WO2012132785A1 - コンビネーションプレス用熱交換器用アルミニウム合金フィン材およびその製造方法 - Google Patents
コンビネーションプレス用熱交換器用アルミニウム合金フィン材およびその製造方法 Download PDFInfo
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- WO2012132785A1 WO2012132785A1 PCT/JP2012/055660 JP2012055660W WO2012132785A1 WO 2012132785 A1 WO2012132785 A1 WO 2012132785A1 JP 2012055660 W JP2012055660 W JP 2012055660W WO 2012132785 A1 WO2012132785 A1 WO 2012132785A1
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- fin material
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- heat exchanger
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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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
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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
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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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
- F28F21/084—Heat exchange elements made from metals or metal alloys from aluminium or aluminium alloys
Definitions
- the present invention relates to an aluminum alloy fin material for a heat exchanger for a combination press used for a heat exchanger and a method for producing the same.
- fin materials aluminum alloy fin materials for heat exchangers used in heat exchangers such as air conditioners (hereinafter referred to as fin materials as appropriate) have also been switched to new refrigerants in line with chlorofluorocarbon regulations, and the air conditioners themselves have become more compact and lightweight.
- the thickness has been further reduced, and the thickness has been reduced to 0.15 mm or less, and recently to about 0.09 mm.
- the draw method consists of an overhanging process, a drawing process, a punching (piercing) and hole expanding process (burring), and a flaring process.
- the drawless system consists of a punching and hole expanding process, an ironing (ironing) process, and a flaring process. Is mainly composed of an overhanging process, a drawing process, a punching and hole expanding process, an ironing process, and a flaring process.
- the piercing & burring molding and the flaring molding for molding the tube hole collar in the copper pipe are indispensable molding processes for the fin material.
- these moldings are severe molding for the fin material whose thickness is reduced to 0.15 mm or less. Therefore, fin materials with improved workability have been developed in response to such thinning.
- the plate thickness is 0.15 mm or less, and the grain size of the intermetallic compound, the maximum length of the large tilt grain, the average grain size of the subcrystal grains in the large tilt grain, and the like are predetermined.
- a defined aluminum alloy fin material having excellent formability is disclosed.
- Patent Document 2 discloses that the plate thickness is less than 0.11 mm, contains a predetermined amount of Fe and Ti, regulates Si and Cu to be equal to or less than a predetermined amount, and prescribes a predetermined elongation rate.
- An aluminum alloy fin material for heat exchangers having excellent stackability (characteristic that contact with adjacent fins due to non-uniform deformation at the time of pipe expansion) is disclosed.
- Patent Document 3 discloses an aluminum alloy fin material for a heat exchanger that has a plate thickness of less than 0.11 mm and that has a predetermined element content and is excellent in anti-Abek resistance.
- Patent Document 4 discloses a high-strength aluminum alloy thin plate for drawless fins having a plate thickness after cold rolling of 0.115 mm and a predetermined element being specified, and a method for manufacturing the same.
- JP 2006-104488 A Japanese Patent No. 4275560 JP 2005-126799 A JP-A-64-8240
- the conventional fin material has the following problems. Although the above-described conventional techniques have improved the workability, in recent years, in addition to further miniaturization, weight reduction, and high performance of heat exchangers, fin materials that are easier to process have been supplied. Since it is expected, further improvement in workability is required.
- cracks often referred to as color cracks may occur during molding. That is, a fine crack is generated on the processed end face during the piercing and burring process, and this causes a color crack during the final reflare molding.
- a color crack occurs, when the copper tube is expanded through the color hole of the fin-molded molded product, the so-called Abek phenomenon that the interval between the laminated fins becomes extremely narrow is caused. It tends to occur.
- the ventilation resistance of a heat exchanger increases by this Abeck phenomenon. That is, the color crack not only impairs the appearance of the fins, but also causes problems such as a decrease in performance as a heat exchanger, thereby reducing the value as a product.
- the fin material described in Patent Document 1 aims to improve color cracking resistance.
- Mn is positively added, depending on the Mn content and production conditions, there is a problem that it becomes easy to work and harden by a coarse intermetallic compound or solid solution Mn. Therefore, there is room for improvement in resistance to color cracking.
- the present invention has been made in view of the above problems, and is intended for a combination press excellent in color cracking resistance and capable of suppressing the occurrence of color cracking during molding processing for a fin material for a combination press. It is an object to provide an aluminum alloy fin material for a heat exchanger.
- the aluminum alloy fin material for a heat exchanger for a combination press contains Fe: 0.010 to 0.4 mass%, the balance is made of Al and inevitable impurities, and the Al purity is 99.30 mass. % Of an aluminum alloy fin material for a heat exchanger for combination press, wherein the thickness of the aluminum alloy fin material for a heat exchanger for combination press is less than 0.115 mm, and the average grain size of the sub-crystal grains is It is characterized by being 2.5 ⁇ m or less and a proof stress of 100 to 130 N / mm 2 . Further, the number of intermetallic compounds having a maximum length exceeding 3 ⁇ m is 2000 pieces / mm 2 or less.
- an Al—Fe-based intermetallic compound is formed, or it dissolves in the aluminum matrix and the sub-crystal grains are refined during press molding. This suppresses work hardening. Moreover, the increase in an intermetallic compound is suppressed by prescribing Al purity. And the elongation in the fin material of thickness less than 0.115 mm increases by making the average particle diameter of a subcrystal grain into 2.5 micrometers or less. Further, by setting the proof stress to 100 to 130 N / mm 2 , the strength becomes appropriate as a fin material for a combination press. In addition, when the number of intermetallic compounds having a maximum length exceeding 3 ⁇ m is 2000 pieces / mm 2 or less, the occurrence of color cracks due to the starting point of coarse intermetallic compounds is prevented.
- the aluminum alloy fin material for a heat exchanger for a combination press according to the present invention further contains Cu: 0.005 to 0.05% by mass with respect to chemical components of the aluminum alloy, Si: 0.15% by mass or less, It is characterized by suppressing to Mn: less than 0.015 mass% and Cr: 0.015 mass% or less.
