CN101600915A - 金属-陶瓷复合材料的薄层的制备方法 - Google Patents
金属-陶瓷复合材料的薄层的制备方法 Download PDFInfo
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- CN101600915A CN101600915A CNA2007800416481A CN200780041648A CN101600915A CN 101600915 A CN101600915 A CN 101600915A CN A2007800416481 A CNA2007800416481 A CN A2007800416481A CN 200780041648 A CN200780041648 A CN 200780041648A CN 101600915 A CN101600915 A CN 101600915A
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- metal
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Abstract
本发明涉及一种制备含有金属纳米颗粒的金属－陶瓷复合材料的薄层的方法。所述方法可用于使用金属陶瓷基选择性吸收表面层涂覆太阳能吸收器，该表面层是以可靠方式非常容易且廉价生产的并且其具有良好的光谱选择性。在所述方法中，通过将金属衬底浸渍在稳定的水性或有机悬浮液中将一种以上薄的金属陶瓷层沉积在衬底上。所述悬浮液由醇性或水性溶液组成，陶瓷纳米粉末分散在所述溶液中，并且所述溶液包含金属离子形式的金属陶瓷的金属部分。
Description
技术领域
本发明涉及包含金属纳米颗粒的金属-陶瓷复合材料的薄层的制备方法，以及所述方法的应用。
背景技术
在高效太阳能集热器中，来自太阳能吸收器表面的几乎全部太阳光谱都被转化为热能。吸收器表面以及与之相连的管道向流过所述管道的诸如水的载热流体散发热量。
吸收器表面是太阳能集热器的最重要部件。通过使用光谱选择性吸收器，这种集热器可以实现很高的光热转化率。这种表面对地球上的太阳光谱中的辐射表现出优良的吸收，同时强烈地反射热波长，也就是说，它们仅仅辐射出少量被吸收的热量。由于没有显示所述表面性质的天然材料存在，因此必须用专门的涂层来产生选择性。
通常，可通过吸收器-反射器串联来获得吸收器光谱选择性的效果。对＜2.5μm的波长具有低反射(高太阳能吸收)并且能透过IR范围内热波长的吸收层被置于对＞2.5μm波长具有高反射(低的热发射率)的金属表面上(图1)。从而，吸收层确保在对热发射率影响最小的情况下具有最大的太阳能吸收，而该热发射率由反射器层或金属衬底主导。许多位于金属衬底上的金属陶瓷复合层都显示出这种光学特性。
普通可商购的选择性太阳能吸收器是由电镀、阳极化以及化学氧化技术来制备。用电化学方法制备的最普遍使用的选择性光热吸收器层是黑铬、黑锌、氧化铜、黑钴、黑镍、氧化铁以及着色氧化铝(pigmented alumina)。
这种吸收器的太阳能吸收率为0.9且热发射率为0.1至0.3，并且通常直至425到500°开尔文的温度都是热稳定的。这些制备方法需要有毒的酸浴以及复杂的金属盐组合。此外，来自所述制备方法的废弃物是有毒且危害生态的，它们的管理(处理)会产生问题。
此外，就这些方法而言，有时很难或者甚至不可能使吸收器的光学性质与所需要的性质非常精确地匹配。
在过去的约二十年中，由于金属-陶瓷复合材料的薄膜或层具有适当且可调整的光学性质，考虑到它们适合作为选择性太阳能吸收器，人们已经对其进行了彻底的研究。
