CN115279717A - 陶瓷表面改性材料 - Google Patents
陶瓷表面改性材料 Download PDFInfo
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- CN115279717A CN115279717A CN202080096082.8A CN202080096082A CN115279717A CN 115279717 A CN115279717 A CN 115279717A CN 202080096082 A CN202080096082 A CN 202080096082A CN 115279717 A CN115279717 A CN 115279717A
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- 239000000463 material Substances 0.000 title claims abstract description 120
- 230000004048 modification Effects 0.000 title description 51
- 238000012986 modification Methods 0.000 title description 51
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Abstract
描述了多孔、无粘合剂的陶瓷表面改性材料及其用途应用。所述陶瓷表面材料是基材上的多孔陶瓷材料的互连网络的形式。所述陶瓷材料可包括基材表面上的金属氧化物、金属氢氧化物和/或其水合物,或者金属碳酸盐或金属磷酸盐。所述基材可以是金属或聚合物颗粒、粉末、挤出物或薄片的形式。
Description
相关申请的交叉引用
本申请要求2019年12月12日提交的PCT申请号PCT/US2019/065978的优先权,并要求2020年3月13日提交的美国临时申请号62/989,092、2020年3月13日提交的美国临时申请号62/989,150、2020年6月12日提交的美国临时申请号63/038,642、2020年6月12日提交的美国临时申请号63/038,693以及2020年6月16日提交的美国临时申请号63/039,965的权益,所有专利文献全文以引用方式并入本文中。
技术领域
本发明涉及一种多孔陶瓷材料,其包括固定在基材表面上的互连陶瓷网络,诸如金属氧化物、金属氢氧化物、金属碳酸盐、金属钛酸盐或金属磷酸盐陶瓷。
背景技术
转化涂层是在许多金属和金属合金上添加功能层的常用方法,提供诸如粘附或腐蚀抑制的功能性质。这些涂层用于将金属表面上的天然氧化物和/或氢氧化物层转化为另一种材料。常用的转化涂层包括铬酸盐和磷酸盐转化、发蓝和阳极氧化。这些工艺都给底层金属增加了保护涂层。其他类型的涂层可以沉积到表面上,诸如油漆、干性油或其他聚合物。这些涂层通常需要底漆或具有粘附问题,使用温度限制并且缺乏耐UV性。需要提供这些现有技术中的两者的优点的新材料。
发明内容
本文提供陶瓷表面改性的基材及其应用。
在一方面,提供一种组合物,其包含多孔陶瓷材料,所述多孔陶瓷材料包括与基材接触的互连网络陶瓷材料。在一些实施方案中,至少约20质量%、30质量%、40质量%、50质量%、55质量%、60质量%、65质量%、70质量%、75质量%、80质量%、85质量%、90质量%或95质量%的陶瓷材料是互连的。在一些实施方案中,多孔陶瓷材料是无粘合剂的。在一些实施方案中,陶瓷材料的互连网络的至少一部分、大部分或基本上全部与基材直接接触。在其他实施方案中,陶瓷网络材料的互连网络可以与基材间接接触,例如,与基材表面上的表面改性或处理接触。
在一些实施方案中,基材和陶瓷材料各自包含原生金属,并且陶瓷材料中的原生金属不同于基材中的原生金属。
