CN1050413A - The meticulous titanium and the titanium alloy method for making that wait the axle microstructure - Google Patents
The meticulous titanium and the titanium alloy method for making that wait the axle microstructure Download PDFInfo
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Abstract
The present invention produces has the meticulous titanium or titanium alloy that waits the axle microstructure.Titanium, alpha titanium alloy or (alpha+beta) titanium alloy are with the amount hydrogenation of 0.02%-2wt%.Hydride material is carried out pre-treatment [promptly 700 ℃ (β point of inversion) above heating] and/or processing (be 450-950 ℃ or be higher than the β point of inversion, be lower than 1100 ℃ of processing down) in case of necessity.This material is aging 10-530 ℃ or 10-700 ℃ (be higher than under the β point of inversion and adding man-hour) then, and last dehydrogenation and recrystallization and the material that must have fine microstructure.
Description
The present invention relates to the titanium and the titanium alloy method for making of fatigue strength and excellent in workability, the particularly meticulous titanium, α iron alloy or (alpha+beta) titanium alloy method for making that wait the axle microstructure.
Titanium and alloy thereof are had many uses, and because of the ratio and the erosion resistance of its excellent strength/density can be used as space material, and it is used also in continuous expansion.The reason of heavy demand titanium and α and (alpha+beta) titanium alloy is intensity height and ductility, but the performance requriements in each field is very strict, aerospace field particularly, in being easy to cause the environment of hoop stress, use, except having good workability, also to have excellent fatigue strength.Therefore set up strict quality standard (as can be referring to AMS4967), to satisfy these requirements, the α particle of material must have the meticulous axle microstructure that waits.
Because restricted to foreign matter content in the titanium, so with microstructures such as conventional processing and thermal treatment can obtain, but be difficult to evenly make with extra care microstructure.
On the other hand, in conjunction with adopting hot-work and thermal treatment often can make the used product in above-mentioned field, it is different, and (can be plate, line, pipe, rod etc., they are made by α and (alpha+beta) titanium alloy.But the shortcoming of hot-work step is that to satisfy the appropriate thermal processing temperature scope of following two requirements too narrow: (1) guarantees to reach the extremely accurately good workability of shape, and (2) form in product and wait a microstructure.
And in the said temperature scope, microstructure is extremely responsive to temperature range, and for example, even temperature slightly raises, particle also can be grown, and therefore the microstructure after the processing becomes inhomogeneous.And any considerable change does not take place in the microstructure that hot-work forms.
Therefore proposed to make the method that waits axle microstructure α and (alpha+beta) titanium alloy, as seeing a kind of method of Japanese patent gazette NO.63-4914, wherein in a specific narrow temperature range, repeat heating and processing, seen a kind of preparation method among the Japanese patent gazette NO.63-4908 in addition, wherein hot-finished material heats under the temperature that is higher than the β point of inversion.Yet these methods reach axle microstructures such as the uniform, fine of material unsatisfactorily.And the former shortcoming also comprises and yields poorly the cost height.
Make in the titanium alloy temporary transient alloying element with hydrogen and seen following document with the technology of improving its workability and microstructure:
(1) U.Zwicker et al, US2892742(1959 published June 30)
This patent description Al content be 6% or above alpha titanium alloy can to make its hydrogen richness by hydrogenation be 0.05-1.0wt%, last to improve hot workability, vacuum dehydrogenation again, but do not mention refining microstructure.
（2）W.R.kerr et al.，“Hydrogen as ar alloying element in titanium（Hydrovac）”，Titanium，80，P.2477-2486
This piece paper illustrated and will can improve hot workability as the Ti-6Al-4V alloy hydride of the example of (alpha+beta) titanium alloy, and this is owing to reduced the β point of inversion, and fine microstructure can be provided.With 60% or lower calendering rate forge and carry out hot-work, forge and in low speed plunger activity system, carry out velocity of plunger 1.27 * 10
-3Or it is lower.That is to say that this processing is not practical complete processing, therefore, technology such as available hot rolling and carry out high strength processing.
(3) N.C.Birla et al., " Anisotropy control throngh the use of hydrogen in Ti-6Al-4V alloy ", Transactions of the Indian Institute of Metals, Vol.37, No.5, October 1984, P.631-635
This piece paper has illustrated that representing the Ti-6Al-4V alloy of (alpha+beta) titanium alloy to carry out hydrogenation β carries out hot rolling subsequently, can improve the anisotropy of tensile strength.But in this technology, 990 ℃ of homogenizing of hydrogenation plate 2 hours, and carry out 50% hot rolling at 730 ℃, and wherein pass through several passages, homogenizing was handled 10 minutes after every time hot rolling, and each calendering rate is 10%, and this just makes that this technology is inapplicable.
(4) D.Eylon et al., US4820360(1989 April 11)
This patent description the method for refining cast titanium alloy goods microstructure, wherein containing and heating casting in the hydrogenation atmosphere so that its hydrogenation in 780-1020 ℃, the hydrogenation casting is cooled to room temperature, wherein adopt the controllable speed of 5-40 ℃/min, and true in it the 650-750 ℃ of cooled hydrogenation casting of heating with dehydrogenation.
