CN107735877B - 制造二次电池的方法 - Google Patents
制造二次电池的方法 Download PDFInfo
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- CN107735877B CN107735877B CN201680037148.XA CN201680037148A CN107735877B CN 107735877 B CN107735877 B CN 107735877B CN 201680037148 A CN201680037148 A CN 201680037148A CN 107735877 B CN107735877 B CN 107735877B
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Abstract
本发明提供一种用于制造二次电池的方法,二次电池具有充电层,充电层因通过在被绝缘材料覆盖的n型金属氧化物半导体上引起光激结构变化而在带隙中形成能级来捕获电子,该方法包括:涂布工序(S1),涂布涂层液,以形成包括将成为充电层(18)的成分的涂层膜;干燥工序(S2),通过干燥在涂布工序(S1)中涂布的涂层液来形成干燥涂层膜;UV照射工序(S3),通过用紫外线照射经由干燥工序(S2)获得的干燥涂层膜来形成UV照射涂层膜;以及煅烧工序(S5),在通过重复包括涂布工序(S1)、干燥工序(S2)和照射工序(S3)的组多次,形成多个UV照射涂层膜之后,煅烧所述多个UV照射涂层膜。
Description
技术领域
本发明涉及一种制造二次电池的方法。
背景技术
本申请的申请人研发了这样一种电池(以下称为量子电池)(专利文件1),其利用金属氧化物半导体在紫外线照射下的光激结构变化。专利文件1中公开的二次电池因是全固态类型而在充放电过程中不会引起任何化学反应,所以是安全的,并且被认为是在输出密度和功率密度方面优于锂离子电池的技术。专利文件1中的二次电池具有包括层叠在衬底上的第一电极、n型金属氧化物半导体层、充电层、p型半导体层和第二电极的结构。
在专利文件1中,利用涂布热分解法形成充电层。具体地,通过按顺序执行涂布工序、干燥工序、煅烧工序和紫外线照射工序来形成充电层。
引文清单
专利文献
专利文件1:国际专利公开号WO2012/046325
发明内容
技术问题
对于这样的电池,认为可以通过增大充电层的体积来增加充电容量。因此,期望增大充电层的厚度。然而,当充电层变厚时,就难以均匀地形成充电层。当充电层未被均匀地形成时,恐怕不能获得足够的电池性能。此外,为了提高生产率,希望缩短各工序的处理时间并减少工序的数量。
鉴于上述问题,本发明的目的是提供一种用于制造二次电池的方法,其能够高生产率地制造高性能二次电池。
技术手段
根据本发明的方面,提供了一种用于制造二次电池的方法,该二次电池具有充电层,充电层因通过在被绝缘材料覆盖的n型金属氧化物半导体上引起光激结构变化而在带隙中形成能级来捕获电子,该方法包括以下工序:涂布涂层液,以形成包括将成为充电层的成分的涂层膜;进行干燥,以通过干燥在涂布工序中涂布的涂层液来形成干燥涂层膜;进行照射,以通过用紫外线照射干燥涂层膜来形成UV照射涂层膜;以及进行煅烧,以在通过重复涂布工序、干燥工序和照射工序多次,形成多个UV照射涂层膜之后,通过煅烧所述多个UV照射涂层膜来形成多个煅烧涂层膜。因此,可以高生产率地制造高性能二次电池。
在上述制造方法中,充电层可以是在同时形成所述多个UV照射涂层膜而不是煅烧所述多个UV照射涂层膜中的每一个的情况下形成。因此,可以缩短制造时间和设备使用时间,并且还可以提高生产率。
在上述制造方法中,煅烧工序中的煅烧温度可以比干燥工序中的干燥温度高。因此,不需要将干燥工序中的温度提高到对电池性能产生影响的程度,从而可以保持高的电池性能。
在上述制造方法中,可以通过用紫外线照射多个煅烧涂层膜来形成充电层。因此,可以形成能够充入能量的充电层。
发明的有益效果
