JP2010106336A - Forging method of magnesium alloy - Google Patents
Forging method of magnesium alloy Download PDFInfo
- Publication number
- JP2010106336A JP2010106336A JP2008281264A JP2008281264A JP2010106336A JP 2010106336 A JP2010106336 A JP 2010106336A JP 2008281264 A JP2008281264 A JP 2008281264A JP 2008281264 A JP2008281264 A JP 2008281264A JP 2010106336 A JP2010106336 A JP 2010106336A
- Authority
- JP
- Japan
- Prior art keywords
- magnesium alloy
- forging
- range
- weight
- alloy material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 108
- 238000005242 forging Methods 0.000 title claims abstract description 101
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000013078 crystal Substances 0.000 claims abstract description 43
- 210000001787 dendrite Anatomy 0.000 claims abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011575 calcium Substances 0.000 claims abstract description 10
- 229910000765 intermetallic Inorganic materials 0.000 claims abstract description 10
- 239000011572 manganese Substances 0.000 claims abstract description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 9
- 239000011701 zinc Substances 0.000 claims abstract description 9
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 229910003023 Mg-Al Inorganic materials 0.000 claims abstract description 4
- 239000000956 alloy Substances 0.000 claims description 56
- 238000005266 casting Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 8
- 229910052787 antimony Inorganic materials 0.000 claims description 7
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 7
- 229910052790 beryllium Inorganic materials 0.000 claims description 7
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 6
- 230000000694 effects Effects 0.000 description 17
- 239000000047 product Substances 0.000 description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000005336 cracking Methods 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 238000010301 surface-oxidation reaction Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001122 Mischmetal Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910001562 pearlite Inorganic materials 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Images
Landscapes
- Forging (AREA)
Abstract
Description
本発明は、マグネシウム合金の鍛造方法に関するものである。 The present invention relates to a method for forging a magnesium alloy.
自動車を軽量化して、燃費削減、排ガス量低減等を図るために、ホイール、サスペンションアーム等の部品にアルミニウム合金が用いられている。また、さらに自動車を軽量化するために、前記自動車の部品にマグネシウム合金を用いることが検討されている。マグネシウムの比重は１．８であり、アルミニウムの比重が２．７であるのに比較してさらに小さく、現在実用化されている金属材料の中では最も小さいことが知られている。 Aluminum alloys are used in parts such as wheels and suspension arms in order to reduce the weight of automobiles and reduce fuel consumption and exhaust gas. Further, in order to further reduce the weight of the automobile, it has been studied to use a magnesium alloy for the parts of the automobile. Magnesium has a specific gravity of 1.8, which is smaller than the specific gravity of aluminum of 2.7, and is known to be the smallest among the metal materials currently in practical use.
前記自動車の部品等に用いられるマグネシウム合金は、ほとんどが鋳造材として用いられている。これは、鍛造用マグネシウム合金の素材が入手困難であり、高価であるためであると考えられる。 Most of the magnesium alloys used for automobile parts are used as casting materials. This is considered to be because the magnesium alloy material for forging is difficult to obtain and is expensive.
ところが、マグネシウム合金の鋳造材は、前記自動車の部品等に用いるには、十分な強度が得られないことがある。そこで、鋳造したマグネシウム合金素材を鍛造に用いることが試みられており、例えば、６〜１２重量％のアルミニウムを含むマグネシウム合金の鋳造体を鍛造用マグネシウム合金として用いる技術が知られている（特許文献１参照）。 However, the magnesium alloy casting material may not have sufficient strength to be used for the automobile parts. Thus, attempts have been made to use a cast magnesium alloy material for forging. For example, a technique is known in which a magnesium alloy casting containing 6 to 12% by weight of aluminum is used as a magnesium alloy for forging (patent document). 1).
前記技術において、６〜１２重量％のアルミニウムを含む前記マグネシウム合金としては、例えば、ＪＩＳに規定されるＡＺ８０合金を挙げることができるとされている。前記ＡＺ８０合金は、例えば、アルミニウム８．０重量％、亜鉛０．６７重量％、マンガン０．２１重量％、ケイ素０．０４２重量％、鉄０．００２重量％、銅０．００５重量％、ニッケル０．００１重量％を含み、残部がマグネシウムと不可避的不純物とからなるものである。 In the said technique, as said magnesium alloy containing 6 to 12 weight% aluminum, it is supposed that the AZ80 alloy prescribed | regulated to JIS can be mentioned, for example. The AZ80 alloy is, for example, aluminum 8.0 wt%, zinc 0.67 wt%, manganese 0.21 wt%, silicon 0.042 wt%, iron 0.002 wt%, copper 0.005 wt%, nickel It contains 0.001% by weight, and the balance consists of magnesium and inevitable impurities.
前記技術では、前記鋳造体を鍛造成形することにより、前記マグネシウム合金の平均結晶粒径を１００μｍ以下とし、結晶粒が微細化した部材を得ることができるとされている。前記部材は、前記鍛造成形の後、さらにＴ６処理を施すことにより結晶粒界に形成されるパーライト組織が微細となり、かつ析出量も多くなるため、前記結晶粒の微細化との相乗効果として、引張強度や伸び等の機械的特性の大幅な向上を図ることができるとされている。 According to the technique, by forging the casting, the magnesium alloy has an average crystal grain size of 100 μm or less, and a member with fine crystal grains can be obtained. Since the pearlite structure formed in the crystal grain boundary becomes fine by further applying the T6 treatment after the forging, the member has a large amount of precipitation, and as a synergistic effect with the refinement of the crystal grains, It is said that mechanical properties such as tensile strength and elongation can be greatly improved.