(5) D.Eylon et al., US4832760(1989 May 23)
This patent description the process for purification of pre-alloyed titanium alloy powder briquetting microstructure, comprising in hydrogeneous atmosphere, adding the hot wafering goods in 780-1020 ℃, to carry out hydrogenation, with 5-40 ℃ speed the briquetting goods are cooled to room temperature, and heat cooled hydrogenation briquetting goods down with dehydrogenation in 650-750 ℃ in a vacuum.
（6）W.R.Kerr，“The Effect of Hydrogen as a Temporary Alloying Element on the Microstructure and Tensile Properties of Ti-6Al-4V”，METALLURGICAL TRANSACTIONS A，Vol.16A，June 1985，P.1077-1087
Method comprises described in this piece paper, to represent the Ti-6Al-4V alloy hydride of (alpha+beta) titanium alloy, heat hydride alloy down at 870 ℃, to add thermalloy under 540-700 ℃ and carry out the eutectoid conversion, and under 650-760 ℃, will transform the alloy dehydrogenation, so that get a meticulous microstructure that waits.
Yet above-mentioned prior art does not all provide the enough meticulous axle microstructure that waits, and that is to say, industrially attempts stably to produce intensity, and when titanium that fatigue property and workability etc. are good and titanium alloy, this method can not be satisfactory.
The objective of the invention is to produce a meticulous microstructure titanium that waits with the degree that can not reach in the prior art, alpha titanium alloy and (alpha+beta) titanium alloy, and propose industrially can stably produce intensity, the method for the above-mentioned materials that fatigue property and workability etc. are good.
For achieving the above object, the present invention is constructed as follows.
Specifically, the present invention relates to titanium and α and (alpha+beta) titanium alloy method for making, it is characterized in that comprising reaching 0.02-2.0wt% hydrogenant material in 10-530 ℃ of aging its amount of hydrogenation, vacuum dehydrogenation then, and make the material recrystallization.In this case, aging before, hydride material can be carried out pre-treatment, heats cooling then under at 700 ℃ or higher temperature.And the present invention also proposes a kind of method, comprising 450-950 ℃ with 30% or higher calendering rate in the above-mentioned hydride material of (alpha+beta) zone processing, aging this material, and make aging material dehydrogenation and recrystallization.In addition, the present invention also comprises a kind of method, comprising above-mentioned hydride material is heat-treated, that is to say, and this material of heating under the temperature that is higher than the β point of inversion, and, carry out above-mentioned processing then with this heating material cooling, aging, and vacuum annealing.Titanium, the processing temperature of alpha titanium alloy and (alpha+beta) titanium alloy preferably is respectively 450-800 ℃, 600-950 ℃ and 550-900 ℃.The present invention also proposes a kind of method, comprising being higher than the β point of inversion and being lower than under 1100 ℃ the temperature with 30% or higher calendering rate machining and hydrogenating material, finish this processing in the single-phase zone of β, 10-700 ℃ of down aging this work material is then with this aging material vacuum annealing.In this case, aforesaid method can comprise a heat treatment step, comprising being higher than the β point of inversion and being lower than the above-mentioned hydride material of heating under 1100 ℃ the temperature, heating material is cooled to 400 ℃ or lower then.
Fig. 1-7 is microgram (* 500), and wherein Fig. 1-5 is corresponding to example of the present invention, and Fig. 6 and 7 is corresponding to comparative example.
The present invention can make titanium and α and the meticulous isometry of (alpha+beta) titanium alloy micro-structural, and need not conventional machining and heat treatment simultaneously, and provides the excellent material such as fatigue behaviour and machinability.
For solving the problems referred to above of prior art, the inventor has considered and has been easy to mix titanium and easy hydrogen from therefrom removing, and has carried out in this respect many researchs, found that the following fact.
(a) when titanium and α and (alpha+beta) titanium alloy when hydrogenation is then aging under quite low temperature, the titanyl compound will be in material subtly precipitation and in hydride, also initiation high density dislocation in zone around it. In order to reach this kind precipitation, hydrogen content is more high, and wears out and carry out for a long time at low temperatures, and the result is more good. This so that hydride so that thin form is made dispersed deposition in a large number, thereby make above-mentioned displacement density higher. When this kind material heats in vacuum, carry out again dehydrogenation and form the nuclear that is recrystallized in a large number from the dislocation of densification is regional simultaneously, so form the meticulous axle micro-structural that waits.
(b) when this material heat under suitable temp at (alpha+beta) two phase region or the single-phase zone of β, when cooling off then, hydrogen is dissolving more equably during heating, causes cooling period to form fine acicular Martin microstructure mutually from stabilization and the β that increases.This makes hydride more uniform and delicate deposit and introduces high density dislocation in hydride and peripheral region thereof simultaneously in follow-up weathering process, therefore can obtain more all even meticulousr recrystallization microstructure after final vacuum annealing.
(c) when titanium and α and the hydrogenation of (alpha+beta) titanium alloy, the hydrogen dissolving, even therefore suitable low-temperature region, the ratio with β phase of superior workability also can improve.
Therefore, in case of necessity after β thermal treatment, wherein material is being higher than heating cooling then under the β point of inversion temperature, carries out hot-work in (alpha+beta) zone being lower than under the used temperature of prior art.This can prevent to add the particle growth that occur man-hour in the prior art under the relatively-high temperature, and during this processing, also contains stress and gather and the hydride deposition, therefore introduces high density dislocation in material.In the follow-up weathering process, hydride deposits and the raising dislocation desity.When this makes follow-up vacuum annealing, in the recrystallization process of appearance, can obtain more meticulous and equiaxial microstructure.