在一些实施方案中,基材上的陶瓷材料具有约1微米至约100微米的厚度。
在各种实施方案中,陶瓷材料包括稀土元素、过渡金属元素、碱土金属元素或铝。在某些实施方案中,陶瓷材料包括氧化物、氢氧化物或层状双氢氧化物。例如,氧化物、氢氧化物或层状双氢氧化物可以包括以下中的一种或多种:铁、铝、镁、铈、锌、锰、钛、铬、钒、锆、镍、钴、铜、银、钽、钨、硅、磷、钙、钡、锡和铕。在某些实施方案中,陶瓷材料包括磷酸盐、碳酸盐、钛酸盐、铝酸盐、锆酸盐、氟铝酸盐、硅酸盐、硫化物、钒酸盐、钨酸盐、锡酸盐或硫酸盐。
基材可以包括铝合金、镁合金、钢合金、镍合金、钛合金、聚合物、纤维素材料(诸如但不限于木材、人造丝或棉)、多糖诸如淀粉(例如热塑性淀粉、直链淀粉或支链淀粉)、半纤维素、角叉菜胶、多糖或玻璃。例如,基材可以是颗粒、粉末、挤出物、薄片或叶状结构的形式。在一些实施方案中,基材包括小于约5mm、4,mm、3mm、2mm、1mm、500微米、250微米或100微米中任一者的最大尺寸。
在一些实施方案中,多孔陶瓷材料主要是结晶的。在一些实施方案中,多孔陶瓷材料包括每平方米投影基材面积约10m2至1500m2的表面积。在一些实施方案中,多孔陶瓷材料包括每克陶瓷材料约15m2至1500m2的表面积。在一些实施方案中,多孔陶瓷材料包括约2nm至约20nm的平均孔径。在一些实施方案中,孔径分布。在一些实施阀杆中,多孔陶瓷材料包括高达约50微米的厚度,例如约0.2微米至约25微米的厚度。在一些实施方案中,多孔陶瓷材料包括大于约10%的孔隙率,例如约30%至约95%的孔隙率。在一些实施方案中,多孔陶瓷材料包括通过压汞孔隙率测定法测定的约100mm3/g至约7500mm3/g的空隙体积。
在一些实施方案中,多孔陶瓷材料包括部分或完全填充有气体、液体或固体物质或其组合的孔隙。例如,多孔陶瓷材料可以包括部分或完全填充有第二陶瓷材料的孔,该第二陶瓷材料的组成可以与和基材接触的互连陶瓷网络的组成相同或不同。在某些实施方案中,互连陶瓷网络和第二陶瓷材料包括不同的组成,其中互连陶瓷网络包括氢氧化物、氧化物或层状双氢氧化物,并且第二陶瓷材料包括磷酸盐、碳酸盐、硅酸盐、硫酸盐、钛酸盐、钨酸盐、锆酸盐、钒酸盐、锡酸盐、锌酸盐或铝酸盐。在一些实施方案中,互连陶瓷网络和第二陶瓷材料各自包含原生金属,并且互连陶瓷网络的原生金属和第二陶瓷材料的原生金属相同或不同。在一些实施方案中,互连陶瓷网络和第二陶瓷材料之间的界面包括梯度,诸如其中该界面包括磷、碳、硅、硫、钨、钛、钒、锰、镁、锌、锡、锆或铝的梯度(例如组成梯度)。在一个实施方案中,互连陶瓷网络包括金属氧化物和/或氢氧化物(例如,氧化镁和/或氢氧化镁),并且第二陶瓷材料是不同的成分(例如,碳酸镁或磷酸镁),并且在两种成分之间的界面处存在梯度,例如界面处的碳或磷梯度。
在另一方面,提供一种金属-陶瓷或聚合物-陶瓷复合材料。金属-陶瓷或聚合物-陶瓷复合材料可包括如本文所述的陶瓷改性基材的“组件”,即用与基材接触的多孔陶瓷材料的互连网络(任选地多孔陶瓷材料的无粘合剂互连网络)改性的基材。例如,可以将多个改性基材加工(例如,经由烧结、铸造或模制)成金属-陶瓷或聚合物-陶瓷复合材料。在某些实施方案中,多个陶瓷改性基材包括颗粒、粉末、薄片或挤出物,例如,各自包括小于约5mm、4,mm、3mm、2mm、1mm、500微米、250微米或100微米中任一者的最大尺寸。
在另一方面,提供一种制造方法。该方法包括将多孔陶瓷材料的无粘合剂互连网络沉积在金属或聚合物基材上,该基材为金属或聚合物颗粒、粉末、挤出物或薄片的形式,从而产生表面改性的金属或聚合物基材。表面改性的金属或聚合物基材被模制、铸造或烧结成整料或网状陶瓷或金属-陶瓷或聚合物-陶瓷复合材料部件。金属或聚合物基材芯包括比多孔陶瓷材料的互连网络更低的熔点,并且该陶瓷足够多孔以在加工(例如,模制、铸造、烧结)期间芯吸熔融金属或聚合物和/或与四羧酸熔融金属或聚合物反应。在一些实施方案中,金属颗粒、粉末、挤出物或薄片包括铝、铝合金、镁、镁合金、锌、锌合金、钙或钙合金。在一些实施方案中,聚合物颗粒、粉末、挤出物或薄片包括聚烯烃、聚酯、聚苯乙烯、聚酰胺、热塑性塑料、淀粉、丙烯酸或聚碳酸酯。在一些实施方案中,陶瓷包括氧化镁、氧化钛、氧化锌、氧化锰、氧化锆、二氧化硅或碳酸钙。