しかしながら、前記鍛造用マグネシウム合金は、鍛造したときに割れを発生することなく、高精度に型充満することができないとの不都合がある。
本発明は、かかる不都合を解消して、鍛造したときに割れを発生することなく、高精度に型充満することができ、優れた機械的強度を備える鍛造品を得ることができるマグネシウム合金の鍛造方法を提供することを目的とする。 The present invention eliminates such inconveniences and forges magnesium alloys that can be filled with high accuracy without cracking when forged, and can provide a forged product with excellent mechanical strength. It aims to provide a method.
かかる目的を達成するために、本発明のマグネシウム合金の鍛造方法は、全量に対し、６〜１０重量％の範囲のアルミニウムと、０．４〜２重量％の範囲の亜鉛と、０．０５〜０．３重量％の範囲のマンガンと、０．４〜１．５重量％の範囲のカルシウムと不可避的不純物とを含むマグネシウム合金からなる鋳造体を１２〜４０℃／秒の範囲の速度で冷却して、樹脂状晶のデンドライトアーム間隔が０．５〜１５μｍの範囲であり、Ｍｇ−Ａｌ金属間化合物からなる晶出物の粒子径が１〜１０μｍの範囲である第１の鍛造用マグネシウム合金素材を形成する工程と、第１の鍛造用マグネシウム合金素材に対して、２５０〜４５０℃の範囲の温度で、２０〜７０％の範囲の加工率の予備加工を施し、第２の鍛造用マグネシウム合金素材を形成する工程と、第２の鍛造用マグネシウム合金素材に対して鍛造加工を施す工程とを備えることを特徴とする。 In order to achieve this object, the magnesium alloy forging method of the present invention is based on the total amount of aluminum in the range of 6 to 10% by weight, zinc in the range of 0.4 to 2% by weight, and 0.05 to A casting made of a magnesium alloy containing manganese in the range of 0.3% by weight, calcium in the range of 0.4 to 1.5% by weight and unavoidable impurities is cooled at a rate in the range of 12 to 40 ° C./second. Then, the first magnesium alloy for forging in which the dendrite arm interval of the resinous crystal is in the range of 0.5 to 15 μm, and the particle diameter of the crystallized product made of the Mg—Al intermetallic compound is in the range of 1 to 10 μm. Forming the raw material and pre-processing the first forging magnesium alloy material at a temperature in the range of 250 to 450 ° C., with a processing rate in the range of 20 to 70%, and the second forging magnesium Form alloy material And a step of forging the second magnesium alloy material for forging.
本発明の鍛造方法では、まず、全量に対し、６〜１０重量％の範囲のアルミニウムと、０．４〜２重量％の範囲の亜鉛と、０．０５〜０．３重量％の範囲のマンガンと、０．４〜１．５重量％の範囲のカルシウムと不可避的不純物とを含むマグネシウム合金からなる鋳造体を鋳造する。 In the forging method of the present invention, first, aluminum in the range of 6 to 10% by weight, zinc in the range of 0.4 to 2% by weight, and manganese in the range of 0.05 to 0.3% by weight with respect to the total amount. And a cast body made of a magnesium alloy containing calcium and unavoidable impurities in the range of 0.4 to 1.5% by weight.
前記マグネシウム合金からなる鋳造体は、全量に対し、６〜１０重量％の範囲の量のアルミニウムを含有することにより、鋳造組織を微細化して結晶粒の粗大化を防止し、さらに柱状晶の発達を抑制する効果を得ることができる。前記マグネシウム合金からなる鋳造体、前記効果を得るために全量に対し、７〜９重量％の範囲のアルミニウムを含むことが好ましい。アルミニウムの含有量が６重量％未満では、鋳造組織を微細化し、柱状晶の発達を抑制する効果が得られないので好ましくない。また、アルミニウムの含有量が１０重量％を超えると、それ以上に鋳造組織を微細化し、柱状晶の発達を抑制する効果が得られないばかりか、鍛造性を阻害するので好ましくない。 The cast body made of the magnesium alloy contains aluminum in an amount in the range of 6 to 10% by weight with respect to the total amount, so that the cast structure is refined to prevent coarsening of crystal grains, and further, columnar crystals develop. The effect which suppresses can be acquired. It is preferable to contain aluminum in a range of 7 to 9% by weight with respect to the total amount in order to obtain the above-mentioned cast body made of the magnesium alloy. If the aluminum content is less than 6% by weight, it is not preferable because the cast structure is refined and the effect of suppressing the development of columnar crystals cannot be obtained. Further, if the aluminum content exceeds 10% by weight, it is not preferable because the cast structure is further refined and the effect of suppressing the development of columnar crystals cannot be obtained, and the forgeability is impaired.
