CN101634005B - Titanium plate coil annealing process - Google Patents
Titanium plate coil annealing process Download PDFInfo
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- CN101634005B CN101634005B CN 200910157794 CN200910157794A CN101634005B CN 101634005 B CN101634005 B CN 101634005B CN 200910157794 CN200910157794 CN 200910157794 CN 200910157794 A CN200910157794 A CN 200910157794A CN 101634005 B CN101634005 B CN 101634005B
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Abstract
The invention provides a titanium plate coil annealing process which comprises the following steps: putting a titanium plate coil into an annealing furnace; replacing gas in the annealing furnace by inert gases until the positive pressure in the annealing furnace is 10-10,000Pa, heating the titanium plate coil to be higher than the recrystalization temperature at a heating speed of 50-200 DEG C/h, and keeping the temperature for 2-25h; cooling the titanium plate coil to the discharge temperature at a cooling speed of 10-150 DEG C/h under the condition of keeping the pressure in the annealing furnace to be 10-10,000Pa; and discharging the titanium plate coil out of the annealing furnace. The annealing process can improve the surface quality of the annealed titanium plate coil without cleaning an oxide layer after annealing, improve the product quality, lower the energy consumption and the material loss and improve the production efficiency.
Description
Technical field
The present invention relates to the thermal treatment process of metallic substance, definitely say, relate to and utilize bell type annealing furnace to handle titanium coiled sheet, especially cold rolling industrial pure titanium coiled sheet.
Background technology
Pure titanium has some characteristics different with steel, and for example crystal has the ppolymorphism body structure, is close-packed hexagonal structure below 882 ℃, and slip system is few, and anisotropy is obvious, and chemical property is active, and cold working working hardening effect is remarkable.Web-like or tabular titanium material (below be called the titanium coiled sheet) need anneal after cold rolling.The industrially pure titanium of cold deformation is according to the different recrystallization temperatures that have between 450-550 ℃ of impurity component and cold deformation rate, and annealing temperature should be higher than recrystallization temperature.The chemical property of titanium is active; High temperature is prone to down generate zone of oxidation with element reaction such as airborne O, H, N, makes the physicochemical property variation, except that hardness and fragility increase and plasticity and elasticity reduction; The adsorptivity of the industrially pure titanium under the high temperature is also stronger; Carbide and dust in surface residues after cold rolling and the annealing intensification atmosphere possibly be adsorbed to the surface, form the annealing blackspot, influence titanium coiled sheet surface quality thus.
Existing titanium coiled sheet annealing treating process comprises vacuum annealing or inert-free gas protection annealing.The flat 9-217157 of JP disclose a kind of vacuum annealing process: at first lehre is vacuumized, be heated to then more than 400 ℃ to annealing temperature, then be heated to 600-700 ℃ and be incubated under the situation of high-purity nitrogen charging into.Under the relative vacuum state, still there is harmful atmosphere in the stove, nitrogen also has a negative impact to the titanium coiled sheet surface quality after the annealing.Vacuum annealing process is high to the requirement of equipment, and security is lower, is inappropriate for the annealing that big volume weighs the titanium coiled sheet.Inert-free gas protection annealing is carried out in open environment, and there is zone of oxidation on the titanium coiled sheet surface after the annealing, and is of poor quality, needs the cleaning zone of oxidation after the annealing, has both increased materials consumption and workload, reduces production efficiency again.Therefore, people's expectation improves above-mentioned existing titanium plate coil annealing process.
Summary of the invention
For this reason, the purpose of this invention is to provide a kind of titanium plate coil annealing process, improve the titanium coiled sheet surface quality after annealing whereby, the zone of oxidation removal treatment after the cancellation annealing improves the quality of products, and cuts down the consumption of energy and spillage of material, enhances productivity.
For realizing this purpose, the present invention provides a kind of titanium plate coil annealing process, comprising:
A, the titanium coiled sheet is put into lehre;
B, use the inert gas replacement furnace gas, to furnace pressure be the 10-10000Pa malleation, with 50-200 ℃/hour rate of heating heating titanium coiled sheet to being higher than its recrystallization temperature and being incubated 2-25 hour;
C, under the condition that keeps furnace pressure 10-10000Pa, with 10-150 ℃/hour speed of cooling cooling titanium coiled sheet to tapping temperature;
D, the titanium coiled sheet is come out of the stove.
