CN103562421A - Pure titanium sheet having excellent balance between press formability and strength and excellent corrosion resistance, and process for manufacturing same - Google Patents
Pure titanium sheet having excellent balance between press formability and strength and excellent corrosion resistance, and process for manufacturing same Download PDFInfo
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- CN103562421A CN103562421A CN201280025980.XA CN201280025980A CN103562421A CN 103562421 A CN103562421 A CN 103562421A CN 201280025980 A CN201280025980 A CN 201280025980A CN 103562421 A CN103562421 A CN 103562421A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
- F28F21/08—Constructions of heat-exchange apparatus characterised by the selection of particular materials of metal
- F28F21/081—Heat exchange elements made from metals or metal alloys
- F28F21/086—Heat exchange elements made from metals or metal alloys from titanium or titanium alloys
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F3/00—Plate-like or laminated elements; Assemblies of plate-like or laminated elements
- F28F3/02—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations
- F28F3/04—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations the means being integral with the element
- F28F3/042—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations the means being integral with the element in the form of local deformations of the element
- F28F3/046—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations the means being integral with the element in the form of local deformations of the element the deformations being linear, e.g. corrugations
Abstract
A pure titanium sheet contains 0.02 to 0.10% of Fe and 0.04 to 0.20% of O, the balance consisting of titanium and unavoidable impurities, and the Fe content and the O content satisfying the relationship (1): [O content (mass %)] + 0.12*[Fe content (mass %)] = 0.050.In the pure titanium sheet, the area fraction of regions that exhibit schmid factors of {11-22}<11-23 > twin of 0.45 or more is at least 43%, each Schmid factor being determined with the axis set in the direction of rolling at a position corresponding to one-fourth of the sheet thickness. Further, the pure titanium sheet has a volume fraction of beta phase of 0.3% or less.
Description
Technical field
The present invention relates to press formability and the balance of intensity and pure titanium plate and the manufacture method thereof of excellent corrosion resistance under room temperature, in detail, even if relate at room temperature also have intensity (tensile strength) more than 343MPa, and have both pure titanium plate and the manufacture method thereof of excellent press formability and slit and corrosion resistant.In addition, the present invention relates to carry out stamping and manufacture the method for the heat exchange component of plate-type heat exchanger for so pure titanium plate.
Background technology
Titanium utilizes its excellent erosion resistance, press formability, specific tenacity, light weight etc., for example, at the structured material of airplane parts, chemical device member, coastal portion (particularly promoting such bay structured material with contact with sea water corrosion), automobile, general in the wide in range field such as building materials, purposes.
In recent years, in various fields, all require to reduce carrying capacity of environment and energy-saving, be considered to light and strong titanium also in order to tackle the demand of further light weight, thin-walled property and to expect high strength.In addition, at the exterior trimming parts of the fuselage of mobile telephone, laptop computer, photographic camera etc., spectacle frame, the formation material of plate-type heat exchanger, the dividing plate of fuel cell, family's electrical article, carry with in machine direction member etc. and be also used, further require the raising of plasticity.
Be used for this pure titanium plate with the specification specifies of JIS H4600, according to the impurity level of Fe, O etc. and intensity etc., have the grade of JIS1 class, 2 classes, 3 classes etc.Its grade more increases, and minimum intensity is higher, according to purposes, distinguishes and uses.
The low situation of the concentration of Fe and O as JIS1 class, although intensity is low, ductility is high, therefore in always requirement, uses the pure titanium plate of JIS1 class in having the member of high formability.
One of purposes of for example using at most among pure titanium plate, can enumerate plate-type heat exchanger (PHE:Plate type Heat Exchanger), in being applicable to the pure titanium plate of this purposes, from improving the viewpoint of rate of heat exchange, generally in order to expand heat exchange useful area, and carry out stamping (the anisotropic shaping that swells) with cold conditions, become complicated corrugated plate shape, for former material, exposed to the open air in extremely harsh extruding environment.In the face of harsh so stamping condition and the pure titanium plate that is utilized, what in specification, use is the pure titanium of the soft JIS1 class that is the most easily shaped.
Yet, the rate of heat exchange of heat exchanger improves, be not limited to the shape according to above-mentioned such heat exchanger itself, such as flow increase that utilizes thermophore (or refrigeration agent) etc., also can realize, because its requirement is had to high resistance to pressure, so require higher intensity and excellent plasticity for pure titanium plate.
As the high pure titanium plate of intensity, use Fe, JIS2 class and 3 classes that O concentration is high.Yet Fe, O concentration more high strength are just higher, but plasticity variation can not make high strength and high formability exist side by side in the prior art.In addition, due to its manufacturing processed, the high temperature and humidity environment that corrosion easily occurs in environment for use is inferior, and the crevice corrosion of Ti product becomes problem.
The means that improve as the press formability that makes pure titanium plate, for example, proposing has the tissue (patent documentation 1) of controlling titanium, or makes Ti Alloying (patent documentation 2).But these technology are that the plasticity that the titanium of usining as object has other a pure titanium plate of intensity (yield strength) level that is equivalent to JIS1 class rises to order, if but improve intensity rank, can't see the raising of plasticity.
The means that improve as the press formability that makes the pure titanium plate that intensity rank is high, proposing has the content of adjusting Fe, O, and controls the technology (patent documentation 3) of the crystal grain diameter of titanium.But, only control the crystal grain diameter of Fe and O content and titanium, be difficult to realize the balance of press formability and intensity.