前記マグネシウム合金からなる鋳造体は、全量に対し、０．４〜２重量％の範囲の量の亜鉛を含有することにより、機械的強度、特に耐力を向上させる効果を得ることができる。前記マグネシウム合金からなる鋳造体は、前記効果を得るために、全量に対し、０．８〜１．５重量％の範囲の亜鉛を含むことが好ましい。亜鉛の含有量が０．４重量％未満では機械的強度を向上する効果が得られず、２重量％を超えると、伸びが不十分になり鍛造性を阻害するので好ましくない。 The cast body made of the magnesium alloy can obtain an effect of improving mechanical strength, particularly proof stress, by containing zinc in an amount of 0.4 to 2% by weight with respect to the total amount. In order to obtain the above effect, the cast body made of the magnesium alloy preferably contains 0.8 to 1.5% by weight of zinc with respect to the total amount. If the zinc content is less than 0.4% by weight, the effect of improving the mechanical strength cannot be obtained, and if it exceeds 2% by weight, the elongation becomes insufficient and the forgeability is hindered.
前記マグネシウム合金からなる鋳造体は、全量に対し、０．０５〜０．３重量％の範囲の量のマンガンを含有することにより、粒界にＭｇ−Ｍｎ金属間化合物が析出して、機械的強度を向上する効果を得ることができる。また、前記マグネシウム合金からなる鋳造体は、粒界にＭｇ−Ｍｎ金属間化合物が析出することにより、高温における機械的強度を向上する効果を得ることもできる。前記マグネシウム合金からなる鋳造体は、前記効果を得るために、全量に対し、０．１〜０．２５重量％の範囲のマンガンを含むことが好ましい。マンガンの含有量が０．０５重量％未満では、機械的強度を向上する効果が得られず、０．３重量％を超えると晶出物が多くなり鍛造性を阻害するので好ましくない。 When the cast body made of the magnesium alloy contains manganese in an amount in the range of 0.05 to 0.3% by weight with respect to the total amount, the Mg—Mn intermetallic compound precipitates at the grain boundary, and mechanically. The effect of improving the strength can be obtained. Moreover, the cast body which consists of the said magnesium alloy can also acquire the effect which improves the mechanical strength in high temperature, when a Mg-Mn intermetallic compound precipitates in a grain boundary. In order to obtain the effect, the cast body made of the magnesium alloy preferably contains 0.1 to 0.25% by weight of manganese with respect to the total amount. If the manganese content is less than 0.05% by weight, the effect of improving the mechanical strength cannot be obtained, and if it exceeds 0.3% by weight, the amount of crystallized substances increases and the forgeability is impaired.
前記マグネシウム合金からなる鋳造体は、全量に対し、０．４〜１．５重量％の範囲の量のカルシウムを含有することにより、粒界にＭｇ−Ｃａ金属間化合物が析出して、機械的強度を向上すると共に、耐クリープ性を向上する効果を得ることができる。また、前記マグネシウム合金からなる鋳造体は、粒界にＭｇ−Ｃａ金属間化合物が析出することにより、高温における機械的強度及び耐クリープ性を向上する効果を得ることもできる。前記マグネシウム合金からなる鋳造体は、前記効果を得るために、全量に対し、０．４〜１．５重量％の範囲のカルシウムを含むことが好ましい。カルシウムの含有量が０．４重量％未満では機械的強度及び耐クリープ性を向上する効果が得られず、１．５重量％を超えるとマグネシウム合金溶湯の粘度が増大して鋳造体を得ることが困難になったり、得られた鋳造体に高温割れが発生するので好ましくない。 The cast body made of the magnesium alloy contains calcium in an amount in the range of 0.4 to 1.5% by weight with respect to the total amount. The effect of improving the creep resistance while improving the strength can be obtained. Moreover, the cast body which consists of the said magnesium alloy can also acquire the effect which improves the mechanical strength and creep resistance in high temperature, when a Mg-Ca intermetallic compound precipitates in a grain boundary. In order to obtain the above effect, the cast body made of the magnesium alloy preferably contains calcium in the range of 0.4 to 1.5% by weight with respect to the total amount. If the calcium content is less than 0.4% by weight, the effect of improving the mechanical strength and creep resistance cannot be obtained. If the calcium content exceeds 1.5% by weight, the viscosity of the magnesium alloy melt increases to obtain a cast body. Is not preferable, and high temperature cracking occurs in the obtained casting.
本発明の鍛造方法では、次に、前記マグネシウム合金からなる鋳造体を１２〜４０℃／秒の範囲の速度で冷却する。この結果、前記組成を備えると共に、樹枝状晶のデンドライトアーム間隔が０．５〜１５μｍの範囲であり、Ｍｇ−Ａｌ金属間化合物からなる晶出物の粒子径が１〜１０μｍの範囲である第１の鍛造用マグネシウム合金素材を得ることができる。 In the forging method of the present invention, the cast body made of the magnesium alloy is then cooled at a speed in the range of 12 to 40 ° C./second. As a result, the composition has the above composition, the dendritic arm has a dendrite arm interval in the range of 0.5 to 15 μm, and the crystallized particle size of the Mg—Al intermetallic compound is in the range of 1 to 10 μm. 1 forging magnesium alloy material can be obtained.