(d) when titanium and α and the hydrogenation of (alpha+beta) titanium alloy, hydrogen is dissolved in the material and has reduced the β point of inversion.This makes the processing carried out in the β zone with superior workability to carry out being lower than under the used temperature of prior art.Therefore, the alligatoring of β particulate can be in the hot procedure that carry out in the β zone, prevented, and meticulous needle-like Martin's microstructure can be in the process of cooling after the β zone machines, formed.This is deposited meticulous hydride in follow-up weathering process, therefore granular micro-structure is made with extra care.
The present invention below is described in detail in detail.
The inventor is with the refining hydrogen richness of different microstructures, Heating temperature, and processing temperature, the calendering rate, and aging temperature carried out a series of tests, thus finished the present invention.
The object of the invention example of material comprises commercially available pure titanium, as JIS(Japanese Industrial Standards) as described in titanium, alpha titanium alloy is as Ti-5Al-2.5Sn, and (alpha+beta) titanium alloy, as Ti-6Al-4V.Also can adopt cast material,, be easy to bloom as ingot, hot rolling, hot-work material or cold-worked material that hot stamping etc. are handled, and powder compact etc.The reason of restriction hydrogen richness is as follows.When hydrogen richness was lower than 0.02wt%, then sedimentary hydride amount can not form the meticulous axle microstructure that waits that requires very little between aging time when subsequent anneal.On the other hand, when hydrogen richness surpassed 2wt%, hydride can a large amount of precipitations between aging time.But in this stage, material is easily crisp, and this brings problem when giving material processing, so that can not carry out follow-up vacuum annealing.Therefore, hydrogen richness is defined as 0.02-2wt%.Method for hydrogenation depends on hydrogenation when dissolving, thermal treatment etc. in the nitrogen atmosphere, but method for hydrogenation and condition are not had particular restriction.
The aging technique of following above-mentioned materials.
When aging temperature was lower than 10 ℃, hydride can deposit subtly, but needed just can finish precipitation for a long time, and this makes this temperature range industrial impracticable.On the other hand, when aging temperature surpassed 530 ℃, though can deposit in a large number, hydride can alligatoring.And when temperature was too high, hydride can dissolve on undesirable ground once more, therefore can not form the meticulous axle microstructure that waits that requires when subsequent anneal.Aging temperature to be defined as 10-530 ℃ thus.Although the hold-time is not specifically limited, should be 1 minute to 50 hours (the following short period of time of high temperature keeps, and keeps for a long time under the low temperature).The object lesson of aging method comprises material is heated to aging temperature and keeps under this temperature from room temperature; Material is remained under 10 ℃ or the higher room temperature; And with material from hydrogenation temperature, pretreatment temperature or processing temperature keep under this temperature after being cooled to aging temperature.
After above-mentioned the wearing out, carry out vacuum annealing at last with dehydrogenation and simultaneously with the material recrystallization.Annealing conditions is not had particular restriction, can under recrystallization typical conditions after the processing, carry out, but preferred annealing temperature should be low as far as possible.Specifically, annealing temperature and time preferably are respectively 500-900 ℃ and 100 hours or shorter.A certain amount of above residual hydrogen is to cause crisp reason and can make the product performance deterioration.Vacuum tightness is about 1 * 10
-1Torr or shorter decompression.Vacuum tightness is high more, and annealing time is short more.From actual angle, preferred decompression is for about 1 * 10
-4Torr, entrap bubble is a rare gas element, as argon gas.
The above-mentioned aging pre-treatment of carrying out in case of necessity before is described as follows.
As mentioned above, the microstructure that the pre-treatment before aging forms in the time of can making final vacuum annealing is more even and meticulousr.When pretreatment temperature was lower than 700 ℃, the β phasor seldom and form the poor effect of above-mentioned Martin's microstructure during refining microstructure.Therefore, pretreatment temperature is defined as 700 ℃ or higher.And be 700 ℃ or when higher, the β phasor increases and forms the single-phase zone of β according to hydrogen richness at pretreatment temperature, therefore can obtain above-mentioned more fine microstructure.The pretreatment temperature upper limit is not specifically limited, but preferred upper limit is about 1100 ℃ that this considers from heat treatment furnace surface oxidation and processing property.Although the hold-time is not had particular restriction, must at least 1 minute.At least the cooling after keeping can take stove cold, any method in the quenching of air cold-peace water, but preferred with higher speed of cooling.The refrigerative outlet temperature is preferably 530 ℃ or higher.
Aforesaid method of the present invention can be used for having the material of acicular microstructure, as above-mentioned commercially available pure titanium, and alpha titanium alloy and (alpha+beta) titanium alloy or above-mentioned welding material, brazing material and welded tube product.
Specifically, having the above-mentioned materials of bodkin shape microstructure and product, to be hydrogenated to hydrogen content be 0.02-2wt%.Hydride material is also carried out pre-treatment in case of necessity, heats postcooling under at 700 ℃ or higher temperature.Material previously treated with dehydrogenation and allow the material recrystallization simultaneously, therefore can form axle microstructure such as meticulous to improve fatigue property and workability etc. 10-530 ℃ of down aging final vacuum annealing.