In addition as above-mentioned, in recent years, although that the Application Areas of pure titanium plate spreads all over scope is wide, while using, require the further raising of slit and corrosion resistant under corrosive environment.
Titanium plate as slit and corrosion resistant is improved discloses and makes pure titanium plate surface attachment platinum group metal element in patent documentation 4.But platinum group metal element is expensive, the problem that has manufacturing cost to uprise is difficult to general.
In addition, as the technology that makes the balance raising of intensity and press formability, in patent documentation 5, disclose the titanium alloy sheet of a kind of Cu of being added with, Ni, Mo.If but add alloying constituent, productivity reduces, and is not suitable for the production of industrialized scale.About erosion resistance, there is no concrete disclosing in addition yet.
So, not yet provide the balance of press formability under room temperature and intensity excellent, but also have both the pure titanium plate of excellent slit and corrosion resistant.
Look-ahead technique document
Patent documentation
Patent documentation 1: TOHKEMY 2004-285457 communique
Patent documentation 2: TOHKEMY 2002-317234 communique
Patent documentation 3: TOHKEMY 2009-228092 communique
Patent documentation 4: Japanese Patent Publication 49-31610 communique
Patent documentation 5: TOHKEMY 2010-236067 communique
Summary of the invention
The present invention forms in view of above-mentioned existing problem, and its object is, a kind of pure titanium plate and manufacture method thereof with the balance of press formability and intensity and this specific character of erosion resistance (slit and corrosion resistant) excellence is provided.In detail, just be to provide a kind of pure titanium plate and manufacture method thereof with following characteristic, at room temperature there is tensile strength more than 343MPa, press formability (anisotropic swelling is shaped and isotropic ductility that swells and be shaped) excellence in addition, in addition also excellence of slit and corrosion resistant.
Can solve the present invention of above-mentioned problem, the balance of press formability and intensity and the pure titanium plate of excellent corrosion resistance, it will be intended to, the meaning that contains Fe:0.02～0.10%(" quality % ", relate to chemical composition below all with), O:0.04～0.20%, surplus consists of titanium and inevitable impurity, the content of described Fe and described O meets following formula (1), and the area occupation ratio that the schmid factor of { 11-22 } < 11-23 > twin crystal that the rolling direction of thickness of slab 1/4 position of take is axle system is more than 0.45 region is as more than 43%, in addition the volume fraction of β phase is below 0.3%.。
［ O content (quality %) ］+0.12 * ［ Fe content (quality %) ］ >=0.050 ... (1)
Manufacture method as the balance of above-mentioned press formability and intensity and the pure titanium plate of excellent corrosion resistance, recommend following mode: through the operation of hot rolling, process annealing, cold rolling, final annealing, and after described process annealing, carry out the oxide skin on pure titanium plate surface and remove processing, afterwards, carry out draft and be more than 70% cold rolling, thereafter, take following formula (2) defined H as on the occasion of condition carry out final annealing.
[formula 1]
Wherein,
T: Heating temperature during final annealing (℃), t: annealing time (second)
X
0: the Fe concentration (quality %) in pure titanium plate
A＝891、B＝0.428、n＝0.135
In addition, above-mentioned pure titanium plate, also can obtain by thering is the manufacture method of following main idea: through the operation of hot rolling, cold rolling, final annealing, and after described hot rolling, do not carry out process annealing and oxide skin carried out in pure titanium plate surface and remove after processing, carry out draft and be more than 20% cold rolling, thereafter, take following formula (2) defined H as on the occasion of condition carry out final annealing.
[formula 2]
Wherein,
T: Heating temperature during final annealing (℃), t: annealing time (second)
X
0: the Fe concentration (quality %) in pure titanium plate
A＝891、B＝0.428、n＝0.135
According to the present invention, on the basis of balance of considering each element, stipulate closely that chemical composition forms, and the schmid factor that is by the specific twin crystal of the crystal grain of pure titanium plate is defined as specific ratio mutually with β, can access not only thus that at room temperature tensile strength is also very high, and also excellent pure titanium plate of press formability and slit and corrosion resistant.Pure titanium plate like this, while requiring the high strength under room temperature in described wide in range like this field, can give play to good shaping processability, and erosion resistance is also more excellent.
China and foreign countries are according to the present invention, and above-mentioned pure titanium plate can be manufactured at an easy rate.
Accompanying drawing explanation
Fig. 1 is the stereographic map for the titanium plate of plate-type heat exchanger (PHE).
Fig. 2 (a) is for the vertical view of the stamping metal die of the method for evaluating press formability is described, Fig. 2 (b) is the summary section between the F-F of Fig. 2 (a).
Embodiment
About the press formability of pure titanium plate, except sliding deformation, twin crystal distortion also contributes to the distortion of former material very much, therefore known, and twin crystal distortion more easily occurs, and press formability is more excellent.Pure titanium is more for soft, and twin crystal distortion more easily occurs, and press formability is better, if but intensity rank is high, be difficult to occur twin crystal distortion, and known press formability is poor.
The present inventors, in order to provide under a kind of state maintaining high intensity levels (tensile strength is more than 343MPa), improve press formability, in addition also excellent pure titanium plate of slit and corrosion resistant, studies for metal structure from various angles, draws the following conclusions.
