CN112304083B - Rapid pretreatment method of formed crucible for vacuum smelting - Google Patents

Rapid pretreatment method of formed crucible for vacuum smelting Download PDF

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CN112304083B
CN112304083B CN202011242250.8A CN202011242250A CN112304083B CN 112304083 B CN112304083 B CN 112304083B CN 202011242250 A CN202011242250 A CN 202011242250A CN 112304083 B CN112304083 B CN 112304083B
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crucible
vacuum
furnace
basket
induction
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CN112304083A (en
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谢君
侯桂臣
盛乃成
周亦胄
张典
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Liaoning Hongyin Metal Co ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/04—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated adapted for treating the charge in vacuum or special atmosphere
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/04—Refining by applying a vacuum
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
    • F27B5/14—Arrangements of heating devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D11/00—Arrangement of elements for electric heating in or on furnaces
    • F27D11/06—Induction heating, i.e. in which the material being heated, or its container or elements embodied therein, form the secondary of a transformer
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Crucibles And Fluidized-Bed Furnaces (AREA)

Abstract

The invention relates to the field of alloy vacuum smelting, in particular to a rapid pretreatment method of a forming crucible for vacuum smelting. The crucible basket is formulated according to the crucible specification, the crucible sleeve with the inner cavity size being consistent with the crucible overall dimension is formed by using a refractory material in the crucible basket in a striking mode and is sintered into a crucible sleeve with the inner cavity size being consistent with the crucible overall dimension, a spare crucible is placed into an induction coil of the crucible pretreatment vacuum furnace together after being placed into the crucible sleeve, a graphite rod is placed into the crucible, the induction coils of the crucible basket and the crucible pretreatment vacuum furnace are determined according to the actual production demand, the furnace is closed and vacuumized, the graphite rod starts to be heated in an induction mode through power transmission for baking, and after the baking is finished, a tool is used for directly placing the processed crucible into the crucible sleeve with the same specification in the vacuum induction smelting furnace for use. The invention can improve the production efficiency, is quick and convenient, has the same crucible treatment process as the treatment process in the vacuum induction melting furnace, can effectively prevent the crucible surface from being oxidized, reduces the pollution probability of alloy liquid, and improves the quality of alloy and castings.