根据本发明,可以提供一种能够以高生产率制造高性能二次电池的制造二次电池的方法。
附图说明
图1是示出本发明的量子电池10的横截面结构的视图;
图2是详细示出图1中的充电层18的结构的视图;
图3是示出用于制造充电层18的方法的工序的流程图;以及
图4是示出特定煅烧时间的示例的表格。
具体实施方式
下文中,将参照附图说明本发明的实施例的示例。下面的描述仅仅是本发明的优选实施例,不旨在将本发明的范围限制为以下实施例。
本发明涉及一种基于在充电层处采用光激结构变化技术的新充电原理来制造电池(下文中,在本说明书中被称为量子电池)的方法。量子电池是能够进行充电放电的二次电池。
光激结构变化是通过用光照射激发来改变材料的原子间距离的现象。作为非晶金属氧化物(诸如氧化锡)的n型金属氧化物半导体具有引起光激结构变化的特性。根据光激结构变化现象,在n型金属氧化物半导体的带隙中形成新的能级。
(电池的结构)
图1是示出本发明的量子电池的横截面结构的视图。在图1中,量子电池10具有层叠结构,其中第一导电电极14、n型金属氧化物半导体层16、充入能量的充电层18、p型金属氧化物半导体层20和第二电极22以该顺序层叠在衬底12上。
衬底12可以由绝缘材料或导电材料制成。例如,能够使用玻璃衬底、聚合物膜的树脂片、金属箔片等作为衬底12的材料。
第一电极14和第二电极22仅仅需要在其上具有导电层。例如,可以使用诸如钛(Ti)的金属电极作为第一电极。此外,诸如铬(Cr)和铜(Cu)的金属电极可以用作第二电极。另一种金属电极的示例包括含铝(Al)的银(Ag)合金膜。用于形成上述的方法的示例包括气相成膜,诸如溅射、离子电镀、电子束沉积、真空沉积和化学沉积。此外,可以通过电解电镀工艺、非电解电镀工艺等形成金属电极。通常地,可以使用铜、铜合金、镍、铝、银、金、锌、锡等作为要用于电镀的金属。
可以使用二氧化钛(TiO2)、氧化锡(SnO2)、氧化锌(ZnO)等作为n型金属氧化物半导体层16的材料。
可以使用颗粒状的n型金属氧化物半导体作为充电层18的材料。通过利用紫外线照射的光激结构变化,n型金属氧化物半导体被形成为具有充电功能的层。n型金属氧化物半导体被硅树脂绝缘涂层覆盖。优选地,使用二氧化钛、氧化锡或氧化锌作为可用于充电层18的n型金属氧化物半导体的材料。可以使用二氧化钛、氧化锡和氧化锌中的任意两种或三种结合在一起的材料。
此外,在本实施例中,充电层18由多个涂层膜18a至18c形成。即,充电层18具有多个涂层膜18a至18c的层叠结构。本文中,以由三层涂层膜18a至18c形成的充电层18为例。也可以具有层叠2层、4层或更多层的涂层膜的层叠结构。
充电层18上的p型金属氧化物半导体层20被形成为防止电子从布置在上方的第二电极22注入到充电层18。可以使用氧化镍(NiO)、铜铝氧化物(CuAlO2)等作为p型金属氧化物半导体层20的材料。
在本实施例中,衬底12上的多层可以以相反的顺序层叠。即,也可以具有其中第一电极14布置在最上层并且第二电极22布置在最下层的层叠结构。下面将描述实际制备的原型。
(原型示例)
衬底12由玻璃形成。在玻璃衬底12上,形成钛导电膜作为第一电极14,并且另外,利用溅射使用二氧化钛(TiO2)在第一电极14上形成n型金属氧化物半导体层16。利用溅射由氧化镍形成p型金属氧化物半导体层20,并且第二电极22由铬导电膜形成。
(充电层18的结构)
由于通过在被绝缘材料覆盖的n型金属氧化物半导体上引起光激结构变化而在带隙中形成能级,充电层18捕获电子。以下将详细描述充电层18的结构。
图2是详细示出图1中的充电层18的结构的视图。充电层18具有以下结构,其中填充有由硅树脂覆盖的二氧化钛,同时使用硅树脂作为绝缘膜28并且使用二氧化钛作为n型金属氧化物半导体26。由于用紫外线照射到二氧化钛引起的光激结构变化,所以充电层18具有储存能量的功能。
