CN114592137B - Explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in one-step furnace - Google Patents
Explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in one-step furnace Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
-
- 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
- B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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- 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
An explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in a one-step furnace belongs to the technical field of titanium-aluminum-niobium ternary alloy materials. The explosion-proof device for producing kilogram-grade gamma-TiAlNb alloy by self-propagating in the one-step furnace comprises a heating area, a slow cooling area and a deep cooling area, wherein the heating area is used for providing heat for initiating the self-propagating reaction of the gamma-TiAlNb alloy and heat supplementing quantity in the slag-metal separation process; the slow cooling area is positioned below the heating area and used for a maintaining stage after the self-propagating reaction occurs and a final alloy cooling stage, and the cryogenic area is positioned below the slow cooling area and is a self-propagating main reaction area and used for taking away reaction heat and limiting the self-propagating violent process, so that an explosion-proof effect is achieved, and the safety of alloy preparation and production devices is ensured.
Description
The application has the application number of 202111254878.4, the application date of 2021, 10 months and 27 days, and the invention name is: the patent refers to the field of 'processes or means for the manufacture of alloys'.
Technical Field
The invention belongs to the technical field of titanium-aluminum-niobium ternary alloy materials, and particularly relates to an explosion-proof device for producing kilogram-level gamma-TiAlNb alloy in a one-step furnace in a self-propagating manner.
Background
The engine is used as the heart of the aircraft, the reliability and the safety of the engine are very important and can represent an international technological level and comprehensive national strength, but after the performance of the aircraft engine is improved at present, the internal environment temperature is gradually improved, the thrust-weight ratio of the aircraft is increased, and the nickel-based alloy commonly used on the blades of the aircraft engine cannot meet the actual requirement. At present, the gamma-TiAl alloy material with low density, high specific strength, strong oxidation resistance and good creep property at high temperature is in the leading edge of research internationally, but the practical application of the gamma-TiAl alloy is greatly limited because the hot processing capability is poor and the room-temperature ductility is about 1 percent. In addition, the special use requirements of nearly hundreds of parts such as fasteners, turbine disks, empennages and the like of airplanes, particularly fighters, also need to adopt ultralight, ultrahigh-temperature-resistant and corrosion-resistant titanium-aluminum-based alloy materials, and the titanium-aluminum-based alloy for military production in China is usually imported from America, Sweden, Germany and the like, and the independent production of large-scale and high-purity gamma titanium-aluminum-based alloy is a 'bottleneck' problem in the high-precision technical field in China. Because the gamma-TiAl binary alloy has large brittleness and is difficult to process, the brittleness of the titanium-aluminum base alloy can be obviously improved by adding a trace amount of the third element Nb. Therefore, the development of an efficient, green and safe kilogram-level gamma titanium aluminum niobium ternary alloy preparation scheme is a crucial step for solving the neck problem in China.
The prior titanium-aluminum-based alloy preparation technology mainly comprises ingot metallurgy, precision casting, self-propagating high-temperature synthesis (SHS) and the like. The ingot metallurgy method is easy to prepare large-size structural parts, but the differences of the melting points, the densities and the nonequilibrium solidification segregation coefficients of the main elements of the TiAl-based alloy are large, and the third component is difficult to homogenize and dissolve in the titanium-aluminum alloy. Therefore, the TiAl-based alloy prepared by the ingot metallurgy method usually has a coarse structure and serious component segregation, and even leads to cracking of the ingot in case of serious component segregation, so that the expected performance requirements are difficult to achieve. In addition, the ingot metallurgy processing steps are multiple, the processing process is complex, the cost of the preparation process is high, and large-scale production cannot be carried out. The precision casting technology is relatively mature, parts with simpler shapes and structures are easy to manufacture, the cost of the precision casting technology mainly comprises casting technology, hot isostatic pressing, electrochemical machining and machining, but the solidification time in the casting process is short, and a large number of air holes are easy to form in the alloy to reduce the fatigue strength of the alloy. In addition, the casting method is used for producing the titanium-aluminum-based alloy, and the titanium element reacts with the crucible, so that the high-purity titanium-aluminum-based alloy is difficult to produce.
Compared with the two methods, the self-propagating high-temperature synthesis technology has obvious advantages, is self-conduction by utilizing substance reaction heat, forms a high-temperature transient field in a very short time, realizes high-efficiency conversion of chemical reaction, and has uniform and fine structure and better deformation processing capacity due to rapid occurrence of temperature rise and temperature drop processes in the reaction process, thus the TiAl-based alloy prepared is easy to manufacture parts with different shapes, and effectively solves the problem of difficult processing and forming. However, the existing self-propagating high-temperature synthesis technology is still limited to the reaction occurring outside the furnace, and additional ignition is needed to promote the reaction, so that the problems of over-high oxygen content of the alloy, more impurities, lower alloy yield, waste of a large amount of reaction heat, incapability of realizing continuous large-scale production and the like are caused.
In conclusion, the self-propagating high-temperature synthesis technology is one of the most promising methods for preparing the gamma-TiAlNb target ternary alloy. At present, a new device and a new method which can realize large-scale continuous production and can fully utilize the advantages of the self-propagating technology are urgently needed to be developed, the controllable regulation (explosion prevention) of the self-propagating reaction process is realized, and the preparation of gamma-TiAlNb high-purity alloy, particularly kilogram-level alloy, is realized.
At present, a KRH method for preparing TiAl alloy by self-propagating reaction has obvious advantages (see the document: A New Process for Titanium alloys Production from TiO) 2 Doi:10.1016/0039- 2 As a main raw material, TiAl alloy is prepared by aluminum powder reduction. The innovation is that Ca and Al are added into the raw materials 2 O 3 The reaction slagging is easy to realize slag-metal separation, and the titanium-aluminum alloy is synthesized by a one-step method, but the alloy components contain a large amount of impurities, and the reaction is violent and uncontrollable. The method has an inherent contradiction that a large amount of Ca as a slagging agent is required to be added for removing oxygen in the titanium dioxide; on the other hand, the addition of a large amount of the slag former Ca can bring about a huge calcium thermal reaction, so that the reaction process is uncontrollable and explosion occurs. At present, the molar ratio of the raw materials adopted in the patent AU2005100278A4 is TiO 2 : al: ca: KClO4 is 25:64:7:4, and in order to reduce the critical temperature of reaction initiation, the raw material contains a large amount of strong oxidant and excessive slag former-calcium. The raw material ratio can generate excessive reaction heat to further cause inevitable explosion reaction, so that the method is only limited to the laboratory preparation of gram-grade TiAl alloy, kilogram-grade production is difficult to realize, and continuous automatic production cannot be realized. Therefore, a new set of explosion-proof method and device needs to be developed, and the gamma titanium aluminum-based alloy above kilogram grade can be safely produced on the premise of properly increasing the reaction initial critical temperature.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an explosion-proof device for producing kilogram-level gamma-TiAlNb alloy in a one-step furnace in a self-propagating way, the self-propagating reaction heat is greatly reduced by adjusting the proportion of raw materials, so severe explosion is avoided, in addition, the whole reaction process is controllable by controlling the generation amount of the reaction heat and the reaction heat consumption amount for inducing the next-level reaction, the production capacity of the TiAlNb alloy is greatly improved, the accurate one-to-one correspondence between the reaction process of the TiAlNb alloy and the functional area of the device can be realized, and the alloy slag-gold separation effect and the alloy quality are improved while the safe large-scale continuous production is realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to an explosion-proof method for self-propagating production of kilogram-grade gamma-TiAlNb alloy in a one-step furnace, which comprises the following steps:
step 1: preparing raw materials according to the preparation magnitude of gamma-TiAlNb alloy above kilogram level; the mass ratio of each raw material is as follows: titanium sponge: aluminum powder: a slag former: a strong oxidant: explosion-proof agent: niobium (46-48): (61-65): (13-15): (35-38): (19-26): (2-4);
in the step 1, the aluminum powder is preferably 400-600 mesh aluminum powder, and more preferably 500 mesh aluminum powder.
