CN1018039B - 制造金属能量转换装置的设备 - Google Patents
制造金属能量转换装置的设备Info
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- CN1018039B CN1018039B CN88107328A CN88107328A CN1018039B CN 1018039 B CN1018039 B CN 1018039B CN 88107328 A CN88107328 A CN 88107328A CN 88107328 A CN88107328 A CN 88107328A CN 1018039 B CN1018039 B CN 1018039B
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- 238000006243 chemical reaction Methods 0.000 title claims description 14
- 229910052783 alkali metal Inorganic materials 0.000 title claims description 10
- 150000001340 alkali metals Chemical class 0.000 title claims description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 75
- 239000002184 metal Substances 0.000 claims abstract description 75
- 230000007246 mechanism Effects 0.000 claims description 26
- 239000003792 electrolyte Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 10
- 238000011068 loading method Methods 0.000 claims description 7
- 239000007784 solid electrolyte Substances 0.000 claims description 7
- 238000010292 electrical insulation Methods 0.000 claims description 6
- 229910001090 inconels X-750 Inorganic materials 0.000 claims description 2
- 229910001235 nimonic Inorganic materials 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 19
- 239000000919 ceramic Substances 0.000 abstract description 6
- 238000007789 sealing Methods 0.000 abstract description 5
- BNOODXBBXFZASF-UHFFFAOYSA-N [Na].[S] Chemical compound [Na].[S] BNOODXBBXFZASF-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000034 method Methods 0.000 description 15
- 238000007731 hot pressing Methods 0.000 description 8
- 239000000565 sealant Substances 0.000 description 6
- -1 aluminium silicon magnesium-manganese Chemical compound 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910000861 Mg alloy Inorganic materials 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910000975 Carbon steel Inorganic materials 0.000 description 3
- 229910000914 Mn alloy Inorganic materials 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000010962 carbon steel Substances 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- CXOWYMLTGOFURZ-UHFFFAOYSA-N azanylidynechromium Chemical compound [Cr]#N CXOWYMLTGOFURZ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