附图说明
图1A至图1B示出了用烷基膦酸单层部分填充孔隙之前(1A)和之后(1B)的陶瓷表面。较大的孔隙被保持并且由于孔隙的部分填充而稍微移动到较小的孔径,而小于约2.7nm的任何孔径被填充并且不再如通过BJH吸附/解吸所测定的那样测量。注意:在约50埃处观察到的效果对应于实验假象,在此期间在非平衡条件下在孔隙中冷凝的液氮探针快速蒸发。
具体实施方式
本发明提供了在基材上沉积的合成的互连陶瓷网络(例如,金属氧化物、氢氧化物、碳酸盐或磷酸盐),其提供所需的功能性质,诸如改善的腐蚀性能和/或改进的导电性。在一些实施方案中,陶瓷是无粘合剂的(例如,表面固定的)。沉积在基材上的第一陶瓷可以包括可及孔隙体积,该孔隙体积部分或完全填充有第二陶瓷(例如,金属氧化物、氢氧化物、碳酸盐或磷酸盐陶瓷),或者第一陶瓷可以部分或完全转化成第二陶瓷(例如,金属氧化物、氢氧化物、碳酸盐或磷酸盐陶瓷),或者其任意组合。所得陶瓷材料可用于许多应用,诸如但不限于金属表面涂层,诸如在热交换器或船只的表面上,以最小化腐蚀或结垢,作为电绝缘体,作为高温阻隔涂层,作为抗UV涂层,和/或操纵冷凝物或流体。
本发明还提供在基材上涂覆非氧化物陶瓷涂层的方法。例如,沉积在金属基材(例如,铝)上的陶瓷金属氧化物(例如,氧化镁)膜或层可以转化成金属化合物(例如,金属磷酸盐或金属碳酸盐)膜或层。转化的膜或层可能保留原始陶瓷金属氧化物膜或层的基础结构的结构伪像。
定义
本文提供的数值范围包括限定该范围的数值。
“一个”、“一种”和“所述”包括多个指代物,除非上下文中另有明确规定。
本文在说明书和权利要求书中使用的短语“和/或”应该被理解为意指如此结合的要素中的“任一者或两者”,即在一些情况下结合存在而在其他情况下分离存在的要素。除了由“和/或”从句具体指明的要素之外,还可以任选地存在其他要素,无论与具体指明的那些要素相关或不相关,除非明确地相反指示。因此,作为非限制性实例,当与诸如“包括”的开放式语言结合使用时,对“A和/或B”的引用在一个实施方案中可以指A而不是B(任选地包括除B之外的要素);在另一个实施方案中,可以指B而不是A(任选地包括除A之外的要素);在又一实施方案中,可以指A和B两者(任选地包括其他要素);等等。”
“粘结剂(Binder)”或粘结剂(binding agent)是通过粘附或内聚以机械、化学方式将其他材料保持或牵引在一起以形成粘结整体的任何材料或物质。
“无粘结剂”是指不存在可外源添加到主要材料中以改善结构完整性的粘结剂,特别是关于有机粘结剂或树脂(例如,聚合物、胶、粘合剂、沥青)或无机粘结剂(例如,石灰、水泥玻璃、石膏等)。
“毛细管爬升”是指由于多孔基材而在与液体的自由表面接触时表面张力驱动液体沿样品向上流动(毛细管爬升与由于重力引起的力(矢量)的方向平行并与之相反)。
“纤维素”材料是指由纤维素或纤维素衍生物(例如纤维素的醚或酯)构成或含有纤维素或纤维素衍生物的材料。
“陶瓷”或“陶瓷材料”是指包括具有离子键或共价键的金属或准金属和非金属的无机化合物的固体材料。“非金属”可以包括氧(氧化物陶瓷),或碳(碳化物)或氮(氮化物)(非氧化物陶瓷)。“金属”可以包括周期表第1族的非氢元素、周期表第2-12族的元素或来自p区(周期表第12-17族)的元素,例如Al、Ga、In、Tl、Sn、Pb、Bi或其组合。“准金属”可以包括B、Si、Ge、As、Sb、Se、Te或Po或其组合。
“接触角”是指通过表面和接触表面处的液-气界面之间的液体测得的角度。
