CN114951649B - Die for rapid smelting or vacuum heat treatment of discharge plasma and application method thereof - Google Patents
Die for rapid smelting or vacuum heat treatment of discharge plasma and application method thereof Download PDFInfo
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- CN114951649B CN114951649B CN202210704494.6A CN202210704494A CN114951649B CN 114951649 B CN114951649 B CN 114951649B CN 202210704494 A CN202210704494 A CN 202210704494A CN 114951649 B CN114951649 B CN 114951649B
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- graphite
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- smelting
- crucible
- blocking agent
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- 238000003723 Smelting Methods 0.000 title claims abstract description 62
- 238000010438 heat treatment Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 37
- 208000028659 discharge Diseases 0.000 title claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 108
- 239000010439 graphite Substances 0.000 claims abstract description 108
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 103
- 238000004806 packaging method and process Methods 0.000 claims abstract description 27
- 239000002981 blocking agent Substances 0.000 claims abstract description 23
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims description 14
- 230000009970 fire resistant effect Effects 0.000 claims description 12
- 238000012544 monitoring process Methods 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000003063 flame retardant Substances 0.000 claims description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 4
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 abstract description 18
- 229910045601 alloy Inorganic materials 0.000 abstract description 17
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 238000012806 monitoring device Methods 0.000 abstract 1
- 238000002490 spark plasma sintering Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 238000003825 pressing Methods 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 229910010038 TiAl Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 230000005676 thermoelectric effect Effects 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010099 solid forming Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/003—Apparatus, e.g. furnaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
- B22D23/06—Melting-down metal, e.g. metal particles, in the mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/12—Appurtenances, e.g. for sintering, for preventing splashing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/34—Methods of heating
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
-
- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- 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
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- 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
Abstract
The invention discloses a rapid smelting or vacuum heat treatment die for discharge plasma and a use method thereof. The graphite heating cavity die consists of the graphite cylinder body and the packaging cover, so that the crucible can be conveniently placed and the position of the crucible can be conveniently adjusted, and the temperature monitoring device is arranged on the graphite cylinder body, so that the temperature change of the melting crucible in the melting die can be monitored in real time. When the mold is used, the contact surfaces between the inner layer of the graphite cavity and the inner surface of the crucible are coated with the refractory blocking agent, so that the reaction between graphite and the crucible and between alloy and the crucible is prevented, and the service life of the mold is prolonged.
Description
Technical Field
The invention belongs to the technical field of hot-pressed sintering dies, and particularly relates to a die for rapid smelting of discharge plasma or vacuum heat treatment and a use method thereof.
Background
The metal is extremely easy to contact with air to react in the high temperature and melting consolidation process; particularly, for active metals such as aluminum, magnesium, titanium and the like, the metal is easy to oxidize or react with other metals to generate intermetallic compounds under high temperature, so that the casting and forming process of the metal is generally carried out under vacuum or atmosphere protection, which greatly limits the optional forming process range of the alloy forming process and reduces the alloy forming efficiency. Spark plasma sintering is a common powder metallurgy vacuum rapid forming sintering process, and the principle is that pulse high-energy current beam current is applied through upper and lower electrode pressure heads under vacuum condition, and rapid temperature rise is realized through thermoelectric effect; therefore, the high vacuum degree (> 0.1 Pa) is suitable for preparing relatively active titanium and titanium-aluminum alloy. However, the powder metallurgy process is suitable for a near-solid hot press forming process, and the axial pressurizing condition is difficult to be suitable for a liquid phase forming mode and a heat treatment process.
Chinese patent publication No. CN202010482082.3 discloses a preparation method of a titanium-aluminum-based high-temperature alloy block based on thermal explosion reaction, wherein Ti and Al mixed powder is used as raw materials, a proper amount of titanium alloy powder is added for alloying, and a novel titanium alloy material is prepared through thermal explosion reaction and hot-pressed sintering. The method belongs to a near-solid forming process of powder metallurgy, is only suitable for micron-sized powder, and has no smelting effect.