Step 2: uniformly mixing and drying the raw materials, placing the raw materials into a reaction kettle in a heating area of a device, determining the calculated value t0 of the surface temperature of the reaction kettle when critical reaction occurs to be 805-815 ℃ under different material proportions, and checking the bottom temperature t3 of the reaction kettle when the environmental temperature t2 in the heating area is 1050-1100 ℃; when the temperature t0-t1 is less than 10 ℃, and the temperature t1-t3 is less than 2 ℃, the reaction materials enter a slow cooling zone;
wherein t0 is a calculated value of the surface temperature of the reaction kettle when the critical reaction occurs; t1 is the actual temperature of the upper surface of the reaction kettle; t2 is the ambient temperature in the heating zone; t3 is the temperature at the bottom of the reaction kettle; t0-t1 is the difference between the calculated value of the surface temperature of the reaction kettle and the actual temperature of the upper surface of the reaction kettle when the critical reaction occurs; t1-t3 is the difference between the actual temperature of the upper surface of the reaction kettle and the temperature of the bottom of the reaction kettle;
and step 3: the reaction materials entering the slow cooling area continuously react, when the detected delta t3/min is more than 100 ℃/min, protective gas is filled into the cryogenic area, and the reaction materials enter the cryogenic area; delta t3/min is the temperature change rate of the bottom of the reaction kettle;
when the temperature t3 at the bottom of the reaction kettle reaches 1060-1100 ℃, the reaction materials entering the deep cooling area indicate that the self-propagating reaction is completely carried out, then the reaction materials are rapidly cooled to 1000-1050 ℃ at a cooling rate of 50-100 ℃/min, and then returned to the heating area again for heat supplementation, wherein the heat supplementation temperature rise rate is 10-15 ℃/min, the temperature is raised to 1250-1300 ℃ when the ambient temperature in the heating area, the temperature is kept for 15-30 min, and slag and gold separation is carried out;
and (3) allowing the reaction material after slag-metal separation to enter a slow cooling area, and slowly cooling at a cooling rate of 15-20 ℃/min to 300-400 ℃ to obtain the kilogram-grade slag-coated gamma-TiAlNb alloy.
In the step 1, CaO is selected as the slagging constituent. The explosion-proof agent is zirconia powder.
In the step 1, NaClO is selected as the strong oxidant 4 (ii) a According to the raw material proportion, the usage amount of the slag former and the strong oxidant in the KRH method is greatly reduced, the critical heating temperature for inducing reaction is properly increased, and meanwhile, the heat generation amount of aluminothermic and calthermic reaction is reduced, and the aim of explosion prevention is fulfilled.
In the step 2, the calculated value t0 of the surface temperature of the reaction kettle when the critical reaction occurs is determined by calculation according to the types of the reaction materials, the addition amount of the reaction materials, the heat insulation effect of the reaction kettle, the heat transfer temperature difference and the like.
In the step 2, the descending speed of the reaction materials entering the traveling mechanism of the slow cooling area is 0.08-0.15 m/s.
In the step 2, when the delta t1 is more than 5 ℃/s, the heating power supply of the heating zone is cut off.
In the step 3, the descending speed of the travelling mechanism entering the cryogenic region is 0.35-0.45 m/s.
An explosion-proof device for self-propagating production of kilogram-level gamma-TiAlNb alloy in a one-step furnace comprises a heating area, a slow cooling area and a deep cooling area, wherein the heating area is a non-ignition heating space and is used for providing starting heat of self-propagating reaction of gamma-TiAlNb alloy above the kilogram level and supplementing heat of a subsequent slag-gold separation process; the slow cooling area is located below the heating area and used for a maintaining stage after a self-propagating reaction occurs and a final cooling alloy obtaining stage, and the cryogenic area is located below the slow cooling area and used as a self-propagating main reaction area and used for taking away a large amount of reaction heat, so that an explosion-proof effect is achieved, and the safety of an alloy preparation process and a production device is guaranteed.
The explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in the one-step furnace is also provided with an automatic control system which is used for accurately controlling the temperature and time, monitoring the production state of the alloy, controlling a travelling mechanism and automatically lifting a material platform to enable the material platform to enter a corresponding device functional area in a corresponding reaction state.
In order to realize the explosion-proof method for producing the kilogram-level gamma-TiAlNb alloy in the one-step furnace in a self-propagating way, the invention also provides an explosion-proof device for producing the kilogram-level gamma-TiAlNb alloy in the one-step furnace in a self-propagating way, which is a non-ignition reaction furnace and comprises a heating zone furnace body, a slow cooling zone furnace body and a deep cooling zone furnace body; the induction heating furnace comprises a heating zone furnace body, a slow cooling zone furnace body and a cryogenic zone furnace body, wherein the heating zone furnace body, the slow cooling zone furnace body and the cryogenic zone furnace body are sequentially connected, the heating zone furnace body is an induction heating furnace body and forms a heating zone, the slow cooling zone furnace body forms a slow cooling zone, the cryogenic zone furnace body forms a cryogenic zone, and the heating zone, the slow cooling zone and the cryogenic zone are sequentially communicated;
the heating furnace comprises a heating area furnace body, a reaction kettle, a first temperature sensor, a second temperature sensor, a temperature sensor and a temperature sensor, wherein the graphite heating body is arranged in the heating area furnace body in an annular mode, the induction heater is arranged on the periphery of the graphite heating body in an annular mode, the three temperature sensors are arranged in the heating area furnace body and are arranged at different positions of the heating area, the first temperature sensor is used for monitoring the actual temperature t1 of the upper surface of the reaction kettle, and the second temperature sensor is used for monitoring the ambient temperature t2 in the heating area;
an automatic lifting platform is further arranged in the explosion-proof device for producing kilogram-grade gamma-TiAlNb alloy in a self-propagating manner in the one-step furnace, a reaction kettle is placed above the automatic lifting platform, and a third temperature sensor for detecting and checking temperature is arranged at the top of the automatic lifting platform and is used for detecting the bottom temperature t3 of the reaction kettle;
the slow cooling zone furnace body is internally provided with cooling water flow of 0.01-0.015m 3 Slow cooling zone cooling circuit of/min, more preferably 0.012m 3 A slow cooling area cooling pipeline of/min;
the furnace body in the deep cooling area is internally provided with cooling water with the flow rate of 0.02-0.025 m 3 A/min cryogenic zone cooling line, more preferably 0.024m 3 A min cryogenic zone cooling pipeline, wherein a gas charging pipeline is arranged at the lower part of the cryogenic zone to assist in filling argon for cooling and preventing oxidation; furthermore, the cooling pipeline of the cryogenic region is a fin high-temperature heat exchange pipe.
The automatic lifting platform controlled by the automatic control system can reciprocate in the heating area, the slow cooling area and the cryogenic area at different speeds.
Further, be provided with feed inlet and discharge gate on the lateral wall in slow cold district.
Furthermore, an explosion-proof valve is arranged above a heating zone furnace body of the explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in the one-step furnace.
