 1.
Table 1 is O, N content experimental data after the melting of sublimate technique
In the present invention, the O, the N content that contain in alloy before and after the process of returns sublimate, adopt noble gas pulsed infrared thermal conductivity method (IGI, LECOTC-436, ASTME1119-2011 are with reference to QB-QT-34-1997) to measure.
embodiment 1
Utilize the GH4169 alloy rising head returns of yttrium oxide crucible to 25Kg to carry out the method for sublimate melting, steps of the method are charging → sublimate melting → casting.
The mass percent of described GH4169 revert is: C is 0.03%, Cr is 18.3%, Ni is 52.7%, Mo is 3.18%, Al is 0.45%, Ti is 1.02%, Nb is 5.26%, Fe is surplus.
Concrete sublimate melting step is:
Step 1: the ingot mould of yttrium oxide crucible and fully preheating is arranged in vacuum induction melting furnace, cleaning crucible and ingot mould, and on sprue cup, install yttrium filtering net additional;
Ingot mould: ingot mold is put into resistance furnace and be warming up to 900 DEG C, insulation 4h, to treat that the ingot mould of abundant preheating is loaded vacuum induction furnace mold indoor to be poured into a mould;
Yttrium oxide crucible and ingot mould cleaning: adopt fly-ash separator by yttrium oxide crucible and ingot mould inner wall cleaning clean;
Step 2: first add 1/3rd pretreated high-temperature alloy return material in yttrium oxide crucible after, add carbon, then add remaining returns, closes vacuum induction melting furnace fire door;
Returns pre-treatment: after returns carry out blast or polishing, utilize industrial ultrasonic cleaning agent under the condition of frequency for 30KHz, ultrasonic cleaning 10min, is put in after cleaning in baking oven and dries 20min under 120 DEG C of condition, obtain pretreated high-temperature alloy return material;
Add carbon amounts: the carbon adding 0.0075 kilogram in the returns of 25 kilograms;
Step 3: vacuum induction melting furnace is vacuumized, starting power transmission after making vacuum tightness in stove reach 0.05Pa, will be now after 10KW heats 10min with small power, after increasing power continues heating 5min to 25KW, increasing power is to 35KW, until furnace charge is all melting down;
Step 4: when being heated to charge-temperature and being 1800 DEG C, vacuumizes until vacuum tightness is 0.1Pa in stove, and start refining, refining time is 15min;
In the present invention, the refining process of this step keeps high temperature high vacuum, and the activity contributing to strengthening carbon is beneficial to deoxidation, promotes decomposition and the eliminating of inclusion simultaneously.
Step 5: after refining terminates, carries out stokehold composition analysis, adds Al, Ti element, when charge composition is adjusted to alloying constituent allowed band, stop power transmission 4min, then give electricity with power 10KW, when to record charge-temperature be 1400 DEG C, carry out casting.
Analytical test containing oxygen, nitrogen quantity is carried out to the GH4169 alloy of embodiment 1 casting.Test result shows that N, O content of high-temperature alloy return material is reduced to 2ppm and 4ppm after sublimate process by sublimate 41ppm, 16ppm before treatment respectively, significantly improves the sublimate effect of superalloy.Adopt N, O constituent content of GH4169 before and after sublimate melting of the present invention in table 1.
The vacuum induction melting furnace adopted in this example 1 is that Jinzhou Electric Furnace Co. Ltd. produces, and model is ZGJL0.025-100-2.5R.For meeting experiment condition of the present invention, yttrium oxide crucible is adopted to carry out the melting of returns.
embodiment 2
Utilize the K424 alloy running channel returns of yttrium oxide crucible to 10Kg to carry out the method for sublimate melting, steps of the method are charging → sublimate melting → casting.
The mass percent of described K424 revert is: C is 0.15%, Cr is 9.7%, Co is 13.6%, W is 1.5%, Mo is 3.1%, Al is 5.2%, Ti is 4.4%, Nb is 0.8%, V is 0.7%, B is 0.015%, Zr is 0.02%, Ce is 0.02%, Ni is surplus.