前記第１の鍛造用マグネシウム合金素材は、前記樹枝状晶のデンドライトアーム間隔が０．５〜１５μｍの範囲であり、前記晶出物の粒子径が１〜１０μｍの範囲であることにより、優れた鍛造性を得ることができ、しかも鍛造したときに優れた機械的強度を備える部材を得ることができる。前記第１の鍛造用マグネシウム合金素材は、前記樹枝状晶のデンドライトアーム間隔が１５μｍを超えるか、前記晶出物の粒子径が１０μｍを超えると、鍛造性が阻害される上、鍛造により得られた部材の機械的強度を向上することができない。また、前記第１の鍛造用マグネシウム合金素材において、前記樹枝状晶のデンドライトアーム間隔を０．５μｍ未満とし、前記晶出物の粒子径を１μｍ未満とすることは、技術的に困難である。 The first forging magnesium alloy material is excellent in that the dendrite arm spacing of the dendritic crystals is in the range of 0.5 to 15 μm, and the particle diameter of the crystallized material is in the range of 1 to 10 μm. Forgeability can be obtained, and a member having excellent mechanical strength when forged can be obtained. The first magnesium alloy material for forging is obtained by forging, if the dendrite arm spacing of the dendritic crystals exceeds 15 μm, or if the particle size of the crystallized material exceeds 10 μm, the forgeability is hindered. The mechanical strength of the remaining member cannot be improved. In the first magnesium alloy material for forging, it is technically difficult to set the dendrite arm interval of the dendritic crystal to less than 0.5 μm and the particle size of the crystallized material to less than 1 μm.
ところで、前記第１の鍛造用マグネシウム合金素材は、前記鋳造体を１２〜４０℃／秒の範囲の速度で冷却するだけでは、結晶粒径を十分に小さくすることができない。そこで、本発明の鍛造方法では、次に、前記第１の鍛造用マグネシウム合金素材に対して、２５０〜４５０℃の範囲の温度で、２０〜７０％の範囲の加工率の予備加工を施す。 By the way, the crystal grain size of the first magnesium alloy material for forging cannot be sufficiently reduced only by cooling the cast body at a speed in the range of 12 to 40 ° C./second. Therefore, in the forging method of the present invention, next, the first magnesium alloy material for forging is preliminarily processed at a temperature in the range of 250 to 450 ° C. and a processing rate in the range of 20 to 70%.
この結果、前記第１の鍛造用マグネシウム合金素材の結晶粒径が微細化された第２の鍛造用マグネシウム合金素材を得ることができる。前記予備加工の温度が２５０℃未満では、前記第１の鍛造用マグネシウム合金素材の結晶粒径を微細化することができない。また、前記予備加工の温度が４５０℃を超えると、結晶粒が部分的に粗大化したり、前記第１の鍛造用マグネシウム合金素材に高温割れを発生するおそれがある。 As a result, a second forging magnesium alloy material in which the crystal grain size of the first forging magnesium alloy material is refined can be obtained. When the temperature of the preliminary processing is less than 250 ° C., the crystal grain size of the first magnesium alloy material for forging cannot be refined. On the other hand, if the temperature of the preliminary processing exceeds 450 ° C., the crystal grains may be partially coarsened or hot cracks may occur in the first forging magnesium alloy material.
一方、前記予備加工の温度が２５０〜４５０℃の範囲であっても、前記加工率が２０％未満であるときには、前記第２の鍛造用マグネシウム合金素材の結晶粒径を微細化することができない。また、前記予備加工の加工率を７０％を超えるものとすることは、経済的に不利になる。 On the other hand, even if the temperature of the preliminary processing is in the range of 250 to 450 ° C., the crystal grain size of the second magnesium alloy material for forging cannot be refined when the processing rate is less than 20%. . In addition, it is economically disadvantageous that the processing rate of the preliminary processing exceeds 70%.
本発明の鍛造方法では、次に、前記第２の鍛造用マグネシウム合金素材に対して鍛造加工を施す。前記第２の鍛造用マグネシウム合金素材は、前述のように結晶粒径が微細化されているので、鍛造したときに割れを発生することなく、高精度に型充満することができ、優れた機械的強度を備える鍛造品を得ることができる。 Next, in the forging method of the present invention, forging is performed on the second magnesium alloy material for forging. Since the second forging magnesium alloy material has a fine crystal grain size as described above, it can be filled with high precision without cracking when it is forged. Forgings with sufficient strength can be obtained.
また、本発明の鍛造方法において、前記マグネシウム合金からなる鋳造体は、全量に対し、０．０１〜０．３重量％の範囲のアンチモンまたは０．００６〜０．２重量％の範囲のベリリウムを含むことが好ましい。前記マグネシウム合金からなる鋳造体は、前記範囲のアンチモンと、前記範囲のベリリウムとを両方とも含んでいてもよく、どちらか一方のみを含んでいてもよい。 In the forging method of the present invention, the cast body made of the magnesium alloy contains 0.01 to 0.3% by weight of antimony or 0.006 to 0.2% by weight of beryllium with respect to the total amount. It is preferable to include. The cast body made of the magnesium alloy may contain both the range of antimony and the range of beryllium, or may contain only one of them.
前記マグネシウム合金からなる鋳造体は、前記範囲のアンチモンまたは前記範囲のベリリウムを含むことにより、鋳造体の組織をさらに微細化して、鍛造性及び鍛造により得られた部材の機械的強度を向上することができると共に、マグネシウム合金溶湯の表面酸化を防止して、鋳造体の表面肌を美麗にすることができる。 The cast body made of the magnesium alloy contains antimony in the above range or beryllium in the above range to further refine the structure of the cast body and improve the forgeability and the mechanical strength of the member obtained by forging. In addition, the surface oxidation of the magnesium alloy melt can be prevented, and the surface skin of the cast body can be made beautiful.