“连续的”或“邻接的”是指包含彼此直接接触的壁和特征,或者在相对于单个孔或结构较大的区域或尺寸上共享公共壁的孔和结构。
“转化涂层”是指表面层,其中反应物与待处理的表面发生化学反应,这将基材或其上的涂层如陶瓷(例如金属氧化物和/或氢氧化物)涂层转化成不同的化合物。该过程通常不是添加或沉积,但可能导致较小的质量变化。
“第一四分位数孔径”是指在增加孔径的方向上测定的累积孔表面积等于通过BJH气体吸附/解吸测量测定的总累积孔表面积的25%时的孔径值。
“功能性材料层”是指可用作与周围环境相互作用的最上表面层或可用作后续材料的界面层(两个其他材料层之间的中间层)的材料层。功能材料层赋予下面的基材和/或其上沉积的材料一种或多种所需的功能性质。
“梯度”在本文中是指材料的一种或多种物理或化学性质的定量增加或降低,其通过沿着材料位于或固定于其上的基材表面从空间上的一个点传递到另一个点来观察,并且在材料上或通过材料的笛卡尔坐标中在x、y或z方向上变化来观察。梯度性质的非限制性实例包括厚度、密度、硬度、延展性、孔径、孔径分布、孔隙填充率或化学或物理组成,包括但不限于氧化态、金属浓度或交联密度,例如导致等电点、电导率、热导率、电容等的变化。
“亲水的”是指对水具有高亲和力的表面。接触角可以非常低(例如,在空气的存在下从表面通过液态水测量时小于30度)和/或不可测量。
“连续陶瓷网络”或“陶瓷材料的连续网络”或“互连陶瓷网络”是指陶瓷材料的网络或基体,其中网络中的陶瓷材料与网络中的其他陶瓷材料物理接触(连接),即大部分陶瓷材料与其他陶瓷材料邻接,从而形成独立式或支撑在基材上的脚手架结构。本文所述的互连陶瓷网络是在宏观区域或体积上的连续陶瓷相,并且可以包含具有可及孔隙体积的孔隙(开放空间),所述可及孔隙体积可以填充或部分填充有另一种材料,诸如但不限于另一种陶瓷。
“层状双氢氧化物”是指一类离子固体,其特征在于具有一般顺序[AcB Z AcB]n的层状结构,其中c表示金属阳离子层,A和B是氢氧根阴离子层,并且Z是其他阴离子和/或中性分子(诸如水)层。在PCT申请第PCT/US2017/052120号中也描述了层状双氢氧化物,其全部内容通过引用并入本文。
“大孔隙”是指固体内的几何空间,其特征尺寸基本上大于单个孔或特征的特征尺寸(例如,厚度),例如,比特征尺寸大至少约5x至约10x或约10x至约100x。
“平均值”是指算术平均值或平均值。
“平均孔径”是使用来自Barrett-Joyner-Halenda(BJH)吸附/解吸方法的总表面积和总体积测量值计算的,即4倍总孔体积除以总表面积(4V/A),假定是圆柱形孔。
“多峰”是指包含多于一种不同模式的分布,其表现为多于一种不同的峰。
流体力学中的“渗透性”是多孔材料允许流体通过其的能力的量度。介质的渗透性与孔隙率有关,但也与介质中孔的形状和它们的连通程度有关。
“孔径分布”是指通过压汞孔隙率测定法(MIP)和Washburn方程测定的每个孔径或孔径范围的相对丰度。
“孔隙率”是材料中空隙(即,“空的”)空间的量度,并且是空隙(即,大空隙)的体积的分数。在总体积上,在0和1之间,或作为在0%和100%之间的百分比。本文公开的孔隙率通过压汞孔隙率测定法测量。
“多孔”是指固体材料内的空间、孔或空隙。
“超疏水”是指非常难以润湿的表面。水滴在超疏水材料上的接触角在此是指固着的液滴接触角>150°。高度疏水接触角>120°。这里提到的接触角是通过液体的表面之间形成的角度。
“每平方米投影基材面积的表面积”是指实际测量的表面积(通常以平方米测量)除以基材的表面积(如果基材是原子级平滑的(没有表面粗糙度)),通常也以平方米测量。
“协同作用”或“协同作用的”是指两种或更多种物质、材料或试剂之间的相互作用或协同作用,以产生比其单独的单独作用的总和更大(正协同作用)或更小(负协同作用)的组合作用。