使用二氧化钛、氧化锡或氧化锌作为将在充电层18中使用的n型金属氧化物半导体26的材料,并且通过在制造过程中分解金属脂肪酸盐而产生上述二氧化钛、氧化锡或氧化锌。因此,作为金属脂肪酸盐,使用金属脂肪酸盐,当通过在氧化气氛下利用紫外线照射而分解该金属脂肪酸盐或通过煅烧而耗干该金属脂肪酸盐时,该金属脂肪酸盐可以变成金属氧化物。例如,可以使用诸如脂肪族一元羧酸、脂肪族二元羧酸、脂肪族三元羧酸和脂肪族四元羧酸的脂肪族多元羧酸作为脂肪酸。
更具体地说,饱和脂肪族一元羧酸包括甲酸、乙酸、丙酸、己酸、庚酸、辛酸、壬酸、癸酸、硬脂酸等。作为不饱和脂肪族一元羧酸,可以使用诸如丙烯酸、丁酸(butane acid)、巴豆酸、异巴豆酸、亚麻酸和油酸的高度不饱和一元羧酸。
此外,脂肪酸盐受热易于分解或烧掉,具有高溶剂溶解度,在被分解或煅烧后提供精确的膜,易于处理且价格便宜,并且易于与金属合成盐。由于这些原因,由脂族酸和金属形成的盐是优选的。
在绝缘膜28中,除了硅树脂以外,还可以采用诸如矿物油、氧化镁(MgO)、二氧化硅(SiO2)的无机绝缘材料。作为绝缘树脂,可以使用诸如聚乙烯、聚丙烯、聚苯乙烯、聚丁二烯、聚氯乙烯、聚甲基丙烯酸甲酯、聚酰胺、聚碳酸酯、聚酰亚胺、乙酰纤维素的热塑性树脂,或者可以使用诸如酚醛树脂、氨基树脂、不饱和聚酯树脂、烯丙树脂、醇酸树脂、环氧树脂和聚氨酯的热固树脂。
(充电层18的制造方法)
图3是示出用于制造充电层18的方法的工序的流程图。
首先,通过在衬底12上形成第一电极14和n型金属氧化物半导体层16来制备衬底。如上所述,可以利用溅射等来形成第一电极14和n型金属氧化物半导体层16。接续,在n型金属氧化物半导体层16上涂布涂层液(涂布工序S1)。即,涂布涂层液以形成包括要成为充电层18的成分的涂层膜18a。具体而言,通过将脂肪酸钛和硅油混合到溶剂中并搅拌在一起来制备涂层液。涂层液仅仅需要包含成为充电层的成分。接续,在旋转制备好的衬底的同时,用旋涂器(spinner)将涂层液旋涂在二氧化钛层上。随着衬底的旋转,形成厚度为0.3~1μm的薄层(涂层膜18a)。该层没有空隙,被认为具有由硅树脂覆盖的二氧化钛的金属盐被嵌入到硅层中的特定结构。本文中,不限于旋涂,可以通过浸涂、模涂、狭缝涂布、凹版涂布、喷涂、幕涂等在n型金属氧化物半导体层16上形成涂层膜。此外,也可以在涂布工序之前用紫外线照射等对n型金属氧化物半导体层16进行表面处理。
在涂布工序S1之后,干燥涂布在衬底12上的涂层液(干燥工序S2)。由于在干燥工序S2中将涂层液干燥,所以涂层液中的溶剂被汽化,从而流体涂层液变为暂时固化的涂层膜18a。因此,可以容易地处理衬底12。例如,将衬底12放置在热板上,并在预定温度下加热预定时间,以使涂层液中的溶剂汽化。为了便于操作,仅仅需要在能够暂时固化涂层膜18a的温度和时间下执行干燥工序S2。不限于热板,干燥方法可以采用利用远红外线的加热干燥、利用真空处理的减压干燥或利用热风循环的干燥。执行干燥工序S2以干燥并汽化溶剂。因此,干燥温度优选为200℃或更低。在干燥工序S2之后,涂层膜18a是干燥的但不是完全固化的状态。将通过干燥工序S2暂时固化的状态下的涂层膜18a表示为干燥涂层膜。
将紫外线(以下称为UV光)照射在已对其执行干燥工序S2的涂层膜18a(干燥涂层膜)上(UV照射工序S3)。可以通过用UV光照射而UV硬化涂层膜18a的表面。例如,在UV照射工序S3中,用UV光照射涂层膜18a大约1至5分钟。根据上述,涂层膜18a的表面可以处于硬化状态。将在UV照射工序S3中表面被硬化的涂层膜18a表示为UV照射涂层膜。
在UV照射工序S3之后,确定是否完成了预定数目的涂层膜(UV照射涂层膜)的层叠(S4)。当预定数量的层的层叠尚未完成时(S4中的否),返回到涂布工序S1。即,当尚未形成预定数量的涂层膜时,将涂层膜层叠。本文中,作为第二层的涂层膜18b形成在作为第一层的涂层膜18a上。与上述类似,执行涂布工序S1、干燥工序S2和照射工序S3。通过重复执行多组来形成预定数目的涂层膜(UV照射涂层膜),其中每组包括涂布工序S1、干燥工序S2和UV照射工序S3。本文中,将三层涂层膜18a至18c层叠。