Furthermore, an explosion-proof device for self-propagating production of kilogram-level gamma-TiAlNb alloy in the one-step furnace is connected with a power box.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention realizes the safe one-step furnace production of the gamma-TiAlNb alloy by adjusting the component proportion of the raw materials. On the basis of the KRH method, the composition ratio of the raw materials is innovatively improved. The sponge titanium is selected to improve the purity of the final product, and in addition, the contents of a slagging agent and a strong oxidant are respectively reduced by 20 percent and 40 percent. Through calculation, the reduction of the contents of the slag former and the strong oxidant can greatly reduce the reaction heat in the self-propagating reaction process, and the brand new material composition completely gets rid of the extremely violent explosion reaction in the process of preparing the TiAl-based alloy by the KRH method and the limitation that the large-scale production cannot be realized. However, the brand new material composition can increase the calculated temperature of the surface of the reaction kettle from 500-550 ℃ to 805-815 ℃ when the self-propagating critical reaction occurs, so that the problem of the temperature rise of the critical point of the induced reaction is solved by the brand new design of the heating mode of the equipment (the heating mode of three pairs of resistance electrodes of the KRH method is changed into the homogenizing heating mode of the induction heating graphite heating element of the invention). Therefore, the reduction of the content of the corresponding components in the raw materials does not influence the self-propagating reaction. The reduction of the use amount of the slag former CaO can still satisfy the whole slag making, greatly reduce the heat generated by the reaction, avoid the generation of the uncontrollable self-propagating reaction caused by excessive reaction heat, and greatly improve the safety of the large-scale production and preparation process.
(2) The invention aims to realize the production of gamma-TiAlNb alloy by a one-step furnace method above kilogram level by a technical means, and a brand new production device has the advantages of reaction in a vacuum furnace, green one-step synthesis, preparation continuity, automatic control of production flow and the like; the designed PLC automatic control system can monitor the temperature of each reaction zone and the alloy production state, automatically control the reaction process and realize the full-process automatic production of the gamma-TiAlNb alloy.
(3) The invention designs a production device for preparing the gamma-TiAlNb alloy by a non-ignition in-furnace method, a self-propagating reaction generation area is the inside of the furnace body, and the structure and the size of the furnace body are further optimized and designed for realizing large-scale production and production safety, so that the harm caused by a large amount of splashing due to too severe reaction in the self-propagating reaction outside the furnace is avoided. The main body of the device is divided into three stages, which correspond to different preparation stages of the gamma-TiAlNb alloy. The heating area at the top of the device is a non-ignition heating space, heat required for inducing self-propagating reaction in the TiAlNb alloy preparation process and heat supplement amount in the subsequent slag-metal separation process are provided, energy loss is reduced, meanwhile, the formation of oxides is reduced through good temperature control, and the alloy yield is improved. The subdivision of the cooling area further promotes the refinement degree of the production flow, controls the self-propagating reaction generation area in the cooling area, promotes the safety of the preparation process and further promotes the quality of the prepared alloy, and the slow cooling area in the middle of the device is an area for cooling the material after the self-propagating reaction occurs, so that the self-propagating reaction can be controlled to be continuously carried out, and the self-propagating reaction is not caused to generate excessive heat and is violently carried out. Be different from traditional cooling process, the slow cooling district uses the less, the moderate cooling water of temperature of flow to carry out the slower alloy cooling process of cooling rate in unit interval, is favorable to the improvement of alloy microstructure to set up the charge door in the slow cooling district, thereby avoid thermal loss. The cryogenic zone at the bottom of the device is the zone where the self-propagating reaction is completely taking place and is also the main zone of the cooling process. A large number of inner fin high-temperature heat exchange tubes are arranged on the side wall of the cryogenic region, and in addition, a large amount of argon is filled in the cryogenic region in the cooling process to enhance the radiation heat exchange of the cryogenic region and prevent oxidation. Therefore, a large amount of heat released by the self-propagating reaction can be taken away in a short time by the large-flow water cooling and air cooling matching in the deep cooling area, the cooling rate in unit time is high, the explosion-proof performance is greatly improved, and the waste heat generated in the production process can be supplied to other production. The cryogenic zone is designed according to the corresponding heat in the preparation process of the gamma-TiAlNb alloy strictly, and the raw materials can generate the heat mainly released by a self-propagating reaction and a strong aluminum powder oxidant in the preparation process of the alloy. Calculating the total heat quantity Q1 of the raw materials of unit mass in the self-propagating reaction to be 2400 KJ; the combined effect of the two is the most important heat source in the cryogenic zone, so that the cryogenic zone needs to carry away a large amount of heat in a short time and ensure the continuous progress of the self-propagating reaction, and the heat Q2 carried away by the cryogenic zone is 600KJ (about 30% of the total).
(4) The three-stage reaction space of the device can safely control the whole flow of the self-propagating reaction in the device. The novel device and the novel method jointly realize the whole process of one-step in-furnace self-propagating reaction, alloy preparation and slag-gold separation, the equipment structure is simple, the preparation process is short, the automation degree is high, and the large-scale continuous green production of the gamma-TiAlNb alloy is met on the basis of greatly improving the safety.
Drawings
FIG. 1 is a cross-sectional view of a structural schematic diagram of an explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in a one-step furnace;
FIG. 2 is a flow chart of an automatic control system;
FIG. 3 is a crystal phase diagram of a kilogram grade γ -TiAlNb alloy produced by self-propagating in a one-step furnace according to example 1 of the present invention;
as the structure names and serial numbers of the parts in fig. 1:1 is the heating zone furnace body, 2 is the slow cooling district furnace body, 3 is the cryogenic zone furnace body, 4 is induction heater, 5 is the graphite heat-generating body, 6 is reation kettle, 7 is first thermocouple, 8 is the second thermocouple, 9 is the third thermocouple, 10 is the business turn over material mouth, 11 is automatic lift platform, 12 is the slow cooling district cooling tube way, 13 is the cryogenic zone cooling tube way, 14 is the pipeline of aerifing, 15 is explosion-proof valve, 16 is the power supply box, 17 is the vacuum pump.
Fig. 2 is a flow chart of the automatic control system, illustrating in detail the reaction flow and the corresponding control process.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
An explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in a one-step furnace has a structural schematic diagram shown in figure 1; the furnace is a non-ignition reaction furnace and comprises a heating zone furnace body 1, a slow cooling zone furnace body 2 and a deep cooling zone furnace body 3; the furnace body 1 of the heating area, the furnace body 2 of the slow cooling area and the furnace body 3 of the cryogenic area are sequentially connected, the furnace body 1 of the heating area is an induction heating furnace body and forms a heating area, the furnace body 2 of the slow cooling area forms a slow cooling area, the furnace body 3 of the cryogenic area forms a cryogenic area, and the heating area, the slow cooling area and the cryogenic area are sequentially communicated;
a graphite heating body 5 is arranged in the heating zone furnace body 1 in an annular mode, an induction heater 4 is arranged on the periphery of the graphite heating body 5 in an annular mode, three thermocouples are arranged in the heating zone furnace body and are arranged at different positions of a heating zone, a thermocouple for detecting the actual temperature t1 on the upper surface of the reaction kettle is a first thermocouple 7, and a thermocouple for detecting the ambient temperature t2 in the heating zone is a second thermocouple 8;
an automatic lifting platform 11 is further arranged in the device, a reaction kettle 6 is placed above the automatic lifting platform 11, and a third thermocouple 9 for detecting and checking temperature t3 is arranged at the top of the automatic lifting platform 11;
a slow cooling zone cooling pipeline 12 is arranged in the slow cooling zone furnace body 2;
a cryogenic zone cooling pipeline 13 is arranged in the cryogenic zone furnace body 3, and an inflation pipeline 14 is arranged at the lower part of the cryogenic zone; the automatic lifting platform 11 is connected with an automatic control system, and the automatic lifting platform is lifted and lowered back and forth in the heating area, the slow cooling area and the cryogenic area at different speeds through the automatic control system.