“厚度”是指基材表面和表面改性(例如,陶瓷)材料顶部之间的长度。
“第三四分位数孔径”是指在增加孔径的方向上测定的累积孔表面积等于通过BJH气体吸附/解吸测量测定的总累积孔表面积的75%时的孔径值。
“迂曲度”是指通过多孔结构的最短路径的分数Δl以及该路径的起点和终点之间的欧几里德(Euclidean)距离Δx。
“可调谐”是指材料的功能、特性或质量被改变或修改的能力。
结构化陶瓷材料
如本文所述的连续或离散涂料或表面改性材料(包括互连陶瓷网络的多孔陶瓷材料)可以是结构化陶瓷,例如无粘合剂(例如表面固定的)陶瓷,诸如结晶度大于约20%的无粘合剂陶瓷,例如陶瓷材料的互连网络。在一些实施方案中,结构化陶瓷是多孔的,例如多孔陶瓷材料的互连网络。在PCT/US19/65978中提供了陶瓷材料的非限制性实例,其全部内容通过引用并入本文。
陶瓷材料的互连网络可以包括金属氧化物和/或氢氧化物陶瓷,例如单一金属或混合金属氧化物和/或氢氧化物陶瓷。在一些实施方案中,陶瓷材料的互连网络包括金属氢氧化物和/或氢氧化物陶瓷,例如单一金属或混合金属氧化物和/或氢氧化物陶瓷。在一些实施方案中,陶瓷材料的互连网络包括金属氧化物和金属氢氧化物陶瓷,其中金属氧化物和金属氢氧化物包括相同或不同的单一金属或混合金属。在一些实施方案中,陶瓷材料的互连网络包括金属氧化物和/或金属氢氧化物陶瓷,其中基材被水或其他化合物水合,导致表面能的变化并潜在地改变陶瓷的金属氧化物与金属氢氧化物组成的比率。在一些实施方案中,陶瓷材料的互连网络包括金属氢氧化物,其中至少一部分的金属氢氧化物为层状双氢氧化物的形式,例如至少约5%、10%、15%、20%、25%、30%、35%、40%、45%、50%、55%、60%、65%、70%、75%、80%、85%、90%或95%的金属氢氧化物为层状双氢氧化物。
在一些实施方案中,“金属氧化物”或“金属氢氧化物”可以分别是金属氧化物或金属氢氧化物的水合物的形式,或者金属氧化物或金属氢氧化物的一部分可以分别是金属氧化物或金属氢氧化物的水合物的形式。
混合金属氧化物或混合金属氢氧化物可以分别包括例如多于一种金属的氧化物或氢氧化物,所述金属诸如但不限于铁、钴、镍、铜、锰、铬、钛、钒、锆、钼、钽、锌、铅、锡、钨、铈、镨、钐、钆、镧、镁、铝或钙。
在一些实施方案中,陶瓷材料的互连网络是无粘合剂陶瓷材料,即在没有粘合剂的情况下沉积在基材上。在一些实施方案中,陶瓷材料的互连网络固定在基材上。
在一些实施方案中,陶瓷材料的互连网络可以是金属磷酸盐、金属碳酸盐、金属硫酸盐、金属硼酸盐、金属钨酸盐、金属钼酸盐、金属钛酸盐、金属锡酸盐、金属硅酸盐和金属钒酸盐或其组合的形式。在一些实施方案中,材料可以包括但不限于铁、钴、镍、铜、锰、铬、钛、钒、锆、钼、钽、锌、铅、锡、钨、铈、镨、钐、钆、镧、镁、铝、钡或钙。
在一些实施方案中,陶瓷材料的互连网络具有开孔多孔结构,例如,其特征在于以下中的一种或多种:能够在1小时内在封闭容器中实现具有大于约5mm的低表面张力的液体(例如,小于约25mN/m,诸如异丙醇)逆着重力沿表面向上的毛细管爬升;约0.1m2/g至约10,000m2/g的表面积;约10nm至约1000nm或约1nm至约1000nm的平均孔径;约0至约1cc/g的通过汞(Hg)侵入孔隙率测定法测量的孔隙体积;以及约1至约1000的曲折度,所述曲折度定义为流体路径的长度与最短距离的“弧线比”;和/或约1至约10,000毫达西的渗透率。
陶瓷材料是多孔的,并且可以具有约5%至约95%的孔隙率。在一些实施方案中,孔隙率可以是至少约或大于约5%、10%、15%、20%、25%、30%、35%、40%、50%、55%、60%、65%、70%、75%、80%、85%、90%或95%中的任一者。在一些实施方案中,孔隙率为约10%至约90%、约30%至约90%、约40%至约80%、或约50%至约70%。