Heat treatment material can carry out hydrogenation in nitrogen atmosphere.For welding construction material, can comprise indifferent gas, weld in the atmosphere as the mixture of argon gas and hydrogen, or will welding again after the material hydrogenation.
The processing in following (alpha+beta) zone of before aging, carrying out in case of necessity.
In the present invention, by rolling, extrude and technology such as exercise is processed.The hydrogenation of material impels (alpha+beta) zone to process at low temperatures as mentioned above.Hydrogen richness is high more, and above-mentioned trend is just big more.But (alpha+beta) zone is processed with a suitable temperature range in low temperature one side.Specifically, when temperature is lower than 450 ℃, during the processing crack can appear.On the other hand, when temperature is lower than 950 ℃, may form the β zone again according to material or hydrogen richness difference.Therefore, processing temperature is limited to 450-950 ℃.
The purpose material, i.e. titanium, (alpha+beta) titanium alloy and alpha titanium alloy are slightly different mutually on workability.With titanium, the order of (alpha+beta) titanium alloy and alpha titanium alloy, workability is variation slightly, and the β point of inversion raises in proper order with this.Therefore, respectively at 450-800 ℃ of low temperature, 550-900 ℃ and 600-950 ℃ of high temperature are processed in each (alpha+beta) zone for titanium preferably, (alpha+beta) titanium alloy and alpha titanium alloy.
According to whether carrying out β thermal treatment before the processing, can change the calendering rate in above-mentioned processing temperature zone.Do not carrying out (situation of claim (3)) in the β process of thermal treatment, with 30% or higher calendering rate just can form a meticulous recrystallization particle that waits by the full annealed that carries out after aging.
Carry out in advance (situation of claim (4)) in the β process of thermal treatment, above-mentioned calendering rate restriction just there is no need.Specifically, when hydride material heated postcooling under the temperature that is higher than the β point of inversion, material also became fine microstructure.Therefore, even the calendering rate is lower than 30% during this materials processing, also can make meticulous recrystallization particle by follow-up aging and vacuum annealing.Calendering rate 15% or more than, effect is very remarkable.
" calendering rate " speech means total calendering rate of one or many processing.
When carrying out the β conversion, material heats postcooling to form fine microstructure under the temperature that is higher than the β point of inversion.In this case, Heating temperature preferably should be low as far as possible.Hold-time is preferably 1-60 minute.Cooling can be cold through stove, and any technology in the quenching of air cold-peace water is carried out.But speed of cooling is high more, and the result is good more.When the refrigerative outlet temperature is lower than about 300 ℃ of β point of inversion, just can obtain fine microstructure.Process after heating more than the β point of inversion at material, method comprises in the process of cooling processes in above-mentioned processing temperature scope, the material reheat will be processed in the said temperature scope after maybe will being chilled to the material reheat of room temperature again in process of cooling, or material be remained in the Heating temperature scope a certain temperature in process of cooling and process in this temperature.
The upper limit to above-mentioned calendering amount does not have specific restriction, but and should the calendering amount can carry out between a common operational zone.In addition, to there not being special restriction process period yet.After the completion of processing, carrying out burin-in process behind the cool to room temperature or in process of cooling.In this case, speed of cooling is not had special restriction, but cooling speed temperature is higher, its effect better.After aging, aged material places vacuum to carry out aforesaid anneal.
Be described in the processing that carry out in the β zone now, before above-mentioned weathering process, process as required.
In this case, hydrogenation reduces the β point of inversion, to process in a certain temperature in the single-phase zone of the β with superior workability.
Exactly, processing is to carry out in the temperature that is higher than the β point of inversion, and finishes in the β zone.When temperature at the β point of inversion during with rising De Taigao, the chap of β particle, this makes the axle microstructure such as meticulous as the final purpose product be difficult to obtain.Reasoning in view of the above, Heating temperature are limited to below 1100 ℃.As above chat, in order to form meticulous needle-like Martin's microstructure in cooling, processing is finished in the β zone.
In the method described in the claim 8, the material after the hydrogenation is being higher than the temperature heating of β point of inversion, to carry out above-mentioned processing.In this case, consider in the microstructure of material to have comprised coarse particles, the calendering amount is limited in 30% or more more, so that refining coarse particles.
In the described method of claim 9, make the material preheater after the hydrogenation, i.e. the heating of temperature more than the β point of inversion, and be cooled to 400 ℃ or lower, and then more than the β point of inversion, process.In the case, carry out β thermal treatment, wherein consider in the microstructure of this material and contain coarse particles as pre-treatment step.Because microstructure is made with extra care by this processing, can be 30% or less in the above-mentioned calendering amount of carrying out man-hour that adds, but reach 15% or when more some more, its effect is significant when the calendering amount.
The term of Shi Yonging " calendering amount " means the total calendering amount in the one or many course of processing herein.
In the present invention, but cold as the cooling stove in the pretreated β thermal treatment, the arbitrary method in the quenching of air cold-peace water is implemented, but speed of cooling is high more, and is good more to the effect of refining microstructure.