前記アンチモンの含有量が０．０１重量％未満では、鋳造体の組織をさらに微細化する効果が十分に得られないことがあり、０．３重量％を超えるとＭｇ−Ｓｂ金属間化合物が析出して、鍛造性及び鍛造により得られた部材の機械的強度を十分に向上することができないことがある。また、前記ベリリウムの含有量が０．００６重量％未満では、マグネシウム合金溶湯の表面酸化を十分に防止できないことがあり、０．２重量％を超えるとマグネシウム合金溶湯の粘度が増大して鋳造欠陥が発生しやすくなる。 If the content of antimony is less than 0.01% by weight, the effect of further refinement of the structure of the cast body may not be obtained sufficiently, and if it exceeds 0.3% by weight, Mg—Sb intermetallic compound is precipitated. Thus, the forgeability and the mechanical strength of the member obtained by forging may not be sufficiently improved. Further, if the beryllium content is less than 0.006% by weight, surface oxidation of the molten magnesium alloy may not be sufficiently prevented. If it exceeds 0.2% by weight, the viscosity of the molten magnesium alloy will increase, resulting in a casting defect. Is likely to occur.
さらに、本発明の鍛造方法において、前記マグネシウム合金からなる鋳造体は、全量に対し、１．２重量％以下の範囲のセリウムを含むことが好ましい。 Furthermore, in the forging method of the present invention, the cast body made of the magnesium alloy preferably contains cerium in a range of 1.2% by weight or less based on the total amount.
前記マグネシウム合金からなる鋳造体は、前記範囲のセリウムを含むことにより、結晶粒界に金属間化合物であるＭｇ９Ｃｅが晶出することにより、高温における機械的強度を向上することができ、特に２５０℃以下の範囲で耐熱性が向上する。前記セリウムは、僅かでも含まれることにより、高温における機械的強度を向上する効果を得ることができるが、含有量が１．２重量％を超えると、それ以上耐熱性を向上する効果が得られないばかりか、前記金属間化合物の晶出が増大して十分な鍛造性が得られなくなることがある。前記セリウムは、希土類金属の混合物であるミッシュメタルとして、前記マグネシウム合金に添加することができる。 The cast body made of the magnesium alloy can improve mechanical strength at high temperatures by containing cerium in the above range, whereby Mg 9 Ce, which is an intermetallic compound, crystallizes at the grain boundary. Heat resistance improves in the range of 250 ° C. or less. Although the cerium is contained in a small amount, it can obtain the effect of improving the mechanical strength at high temperature, but when the content exceeds 1.2% by weight, the effect of further improving the heat resistance is obtained. In addition, the crystallization of the intermetallic compound may increase and sufficient forgeability may not be obtained. The cerium can be added to the magnesium alloy as a misch metal that is a mixture of rare earth metals.
次に、添付の図面を参照しながら本発明の実施の形態についてさらに詳しく説明する。 Next, embodiments of the present invention will be described in more detail with reference to the accompanying drawings.
本実施形態の鍛造方法では、まず、全量に対し、６〜１０重量％の範囲のアルミニウムと、０．４〜２重量％の範囲の亜鉛と、０．０５〜０．３重量％の範囲のマンガンと、０．４〜１．５重量％の範囲のカルシウムと不可避的不純物とを含むマグネシウム合金からなる鋳造体を鋳造する。 In the forging method of this embodiment, first, aluminum in the range of 6 to 10% by weight, zinc in the range of 0.4 to 2% by weight, and in the range of 0.05 to 0.3% by weight with respect to the total amount. A cast body made of a magnesium alloy containing manganese, calcium in the range of 0.4 to 1.5% by weight and inevitable impurities is cast.
また、前記マグネシウム合金からなる鋳造体は、全量に対し、０．０１〜０．３重量％の範囲のアンチモンまたは０．００６〜０．２重量％の範囲のベリリウムを含むことが好ましい。前記マグネシウム合金からなる鋳造体は、前記範囲のアンチモンと、前記範囲のベリリウムとを両方とも含んでいてもよく、どちらか一方のみを含んでいてもよい。 The cast body made of the magnesium alloy preferably contains 0.01 to 0.3% by weight of antimony or 0.006 to 0.2% by weight of beryllium with respect to the total amount. The cast body made of the magnesium alloy may contain both the range of antimony and the range of beryllium, or may contain only one of them.
さらに、前記マグネシウム合金からなる鋳造体は、全量に対し、１．２重量％以下の範囲のセリウムを含むことが好ましい。 Further, the cast body made of the magnesium alloy preferably contains cerium in a range of 1.2% by weight or less based on the total amount.
本実施形態の鍛造方法では、次に、前記マグネシウム合金からなる鋳造体を１２〜４０℃／秒の範囲の速度で冷却し、第１の鍛造用マグネシウム合金素材を得る。 In the forging method of the present embodiment, the cast body made of the magnesium alloy is then cooled at a speed in the range of 12 to 40 ° C./second to obtain the first magnesium alloy material for forging.
次に、前述のようにして得られた第１の鍛造用マグネシウム合金素材における前記鋳造体の冷却速度と、前記樹枝状晶のデンドライトアーム間隔（ＤＡＳ）、前記晶出物の粒子径及び結晶粒径との関係を図１に示す。図１から、前記マグネシウム合金からなる鋳造体を１２℃／秒以上の速度で冷却することにより、前記樹枝状晶のデンドライトアーム間隔を１５μｍ以下にすることができると共に、前記晶出物の粒子径を１０μｍ以下とすることができることが明らかである。また、前記樹枝状晶のデンドライトアーム間隔と、前記晶出物の粒子径との間には、相関関係があることが明らかである。 Next, the cooling rate of the cast body in the first magnesium alloy material for forging obtained as described above, the dendrite arm dendrite arm interval (DAS), the crystallized particle diameter, and the crystal grains The relationship with the diameter is shown in FIG. From FIG. 1, the dendrite arm interval of the dendritic crystals can be made 15 μm or less by cooling the cast body made of the magnesium alloy at a rate of 12 ° C./second or more, and the particle diameter of the crystallized product It is clear that can be made 10 μm or less. In addition, it is clear that there is a correlation between the dendrite arm spacing of the dendrites and the particle size of the crystallized product.