The side wall of the furnace body 2 of the slow cooling area is provided with a feed inlet 10. Above the device is arranged an explosion-proof valve 15. An explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in the one-step furnace is connected with a power box 16. The vacuum pump 17 is communicated with the interior of an explosion-proof device for self-propagating production of kilogram-level gamma-TiAlNb alloy in the one-step furnace and is used for maintaining the vacuum state in the device.
The device is combined with the device for preparation, and the adopted device main body is divided into three stages, which correspond to different preparation stages of the gamma-TiAlNb alloy. The mixed raw materials are placed in a crucible, the crucible is placed in a reaction kettle in the preparation process, and the reaction kettle is placed on an automatic lifting platform 11 through a feeding port 10 arranged in a slow cooling area. Then the automatic lifting platform 11 is lifted into the heating area, the periphery of the reaction kettle entering the heating area is coated with the graphite heating body 5, and the induction heater 4 is matched to perform non-ignition heating of the heating area, so that the self-propagating reaction is promoted. Then, the automatic lifting platform 11 drives the reaction kettle 6 to descend to a cryogenic region located at the bottom of the device, complete self-propagating reaction is achieved, after cooling is carried out in the cryogenic region for a period of time, the automatic lifting platform 11 drives the reaction kettle 6 to ascend to a heating region again for heat preservation of alloy, so that alloy quality is thoroughly improved by slag-gold separation, after heat preservation is finished, the reaction platform descends to a slow cooling region for slow cooling, and the whole preparation process is finished in the slow cooling region.
In the whole preparation process, the whole process is reacted in the furnace and is completed by an automatic control system. The monitoring of the alloy production state is fed back by thermocouples, timing devices and limiting devices arranged in each reaction area, and the alloy reaction temperature, the position of a platform and the alloy reaction process can be directly checked through an external display.
In the explosion-proof method for producing kilogram-grade γ -TiAlNb alloy by self-propagating in one-step furnace of this embodiment, the automatic control flow is shown in fig. 2, and the specific steps in the implementation process are as follows:
step one, preparing raw materials according to the preparation magnitude of gamma-TiAlNb alloy above kilogram level, wherein the raw materials comprise Ti, Al, CaO and NaClO in a mass ratio 4 :ZrO 2 :Nb＝46:Mixing the raw materials at a ratio of 61:15:38:26:2, wherein the total mass is 10kg, uniformly mixing, and then sending the mixture to a drying oven for drying treatment to obtain a raw material mixture.
And step two, placing the pretreated raw material mixture into a ceramic crucible, placing the crucible into a reaction kettle, and preventing the alloy from directly colliding with the reaction kettle due to violent reaction on the basis of heat preservation and heat insulation.
And step three, placing the reaction kettle on an automatic lifting platform 11 through a feeding port 10 arranged in a slow cooling area. The vacuum pump 17 is vacuumized to 10 -3 Heating was started at Pa. And the TiAlN alloy is prepared according to the operation of an automatic control system. Thermocouples arranged in a heating area and an automatic lifting platform provide corresponding time signals, the ambient temperature t2 in the heating area reaches 1100 ℃, the actual temperature t1 on the upper surface of a reaction kettle reaches 800 ℃, the calculated value t0 of the surface temperature of the reaction kettle when critical reaction occurs is 815 ℃, an automatic control system receives the temperature t3 of the bottom of the reaction kettle to check the temperature signals according to the relation of t0, t1 and t2, the temperature signals meet the conditions that t0-t1 is less than 10 ℃, t1-t3 is less than 2 ℃, the automatic lifting platform is started, reaction materials in the reaction kettle begin to descend to a slow cooling area at the speed of 0.1m/s, and the descending process receives a small amount of heat to induce self-propagating reaction to occur.
And step four, the real-time temperature change can be seen from the operation screen, when the delta t3/min is more than 100 ℃/min, the self-propagating reaction is continuously generated, and the feedback signal excites the argon to be supplemented in the cryogenic region. The automatic lifting platform descends to the cryogenic zone at the speed of 0.4m/s, and the temperature t3 at the bottom of the reaction kettle is 1100 ℃, which indicates that the self-propagating reaction is completely carried out in the cryogenic zone. And after the temperature enters the descending process, rapidly cooling the temperature at the cooling rate of 50 ℃/min to reduce the temperature t3 at the bottom of the reaction kettle to 1050 ℃, and then raising the temperature to the heating zone again for heating and heat preservation.
Step five, the heat required by the heat preservation of the heating area is still supplied by the induction heater, the heat supplementing temperature rise rate is 10 ℃/min, the ambient temperature t2 in the heating area needs to be maintained at 1300 ℃ in the heat preservation process, the heat preservation is carried out for 30min, and when the corresponding time and temperature signals meet the requirements, the platform is cooled to the slow cooling area.
Step six, the reaction platform is lowered to a slow cooling area in the middle of the device, cooling water maintains the cooling rate of 20 ℃/min to slowly cool the alloy, when t3 is 400 ℃, the preparation process of the gamma-TiAl alloy coated by the first-round slag is finished, the reaction kettle is taken out, the step one is repeated, and continuous production can be carried out;
the prepared gamma-TiAlNb alloy is analyzed, the crystal phase diagram is shown in figure 3, and the gamma titanium aluminum eutectic structure with the alternately grown lamella can be seen; the hardness of the alloy is tested, the test force is 49N, the load retention time is 15s, the microhardness of the alloy is 435.3HV after the test is carried out, and the microhardness is improved by more than one time compared with the titanium-aluminum solid solution alloy prepared by the common smelting method of titanium sponge and aluminum powder.
Example 2
The explosion-proof method for self-propagating production of kilogram-grade gamma-TiAlNb alloy in a one-step furnace of the embodiment adopts the same device as the embodiment 1, and the specific steps in the implementation process of the embodiment are as follows:
step one, preparing raw materials according to the preparation magnitude of gamma-TiAlNb ternary alloy above kilogram level, wherein the raw materials comprise Ti, Al, CaO and NaClO in a mass ratio 4 :ZrO 2 The raw materials are mixed together with the total mass of 10kg, Nb is 48:65:13:35:19:2, and the mixture is sent to a drying oven to be dried after being uniformly mixed, so that a raw material mixture is obtained.
Step two, placing the pretreated raw material mixture into a ceramic crucible, placing the crucible into a reaction kettle, starting to vacuumize until the vacuum degree reaches 10 -3 Heating was started at Pa.
The three thermocouples distributed in the heating area can be used for detecting the actually measured temperature t1 of the upper surface of the reaction kettle and the ambient temperature t2 in the heating area, the thermocouples arranged in the automatic lifting platform can provide check temperature, namely the temperature t3 of the bottom of the reaction kettle, and the purpose of accurate production is achieved by combining temperature feedback and check with an automatic control system. Due to the change of the raw material proportion, the surface temperature of the reaction kettle rises to 805-815 ℃ when the critical reaction occurs, so that in order to stimulate the self-propagating reaction, the temperature difference exists in the heat exchange process, the ambient temperature t2 in the heating area reaches 1050 ℃ through calculation, the calculated value t0 reaches 805 ℃ according to the relation of t0, t1 and t2, the automatic control system receives the t3 check temperature signal according to the relation of t0, t1 and t2, at the moment, the temperature signal meets the condition that t0-t1 is less than 10 ℃, and t1-t3 is less than 2 ℃, the automatic lifting platform is started and is lowered to the slow cooling area at the speed of 0.1m/s, and a small amount of heat is received in the lowering process so as to induce the self-propagating reaction to occur. However, when the delta t1/s is more than 5 ℃/s in the heating zone, the reaction is considered to be carried out in the heating zone, the power supply of the heating zone is immediately cut off, and the safety valve is synchronously started, so that the equipment and the production safety are ensured.