Chinese patent, publication No. CN102312111a, discloses a method for smelting TiAl alloy by using a vacuum consumable arc furnace, the process adopts a high-energy beam process to quickly smelt the TiAl alloy, the energy input is high, the smelting temperature cannot be controlled, the burning loss of alloy element Al is easy to be caused, the components of the alloy element are unstable, the cutting and heating up and cooling down rates cannot be controlled, and the stability of product quality cannot be ensured.
The Chinese patent, publication No. CN201510028165.4, discloses a method for preparing TiAl alloy plates by spark plasma sintering and hot rolling of a jacket, which belongs to the traditional powder metallurgy solid phase forming method, can only aim at powder near solid phase forming, cannot achieve smelting and casting effects and heat treatment processes, and greatly limits the types of raw materials.
Disclosure of Invention
The novel matching mode of the high-temperature resistant conductive graphite heating cavity and the smelting crucible in the cavity is adopted, so that the alloy forming process and the heat treatment method are widened, the forming efficiency of active metals is improved, the problem of axial pressurization in the spark plasma sintering process is solved, and the control of heating and cooling rate control organization in the smelting process is realized.
The invention is realized by the following technical scheme:
the first aspect provides a die for rapid melting or vacuum heat treatment of discharge plasma, comprising a high-temperature resistant conductive graphite heating cavity; the high-temperature-resistant conductive graphite heating cavity is formed by matching a graphite cylinder body with a graphite packaging cover, a first press column electrode matching groove is formed in the top of the graphite packaging cover, and a second press column electrode matching groove is formed in the bottom of the graphite cylinder body.
As a further explanation of the present invention, a melting crucible is placed inside the graphite cylinder, and the melting crucible has an open cup shape.
As a further illustration of the invention, both the inner wall of the high temperature resistant conductive graphite heating cavity and the inner wall of the melting crucible are coated with a refractory blocker, and the refractory blocker thickness is >0.5mm.
As a further illustration of the present invention, the nominal composition of the fire-resistant blocker is 99.97% yttria and a fire-retardant binder, which are mixed and thoroughly stirred in a mass ratio of 10-20:1.
As a further illustration of the invention, the alloy feedstock within the melting crucible is not more than 2/3 of the volume of the melting crucible when in use.
As a further illustration of the invention, the side wall or bottom of the graphite cylinder is provided with an infrared temperature monitoring hole and a thermocouple temperature monitoring hole.
As a further illustration of the invention, a thermal insulation graphite felt is provided outside the mold.
As a further explanation of the invention, the packaging matching surface of the graphite packaging cover is provided with a graphite packaging limit structure.
A second aspect provides a method for using the die for rapid melting or vacuum heat treatment of discharge plasma, comprising:
preparing a refractory blocking agent, uniformly coating the refractory blocking agent on the bottom wall of a graphite cylinder body and the inner wall of a smelting crucible, and repeatedly coating the refractory blocking agent after the refractory blocking agent is solidified until the thickness of the refractory blocking agent is more than 0.5mm;
placing raw materials into the smelting crucible, wherein the volume of the raw materials is not more than 2/3 of the volume of the smelting crucible, and then placing the smelting crucible into the graphite cylinder body and packaging a graphite packaging cover;
and sleeving the thermal insulation graphite felt outside the die, putting the thermal insulation graphite felt into a discharge plasma sintering furnace for vacuumizing, and heating and smelting or heat treatment after reaching a specified vacuum degree.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) The invention realizes the vacuum smelting or heat treatment of the alloy under the temperature control condition, can realize the regulation and control of the heating rate and the cooling rate in the heat treatment process, can control the alloy structure and is beneficial to the stability of the product quality; and the smelting can realize programmed control, so that the labor cost is reduced.
(2) The blocking agent is used for the contact surface, so that the problem of demoulding of the smelted sample can be solved while the mould is protected, the service life of the crucible is prolonged, and the production efficiency is improved.
(3) The smelting mould widens the application range of the spark plasma sintering furnace, so that the liquid phase forming mode is also suitable for the spark plasma sintering furnace.
(4) According to the invention, a novel matching mode of the high-temperature-resistant conductive graphite heating cavity and the smelting crucible in the cavity is adopted, so that the problem of axial pressurization in the spark plasma sintering process is solved.