一方、図１から、前記マグネシウム合金からなる鋳造体を１２℃／秒以上の速度で冷却しても、得られた鍛造用マグネシウム合金素材の結晶粒径を１５０μｍ以下とすることができないことが明らかである。 On the other hand, it is clear from FIG. 1 that even if the cast body made of the magnesium alloy is cooled at a rate of 12 ° C./second or more, the crystal grain size of the obtained magnesium alloy material for forging cannot be made 150 μm or less. It is.
ここで、前記樹枝状晶のデンドライトアーム間隔は、試料をミクロ研磨した後、金属顕微鏡で１００〜２００倍に拡大して写真撮影し、撮影された画像から樹枝状晶の二次枝の間隔を測定し、その実測値に顕微鏡の倍率を乗じることにより算出した。また、前記晶出物の粒子径及び鍛造用マグネシウム合金素材の結晶粒径は、例えば２００〜４００倍のミクロ写真の画像に任意の直線を引き、該直線にかかった晶出物の粒子径または鍛造用マグネシウム合金素材の結晶粒径をスケールで測定し、その実測値に該画像の倍率を乗じることにより算出した。
Here, the dendritic arm spacing of the dendritic crystal is obtained by taking a photograph by enlarging the
そこで、本実施形態の鍛造方法では、次に、前記第１の鍛造用マグネシウム合金素材に対して、２５０〜４５０℃の範囲の温度で、２０〜７０％の範囲の加工率の予備加工を施すことにより、第２の鍛造用マグネシウム合金素材を得る。 Therefore, in the forging method of the present embodiment, next, the first forging magnesium alloy material is preliminarily processed at a temperature in the range of 250 to 450 ° C. and a processing rate in the range of 20 to 70%. Thus, a second magnesium alloy material for forging is obtained.
次に、第１の鍛造用マグネシウム合金素材として、初期結晶粒径がそれぞれ２６５μｍ、２４５μｍ、１５０μｍの３種のマグネシウム合金素材を用意し、各マグネシウム合金素材に対して、４００℃の温度下、１０〜８０％の範囲で加工率を変化させて加工を施し、得られた鍛造用マグネシウム合金素材の結晶粒径を測定した。結果を図２に示す。図２から、初期結晶粒径の大きさに関わらず、加工率を２０％以上とすることにより、結晶粒径を１０μｍ以下に微細化できることが明らかである。 Next, as the first forging magnesium alloy material, three kinds of magnesium alloy materials having initial crystal grain sizes of 265 μm, 245 μm, and 150 μm, respectively, are prepared. Processing was performed while changing the processing rate in a range of ˜80%, and the crystal grain size of the obtained magnesium alloy material for forging was measured. The results are shown in FIG. From FIG. 2, it is clear that the crystal grain size can be reduced to 10 μm or less by setting the processing rate to 20% or more regardless of the initial crystal grain size.
本実施形態の鍛造方法では、次に、前記第２の鍛造用マグネシウム合金素材に対して鍛造加工を施すことにより、最終製品としての鍛造品を得る。 In the forging method of the present embodiment, a forged product as a final product is obtained by forging the second magnesium alloy material for forging.
次に、前記第２の鍛造用マグネシウム合金素材における結晶粒径と引張強度及び伸びとの関係を図３に示す。図３から、前記第２の鍛造用マグネシウム合金素材、結晶粒径が１０μｍ以下に微細化されていることにより、優れた引張強度及び伸びを備えていることが明らかである。 Next, the relationship between the crystal grain size, the tensile strength, and the elongation in the second magnesium alloy material for forging is shown in FIG. FIG. 3 clearly shows that the second magnesium alloy material for forging and the crystal grain size are refined to 10 μm or less, thereby providing excellent tensile strength and elongation.
前記第２の鍛造用マグネシウム合金素材は前述のように優れた伸びを備えているので、本実施形態の鍛造方法では、該第２の鍛造用マグネシウム合金素材に対して鍛造加工を施すことにより、割れを発生することなく、高精度に型充満することができる。従って、本実施形態の鍛造方法では、自動車用ピストン等の自動車や鉄道車両用の複雑な形状を備える部材を、従来よりも少ない工程で容易に製造することができる。 Since the second forging magnesium alloy material has excellent elongation as described above, in the forging method of this embodiment, by forging the second forging magnesium alloy material, The mold can be filled with high accuracy without causing cracks. Therefore, in the forging method of the present embodiment, a member having a complicated shape for automobiles and railway vehicles such as automobile pistons can be easily manufactured with fewer steps than in the past.
また、前記第２の鍛造用マグネシウム合金素材は前述のように優れた引張強度を備えているので、該第２の鍛造用マグネシウム合金素材に対して鍛造加工を施すことにより、自動車用ピストン等の自動車や鉄道車両用の大きな強度の要求される部材を製造することができる。 Further, since the second forging magnesium alloy material has an excellent tensile strength as described above, by subjecting the second forging magnesium alloy material to forging, the piston for automobiles and the like A member requiring high strength for automobiles and railway vehicles can be manufactured.