That is, if carry out cold rollingly along a direction, pure titanium plate produces intensity anisotropy, compares the width of low ductility, the intensity step-down of the rolling direction of high ductibility, if therefore carry out stampingly, the distortion of the rolling direction that intensity is low is preferentially carried out.Therefore, for press formability is improved, effectively carry out organizational controls, promote to contribute to the sensitization towards the twin crystal distortion of the rolling direction distortion as main deformation direction, importantly, even if form, to make tensile strength rank be that 343MPa twin crystal also easily occurs when above and is out of shape crystalline orientation.
Therefore in the present invention, the schmid factor of exerting one's influence for twin crystal distortion generation difficulty is studied, it found that, the value of the schmid factor of the twin crystal distortion while applying tension load for the rolling direction of the rolling surface of 1/4 * thickness of slab of pure titanium plate and distribution proportion (area occupation ratio) thereof are if in specific scope, can either maintain high intensity levels, can improve press formability again, thereby reach the present invention.
Specifically, the crystal grain of the principal phase of pure titanium plate has hexagonal crystal crystalline texture, and the twin crystal of primary activity while being shaped that swells is { 11-22 } < 11-23 >.Therefore, the plasticity when making Accompanying Deformation in rolling direction improves, and while effectively producing load in rolling direction, makes activeization of activity of { 11-22 } < 11-23 > twin crystal system.For this reason, the schmid factor of raising { 11-22 } < 11-23 > twin crystal system is effective.
So the result that the present inventors study is repeatedly that, in order to make the activity of twin crystal distortion easy, the value of the schmid factor of above-mentioned twin crystal system at least needs more than 0.45.
But, if it is very few to have the ratio of crystal grain of schmid factor more than so specific value, even if the activity of twin crystal distortion easily occurs, whole for former material, for the raising of press formability also without much benefits.Therefore above-mentioned schmid factor is that the area occupation ratio in more than 0.45 region need to, for the more than 43% of integral body, be preferably more than 45%.If existed more than 43% in area occupation ratio, both can access and can maintain intensity rank more than 343MPa, there is again the pure titanium plate of especially excellent press formability.The upper limit of its area occupation ratio is not particularly limited.
Also have, represent that in the Miller's indices of crystal face, index becomes while bearing, and generally adopts the Description Method of additional whippletree on numeral.But index becomes while bearing, in this manual, in order conveniently to be explained by negative.Therefore ,-2 in above-mentioned { 11-22 } represents that index is for negative.
So in the present invention, as the index for press formability is improved, adopt schmid factor.Generally along specific crystal face, make the size of the needed critical resolved shear stress of dislocation moving (τ), because crystal face and crystallographic axis are to different, known by ［ τ=σ cos φ cos λ ］ (in formula, σ represent tensile axis to tensile stress, φ represents the angle of slip plane normal and tensile axis, and λ represents the angle of slip direction and tensile axis) provide.
［ cos φ cos λ ］ in above-mentioned formula is called schmid factor, represents to act among the external force of tensile axis the ratio of the power of utilizing for moving dislocation.While applying external force to titanium plate,, because movable under less external force, easily there is viscous deformation so result is metal sheet in the slip system that the value of schmid factor is high/twin crystal system.Meet the pure titanium plate of the important document of above-mentioned schmid factor, while applying tension load in rolling direction, twin crystal distortion is promoted, and the press formability that principal strain directions is rolling direction (the particularly anisotropic plasticity that swells) significantly improves.
Also have, be known that the common impurity content of pure titanium plate more many be more high strength, twin crystal distortion is more difficult to occur, so press formability is poor.But in the present invention, as described later, because tightly stipulate that chemical composition forms, and so that being out of shape incidental mode, twin crystal controls schmid factor, so, even if impurity content is many, tensile strength is high, also can make twin crystal distortion sensitization, and consequently press formability improves.
In addition, the present inventors also find, in order to improve slit and corrosion resistant, particularly, due to crevice corrosion easily occurring under high temperature and humidity environment, in order still to make slit and corrosion resistant improve, importantly suppress separating out of β phase under such environment.That is, titanium of the present invention, is preferably and take the metal structure that α phase (hexagonal crystal) is main body.If the volumetric ratio of β phase (body-centered cubic brilliant) is high, slit and corrosion resistant worsens, thus the volume fraction of β phase on be limited to below 0.3%, be preferably below 0.2% more preferably 0%.
In addition,, in pure titanium plate of the present invention, suitably adjusting and bringing the element of impact for press formability and tensile strength is that Fe and O are also very important.The scope of these each compositions of pure titanium plate of the present invention is set and be the reasons are as follows.
Fe：0.02～0.10%
Fe is the element that contributes to the intensity raising of pure titanium plate, and in order to bring into play such effect, the content of Fe is more than 0.02%, to be preferably more than 0.03%.But if Fe content becomes too much, even if annealing conditions is suitably changed, it is many that the β generating also becomes mutually, slit and corrosion resistant is deteriorated.Therefore, Fe content, below 0.10%, is preferably below 0.08%, more preferably below 0.07%.