金属-陶瓷复合材料，同样称为金属陶瓷，其包含陶瓷基体，该基体具有分散于其中的金属纳米颗粒。由于许多金属陶瓷层具有相当高的IR透明度并且同时具有很高的太阳能吸收，它们注定要被用作选择性吸收器。因此，使用这种金属陶瓷层作为吸收器被人们广泛接受。此外，这种涂层在变化的热条件下同样显示出长时间的稳定性。
复合纳米材料涂层的光学性质易受层厚度、金属相体积分数、几何形状以及粒度的影响。同时，传导性颗粒的分布特征可能对金属陶瓷层的归一化折射指数产生决定性影响。例如，从空气-金属陶瓷分界面直至衬底-金属陶瓷分界面的金属颗粒浓度的逐渐增大会导致由表面反射降低而引起的更高吸收率。
经由溅射技术而沉积是一种非常洁净的方法，其不需要化学浴以及有害的酸。这种沉积方法可实现由高纯度目标材料产生具有受控层厚度的高质量光学涂层。商业上，已经通过使用圆柱型或滚动型溅射技术生产出各种选择性金属介电涂层，例如SS-C、SS-AIN(SS＝不锈钢)、Al-N和TiNOx。
这种情形中存在的问题是，溅射技术相当麻烦并且昂贵，分别需要高技术的电压源以及大真空室或者洁净室条件，并且需要能调整气体组成、层厚度以及压力条件的精确控制系统和调节系统。总体上，该方法需要的能量消耗同样很高。
考虑到太阳能市场目前的状况，其仍然处于发展的初始阶段，吸收器层仍然是集热器最昂贵的部件，所以溅射目前并不是生产低价太阳能集热器的经济手段。
与溅射层相反，太阳能吸收器涂料代表了一种价格较低廉的变化形式，然而，它们显示出由所引入有机聚合物粘合剂振动方式而引起的80至90％的非常高的热发射率，并且它们的长期稳定性依然较差。通过使用有机改性的硅氧烷树脂已经使这种涂料的稳定性得到了改善。然而，到目前为止，由于涂料基吸收器的光学性质低劣，通常它们被用于非选择性或中等选择性的吸收器。
通过将石墨层与机械磨光衬底结合，人们获得了一种低成本、机械制备的太阳能吸收器。就磨光参数而言，这种涂层是高灵敏度的，太阳能吸收在0.9左右并且热发射高达0.22。
DE 196 20 645C2描述了一种溶胶-凝胶技术，其中传导性颗粒被引入起始溶胶中，或者引入还不是非常粘稠的待形成的凝胶中。在该方法中，必须在惰性气氛以及高压(10Pa直至1000Pa)下将传导性颗粒雾化下降至小于70nm。随后通过筛选法分离较大的颗粒。在该方法中，必须用介电层涂覆金属颗粒以防止化学影响和扩散。所制备的金属纳米颗粒非常大的反应表面会因为颗粒的化学氧化而产生问题，因此必须阻止这种氧化。此外，表面处理、颗粒雾化以及筛选都是昂贵的附加步骤，导致这种制备方法成本增加。
先前的研究主要局限于微观结构，并且通过有关纳米颗粒的分布以及它们可塑性的改良来改善金属陶瓷纳米颗粒的机械性能。主要是Sekino等人，他们通过使用传统的粉末冶金法-还原并且随后烧结陶瓷且金属氧化的粉末，例如W-Al2O3(T.Sekino，A.Nakahira and K.Niihara，Relationshipbetween microstructure and high temperature mechanical properties forAl2O3/W nanocomposites.Transactions of the materials research society ofJapan16B(1994)1513-1516，and T.Sekino，A.Nakahira，M.Nawa and K.Niihara，Fabrication of Al2O3/W Nanocomposite.J.Japan Soc.of Powd.andPowd.Metal 38(1991)326-330)，或者通过用于制备诸如Ni-Al2O3的金属陶瓷复合粉末的化学法，例如溶胶-凝胶法(T.Sekino，T.Nakajima，S.Ueda andK.Niihara，Reduction and sintering