Finish after the above-mentioned processing, make this material place vacuum to carry out above-mentioned aging and annealing.At this moment, opposite with the processing of carrying out in (alpha+beta) zone, the upper limit of its aging temperature can increase to 700 ℃, can shorten digestion time like this, but when aging temperature be 530 ℃ or when lower, can be more remarkable to the effect of the refining effect of microstructure.
In the present invention described above, appearance is slightly inhomogeneous in the material microstructure after vacuum annealing as mould because around former β granule boundary still leaves thick α phase, then can cool off annealing process more once or twice, with this microstructure of homogenizing.
In addition, in the present invention, treating processes of the present invention can repeat secondary or repeatedly.Can obtain a meticulousr microstructure that waits like this.
As mentioned above, each method of the present invention can both stably make on technical scale has meticulous titanium and the titanium alloy material that waits the axle microstructure, so that can stably provide above-mentioned has well intensity, the material of fatigue resistance and workability etc.
Use a Ti-6Al-4V plate (thick 4mm) to test as representational (alpha+beta) alloy, will narrate test-results below, this plate does not carry out with multiple different hydrogen richness and aging condition through the overaging pre-treatment.All for the examination materials under vacuum in 700 ℃ annealing 5 hours so that dehydrogenation and recrystallization.
Experiment condition and the evaluation result of the microstructure of the material that makes at last listed in the table I.Hydrogen richness is a 2.2%(weight) No. 25 material become very crisp, and when aging, split, therefore can not carry out follow-up vacuum annealing and handle.Fig. 1 is a microgram in one embodiment of the present of invention (in the table 1 No. 14), wherein, have 0.9%(weight) hydrogen content and as a kind of material of the representative example of microstructure 500 ℃ aging 8 hours down, in a vacuum in 700 ℃ of annealing 5 hours, make this material dehydrogenation whereby then.Fig. 6 is the microgram of a contrast material, and this contrast material is to make with recrystallization by the anneal of material after repeating to heat with hot rolling, making above-mentioned thermal treatment then under the situation of hydrogenation not.This shows,, can obtain a kind of meticulous material that waits the axle microstructure that has according to the present invention.
Titanium (JIS2 level) and Ti-5Al-2.5Sn alloy have also been carried out as experiment same as above, thus be, as final step and the annealing of carrying out in a vacuum is that this material was kept 1 hour down at 600 ℃.Experiment condition and the results are shown in table 2 and the table 3 as can be seen, can reach and top described identical effect from the result who lists.
Table 1
The experimental result of Ti-6Al-4V alloy
Table 2
The experimental result of titanium (JIS rank 2)
Table 3
The experimental result of Ti-5Al-2.5Sn
Experimentize as the representative of (alpha+beta) titanium alloy with a Ti-6Al-4V plate (thick 4mm), will narrate its experimental result below, except that the hydrogenation amount with aging condition is different, this plate passes through differing temps pre-treatment.All are for trying material all in a vacuum in 700 ℃ of annealing 5 hours, so that dehydrogenation and recrystallization.
Experimental temperature and the evaluation result of the microstructure of the material that makes at last listed in table 4.A kind of hydrogen richness is a 2.2%(weight) material (in the table 4 No. 24) become very crisp, and in aging cracking, so can not carry out vacuum annealing.Fig. 2 is a microgram in the one embodiment of the invention, wherein, its hydrogen content is a 1.0%(weight) and as a kind of material of a representative example of this microstructure 830 ℃ of pre-treatment, 500 ℃ aging 8 hours down, and in a vacuum in 700 ℃ of annealing 5 hours, so that dehydrogenation and recrystallization.Fig. 6 is a kind of microgram of contrast material, and this contrast material is not have under the hydrogenant situation, by repeating to heat with hot rolling, making anneal of material through above-mentioned processing so that its recrystallization is made then.Thus, can make a kind of meticulous material that waits the axle microstructure that has according to the present invention.
Carried out experiment same as described above to titanium (JIS2 level) with as the Ti-5Al-2.5Sn of the representative example of alpha titanium alloy, different is, as final step and the anneal of in a vacuum titanium being carried out is that this material was kept 1 hour down at 600 ℃.Its experiment condition and the results are shown in table 5 and 6.From these results, as can be seen, can obtain the result identical with above-mentioned experiment.
Table 4
Experimental result (having carried out pre-treatment) to the Ti-6Al-4V alloy
A collection of Ti-6Al-4V alloy sheets as the representative of (alpha+beta) titanium alloy has been carried out hydrogenation, so that their hydrogen richness be respectively 0.01%, 0.05%, 0.2%, 0.5%, 0.9%, 1.5% and 2.2%(weight), make each piece plate all in 500 ℃, 600 ℃, 700 ℃ and 800 ℃ heating down, carrying out hot rolling then, to make its calendering amount be 30%, 60%, 70% and 80%.After rolling, these materials are cooled to room temperature, are heated to 500 ℃, keep 8 hours under this temperature so that wear out, then 1 * 10
-4In the vacuum of torr in 700 ℃ the heating 1 hour so that its dehydrogenation and recrystallization.