Drawings
FIG. 1 is an assembly view of a mold for electric discharge plasma flash smelting or vacuum heat treatment provided by the present invention;
FIG. 2 is a cross-sectional view of a graphite packing cover and graphite cylinder of the present invention;
FIG. 3 is a pictorial view of a die for spark plasma flash smelting or vacuum heat treatment provided by the invention;
FIG. 4 is a physical diagram of the heat-treated aluminum powder agglomerate in example 1 of the present invention;
fig. 5 is an XRD pattern of Al powder in example 1 of the present invention.
Reference numerals:
1-graphite gradually increasing a reducing pressure head; 2-graphite press columns; 3-graphite encapsulation cover; 4-graphite cylinder; 5-a high-temperature resistant conductive graphite heating cavity; 6-smelting a crucible; 7-graphite packaging limit structure; 8, graphite lower gradual change pressure head; 9-a first press-stud electrode fitting groove; 10-packaging the matching surface; 11-an infrared temperature monitoring hole; 12-a second press-stud electrode fitting groove; 13 thermocouple temperature monitoring holes.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present invention, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
The technical scheme of the present invention will be explained in conjunction with specific embodiments.
As shown in fig. 2, a mold for rapid melting or vacuum heat treatment of discharge plasma is provided, which comprises a high-temperature resistant conductive graphite heating cavity 5; the high-temperature-resistant conductive graphite heating cavity 5 is formed by matching a graphite cylinder body 4 with a graphite packaging cover 3, a first press column electrode matching groove 9 is formed in the top of the graphite packaging cover 3, and a second press column electrode matching groove 12 is formed in the bottom of the graphite cylinder body 4.
The graphite packaging limit structure 7 is arranged on the packaging matching surface 10 of the graphite packaging cover 3, so that the packaging connection of the graphite packaging cover 3 and the graphite cylinder body 4 is realized, and the matching tolerance of the graphite packaging cover and the graphite cylinder body 4 is 1+0.5mm.
The smelting crucible 6 is arranged in the graphite cylinder body 4, and the smelting crucible 6 is in an open cup shape so as to ensure that no pressure difference exists in a cavity in the vacuumizing process.
The invention designs a sealed graphite heating cavity and a heat preservation die sleeve by utilizing the characteristic of rapid heating of discharge of a discharge plasma sintering furnace, and rapidly heats a crucible in the graphite cavity to a set temperature by the thermoelectric effect of graphite, so that raw materials in the crucible are rapidly melted, and specific alloy smelting is carried out, or heat preservation is carried out on a metal block sample at a specific temperature.
According to the invention, a novel matching mode of the high-temperature-resistant conductive graphite heating cavity and the smelting crucible in the cavity is adopted, so that the problem of axial pressurization in the spark plasma sintering process is solved (as the raw material is placed in the smelting crucible, when the raw material is axially pressurized in the spark plasma sintering process, the pressure acts on the high-temperature-resistant conductive graphite heating cavity through the pressing column, so that the raw material in the smelting crucible cannot be subjected to the pressure), and the smelting mold widens the application range of the spark plasma sintering furnace, so that the liquid phase forming mode is also suitable for the spark plasma sintering furnace.
Furthermore, the inner wall of the high-temperature resistant conductive graphite heating cavity 5 and the inner wall of the smelting crucible 6 are coated with a fire-resistant blocking agent, and the thickness of the fire-resistant blocking agent is more than 0.5mm. The nominal component of the fire-resistant blocking agent is 99.97% of yttrium oxide and a flame-retardant binder, and the yttrium oxide and the flame-retardant binder are mixed and fully stirred in a mass ratio of 10-20:1. The blocking agent is used for the contact surface, so that the problem of demoulding of the smelted sample can be solved while the mould is protected, the service life of the crucible is prolonged, and the production efficiency is improved.