O：0.04～0.20%
O is for guaranteeing that in the intensity of pure titanium plate be effective element, and in order to bring into play such effect, the content of O is more than 0.04%, is preferably more than 0.045%, more preferably more than 0.050%, more preferably more than 0.07%.But if O content becomes too much, intensity becomes too high, press formability reduces on the contrary, or has limit portion crackle and rupture when cold rolling.Therefore O content, below 0.20%, is preferably below 0.18%, more preferably below 0.15%.
In addition in the present invention, from the interpolation by Fe and O on one side, realize the raising of intensity and the balance of press formability, Yi Bian suppress separating out of β phase, realize the viewpoint of the raising of slit and corrosion resistant and set out, importantly stipulate the relation of the content of Fe and O.Specifically, need to be in the mode of formula (1), i.e. ［ O content (quality %) ］+0.12 * ［ Fe content (quality %) ］ >=0.050(formula (1)), in above-mentioned scope, adjust the content of Fe and O.The Fe being derived by above-mentioned formula (1) and the content of O were lower than 0.050 o'clock, and intensity is likely not enough.In order further to improve the additive effect of above-mentioned Fe and O, the adjustment mode of expectation is that the value of formula (1) is preferably more than 0.055, more preferably more than 0.060, more preferably more than 0.080.
Pure titanium plate of the present invention, except mentioned component, surplus consists of titanium and inevitable impurity.In " inevitably impurity ", in the impurity element inevitably comprising in the titanium sponge that comprises raw material (the representational N of having, C, H, Si, Cr, Ni etc.) ，Huo manufacturing process, be likely absorbed into element in goods (such as H etc.).
Among these inevitable impurity, for example N is also the element that contributes to the intensity of pure titanium plate to improve, if but many containing quantitative change, lose cold ductility, so N content is preferably below 0.02%, more preferably below 0.01%.On the other hand, N content can be also 0%, but excessively minimizing can cause cost rising, is therefore preferably more than 0.001%, more preferably more than 0.002%.
C is the element that contributes to intensity to improve, if but many containing quantitative change, damage on the contrary cold ductility, so C content is preferably lower than 0.015%, more preferably below 0.012%.On the other hand, the lower limit of C content is not particularly limited, and can be also 0%, but excessively instead minimizing causes cost rising, is therefore preferably more than 0.002%, more preferably more than 0.003%.
Pure titanium plate of the present invention, at room temperature (25 ℃) have tensile strength more than 343MPa.This be due to as above-mentioned, pure titanium plate is used in various fields, even if at room temperature also require to have high strength.The tensile strength of pure titanium plate of the present invention, more than being preferably 370MPa.But, too high if tensile strength becomes, ductility reduces, and therefore press formability variation is preferably below 600MPa.
As above-mentioned, the intensity of pure titanium plate and ductility are contrary characteristics, but pure titanium plate provided by the invention, as the pure titanium plate that can meet this two specific character, there is more than 343MPa tensile strength and excellent press formability, and there is excellent slit and corrosion resistant.
Next, take above-mentioned pure titanium plate describes for creating conditions as example.For example, in the situation of pure titanium plate, generally by following operation, manufactured.The physical property of titanium, because form and imposing a condition of each operation and different according to the chemical composition of the used former material of titanium, so as a series of manufacturing process, should synthetically select and determine condition, also may not necessarily set closely for the condition of each operation.
Pure titanium plate is generally by casting, to be adjusted the titanium ingot being grouped into for specific one-tenth to obtain.Through ［ I. cogging forge rolling ］ → ［ II. hot rolling ］ → ［ III. process annealing ］ → ［ IV. cold rolling ］ → ［ V. final annealing ］ each operation manufacture thereafter.At each inter process, also can carry out as required shot-peening, cleanup acid treatment etc. and carry out oxide skin and remove processing.
Above-mentioned ［ rolling is forged in I. cogging ］ is as required and the operation of carrying out, in order to break thick cast structure, implements, and for example, from productivity (workability) grade, at about 800～1100 ℃, starts equal heat forged or rolling.
［ II. hot rolling ］, for example, after about 700～950 ℃ maintenances, be rolled into the thickness of slab into expectation.
［ III. process annealing ］ be as required and the operation of carrying out, for example, after soaking is carried out in 700～850 ℃ of left and right, and air cooling.
While carrying out ［ process annealing ］, after process annealing, carry out oxide skin and remove processing, carry out afterwards ［ IV. is cold rolling ］.［ IV. is cold rolling ］ before final annealing, carried out is more than 70% draft, is preferably more than 80%.By the draft with more than 70%, undertaken cold rollingly, more than can be on one side the tensile strength of pure titanium plate being maintained to 343MPa with ［ V. final annealing ］ thereafter, obtain the also characteristic of excellence of press formability on one side.
; if manufactured on above-mentioned pure titanium plate of the present invention; the draft that makes ［ IV. is cold rolling ］ after process annealing is more than 70%, and the schmid factor that can make { 11-22 } < 11-23 > twin crystal system is that the area occupation ratio of more than 0.45 crystal grain reaches more than 43%.This is more than 70% because of the draft that makes ［ IV. is cold rolling ］ after process annealing, implement ［ V. final annealing ］ thereafter, can access the crystalline orientation of above-mentioned expectation, thus can access good press formability, and more than also tensile strength can being maintained to 343MPa.
Also have, draft is higher, and press formability more improves, if but excessively improve draft, at generation limit, the end of pure titanium plate portion crackle, or pure titanium plate ruptures and hinders productivity when cold rolling, and therefore preferably draft is below 95%, more preferably below 90%.