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- 230000014759 maintenance of location Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000616 Ferromanganese Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 229910000720 Silicomanganese Inorganic materials 0.000 description 1
- JRBRVDCKNXZZGH-UHFFFAOYSA-N alumane;copper Chemical compound [AlH3].[Cu] JRBRVDCKNXZZGH-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008393 encapsulating agent Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910001055 inconels 600 Inorganic materials 0.000 description 1
- 229910001098 inconels 690 Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
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Abstract
以前一直用气动压头在炉内将金属密封零件与钠硫电池的α氧化铝陶瓷盖热压连接在一起。本发明提出了一种采用盘簧的弹簧加载夹具,该夹具包括一对固定在可分离的两部分上的卡口,要封接的零件首先放入夹具中压在一起,然后放入炉内进行热压连接。
Description
本发明涉及碱金属能量转换装置,例如碱金属电池特别是钠硫电池(这种电池通常用一种固体电解质零件将在电池工作温度下呈液体状态的阴极和阳极反应剂隔开来)的制造设备。
通常,这种装置包括:一个外壳、一个将外壳之内部分开成为两个极区的固体电解质零件、一个同电解质零件相连接的电绝缘零件和至少一个封接到绝缘零件上的金属零件。这种结构一般组成电池装置密封结构之一部分,它既使两个电极区彼此隔开,又使电极区与外部环境隔开。例如,这种装置的外壳可以是金属的,所以电极区的任一种密封都要求在外壳金属与电解质零件间有一密封层,但是,外壳金属同电解质零件之间必须是电绝缘的,因此用插入电绝缘零件的办法来保持它们间的绝缘。
专利GB-A-2102622公开了应用于钠硫电池中的这种结构的实例。这种电池带有一个α氧化铝盖盖住了管式电解质零件。中心的集流器装在穿通α氧化铝盖的一个孔中,并由盖子使它与电解质零件隔开来。位于电解质零件外面的外电极区通过一个外表面焊到电池金属外壳上、内表面封接到α氧化铝盖上的闭合金属零件进行密封。金属闭合零件与α氧化铝盖间的这层密封层有时是通过在金属闭合零件与陶瓷盖间加一层软材料(例如铝)热压连接而成的。
这种连接是在绝缘零件即α氧化铝陶瓷同电解质零件连接后进行的,因为这种连接易受高温釉化的影响,釉化会毁坏在金属闭合零件
与陶瓷盖之间放入中间层进行热压连接制成的隔离层。
另一方面,专利EP-A-0166605公开了一种把金属零件直接热压连接到绝缘陶瓷盖上以形成两者间的密封层的技术,这种密封层不受随后的温度循环的不良影响,例如不受绝缘零件随后用釉化法与电解质零件连接时所需的高温的影响。在绝缘零件连接到电解质零件之前就能够使金属零件与绝缘零件间形成这样一种密封层的技术,大大简化了这种封闭层的制造工艺。所以,可以同时将多个金属零件与绝缘零件彼此密封起来制成多个密封对。
显然,钠硫电池和其他碱金属能量转换装置的密封对于制造性能良好而又安全可靠的电池来说是十分重要的,而且由于这些电池的工作温度高(一般350℃),故这个问题极难解决。而采用粘接剂的连接技术的可行性至今尚未证实。
绝缘陶瓷零件一般用α氧化铝制成,并且其强度足以经受住热压连接时对它所加的相当大的压力。但是,电解质零件一般用β氧化铝制成,这种材料比较脆,而且,在用热压工艺与固定到它上面的绝缘零件相连接的过程中容易损坏,因此,迄今用来将一个或几个金属闭合零件固定到绝缘零件上的连接技术不得不取决于绝缘零件是本身连接到固体电解质零件上,还是像闭合金属零件和陶瓷盖之间放有一层中间层那样进行连接。而且这种绝缘零件和电解质零件的组合件的形状要求必须一个电池接一个电池的单独将金属零件与绝缘零件连接在一起。
现用的连接技术一般是靠置于处理炉内的气动压机的压头来施加必要的连接压力的。在这种机构中,要连接在一起的零件必须先装入热处理炉内,再使热处理炉内的温度升高到500~600℃,然后
用压头在很短的时间内对其施加一个足以使零件按照要求连接在一起的压力。