- the aluminum alloy fin material for a heat exchanger for a combination press according to the present invention is characterized by further containing Ti: 0.01 to 0.05% by mass with respect to the chemical component of the aluminum alloy. According to such a configuration, the ingot structure is refined by adding a predetermined amount of Ti.
- the aluminum alloy fin material for a heat exchanger for a combination press according to the present invention may be provided with a surface treatment film on the surface of the fin material.
- the surface treatment film include a corrosion-resistant film, a hydrophilic film, and a lubricating film. According to such a structure, the characteristics according to use environment, a use, etc., such as corrosion resistance, hydrophilicity, and moldability, can be improved.
- the method for producing an aluminum alloy fin material for a heat exchanger for a combination press is a method for producing the aluminum alloy fin material for a heat exchanger for a combination press (not provided with a surface treatment film) as described above.
- a heat treatment step in which an aluminum alloy ingot having an alloy chemical component is subjected to a heat treatment at a temperature of 450 to 500 ° C. for 1 hour or more, and after the heat treatment, a finish temperature of hot finish rolling becomes 250 ° C. or more and less than 300 ° C.
- a temper annealing step of performing temper annealing for 1 to 6 hours.
- the structure of the ingot is homogenized by the heat treatment process, and the hot rolled sheet is rolled without being recrystallized by the hot rolling process. And it is made into thickness less than 0.115mm without producing coarsening of a subcrystal grain after refining annealing by a cold working process, and elongation is given by refining annealing process, and refinement of a subcrystal grain Is promoted.
- the aluminum alloy fin material for a heat exchanger for a combination press according to the present invention can suppress color cracking when it is formed. For this reason, it is possible to prevent the appearance of the fins from being damaged and the occurrence of problems such as deterioration in performance as a heat exchanger.
- the method for producing an aluminum alloy fin material for a heat exchanger for a combination press according to the present invention can produce an aluminum alloy fin material for a heat exchanger having excellent color cracking resistance.
- the fin material according to the present invention is for a combination press containing a predetermined amount of Fe, the balance being Al and inevitable impurities, and an aluminum alloy having an Al purity of 99.30% by mass or more.
- the fin material has a thickness of less than 0.115 mm, an average grain size of subcrystal grains of 2.5 ⁇ m or less, and a proof stress of 100 to 130 N / mm 2 .
- the number of intermetallic compounds exceeding 3 ⁇ m is defined as 2000 pieces / mm 2 or less.
- the chemical component of an aluminum alloy it is preferable to contain a predetermined amount of Cu as necessary, and to suppress Si, Mn, Cr to a predetermined amount or less or less than a predetermined amount among unavoidable impurities contained in the aluminum alloy. . Furthermore, you may contain predetermined amount of Ti as needed.
- Fe 0.010 to 0.4 mass%
- Fe is an element that contributes to suppression of work hardening because it can form Al—Fe-based intermetallic compounds (or solid solution in an aluminum matrix) to make fine sub-crystal grains fine during press molding.
- it has the effect which contributes to the magnitude
- the Fe content is less than 0.010% by mass, the above effects cannot be obtained, and the color cracking property is inferior in press molding. On the other hand, if it exceeds 0.4% by mass, the strength becomes too high, a coarse intermetallic compound is formed, and the color cracking resistance is inferior. Therefore, the Fe content is 0.010 to 0.4 mass%.
- Cu 0.005 to 0.05 mass%
- the Cu content is set to 0.005 to 0.05 mass%. More preferably, the content is 0.01 to 0.05% by mass.
- Si 0.15 mass% or less (including 0 mass%)
- Si is an element mixed as an unavoidable impurity.
- the crystallized product intermetallic compound
- Si content shall be 0.15 mass% or less. In addition, you may suppress to 0 mass%.
- Mn is an element mixed as an unavoidable impurity.
- the crystallized product intermetallic compound
- the crystallized product becomes coarse, which becomes a stress concentration point at the time of forming, and cracks. Is the starting point. Therefore, when it contains Mn, Mn content is suppressed to less than 0.015 mass%. Furthermore, it is preferable to suppress to less than 0.005 mass%. In addition, you may suppress to 0 mass%.
- Cr 0.015 mass% or less (including 0 mass%)
- Cr is an element mixed as an unavoidable impurity.
- the crystallized product intermetallic compound
- the crystallized product becomes coarse, which becomes a stress concentration point at the time of forming and cracks. Is the starting point. Therefore, when it contains Cr, Cr content is suppressed to 0.015 mass% or less. In addition, you may suppress to 0 mass%.
- Ti 0.01 to 0.05% by mass
- the molten metal at any stage introduced into the degassing device and the molten metal flow rate control device may be added, and the Ti content is allowed to be 0.05 mass%. If the Ti content is less than 0.01% by mass, the effect of refining the ingot structure cannot be obtained.
- the crystallized product (intermetallic compound) becomes coarse, and this becomes a stress concentration point at the time of molding and becomes a starting point of cracking. Therefore, when Ti is added, the Ti content is 0.01 to 0.05 mass%.
- the fin material is composed of Al and inevitable impurities.
- unavoidable impurities in addition to the above-described Si, Mn, Cr, for example, Mg, Zn, Zr, Ce, Ga, V, which are contained in a metal base or an intermediate alloy within a generally known range. Ni and the like are allowed to contain up to 0.05% by mass, as long as the Al purity is not less than 99.30% by mass.
- Al purity 99.30% by mass or more If the Al purity is less than 99.30% by mass, the color cracking increases and the corrosion resistance decreases with the increase of intermetallic compounds. Moreover, the proof stress is increased. Therefore, Al purity shall be 99.30 mass% or more.
- the present invention is directed to a fin material having a thickness of less than 0.115 mm from the viewpoint of reducing the thickness of the fin material in response to recent demands for downsizing, weight reduction, and high performance of heat exchangers. Therefore, the thickness of the fin material is less than 0.115 mm.
- the average grain size of the sub-crystal grains in the alloy be 2.5 ⁇ m or less. If the average grain size of the sub-crystal grains exceeds 2.5 ⁇ m, sufficient elongation of the fin material cannot be obtained. Therefore, the average grain size of the sub-crystal grains is 2.5 ⁇ m or less.