当预定数量的层的层叠已经完成时(S4中的是),进入接下来的煅烧工序(煅烧工序S5)。本文中,涂布工序S1、干燥工序S2和UV照射工序S3可以在相同条件或不同条件下重复。
在煅烧工序S5中,煅烧涂层膜18a~18c(UV照射涂层膜)。通过在煅烧工序S5中升高衬底12的温度,可以改变涂层膜18a~18c中的接合状态的结构。例如,将衬底12放入热处理炉中,在380~400℃下在大气中进行5~30分钟的热处理。可以通过在500℃或更低的温度下进行热处理而断开脂肪酸的分子键合。不限于在大气中进行热处理,在煅烧工序S5中的热处理可以采用真空加热、在气体气氛中加热等。煅烧工序S5中的煅烧温度比干燥工序S2中的干燥温度高。即,在煅烧工序S5中,衬底12处于比干燥工序S2中的干燥温度更高的温度。将在煅烧工序S5中煅烧的涂层膜18a~18c表示为经煅烧涂层膜。
在煅烧工序S5之后,进行到下一个工序(后续工序S6)。在后续工序S6中,例如,用紫外线照射涂层膜18a至18c(经煅烧涂层膜)。由于改变了涂层膜18a~18c(经煅烧涂层膜)的二氧化钛的原子间距离,紫外线照射引起光激结构变化现象。结果,在二氧化钛的带隙中形成新的能级。可以通过将电子捕获到新能级来执行能量充入。
例如,使用20~50mW/cm2的低压水银灯照明度,用紫外线照射2~4小时。反复进行照射,直到经煅烧涂层膜18a~18c具有由此改变的分子结构,并成为能够被充电的层。由此,形成充电层18。本文中,不限于低压水银灯,可以采用高压水银灯或氙灯作为紫外线光源。
可以在充电层18上形成p型金属氧化物半导体层20、第二电极22等。优选地,紫外光源发出波长405nm或更短的光。后续工序S6中紫外线的照射量大于UV照射工序S3的照射量。
如上所述,在形成充电层18之后,形成p型金属氧化物半导体层20和第二电极22。由此,完成量子电池10。
(效果)
根据本实施例的制造方法,通过重复执行多组来层叠预定数量的UV照射涂层膜,其中每组包括涂布工序S1、干燥工序S2和UV照射工序S3。因此,充电层18可以变厚并且其充电容量可以增加。
此外,在本实施例中,在重复层叠涂层膜的同时,在对干燥涂层膜的表面进行UV照射工序S3之后进行涂布工序S1。即,上层的涂层膜形成于在UV照射工序S3中UV硬化(干燥)的下层的UV照射涂层膜上。根据上述,当将要形成上层涂层膜时,能够抑制下层涂层膜与上层涂层膜的剥离和下层涂层膜的溶解。因此,可以抑制上下涂层膜的不均匀性。因此,可以均匀地层叠UV照射涂层膜18a~18c,并且可以制造高性能的量子电池10。
此外,由于对每层进行UV照射工序S3,所以干燥涂层膜18a至18c的表面被UV硬化。在作为UV照射工序S3的前一工序的干燥工序S2中,不需要涂层膜18a至18c的表面完全干燥。因此,不需要将干燥工序S2中的温度提高到对电池性能产生影响的程度,使得能够维持高的电池性能。此外,由于干燥温度低于煅烧温度,所以不需要将干燥工序S2中的温度升高至对电池性能产生影响的程度。因此,可以保持高的电池性能。例如,在本实施例的制造方法中,不需要将衬底12的温度反复升高至涂层膜中的接合状态发生变化的煅烧温度。因此,在本实施例的制造方法中,可以防止经煅烧涂层膜被多次加热至煅烧温度。结果是,可以防止量子电池10的电池性能恶化。
在本实施例中,在形成多个UV煅烧的涂层膜18a~18c之后,多个UV煅烧的涂层膜18a~18c一次性被煅烧。据此,可以缩短制造时间。例如,假定煅烧工序S5一次需要四个小时,并且将要层叠三层薄膜。如果在三个涂布工序S1中的每个之后均进行四小时的煅烧,则煅烧工序S5的总时间需要12小时(四小时×3)。在本实施例中,因为在进行三次涂布工序S1之后一次性执行煅烧工序S5,所以煅烧工序S5的时间变为四小时。因此,在本实施例中,煅烧时间可以缩短八小时。本文中,UV照射工序S3所需要的时间为1至5分钟,远远短于煅烧工序S5所需的时间。因此,可以制造具有高性能的量子电池10。