Step 1: the ingot mould of yttrium oxide crucible and fully preheating is arranged in vacuum induction melting furnace, cleaning crucible and ingot mould, and on sprue cup, install yttrium filtering net additional;
Ingot mould: graphite formwork is put into molding flask moulding, then puts into resistance furnace and is warming up to 600 DEG C of insulation 2h, to treat that the ingot mould of abundant preheating is loaded vacuum induction furnace mold indoor to be poured into a mould;
Yttrium oxide crucible and ingot mould cleaning: adopt fly-ash separator by yttrium oxide crucible and ingot mould inner wall cleaning clean;
Step 2: first add 1/3rd pretreated high-temperature alloy return material in yttrium oxide crucible after, add carbon, then add remaining returns, closes vacuum induction melting furnace fire door;
Returns pre-treatment: after returns carry out blast or polishing, with acetone be under the condition of 40KHz in frequency, ultrasonic cleaning 5min, is put in after cleaning in baking oven and dries 30min under 80 DEG C of condition, obtain pretreated high-temperature alloy return material;
Add carbon amounts: the carbon adding 0.005 kilogram in the returns of 10 kilograms; Described carbon adds with carbon-returns master alloy form;
Step 3: vacuum induction melting furnace is vacuumized, starting power transmission after making vacuum tightness in stove reach 0.05Pa, will be now that 6KW heats 10min with small power, after increasing power continues heating 10min to 15KW, increasing power is to 30KW, until furnace charge is all melting down;
Step 4: when being heated to start refining when charge-temperature is 2000 DEG C, until vacuum tightness is 1Pa in stove, refining time is 10min;
In the present invention, the refining process of this step keeps high temperature high vacuum, and the activity contributing to strengthening carbon is beneficial to deoxidation, promotes decomposition and the eliminating of inclusion simultaneously.
Step 5: after refining terminates, carries out stokehold composition analysis, adds Al, Ti, Ce, B element, when charge composition is adjusted to alloying constituent allowed band, stop power transmission 4min, then give electricity with power 10KW, when to record charge-temperature be 1500 DEG C, carry out casting.
Analytical test containing oxygen, nitrogen quantity is carried out to the K424 alloy of embodiment 2 casting.Test result shows that N, O content of high-temperature alloy return material is reduced to 2ppm and 3ppm after sublimate process by sublimate 57ppm, 19ppm before treatment respectively, significantly improves the sublimate effect of superalloy.Before and after sublimate melting, N, O constituent content of K424 is in table 1.
Adopt the DZ17G alloy of processing step to 10Kg of embodiment 2, DZ125 alloy and K417 alloy to carry out sublimate process, N, O constituent content before and after its melting is in table 1.
embodiment 3
Utilize yttrium oxide crucible to the Ni of 25Kg
3al alloy waste foundry goods returns carry out the method for sublimate melting, steps of the method are charging → sublimate melting → casting.
Described Ni
3the mass percent of Al revert is: Mo is 14.3%, Al is 7.8%, Ni is surplus.
Step 1: the ingot mould of yttrium oxide crucible and fully preheating is arranged in vacuum induction melting furnace, cleaning crucible and ingot mould, and on sprue cup, install alumina-ceramic filtering net additional;
Ingot mould: yttrium oxide shuttering is put into molding flask moulding, then puts into resistance furnace and is warming up to 900 DEG C of insulation 2h, to treat that the ingot mould of abundant preheating is loaded vacuum induction furnace mold indoor to be poured into a mould;
Yttrium oxide crucible and ingot mould cleaning: adopt fly-ash separator by yttrium oxide crucible and ingot mould inner wall cleaning clean;
Step 2: first add 1/3rd pretreated high-temperature alloy return material in yttrium oxide crucible after, add carbon, then add remaining returns, closes vacuum induction melting furnace fire door;
Returns pre-treatment: after returns carry out blast or polishing, utilize industrial ultrasonic cleaning agent under the condition of frequency for 50KHz, ultrasonic cleaning 5min, is put in after cleaning in baking oven and dries 20min under 100 DEG C of condition, obtain pretreated high-temperature alloy return material.