- a lower limit is not specified in particular, it may be 0 ⁇ m (that is, it does not have to include subcrystal grains). By setting it as such a range, generation
- orientation analysis of a scanning electron microscope (SEM) structure is performed by an EBSD (Electron Back Scattered Diffraction Pattern) method.
- SEM scanning electron microscope
- EBSD Electro Back Scattered Diffraction Pattern
- a sample is irradiated with an electron beam, and the crystal orientation is specified by utilizing reflected electron Kikuchi line diffraction generated at that time.
- OIM Orientation Imaging Microscopy.TM manufactured by TSL can be used.
- the average grain size of the sub-crystal grains is calculated from the SEM / EBSD measurement data, the number of crystal grains is calculated, the total area of the fin material is divided by the number of crystal grains, and the area of each crystal grain is approximated to a circle.
- the diameter of the case is defined as the average grain size of the subgrains.
- the average grain size of the sub-crystal grains and the number of intermetallic compounds can be controlled by the component composition and the production conditions described later.
- the average grain size of subgrains is the content of each component, homogenization heat treatment conditions (temperature and time), hot finish rolling finish temperature, cold work rate, temper annealing conditions (temperature and time) ),
- the number of intermetallic compounds is controlled by the content of each component, homogenization heat treatment conditions (temperature and time), and the like.
- the proof stress is 100 to 130 N / mm 2 .
- the yield strength is less than 100 N / mm 2 , the strength is insufficient, and color cracks occur during combination press molding.
- the proof stress is 100 to 130 N / mm 2 .
- the proof stress can be measured by, for example, cutting out a tensile test piece according to JIS No. 5 from a fin material so that the tensile direction is parallel to the rolling direction and performing a tensile test according to JISZ2241.
- the average grain size, the yield strength, and the number of intermetallic compounds of the subcrystalline grains can be controlled by the component composition and the production conditions described later.
- the average grain size of subgrains is the content of each component, homogenization heat treatment conditions (temperature and time), hot finish rolling finish temperature, cold work rate, temper annealing conditions (temperature and time) ) And the like are controlled by the content of each component, homogenization heat treatment conditions (temperature and time), temper annealing conditions (temperature and time), and the like.
- the number of intermetallic compounds is controlled by the content of each component, homogenization heat treatment conditions (temperature and time), and the like.
- the fin material according to the present invention may be provided with a surface treatment film on the surface of the fin material.
- the fin material surface means one side or both sides of the fin material.
- Examples of the surface treatment film include a chemical film, a resin film, and an inorganic film depending on the use environment and application, and these may be combined (a resin film and an inorganic film are provided on the chemical film).
- examples of the resin film and the inorganic film include a corrosion-resistant resin film, a hydrophilic resin film, a hydrophilic inorganic film, and a lubricating resin film, and these may be appropriately combined.
- Examples of the chemical conversion film include phosphoric acid chromate.
- Examples of the corrosion-resistant resin film include epoxy-based, urethane-based, acrylic-based, and polyester-based resins, and the film thickness is preferably 0.5 to 5 ⁇ m.
- Examples of the hydrophilic film include water glass-based inorganic substances, resins containing polyacrylic acid or polyacrylate, resins containing sulfonic acid groups or sulfonic acid group derivatives, and the like. 0.05 to 10 ⁇ m is preferable.
- Examples of the lubricating resin film include a resin containing polyether polyol, and the film thickness is preferably 0.1 to 10 ⁇ m.
- a hydrophilic resin film is provided on the surface side of the corrosion-resistant resin film. It is preferable that a lubricating resin film is provided on the surface side of the conductive inorganic film.
- the manufacturing method of the fin material according to the present invention is a manufacturing method of the above-described fin material, and includes a heat treatment process, a hot rolling process, a cold working process, and a temper annealing process. Furthermore, you may include an ingot preparation process and a surface treatment process as needed. Hereinafter, each step will be described.
- the ingot production step is a step of producing an aluminum alloy ingot by melting and casting an aluminum alloy.
- an ingot having a predetermined shape is produced from a molten metal in which the aluminum alloy having the chemical components described above is melted.
- the method for melting and casting the aluminum alloy is not particularly limited, and a conventionally known method may be used. For example, it can be melted using a vacuum induction furnace and cast using a continuous casting method or a semi-continuous casting method.
- the heat treatment step is a step of subjecting the aluminum alloy ingot having the chemical composition of the aluminum alloy to a heat treatment (homogenization heat treatment) at a temperature of 450 to 500 ° C. for 1 hour or longer. If the heat treatment temperature is less than 450 ° C., the ingot structure is not sufficiently homogenized. In addition, the hot workability is reduced. Further, the subcrystal grain size becomes large. On the other hand, if it exceeds 500 ° C., the fine intermetallic compound that is refined during heating becomes coarse, the sub-crystal grains become coarse, and the elongation decreases. Further, the yield strength is increased. In addition, the amount of solid solution increases. Therefore, the heat treatment temperature is 450 to 500 ° C. Moreover, since the said effect is acquired if heat processing is holding time 1 hour or more, it is not necessary to prescribe
- the hot rolling step is a step of performing hot rolling after the heat treatment under the condition that the finish temperature of hot finish rolling is 250 ° C. or higher and lower than 300 ° C.
- the finish temperature of hot finish rolling is less than 250 ° C.
- the rollability of the material is lowered, and the rolling itself becomes difficult or the thickness control becomes difficult, and the productivity is lowered.
- 300 ° C. or higher since a recrystallized structure is formed in the hot-rolled sheet, a fibrous group of identical crystal orientations is generated after temper annealing, and constriction occurs during the piercing and burring process.
- the finish temperature of hot finish rolling is 250 ° C. or higher and lower than 300 ° C. More preferably, it is 260 to 290 ° C.
- the cold working step is a step of performing cold working (cold rolling) with a cold working rate of 96% or more after the hot rolling. After the hot rolling is completed, the cold working is performed once or a plurality of times, so that the fin material has a desired final thickness. However, if the cold working rate is less than 96%, the sub-crystal grains become coarse after temper annealing. Moreover, the yield strength is lowered. Therefore, the cold working rate in cold working is 96% or more.
- the cold working rate is a working rate from the intermediate annealing to the final plate thickness.