According to the present invention; Above-mentioned heat-processed can be carried out in two steps; Earlier the titanium coiled sheet is heated to 350-450 ℃ and be incubated 1-25 hour, then the titanium coiled sheet is heated above its recrystallization temperature and is incubated 2-25 hour with 50-200 ℃/hour rate of heating with 50-200 ℃/hour speed.
As everyone knows, the difference that the commercial titanium coiled sheet is looked its composition has different recrystallization temperatures, roughly between 450-550 ℃.The present invention stipulates for this reason, in step B, the titanium coiled sheet is heated above 550 ℃.Need not limit the upper limit of Heating temperature in principle, but cause the thick consideration of excessive grain from economy and the too high meeting of Heating temperature, preferred 750 ℃ is the Heating temperature upper limit.Preferred 580-750 ℃ Heating temperature scope.
In above-mentioned titanium plate coil annealing process; Preferably before the step B earlier with the nitrogen purging stove in 15-45 minute to replace furnace atmosphere; Use the inert gas replacement furnace atmosphere then, and/or preferred in the process of cooling of step C with in the nitrogen purging stove 15-45 minute, here; Nitrogen purging in the process of cooling is preferably in when the titanium coiled sheet reaches tapping temperature soon and carries out, and doing like this is in order to replace furnace atmosphere.In heat-processed, purging nitrogen earlier mainly is in order to save the consumption of rare gas element.
According to the present invention, preferably adopt bell type annealing furnace to carry out above-mentioned annealing process, it comprises inner cover, active heating mantles and active cooling cowl; This moment is in steps A; The titanium coiled sheet is hung into inner cover, in the heat-processed of step B, before the titanium coiled sheet being heated above recrystallization temperature and insulation with heating mantles; Earlier the titanium coiled sheet is heated to 350-450 ℃ and be incubated 1-25 hour with heating mantles, in this process with 20-120 rice
3/ hour flow rare gas element is fed inner cover.
Inert gas pressure is in prescribed level in the stove in order to keep, preferably in the heating of step B and insulating process all the time with 20-120 rice
3/ hour flow in stove, feed rare gas element such as argon gas.Like this, leak although furnace gas in heating and insulating process, possibly occur, above-mentioned pressurize measure can guarantee furnace pressure level up to specification, obtains good annealing coiled sheet quality thus.
In any one embodiment of above-mentioned titanium plate coil annealing process, in step C, be the 10-10000Pa malleation for keeping the lehre internal pressure, preferably with 1-20 rice
3/ hour flow rare gas element such as argon gas are fed lehre, for example the inner cover of bell type annealing furnace guarantees furnace pressure level up to specification thus, and then obtains good annealing coiled sheet quality.
According to titanium plate coil annealing process of the present invention, in above-mentioned process of cooling, can carry out slow cooling to the titanium coiled sheet earlier, then the titanium coiled sheet is quickly cooled to tapping temperature, can prevent the annealing bonding of titanium coiled sheet like this.Slow cooling can be adopted 10-50 ℃/hour speed of cooling and 1-5 hour cooling time.When carrying out annealing process with above-mentioned bell type annealing furnace, in above-mentioned process of cooling, still cover at heating mantles under the situation of inner cover and be with the heating mantles cooling earlier, with cooling cowl the titanium coiled sheet is cooled to tapping temperature then.Annealing process of the present invention can adopt the lehre of other type to implement.When the heating mantles with bell type annealing furnace carries out slow cooling, also can adopt 10-50 ℃/hour speed of cooling and 1-5 hour cooling time.Be preferably in and also feed rare gas element in the annealing process, to protect cooling.
In above-mentioned titanium plate coil annealing process,, can before steps A, carry out skimming treatment to titanium coiled sheet surface through the chemical bases washing method for obtaining better titanium coiled sheet surface quality.Annealing process according to the present invention is preferred for bell type annealing furnace the cold rolling industrial pure titanium coiled sheet being carried out anneal, can certainly be used to handle the titanium material that other is in cold working state or cold conditions, especially becomes the form of plate, band, line.