显然,可以多次执行煅烧工序S5。例如,在形成作为第一层和第二层的UV照射涂层膜之后执行第一煅烧工序S5,并且在形成作为第三层和第四层的UV照射涂层膜之后执行第二煅烧工序S5。同样在这种情况下,优选地,在每层执行涂布工序S1、干燥工序S2和UV照射工序S3,以形成UV照射涂层膜。
图4是示出特定煅烧时间的示例的表格。图4分别示出在每个涂布工序S1之后执行煅烧的制造方法1和在执行多次涂布之后一次性执行煅烧的制造方法2的煅烧时间。
在形成两层涂层膜的情况下,在每个涂布工序S1之后进行煅烧的制造方法1需要8.5小时的总煅烧时间。另一方面,在形成两层UV照射涂层膜的情形下,进行一次煅烧的制造方法2需要4.5小时的煅烧时间。
在进行两组重复地形成两层涂层膜的情形下(两层×2),制造方法1需要17小时的煅烧时间。即,由于总共进行四次煅烧,所以制造方法1需要两层的煅烧时间(8.5小时)的两倍。另一方面,在制造方法2中,由于一次煅烧两层UV照射涂层膜,所以需要执行两次煅烧。因此,制造方法2的煅烧时间为两层的煅烧时间(4.5小时)的两倍,即9小时。
在形成三层涂层膜的情况下,在每个涂布工序S1之后进行煅烧的制造方法1需要13个小时的总煅烧时间。另一方面,在形成三层UV照射涂层膜的情况下,一次性执行煅烧的制造方法2需要五个小时的煅烧时间。由于充电层18变厚,所以一次煅烧三层的情形下的煅烧时间变得比一次煅烧两层的情形下的煅烧时间长。
在进行两组重复地形成三层涂层膜的情形下(三层×2),制造方法1需要26小时的煅烧时间。即,由于总共进行六次煅烧,所以制造方法1需要为三层进行的煅烧时间(13小时)的两倍。另一方面,在制造方法2中,由于一次煅烧三层UV照射涂层膜,所以需要执行两次煅烧。因此,制造方法2的煅烧时间为三层的煅烧时间(5小时)的两倍,即10小时。
作为制造方法2,由于在形成多个UV照射涂层膜之后一次煅烧多个UV照射涂层膜,所以可以缩短制造时间。因此,制造方法2提高了生产率。
显然,充电层18不限于两层或三层,其可以具有四层或更多层。在层叠多层涂层膜(即,两层或更多层)的情况下,也可以采用上述制造方法2。由于可以消除每次层叠涂层膜之后都进行的3~4小时的煅烧程序S5,所以可以缩短制造时间和设备使用时间。此外,在制造方法2中,由于一次煅烧多层UV照射涂层膜,所以也可以减少工序数。因此,制造方法2可以提高生产率并有助于降低量子电池的成本。
以上描述了本发明的实施例的示例。本发明包括不脱离其目的和优点的适当修改,并且不旨在限于上述实施例。
本申请基于并要求于2015年6月25日提交的日本专利申请No.2012-127653的优先权权益,其公开内容以引用的方式全部并入本文。
附图标记列表
10 量子电池
12 衬底
14 第一电极
16 N型金属氧化物半导体层
18 充电层
18a~18c 干燥涂层膜、UV照射涂层膜、经煅烧涂层膜
20 P型金属氧化物半导体层
22 第二电极
Claims (4)
1.一种用于制造二次电池的方法,二次电池具有充电层,充电层因通过在被绝缘材料覆盖的n型金属氧化物半导体上引起光激结构变化而在带隙中形成能级来捕获电子,所述方法包括以下工序:
涂布涂层液,以形成包括将成为充电层的成分的涂层膜;
进行干燥,以通过干燥在涂布工序中涂布的涂层液来形成干燥涂层膜;
进行照射,以通过用紫外线照射干燥涂层膜来形成UV照射涂层膜;以及
进行煅烧,以在通过重复包括涂布工序、干燥工序和照射工序的组多次,形成多个UV照射涂层膜之后,通过煅烧所述多个UV照射涂层膜来形成多个煅烧涂层膜。
2.根据权利要求1所述的用于制造二次电池的方法,其中,在形成所述多个UV照射涂层膜之后同时煅烧所述多个UV照射涂层膜来形成所述多个煅烧涂层膜,而不是在每个照射步骤之后煅烧所述多个UV照射膜中的每一个来形成所述多个煅烧涂层膜。
3.根据权利要求1或2所述的用于制造二次电池的方法,其中,煅烧工序中的煅烧温度比干燥工序中的干燥温度高。
4.根据权利要求1或2所述的用于制造二次电池的方法,其中,通过用紫外线照射所述多个煅烧涂层膜来形成充电层。
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