To this through hot rolling, aging and in a vacuum the result that estimates of the microstructure of the material of anneal list in table 7-12.Through hydrogenation so that its hydrogen richness be 0.05%, 0.2%, 0.5%, 0.9% and 1.5%(weight) and under 600 ℃, 700 ℃ and 800 ℃, follow its calendering amount be 30% or bigger hot rolled material have axle microstructure such as meticulous.Fig. 3 is the microgram of a representative example, and wherein, its hydrogen richness is a 0.2%(weight) a kind of material under 750 ℃, carry out hot rolling, its calendering amount is 80%.When having carried out hot rolling and subsequently behind the cool to room temperature, its hydrogen richness is a 2.2%(weight) a kind of material become very crisp, this makes processing subsequently become impossible.
Fig. 7 is a kind of microgram of contrast material, and this contrast material is by ordinary method, and promptly recrystallization makes by with 80% calendering amount not hydrogenous Ti-6Al-4V alloy being carried out under 950 ℃.
Compare with the material that makes with ordinary method, the material that makes by the present invention has meticulousr axle microstructure and superior fatigue resistance and the workability of waiting.
Making its hydrogen richness is 0.2%(weight) hydrogenation a collection of Ti-6Al-4V ((alpha+beta) type) plate carry out β thermal treatment, promptly, under above-mentioned hydrogen richness, in 850 ℃ and 950 ℃ of heating being higher than the β transformation point, air cooling is to room temperature again, be 22%, 40%, 60% and 80% o'clock in the calendering amount then, in 500 ℃, 600 ℃, 700 ℃, 750 ℃ and 800 ℃ of following hot rollings.After the hot rolling, make this batch of material be cooled to room temperature, 500 ℃ of heating, kept 8 hours so that aging, and 1 * 10 in this temperature
-4In the vacuum of torr in 700 ℃ the heating 1 hour, to make it dehydrogenation and recrystallization.The evaluation result of the microstructure of above-mentioned materials is listed in table 13 and 14.All these are all having axle microstructures such as meticulous through the hot rolled material under 600 ℃, 700 ℃, 750 ℃ and 800 ℃ under all calendering amounts.
Embodiment 5
(1) hydrogenation Ti-6Al-4V alloy ((alpha+beta) type) plate with different hydro content carries out β thermal treatment, that is, corresponding to above-mentioned hydrogen richness, make it be higher than the temperature heating of transformation point, and air cooling is to room temperature then.Material after this thermal treatment and above-mentioned without the heat treated material of β 750 ℃ of following hot rollings, its calendering amount is 60%, to make the plate of thick 4mm.Then, these plates are aging under different condition, and 1 * 10
-4In the vacuum of torr in 730 ℃ the heating 5 hours, to make it dehydrogenation and recrystallization.The granularity of the finished product and aspect ratio are listed in the table 15 with β thermal treatment temp and aging condition.Fig. 4 is a microgram of No. 16 material of the present invention that be shown in Table 15.A kind of hydrogen richness be the material of 2.2%(weight also under these conditions through hot rolling, but it is very crisp to become after this material cooled, so that can not carry out follow-up processing.
Obviously, can make a kind of (alpha+beta) titanium alloy by the present invention with meticulous microstructure such as axle such as grade.
(2) JIS2 level titanium is heat-treated so that make it aging, then 1 * 10 by the mode in above-mentioned (1)
-4In the vacuum of torr in 630 ℃ annealing 5 hours, to make it dehydrogenation and recrystallization.It the results are shown in table 16.Can be obvious from these results, can make titanium according to the present invention with meticulous microstructure such as axle such as grade.
(3) make of the representative of Ti-5Al-2.5Sn alloy, it is handled, by the mode described in above-mentioned (1) until finishing last processing as alpha titanium alloy.It the results are shown in table 17.From these results as can be seen, can make alpha titanium alloy by the present invention with meticulous microstructure such as axle such as grade.
Table 15
Experimental result to the Ti-6Al-4V alloy
Embodiment 6
(1) a Ti-6Al-4V alloy sheets of representative (alpha+beta) titanium alloy is in 1 atmospheric nitrogen atmosphere, in 800 ℃ of heating 1-40 hour, carry out hot rolling under the temperature that is shown in Table 18 to make it to have, making the calendering amount is 60%, to make the slab of a collection of thick 6mm.After the hot rolling, make these plates be cooled to room temperature, 500 ℃ keep making it to wear out in 8 hours and under vacuum in 700 ℃ of annealing 5 hours, to make it dehydrogenation and recrystallization.
Observed the microstructure of the middle portion of each material, it the results are shown in table 18, by discovery, by make hydrogen content be 0.25%, 1.6% and 2.1%(weight) material in the β zone in 910 ℃ and 1000 ℃ heating and make its hot rolling and the prepared material in aging back has the axle microstructure such as meticulous of requirement.
By making its hydrogen richness is 0.25%(weight) a kind of material 910 ℃ of following hot rollings, under 500 ℃ to this hot rolling after material carry out 8 hours aging and in vacuum, make this aging after anneal of material, a representational microstructure of the material after above-mentioned processing is shown among Fig. 5.Hydrogen richness is low to moderate and all produces the microstructure that requires under 0.006% any temperature of material.Its hydrogen richness be 0.25%, 1.6% and 2.1%(weight) the microstructure of material be refined to a certain degree through 1100 ℃ of hot rollings, but the microstructure that can not obtain requiring from these materials, this is because the β particle of beginning is thick.Hydrogen richness is to ftracture in 2.1% the material treating processes after aging.