When the delta t3/min is more than 100 ℃/min, the self-propagating reaction is continuously generated, and the feedback signal excites the supplement of argon in the cryogenic region. The automatic lifting platform is lowered to a cryogenic zone at the speed of 0.35m/s to carry out self-propagating reaction, and when the reaction is carried out, a large amount of heat released in the TiAlNb ternary alloy preparation process is rapidly cooled at the cooling rate of 50 ℃/min in the cryogenic zone, so that the cooling rate in unit time is high, and the explosion-proof performance is greatly improved; the slow cooling area is an area for cooling the alloy after the self-propagating reaction, and has the advantages of small flow, moderate temperature and slow cooling rate.
When t3 is 1080 ℃, the reaction is completely carried out, the temperature is continuously reduced, and the automatic lifting platform is lifted to the heating zone again to carry out heating and heat preservation when the temperature signal t3 is 1030 ℃ in the TiAl alloy preparation process. The slag can be kept for 30min at the temperature in the heat preservation process, the slag-gold settling separation time is prolonged, and the slag-gold separation capacity is improved. In the heat supplementing process of the heating zone, the ambient temperature t2 in the heating zone is maintained at 1250 ℃ at a heating speed of 10 ℃/min, the temperature is preserved for 30min, temperature response and time response signals are transmitted to the automatic lifting platform, the reaction platform descends to a slow cooling zone in the middle of the device, the alloy is slowly cooled, the cooling rate is 15 ℃/min, and the alloy is slowly cooled to avoid alloy cracking caused by too fast temperature reduction. When the temperature in the slow cooling area is reduced to 380 ℃, the preparation process of the gamma-TiAlNb alloy is completed, the reaction kettle is taken out, the step one is repeated, and continuous production can be carried out.
Example 3
The embodiment of the invention provides an explosion-proof method for self-propagating production of kilogram-level gamma-TiAlNb alloy in a one-step furnace, which adopts the same device as the embodiment 1, and the implementation process of the embodiment comprises the following specific steps:
step one, preparing raw materials according to the preparation magnitude of gamma-TiAlNb alloy above kilogram level, wherein the raw materials comprise Ti, Al, CaO and NaClO in a mass ratio 4 :ZrO 2 The raw materials are mixed together, wherein the total mass of the mixed materials is 10kg, the mixed materials are uniformly mixed, and then the mixed materials are sent to a drying box to be dried, so that a raw material mixture is obtained.
Secondly, placing the pretreated raw material mixture into a ceramic crucible, placing the crucible into a reaction kettle, starting to vacuumize until the vacuum degree reaches 10 -3 Heating was started at Pa.
Wherein, three thermocouples distributed in the heating area can be used for detecting actual measurement temperature t1 of the upper surface of the reaction kettle, ambient temperature t2 in the heating area, thermocouples arranged in the automatic lifting platform can provide check temperature t3, and the purpose of accurate production is achieved by combining temperature feedback and check with an automatic control system. Due to the change of the raw material proportion, when the calculated value t0 of the surface temperature of the reaction kettle is 810 ℃ when the critical reaction occurs and the ambient temperature t2 in the heating area is 1060 ℃, the automatic control system receives a t3 checking temperature signal according to the relation of t0, t1 and t2, at the moment, the automatic lifting platform is started and is lowered to a slow cooling area at the speed of 0.12m/s when the temperature t0-t1 is less than 10 ℃ and t1-t3 is less than 2 ℃, and the self-propagating reaction is induced to occur after a small amount of heat is received in the lowering process. However, when the delta t1 is more than 5 ℃/s in the heating zone, the reaction is considered to be carried out in the heating zone, the power supply of the heating zone is immediately cut off, and the safety valve is synchronously started, so that the equipment and the production safety are ensured.
When the delta t3/min is more than 100 ℃/min, the self-propagating reaction is continuously generated, and the feedback signal excites the supplement of argon in the cryogenic region. The automatic lifting platform is lowered to a cryogenic zone at the speed of 0.40m/s to carry out self-propagating reaction, and when the reaction is carried out, a large amount of heat released in the TiAlNb alloy preparation process is rapidly cooled at the cooling rate of 60 ℃/min in the cryogenic zone, so that the cooling rate in unit time is high, and the explosion-proof performance is greatly improved; the slow cooling area is an area for cooling the alloy after the self-propagating reaction, and has the advantages of small flow, moderate temperature and slow cooling rate.
When the temperature t3 is 1070 ℃, the reaction is completely carried out, the temperature is continuously reduced, and the automatic lifting platform is lifted to the heating zone again for heating and heat preservation when the temperature signal t3 is 1020 ℃ in the TiAlNb alloy preparation process. The slag can be kept for 25min at the temperature in the heat preservation process, the slag-gold settling separation time is prolonged, and the slag-gold separation capacity is improved. In the heat supplementing process of the heating zone, the ambient temperature t2 in the heating zone is maintained at 1270 ℃ at the heating speed of 12 ℃/min, the temperature is kept for 25min, temperature response and time response signals are transmitted to the automatic lifting platform, the reaction platform descends to a slow cooling zone in the middle of the device, the alloy is slowly cooled, the cooling rate is 17 ℃/min, and the alloy is slowly cooled to avoid alloy cracking caused by too fast temperature reduction. When the temperature in the slow cooling area is reduced to 350 ℃, the preparation process of the gamma-TiAlNb alloy is completed, the reaction kettle is taken out, the step one is repeated, and continuous production can be carried out.
Example 4
The method for producing more than kilogram grade gamma-TiAlNb alloy in a one-step furnace adopts the same device as the embodiment 1, and the specific steps in the implementation process of the embodiment are as follows:
step one, preparing raw materials according to the preparation magnitude of gamma-TiAlNb alloy above kilogram level, wherein the raw materials comprise Ti, Al, CaO and NaClO in a mass ratio 4 :ZrO 2 The raw materials are mixed together, wherein the total mass of the mixed materials is 10kg, the mixed materials are uniformly mixed, and then the mixed materials are sent to a drying box to be dried, so that a raw material mixture is obtained.
Secondly, placing the pretreated raw material mixture into a ceramic crucible, and placing the crucible into a reaction kettle
Wherein, three thermocouples distributed in the heating area can be used for detecting actual measurement temperature t1 of the upper surface of the reaction kettle, ambient temperature t2 in the heating area, thermocouples arranged in the automatic lifting platform can provide check temperature t3, and the purpose of accurate production is achieved by combining temperature feedback and check with an automatic control system. Due to the change of the raw material proportion, when the ambient temperature t2 in a heating zone reaches 1070 ℃, the calculated value t0 of the surface temperature of the reaction kettle reaches 810 ℃ when critical reaction occurs, and according to the relation among t0, t1 and t2, an automatic control system receives a t3 checking temperature signal, at the moment, the conditions that t0-t1 is less than 10 ℃ and t1-t3 is less than 2 ℃ are met, an automatic lifting platform is started and is descended to a slow cooling zone at the speed of 0.10m/s, and a small amount of heat is received in the descending process to induce the self-propagating reaction to occur. However, when the delta t1 is more than 5 ℃/s in the heating zone, the reaction is considered to be carried out in the heating zone, the power supply of the heating zone is immediately cut off, and the safety valve is synchronously started, so that the equipment and the production safety are ensured.