Description

Rapid pretreatment method of formed crucible for vacuum smelting
Technical Field
The invention relates to the field of alloy vacuum smelting, in particular to a rapid pretreatment method of a forming crucible for vacuum smelting.
Background
At present, the pretreatment of a formed crucible for vacuum smelting is generally divided into pretreatment in a vacuum furnace and pretreatment outside the vacuum furnace under normal pressure, the pretreatment in the vacuum furnace occupies the normal production time of the vacuum furnace, only one crucible can be pretreated at a time, the production efficiency is seriously influenced, the cost is higher, the pretreatment outside the vacuum furnace is generally carried out under normal pressure, oxides are attached to the surface of the crucible during high-temperature baking, the alloy adopting vacuum smelting generally has higher requirements on the content of gas impurities, the oxides attached to the surface of the crucible are unfavorable for the product quality, and the two modes require a series of complicated processes of crucible dismantling, new crucible positioning, sand filling, sealing and the like during the forging of the crucible, so that the production efficiency is low.
Disclosure of Invention
In view of this, the main object of the present invention is to provide a method for rapidly pretreating formed crucibles for vacuum melting, which can simultaneously pretreat more than two crucibles at a time, not only can improve the production efficiency, but also can prevent the surfaces of the crucibles from being oxidized, reduce the pollution probability of the alloy liquid, and improve the alloy quality.
The technical scheme of the invention is as follows:
a rapid pretreatment method of a forming crucible for vacuum smelting comprises the following steps:
(1) a crucible basket is made according to the specification of the crucible, and a crucible sleeve with the inner cavity size consistent with the overall size of the crucible is made and sintered in the crucible basket by using refractory materials;
(2) after the spare crucible is placed into the crucible sleeve, the spare crucible is placed into the inner side of an induction coil of a crucible pretreatment vacuum furnace together, and a graphite rod is placed into the crucible;
(3) closing the crucible to pretreat the furnace body of the vacuum furnace, vacuumizing, starting power transmission to inductively heat the graphite rod, baking the crucible by low-power transmission at first, removing moisture and gas adsorbed on the surface, and baking the crucible by high-power transmission to thoroughly remove the gas in the crucible;
(4) after baking, directly putting the crucible into a crucible sleeve with the same specification in a vacuum induction melting furnace by using a tool for use;
(5) and putting other pretreated spare crucibles into a vacuum environment for storage and spare use.
The rapid pretreatment method of the formed crucible for vacuum smelting comprises the step (1), wherein a crucible basket is a container for making a crucible sleeve aiming at the crucible, the crucible basket is made of a non-ferromagnetic material, and the inner diameter of the crucible basket is 40-60 mm larger than the outer diameter of the crucible.
The rapid pretreatment method of the forming crucible for vacuum smelting comprises the step (1), wherein the refractory material is a mixture of more than two of aluminum oxide, magnesium oxide, calcium oxide and silicon oxide.
In the step (2), the crucible pretreatment vacuum furnace is equipment which is provided with more than two induction coils in a furnace body and is independently used for heating in a vacuum environment.
In the step (2), the graphite rod is a cylindrical graphite rod with the outer diameter being 20-30 mm smaller than the inner diameter of the crucible, and the length of the graphite rod is 1.1-1.3 times of the height of the crucible.
According to the rapid pretreatment method of the forming crucible for vacuum smelting, in the step (3), the vacuum degree is reduced to be below 100Pa by vacuumizing.
In the step (3), the low-power transmission roasting crucible is heated for 1-3 hours by 10% -30% of the rated power of the used equipment.
According to the rapid pretreatment method of the formed crucible for vacuum smelting, in the step (3), the high-power transmission baking crucible is heated for 10-30 min by using 60% -80% of rated power of equipment.
The rapid pretreatment method of the formed crucible for vacuum smelting comprises the step (4), wherein the tool is a crucible taking and placing tool which is placed in the crucible, props against the inner wall of the crucible in an expanding mode and is provided with a long handle.
The rapid pretreatment method of the forming crucible for vacuum smelting comprises the step (5), wherein the vacuum environment is a vacuum tank or vacuum furnace equipment, and the vacuum degree is not more than 1000 Pa.
The design idea of the invention is as follows: demolish to traditional vacuum melting crucible when using, beat system and pretreatment process inefficiency, the not high scheduling problem of metallurgical quality, adopt crucible basket technique to replace directly to beat the system crucible in induction coil, realize the quick replacement of crucible in the vacuum furnace, adopt crucible cover technique to replace traditional crucible and demolish this process of system crucible again after demolising, exempt from to demolish when realizing the crucible and beat the system again, and combine special crucible vacuum pretreatment equipment in batches, thoroughly solve the inefficiency of traditional vacuum melting crucible when using, the not high scheduling problem of metallurgical quality, improve the production efficiency and the metallurgical quality of the relevant product of enterprise by a wide margin.