The present invention's regulation, in step B, rare gas element is fed lehre can carry out with heat temperature raising simultaneously, perhaps can feed rare gas element earlier, carries out heat temperature raising then.Perhaps, when the rare gas element feeding does not finish as yet, just can carry out heat temperature raising.Preferred 100-120 ℃/hour speed of cooling in step C.Also can adopt≤50 ℃/hour speed of cooling.Tapping temperature is determined on a case-by-case basis, and is chosen as 20-100 ℃ usually, preferably is lower than 50 ℃.
The present invention's regulation is come out of the stove from step B to the titanium coiled sheet, preferably exists rare gas element with protection titanium coiled sheet in the lehre all the time.Especially behind inert gas replacement, furnace pressure can remain 10-10000Pa.For this reason, preferably after gas displacement, mend rare gas element in each step before come out of the stove.
Titanium plate coil annealing process of the present invention preferably adopts bell type annealing furnace; But be characterized in the opening type inner cover, active heating mantles and the active cooling cowl that comprise that the available hydraulic pin compresses; Heating mantles is equipped with burner, is used for according to implementing annealing temperature control by the TP of lehre such as the temperature of thermocouple measurement.Certainly, the present invention also can adopt the lehre of other type.
In the present invention; The chemical ingredients National standard GB/T 3620.1-2007 of titanium coiled sheet; For example the titanium coiled sheet contain≤0.50% Fe ,≤0.08% C ,≤0.05% N ,≤0.015% H and≤0.48% O; And single amount≤0.10% and other unavoidable impurities of total amount≤0.40%, surplus is Ti.
In above-mentioned titanium plate coil annealing process, preferably adopt purity greater than 95% to 99.99999% argon gas as rare gas element.If purity of argon is less than or equal to 95%, then possibly have a negative impact to the titanium coiled sheet surface quality after annealing because of wherein being doped with oxygen.From economy, purity of argon is unsuitable too high, therefore selects 99.99999% as the upper limit.Preferred purity is the argon gas more than 99.9%.
Description of drawings
Below, specify embodiments of the invention in conjunction with accompanying drawing, wherein:
Fig. 1 is used to implement the synoptic diagram according to the bell type annealing furnace of titanium plate coil annealing process of the present invention;
Fig. 2 is the annealing process curve synoptic diagram according to the 2nd embodiment of the present invention.
Embodiment
The present invention provides titanium plate coil annealing process; Its available bell type annealing furnace is implemented; As shown in Figure 1; It comprises openable inner cover 1, active heating mantles and active cooling cowl, and heating mantles is furnished with a plurality of burners, is used for heating the titanium coiled sheet 3 that is placed into inner cover according to the temperature of being surveyed by the TP such as the thermopair of lehre.
Titanium plate coil annealing process of the present invention comprises: the titanium coiled sheet is put into lehre; Use rare gas element 2 displacement furnace atmosphere to furnace pressures to be the 10-10000Pa malleation, the titanium coiled sheet is heated above its recrystallization temperature and is incubated 2-25 hour with 50-200 ℃/hour rate of heating; Under the condition that keeps furnace pressure 10-10000Pa, cool off the titanium coiled sheet to tapping temperature with 10-150 ℃/hour speed of cooling; The titanium coiled sheet is come out of the stove.It is favourable in above-mentioned heating and insulating process and process of cooling, keeping in the stove inert gas pressure to be in prescribed level, can improve the surface quality of annealing product whereby.
Below, specifically describe the present invention in conjunction with a plurality of embodiment of annealing process of the present invention.
The 1st embodiment
The 1st embodiment of titanium roll bending annealing process of the present invention comprises: clean the titanium coiled sheet with conventional chemical bases washing method, so that skimming treatment is carried out on its surface; To pass through the titanium coiled sheet of skimming treatment and put into lehre; With in the nitrogen purging stove 15 minutes, with the displacement furnace air; Behind the nitrogen purging; Using purity is that 99.99% argon gas is thoroughly replaced furnace atmosphere; To furnace pressure be the 7000Pa malleation; At metathetical simultaneously, the titanium coiled sheet is heated to 390 ℃ and be incubated 2 hours, is heated to 620 ℃ and be incubated 2 hours with 150 ℃/hour rate of heating subsequently with 200 ℃/hour rate of heating; Under the condition that keeps furnace pressure 7000Pa, the titanium coiled sheet is cooled to about 50 ℃ with 100 ℃/hour speed of cooling; At the end of colling stages, with in the nitrogen purging stove 15 minutes; The titanium coiled sheet is come out of the stove.