When the delta t3/min is more than 100 ℃/min, the self-propagating reaction is continuously generated, and the feedback signal excites the supplement of argon in the cryogenic region. The automatic lifting platform is lowered to a cryogenic region at the speed of 0.40m/s to carry out self-propagating reaction, and when the reaction is carried out, a large amount of heat released in the TiAlNb alloy preparation process is rapidly cooled in the cryogenic region at the cooling rate of 70 ℃/min, so that the cooling rate in unit time is high, and the explosion-proof performance is greatly improved; the slow cooling zone is a zone for cooling the alloy after the self-propagating reaction, and has the advantages of small flow, moderate temperature and slow cooling rate.
When t3 is 1080 ℃, the reaction is completely carried out, the temperature is continuously reduced, and the automatic lifting platform is lifted to the heating zone again to carry out heating and heat preservation when the temperature signal t3 is 1030 ℃ in the TiAlNb alloy preparation process. The slag can be kept for a certain time at the temperature in the heat preservation process, the slag-gold settling separation time is prolonged, and the slag-gold separation capacity is improved. In the heat supplementing process of the heating zone, the ambient temperature t2 in the heating zone is maintained at 1270 ℃ at the heating speed of 15 ℃/min, the temperature is preserved for 30min, temperature response and time response signals are transmitted to the automatic lifting platform, the reaction platform descends to a slow cooling zone in the middle of the device, the alloy is slowly cooled at the cooling rate of 20 ℃/min, and the alloy is prevented from cracking due to the fact that the temperature is reduced too fast through slow cooling. When the temperature in the slow cooling area is reduced to 370 ℃, the preparation process of the gamma-TiAlNb alloy is completed, the reaction kettle is taken out, the step one is repeated, and continuous production can be carried out.
Example 5
The method for producing more than kilogram grade gamma-TiAlNb alloy in a one-step furnace adopts the same device as the embodiment 1, and the specific steps in the implementation process of the embodiment are as follows:
step one, preparing raw materials according to the preparation magnitude of gamma-TiAlNb alloy above kilogram level, wherein the raw materials compriseAccording to the mass ratio of Ti to Al to CaO: NaClO 4: :ZrO 2 The raw materials are mixed together, wherein the total mass of the mixed materials is 10kg, the mixed materials are uniformly mixed, and then the mixture is sent to a drying box to be dried, so that a raw material mixture is obtained.
Secondly, placing the pretreated raw material mixture into a ceramic crucible, placing the crucible into a reaction kettle,
wherein, a plurality of thermocouples distributed in the heating zone can be used for detecting the actual measurement temperature t1 of reation kettle upper surface, and ambient temperature t2 in the heating zone arranges that the thermocouple arranged in automatic lift platform can provide check temperature t3, combines with automatic control system through feedback and the check of temperature, reaches the purpose of accurate production. Due to the change of the raw material proportion, the ambient temperature t2 in the heating zone reaches 1090 ℃ and the calculated value t0 of the surface temperature of the reaction kettle reaches 812 ℃ when the critical reaction occurs, and according to the relation of t0, t1 and t2, the automatic control system receives t3 checking temperature signals, at the moment, the temperature t0-t1 is less than 10 ℃, and t1-t3 is less than 2 ℃, the automatic lifting platform is started and descends to the slow cooling zone at the speed of 0.12m/s, and the descending process receives a small amount of heat to induce the self-propagating reaction to occur. However, when the delta t1 is more than 5 ℃/s in the heating zone, the reaction is considered to be carried out in the heating zone, the power supply of the heating zone is immediately cut off, and the safety valve is synchronously started, so that the equipment and the production safety are ensured.
When the delta t3/min is more than 100 ℃/min, the self-propagating reaction is continuously generated, and the feedback signal excites the supplement of argon in the cryogenic region. The automatic lifting platform is lowered to a cryogenic zone at the speed of 0.4m/s to carry out self-propagating reaction, and when the reaction is carried out, a large amount of heat released in the TiAlNb alloy preparation process is rapidly cooled in the cryogenic zone at the cooling rate of 100 ℃/min, so that the cooling rate in unit time is high, and the explosion-proof performance is greatly improved; the slow cooling area is an area for cooling the alloy after the self-propagating reaction, the flow is small, the temperature is moderate, the cooling rate is slow,
when the temperature t3 is 1100 ℃, the reaction is completely carried out, the temperature starts to be continuously reduced, and the automatic lifting platform is lifted to the heating zone again for heating and heat preservation when the temperature signal t3 is 1025 ℃ in the TiAlNb alloy preparation process. The slag can be kept for a certain time at the temperature in the heat preservation process, the slag-gold settling separation time is prolonged, and the slag-gold separation capacity is improved. In the heat supplementing process of the heating zone, the ambient temperature t2 in the heating zone is maintained at 1275 ℃ at the heating speed of 12 ℃/min, the temperature is kept for 25min, temperature response and time response signals are transmitted to the automatic lifting platform, the reaction platform descends to a slow cooling zone in the middle of the device, the alloy is slowly cooled, the cooling rate is 15 ℃/min, and the alloy is slowly cooled to avoid alloy cracking caused by too fast temperature reduction. When the temperature in the slow cooling area is reduced to 400 ℃, the preparation process of the gamma-TiAlNb alloy is completed.
Example 6
The method for producing more than kilogram grade gamma-TiAlNb alloy in a one-step furnace adopts the same device as the embodiment 1, and the specific steps in the implementation process of the embodiment are as follows:
step one, preparing raw materials according to the preparation magnitude of gamma-TiAlNb alloy above kilogram level, wherein the raw materials comprise Ti, Al, CaO and NaClO in a mass ratio 4 :ZrO 2 The raw materials are mixed together with the total mass of 10kg, Nb is 48:64:14:36:21:3, and the mixture is sent to a drying oven to be dried after being uniformly mixed, so that a raw material mixture is obtained.
Secondly, placing the pretreated raw material mixture into a ceramic crucible, placing the crucible into a reaction kettle,
wherein, three thermocouples distributed in the heating area can be used for detecting actual measurement temperature t1 of the upper surface of the reaction kettle, ambient temperature t2 in the heating area, thermocouples arranged in the automatic lifting platform can provide check temperature t3, and the purpose of accurate production is achieved by combining temperature feedback and check with an automatic control system. Due to the change of the raw material proportion, the calculated value t0 of the surface temperature of the reaction kettle is 808 ℃ when the critical reaction occurs, and the ambient temperature t2 in the heating zone is 1175 ℃. According to the relation of t0, t1 and t2, an automatic control system receives a t3 checking temperature signal, at the moment, the temperature meets the conditions that t0-t1 is less than 10 ℃, t1-t3 is less than 2 ℃, an automatic lifting platform is started, the temperature is reduced to a slow cooling area at the speed of 0.1m/s, and a small amount of heat is received in the reduction process to further induce self-propagating reaction to occur. However, when the delta t1 is more than 5 ℃/s in the heating zone, the reaction is considered to be carried out in the heating zone, the power supply of the heating zone is immediately cut off, and the safety valve is synchronously started, so that the equipment and the production safety are ensured.
When the delta t3/min is more than 100 ℃/min, the self-propagating reaction is continuously generated, and the feedback signal excites the supplement of argon in the cryogenic region. The automatic lifting platform is lowered to a cryogenic zone at the speed of 0.37m/s to carry out self-propagating reaction, and when the reaction is carried out, a large amount of heat released in the TiAlNb alloy preparation process is rapidly cooled at the cooling rate of 80 ℃/min in the cryogenic zone, so that the cooling rate in unit time is high, and the explosion-proof performance is greatly improved; the slow cooling area is an area for cooling the alloy after the self-propagating reaction, and has the advantages of small flow, moderate temperature and slow cooling rate.