- the temper annealing step is a step of performing temper annealing (finish annealing) that is maintained at a temperature of 180 to 260 ° C. for 1 to 6 hours after the cold working. If the tempering annealing temperature is less than 180 ° C., sufficient elongation cannot be obtained. Moreover, the proof stress is increased. On the other hand, when it exceeds 260 ° C., recrystallized grains are generated after annealing, and cracks are generated starting from this. Further, the refinement of sub-crystal grains is not promoted. Furthermore, the yield strength is lowered. Therefore, the temperature of temper annealing is set to 180 to 260 ° C. The temper annealing is usually performed for 1 hour or longer, and the effect is saturated after 6 hours, so the holding time is 1 to 6 hours.
- the surface treatment step is a step of subjecting the fin material after the temper annealing to a surface treatment.
- a chemical conversion film when a chemical conversion film is formed, it can be performed by a chemical conversion treatment using a normal coating type or reactive type chemical.
- a resin film such as a corrosion-resistant resin film, a hydrophilic resin film, or a lubricating resin film, it can be carried out by applying and drying using a roll coater.
- a foreign material removing process for removing foreign substances such as dust
- a chamfering process for chamfering an ingot a temper annealing process and a surface treatment process
- machining that is appropriately performed as a fin material.
- a process or the like may be included.
- the fin material manufactured in this way is shape
- Combination molding (combination press) is stretched in the first process, drawn in the second process, punched and hole expanded in the third process (piercing and burring), ironing in the fourth process, and flared in the fifth process. Is to be applied.
- the fin material of this invention is excellent in color cracking resistance, generation
- Example preparation (Example No. 1 to 10, Comparative Example No. 11 to 21) An aluminum alloy having the composition shown in Table 1 was melted and cast into an ingot, and the ingot was subjected to chamfering and then subjected to homogenization heat treatment at 480 ° C. for 4 hours. This homogenized ingot was hot-rolled by controlling the finish temperature of hot finish rolling to be 270 ° C. to obtain a hot-rolled sheet having a thickness of 3.0 mm. Further, after cold rolling at a cold working rate of about 97.0% or 97.3%, respectively, the sheet thickness was set to 90 ⁇ m and 80 ⁇ m, and then subjected to temper annealing at the temperature and holding time shown in Table 1. Fin material was used.
- Example No. 22 to 27, Comparative Example No. 28 to 35 Aluminum alloys shown in Table 2 (Alloys A, B, and C corresponding to Table 1) were melted and cast to form ingots, and after the surfaces were subjected to face grinding, homogenization heat treatment and hot rolling were performed. A hot rolled plate having a thickness of 3.0 mm was used. Furthermore, no. Except 35, cold rolling was performed at a cold working rate of about 97.0% or 97.3% to make the plate thickness 90 ⁇ m and 80 ⁇ m, respectively, and then subjected to temper annealing to obtain a fin material. No. In No.
- a hot rolled plate having a thickness of 3.0 mm was subjected to cold rolling at a cold working rate of 50%, and then subjected to intermediate annealing at 360 ° C. for 3 hours using a batch furnace. Thereafter, cold rolling was performed at a cold working rate of about 94.0% or 94.7%, respectively, so that the plate thickness was 90 ⁇ m and 80 ⁇ m, and then temper annealing was performed to obtain a fin material.
- Table 2 shows the conditions for the homogenization heat treatment, the finish temperature of the hot finish rolling, and the temper annealing. In addition, No. 30 is a thing which could not manufacture a fin material.
- Example No. 36 to 39 Comparative Example No. 40 to 43
- No. in Table 2 No. 22 which is the same fin material as that of No. 22. 36, 37, No. 2 in Table 2.
- No. 27, which is the same fin material as No. 27. 38, 39, No. 2 in Table 2.
- No. 29, which is the same fin material as No. 29. 40, 41, No. 2 in Table 2.
- No. 32 which is the same fin material as No. 32.
- the following surface treatments were performed on 42 and 43.
- No. 1 Surface treatment under the same conditions as Comparative Example 1 of JP 2010-223520 A (comprising a chemical conversion film, a hydrophilic film, and a lubricating film in this order)
- No. 2 Surface treatment under the same conditions as Example 1 of Japanese Patent No. 3383914 (comprising a chemical conversion film, a hydrophilic film, and a lubricating resin film in this order)
- No. 3 Surface treatment under the same conditions as in Example 1 of JP 2008-224204 (comprising a chemical conversion film, a corrosion-resistant resin film, and a hydrophilic film in this order)
- No. 4 Surface treatment under the same conditions as Comparative Example 21 of JP 2010-223514 A (comprising a chemical conversion film and a corrosion-resistant resin film in this order)
- Component composition is shown in Table 1, and production conditions are shown in Tables 2 and 3. In the table, those not satisfying the scope of the present invention are indicated by underlining the numerical values, and those not containing a component are indicated by “ ⁇ ”. In addition, No. Since “30” was not able to produce the fin material, “-” is written in the temper annealing column.
- No. 16 is based on the aluminum alloy fin material based on the description of Patent Document 1 (Invention Example 1 of Table 2 (however, the hot rolling end temperature and the plate thickness after hot rolling (3.5 mm) are different), No. 13 is based on an aluminum alloy fin material based on the description of Patent Document 2 (Invention Example 4 in Table 1 (however, the processing method (drawing process) is different)), and No.
- No. 34 is an aluminum alloy based on the description of Patent Document 4, which is based on the aluminum alloy fin material based on the description in Reference 3 (Invention Example 3 in Table 1 (however, the processing method (drawless processing) is different)) It is based on a fin material (Invention Example 11 in Table 2 (however, the plate thickness after cold rolling (0.115 mm thickness) is different)).
- the average grain size of subcrystal grains and the number of intermetallic compounds of 3 ⁇ m or more were measured by the following method. Furthermore, strength and elongation were measured by the following methods.
- the average grain size of the sub-crystal grains is based on the data obtained by analyzing the orientation of the scanning electron microscope (SEM) structure obtained by photographing the sample surface at an observation magnification of 1,000 times by the EBSD method at a measurement interval of 0.10 ⁇ m. Calculation was performed by automatic calculation on OIM (Orientation Imaging Microscopy.TM) software. That is, the total area of the fin material was divided by the number of crystal grains counted by SEM / EBSD measurement data, and the diameter when the area of each crystal grain was approximated to a circle was defined as the average grain size of the subcrystal grains.