(2) a Ti-6Al-4V alloy block of representative (alpha+beta) titanium alloy is under nitrogen atmosphere under 1 normal atmosphere, in 850 ℃ of heating 2-30 hour, to prepare a collection of hydride material that its hydrogen richness is shown in table 19, and do hot stamping in 950 ℃ of calendering amounts with 80%, be the garden shape rod of 40mm with the preparation diameter.After the hot stamping, make this garden rod be cooled to room temperature, under temperature shown in the table 19, keep 8 hours then to make it aging.After this, this garden rod is in a vacuum in 750 ℃ of annealing 15 hours, to make it dehydrogenation and recrystallization.Observed the microstructure of each material middle portion.Shown in table 19, when aging temperature is 50 ℃, 300 ℃ and 500 ℃, its hydrogen richness be 0.21%, 1.3% and 2.2%(weight) material production a meticulous microstructure that waits that requires.Its hydrogen richness is low to moderate 0.007%(weight) material under any aging temperature, microstructures that produce to require all.For the material of any hydrogen richness, after aging under 0 ℃, has a kind of uneven microstructure: after aging under 800 ℃, then have an a kind of thick microstructure that waits.Its hydrogen richness is a 2.2%(weight) the treating processes of material after aging in ftracture.
JIS2 level industrially pure titanium also carries out as following processing, that is, wear out by same way as of describing in (2), then 1 * 10
-4In 650 ℃ of annealing 3 hours,, find that the gained result is in the vacuum of torr,, can obtain having the meticulous pure titanium of JIS2 level that waits the axle microstructure by the present invention to make it dehydrogenation and recrystallization.
Embodiment 7
A kind of Ti-5Al-2.5Sn alloy block of representing alpha titanium alloy is under 1 atmospheric nitrogen atmosphere, in 850 ℃ of heating 1-24 hour, to prepare a collection of hydride material that its hydrogen richness is shown in Table 20, carry out β thermal treatment then, that is, 1000 ℃ the heating 2 hours and subsequently air cooling to room temperature.After this, the calendering calorimetric with 40% under temperature shown in the table 20 of this batch of material is rolled, to make the slab of 8mm.After the hot rolling, these plates are cooled to 500 ℃, keep 8 hours to make it aging under this temperature.Then, the plate after making this aging is in a vacuum in 700 ℃ of annealing 10 hours, to make it dehydrogenation and recrystallization.
Observed the microstructure of the middle portion of each material, it the results are shown in table 20, find among logical these results, by to its hydrogen richness be 0.20%, 1.4% and 2.2%(weight) material under 940 ℃ and 1020 ℃, heat a microstructure such as meticulous that has requirement with aging then prepared those plates of hot rolling in the β zone.Its hydrogen richness is low to moderate 0.007%(weight) the microstructure that under any temperature, all produce to require of material.By at 1120 ℃ of its hydrogen richnesss of following hot rolling be 0.20%, 1.4% and 2.2%(weight) material, its microstructure is refined to certain certain degree.But from their initial β particle is thick.Its hydrogen richness is a 2.2%(weight) the operation of material after aging in ftracture.
Embodiment 8
Make a collection of Ti-6Al-4V alloy sheets (thick 4mm) the opposite side welding of representative (alpha+beta) titanium alloy, make the welding assembly material that makes thus change the experiment (digestion time is 8 hours) of hydrogen richness and aging temperature.All these materials are all in a vacuum in 700 ℃ of annealing 5 hours, to make it dehydrogenation and recrystallization.
Experiment condition and the evaluation result of the microstructure in the welding metal of the welding thing that obtains at last and heat effect district listed in table 21.Its hydrogen richness is a 2.1%(weight) material very crisp after aging, therefore be difficult to handle, it makes subsequent annealing not carry out.Therefore obviously, can make material by the present invention with meticulous microstructure such as axle such as grade.
In the foregoing description 1 and 2, experiment is carried out at flaky material, but to difform material such as plate, rod and line, cast material and powder compact, has all observed identical effect.In the foregoing description 3-7, experiment is to carry out at the hot stamping of the hot rolling of plate and piece, but base bar and powder base have also been observed identical effect when replacing the thermal shocking method as work material and with forging method.
The present invention is not limited in the foregoing description.
Claims (11)
1, the titanium and the titanium alloy material method for making that have axle microstructure such as meticulous, comprising titanium hydride in 0.02%-2wt% hydrogen, alpha titanium alloy or (alpha+beta) titanium alloy, 10-530 ℃ of aging hydride material also allows this material vacuum dehydrogenation, makes the material recrystallization simultaneously.
2, claim 1 method for making, titanium hydride wherein, alpha titanium alloy or (alpha+beta) titanium alloy carry out pre-treatment, wherein in 700-1100 ℃ of heating postcooling, carry out said aging afterwards.
3, claim 1 method for making, titanium hydride wherein, alpha titanium alloy or (alpha+beta) titanium alloy (alpha+beta) zone in 450-950 ℃ with 30% or higher reduction ratio processing after carry out said aging.
4, claim 1 method for making, titanium hydride wherein, alpha titanium alloy or (alpha+beta) titanium alloy are heat-treated, and wherein material is processed postcooling under the temperature that is higher than the β transformation efficiency, processes in (alpha+beta) zone at 450-950 ℃, carries out said aging afterwards.