When t3 is 1090 ℃ in the cryogenic zone, the reaction is completely carried out, the temperature is continuously reduced, and the automatic lifting platform is lifted to the heating zone again to carry out heating and heat preservation when the temperature signal t3 is 1040 ℃ in the TiAlNb alloy preparation process. The slag can be kept for 30min at the temperature in the heat preservation process, the slag-gold settling separation time is prolonged, and the slag-gold separation capacity is improved. In the heat supplementing process of the heating zone, the ambient temperature t2 in the heating zone is maintained at 1280 ℃ at the heating speed of 13 ℃/min, the temperature is preserved for 30min, temperature response and time response signals are transmitted to the automatic lifting platform, the reaction platform descends to a slow cooling zone positioned in the middle of the device, the alloy is slowly cooled at the cooling rate of 18 ℃/min, and the alloy is prevented from cracking due to the fact that the temperature is reduced too fast through slow cooling. When the temperature in the slow cooling area is reduced to 400 ℃, the preparation process of the gamma-TiAlNb alloy is completed, the reaction kettle is taken out, the step one is repeated, and continuous production can be carried out.
Example 7
The method for producing more than kilogram grade gamma-TiAlNb alloy in a one-step furnace adopts the same device as the embodiment 1, and the specific steps in the implementation process of the embodiment are as follows:
step one, preparing raw materials according to the preparation magnitude of gamma-TiAlNb alloy above kilogram level, wherein the raw materials comprise Ti, Al, CaO and NaClO in a mass ratio 4 :ZrO 2 The raw materials are mixed together with the total mass of 10kg, wherein the total mass of the mixed materials is 48:61:15:38:26:4, and the mixed materials are sent to a drying box to be dried to obtain a raw material mixture.
Secondly, placing the pretreated raw material mixture into a ceramic crucible, placing the crucible into a reaction kettle,
wherein, a plurality of thermocouples distributed in the heating zone can be used for detecting the actual measurement temperature t1 of reation kettle upper surface, and ambient temperature t2 in the heating zone arranges that the thermocouple arranged in automatic lift platform can provide check temperature t3, combines with automatic control system through feedback and the check of temperature, reaches the purpose of accurate production. Due to the change of the proportion of the raw materials, the calculated value t0 of the surface temperature of the reaction kettle when the critical reaction occurs is 813 ℃, the ambient temperature t2 in the heating area is 1070 ℃, the automatic control system receives a t3 checking temperature signal according to the relation of t0, t1 and t2, at the moment, the automatic lifting platform is started and descends to a slow cooling area at the speed of 0.15m/s when the temperature meets the conditions that t0-t1 is less than 10 ℃ and t1-t3 is less than 2 ℃, and a small amount of heat is received in the descending process to further induce the self-propagating reaction to occur. However, when the delta t1 is more than 5 ℃/s in the heating zone, the reaction is considered to be carried out in the heating zone, the power supply of the heating zone is immediately cut off, and the safety valve is synchronously started, so that the equipment and the production safety are ensured.
When the delta t3/min is more than 100 ℃/min, the self-propagating reaction is continuously generated, and the feedback signal excites the supplement of argon in the cryogenic region. The automatic lifting platform is lowered to a cryogenic zone at the speed of 0.35m/s to carry out self-propagating reaction, and when the reaction is carried out, a large amount of heat released in the TiAlNb alloy preparation process is rapidly cooled at the cooling rate of 70 ℃/min in the cryogenic zone, so that the cooling rate in unit time is high, and the explosion-proof performance is greatly improved; the slow cooling area is an area for cooling the alloy after the self-propagating reaction, the flow is small, the temperature is moderate, the cooling rate is slow,
when the temperature t3 is 1100 ℃, the reaction is completely carried out, the temperature is continuously reduced, and the automatic lifting platform is lifted to the heating zone again to carry out heating and heat preservation when the temperature signal t3 is 1030 ℃ in the TiAlNb alloy preparation process. The slag can be kept for 29min at the temperature in the heat preservation process, the slag-gold settling separation time is prolonged, and the slag-gold separation capacity is improved. In the heat supplementing process of the heating zone, the ambient temperature t2 in the heating zone is maintained at 1250 ℃ at a heating speed of 10 ℃/min, the temperature is kept for 29min, temperature response and time response signals are transmitted to the automatic lifting platform, the reaction platform descends to a slow cooling zone in the middle of the device, the alloy is slowly cooled, the cooling rate is 17 ℃/min, and the alloy is slowly cooled to avoid alloy cracking caused by too fast temperature reduction. When the temperature in the slow cooling area is reduced to 400 ℃, the preparation process of the gamma-TiAlNb alloy is completed, the reaction kettle is taken out, the step one is repeated, and continuous production can be carried out.
Example 8
The method for producing more than kilogram grade gamma-TiAlNb alloy in a one-step furnace adopts the same device as the embodiment 1, and the specific steps in the implementation process of the embodiment are as follows:
step one, preparing raw materials according to the preparation magnitude of gamma-TiAlNb alloy above kilogram level, wherein the raw materials comprise Ti, Al, CaO and NaClO in a mass ratio 4 :ZrO 2 The raw materials are mixed together with a total mass of 10kg in 46:63:15:38:26:4, and after uniform mixing, the mixture is sent to a drying oven to be dried, so that a raw material mixture is obtained.
Secondly, placing the pretreated raw material mixture into a ceramic crucible, placing the crucible into a reaction kettle,
wherein, a plurality of thermocouples distributed in the heating zone can be used for detecting the actual measurement temperature t1 of reation kettle upper surface, and ambient temperature t2 in the heating zone arranges that the thermocouple arranged in automatic lift platform can provide check temperature t3, combines with automatic control system through feedback and the check of temperature, reaches the purpose of accurate production. Due to the change of the raw material proportion, the calculated value t0 of the surface temperature of the reaction kettle rises to 814 ℃ when the critical reaction occurs, the ambient temperature t2 in the heating area is 1100 ℃, the automatic control system is excited under the combined action of t0, t1 and t2 to receive a t3 checking temperature signal, at the moment, the temperature is satisfied with t0-t1 being less than 10 ℃, and t1-t3 being less than 2 ℃, the automatic lifting platform is started and is reduced to a slow cooling area at the speed of 0.15m/s, and a small amount of heat is received in the reduction process to further induce the self-propagating reaction to occur. However, when the delta t1 is more than 5 ℃/s in the heating zone, the reaction is considered to be carried out in the heating zone, the power supply of the heating zone is immediately cut off, and the safety valve is synchronously started, so that the equipment and the production safety are ensured.
When the delta t3/min is more than 100 ℃/min, the self-propagating reaction is continuously generated, and the feedback signal excites the supplement of argon in the cryogenic region. The automatic lifting platform is lowered to a cryogenic zone at the speed of 0.45m/s to carry out self-propagating reaction, and when the reaction is carried out, a large amount of heat released in the TiAlNb alloy preparation process is rapidly cooled at the cooling rate of 75 ℃/min in the cryogenic zone, so that the cooling rate in unit time is high, and the explosion-proof performance is greatly improved; the slow cooling area is an area for cooling the alloy after the self-propagating reaction, the flow is small, the temperature is moderate, the cooling rate is slow,
when t3 is 1080 ℃, the reaction is completely carried out, the temperature is continuously reduced, and the automatic lifting platform is lifted to the heating zone again to carry out heating and heat preservation when the temperature signal t3 is 1035 ℃ in the TiAlNb alloy preparation process. The heat preservation process can lead Al to be generated 2 O 3 The slag is kept for 26min at the temperature, the slag-gold settling separation time is prolonged, and the slag-gold separation capacity is improved. In the heat supplementing process of the heating zone, the ambient temperature t2 in the heating zone is maintained at 1250 ℃ at a heating speed of 10 ℃/min, the temperature is maintained for 26min, temperature response and time response signals are transmitted to the automatic lifting platform, the reaction platform is lowered to a slow cooling zone positioned in the middle of the device, the alloy is slowly cooled at a cooling rate of 20 ℃/min, and the alloy is prevented from cracking due to the fact that the temperature is reduced too fast through slow cooling. When the temperature in the slow cooling area is reduced to 375 ℃, the preparation process of the gamma-TiAlNb alloy is completed, the reaction kettle is taken out, and the first step is repeated, so that continuous production can be realized.