- SEM scanning electron microscope
- the number of crystal grains a crystal grain surrounded by a crystal grain boundary whose orientation difference between adjacent crystal grains is within 2 ° was counted as one crystal grain.
- Number of intermetallic compounds exceeding 3 ⁇ m The number of compounds having a size exceeding 3 ⁇ m was calculated by image analysis of a scanning electron microscope (SEM) structure obtained by photographing a sample surface with an observation magnification of 500 times and an area of 1.0 mm 2 .
- the size of a compound means the maximum length of each compound.
- a tensile test piece according to JIS No. 5 was cut out from the fin material so that the tensile direction was parallel to the rolling direction.
- a tensile test according to JISZ2241 was performed on this test piece, and tensile strength, 0.2% yield strength, and elongation were measured.
- the tensile speed in evaluation of a present Example and a comparative example was performed at 5 mm / min.
- the produced fin material was press-molded by combination molding, and the color cracking resistance was evaluated.
- the color cracking resistance evaluation was evaluated by visually counting the cracks generated in the collar portion with respect to 400 holes of the press-formed product.
- “Number of cracks / 400 ⁇ 100 (%)” was defined as an occurrence rate, and the occurrence rate was defined as ( ⁇ ) when less than 3%, ( ⁇ ) when 3% or more and less than 5%, and ( ⁇ ) when 5% or more. And what was either ((double-circle)) or ((circle)) in all 90 micrometers and 80 micrometers was set as the pass.
- No. No. 15 was inferior in color cracking resistance due to work hardening because the Cu content exceeded the upper limit.
- No. 16 since the Mn content exceeded the upper limit, coarse intermetallic compounds increased and the color cracking resistance was poor.
- No. 28 was inferior in color cracking resistance because the temperature of the homogenization heat treatment was less than the lower limit value, so that the subcrystal grain size was large.
- No. No. 29 was inferior in color cracking resistance because the temperature of the homogenization heat treatment exceeded the upper limit value, so that the subcrystal grain size was increased, the proof stress exceeded the upper limit value.
- No. No. 30 because the finish temperature of hot finish rolling was less than the lower limit, rolling itself was difficult, and the fin material could not be manufactured.
- No. No. 31 because the finish temperature of hot finish rolling exceeds the upper limit, the subcrystal grain size was large and the color cracking resistance was poor.
- No. No. 32 had a mixed grain structure because the tempering temperature exceeded the upper limit, and the proof stress was less than the lower limit, resulting in poor color cracking resistance.
- the fin materials of 16, 13, 17, and 34 are assumed to be the conventional aluminum alloy fin materials described in Patent Document 1, Patent Document 2, Patent Document 3, and Patent Document 4, respectively. As shown in this example, these conventional aluminum alloy fin materials do not satisfy a certain level in the above evaluation. Therefore, this example objectively revealed that the aluminum alloy fin material for a heat exchanger for a combination press according to the present invention is superior to the conventional aluminum alloy fin material.