在一些实施方案中,多孔陶瓷材料具有约1至10,000毫达西的渗透性。在一些实施方案中,渗透性可以是至少约1、10、100、500、1000、5000或10,000毫达西中的任一者。在一些实施方案中,渗透性为约1至约100、约50至约250、约100至约500、约250至约750、约500至约1000、约750至约2000、约1000至约2500、约2000至约5000、约3000至约7500、约5000至约10,000、约1至约1000、约1000至约5000、或约5000至约10,000毫达西。
在一些实施方案中,多孔陶瓷材料包括通过压汞孔隙率测定法测定的约100mm3/g至约7500mm3/g的空隙体积。在一些实施方案中,空隙体积为至少约100、200、300、400、500、600、700、800、900、1000、1500、2000、2500、3000、3500、4000、4500、5000、5500、6000、6500、7000或7500mm3/g中的任一者。在一些实施方案中,空隙体积为约100至约500、约200至约1000、约400至约800、约500至约1000、约800至约1500、约1000至约2000、约1500至约3000、约2000至约5000、约3000至约7500、约250至约5000、约350至约4000、约400至约3000、约250至约1000、约250至约2500、约2500至约5000或约500至约4000mm3/g中的任一者。
本文公开的多孔陶瓷材料的特征可以在于其与液体材料的相互作用。如前所述,陶瓷材料的特征可以在于能够在1小时内在封闭容器中实现具有大于约5mm的低表面张力的液体(例如,小于约25mN/m,诸如异丙醇)逆着重力沿表面向上的毛细管爬升。可以使用在20℃下表面张力小于约25mN/m的其他溶剂,包括但不限于全氟己烷、全氟庚烷、全氟辛烷、正己烷(HEX)、聚二甲基硅氧烷(Baysilone M5)、叔丁基氯、正庚烷、正辛烷(OCT)、异丁基氯、乙醇、甲醇、异丙醇、1-氯丁烷、异戊基氯、丙醇、正癸烷(DEC)、乙基溴、甲基乙基酮(MEK)、正十一烷、环己烷。可以使用在20℃下表面张力>25mN/m的其他溶剂,包括:丙酮(2-丙酮)、正十二烷(DDEC)、异戊腈、四氢呋喃(THF)、二氯甲烷、正十四烷(TDEC)、均四氯甲烷、正十六烷(HDEC)、氯仿、1-辛醇、丁腈、对伞花烃、异丙苯、甲苯、二丙二醇单甲醚、1-癸醇、乙二醇单乙醚(乙基溶纤剂)、1,3,5-三甲苯(均三甲苯)、苯、间二甲苯、正丙基苯、乙基苯、正丁基苯、1-硝基丙烷、邻二甲苯、十二烷基苯、富马酸二乙酯、萘烷、硝基乙烷、二硫化碳、环戊醇、1,4-二噁烷、1,2-二氯乙烷、氯苯、二丙二醇、环己醇、六氯丁二烯、溴苯、吡咯(PY)、N,N-二甲基乙酰胺(DMA)、硝基甲烷、邻苯二甲酸二乙酯、N,N-二甲基甲酰胺(DMF)、吡啶、甲基萘、苄醇、邻氨基苯甲酸乙酯、碘苯、N-甲基-2-吡咯烷酮、磷酸三甲苯酯(TCP)、间硝基甲苯、溴仿、邻硝基甲苯、异硫氰酸苯酯、a-氯萘、糠醛(2-糠醛)、喹啉、1,5-戊二醇、苯胺(AN)、聚乙二醇200(PEG)、邻氨基苯甲酸甲酯、硝基苯、a-溴萘(BN)、二乙二醇(DEG)、1,2,3-三溴丙烷、苯甲酸苄酯(BNBZ)、1,3-二碘丙烷、3-吡啶甲醇(PYC)、乙二醇(EG)、2-氨基乙醇、均四溴乙烷、二碘甲烷(DI)、硫二甘醇(2,2'-硫代二乙醇)(TDG)、甲酰胺(FA)、甘油(GLY)、水(WA)和汞。
多孔陶瓷表面改性材料(互连陶瓷网络)可以具有在各种温度下实现水毛细管爬升的能力。这些材料可以具有分离可混溶材料和二元共沸物(例如乙醇-水、乙酸乙酯-乙醇或丁醇-水)以破坏三元共沸物或从包括乙醇和水的混合物中去除戊醇的能力。