The titanium coiled sheet of annealed processing can directly be sent to road, back manufacturing procedure, need not further to clear up titanium coiled sheet surface.
The 2nd embodiment
The 2nd embodiment of titanium roll bending annealing process of the present invention comprises: clean the titanium coiled sheet with conventional chemical bases washing method, so that skimming treatment is carried out on its surface; To pass through the titanium coiled sheet of skimming treatment and put into lehre; With in the nitrogen purging stove 45 minutes, with the displacement furnace atmosphere; Behind the nitrogen purging; Argon gas with 99.999% is thoroughly replaced furnace atmosphere; To furnace pressure be the 6000Pa malleation; With 150 ℃/hour rate of heating the titanium coiled sheet is heated to 410 ℃ and be incubated 1.5 hours subsequently, then is heated to 580 ℃ and be incubated 2 hours with 130 ℃/hour rate of heating, in above-mentioned heating and insulating process all with 30 meters
3/ hour flow feed above-mentioned argon gas; Under the condition that keeps furnace pressure 6000Pa, with 100 ℃/hour speed of cooling the titanium coiled sheet is cooled to 45 ℃, in process of cooling with 4 meters
3/ hour flow with argon gas the titanium coiled sheet is protected cooling; At the end of colling stages, with in the nitrogen purging stove 45 minutes; The titanium coiled sheet is come out of the stove.
Fig. 2 representes the annealing process curve of the 2nd embodiment, and the titanium coiled sheet of annealed processing can directly be sent to road, back manufacturing procedure, need not further to clear up titanium coiled sheet surface.
The 3rd embodiment
The 3rd embodiment of titanium roll bending annealing process of the present invention comprises: the titanium coiled sheet is put into lehre; With the nitrogen purging lehre inner 37 minutes, with the displacement furnace air; Behind the nitrogen purging; Argon gas with 99.99% is thoroughly replaced furnace atmosphere; To furnace pressure be the 10000Pa malleation; At metathetical simultaneously, the titanium coiled sheet is heated to 400 ℃ and be incubated 2 hours, then is heated to 650 ℃ and be incubated 3 hours with 170 ℃/hour rate of heating with 170 ℃/hour rate of heating; Under the condition that keeps furnace pressure 10000Pa, the titanium coiled sheet is cooled to 35 ℃ with 50 ℃/hour speed of cooling; At the end of colling stages, with in the nitrogen purging stove 30 minutes; The titanium coiled sheet is come out of the stove.
The titanium coiled sheet of annealed processing can directly be sent to road, back manufacturing procedure subsequently, need not further to clear up titanium coiled sheet surface.
The 4th embodiment
The 4th embodiment of titanium plate coil annealing process of the present invention can utilize above-mentioned bell type annealing furnace to implement, and this annealing process comprises: the inner cover of the titanium coiled sheet being put into lehre; With the nitrogen purging lehre inner 20 minutes, with the displacement furnace air; Thoroughly replace inner cover atmosphere with rare gas element, to furnace pressure be the 3000Pa malleation, at metathetical simultaneously, with heating mantles the titanium coiled sheet is heated to about 660 ℃ and be incubated 2 hours according to 100 ℃/hour rate of heating; Under the condition that keeps furnace pressure 3000Pa; Be with the heating mantles cooling; This moment with cooling time of 45 ℃/hour speed of cooling and 4 hours with about titanium coiled sheet slow cooling to 480 ℃; With rare gas element the titanium coiled sheet is protected cooling in cooling in the journey, with cooling cowl the titanium coiled sheet is cooled to room temperature according to 150 ℃/hour speed of cooling subsequently, in this process of cooling, use rare gas element to protect cooling; At the end of colling stages, with in the nitrogen purging stove 25 minutes; Hang out inner cover, the titanium coiled sheet is come out of the stove.Can directly be sent to later process through above-mentioned annealed titanium coiled sheet, need not further to clear up titanium coiled sheet surface, the annealing bonding also not occur.