5, claim 3 or 4 method for makings, wherein (alpha+beta) regional titanium processing temperature is 450-800 ℃.
6, claim 3 or 4 method for makings, wherein (alpha+beta) region alpha titanium alloy processing temperature is 600-950 ℃.
7, claim 3 or 4 method for makings, wherein (alpha+beta) zone (alpha+beta) titanium alloy processing temperature is 550-900 ℃.
8, claim 1 method for making, titanium hydride wherein, alpha titanium alloy or (alpha+beta) titanium alloy be in being higher than the β point of inversion, is lower than under 1100 ℃ the temperature with 30% or higher reduction ratio is processed and finish in the single-phase zone of β, wears out under 10-700 ℃ then.
9, claim 1 method for making, titanium hydride wherein, alpha titanium alloy or (alpha+beta) titanium alloy are being higher than the β point of inversion, be lower than under 1100 ℃ the temperature heating postcooling to 400 ℃ or lower and heat-treat, this heat treatment material is being higher than the β point of inversion, is lower than under 1100 ℃ the temperature processing and finishes in the single-phase zone of β.Under 10-700 ℃, carry out said aging then.
10, claim 1 or 2 method for makings, wherein the acicular microstructure material is with amount hydrogenation and 10-530 ℃ of down aging final vacuum annealing of 0.02-2wt%.
11, claim 10 method for making, wherein said acicular microstructure is the acicular microstructure that comprises the welding construction material of said material.
Applications Claiming Priority (8)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP198637/89 | 1989-07-31 | ||
| JP19863789 | 1989-07-31 | ||
| JP89-198637 | 1989-07-31 | ||
| JP266310/89 | 1989-10-16 | ||
| JP89-266310 | 1989-10-16 | ||
| JP89-336095 | 1989-12-25 | ||
| JP336095/89 | 1989-12-25 | ||
| JP33609589A JPH03197655A (en) | 1989-12-25 | 1989-12-25 | Production of titanium alloy having fine grain structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1050413A true CN1050413A (en) | 1991-04-03 |
| CN1023495C CN1023495C (en) | 1994-01-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90106559 Expired - Fee Related CN1023495C (en) | 1989-07-31 | 1990-07-31 | Process for preparing titanium and titanium alloy materials having fine equiaxed microstoucture |
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| CN (1) | CN1023495C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912972A (en) * | 2010-08-05 | 2010-12-15 | 成都韵智科技有限公司 | Preparation method of superfine Ti powders |
| CN107406911A (en) * | 2015-02-10 | 2017-11-28 | 冶联科技地产有限责任公司 | The method for producing titanium or titanium alloy product |
| CN109252121A (en) * | 2018-10-30 | 2019-01-22 | 江苏希诺实业有限公司 | A kind of processing method of the pure titanium article surface acicular crystal decorative pattern of thin-walled |
| CN113039299A (en) * | 2018-11-15 | 2021-06-25 | 日本制铁株式会社 | Titanium alloy wire rod and method for manufacturing titanium alloy wire rod |
| CN113874534A (en) * | 2019-03-16 | 2021-12-31 | 普拉西斯粉末技术股份有限公司 | Microstructure improvement of titanium alloy |
-
1990
- 1990-07-31 CN CN 90106559 patent/CN1023495C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912972A (en) * | 2010-08-05 | 2010-12-15 | 成都韵智科技有限公司 | Preparation method of superfine Ti powders |
| CN101912972B (en) * | 2010-08-05 | 2011-12-28 | 成都韵智科技有限公司 | Preparation method of superfine Ti powders |
| CN107406911A (en) * | 2015-02-10 | 2017-11-28 | 冶联科技地产有限责任公司 | The method for producing titanium or titanium alloy product |
| US10407745B2 (en) | 2015-02-10 | 2019-09-10 | Ati Properties Llc | Methods for producing titanium and titanium alloy articles |
| CN107406911B (en) * | 2015-02-10 | 2019-09-24 | 冶联科技地产有限责任公司 | The method for producing titanium or titanium alloy product |
| CN110592402A (en) * | 2015-02-10 | 2019-12-20 | 冶联科技地产有限责任公司 | Method for producing titanium and titanium alloy products |
| CN109252121A (en) * | 2018-10-30 | 2019-01-22 | 江苏希诺实业有限公司 | A kind of processing method of the pure titanium article surface acicular crystal decorative pattern of thin-walled |
| CN109252121B (en) * | 2018-10-30 | 2021-07-20 | 希诺股份有限公司 | Processing method of needle-shaped crystal patterns on surface of thin-wall pure titanium product |
| CN113039299A (en) * | 2018-11-15 | 2021-06-25 | 日本制铁株式会社 | Titanium alloy wire rod and method for manufacturing titanium alloy wire rod |
| CN113039299B (en) * | 2018-11-15 | 2022-07-19 | 日本制铁株式会社 | Titanium alloy wire rod and method for manufacturing titanium alloy wire rod |
| CN113874534A (en) * | 2019-03-16 | 2021-12-31 | 普拉西斯粉末技术股份有限公司 | Microstructure improvement of titanium alloy |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1023495C (en) | 1994-01-12 |
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