多孔陶瓷表面改性材料(互连陶瓷网络)的孔隙可以包括填充有一种或多种气体的开孔,可以包括部分填充的孔隙(例如,部分填充有一种或多种固体材料),或可以包括完全或基本上填充的孔隙(例如,完全或基本上填充有一种或多种液体和/或固体材料)。在一些实施方案中,孔隙部分地、基本上或完全填充有气体、液体或固体物质或其组合。
在一些实施方案中,多孔陶瓷材料的可及孔隙体积部分填充有第一材料,并且然后部分或完全填充有第二材料。在一些实施方案中,第二材料作为部分填充的孔隙上的材料层添加。在一些实施方案中,第一材料是气体、固体或液体,或者气体、液体和/或固体物质的组合。在一些实施方案中,第二材料是气体、固体和/或液体物质,或者是环境(例如,空气)。实例包括并且由此赋予的功能包括孔隙率、芯吸、排斥性和/或润湿行为的变化;复合材料(包括多孔材料和第二材料)的变化,以改变电/介电性能,改变机械性质如耐磨性、硬度、韧性、触感、弹性模量、屈服强度、屈服应力、杨氏模量、表面(压缩或拉伸)应力和/或弹性;热性质如热扩散率、电导率、热膨胀系数、热界面应力和/或热各向异性的变化;光学性质如发射率、颜色、反射率和/或吸收系数的改变;化学性质如腐蚀、催化、反应性、惰性、相容性、耐结垢性、离子泵阻塞、耐微生物性和/或微生物相容性的改变;和/或作为生物催化的底物。
在一些实施方案中,第一材料以正或负协同方式与第二材料相互作用以改变陶瓷材料的一种或多种功能特性,诸如但不限于润湿性、硬度、弹性、机械、电、压电、光学、粘附或热性质、微生物亲和力或耐受性、生物膜生长的改变、催化活性、渗透性、美学外观、抗液性和/或耐腐蚀性。
可用于部分或完全填充孔隙的非限制性材料包括能够掺入到表面的分子,诸如具有头基和尾基的分子,其中头基是硅烷、膦酸酯或膦酸、羧酸、乙烯基、氢氧化物、硫醇或铵化合物。尾基可以包括任何官能团,诸如烃、碳氟化合物、乙烯基、苯基和/或季铵基。其他陶瓷材料(第二陶瓷材料)也可以部分或完全沉积到孔隙中。聚合物也可以部分或完全沉积到孔隙中。第二陶瓷材料可以包括例如锌、铝、锰、镁、铈、钆和钴的一种或多种氧化物。此外,陶瓷材料可以包括可添加到表面改性材料中的任何固体材料,包括主要以离子键和共价键保持的金属、非金属或准金属原子的无机化合物,例如粘土、二氧化硅和玻璃。其他陶瓷(第二陶瓷材料)可以包括金属磷酸盐、金属碳酸盐、金属硫酸盐、金属硼酸盐、金属钨酸盐、金属钼酸盐、金属钛酸盐、金属锡酸盐、金属硅酸盐、金属钒酸盐或金属锌酸盐。在一些实施方案中,第二陶瓷材料可以包括但不限于铁、钴、镍、铜、锰、铬、钛、钒、锆、钼、钽、锌、铅、锡、钨、铈、镨、钐、钆、镧、镁、铝、钡或钙。聚合物可以包括例如天然聚合物材料,诸如汉麻、虫胶、琥珀、羊毛、丝、天然橡胶、纤维素和其他天然纤维、糖、半纤维素和全纤维素、多糖和生物衍生材料如胞外蛋白、DNA、壳多糖。合成聚合物包括例如含有聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、合成橡胶、酚醛树脂(或酚醛塑料)、氯丁橡胶、尼龙、聚丙烯腈、PVB、有机硅、聚异丁烯、PEEK、PMMA和PTFE的聚合物和共聚物。
在一些实施方案中,多孔陶瓷材料的可及孔隙体积被薄复合聚合物层部分填充,以产生具有由聚合物提供的孔隙率和功能性的表面改性材料。在其他实施方案中,孔隙被厚聚合物层完全填充,以产生具有厚聚合物层的表面改性材料,所述厚聚合物层具有多孔基体材料和聚合物层的复合性质。本文的组合物中描述的聚合物包括共聚物。
在一些实施方案中,多孔陶瓷材料的可及孔隙体积部分或完全填充有沉积在表面改性材料的表面上的材料层。在一些实施方案中,沉积向表面改性材料中添加一个或多个官能团的材料层,所述官能团诸如但不限于铵基(例如季铵基)、烷基、全氟烷基、氟烷基。在一些实施方案中,沉积聚合物或陶瓷层。在一个实施方案中,沉积陶瓷顶表面层,该陶瓷顶表面层是与基材上的无粘结剂多孔陶瓷材料的陶瓷相同或不同的陶瓷。由此赋予的官能团和功能的实例包括用于抗微生物功能的季铵基团、用于斥水性和烃亲和性的烷基链、用于防水和防油功能的全氟烷基、用于机械性能功能的聚合物、用于美学功能、光电功能或防腐功能的其他陶瓷。