Comparative example
The utility model provides an in-furnace method apparatus for producing of gamma-TiAlNb alloy, does not set up the cryogenic zone, then in self-propagating reaction process, a large amount of heat that instantaneous release can not disappear in the short time, can greatly influence production safety and equipment safety, in the experiment of preparing 0.5 kg material, the explosion leads to 8mm thick steel reation kettle to burst.
The preparation method of the gamma-TiAlNb commercial alloy provided by the embodiment has the advantages of simple device structure, high automation degree, simple and safe operation and easy large-scale continuous production. The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. An explosion-proof device for self-propagating production of kilogram-level gamma-TiAlNb alloy in a one-step furnace is characterized by comprising a heating area, a slow cooling area and a deep cooling area, wherein the heating area is a non-ignition heating space and is used for providing starting heat of self-propagating reaction of gamma-TiAlNb alloy above the kilogram level and supplementing heat of a subsequent slag-gold separation process; the slow cooling area is positioned below the heating area and is used for a maintaining stage after the self-propagating reaction occurs and a final cooling stage to obtain an alloy; the cryogenic zone is positioned below the slow cooling zone, is a self-propagating main reaction zone, is used for taking away reaction heat, limits the violent self-propagating, plays a role in explosion prevention, and ensures the safety of an alloy preparation process and a production device;
the explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in the one-step furnace comprises a heating zone furnace body, a slow cooling zone furnace body and a deep cooling zone furnace body; the induction heating furnace comprises a heating zone furnace body, a slow cooling zone furnace body and a cryogenic zone furnace body, wherein the heating zone furnace body, the slow cooling zone furnace body and the cryogenic zone furnace body are sequentially connected, the heating zone furnace body is an induction heating furnace body and forms a heating zone, the slow cooling zone furnace body forms a slow cooling zone, the cryogenic zone furnace body forms a cryogenic zone, and the heating zone, the slow cooling zone and the cryogenic zone are sequentially communicated;
the heating furnace comprises a heating area furnace body, a graphite heating body, an induction heater, three temperature sensors, a first temperature sensor, a second temperature sensor, a third temperature sensor, a fourth temperature sensor, a fifth temperature sensor and a sixth temperature sensor, wherein the graphite heating body is arranged in the heating area furnace body in a surrounding manner, the induction heater is arranged on the periphery of the graphite heating body in a surrounding manner, the three temperature sensors are arranged in the heating area furnace body and are arranged at different positions of the heating area, the first temperature sensor is used for detecting the actual temperature t1 on the upper surface of the reaction kettle, and the second temperature sensor is used for detecting the ambient temperature t2 in the heating area;
an automatic lifting platform is further arranged in the explosion-proof device for producing kilogram-grade gamma-TiAlNb alloy in a self-propagating manner in the one-step furnace, a reaction kettle is placed above the automatic lifting platform, and a third temperature sensor for detecting and checking temperature is arranged at the top of the automatic lifting platform and is used for detecting the bottom temperature t3 of the reaction kettle;
the explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in the one-step furnace is also provided with an automatic control system for accurately controlling the temperature and time, monitoring the production state of the alloy, controlling a travelling mechanism and automatically lifting a material platform to enable the material platform to enter a corresponding device functional area in a corresponding reaction state;
the explosion-proof method of the explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in the one-step furnace comprises the following steps:
step 1: preparing raw materials according to the preparation magnitude of gamma-TiAlNb alloy above kilogram level; the mass ratio of each raw material is as follows: titanium sponge: aluminum powder: a slag former: a strong oxidant: explosion-proof agent: niobium = (46-48): (61-65): (13-15): (35-38): (19-26): (2-4); the slagging agent is CaO, the explosion-proof agent is zirconia powder, and the strong oxidant is NaClO 4 ；
Step 2: uniformly mixing and drying the raw materials, placing the raw materials into a reaction kettle in a heating area of a device, and checking by adopting the bottom temperature t3 of the reaction kettle when the calculated value t0 of the surface temperature of the reaction kettle is 805-815 ℃ when critical reaction is determined to occur under different material proportions and the environmental temperature t2 in the heating area is 1050-1100 ℃; when the temperature t0-t1 is less than 10 ℃, and the temperature t1-t3 is less than 2 ℃, the reaction materials enter a slow cooling area;
and step 3: the reaction materials entering the slow cooling area continuously react, when the detected delta t3/min is more than 100 ℃/min, protective gas is filled into the cryogenic area, and the reaction materials enter the cryogenic area; delta t3/min is the temperature change rate of the bottom of the reaction kettle;
when the temperature t3 at the bottom of the reaction kettle reaches 1060-1100 ℃, the reaction materials entering the deep cooling area indicate that the self-propagating reaction is completely carried out, then the reaction materials are rapidly cooled to 1000-1050 ℃ at a cooling rate of 50-100 ℃/min, and then returned to the heating area again for heat supplementation, wherein the heat supplementation temperature rise rate is 10-15 ℃/min, the temperature is raised to 1250-1300 ℃ when the ambient temperature in the heating area, the temperature is kept for 15-30 min, and slag and gold separation is carried out;
and (3) allowing the reaction material after slag-metal separation to enter a slow cooling area, and slowly cooling at a cooling rate of 15-20 ℃/min to 300-400 ℃ to obtain the kilogram-grade slag-coated gamma-TiAlNb alloy.
2. The explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in a one-step furnace according to claim 1, wherein the slow cooling zone furnace body is internally provided with cooling water flow of 0.01-0.015 m 3 A slow cooling area cooling pipeline of/min.
3. The explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in a one-step furnace according to claim 1, wherein the furnace body in the cryogenic region is internally provided with 0.02-0.025 m 3 A/min cryogenic zone cooling pipeline, and a gas filling pipeline is arranged at the lower part of the cryogenic zone to assist the cooling of the argon filling gas and prevent the oxidation.
4. The explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in a one-step furnace according to claim 1, wherein an automatic lifting platform controlled by an automatic control system is used for reciprocating lifting in the heating area, the slow cooling area and the cryogenic area at different speeds.
5. The explosion-proof device for self-propagating production of kilogram-grade gamma-TiAlNb alloy in a one-step furnace according to claim 1, wherein a feeding hole and a discharging hole are arranged on the side wall of the slow cooling area.
6. The explosion-proof device for self-propagating production of kilogram-level gamma-TiAlNb alloy in the one-step furnace according to claim 1, wherein an explosion-proof valve is arranged above a heating zone furnace body of the explosion-proof device for self-propagating production of kilogram-level gamma-TiAlNb alloy in the one-step furnace.
7. The explosion-proof device for self-propagating production of kilogram-level gamma-TiAlNb alloy in the one-step furnace according to claim 1, wherein the explosion-proof device for self-propagating production of kilogram-level gamma-TiAlNb alloy in the one-step furnace is connected with a power supply box.
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Application publication date: 20220607 Assignee: Liaoning Dongzhi Guoguang Titanium Technology Co.,Ltd. Assignor: Northeastern University Contract record no.: X2023210000271 Denomination of invention: One step furnace self propagating production in kilograms g- Explosion proof device of TiAlNb alloy Granted publication date: 20220802 License type: Exclusive License Record date: 20231130 |
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