采用气动压头来加压,有一定的弊病,例如,热处理炉就不能只是一个简单的炉子,而是必须设计成不仅能固定气动压头而且还必须有足够的强度以承受压头所加的压力的结构。
另外,在为了处理大批零件而将这种众所周知的机构按比例加大时也会遇到一些问题。当按照一个电池接一个电池排在一起进行连接时,必须要用许多的压头,但是,为保证这许多压头与各自的电池有精确的直线排列并对其进行控制,就使得这类机构变得相当复杂而且成本高。
此外,用这类机构进行处理时,还会碰到一些类似的缺点。
根据本发明提出了一种制造碱金属能量转换装置的设备,所制成的碱金属能量转换装置含有一个外壳、一个将外壳之内部分开成为两个电极区的固态电解质零件、一个连接到电解质零件上的电绝缘零件、以及至少一个封接到绝缘零件上的金属零件,该制造设备包括:用来按预定的排列方式定位绝缘零件和金属零件的机构和固定到定位机构上用来施加压力将金属零件压到绝缘零件上的机构。
因此,完全解决了采用气动压头所带来的问题,只要用一个简单的炉子作为对能量转换装置进行热处理的处理室。另外,将许多根据本发明的设备放入或穿过热处理炉就能迅速地对大量的能量转换装置进行处理。必须明白,这里所用的“金属零件”一词不仅是其表面焊到电池的金属外壳上以隔离外电极区的外金属零件,而且也指装在α氧化铝盖的小孔内的、密封集流器四周的内金属零件。
用来施加压力的装置最好直接对金属零件施加所述的压力,而且
用来定位的机构最好包括与绝缘零件之一部分相接触的凸缘,并完全承受加压装置对所述绝缘零件所加的载荷。
因此,显著地减少了在连接过程中损坏较脆的β氧化铝电解质零件的可能性。
用来定位的机构最好包括互相配合的且可离的第一和第二部分,其中一个部分带有用来对其施加连接力的机构。在这种结构中,第一个可分离的部分可以带有用来对其施加连接力的机构,而第二个可分离的部分又可以由两部分组成,其中第一部分包括上述凸缘,而第二部分则可绕第一部分转动并与第一个可分离的部分相配合。在该结构的两个可分离部分之间采用卡口固紧的机构特别有利,因为,当第二部分按照紧固卡口锁紧连接方向移动时,可以防止在锁紧和松开时加到陶瓷和密封组件上的扭矩。
下面结合附图阐述制造碱金属能量转换装置的设备。其中,图1为按照本发明的一种设备的横剖面图。图2a和2b为按照本发明的另一种设备的横剖面图。
现参见图1,从图中可以看出,第一部分1与第二部分5是相配合的。这两部分1和5是可以分离的,并且分别带有一个紧固卡口的阴、阳部分。三个定位止动器(图中4示出了其中的一个)成120°
坐落在第一部分1的外圆柱表面上,并且被固定到第二部分5中的沟槽里。用来加力的机构包括串联在中心杆2中的一组八个高温环状盘簧7,它们的材料为Nimonic90、Nimonic80A或Inconel x-750;此外,还包括一个加载零件3。这种用来加力的机构被固定到第一部分上,并且用来对碱金属能量转换装置的外金属零件8施加压力。这种金属零件基本上是环形的,并且与一环形金属衬垫零件9相接触,衬垫零件9的横截面形状实际上是可变的,并且被置于金属零件8和用上釉法连接到固体电解质零件13(图中只示出它的一部分)上的电绝缘零件10之间。电解质零件13是管状的。金属零件8中心处有一个孔,一个柱形定位销6穿过该孔固定到中心杆2上。通常,绝缘零件10是一个盘形α氧化铝陶瓷的盖子。
下面阐述图2a和2b,图中对应于图1中已经阐述过的零件标以同样的号码。这一实施例与图1实施例的不同点如下:它使用了六个高温环形盘簧,每个都比图1实施例中的一个盘簧厚。这种结构提高了弹簧的加载力及寿命。串连套入盘簧的中心杆2和加载零件3是整体的。在第一部分的封闭端面上有一个孔,中心杆就插在这个孔中,使加载零件3和弹簧7可从非加压位置(一般为图2a中的12)上移动到加压位置(一般为图2b中的11)上。加载零件3的外形有利于通过其凸缘22与金属零件8的凸缘23相配合的方法使金属零件8在绝缘零件10中正确定位。另一个不同是,第二部分5又包括两个部分,即带有一个凸缘14(绝缘零件10的凸缘15被压入14中)的第一部分21和通过定位止动器4与第一部分1相配合的第二部分20。第二部分20通过一个隔离环与第一部分21相配合,它可使第二部分20能够绕第一部分21转动。这种结构特别合
乎需要,因为在将金属零件8固定到绝缘零件10的过程中,也就是当锁紧和松开第一和第二部分时,它能够防止陶瓷或密封材料产生不希望的扭曲。
除了金属零件8和金属衬垫零件9外,图中还示出了另一个内金属零件18及其相应的内金属衬垫零件16。内金属零件18用来密封在后阶段由α氧化铝绝缘零件10中的孔插入的集流器(图中未示出)周围。金属零件8的形状可做成有利于衬垫零件9相对于零件8的正确定位,在成形时就在金属零件8上制出带有隆起的部位17。
下面参考图1所示的上述本发明的一种实施例说明制造本发明的一种碱金属能量转换装置的方法。
将已用上釉法连接到固体电解质零件13上的电绝缘件10加载压入第二部分5中。