Further, the side wall or the bottom of the graphite cylinder body 4 is provided with an infrared temperature monitoring hole 11 and a thermocouple temperature monitoring hole 13, which are used for monitoring the temperature change of the melting crucible 6 in the graphite cylinder body 4 in real time under different temperature conditions. The invention realizes the vacuum smelting or heat treatment of the alloy under the temperature control condition, can realize the regulation and control of the heating rate and the cooling rate in the heat treatment process, can control the alloy structure and is beneficial to the stability of the product quality; and the smelting can realize programmed control, so that the labor cost is reduced.
Further, the heat-insulating graphite felt is arranged outside the die to ensure the temperature stability in the smelting process.
As shown in fig. 1, in one implementation manner, the die is used in combination with a graphite upper gradual change diameter press head 1 and a graphite lower gradual change press head 8, wherein the graphite upper gradual change diameter press head 1 and the graphite lower gradual change press head 8 are respectively positioned at the upper end and the lower end of the high-temperature-resistant conductive graphite heating cavity 5, and graphite press columns 2 are respectively arranged at the ends of the graphite upper gradual change diameter press head 1 and the graphite lower gradual change press head 8. The contact area of the die and the upper and lower pressing columns is reduced through the gradual pressing columns, so that the purpose of reducing the heat conduction effect is achieved, the temperature of the die in the heat preservation process is more stable, and the power consumption of a machine is reduced.
Example 1
The embodiment provides a use method for a discharge plasma rapid melting or vacuum heat treatment die, aiming at the problems of easy cracking and the like in the sintering forming process caused by larger stress after aluminum powder ball milling, and vacuum heat treatment experiments are needed. The specific implementation steps are as follows:
step 1, preparing a 5:1 yttrium oxide blocking agent, and repeatedly coating the inner surfaces of the bottom of a corundum smelting crucible and the bottom of a graphite cylinder body to ensure that the thickness of the blocking agent is about 0.8mm;
step 2, placing 20g of weighed Ti-48Al-5Nb alloy raw material into a corundum smelting crucible, placing the smelting crucible filled with raw material into the middle position of the bottom of a graphite cylinder, sealing a graphite packaging cover, and sleeving a thermal insulation graphite felt on the outer layer of a graphite smelting mould;
and step 3, assembling the graphite smelting mould from bottom to top, aligning an infrared temperature measuring device with an infrared temperature monitoring hole of the graphite smelting mould, closing a furnace door after the axial center position of the graphite smelting mould is adjusted, and starting vacuumizing.
Step 4, setting a smelting program, applying pressure of 0.5 ton, heating at a speed of 100 ℃/min, preserving heat at 600 ℃ for 1h, cooling to room temperature, and performing heat treatment at a vacuum degree of less than 0.5Pa
And 5, taking out a smelting crucible in the graphite smelting mould, and pouring out a powder product.
Table 1 shows the oxygen content of the Al powder in example 1.
TABLE 1 oxygen content of powders
Fig. 5 is an XRD pattern of Al powder in example 1. It can be clearly observed that after ball milling, the powder is subjected to peak shift due to stress; and after heat treatment, the peak shift disappeared, indicating that the stress disappeared during the heat treatment.
Example 2
The embodiment provides a use method for a discharge plasma rapid smelting or vacuum heat treatment die, which comprises the following specific implementation steps:
step 1, preparing a 5:1 yttrium oxide blocking agent, and repeatedly coating the inner surfaces of the bottom of a corundum smelting crucible and the bottom of a graphite cylinder body to ensure that the thickness of the blocking agent is about 0.8mm;
step 2, placing 20g of weighed titanium-aluminum alloy raw materials into a corundum smelting crucible, placing the smelting crucible filled with the raw materials into the middle position of the bottom of a graphite cylinder body, sealing a graphite packaging cover, and sleeving a thermal insulation graphite felt on the outer layer of a graphite smelting mould;
and step 3, assembling the graphite smelting mould from bottom to top, aligning an infrared temperature measuring device with an infrared temperature monitoring hole of the graphite smelting mould, closing a furnace door after the axial center position of the graphite smelting mould is adjusted, and starting vacuumizing.
Step 4, setting a smelting program, applying pressure of 0.5 ton, heating at a heating rate of 200 ℃/min, preserving heat for 0.5h at 1800 ℃, cooling to room temperature at 10 ℃/min, and smelting at a vacuum degree of <0.5Pa
And 5, taking out a smelting crucible in the graphite smelting mould, and pouring out a smelting ingot casting product.