of a nickel-dispersed-alumina compositeand its properties.J.Am.Ceram.Soc.80(1997)1139-1148，and T.Sekino，T.Nakajima and K.Niihara，Mechanical and magnetic properties ofnickel-dispersed alumina-based nanocomposite.Mater.Lett.29(1996)165-169).，从而研究了各种金属陶瓷纳米复合物的机械性能。这些方法用于制备复合物中金属含量为5至30％且金属颗粒大小为约40-150nm的主体样品。
在最近的几十年中，人们通过不同方法制备了各种光谱选择性Ni-Al2O3复合层。这些层通过平面RF磁控溅射，使用热压Ni-Al2O3目标物，在实验室规模下制备。使用这种方法难以实现复合物层中镍含量的变化，并且必须在复合物目标上以特殊的几何形状排列额外的Ni粒以便获得更高的金属体积分数。通过使用78nm SiO2抗反射层，才能获得约0.94的太阳能吸收值和0.07的热发射值。
已知的方法还有通过磷酸阳极化铝衬底，随后借助于NiSO4浸渍浴中的a.c.电解使经阳极化处理的铝着色。该方法获得了0.93-0.96的太阳能吸收以及0.1-0.2的热发射率。使用相同的制备方法并且研究各种浸渍参数对层光学性质的影响，获得了超过0.9的太阳能吸收率以及0.14的热发射率。
虽然商业上在太阳能收集器中使用着色氧化铝涂层，但通常认为它们不具有特别的选择性。
基于先前有关溶胶-凝胶基抗反射层以及C-SiO2复合物层的研究，人们由Ni-Al2O3溶胶制备得到了Ni-铝层，它能实现0.83的太阳能吸收以及0.03的热发射，并且金属陶瓷层的镍含量为65％。
发明内容
本发明以提供非常简单、可靠并且廉价的金属-陶瓷复合材料的薄层的制备方法为目标，该方法能获得具有耐空气湿度并且耐高温的优良光谱选择性的层，并且该方法可与各种材料一起使用。
根据本发明，通过包含权利要求1特征的方法实现了所述目标。从属权利要求叙述了有利的具体实施方案。该方法的优选应用是用于涂覆金属陶瓷基选择性太阳能吸收器。
使用根据本发明的方法，通过将金属衬底浸渍在稳定化的水性或有机悬浮液中，使一层或更多层厚度为50至2,000nm的薄金属陶瓷层沉积在该衬底上。所述悬浮液由醇性溶液或水溶液组成，粒度小于30nm的陶瓷纳米颗粒分散于其中。该溶液包含金属离子形式的金属陶瓷的金属部分。
依据溶剂的种类(水或醇)，悬浮液既可以通过静电稳定也可以通过空间稳定来稳定。为了消除团块或聚结物，通过机械以及超声分散技术使悬浮液充分分散。
以上方法所需的材料可以相当低廉的成本容易地获得。有利地，该方法不需要有毒酸浴，必须相应地不使用该有毒酸浴。同样，本方法容许简单地通过调节溶于溶液中金属离子的浓度来分别设置薄层或复合物中金属和陶瓷的体积因数(bulk factor)。
所制备的悬浮液可通过喷雾或浸渍而施加在反射器衬底上。当涂覆大表面时，这种方法同样适合于大规模生产。除了在车间和工艺控制方面的低要求外，本方法的进一步优点在于，其可涂覆几乎任何种类的表面而非仅仅是平面表面。
就本发明涂覆方法的衬底而言，可使用任何适于太阳能吸收器的衬底。优选地，该衬底由低发射率的金属或金属合金，例如铜或铝组成。当使用玻璃管或玻璃衬底时，为了实现类似的效果，最初可用土伦试剂将玻璃镀银。在干燥之后，可以施加金属陶瓷层。
根据权利要求8的具体实施方案，金属陶瓷的金属部分可以选自由包含Cu、Ni、Fe、Cr、Zn、Ti、Ag、Co、Al、Pd和Zr的组，以相应金属盐的形式形成。