次に、本発明の鍛造方法の実施例と比較例とを示す。 Next, examples and comparative examples of the forging method of the present invention are shown.
まず、それぞれ表１に示す組成を備えるマグネシウム合金からなる鋳造体を鋳造し、得られた鋳造体を１５℃／秒の冷却速度で一方向凝固させることにより、試料１〜１４の第１の鍛造用マグネシウム合金素材を製造した。 First, castings made of magnesium alloys each having the composition shown in Table 1 were cast, and the obtained castings were solidified unidirectionally at a cooling rate of 15 ° C./second, whereby first forgings of samples 1 to 14 were performed. Magnesium alloy material was manufactured.
次に、前記第１の鍛造用マグネシウム合金素材のうち、試料１〜８については、本発明の鍛造方法の実施例として、４００℃の温度下に２１〜２６％の範囲の加工率で予備加工を施して、第２の鍛造用マグネシウム合金素材を形成し、該第２の鍛造用マグネシウム合金素材の結晶粒径を測定した。結果を表１に示す。 Next, of the first magnesium alloy material for forging, samples 1 to 8 are preliminarily processed at a processing rate in the range of 21 to 26% at a temperature of 400 ° C. as an example of the forging method of the present invention. The second forging magnesium alloy material was formed, and the crystal grain size of the second forging magnesium alloy material was measured. The results are shown in Table 1.
一方、前記第１の鍛造用マグネシウム合金素材のうち、試料９，１１〜１４については、本発明の鍛造方法の比較例として、全く予備加工を施さずに第２の鍛造用マグネシウム合金素材とし、該第２の鍛造用マグネシウム合金素材の結晶粒径を測定した。また、試料１０については、本発明の鍛造方法の比較例として、４００℃の温度下に１０％の加工率で予備加工を施して、第２の鍛造用マグネシウム合金素材を形成し、該第２の鍛造用マグネシウム合金素材の結晶粒径を測定した。結果を表１に示す。
On the other hand, among the first magnesium alloy material for forging, samples 9, 11 to 14 are used as a comparative example of the forging method of the present invention as a second magnesium alloy material for forging without any preliminary processing. The crystal grain size of the second magnesium alloy material for forging was measured. For
一方、表１から、第１の鍛造用マグネシウム素材に４００℃の温度下に、全く予備加工を施さないか、１０％の加工率で予備加工を施して、第２の鍛造用マグネシウム合金素材とした試料９〜１４（比較例）においては、該第２の鍛造用マグネシウム合金素材の結晶粒径が１００〜１３０μｍの範囲であり、該結晶粒径を微細化することができないことが明らかである。 On the other hand, from Table 1, the first forging magnesium material was not preliminarily processed at a temperature of 400 ° C. or preliminarily processed at a processing rate of 10%, and the second forging magnesium alloy material and In the samples 9 to 14 (comparative examples), the crystal grain size of the second magnesium alloy material for forging is in the range of 100 to 130 μm, and it is clear that the crystal grain size cannot be reduced. .
なし。 None.
Claims (3)
前記工程で得られた第１の鍛造用マグネシウム合金素材に対して、２５０〜４５０℃の範囲の温度で、２０〜７０％の範囲の加工率の予備加工を施し、第２の鍛造用マグネシウム合金素材を形成する工程と、
第２の鍛造用マグネシウム合金素材に対して鍛造加工を施す工程とを備えることを特徴とするマグネシウム合金の鍛造方法。 Aluminum in the range of 6-10 wt%, zinc in the range of 0.4-2 wt%, manganese in the range of 0.05-0.3 wt%, and 0.4-1.5 wt. A casting made of a magnesium alloy containing calcium in the range of wt% and inevitable impurities is cooled at a rate in the range of 12 to 40 ° C./second, and the dendrite arm spacing of the resinous crystals is in the range of 0.5 to 15 μm. A step of forming a first forging magnesium alloy material in which the particle size of the crystallized product made of Mg-Al intermetallic compound is in the range of 1 to 10 μm;
The first forging magnesium alloy material obtained in the above step is preliminarily processed at a temperature in the range of 250 to 450 ° C. and a processing rate in the range of 20 to 70%. Forming the material;
And a second forging method for forging the magnesium alloy material for forging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008281264A JP5356777B2 (en) | 2008-10-31 | 2008-10-31 | Magnesium alloy forging method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008281264A JP5356777B2 (en) | 2008-10-31 | 2008-10-31 | Magnesium alloy forging method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2010106336A true JP2010106336A (en) | 2010-05-13 |
| JP5356777B2 JP5356777B2 (en) | 2013-12-04 |
Family
ID=42296072
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2008281264A Active JP5356777B2 (en) | 2008-10-31 | 2008-10-31 | Magnesium alloy forging method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP5356777B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010106335A (en) * | 2008-10-31 | 2010-05-13 | Miyamoto Kogyo Kk | Magnesium alloy for forging |
| JP2011099136A (en) * | 2009-11-04 | 2011-05-19 | Ahresty Corp | Heat-resistant magnesium alloy and method for manufacturing alloy casting |
| CN103290289A (en) * | 2013-04-03 | 2013-09-11 | 常州华晨铸造有限公司 | Magnesium alloy and preparation method thereof |
| JP2017078184A (en) * | 2015-10-19 | 2017-04-27 | 権田金属工業株式会社 | Magnesium alloy manufacturing method, magnesium alloy casting material, magnesium alloy rolled material and magnesium alloy molded body |
| JP2019104961A (en) * | 2017-12-12 | 2019-06-27 | 富士通株式会社 | Magnesium alloy, production method thereof and electronic apparatus |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109207824A (en) * | 2017-06-29 | 2019-01-15 | 比亚迪股份有限公司 | A kind of magnesium alloy and preparation method thereof and mobile phone |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003239033A (en) * | 2001-12-14 | 2003-08-27 | Matsushita Electric Ind Co Ltd | Magnesium alloy cast and its casting method |