On the other hand, while not carrying out ［ III. process annealing ］,, after ［ II. hot rolling ］, after removing processing, oxide skin carries out ［ IV. is cold rolling ］.And in this case, ［ IV. is cold rolling ］ carried out before final annealing is more than 20%, is preferably more than 25% draft.While omitting process annealing, by suitably carrying out cold rolling and final annealing, more than also the tensile strength of pure titanium plate can being brought up to 343MPa, there is in addition the also characteristic of excellence of press formability.Do not carry out process annealing and when cold rolling, even the low characteristic that also can access above-mentioned excellence of draft, its reason is, during hot rolling, in former material, formed Deformation structure is not given up by process annealing, but stays in former material.Do not carry out process annealing, with low draft, can access the characteristic of press formability excellence, therefore yet, also can be applicable to following situation, the hot rolling of for example thick situation of but not taking high draft of the thickness of slab of pure titanium plate, and process, the situation that the thickness of slab of pure titanium plate is very thin.In addition, preferably draft is below 95%, more preferably below 90%.
［ V. final annealing ］, so that aftermentioned formula (2) is on the occasion of like this after the condition of Heating temperature and annealing time is annealed, air cooling is to room temperature, by being such condition, the separating out of the β phase that can suppress slit and corrosion resistant to impact.In pure titanium plate of the present invention, as above-mentioned, make micro-Fe contain, but because β Heating temperature and the hold-time of separating out mutually by Fe content, determined, so following formula (2) on the occasion of condition under carry out final annealing.So-called formula (2), that is,
[formula 3]
Wherein, in formula, T: Heating temperature during final annealing (℃), t: annealing time (second), X
0: the Fe concentration (quality %) in pure titanium plate, A=891, B=0.428, n=0.135.
Also have, the experiment of formula (2) based on following obtains.That is, as above-mentioned, the maintenance temperature when speed of separating out of β phase exists with ... Fe concentration in pure titanium plate and thermal treatment, Fe concentration is higher, and temperature is higher, and speed is faster.Therefore, use with the diffusion of atom and concentration and be assigned as basis and the speed of separating out formula that calculates, try to achieve the basic relational expression (formula 2) as speed of separating out, each coefficient A, B in formula (2) determine based on experimental data.
In formula, heating when T is final annealing (annealing) temperature (℃), preferably 550 ℃≤T(℃)≤890 ℃.If annealing temperature T is lower than 550 ℃, recrystallize does not occur, and ductility is significantly deteriorated.The temperature of the needed lower limit of recrystallize changed according to the hold-time, for example the hold-time shorter, need higher temperature.Heating temperature T is preferably more than 600 ℃, more preferably more than 700 ℃.Be heated in addition beta transformation point above and while annealing, cooling rear formation acicular structure and hinder press formability is therefore preferably carried out final annealing below β transformation temperature.Heating temperature T is preferably below 870 ℃, more preferably below 850 ℃.
Also have, the condition of other of cold rolling and final annealing and the condition of other operation, can adopt general condition.
In formula, the meaning of t is annealing time (second) in addition, is above-mentioned Heating temperature T(℃) under hold-time, if but in the scope in said temperature territory, substantially at Heating temperature T(℃) maintenance in the ± scope of 5 ℃.If annealing time t is too short, control annealing operation difficulty, annealing time t is long in addition, and productivity is variation also.Therefore annealing time t(second) preferably in 10 seconds≤t(second)≤120,000(second) scope in.
About the thickness of pure titanium plate of the present invention, consider the settings such as needed intensity, be not particularly limited.
Pure titanium plate of the present invention, both there is high strength, ductility is excellent again, and there is also excellent characteristic of slit and corrosion resistant under high temperature and humidity environment, therefore at airplane parts, chemical device member, the structural wood of coastal portion (particularly promoting such gulf bank structural wood with contact with sea water corrosion), automobile, building materials, mobile telephone, laptop computer, the fuselage of photographic camera etc., spectacle frame, the formation material of plate-type heat exchanger, the dividing plate of fuel cell, the exterior trimming parts of family's electrical article, the wide field of conveying use machine direction member etc., can be widely used in requirement has the purposes of height plasticity and mechanical intensity.Particularly be applicable to the heat exchange component of plate-type heat exchanger.
[embodiment]
Below, enumerate embodiment and be described more specifically the present invention, but the present invention is not limited by following embodiment certainly, in the scope that can meet the forward and backward aim of stating, can certainly suitably be changed enforcement, these are all included in the scope of technology of the present invention.
To contain the Fe, the O that in table 1, by " composition ", are represented, surplus is the raw material of titanium and inevitable impurity, by CCIM(cold-crucible induction melting), by casting, obtain titanium ingot bar.This ingot bar split rolling method is become to the bulk of wide 130mm * thick 45mm, reheat to 750 ℃ and implement hot rolling, obtain the hot-rolled sheet (No.3～16) of thick about 4mm.Also have, A partial experiment material is considered the cold rolling rate described in final thickness of slab (0.5mm) and table 1, for the thickness of slab of hot-rolled sheet, carries out building up by welding, suitable adjustment thickness of slab.The hot-rolled sheet of a part described in table 1 carries out, after the process annealing of 5 minutes, in salt stove, flooding with 700 ℃, pickling thereafter and carry out the processing of deoxygenated skin.Also have, another part does not carry out process annealing, carries out the processing of deoxygenated skin.After deoxygenated skin is processed, by building up by welding and pickling, adjust thickness of slab, with " draft " shown in table 1, carry out cold rollingly, thereafter, with " final annealing condition " shown in table 1, carry out final annealing.Also have, A partial experiment material, draft is beyond 85%.After final annealing, in nitric acid hydrofluoric acid solution, flood and the processing of enforcement deoxygenated skin, obtain the pure titanium plate as the thickness of slab 0.5mm of test material.The H value of each pure titanium plate is calculated based on above-mentioned formula (2), describes in " the value H of formula (2) " hurdle of table 1.
For resulting each pure titanium plate, carry out following evaluation.
(schmid factor Measuring determines method)
By in field emission type scanning electronic microscope (Field Emission Scanning Electron Microscope:FESEM) (NEC society system, JSM5410) on, be equipped with the crystalline orientation analytical method of Electron Back-Scattered Diffraction (Electron Backscatter Diffraction Pattern:EBSP) system, evaluate the set tissue on the pure titanium plate surface of any part.
Specifically, the rolling surface surface of grinding pure titanium plate to thickness of slab 1/4 after, be placed in SEM lens barrel, irradiation electron rays high sensitivity camera are taken and are projected to the EBSP on screen, as image input computer, for this image, analyze, try to achieve crystalline orientation.At this moment, the schmid factor of { 11-22 } < 11-23 > twin crystal system when each measurement point evaluation makes tension load direction consistent with rolling direction, the data of collecting orientation mapping.Also have, this measurement field range is 1mm * 1mm, and measuring spacing is 1 μ m.At this, the azimuth difference of the measurement point being adjacent to each other for ± 15 ° with interior to belong to same crystal face.
(schmid factor of { 11-22 } < 11-23 > twin crystal system is the area occupation ratio of more than 0.45 crystal grain (α phase))
After the measurement of above-mentioned schmid factor, schmid factor is to make the total of more than 0.45 measurement point divided by the quantity of whole measurement point, be multiplied by again 100, try to achieve the area occupation ratio that schmid factor is more than 0.45 crystal grain, describe in " set tissue (%) " hurdle of table 1.
(volume fraction of β phase)
For the rolling surface surface of pure titanium plate, carry out mechanical mill until polishing is carried out in 1/4 position of thickness of slab, with chemical grinding, be processed into after minute surface, implement reflection electronic picture (BSE) and observe.For each sample, with 10,000 times of observations of multiplying power, the region of 270 μ m * 230 μ m arbitrarily, try to achieve volume fraction average of β phase, be documented in " β phase volume rate (%) " hurdle of table 1.In the present embodiment, if the volume fraction of β phase is below 0.3%, be qualified.
(tensile strength evaluation)
From pure titanium plate, extract No. 13 test films (direction that rolling direction is consistent with load axle (L direction)) of JISZ2201 defined, at room temperature based on JISH4600, implement tension test, measure tensile strength.Result is charged in " tensile strength " hurdle of table 1.Tensile strength is that average evaluation more than 343MPa is qualified.
(press formability (score))
Fig. 2 (a) is (b) explanatory view of the evaluation method of press formability (the anisotropic plasticity that swells).The pure titanium plate that is used as above-mentioned test material and makes, use the stamped metal mould ［ size: 160mm * 160mm(evaluation portion: 100mm * 100mm) of the heat exchange section of simulation plate-type heat exchanger, spacing: 10mm, maximum height: 4mm, there is radius of curvature R: 0.4,0.6,0.8,1.0,1.4,1.8(mm) herringbone (ヘ リ ン ボ ー Application) moulds of 6 kinds of crest lines, according to crest line, the different metal die of radius of curvature R at peak ］, with the press formability of 80ton oil pressure stamping machine evaluation titanium plate.Punching press condition is, at two sided coatings press oil (the kinetic viscosity 34mm of the metal die as test film
240 ℃ of/s(temperature)), make respectively to test the rolling direction of material and the above-below direction of Fig. 2 (a) consistent and be configured on the metal die of downside, with pressing plate, restrain after flange part, with the condition of drawing velocity 1mm/ second, compression distance 3.4mm, implement.
The crackle measuring position of test material, shown in Fig. 2 ［ Fig. 2 (a) is vertical view, and Fig. 2 (b) is sectional view ］, is 36 places of the intersection point of rib portion and dotted line (peak side 5 places, paddy side 1 place).
As the basic point of crackle, about A line (peak side), C line (peak side), C ' line (paddy side) and E line (peak side), during with visual judgement, flawless (perfecting) obtains 2 minutes, and (part attenuates constriction, the phenomenon of necking down) be inclined to obtain 1 minute, if there is constriction, obtain 1 minute, if cracked, be 0 minute, about B line (peak side), D line (peak side), flawless (perfecting) obtains 2 minutes, if there is constriction, is 0.5 minute, if cracked, is 0 minute.
The score of plasticity is calculated by following formula (3), the index of evaluating as press formability of the present invention.Specifically, the inverse that each mark is multiplied by radius of curvature R makes the status number value of crackle, tries to achieve its total.Situation to crackle, constriction unconfirmed is made after this aggregate value stdn as 100, be multiplied by again the function F (T, μ, t) that exists with ... temperature (T), lubricating oil viscosity (μ), test film thickness of slab (t), and exist with ... the angle (α) of the crest line of metal die, the function G (α, p) of spacing (p), as plasticity score, calculate.Also have, in the present embodiment, because make the angle (α) of crest line of temperature (T), lubricating oil viscosity (μ), test film thickness of slab (t), metal die and spacing (p) certain, so cheap property ground 1 counts the score F * G, and description is in " plasticity score " hurdle of table 1.
Plasticity score=(F * G) * and Σ E(ij)/R(j)/(Σ A, C, C ', E2/R(j))+(Σ B, D1/R(j)) * 100 ... (3)
In formula,
About A, C, C ', E, carry out E(ij)=1.0 * (flawless: 2, necking down: 1, have crackle: calculating 0),
About B, D, carry out E(ij)=0.5 * (flawless: 2, necking down: 1, have crackle: 0) calculate.
Plasticity score, has excellent formability 70 above being evaluated as.
(crevice corrosion test)
From the pure titanium plate of making, cut the test film of 30mm * 50mm, the hole of opening in the central 7mm φ, makes many U-shapeds folders (ASTMG1671) by this hole by テ Off ロ Application (registered trademark) and is installed on two sides,
Using it as crevice corrosion evaluation test film.These many U-shaped folders (マ Le チ Network レ PVC ス: multi-clevis) form 12 place's clearance portion, in this test, because many U-shaped folders are installed on the two sides of test film, so portion adds up to 24 places between gap.This test film is immersed in the 10%NaCl aqueous solution of boiling to 360 hours, thereafter, Visual Confirmation crevice corrosion has or not generation, measures the occurrence positions number of crevice corrosion.The occurrence positions quantity of crevice corrosion is sentenced lower time 5, and slit and corrosion resistant is evaluated as well.Result is described in " erosion resistance corrosion rate " hurdle of table 1.
(comprehensive evaluation)
As the mechanical characteristic under room temperature, tensile strength under room temperature is more than 343MPa, must being divided into more than 70 minutes of press formability, 5, the situation under sentencing is respectively qualified to crevice corrosion generation number, meet the balance excellence that whole examples is evaluated as intensity and press formability, be evaluated as in addition slit and corrosion resistant also excellent.Result is presented in table 1.
[table 1]
Formula (1)=[O content (quality %)]+0.12 * [Fe content (quality %)]
By table 1, can be investigated as follows.That is, No.2～6,9,10,12～16th, meet the pure titanium plate of important document given to this invention, and the intensity under known not only room temperature and the balance of press formability are excellent, and slit and corrosion resistant is also excellent.
With respect to this, No.1,7,8,11 is because so can not guarantee the intensity under room temperature, there is press formability and the poor such problem of slit and corrosion resistant under room temperature in discontented foot important document given to this invention.
No.1 and No.11 are the low examples of cold rolling draft before final annealing.In this embodiment, there is the area occupation ratio that schmid factor is the crystal grain of more than 0.45 value (in table, being " set tissue (%) ") lower than 43%, so press formability is poor.
No.7 is that the contained O amount of pure titanium plate is few, and the value of formula (1) is lower than the example of regulation of the present invention, and tensile strength is lower than 343MPa.
No.8 is that the value of formula (2) is lower than the example (in table, the value of " H " is for negative) of regulation of the present invention.In this embodiment, there is the area occupation ratio that schmid factor is the crystal grain of more than 0.45 value (in table, being " set tissue (%) ") lower than 43%, and the volume fraction of β phase is lower than regulation, thus press formability and slit and corrosion resistant poor.
With reference to specific embodiment, describe the present invention, but without departing from the spirit and scope of the present invention, can carry out various changes and modification, this is clearly to those skilled in the art.
The Japanese patent application (patent application 2011-120766) of the application based on May 30th, 2011 application, the Japanese patent application (patent application 2012-074836) of application on March 28th, 2012, its content this with reference to and quote.
[utilizability in industry]
Pure titanium plate of the present invention, for fuselage, spectacle frame, the formation material of plate-type heat exchanger, the exterior trimming parts of the dividing plate of fuel cell, family's electrical article of the structured material of airplane parts, chemical plant facility member, coastal portion (particularly with contact with sea water, corrosion promotes such gulf bank structured material), automobile, building materials, mobile telephone, laptop computer, photographic camera etc., carry with machine direction member etc. useful.
Claims (6)
1. a press formability and the balance of intensity and the pure titanium plate of excellent corrosion resistance, it is characterized in that, the meaning that contains Fe:0.02～0.10%(" quality % ", about chemical composition below all with), O:0.04～0.20%, surplus consists of titanium and inevitable impurity
The content of described Fe and described O meets following formula (1), and,
The area occupation ratio that the schmid factor of { 11-22 } < 11-23 > twin crystal system that the rolling direction of thickness of slab 1/4 position of take is axle is more than 0.45 region is more than 43%,
And the volume fraction of β phase is below 0.3%,
［ O content (quality %) ］+0.12 * ［ Fe content (quality %) ］ >=0.050 ... (1).