参照根据权利要求9的具体实施方案，陶瓷部分可以选自包含Al2O3、AlN、SiO2、TiO2、ZrO2、Y2O3、WO3、Ta2O5、V2O5、Nb2O5、CeO2的组的纳米粉末，或者两种或三种不同纳米粉末的混合物。
在根据权利要求10的具体实施方案中，相继施加若干具有不同金属含量(从低到高)的层，从而降低表面的反射损失。有利地，该方法能对总体涂层的光学性质作出特别好的调整。单个的层可以相继施加，只要之前施加的涂层已经干燥。
与同样已知的溶胶-凝胶系统形成对比，有利地，本发明中不需要使用过于昂贵的金属醇盐。此外，不存在为精密调整层及其性质而不得不精确控制的复杂化学反应。尤其是，这种情形同样适用于发生在溶胶-凝胶系统中的水解步骤。溶胶-凝胶系统进一步的问题在于存储时间短并且过早地形成网状组织，该组织随时间增长并且相应地使工艺复杂化。同样，由于干燥时在薄层中形成了裂缝，所以避免了溶胶-凝胶系统中的发生的问题。液态粉末悬浮液与溶胶-凝胶系统相比的另一个优点在于，液态粉末悬浮液更稳定并且显示出更长的储存时间。当搅拌这种液态粉末悬浮液时，这种优势尤其明显。即使停止搅拌时，稳定化的悬浮液也可使用若干小时。甚至老化的悬浮液也可以再分散。以下，将详细描述本发明的一个具体实施方案。
下文中，将参照本发明的具体实施方案详细说明本发明。
具体实施方式
具体实施方案：Ni-Al
2
O
3
金属陶瓷太阳能吸收器
使用铜和铝衬底作为起始材料。在涂覆之前，对表面进行精细抛光以消除表面质量对太阳能吸收的负面影响。此外，除去表面粗糙性使层均匀施加而在不想要的非均匀位置上没有不期望的附着物。
随后，用乙醇和蒸馏水清洁衬底。
为了制备固体含量为2至20重量％的悬浮液，首先在烧杯中将金属盐溶于200ml蒸馏水中，所述金属盐例如，在本实施例中，为镍盐(其量取决于层中所需要的金属部分)。然后，加入平均粒度为5至30nm的Al2O3纳米粉末。在控制温度(冷却)以及高转速下，机械分散该混合物30分钟。为了避免沉积和结块，全部悬浮液是静电或静电空间(electrosterically)稳定的(取决于溶剂)。可额外地使用超声分散以便获得更细的粒度分布。
优选地，向悬浮液中加入润湿剂和粘合剂以增强衬底的润湿以及薄膜的附着力。
在分散30分钟之后，用亚微米过滤器过滤该溶液。
将衬底浸入所制备的悬浮液中。待涂覆部件应当保持若干秒时间的浸渍以便达到衬底和溶液之间的平衡状态。随后，在受控制条件以及恒定速度下将衬底从浴中撤出。在从浴中除去待涂覆部件之后，在干燥箱中干燥部件。此后，对干燥的样品进行热处理，从而获得相应的涂层硬度。这种热处理可在约500K至1,000K的烘箱中进行。在纯氢或惰性气氛下进行烧结，从而还原镍的氧化相并且避免衬底的任何氧化。
以下参照附图1至3来说明本发明的具体实施方案。图1描述了包含抗反射涂层(图1b)或不包含抗反射涂层(图1a)的Ni-Al2O3吸收器的吸收器-反射器串联(tandem)。图2显示了通过根据权利要求1方法沉积的沉积Ni-Al2O3层的表面(图2a)和横截面(图2b)的2幅显微照片。
通过将金属陶瓷层中的Ni含量调节为20重量％并且通过在抛光的铝衬底上沉积不同层厚度(通过改变拉伸速度而获得)的单个金属陶瓷层，将会获得图3中所示的选择性。含有粘合剂的样品表明吸收率为0.87并且热发射率为0.08。光学性质可通过最后的抗反射层进一步改善。
图3显示了不具有抗反射层的Ni-Al2O3吸收器的反射比，所述吸收器包含20重量％的Ni，并且是通过浸渍技术，以不同的拉伸速度(不同的层厚度)在铝衬底上沉积而成。此外，图3还显示了粘合剂对反射特征的影响。
Claims (12)
1.一种用于制备含有金属纳米颗粒的金属-陶瓷复合材料的薄层的方法，其特征在于
a.该方法以水性或醇性溶液开始，在所述溶液中金属陶瓷的金属部分以溶解的金属离子形式存在，