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Abstract
Description
前記した従来の技術では、加工性の向上が図られてはいるものの、近年においては、熱交換器のさらなるコンパクト化や軽量化、高性能化に加え、より加工のし易いフィン材の供給が期待されていることから、さらなる加工性の向上が求められている。
ここで、特許文献1に記載のフィン材は、耐カラー割れ性の改善を図っている。しかし、Mnを積極添加しているため、Mnの含有量および製造条件によっては、粗大な金属間化合物、あるいは、固溶Mnにより加工硬化しやすくなるという問題がある。そのため、耐カラー割れの改善には余地がある。
このような構成によれば、Tiを所定量添加することで、鋳塊組織が微細化される。
このような構成によれば、耐食性や親水性、成形性等、使用環境や用途等に応じた特性を向上させることができる。
本発明に係るフィン材は、Feを所定量含有し、残部がAlおよび不可避的不純物からなり、Al純度が99.30質量%以上のアルミニウム合金からなるコンビネーションプレス用としてのものである。そして、このフィン材の厚みが0.115mm未満であり、亜結晶粒の平均粒径を2.5μm以下および耐力を100~130N/mm2に規定したものである。また、3μmを超える金属間化合物を2000個/mm2以下に規定したものである。また、アルミニウム合金の化学成分について、必要に応じてCuを所定量含有し、アルミニウム合金に含まれる不可避的不純物のうち、Si、Mn、Crを所定量以下または所定量未満に抑制することが好ましい。さらに、必要に応じてTiを所定量含有してもよい。
以下、各構成について、まず、化学成分について説明した後、その他の構成について説明する。
Feは、Al-Fe系金属間化合物を形成(あるいは、アルミニウムマトリクス中に固溶)して、プレス成形時における亜結晶粒を微細にすることができるために、加工硬化抑制に寄与する元素であり、カラー割れ不良を減少させる効果がある。また、アルミニウム合金板の亜結晶粒の大きさに寄与する効果や、強度を向上させる効果も有する。Fe含有量が0.010質量%未満では、前記の効果が得られずに、プレス成形でカラー割れ性に劣る。一方、0.4質量%を超えると、強度が高くなり過ぎ、また、粗大な金属間化合物が形成され、耐カラー割れ性が劣る。したがって、Fe含有量は、0.010~0.4質量%とする。
薄肉化した時の剛性を確保するためには、さらにCuを添加することが望ましい。その効果は、0.005質量%以上の添加により得られる。一方で、Cu含有量が0.05質量%を超えると、加工硬化を招き、耐アベック性を低下させる他、耐カラー割れ性および耐食性の低下を招く。したがって、剛性を確保させるためにCuを添加する場合には、Cu含有量は、0.005~0.05質量%とする。さらに好ましくは、0.01~0.05質量%である。
Siは、不可避的不純物として混入する元素であるが、Si含有量が0.15質量%を超えると、晶出物(金属間化合物)が粗大化し、これが成形加工時の応力集中点となり、割れの起点となる。したがって、Siを含有する場合には、Si含有量は、0.15質量%以下とする。なお、0質量%まで抑制してもよい。
Mnは、不可避的不純物として混入する元素であるが、Mn含有量が0.015質量%以上になると、晶出物(金属間化合物)が粗大化し、これが成形加工時の応力集中点となり、割れの起点となる。したがって、Mnを含有する場合には、Mn含有量は、0.015質量%未満に抑制する。さらには、0.005質量%未満に抑制することが好ましい。なお、0質量%まで抑制してもよい。
Crは、不可避的不純物として混入する元素であるが、Cr含有量が0.015質量%を超えると、晶出物(金属間化合物)が粗大化し、これが成形加工時の応力集中点となり、割れの起点となる。したがって、Crを含有する場合には、Cr含有量は、0.015質量%以下に抑制する。なお、0質量%まで抑制してもよい。
Tiは、鋳塊組織の微細化のために、Al-Ti-B中間合金として添加しても良い。すなわち、Ti:B=5:1あるいは5:0.2の割合としたAl-Ti-B鋳塊微細化剤を、ワッフルあるいはロッドの形態で溶湯(スラブ凝固前における、溶解炉、介在物フィルター、脱ガス装置、溶湯流量制御装置へ投入された、いずれかの段階での溶湯)へ添加してもよく、Ti量で、0.05質量%までの含有は許容される。Ti含有量が0.01質量%未満では、鋳塊組織微細化の効果が得られない。一方、0.05質量%を超えると、晶出物(金属間化合物)が粗大化し、これが成形加工時の応力集中点となり、割れの起点となる。したがって、Tiを添加する場合には、Ti含有量は、0.01~0.05質量%とする。
フィン材の成分は前記の他、残部がAlおよび不可避的不純物からなるものである。なお、不可避的不純物として、前記したSi、Mn、Crの他、例えば、地金や中間合金に含まれている、通常知られている範囲内のMg、Zn、Zr、Ce、Ga、V、Ni等は、Al純度が、99.30質量%未満とならない範囲で、それぞれ0.05質量%までの含有は許容される。
Al純度が、99.30質量%未満では、金属間化合物の増加に伴い、カラー割れが増加し、耐食性が低下する。また、耐力が高くなる。したがって、Al純度は、99.30質量%以上とする。
本発明は、近年における熱交換器のコンパクト化や軽量化、高性能化等の要請により、フィン材の薄肉化を図る観点から、0.115mm未満の厚みのフィン材を対象とする。したがって、フィン材の厚みは、0.115mm未満とする。
0.115mm未満の厚みのフィン材での伸びの増加のためには、合金中の亜結晶粒の平均粒径を2.5μm以下とすることが必要である。亜結晶粒の平均粒径が2.5μmを超えると、フィン材の伸びが十分に得られない。したがって、亜結晶粒の平均粒径は、2.5μm以下とする。なお、下限値は特に規定しないが、0μmであってもよい(すなわち、亜結晶粒を含まなくてもよい)。この様な範囲にすることにより、固溶Mnや固溶Cu等により加工硬化するような場合であっても、カラー割れの発生を抑制することができる。
まず、走査電子顕微鏡(SEM:Scanning Electron Microscopy-Electron)組織をEBSD(Electron Back Scattered Diffraction Pattern)法により方位解析する。EBSD法は、試料に電子線を照射し、その際に生じる反射電子菊池線回折を利用して結晶方位を特定するものである。また、結晶方位解析には、例えば、TSL社製OIM(Orientation Imaging Microscopy. TM)を用いることができる。
そして、亜結晶粒の平均粒径は、このSEM/EBSD測定データにより結晶粒の数を算出し、フィン材の全面積を結晶粒の数で除し、各結晶粒の面積を円と近似した場合の直径を亜結晶粒の平均粒径と定義する。