In the above-described embodiments, before heating, mainly be in order to save argon gas consumption, and the end of colling stages mainly is in order to replace furnace atmosphere with nitrogen purging with nitrogen purging.
In the bell type annealing furnace that heats with heating mantles and be incubated, thermopair can be set, the burner on the heating mantles can be controlled annealing temperature according to the temperature that records thus.In annealing process of the present invention; Being preferably in and remaining furnace pressure in above-mentioned heating, insulation and the process of cooling is the 10-10000Pa malleation; Filling with inert gas in above-mentioned each step as necessary and practical situation are mended to stove for this reason; Obtain better titanium coiled sheet quality thus, the benefit inbound traffics of rare gas element can depend on the circumstances.In adopting band heating mantles refrigerative annealing process, the selection of speed of cooling and time can be looked factor such as batch, coiled sheet material, form and performance and decide.
Compared with prior art; The present invention has advantage and effect: compare with inert-free gas protection annealing; Through keeping malleation in the stove; When reducing rare gas element consumption; The outside air of avoiding being caused by reasons such as sealing, leakage, breakages gets in the stove and makes titanium coiled sheet and element reactions such as airborne O, H, N, can make the surperficial non-oxidation layer of titanium coiled sheet after the annealing thus, can directly send into next procedure; Omitted not only that the alkaline bath water behind the conventional annealing is quick-fried, pickling process, zone of oxidation machinery reconditioning and increase work efficiency thus, reduce production costs and energy consumption, minimizing environmental pollution, and fundamentally solved exist in the prior art, cause product physicochemical property variation, hardness increase, plasticity and problems such as elasticity reduction, fragility increase because of surface contamination layer.The present invention has also that technology is simple, flow process short, easy to operate, advantage such as control is easy.Compare with vacuum annealing, the simplified operation flow process reduces equipment requirements; Reduce operation easier; Improve the security of production process, avoid the existing titanium coiled sheet existing adhesion problem of annealing, can make the titanium coiled sheet product physicochemical property after the annealing satisfy the product standard requirement.
Claims (9)
1. titanium plate coil annealing process comprises:
A, the titanium coiled sheet is put into lehre;
B, when using inert gas replacement furnace gas to furnace pressure as the 10-10000Pa malleation, with 50-200 ℃/hour rate of heating the titanium coiled sheet is heated above its recrystallization temperature and is incubated 2-25 hour;
C, under the condition that keeps furnace pressure 10-10000Pa, with 10-150 ℃/hour speed of cooling cooling titanium coiled sheet to tapping temperature;
D, the titanium coiled sheet is come out of the stove;
It is characterized in that, in the heating and insulating process of step B, all the time with 20-120 rice
3/ hour flow feed rare gas element to lehre.
2. titanium plate coil annealing process according to claim 1 is characterized in that, before step B, earlier with nitrogen purging lehre 15-45 minute with the displacement furnace atmosphere, and/or in the process of cooling of step C, with interior 15-45 minute of nitrogen purging stove.
3. titanium plate coil annealing process according to claim 2 is characterized in that the heating of step B is so carried out, and at first the titanium coiled sheet is heated to 350-450 ℃ and be incubated 1-25 hour, then the titanium coiled sheet is heated above its recrystallization temperature and insulation.
4. titanium plate coil annealing process according to claim 2; It is characterized in that; The cooling of step C is so carried out; At first with 10-50 ℃/hour speed of cooling and 1-5 hour slow cooling cooling time titanium coiled sheet, this moment, rare gas element was passed into lehre, then to be higher than 50 ℃/hour speed of cooling cooling titanium coiled sheet to tapping temperature.