b.将上述溶液用作粉末基步骤的基础，在该步骤中，制备其中分散有陶瓷纳米颗粒的水性或醇性的稳定悬浮液，
c.所述陶瓷纳米颗粒是空间或静电稳定的，
d.当冷却时，通过机械或超声分散技术除去所述悬浮液中包含的聚结固体颗粒，
e.使用无机润湿剂和粘合剂以增强衬底的湿润和层对衬底的粘附，
f.通过喷雾或浸渍将所制备的悬浮液施加到反射器衬底上，
g.在干燥之后，在H2或惰性气氛中烧结样品。
2.如权利要求1所述的方法，其特征在于所述金属的粒度小于40nm。
3.如权利要求1所述的方法，其特征在于制备层厚度约为50nm至2μm的各个层。
4.如权利要求1所述的方法，其特征在于在不高于1,000°K的温度下进行烧结。
5.如权利要求1所述的方法，其特征在于所述衬底由反射器金属或低发射率的金属合金组成，例如铜或铝。
6.如权利要求1所述的方法，其特征在于首先通过土伦试剂将玻璃衬底镀银，并且在根据权利要求1的干燥之后用所述金属陶瓷涂覆。
7.如权利要求1所述的方法，其特征在于通过改变所述溶液中金属离子浓度来可分别简单地调节所述薄层或所述复合材料中的金属和陶瓷的装填量。
8.如权利要求1所述的方法，其特征在于所述金属陶瓷的金属部分选自由包含Cu、Ni、Fe、Cr、Zn、Ti、Ag、Co、Al、Pd和Zr的组，以相应金属盐的形式形成。
9.如权利要求1所述的方法，其特征在于所述金属陶瓷的所述陶瓷部分选自由包含Al2O3、AlN、SiO2、TiO2、ZrO2、Y2O3、WO3、Ta2O5、V2O5、Nb2O5、CeO2的组的纳米粉末形成。
10.如前述权利要求中任意一项所述的方法，其特征在于相继施加多个金属陶瓷层，各个层在它们的金属含量方面具有差别，并且此外，在所述金属陶瓷各层上沉积最后的抗反射层以便获得更好的光学性质和热稳定性。
11.如权利要求1和10所述的方法，其特征在于通过不具有金属部分的稀释的稳定化陶瓷悬浮液来施加抗反射层。
12.权利要求1至11所述方法用于涂覆金属陶瓷基选择性太阳能吸收器的用途。
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| CN102328476A (zh) * | 2011-08-23 | 2012-01-25 | 北京天瑞星真空技术开发有限公司 | 一种具有TiO2和Al2O3双陶瓷结构高温太阳能选择性吸收涂层及其制备方法 |
| CN103029365A (zh) * | 2011-09-30 | 2013-04-10 | 中国科学院大连化学物理研究所 | 一种中高温太阳能选择性吸收涂层 |
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|---|---|
| WO2008055496A1 (de) | 2008-05-15 |
| AU2007317053B2 (en) | 2011-04-28 |
| US20100035081A1 (en) | 2010-02-11 |
| KR20090080093A (ko) | 2009-07-23 |
| EP2122270A1 (de) | 2009-11-25 |
| CA2668736A1 (en) | 2008-05-15 |
| AU2007317053A1 (en) | 2008-05-15 |
| MX2009005005A (es) | 2009-07-31 |
| IL198351A0 (en) | 2010-02-17 |
| JP2010509498A (ja) | 2010-03-25 |
| BRPI0718831A2 (pt) | 2014-02-04 |
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