The embodiments given above are preferred examples for realizing the present invention, and the present invention is not limited to the above-described embodiments. Any immaterial additions and substitutions made by those skilled in the art according to the technical features of the technical scheme of the invention are all within the protection scope of the invention.
Claims (2)
1. A method for using a die for rapid melting or vacuum heat treatment of discharge plasma is characterized in that,
the die comprises a high-temperature resistant conductive graphite heating cavity (5); the high-temperature-resistant conductive graphite heating cavity (5) is formed by matching a graphite cylinder body (4) with a graphite packaging cover (3), a first press column electrode matching groove (9) is formed in the top of the graphite packaging cover (3), and a second press column electrode matching groove (12) is formed in the bottom of the graphite cylinder body (4);
a smelting crucible (6) is arranged in the graphite cylinder body (4), and the smelting crucible (6) is in an open cup shape;
the inner wall of the high-temperature resistant conductive graphite heating cavity (5) and the inner wall of the smelting crucible (6) are coated with a fire-resistant blocking agent, and the thickness of the fire-resistant blocking agent is more than 0.5 and mm;
the nominal components of the fire-resistant blocking agent are 99.97% of yttrium oxide and a flame-retardant binder, and the yttrium oxide and the flame-retardant binder are mixed and fully stirred in a mass ratio of 10-20:1;
an infrared temperature monitoring hole (11) and a thermocouple temperature monitoring hole (13) are formed in the side wall of the graphite cylinder body (4);
a thermal insulation graphite felt is arranged outside the die;
when the die is used, the die is matched with a graphite upper gradual change diameter pressure head (1) and a graphite lower gradual change pressure head (8), the graphite upper gradual change diameter pressure head (1) and the graphite lower gradual change pressure head (8) are respectively positioned at the upper end and the lower end of a high-temperature-resistant conductive graphite heating cavity (5), graphite press columns (2) are respectively arranged at the ends of the graphite upper gradual change diameter pressure head (1) and the graphite lower gradual change pressure head (8), and the diameter of the graphite press columns (2) is smaller than that of the high-temperature-resistant conductive graphite heating cavity (5);
the method comprises the following steps:
preparing a fire-resistant blocking agent, uniformly coating the fire-resistant blocking agent on the bottom wall of a graphite cylinder body (4) and the inner wall of a smelting crucible (6), and repeatedly coating the fire-resistant blocking agent after the fire-resistant blocking agent is solidified until the thickness of the fire-resistant blocking agent is more than 0.5 and mm;
placing a titanium-aluminum alloy raw material into the smelting crucible (6), wherein the volume of the raw material is not more than 2/3 of the volume of the smelting crucible (6), and then placing the smelting crucible (6) into the graphite cylinder (4) and packaging a graphite packaging cover (3);
and sleeving the thermal insulation graphite felt outside the die, putting the thermal insulation graphite felt into a discharge plasma sintering furnace for vacuumizing, and heating and smelting or heat treatment after reaching a specified vacuum degree.
2. The use method of the die for rapid melting or vacuum heat treatment of discharge plasma according to claim 1, wherein a graphite packaging limit structure (7) is arranged on a packaging matching surface (10) of the graphite packaging cover (3).
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101493284A (en) * | 2009-02-24 | 2009-07-29 | 上海大学 | Crucible for fusing titan and method of preparation thereof |
| CN102765946A (en) * | 2012-07-05 | 2012-11-07 | 中国科学院宁波材料技术与工程研究所 | Current assisted method for quickly preparing powder |
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| DE102016004548A1 (en) * | 2016-04-13 | 2017-10-19 | Forschungszentrum Jülich GmbH | Process for the production of metallic or ceramic components and components |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101493284A (en) * | 2009-02-24 | 2009-07-29 | 上海大学 | Crucible for fusing titan and method of preparation thereof |
| CN102765946A (en) * | 2012-07-05 | 2012-11-07 | 中国科学院宁波材料技术与工程研究所 | Current assisted method for quickly preparing powder |
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