5. titanium plate coil annealing process according to claim 1 is characterized in that lehre is a bell type annealing furnace; Comprise inner cover, active heating mantles and active cooling cowl, in steps A, the titanium coiled sheet is hung into inner cover; In step B; Earlier the titanium coiled sheet is heated to 350-450 ℃ and be incubated 1-25 hour, then continues the titanium coiled sheet is heated above its recrystallization temperature and insulation, in the process of cooling of step C with heating mantles with heating mantles; Still cover at heating mantles and be with the heating mantles cooling under the situation of inner cover earlier, then the titanium coiled sheet is cooled to tapping temperature with cooling cowl.
6. titanium plate coil annealing process according to claim 5 is characterized in that, in the cooling of band heating mantles, adopts 10-50 ℃/hour speed of cooling and 1-5 hour cooling time.
7. titanium plate coil annealing process according to claim 1; It is characterized in that; Adopt purity greater than 95% to 99.99999% argon gas as rare gas element; And in the heat-processed of step B, earlier the titanium coiled sheet is warmed up to 350-450 ℃ and be incubated 1-25 hour, then the titanium coiled sheet is warmed up to and is higher than 550-750 ℃ and be incubated 2-25 hour with 50-200 ℃/hour speed with 50-200 ℃/hour speed.
8. according to each described titanium plate coil annealing process in the claim 1 to 5, it is characterized in that, in step C, for keeping furnace pressure 10-10000Pa, with 1 meter
3/ hour to 20 meters
3/ hour flow rare gas element is fed lehre.
9. according to each described titanium plate coil annealing process in the claim 1 to 5, it is characterized in that, before steps A, skimming treatment is carried out on the surface of titanium coiled sheet through the chemical bases washing method.
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| CN 200910157794 CN101634005B (en) | 2008-07-25 | 2009-07-24 | Titanium plate coil annealing process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810058727.X | 2008-07-25 | ||
| CN200810058728.4 | 2008-07-25 | ||
| CNA2008100587284A CN101322977A (en) | 2008-07-25 | 2008-07-25 | Coil cold rolling industrial pure titanium plate coil |
| CNA200810058727XA CN101323938A (en) | 2008-07-25 | 2008-07-25 | Process for cold rolling industry pure titanium coil annealing by cover-type annealing furnace |
| CNA2009100941269A CN101481785A (en) | 2009-02-24 | 2009-02-24 | Annealing process for cold rolled titanium sheet coil |
| CN200910094126.9 | 2009-02-24 | ||
| CN 200910157794 CN101634005B (en) | 2008-07-25 | 2009-07-24 | Titanium plate coil annealing process |
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| CN101634005A CN101634005A (en) | 2010-01-27 |
| CN101634005B true CN101634005B (en) | 2012-07-18 |
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| CNA200810058727XA Pending CN101323938A (en) | 2008-07-25 | 2008-07-25 | Process for cold rolling industry pure titanium coil annealing by cover-type annealing furnace |
| CN200910157798A Pending CN101634006A (en) | 2008-07-25 | 2009-07-24 | Titanium plate coil blowing and annealing process |
| CN200910157799A Pending CN101634007A (en) | 2008-07-25 | 2009-07-24 | Titanium plate coil pressure control annealing process |
| CN200910157800A Pending CN101634008A (en) | 2008-07-25 | 2009-07-24 | Titanium coiled sheet controlled cooling and annealing process |
| CN 200910157794 Active CN101634005B (en) | 2008-07-25 | 2009-07-24 | Titanium plate coil annealing process |
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| CNA200810058727XA Pending CN101323938A (en) | 2008-07-25 | 2008-07-25 | Process for cold rolling industry pure titanium coil annealing by cover-type annealing furnace |
| CN200910157798A Pending CN101634006A (en) | 2008-07-25 | 2009-07-24 | Titanium plate coil blowing and annealing process |
| CN200910157799A Pending CN101634007A (en) | 2008-07-25 | 2009-07-24 | Titanium plate coil pressure control annealing process |
| CN200910157800A Pending CN101634008A (en) | 2008-07-25 | 2009-07-24 | Titanium coiled sheet controlled cooling and annealing process |
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| CN101634007A (en) | 2010-01-27 |
| CN101634006A (en) | 2010-01-27 |
| CN101634005A (en) | 2010-01-27 |
| CN101634008A (en) | 2010-01-27 |
| CN101323938A (en) | 2008-12-17 |
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