环形凸缘15从绝缘零件10的外周延长出去并与第二部分的内延凸缘14相接触。将金属零件18和中间金属衬垫零件9相互自由地贴在一起,再将衬垫零件自由地放到绝缘零件10上,随后将第一部分1降落到第二部分上,定位销6应插入绝缘零件10的中心孔中。然后用力将这两部分压在一起,压缩盘簧组7,加载零件3则将中心杆2从非压缩位置(图中标以12处)上滑到压缩位置(图中标以11处)上。而后将定位止动器(图中示出了其中之一:4)卡入与其相配合的槽中,使第一部分固定到第二部分上,因此,绝缘零件10、金属零件8和金属衬垫零件9则按预定的排列直接定位在一起,此时,加载弹簧7通过加载零件3将金属零件压向绝缘零件。
内金属零件18可以与金属零件8同时进行连接。在某种情况下,金属零件8和18单独连接可能更方便些。
将该装置放入热处理炉中,使炉中的温度升至峰值,保温后再降温。在高温和压力的综合作用下,使金属零件8的内圆柱表面上的或内圆柱表面附近上的一狭窄环形区通过中间的衬垫零件9与绝缘零件10热压在一起。
许多不同的材料组合都可获得满意的连接性能,现详细说明于下:
金属零件 金属衬垫零件
带二铬碳化物表面层的0.2%碳钢 铝硅镁锰合金
带二铬氮化物表面层的0.2%碳钢 铝硅镁锰合金
化学纯铝 铝硅镁锰合金
下列材料也可满意地用作金属零件和金属衬垫零件:
铝锰铁硅合金
铝锰镁铬合金
铝锰镁合金
铝铜合金
铝-5.0%镁合金
铝-3.0%镁合金
显然,这些材料也适合于内金属零件和内金属衬垫零件,有关金属零件和金属衬垫零件的性能标准也可扩大到内金属零件和内金属衬垫零件。
此外,下列材料适用于金属零件:
镀铬钢
镀铜钢
镀铝钢
镍基高温合金,例如Inconel 600、Inconel 690和Haynes188。
正确选择材料的目的是为了获得一种耐腐蚀的密封层。可以肯定,金属衬垫零件9的材料熔点应稍低于金属零件8的熔点,这样,在进行连接时金属零件的材料就不会发生任何熔融。
另外,金属衬垫零件9的形状最好做成在受压而后加热时能发生实质性的变形,例如,它可做成以锥形可变形部分与绝缘零件10和/或金属零件8相接触的形状。
因此,在热压连接过程中基本上不会产生任何表面氧化层,从而有利于连接。典型的横截面可以是三角形或菱形。
还应该清楚,必须小心控制连接温度和压力曲线。对于采用铝硅锰镁合金连接带二铬碳化物或二铬氮化物表面层的0.2%碳钢,下列条件可获得满意的连接:
连接温度:
在高达540℃~600℃的峰值温度下进行热处理;在峰值温度下保温2小时;在1小时内冷却到160℃以下,然后空淬。
在峰值温度下的保温时间稍短一些但冷却时间长一些也可获得满意的效果。
压力:
对于三角形截面、直径为20毫米的环形金属衬垫零件,加载为20~40Kg。
显然,对于温度高于600℃,保温为2小时的条件,加载值可以降低,而对于温度低于540℃时,保温时间和/或加载值可以增
加。
另外,热压连接环境可以是约为5×10-4~1×10-2毫巴的低真空,也可换用例如氩气等惰性气体环境或用氩中含5%氢的低还原气氛。也可采用完全还原的气氛。
在进行热压连接使金属零件8与绝缘零件10牢固地粘在一起后,即从该设备上卸下由此法成形的能量转换装置的分组件,以便将该装置的外壳(图中未示出)焊到金属零件上。通常,只对外壳一端的周边进行焊接。
进一步改进本发明的设备还可方便地用来使许多成对的绝缘零件和金属零件按预定的排列方式排放在一起形成该零件对的层叠组件。然而,这种改进对于内金属零件的连接特别适用,因为这些零件可以在将电解质零件连结到支撑绝缘零件之前与各自的绝缘零件连接在一起。因此,层叠组件可以包括许多对内金属零件和绝缘零件。
Claims (13)
1、一种制造碱金属能量转换装置的设备,所制成的能量转换装置有一个外壳、一个将该外壳的内部分开成为两个电极区的固体电解质零件,一个与电解质零件相连接的电绝缘零件和至少一个封接到绝缘零件上的金属零件,其特征在于它包括一个用来按预定排列定位绝缘零件和金属零件的机构,一个固定到定位机构上并用来施加压力将金属零件压到绝缘零件上的机构。
2、根据权利要求1的设备,其特征在于,用来加力的机构可以对金属零件直接施加所述的压力。
3、根据权利要求1或2中之一项的设备,其特征在于,用来定位的机构包括一个与绝缘零件的一部分相接触、并完全承受加力机构对上述绝缘零件所加的载荷的凸缘。
4、根据权利要求3的设备,其特征在于,用来定位的机构包括第一个和第二个互相配合的、可分离的部分,其中一个带有用来施加连接力的机构。
5、根据权利要求4的设备,其特征在于,第一个可分离的部分带有一个用来施加连接力的机构,而第二个可分离的部分又包括两个部分,其第一部分包括上述与绝缘零件的一部分相接触的凸缘,其第二部分可以与第一部分作相对运动并用来与第一个可分离的部分相配合。
6、根据权利要求5的设备,其特征在于,每一部分分别包括紧固卡口的阴、阳部分,而第二个可分离部分的第二部分可按紧固卡口的锁紧和松开方向绕上述第一部分旋转。
7、根据权利要求1的设备,其特征在于,用来加力的机构包括一组高温盘簧。
8、根据权利要求7的设备,其特征在于,盘簧的材料是Nimonic90、Nimonic 80A或Inconel x-750。
9、根据权利要求3的设备,其特征在于,凸缘是带有一个内孔大小能放入电解质零件的环形件。
10、根据权利要求1的设备,其特征在于,绝缘零件上有一个圆形中心孔,用来定位的机构还包括一个穿过上述中心孔的圆形定位销。
11、根据权利要求10的设备,其特征在于,金属零件用定位销定位到绝缘零件和第一个可分离部分的内壁上的预定位置上。