| WO2006003833A1 (en) * | 2004-06-30 | 2006-01-12 | Sumitomo Electric Industries, Ltd. | Method for producing magnesium alloy product |
| WO2006003899A1 (en) * | 2004-06-30 | 2006-01-12 | Sumitomo Electric Industries, Ltd. | Method for producing magnesium alloy product |
| JP2006263745A (en) * | 2005-03-22 | 2006-10-05 | Sumitomo Electric Ind Ltd | Method for manufacturing long-length magnesium material |
-
2008
- 2008-10-31 JP JP2008281264A patent/JP5356777B2/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003239033A (en) * | 2001-12-14 | 2003-08-27 | Matsushita Electric Ind Co Ltd | Magnesium alloy cast and its casting method |
| WO2006003833A1 (en) * | 2004-06-30 | 2006-01-12 | Sumitomo Electric Industries, Ltd. | Method for producing magnesium alloy product |
| WO2006003899A1 (en) * | 2004-06-30 | 2006-01-12 | Sumitomo Electric Industries, Ltd. | Method for producing magnesium alloy product |
| JP2006263745A (en) * | 2005-03-22 | 2006-10-05 | Sumitomo Electric Ind Ltd | Method for manufacturing long-length magnesium material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010106335A (en) * | 2008-10-31 | 2010-05-13 | Miyamoto Kogyo Kk | Magnesium alloy for forging |
| JP2011099136A (en) * | 2009-11-04 | 2011-05-19 | Ahresty Corp | Heat-resistant magnesium alloy and method for manufacturing alloy casting |
| CN103290289A (en) * | 2013-04-03 | 2013-09-11 | 常州华晨铸造有限公司 | Magnesium alloy and preparation method thereof |
| JP2017078184A (en) * | 2015-10-19 | 2017-04-27 | 権田金属工業株式会社 | Magnesium alloy manufacturing method, magnesium alloy casting material, magnesium alloy rolled material and magnesium alloy molded body |
| JP2019104961A (en) * | 2017-12-12 | 2019-06-27 | 富士通株式会社 | Magnesium alloy, production method thereof and electronic apparatus |
| JP7078839B2 (en) | 2017-12-12 | 2022-06-01 | 富士通株式会社 | Magnesium alloy, its manufacturing method, and electronic equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| JP5356777B2 (en) | 2013-12-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10612116B2 (en) | Increasing strength of an aluminum alloy | |
| CN109072356B (en) | Die casting alloy | |
| EP2369025B1 (en) | Magnesium alloy and magnesium alloy casting | |
| JP3861720B2 (en) | Forming method of magnesium alloy | |
| JP5703881B2 (en) | High strength magnesium alloy and method for producing the same | |
| JP2011208253A (en) | Aluminum die-cast alloy for vehicle material | |
| JP2010018875A (en) | High strength aluminum alloy, method for producing high strength aluminum alloy casting, and method for producing high strength aluminum alloy member | |
| RU2673593C1 (en) | High-strength aluminium-based alloy | |
| JP5356777B2 (en) | Magnesium alloy forging method | |
| JP6229130B2 (en) | Cast aluminum alloy and casting using the same | |
| CN101285144A (en) | Magnesium alloy for semi-solid forming and preparation method of semi- solid blank | |
| JP5215710B2 (en) | Magnesium alloy with excellent creep characteristics at high temperature and method for producing the same | |
| JP4433916B2 (en) | Magnesium alloy and magnesium alloy member for plastic working | |
| JP2004162090A (en) | Heat resistant magnesium alloy | |
| JP2009203516A (en) | Aluminum alloy | |
| JP2008075176A (en) | Magnesium alloy excellent in strength and elongation at elevated temperature and its manufacturing method | |
| JP5575028B2 (en) | High strength aluminum alloy, high strength aluminum alloy casting manufacturing method and high strength aluminum alloy member manufacturing method | |
| JP5415739B2 (en) | Magnesium alloy for forging | |
| JP6569453B2 (en) | High toughness aluminum alloy casting and manufacturing method thereof | |
| JP2015137388A (en) | Aluminum alloy casting and manufacturing method therefor | |
| JPH11246925A (en) | Aluminum alloy casting with high toughness, and its manufacture | |
| JP2006161103A (en) | Aluminum alloy member and manufacturing method therefor | |
| JP5590413B2 (en) | High thermal conductivity magnesium alloy | |
| Liping et al. | Grain coarsening in semi-solid state and tensile mechanical properties of thixoformed AZ91D-RE | |
| JP5449754B2 (en) | Forging piston for engine or compressor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20111027 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20130507 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20130708 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20130730 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20130829 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 5356777 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |