CN104846304A - Tantalum and niobium and tantalum niobium alloy vacuum annealing cooling method - Google Patents
Tantalum and niobium and tantalum niobium alloy vacuum annealing cooling method Download PDFInfo
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Abstract
The invention discloses a tantalum and niobium and tantalum niobium alloy vacuum annealing cooling method, the method is as follows: a material is filled into a vacuum furnace, the vacuum furnace is vacuumized, when the vacuum degree of the vacuum furnace reaches up to the vacuum degree meeting heating requirements, heating operation is performed; when the temperature in the vacuum furnace reaches up to the temperature meeting the heat preservation requirements, the heat preservation is performed; when the heat preservation of the vacuum furnace is performed for scheduled time, the cooling operation is performed; when the temperature in the vacuum furnace is cooled to 900-600 DEG C, vacuumizing operation of the vacuum furnace is stopped, and an inert gas is introduced into the vacuum furnace; and when the temperature in the vacuum furnace is dropped to material discharge temperature, the material is deaired and discharged. Compared with the prior art, tantalum and niobium and tantalum niobium alloy vacuum annealing cooling time can be significantly shortened, and the production efficiency is improved.
Description
Technical field
The present invention relates to rare metal Field of Heat-treatment, be specifically related to the method for cooling of a kind of tantalum niobium and alloy vacuum annealing thereof.
Background technology
Tantalum niobium and alloy thereof owing to having high-melting-point, corrosion-resistant, cold-forming property good and other many-sided premium properties, makes it have a wide range of applications in electronic industry, chemical industry, space flight and aviation, nuclear power and high temperature resistant field.
The production technique of tantalum niobium and alloy thereof is, the method for tantalum niobium and the melting of alloy electron beam furnace or powder smelting sintering is made ingot blank, then through press working, such as: the methods such as extruding, forging, rolling, drawing are processed into various section bar or goods.In pressing process, tantalum niobium and alloy thereof can produce work hardening, and intensity raises, the phenomenon that plasticity declines, at this moment just needs to carry out anneal, eliminates material internal stress, recover plasticity, so that carry out follow-up press working or reach the performance requriements of the finished product.
To the requirement of impurity atom content very strictly, such as, the interstitial element content requirement in tantalum pipe is: C :≤100ppm, N :≤100ppm, H :≤15ppm, O :≤150ppm(ASTMB521, RO5200) for tantalum niobium and alloy thereof; Interstitial element content requirement in niobium pipe is: C :≤100ppm, N :≤100ppm, H :≤15ppm, O :≤250ppm(ASTMB394, RO4210).Therefore, when tantalum niobium and alloy annealing thereof, in order to prevent introducing impurity atom, require very high to annealing atmosphere.
In prior art, tantalum niobium and alloy thereof adopt vacuum annealing process, and namely annealing process completes in vacuum environment.In vacuum environment, the constituent contents such as C, O, N are extremely low, can meet tantalum niobium and alloy thereof to the requirement of annealing atmosphere, can prevent tantalum niobium and alloy oxidation thereof simultaneously.
In actual production, tantalum niobium and alloy vacuum annealing process thereof are for be evacuated to vacuum oven internal pressure about 1 × 10 at vacuum oven
-3start heat temperature raising during Pa, continue to vacuumize simultaneously and keep vacuum oven internal pressure≤5 × 10 in heat-processed
-2pa.
Be incubated for some time after reaching predetermined temperature, after insulation terminates, cut off heating power supply, furnace cooling, vacuum system works always and to quit work when vacuum furnace temperature is about 100 DEG C, tantalum niobium and alloy is to be cooled comes out of the stove to lower than when 60 DEG C.
Tantalum niobium and alloy thereof generally press a batch production according to customer demand.To carry out press working from ingot casting, its operation is often very long, repeatedly will carry out the press working of more than 20 passages, just will can produce the finished product therebetween through reaching 4-6 vacuum annealing.
And the time of general press working is often very short, can complete in several hours, and once anneal, approximately needing 20-24 hour from shove charge to the whole annealing process of coming out of the stove, wherein, about needing 2-3 hour from shove charge to being evacuated to high vacuum, temperature-rise period is about 1-1.5 hour, insulation 1-2 hour, altogether about needs 4-6.5 hour, accounts for about 1/4th of whole annealing time.Process of cooling is about 16-18 hour, accounts for 3/4ths of whole annealing time.
From the above, the process of cooling of tantalum niobium and alloy vacuum annealing thereof takes a large amount of time, have impact on production efficiency, becomes the bottleneck of tantalum niobium and alloy production thereof.
Summary of the invention
The process of cooling time based on tantalum niobium and alloy vacuum annealing thereof in prior art is long, the problem that production efficiency is lower, the invention provides the method for cooling of a kind of tantalum niobium and alloy vacuum annealing thereof, to reduce the cooling time of its vacuum annealing, enhances productivity.Its technical scheme is as follows:
A method of cooling for tantalum niobium and alloy vacuum annealing thereof, comprising:
Material is loaded vacuum oven, and described material is selected from tantalum, tantalum alloy, niobium and niobium alloy;
Vacuum pumping is carried out to vacuum oven, when the vacuum tightness in vacuum oven reaches the vacuum tightness heating up and require, warming temperature is carried out to it;
When the temperature in vacuum oven reaches the temperature of thermal requirements, insulation operation is carried out to it;
After vacuum oven is incubated the scheduled time, cooling operation is carried out to it; When the temp. in vacuum furnace is down to 900 DEG C ~ 600 DEG C, vacuum pumping is stopped to vacuum oven and pass into rare gas element in vacuum oven;
When the temperature in vacuum oven is down to the tapping temperature of described material, vacate stove by broken for described material.
In a kind of preferred embodiment of the present invention, described cooling operation is charged cooling operation, and described method also comprises: after the temp. in vacuum furnace is down to 900 DEG C ~ 600 DEG C, before stopping vacuum pumping to vacuum oven, stop described charged cooling operation.
In another preferred embodiment of the invention, described cooling operation is furnace cooling operation.
In a kind of preferred embodiment of the present invention, when the temp. in vacuum furnace is down to 850 DEG C ~ 750 DEG C, vacuum pumping is stopped to vacuum oven and pass into rare gas element in vacuum oven.
In a kind of more preferred of the present invention, when the temp. in vacuum furnace is down to 800 DEG C, vacuum pumping is stopped to vacuum oven and pass into rare gas element in vacuum oven.
In a kind of preferred embodiment of the present invention, described rare gas element is selected from argon gas, helium or its mixed gas.
In a kind of preferred embodiment of the present invention, when the temp. in vacuum furnace is down to 900 DEG C ~ 600 DEG C, vacuum pumping is stopped to vacuum oven and in vacuum oven, passes into rare gas element, until vacuum oven internal pressure>=1 × 10
-6mpa, is preferably 10
-6~ 10
-1mpa, is more preferably 10
-4~ 10
-1during Mpa, stop passing into rare gas element operation.
In a kind of preferred embodiment of the present invention, described in pass into rare gas element and be: disposablely pass into rare gas element, or repeatedly pass into rare gas element.
In a kind of preferred embodiment of the present invention, described in vacuum oven, pass into rare gas element after comprise further: adopt rare gas element in cooling blower stirring vacuum furnace.
In a kind of preferred embodiment of the present invention, by described material broken vacate stove before, comprise further: discharge rare gas element, then repeat to be filled with rare gas element.