Add carbon amounts: the carbon adding 0.005 kilogram in the returns of 25 kilograms;
Step 3: vacuum induction melting furnace is vacuumized, start power transmission after making vacuum tightness in stove reach 0.05Pa, will be now after 12KW heats 10min with small power, increasing power continues heating 15min to 25KW, increasing power is to 35KW, until furnace charge is all melting down;
Step 4: when being heated to start refining when charge-temperature is 1900 DEG C, vacuumizes until vacuum tightness is 1Pa in stove, and start refining, refining time is 15min;
In the present invention, the refining process of this step keeps high temperature high vacuum, and the activity contributing to strengthening carbon is beneficial to deoxidation, promotes decomposition and the eliminating of inclusion simultaneously.
Step 5: after refining terminates, carries out stokehold composition analysis, adds Al element, when charge composition is adjusted to alloying constituent allowed band, stops power transmission 3min, then gives electricity with power 10KW, when to record charge-temperature be 1500 DEG C, carry out casting.
To the Ni of embodiment 3 casting
3al alloy carries out the analytical test containing oxygen, nitrogen quantity.Test result shows that N, O content of high-temperature alloy return material is reduced to 2ppm and 3ppm after sublimate process by sublimate 33ppm, 18ppm before treatment respectively, significantly improves the sublimate effect of superalloy.Ni before and after sublimate melting
3n, O constituent content of Al is in table 1.
Show through above-described embodiment result, the present invention utilizes yttrium oxide crucible to carry out sublimate melting to high-temperature alloy return material, high-temperature alloy return material can be smelted in batches, achieve the target of high-temperature alloy return material super low loading of O, N after sublimate is smelted, meet technical requirement completely, improve the utilization ratio of resource.
Melting technology process of the present invention is simple, and easy operation control, only takes melting once technique, need not repeatedly melting add freezing and repeatedly add reductor and the O of returns, N content can be reduced to below 5ppm, significantly simplify processing step, reduce energy consumption.
The present invention only in melting early stage in the scope that alloying constituent allows, add carbon and carry out deoxidation, avoid deoxidation introduce simultaneously that alloy melt has an impact, need the strict harmful element controlling content.
In the embodiment of the present invention 2, technique of the present invention is adopted to carry out sublimate melting to DZ17G, DZ125 and K417 revert, in superalloy after melting, O and N content be not all more than 4ppm, lower than in patent publication No. CN101440436A to the result of high-temperature alloy return material process.In addition, adopt method of the present invention, while the more excellent sublimate effect of acquisition, do not introduce and need the strict harmful element calcium controlling content, while deoxidation, therefore eliminate the impact of harmful element alloy melt.
Calcium oxide, magnesium oxide and alumina crucible that the yttrium oxide crucible that the present invention adopts is commonly used than superalloy melting have higher stability, at high temperature be difficult to react with active metal Al, Ti, Hf, Nb, Ta, Zr, Re, the B in returns and rare earth element etc., therefore yttrium oxide crucible is adopted to carry out sublimate melting to the returns containing alloy with high activity element, decrease the possibility of yttrium oxide crucible to oxygen supply in returns, there is result of use more better than other conventional crucible.
The yttrium oxide crucible adopted can carry out sublimate melting to returns under up to the condition of 1600 ~ 2000 DEG C, so high vacuum induction melting temperature contributes to the activity improving carbon, impel the volatilization with low melting point element that removes of the elemental gas such as oxygen, nitrogen, thus purification aluminium alloy, and eliminate Structure Heredity by ultrahigh-temperature melt treatment.
By sublimate melting technology of the present invention, not only effectively can realize the super low loading of high-temperature alloy return material O, N element after sublimate, and there is de-C effect preferably, after sublimate process, in returns, C content is all in the allowed band of the former alloying constituent of returns.
Claims (2)
1. utilize yttrium oxide crucible to carry out a method for sublimate melting to high-temperature alloy return material, sublimate melting process can be carried out to high-temperature alloy return material; Described high-temperature alloy return material is stub bar, running channel, rising head, scrapped parts or chip waste material; The step of this sublimate melting is charging → sublimate melting → casting:
Wherein, charging includes, step 1: be arranged in vacuum induction melting furnace by the ingot mould of yttrium oxide crucible and fully preheating, cleaning crucible and ingot mould, and on sprue cup, install aluminum oxide or yttrium filtering net additional;
Yttrium oxide crucible and ingot mould cleaning: adopt fly-ash separator by yttrium oxide crucible and ingot mould inner wall cleaning clean;
Step 2: first add 1/3rd pretreated high-temperature alloy return material in yttrium oxide crucible after, add carbon, and then add remaining returns, closes vacuum induction melting furnace fire door;
Wherein, sublimate melting includes, step 3: vacuum induction melting;
Step 4: refining;
Wherein, casting is step 5;
It is characterized in that:
In step 1,
Described ingot mould is by ingot mold or graphite ingot mould, yttrium oxide shuttering after molding flask moulding, puts into resistance furnace, is warming up to 600 ~ 900 DEG C, insulation 2 ~ 4h, indoor to treat that the ingot mould of abundant preheating is loaded vacuum induction furnace mold, in order to cast;
In step 2,
Described returns are GH4169 alloy, K424 alloy, DZ17G alloy, DZ125 alloy, K417 alloy or Ni
3al alloy;
Add carbon amounts: the carbon adding 0.01 ~ 0.2 kilogram in the returns of 100 kilograms, the actual carbon content in the carbon content scope that concrete add-on allows according to alloying constituent and returns and determining; Adding of carbon is added with carbon or returns-carbon master alloy form;
To the pre-treatment of high-temperature alloy return material be, after adopting common process to carry out blast or grinding process to returns, recycle industrial ultrasonic cleaning agent or acetone under frequency is the condition of 30 ~ 50KHz, ultrasonic cleaning 5 ~ 10min, be put in after cleaning in baking oven and dry 10 ~ 30min under 80 ~ 120 DEG C of conditions, obtain pretreated high-temperature alloy return material;
Step 3: vacuum induction melting furnace is vacuumized, power transmission is started after making vacuum tightness in stove reach 0.05Pa, to be now that 5 ~ 15KW heats 10 ~ 15min with small power, after increasing power to 15 ~ 25KW continues heating 5 ~ 10min, increasing power to 30 ~ 40KW, until furnace charge is all melting down;
Step 4: when being heated to charge-temperature and being 1600 DEG C ~ 2000 DEG C, vacuumize until vacuum tightness≤1Pa in stove, start refining, refining time is 10 ~ 30min;
Step 5: after refining terminates, carry out stokehold composition analysis, when not meeting the scope that revert alloy composition allows, carry out the composition adjustment of respective element, when charge composition is adjusted to alloying constituent allowed band, stop power transmission 2 ~ 5min, then give electricity with power 10 ~ 15KW, when to record charge-temperature be 1400 DEG C ~ 1500 DEG C, carry out casting;
After sublimate melting process, the O of returns, N content are reduced to below 5ppm.
2. the yttrium oxide crucible that utilizes according to claim 1 carries out the method for sublimate melting to high-temperature alloy return material, it is characterized in that: yttrium oxide crucible use temperature reaches 1600 ~ 2000 DEG C, the activity of carbon can be improved, be beneficial to deoxidation denitrogenation purification aluminium alloy.
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| CN104046820B (en) * | 2014-06-06 | 2016-06-29 | 南京理工大学 | In a kind of fusion process, substep is multi-form adds the method that carbon smelts nickel base superalloy |
| CN106756141B (en) * | 2016-12-28 | 2018-08-28 | 北京有色金属研究总院 | The gas shield solid-liquid mixing coagulation system of Cu-Nb in-situ composites |
| CN107311658A (en) * | 2017-06-12 | 2017-11-03 | 上海大学 | Y2O3The preparation method of crucible and the application in high activity metal melting |
| CN110106374A (en) * | 2018-12-22 | 2019-08-09 | 北京航空航天大学 | A method of high-purity high temperature alloy is prepared using material is returned |
| CN117253568B (en) * | 2023-11-15 | 2024-01-26 | 沈阳恒泰鑫源精铸耐材有限公司 | Coating process optimization method and system for preparing yttrium oxide crucible |
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| CN101498549A (en) * | 2009-03-16 | 2009-08-05 | 北京航空航天大学 | Crucible with Y2O3 anti-corrosion coating and method for producing Y2O3 anti-corrosion coating by slip-casting shaping process |
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| CN1552928A (en) * | 2003-05-31 | 2004-12-08 | 中国科学院金属研究所 | Ultrapure smelting process for nickel-base high-temperature alloy |
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