なお、亜結晶粒の平均粒径および金属間化合物の個数は、成分組成と、後記する製造条件により制御することができる。具体的には、亜結晶粒の平均粒径は、各成分の含有量、均質化熱処理条件(温度と時間)、熱間仕上げ圧延終了温度、冷間加工率、調質焼鈍条件(温度と時間)、金属間化合物の個数は、各成分の含有量、均質化熱処理条件(温度と時間)等により制御する。
本発明のフィン材は、コンビネーションプレス用としてのものであるため、耐力は100~130N/mm2とする。耐力が100N/mm2未満では、強度が不足し、コンビネーションプレス成形の際にカラー割れが生じる。一方、130N/mm2を超えると、強度が高過ぎ、コンビネーションプレス成形の際にカラー割れが生じる。したがって、耐力は100~130N/mm2とする。なお、好ましくは100N/mm2以上130N/mm2未満、さらに好ましくは、100N/mm2以上120N/mm2未満である。
耐力の測定は、例えば、フィン材から、引張方向が圧延方向と平行になるようにJIS5号による引張試験片を切り出し、JISZ2241による引張試験を実施することで行なうことができる。
(表面処理皮膜)
表面処理皮膜としては、使用環境や用途に応じ、化成皮膜や樹脂皮膜、無機皮膜が挙げられ、これらを組み合わせ(化成皮膜上に樹脂皮膜、無機皮膜を設け)てもよい。また、樹脂皮膜、無機皮膜としては、耐食性樹脂皮膜、親水性樹脂皮膜、親水性無機皮膜、潤滑性樹脂皮膜等が挙げられ、これらを適宜組み合わせてもよい。
本発明に係るフィン材の製造方法は、前記したフィン材の製造方法であって、熱処理工程と、熱間圧延工程と、冷間加工工程と、調質焼鈍工程と、を行うものである。さらに必要に応じて、鋳塊作製工程や表面処理工程を含んでもよい。
以下、各工程について説明する。
鋳塊作製工程は、アルミニウム合金を溶解、鋳造してアルミニウム合金鋳塊を作製する工程である。
鋳塊作製工程では、前記した化学成分を有するアルミニウム合金を溶解した溶湯から、所定形状の鋳塊を作製する。アルミニウム合金を溶解、鋳造する方法は、特に限定されるものではなく、従来公知の方法を用いればよい。例えば、真空誘導炉を用いて溶解し、連続鋳造法や、半連続鋳造法を用いて鋳造することができる。
熱処理工程は、前記アルミニウム合金の化学成分を有するアルミニウム合金鋳塊に、450~500℃の温度で1時間以上の熱処理(均質化熱処理)を施す工程である。
熱処理温度が450℃未満では、鋳塊の組織の均質化が不十分となる。また、熱間加工性の低下を招く。さらに亜結晶粒径が大きくなる。一方、500℃を超えると、加熱中で微細化する微細金属間化合物が粗大化し、亜結晶粒が粗大化して伸びが低下する。さらに、耐力が高くなる。また、固溶量の増加を招く。したがって、熱処理温度は、450~500℃とする。また、熱処理は保持時間1時間以上であれば前記効果を得られるため、特に上限を規定する必要はない。一方で、10時間を超えると効果が飽和することから、経済的には、熱処理時間は24時間以内が好ましい。
熱間圧延工程は、前記熱処理後に、熱間仕上げ圧延の終了温度が250℃以上300℃未満となる条件で熱間圧延を施す工程である。
熱間仕上げ圧延の終了温度が250℃未満では、材料の圧延性が低下し、圧延自体が困難となったり、板厚制御が難しくなったりして、生産性が低下する。一方、300℃以上では、熱延板で再結晶組織となるために、調質焼鈍後に繊維状の同一結晶方位群が生成し、ピアス&バーリング工程時にくびれを生じる。また、亜結晶粒径が大きくなる。したがって、熱間仕上げ圧延の終了温度は、250℃以上300℃未満とする。より好ましくは、260~290℃である。
冷間加工工程は、前記熱間圧延後に、冷間加工率96%以上の冷間加工(冷間圧延)を施す工程である。
熱間圧延終了後、冷間加工を1回、あるいは複数回行なって、フィン材を所望の最終板厚とする。ただし、冷間加工率が96%未満では、調質焼鈍後に亜結晶粒が粗大化する。また、耐力が低くなる。したがって、冷間加工における冷間加工率は、96%以上とする。ここで、冷間加工の途中で中間焼鈍を行なった場合、冷間加工率は中間焼鈍後から最終板厚までの加工率である。よって、中間焼鈍を行なうと、96%以上の冷間加工率とすることが困難となることから、中間焼鈍は行なわない。なお、冷間加工率は高いほど好ましいため、上限は特に設けない。
調質焼鈍工程は、前記冷間加工後に、180~260℃の温度で1~6時間保持する調質焼鈍(仕上げ焼鈍)を施す工程である。
調質焼鈍の温度が180℃未満では、充分な伸びが得られない。また、耐力が高くなる。一方、260℃を超えると、焼鈍後に再結晶粒を生じ、これを起点に割れが生じる。また、亜結晶粒の微細化が促進されない。さらに、耐力が低くなる。したがって、調質焼鈍の温度は、180~260℃とする。なお、調質焼鈍は1時間以上行うことが通常であり、6時間を超えると効果が飽和することから、保持時間は1~6時間とする。
表面処理工程は、調質焼鈍後のフィン材に表面処理を施す工程である。
表面処理工程において、化成皮膜を形成する場合には、通常の塗布型または反応型の薬剤を用いた化成処理によって行うことができる。耐食性樹脂皮膜、親水性樹脂皮膜、潤滑性樹脂皮膜等の樹脂皮膜を形成する場合には、ロールコーターを用いた塗布、乾燥によって行うことができる。
コンビネーション成形(コンビネーションプレス)は、第1工程で張出し、第2工程で絞り成形、第3工程で打ち抜きおよび穴広げ加工(ピアス&バーリング成形)、第4工程でしごき加工、第5工程でリフレア加工を施すものである。そして、本発明のフィン材は、耐カラー割れ性に優れるため、コンビネーション方式による成形加工時のカラー割れの発生を抑制することができる。
(実施例No.1~10、比較例No.11~21)
表1に示す組成のアルミニウム合金を、溶解、鋳造して鋳塊とし、この鋳塊に面削を施した後に、480℃にて4時間の均質化熱処理を施した。この均質化した鋳塊に、熱間仕上げ圧延の終了温度を270℃となるように制御して熱間圧延を施し、板厚3.0mmの熱間圧延板とした。さらに、それぞれ97.0%または97.3%程度の冷間加工率で冷間圧延を施して板厚を90μmおよび80μmとした後、表1に示す温度および保持時間の調質焼鈍を施してフィン材とした。
表2に示すアルミニウム合金(表1に対応する合金A,B,C)を、溶解、鋳造して鋳塊とし、この鋳塊に面削を施した後に、均質化熱処理、熱間圧延を施し、板厚3.0mmの熱間圧延板とした。さらに、No.35以外は、それぞれ97.0%または97.3%程度の冷間加工率で冷間圧延を施して板厚を90μmおよび80μmとした後、調質焼鈍を施してフィン材とした。No.35は、板厚3.0mmの熱間圧延板に50%の冷間加工率で冷間圧延を施した後、バッチ炉を用いて360℃×3hの中間焼鈍を実施した。その後さらに、それぞれ94.0%または94.7%程度の冷間加工率で冷間圧延を施して板厚を90μmおよび80μmとした後、調質焼鈍を施してフィン材とした。均質化熱処理、熱間仕上げ圧延の終了温度、調質焼鈍の条件は、表2に示すとおりである。なお、No.30はフィン材を製造できなかったものである。
表2のNo.22と同様のフィン材であるNo.36、37、表2のNo.27と同様のフィン材であるNo.38、39、表2のNo.29と同様のフィン材であるNo.40、41、表2のNo.32と同様のフィン材であるNo.42、43に対して以下の表面処理(No.1~4)を行った。
No.2:特許第3383914号公報の実施例1と同じ条件の表面処理(化成皮膜、親水性皮膜、潤滑性樹脂皮膜をこの順に備える)
No.3:特開2008-224204号公報の実施例1と同じ条件の表面処理(化成皮膜、耐食性樹脂皮膜、親水性皮膜をこの順に備える)
No.4:特開2010-223514号公報の比較例21と同じ条件の表面処理(化成皮膜、耐食性樹脂皮膜をこの順に備える)
亜結晶粒の平均粒径は、観察倍率1,000倍で試料表面を撮影した走査電子顕微鏡(SEM)組織を、測定間隔0.10μmにてEBSD法により方位解析したデータを基に、TSL社製OIM(Orientation Imaging Microscopy. TM)ソフト上で自動計算することにより算出した。すなわち、フィン材の全面積をSEM/EBSD測定データによりカウントされた結晶粒の数で除し、各結晶粒の面積を円と近似した場合の直径を亜結晶粒の平均粒径と定義した。なお、結晶粒の数は、隣接結晶粒間の方位差が2°以内の結晶粒界に囲まれた結晶粒を一つの結晶粒としてカウントした。
〔3μmを超える金属間化合物の個数〕
サイズが3μmを超える化合物数は、観察倍率500倍で、面積1.0mm2の試料表面を撮影した走査電子顕微鏡(SEM)組織を画像解析することにより算出した。なお、化合物のサイズとは個々の化合物の最大の長さを言う。
フィン材から、引張方向が圧延方向と平行になるようにJIS5号による引張試験片を切り出した。この試験片で、JISZ2241による引張試験を実施し、引張強さ、0.2%耐力、および、伸びを測定した。なお、本実施例および比較例の評価における引張速度は5mm/minで行った。
作製したフィン材にコンビネーション成形によりプレス成形を実施し、耐カラー割れ性を評価した。
耐カラー割れ性評価は、プレス成形品400穴に対して、カラー部に生じた割れを目視にてカウントすることで評価した。
「割れ数/400×100(%)」を発生率とし、発生率が3%未満を(◎)、3%以上5%未満を(○)、5%以上を(×)とした。そして、90μmおよび80μmのすべてにおいて(◎)、(○)のいずれかであったものを合格とした。
表1に示すように、実施例であるNo.1~10は、本発明の範囲を満たすため、耐カラー割れ性に優れていた。
No.11は、Si含有量が上限値を超えるため、粗大な金属間化合物が増加し、耐カラー割れ性に劣った。
表2に示すように、実施例であるNo.22~27は、本発明の範囲を満たすため、耐カラー割れ性に優れていた。
No.28は、均質化熱処理の温度が下限値未満のため、亜結晶粒径が大きくなり、耐カラー割れ性に劣った。No.29は、均質化熱処理の温度が上限値を超えるため、亜結晶粒径が大きくなり、また耐力が上限値を超え、耐カラー割れ性に劣った。
No.36~43における表面処理を施したフィン材の耐カラー割れ性は、表面処理を実施していないフィン材と同様の結果となった。
Claims (6)
- Fe:0.010~0.4質量%を含有し、残部がAlおよび不可避的不純物からなり、Al純度が99.30質量%以上のアルミニウム合金からなるコンビネーションプレス用熱交換器用アルミニウム合金フィン材であって、
前記コンビネーションプレス用熱交換器用アルミニウム合金フィン材の厚みが0.115mm未満であり、亜結晶粒の平均粒径が2.5μm以下および耐力が100~130N/mm2であることを特徴とするコンビネーションプレス用熱交換器用アルミニウム合金フィン材。 - さらに、最大長さが3μmを超える金属間化合物が2000個/mm2以下であることを特徴とする請求項1に記載のコンビネーションプレス用熱交換器用アルミニウム合金フィン材。
- 前記アルミニウム合金の化学成分について、さらに、Cu:0.005~0.05質量%を含有し、Si:0.15質量%以下、Mn:0.015質量%未満、Cr:0.015質量%以下に抑制することを特徴とする請求項1または請求項2に記載のコンビネーションプレス用熱交換器用アルミニウム合金フィン材。
- 前記アルミニウム合金の化学成分について、さらに、Ti:0.01~0.05質量%を含有することを特徴とする請求項1から請求項3のいずれか一項に記載のコンビネーションプレス用熱交換器用アルミニウム合金フィン材。
- フィン材表面に表面処理皮膜を備えることを特徴とする請求項1から請求項4のいずれか一項に記載のコンビネーションプレス用熱交換器用アルミニウム合金フィン材。
- 請求項1から請求項4のいずれか一項に記載のコンビネーションプレス用熱交換器用アルミニウム合金フィン材の製造方法であって、
前記アルミニウム合金の化学成分を有するアルミニウム合金鋳塊に、450~500℃の温度で1時間以上の熱処理を施す熱処理工程と、
前記熱処理後に、熱間仕上げ圧延の終了温度が250℃以上300℃未満となる条件で熱間圧延を施す熱間圧延工程と、
前記熱間圧延後に、冷間加工率96%以上の冷間加工を施す冷間加工工程と、
前記冷間加工後に、180~260℃の温度で1~6時間保持する調質焼鈍を施す調質焼鈍工程と、を行うことを特徴とするコンビネーションプレス用熱交換器用アルミニウム合金フィン材の製造方法。
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EP12764342.7A EP2692882A4 (en) | 2011-03-31 | 2012-03-06 | COMBINATION PRESSED ALUMINUM ALLOY LAMINATE MATERIAL FOR HEAT EXCHANGERS AND MANUFACTURING METHOD THEREFOR |
CN201280009048.8A CN103380222B (zh) | 2011-03-31 | 2012-03-06 | 组合冲压用热交换器用铝合金翅片材及其制造方法 |
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JP2011080854A JP5693333B2 (ja) | 2011-03-31 | 2011-03-31 | コンビネーションプレス用熱交換器用アルミニウム合金フィン材 |
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- 2012-03-06 MY MYPI2013002681A patent/MY161709A/en unknown
- 2012-03-06 WO PCT/JP2012/055660 patent/WO2012132785A1/ja active Application Filing
- 2012-03-06 CN CN201280009048.8A patent/CN103380222B/zh active Active
- 2012-03-06 EP EP12764342.7A patent/EP2692882A4/en not_active Withdrawn
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EP2692882A1 (en) | 2014-02-05 |
MY161709A (en) | 2017-05-15 |
CN103380222B (zh) | 2016-02-10 |
AU2012235013B2 (en) | 2015-08-27 |
EP2692882A4 (en) | 2014-11-05 |
CN103380222A (zh) | 2013-10-30 |
AU2012235013A1 (en) | 2013-08-15 |
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