12、根据权利要求10的设备,其特征在于,金属零件用定位销定位在绝缘零件的预定位置上,加载零件用来传递来自弹簧的压力,该加载零件是与金属零件同时成形出来的。
13、根据权利要求1的设备,其特征在于,包括用来按预定排列将许多对绝缘零件和金属零件固定成上述零件对的层叠组件的机构。
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CA2180882A1 (en) | 1996-07-10 | 1998-01-11 | Vic De Zen | Substructure for composite products and products formed therewith |
KR100957075B1 (ko) * | 2006-02-23 | 2010-05-13 | 주식회사 엘지화학 | 전극 고정용 부재가 장착되어 있는 전극조립체 및 이를포함하고 있는 이차전지 |
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CN103123987B (zh) * | 2012-12-12 | 2015-01-14 | 上海电气钠硫储能技术有限公司 | 一种钠硫电池储钠管 |
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CN105489822A (zh) * | 2016-01-05 | 2016-04-13 | 江苏正昀新能源技术股份有限公司 | 一种新型锂电池模组的连接固定结构 |
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US3971875A (en) * | 1974-01-04 | 1976-07-27 | General Dynamics Corporation | Apparatus and method for vacuum hot press joining, compacting and treating of materials |
US3941297A (en) * | 1975-06-02 | 1976-03-02 | Western Electric Company, Inc. | Method and apparatus for simultaneously bonding a plurality of lead frames to a plurality of planar articles |
FR2333358A1 (fr) * | 1975-11-28 | 1977-06-24 | Comp Generale Electricite | Generateur electrochimique du type soufre-sodium |
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US4315591A (en) * | 1979-03-08 | 1982-02-16 | General Electric Company | Method for thermo-compression diffusion bonding a structured copper strain buffer to each side of a substrateless semiconductor device wafer |
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JPS5916282A (ja) * | 1982-07-19 | 1984-01-27 | Yuasa Battery Co Ltd | ナトリウム−硫黄電池の製造法 |
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KR890702274A (ko) | 1989-12-23 |
GB2230378A (en) | 1990-10-17 |
DE3850674T2 (de) | 1994-11-03 |
WO1989004069A1 (en) | 1989-05-05 |
JPH03501664A (ja) | 1991-04-11 |
GB9009112D0 (en) | 1990-07-18 |
EP0408552A1 (en) | 1991-01-23 |
ZA887879B (en) | 1989-07-26 |
GB2230378B (en) | 1991-03-27 |
EP0408552B1 (en) | 1994-07-13 |
US5075957A (en) | 1991-12-31 |
DE3850674D1 (de) | 1994-08-18 |
GB8724817D0 (en) | 1987-11-25 |
CN1034453A (zh) | 1989-08-02 |
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