The invention has the advantages and beneficial effects that:
the invention adopts the crucible pretreatment under the vacuum condition outside the furnace, which has more use value for the calcium oxide crucible which is easy to deliquesce under the normal pressure, and adopts the mode of combining the crucible basket and the crucible sleeve, thereby saving the time of casting the crucible shape each time and the trouble of integral transportation, and simultaneously pretreating more than two crucibles at one time, not only greatly improving the production efficiency, being fast and convenient, meeting the requirement of industrialized production, but also preventing the surface of the crucible from being oxidized, improving the metallurgical quality of alloy ingots or castings and reducing the pollution probability of alloy liquid.
Drawings
FIG. 1 is a crucible baking power-time curve in example 1.
FIG. 2 is a view showing a state in which dross is generated in a crucible in example 1.
FIG. 3 is a view showing a state where dross is pretreated at normal pressure in a crucible according to example 1.
FIG. 4 is a crucible baking power-time curve in example 2.
FIG. 5 is a view showing a state in which dross is generated in a crucible in example 2.
FIG. 6 is a view showing a state where dross is pretreated at normal pressure in a crucible according to example 2.
FIG. 7 is a schematic view of the structure of a crucible pretreatment vacuum furnace. In the figure, 1 furnace body, 2 induction coils, 3 cooling water inlets and 4 cooling water outlets.
FIG. 8 is a schematic view of the combination structure of the crucible basket, the crucible cover and the crucible. Wherein, (a) a front view; (b) a top view; in the figure, 5 crucible baskets, 6 crucible sleeves and 7 crucibles.
Detailed Description
As shown in fig. 7-8, six induction coils 2 are uniformly distributed on the inner side of a furnace body 1 of a crucible pretreatment vacuum furnace, and a cooling water inlet 3, a cooling water outlet 4, a vacuum pipeline and a power supply are respectively arranged on the outer side of the furnace body 1, and the crucible pretreatment vacuum furnace has the following specific structure:
the vacuum pipeline is communicated with the inner cavity of the furnace body 1 and is used for vacuumizing the furnace body 1; when the crucible heating device is used, the combined structure of the crucible basket 5, the crucible sleeve 6 and the crucible 7 is arranged on the inner side of the induction coil 2, the graphite rod is placed in the crucible 7, the induction coil 2 is connected with a power supply through a circuit, and the induction coil 2 is used for carrying out induction heating on the graphite rod. The induction coil 2 is wound by a hollow copper pipe to form a spiral barrel, the cooling water inlet 3 and the cooling water outlet 4 are respectively communicated with the hollow copper pipe of the induction coil 2 through pipelines, and the hollow copper pipe of the induction coil 2 is internally communicated with cooling water.
In the specific implementation process, the rapid pretreatment method of the forming crucible for vacuum smelting comprises the following steps:
(1) a crucible basket 5 with a proper size is made according to the specification of a crucible 7, a crucible sleeve 6 with the inner cavity size consistent with the external dimension of the crucible is made and sintered in the crucible basket 5 by using refractory materials, and the crucible sleeve 6 can be recycled for a long time;
(2) after a spare crucible 7 is placed into a crucible sleeve 6, the combined structure of the crucible basket 5, the crucible sleeve 6 and the crucible 7 is placed into the inner side of an induction coil 2 of a crucible pretreatment vacuum furnace, a graphite rod with a proper size is placed into the crucible 7, and the number of the crucible basket 5 and the number of the induction coils 2 of the crucible pretreatment vacuum furnace are determined according to actual production requirements;
(3) closing the furnace, sealing the furnace body 1, vacuumizing, starting to inductively heat the graphite rod by power transmission, firstly baking the crucible 7 by low-power transmission to remove moisture and gas adsorbed on the surface, and then baking the crucible 7 by high-power transmission to thoroughly remove the gas adsorbed on the crucible 7;
(4) after baking, the processed crucible 7 can be directly placed into a crucible sleeve with the same specification in a vacuum induction melting furnace by using a tool for use;
(5) and putting the other pretreated spare crucibles 7 into a vacuum environment for storage and spare use.
The present invention will be explained in further detail below by way of examples and figures.
Example 1
As shown in fig. 7 to 8, in the present embodiment, 6 crucibles 7 used in a 10kg vacuum induction melting furnace are pretreated, specifically as follows:
(1) 6 spare crucibles 7 are placed in a crucible cover 6 which is formed by beating using a crucible basket 5 outside the furnace, wherein: the crucible 7 used in the 10kg vacuum induction melting furnace is an isostatic compaction magnesia crucible, and the size of the crucible is 130mm of outer diameter, 105mm of inner diameter and 215mm of height; the crucible basket 5 is made of a stainless steel plate with the diameter of 170mm multiplied by 245mm in height and the thickness of about 1mm and without magnetic conductivity; the crucible cover 6 is formed by mixing alumina (mass fraction 85%) and magnesia (mass fraction 15%), beating and sintering;
(2) simultaneously placing 6 manufactured crucibles 7 into induction coils 2 corresponding to the crucible pretreatment vacuum furnace, and placing cylindrical graphite rods with the size of 85mm in diameter and 260mm in height into each crucible 7;
(3) closing the furnace, sealing the furnace body 1, vacuumizing to 50Pa, and starting to heat the graphite rod by power transmission induction: firstly, baking the crucible for 2 hours by using 10KW power transmission, then baking the crucible for 15 minutes by using 35KW power transmission, powering off and cooling, storing the pretreated crucible in a crucible pretreatment vacuum furnace for later use, and showing a crucible baking power-time curve in figure 1.
Putting the pretreated crucible into a vacuum induction melting furnace, putting metallic nickel into the crucible for washing the furnace, observing the state of liquid level scum after the metallic nickel is completely melted, taking a picture for recording, sampling in a metallic nickel ingot after washing the furnace to detect the content of harmful gas oxygen and nitrogen, and comparing with a furnace washing result of the crucible processed under normal pressure, wherein the results are as follows:
Figure BDA0002768805270000041
Figure BDA0002768805270000051
as can be seen from the comparison results, the crucible pretreated under normal pressure can not completely remove the gas adsorbed on the crucible, a large amount of scum (area fraction is about 29%) exists around the liquid level during furnace washing, and the O, N content is relatively high, particularly the O content is about 3 times higher than that of the corresponding result of the embodiment, which is very unfavorable for the purity of alloy or casting by vacuum smelting, and the crucible pretreated by the embodiment provides a strong guarantee for obtaining high-purity alloy or casting.
Example 2
As shown in fig. 7 to 8, in the present embodiment, the pretreatment is performed on 6 crucibles 7 used in a 25kg vacuum induction melting furnace, and the specific process is as follows:
(1) 6 spare crucibles 7 are placed inside a crucible cover 6, which is made by using a crucible basket 5 outside the furnace, wherein: the crucible 7 used in the 25kg vacuum induction melting furnace is an isostatic compaction magnesia crucible, and the size of the crucible is 180mm in outside diameter, 145mm in inside diameter and 315mm in height; the crucible basket 5 is 230mm in diameter and 360mm in height, and is made of a non-magnetic stainless steel plate with the thickness of about 1 mm; the crucible cover 6 is formed by mixing alumina (mass fraction 85%) and magnesia (mass fraction 15%), beating and sintering;
(2) simultaneously placing 6 manufactured crucibles 7 into induction coils 2 corresponding to the crucible pretreatment vacuum furnace, and placing cylindrical graphite rods with the size of 120mm in diameter and 350mm in height into each crucible 7;
(3) closing the furnace, sealing the furnace body 1, vacuumizing to 50Pa, and starting to heat the graphite rod by power transmission induction: firstly, baking the crucible for 3 hours by using 20KW power transmission, then baking the crucible for 25 minutes by using 80KW power transmission, powering off and cooling, storing the pretreated crucible in a crucible pretreatment vacuum furnace for later use, and showing a crucible baking power-time curve in figure 4.
Crucible baking power-time curve:
the pretreated crucible is placed into a vacuum induction melting furnace, metal nickel is placed into the crucible for furnace washing, after the metal nickel is completely melted, the state of liquid level scum is observed, photographing and recording are carried out, after the furnace washing, the content of harmful gas oxygen and nitrogen is detected in a metal nickel ingot, and compared with the furnace washing result of the crucible processed under normal pressure, the results are as follows:
Figure BDA0002768805270000052
Figure BDA0002768805270000061
as can be seen from the comparison results, the crucible pretreated under normal pressure can not completely remove the gas adsorbed on the crucible, a large amount of scum (about 30 percent of area) exists around the liquid level during furnace washing, the O, N content is relatively high, and particularly the O content is more than 2 times higher than the corresponding result of the embodiment, which is very unfavorable for the purity of alloy or casting smelted by vacuum, while the crucible pretreated by the embodiment provides a strong guarantee for obtaining high-purity alloy or casting.
The results of the embodiment and the comparative example show that the invention can simultaneously pretreat more than two crucibles at one time under the vacuum condition, is suitable for integrally forming crucibles with the capacity of 50kg and below, has more use value for calcium oxide crucibles which are easy to deliquesce under normal pressure, and adopts the mode of combining the crucible basket and the crucible sleeve, thereby saving the time of forging the crucible shape each time and the trouble of integrally carrying.

Claims (6)

1. A rapid pretreatment method of a forming crucible for vacuum smelting is characterized by comprising the following steps:
(1) a crucible basket is made according to the specification of the crucible, and a crucible sleeve with the inner cavity size consistent with the overall size of the crucible is made and sintered in the crucible basket by using refractory materials;
(2) after the spare crucible is placed into the crucible sleeve, the spare crucible is placed into the inner side of an induction coil of a crucible pretreatment vacuum furnace together, and a graphite rod is placed into the crucible;
(3) closing the furnace, sealing the crucible, pretreating the furnace body of the vacuum furnace, vacuumizing, supplying power, starting to inductively heat the graphite rod, firstly supplying power at low power, baking the crucible, removing moisture and gas adsorbed on the surface, then supplying power at high power, baking the crucible, and completely removing the gas in the crucible;
(4) after baking, directly putting the crucible into a crucible sleeve with the same specification in a vacuum induction melting furnace by using a tool for use;
(5) putting the pretreated other spare crucibles into a vacuum environment for storage and standby;
in the step (1), the crucible basket is a container for making a crucible sleeve aiming at the crucible, the crucible basket is made of a stainless steel plate without magnetic conductivity, and the inner diameter of the crucible basket is 40-60 mm larger than the outer diameter of the crucible;
in the step (1), the refractory material is a mixture of more than two of aluminum oxide, magnesium oxide, calcium oxide and silicon oxide;
in the step (3), heating the low-power-transmission baking crucible for 1-3 hours by using 10% -30% of rated power of equipment;
in the step (3), heating the high-power transmission baking crucible for 10-30 min by using 60-80% of rated power of equipment;
six induction coils of furnace body inboard equipartition of crucible preliminary treatment vacuum furnace, the outside of furnace body sets up cooling water inlet, cooling water outlet, vacuum pipe and power respectively, and concrete structure is as follows:
the vacuum pipeline is communicated with the inner cavity of the furnace body and is used for vacuumizing the furnace body; when the crucible is used, the combined structure of the crucible basket, the crucible sleeve and the crucible is arranged on the inner side of the induction coil, the graphite rod is placed in the crucible, the induction coil is connected with a power supply through a circuit, and the induction coil carries out induction heating on the graphite rod; the induction coil is wound by a hollow copper pipe to form a spiral barrel, a cooling water inlet and a cooling water outlet are respectively communicated with the hollow copper pipe of the induction coil through pipelines, and the hollow copper pipe of the induction coil is internally communicated with cooling water.
2. The method for rapidly pretreating a formed crucible for vacuum smelting according to claim 1, wherein in the step (2), the crucible pretreatment vacuum furnace is a device which is provided with more than two induction coils in a furnace body and is independently used for heating in a vacuum environment.
3. The method for quickly pretreating the formed crucible for vacuum smelting according to claim 1, wherein in the step (2), the graphite rod is a cylindrical graphite rod with an outer diameter of 20-30 mm smaller than the inner diameter of the crucible, and the length of the graphite rod is 1.1-1.3 times of the height of the crucible.
4. The method for rapidly pretreating a forming crucible for vacuum smelting according to claim 1, wherein in the step (3), the vacuum degree is reduced to below 100 Pa.
5. The method for quickly pretreating a formed crucible for vacuum smelting according to claim 1, wherein in the step (4), the tool is a crucible taking and placing tool which is placed in the crucible, props against the inner wall of the crucible in an opening manner and is provided with a long handle.
6. The method for rapidly pretreating a forming crucible for vacuum smelting according to claim 1, wherein in the step (5), the vacuum environment is a vacuum tank or a vacuum furnace device, and the vacuum degree is not more than 1000 Pa.
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CN113865342B (en) * 2021-09-27 2023-05-30 先导薄膜材料有限公司 Maintenance method of cold crucible
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CN102798292A (en) * 2012-09-10 2012-11-28 江西稀有稀土金属钨业集团有限公司 Method for baking vacuum induction melting furnace
CN105486084A (en) * 2014-10-09 2016-04-13 中国科学院金属研究所 Crucible basket cover and preparation method thereof
CN109536818A (en) * 2018-12-22 2019-03-29 北京航空航天大学苏州创新研究院 A method of preparing high-purity blade of aviation engine bonding coat target

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN102192649A (en) * 2010-10-15 2011-09-21 中国南方航空工业(集团)有限公司 Crucible basket for vacuum smelting furnace and manufacturing method of crucible basket
CN102798292A (en) * 2012-09-10 2012-11-28 江西稀有稀土金属钨业集团有限公司 Method for baking vacuum induction melting furnace
CN105486084A (en) * 2014-10-09 2016-04-13 中国科学院金属研究所 Crucible basket cover and preparation method thereof
CN109536818A (en) * 2018-12-22 2019-03-29 北京航空航天大学苏州创新研究院 A method of preparing high-purity blade of aviation engine bonding coat target

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