In the prior art, the cooling stages of vacuum annealing carries out under vacuum.The mode of its heat transmission is mainly radiation delivery; technical scheme of the present invention is at the cooling stages of vacuum annealing; when furnace temperature is down to 900 DEG C ~ 600 DEG C; rare gas element is passed into vacuum oven; make tantalum niobium and alloy thereof under the protection of rare gas element, continue cooling; the transfer mode of its heat is that conduction, convection current and radiation three kinds of modes coexist; compared with prior art; heat transfer efficiency is high; speed of cooling is fast; therefore, significantly can shorten the cooling time of tantalum niobium and alloy vacuum annealing thereof, thus improve production efficiency.
Embodiment
Technical scheme of the present invention passes into rare gas element at the cooling stages of annealing, to reduce the cooling time of tantalum niobium and alloy vacuum annealing thereof, thus enhances productivity.
Tantalum niobium and alloy thereof are in annealing process, and temperature during insulation is approximately 1200 DEG C; In whole temperature-fall period after insulation terminates, cooling rate is different, roughly can be divided into three phases, 1200 DEG C ~ about 900 DEG C, is the high temperature fast cooling stage, about about 20 minutes of temperature fall time; 900 DEG C ~ 300 DEG C is middling speed temperature-fall period, the about 5-8 hour of temperature fall time; Less than 300 DEG C is the slow cooling stage, the about 6-10 hour of temperature fall time.
Present inventor finds unexpectedly: when temperature is down to 900 DEG C ~ 600 DEG C, be preferably 850 DEG C ~ 750 DEG C, when being more preferably 800 DEG C, pass into the cooling time that rare gas element significantly can not only shorten tantalum niobium and alloy vacuum annealing thereof, thus improve production efficiency, but also following unforeseeable technique effect can be realized simultaneously:
1. the quality of tantalum niobium and alloy can be ensured while shortening cooling time.
In higher temperature, such as, time at 1200 DEG C ~ 900 DEG C, because temperature is higher, if pass into rare gas element at this moment, owing to there is microchemistry impurity in rare gas element, temperature is higher, these impurity are easier to react with tantalum niobium and alloy thereof, affects its quality.Contriver finds unexpectedly, in the temperature range of 900 DEG C ~ 600 DEG C, the microchemistry impurity existed in rare gas element can't with tantalum niobium or its alloy reaction.Therefore, ensure that the quality of tantalum niobium and alloy.
2. the life-span of tantalum niobium vacuum annealing furnace can be ensured while the cooling time shortening tantalum niobium and alloy thereof.
The well heater of tantalum niobium vacuum annealing furnace and thermoscreen generally make of refractory metal, and are fixed in body of heater with alumina-ceramic, and alumina-ceramic also plays insulating effect.Well heater and thermoscreen common used material are high temperature molybdenum alloy, and when temperature is higher and temperature sharply changes, molybdenum heater and thermoscreen are very easily out of shape and damage; Alumina-ceramic part also can burst, and causes decreasing insulating.According to life-time service experience, if pass into rare gas element cooling 1200 DEG C ~ 900 DEG C time, because now temperature is high, and speed of cooling quickly, 100-200 DEG C/min can be reached, often cause thermoscreen and heater texturing in body of heater, time serious, well heater ruptures because of distortion, causes unnecessary loss.Contriver finds unexpectedly, be less than 900 DEG C, such as, when passing into rare gas element in the temperature range of 900 DEG C ~ 600 DEG C, any substantial effect can't be caused by body of heater, especially can't produce any significant modification for the thermoscreen in body of heater and well heater.Therefore, method of cooling of the present invention can not only shorten the work-ing life also not affecting tantalum niobium vacuum annealing furnace cooling time of tantalum niobium and alloy thereof.
It should be noted that, the vacuum oven that technical solution of the present invention adopts is at body of heater or between high vacuum valve and body of heater, add rare gas element feedway.
And on vacuum oven, a refrigerating unit with cooling blower can be increased, after passing into rare gas element, start cooling blower and stir, strengthen convective heat exchange effect, can add and cool but speed.The vacuum oven that technical solution of the present invention adopts is prior art, to its technological transformation carried out to those skilled in the art, easily realizes, does not here repeat.In addition, every vacuum oven that can realize technical solution of the present invention can use in the present invention, and its specific form can not be construed as limiting the invention.
Rare gas element of the present invention refers to the gas of the annealing atmosphere that can meet tantalum niobium and alloy thereof, such as, can be argon gas, helium, neon, xenon, Krypton, radon gas, or their mixed gas; Consider cost, the present invention adopts argon gas, helium or their mixed gas as rare gas element, and purity is not less than 99%(percent by volume).But the gas of other kind, as long as the annealing atmosphere that can meet tantalum niobium and alloy thereof, just can realize technical scheme of the present invention, those skilled in the art can select according to practical situation.
In the present invention, the amount of inert gas passed into is larger, and cooling performance is better; But meanwhile, corresponding production cost is also higher.The unexpected discovery of the present inventor by select the amount passing into rare gas element to make to have leisure furnace pressure reach>=1 × 10
-6mpa, is preferably 10
-6~ 10
-1mpa, is more preferably 10
-4~ 10
-1during Mpa, while realizing extraordinary cooling performance, significantly can save production cost.Be understandable that, in actual production process, the amount of inert gas passed into can be determined according to concrete performance by those skilled in the art.
In the process passing into rare gas element cooling, along with the decline of temperature, because gas expands with heat and contract with cold, furnace pressure can decline thereupon, now can pass into rare gas element again in stove, pressure when making pressure recovery pass into rare gas element to first time, can improve rate of cooling so to a certain extent further.
Below by specific embodiment, technical solution of the present invention is described.
Embodiment 1
Tantalum tubing is about 100kg shove charge, send and add thermoelectricity after vacuumizing, to 1200 DEG C of insulations 2 hours, then charged cooling, cooling rate 20 DEG C/min, when temperature is down to 750 DEG C, broke and adds thermoelectricity.Then, close the large valve of high vacuum, foreline valve, diffusion pump, mechanical pump successively, cooling water pressure keeps 0.1-0.2MPa.This technique is state of the art, and therefore not to repeat here.
Open argon gas charging valve on body of heater, slowly inflate in stove.When body of heater internal pressure is 0.09MPa, stop inflation, close all valves, start cooling blower, furnace cooling.
When furnace temperature is cooled to about 60 DEG C, stop cooling blower, stop water coolant, break and vacate stove.Inspection product is all qualified.The whole vacuum annealing time is about 12 hours.Check thermoscreen and well heater, intact, alumina-ceramic part is intact.
Embodiment 2
Niobium zirconium silk material is about 100kg shove charge, send and add thermoelectricity after vacuumizing, to 1150 DEG C of insulations 1 hour, then charged cooling, cooling rate 20 DEG C/min, when temperature is down to 850 DEG C, broke and adds thermoelectricity.Then, close the large valve of high vacuum, foreline valve, diffusion pump, mechanical pump successively, cooling water pressure keeps 0.1-0.2MPa.This technique is state of the art, and therefore not to repeat here.
Open helium gas charging valve door on body of heater, slowly inflate in stove.When body of heater internal pressure is 0.001MPa, stop inflation, close all valves, furnace cooling.
When furnace temperature is cooled to about 60 DEG C, stop water coolant, break and vacate stove.Inspection product is all qualified.The whole vacuum annealing time is about 16 hours.Check thermoscreen and well heater, intact, alumina-ceramic part is intact.
Embodiment 3
Being the tantalum-tungsten alloy of 10% by the massfraction of Ta10W(tungsten) bar is about 100kg shove charge, send after vacuumizing and add thermoelectricity, to 1450 DEG C of insulations 1 hour, break and add thermoelectricity, furnace cooling, when temperature is down to 900 DEG C, close the large valve of high vacuum, foreline valve, diffusion pump, mechanical pump successively, cooling water pressure keeps 0.1-0.2MPa.This technique is state of the art, and therefore not to repeat here.
Open the charging valve of the mixed gas (percentage ratio is percent by volume for argon gas 35%, helium 65%) of argon gas and helium on body of heater, slowly inflate in stove.When body of heater internal pressure is 0.1MPa, stop inflation, close all valves, furnace cooling.
When furnace temperature is cooled to about 200 DEG C, starts mechanical pump, open low little valve, after finding time 5-30 minute, close low little valve and mechanical pump.Mixed gas to the body of heater internal pressure being again filled with argon gas and helium according to above-mentioned inflation method in stove is 0.1MPa, when furnace temperature is cooled to about 60 DEG C, stops water coolant, breaks and vacates stove.Inspection product is all qualified.The whole vacuum annealing time is about 14 hours.Check thermoscreen and well heater, intact, alumina-ceramic part is intact.
Embodiment 4
Niobium zirconium silk material is about 100kg shove charge, send and add thermoelectricity after vacuumizing, to 1150 DEG C of insulations 1 hour, then charged cooling, cooling rate 20 DEG C/min, when temperature is down to 600 DEG C, broke and adds thermoelectricity.Then, close the large valve of high vacuum, foreline valve, diffusion pump, mechanical pump successively, cooling water pressure keeps 0.1-0.2MPa.This technique is state of the art, and therefore not to repeat here.
Open helium gas charging valve door on body of heater, slowly inflate in stove.Treat that body of heater internal pressure is 5 × 10
-6during MPa, stop inflation, close all valves, furnace cooling.
When furnace temperature is cooled to about 60 DEG C, stop water coolant, break and vacate stove.Inspection product is all qualified.The whole vacuum annealing time is about 19 hours.Check thermoscreen and well heater, intact, alumina-ceramic part is intact.
Embodiment 5
Niobium zirconium silk material is about 100kg shove charge, send after vacuumizing and add thermoelectricity, to 1150 DEG C of insulations 1 hour, break and add thermoelectricity, furnace cooling, when temperature is down to 800 DEG C, close the large valve of high vacuum, foreline valve, diffusion pump, mechanical pump successively, cooling water pressure keeps 0.1-0.2MPa.This technique is state of the art, and therefore not to repeat here.
Open argon gas charging valve on body of heater, slowly inflate in stove.Treat that body of heater internal pressure is 10
-4during M Pa, stop inflation, close all valves, furnace cooling, when body of heater internal pressure is down to 0.85 × 10
-4during MPa, open argon gas charging valve on body of heater, continue slowly to inflate in stove, until body of heater internal pressure is 10
-4during M Pa, stop inflation, close all valves, continue furnace cooling.
When furnace temperature is cooled to about 60 DEG C, stop water coolant, break and vacate stove.Inspection product is all qualified.The whole vacuum annealing time is about 17 hours.Check thermoscreen and well heater, intact, alumina-ceramic part is intact.
Comparative example 1
Tantalum pipe is about 100kg shove charge, send after vacuumizing and add thermoelectricity, after 2 hours to 1200 DEG C of insulations, break and add thermoelectricity.Furnace cooling, when temperature is down to about 100 DEG C, closes vacuum system.When continuing to cool to the furnace about 60 DEG C, stop water coolant, break and vacate stove.Inspection product is all qualified.The whole vacuum annealing time is about 24 hours.Check thermoscreen and well heater, intact, alumina-ceramic part is intact.
Comparative example 2
Tantalum tubing is about 100kg shove charge, send and add thermoelectricity after vacuumizing, to 1200 DEG C of insulations 2 hours, then break and add thermoelectricity, close the large valve of high vacuum, foreline valve, diffusion pump, mechanical pump successively, cooling water pressure kept 0.1-0.2MPa.This technique is state of the art, and therefore not to repeat here.
Open argon gas charging valve on body of heater, slowly inflate in stove.When body of heater internal pressure is 0.09MPa, stop inflation, close all valves, furnace cooling.
When furnace temperature is cooled to about 60 DEG C, stop water coolant, break and vacate stove.Inspection product section is defective.The whole vacuum annealing time is about 13 hours.Check thermoscreen and well heater, thermoscreen warpage, well heater bends, and there is crackle local.Alumina-ceramic part comes off individually.
As can be seen from above embodiment and comparative example we, when using technical scheme of the present invention to anneal to tantalum niobium and alloy thereof, annealing time obviously shortens, and improves production efficiency, and qualified product; Thermoscreen and well heater simultaneously, intact, alumina-ceramic part is intact, does not damage equipment.
The foregoing is only preferred embodiment of the present invention, be not intended to limit protection scope of the present invention.All any amendments done within the spirit and principles in the present invention, equivalent replacement, improvement etc., be all included in protection scope of the present invention.
Claims (10)
1. a method of cooling for tantalum niobium and alloy vacuum annealing thereof, is characterized in that, the method comprises:
Material is loaded vacuum oven, and described material is selected from tantalum, tantalum alloy, niobium and niobium alloy;
Vacuum pumping is carried out to vacuum oven, when the vacuum tightness in vacuum oven reaches the vacuum tightness heating up and require, warming temperature is carried out to it;
When the temperature in vacuum oven reaches the temperature of thermal requirements, insulation operation is carried out to it;
After vacuum oven is incubated the scheduled time, cooling operation is carried out to it; When the temp. in vacuum furnace is down to 900 DEG C ~ 600 DEG C, vacuum pumping is stopped to vacuum oven and pass into rare gas element in vacuum oven;
When the temperature in vacuum oven is down to the tapping temperature of described material, vacate stove by broken for described material.
2. the method for claim 1, it is characterized in that, described cooling operation is charged cooling operation, and described method also comprises: after the temp. in vacuum furnace is down to 900 DEG C ~ 600 DEG C, before stopping vacuum pumping to vacuum oven, stop described charged cooling operation.
3. the method for claim 1, is characterized in that, described cooling operation is furnace cooling operation.
4. as the method in claims 1 to 3 as described in any one claim, it is characterized in that, when the temp. in vacuum furnace is down to 850 DEG C ~ 750 DEG C, vacuum pumping is stopped to vacuum oven and pass into rare gas element in vacuum oven.
5. as the method in claims 1 to 3 as described in any one claim, it is characterized in that, when the temp. in vacuum furnace is down to 800 DEG C, vacuum pumping is stopped to vacuum oven and pass into rare gas element in vacuum oven.
6. as the method in claims 1 to 3 as described in any one claim, it is characterized in that, described rare gas element is selected from argon gas, helium or its mixed gas.
7. as the method for cooling in claims 1 to 3 as described in any one claim, it is characterized in that, when the temp. in vacuum furnace is down to 900 DEG C ~ 600 DEG C, vacuum pumping is stopped to vacuum oven and in vacuum oven, passes into rare gas element, until vacuum oven internal pressure>=1 × 10
-6mpa, is preferably 10
-6~ 10
-1mpa, is more preferably 10
-4~ 10
-1during Mpa, stop passing into rare gas element operation.
8., as the method for cooling in claims 1 to 3 as described in any one claim, it is characterized in that, described in pass into rare gas element and be: disposablely pass into rare gas element, or repeatedly pass into rare gas element.
9., as the method in claims 1 to 3 as described in any one claim, it is characterized in that, described in vacuum oven, pass into rare gas element after comprise further: adopt rare gas element in cooling blower stirring vacuum furnace.
10., as the method for cooling in claims 1 to 3 as described in any one claim, it is characterized in that, by described material broken vacate stove before, comprise further: discharge rare gas element, then repeat to be filled with rare gas element.
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Application publication date: 20150819 |