2. a manufacture method, is the manufacture method of the balance of press formability claimed in claim 1 and intensity and the pure titanium plate of excellent corrosion resistance, it is characterized in that,
Through the operation of hot rolling, process annealing, cold rolling, final annealing, and,
After described process annealing, carry out the oxide skin on pure titanium plate surface and remove processing, afterwards, carry out draft and be more than 70% cold rolling, thereafter, take following formula (2) defined H as on the occasion of condition carry out final annealing,
[formula 1]
Wherein,
T: Heating temperature during final annealing (℃), t: annealing time (second)
X
0: the Fe concentration (quality %) in pure titanium plate
A＝891、B＝0.428、n＝0.135。
3. a manufacture method, is the manufacture method of the balance of press formability claimed in claim 1 and intensity and the pure titanium plate of excellent corrosion resistance, it is characterized in that,
Through hot rolling, cold rolling, the operation of final annealing, and,
After described hot rolling, do not carry out process annealing, but remove after processing in the oxide skin of carrying out pure titanium plate surface, carry out draft and be more than 20% cold rolling, thereafter, take following formula (2) defined H as on the occasion of condition carry out final annealing,
[formula 2]
Wherein,
T: Heating temperature during final annealing (℃), t: annealing time (second)
X
0: the Fe concentration (quality %) in pure titanium plate
A＝891、B＝0.428、n＝0.135。
4. a manufacture method for the heat exchange component of plate-type heat exchanger, is characterized in that, comprises pure titanium plate claimed in claim 1 is carried out to stamping operation.
5. a manufacture method for the heat exchange component of plate-type heat exchanger, is characterized in that,
Comprise:
The manufacture method of pure titanium plate according to claim 2 is manufactured the operation of pure titanium plate;
To manufacturing the pure titanium plate forming, carry out stamping stamping procedure.
6. a manufacture method for the heat exchange component of plate-type heat exchanger, is characterized in that,
Comprise:
The manufacture method of pure titanium plate according to claim 3 is manufactured the operation of pure titanium plate;
To manufacturing the pure titanium plate forming, carry out stamping stamping procedure.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011120766 | 2011-05-30 | ||
| JP2011-120766 | 2011-05-30 | ||
| JP2012-074836 | 2012-03-28 | ||
| JP2012074836A JP5937865B2 (en) | 2011-05-30 | 2012-03-28 | Production method of pure titanium plate with excellent balance of press formability and strength, and excellent corrosion resistance |
| PCT/JP2012/063914 WO2012165470A1 (en) | 2011-05-30 | 2012-05-30 | Pure titanium sheet having excellent balance between press formability and strength and excellent corrosion resistance, and process for manufacturing same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103562421A true CN103562421A (en) | 2014-02-05 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201280025980.XA Pending CN103562421A (en) | 2011-05-30 | 2012-05-30 | Pure titanium sheet having excellent balance between press formability and strength and excellent corrosion resistance, and process for manufacturing same |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP2716778A4 (en) |
| JP (1) | JP5937865B2 (en) |
| KR (1) | KR20140004793A (en) |
| CN (1) | CN103562421A (en) |
| WO (1) | WO2012165470A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109477168A (en) * | 2016-06-30 | 2019-03-15 | 新日铁住金株式会社 | Titanium sheet metal and its manufacturing method |
| CN109930028A (en) * | 2019-03-29 | 2019-06-25 | 盐城华旭机械制造有限公司 | One kind being based on stamping forming metal plate plate and its processing technology |
| CN111032894A (en) * | 2017-08-31 | 2020-04-17 | 日本制铁株式会社 | Titanium plate |
| CN111020293A (en) * | 2019-12-30 | 2020-04-17 | 宝鸡鑫诺新金属材料有限公司 | High-performance TA1 rod wire material and preparation method thereof |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6263040B2 (en) * | 2013-03-19 | 2018-01-17 | 株式会社神戸製鋼所 | Titanium plate |
| JP5973975B2 (en) * | 2013-09-24 | 2016-08-23 | 株式会社神戸製鋼所 | Titanium plate |
| CN107385277B (en) * | 2017-06-29 | 2019-09-20 | 西安赛特思迈钛业有限公司 | A kind of watch structure part pure titanium rod material and preparation method thereof |
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- 2012-03-28 JP JP2012074836A patent/JP5937865B2/en not_active Expired - Fee Related
- 2012-05-30 KR KR1020137031469A patent/KR20140004793A/en not_active Application Discontinuation
- 2012-05-30 EP EP12793298.6A patent/EP2716778A4/en not_active Withdrawn
- 2012-05-30 WO PCT/JP2012/063914 patent/WO2012165470A1/en active Application Filing
- 2012-05-30 CN CN201280025980.XA patent/CN103562421A/en active Pending
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| CN101910432A (en) * | 2008-03-25 | 2010-12-08 | 住友金属工业株式会社 | Titanium plate and process for manufacturing titanium plate |
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| CN109477168A (en) * | 2016-06-30 | 2019-03-15 | 新日铁住金株式会社 | Titanium sheet metal and its manufacturing method |
| CN111032894A (en) * | 2017-08-31 | 2020-04-17 | 日本制铁株式会社 | Titanium plate |
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Also Published As
| Publication number | Publication date |
|---|---|
| KR20140004793A (en) | 2014-01-13 |
| WO2012165470A1 (en) | 2012-12-06 |
| EP2716778A4 (en) | 2014-11-19 |
| JP5937865B2 (en) | 2016-06-22 |
| JP2013011013A (en) | 2013-01-17 |
| EP2716778A1 (en) | 2014-04-09 |
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