在一些实施方案中,多孔陶瓷材料的可及孔隙体积部分或完全填充有气体、液体或固体物质或其组合,并且组合物还包含在陶瓷材料上的顶表面材料层,并且顶表面材料赋予一种或多种功能,诸如但不限于与液体的润湿性和/或液体中化合物的选择性分离。在某些实施方案中,顶表面材料是与孔隙被部分、基本上或完全填充的物质分离的材料,并且其自身不填充或挤入孔隙中。在一些实施方案中,顶表面材料与孔隙中的物质相互作用。例如,顶表面材料可以与孔隙中的物质相互作用,以提供一种或多种功能,诸如但不限于热管理、电化学反应性调节和/或机械性能调节。在某些实施方案中,顶表面材料是与无粘结剂多孔陶瓷材料接触的周围环境。
在一些实施方案中,多孔陶瓷材料的可及孔隙体积基本上或完全填充有聚合物或陶瓷材料。
在一些实施方案中,孔隙中的材料与陶瓷材料相互作用。此类材料和由此赋予的功能的实例包括通过环境液体或蒸气对表面改性材料的氧化、微量组分(例如,环境污染物)的冷凝、从环境空气中捕获或氧化有害环境材料如CO或H2S以及/或在环境中收集和保留材料。
在一些实施方案中,环境中或添加到孔隙中的水分与孔隙中的材料相互作用,以改性孔隙中的材料或表面改性材料。此类材料和由此赋予的功能的实例包括润湿行为的变化、光学性质的变化、氧化态或反应性的变化、蒸发速率的变化、结霜、结冰或冷凝。
在一些实施方案中,孔隙中的材料可以被设计成与陶瓷材料相互作用以“调整”整个表面的性质。可调性质的实例包括但不限于润湿性、硬度、耐微生物性、催化活性、耐腐蚀性、颜色和/或光化学活性。
在一些实施方案中,陶瓷表面改性材料(互连陶瓷网络)和孔隙中的材料以协同方式相互作用,例如,仅与表面改性材料和/或孔隙中的材料的功能相比,增强或降低表面改性材料和/或孔隙中的材料的至少一种功能。在一些实施方案中,孔隙中的两种或更多种材料以协同方式相互作用,例如,仅与材料的功能相比,增强或降低孔隙中的至少一种材料的至少一种功能。
在一些实施方案中,陶瓷表面改性材料(互连陶瓷网络)是不对称的,例如,不是球形、圆柱形、立方形或以其他方式有序的孔隙形态,所述孔隙形态具有明确的、相对恒定的表面积与体积的正态分布,其特征在于第一四分位数处的孔径与第三四分位数处的孔径的比率作为无粘结剂陶瓷表面改性的厚度的函数。特别地,当与球形、圆柱形或立方体结构相比时,孔隙形态围绕其中心不对称。不对称孔隙的非限制性实例描述于PCT申请第PCT/US19/39743号中,其全文以引用方式并入本文。
多孔陶瓷表面改性材料(互连陶瓷网络)的特征可在于随着与基材的距离而变化的宽孔径分布。特别地,在距基材给定距离处的孔隙结构可以局部表征,例如如本文所述,并且在不同距离处具有不同的表征。所得不对称性由基材、离子迁移率、加工条件如温度、压力和浓度的组合原位确定。不对称度可以通过本体方法如混合、搅拌、电场调制和槽式过滤,或通过表面定向的处理方法如剪切速率、撞击流或表面电荷改性和调制来进一步改性。不对称性可以通过各种方法如蚀刻、径迹蚀刻、离子束研磨、氧化、光催化或通过另外的方法非原位确定。这些方法是指具有厚度和/或孔隙深度的较窄或对称孔隙结构的材料,诸如沸石、径迹蚀刻膜或膨胀PTFE膜。
在一些实施方案中,多孔陶瓷表面改性材料(互连陶瓷网络)包括范围为约2nm至约50nm的中孔平均孔径。在其他实施方案中,平均孔径范围为约50nm至约1000nm。在一些实施方案中,无粘结剂多孔陶瓷材料包括约2nm至约20nm的平均孔径。在一些实施方案中,平均孔径为至少约2、3、4、5、6、7、8、9、10、11、12、13、14、15、16、17、18、19或20nm中的任一者。在一些实施方案中,平均孔径为约2至约5、约4至约9、约5至约10、约7至约12、约9至约15、约12至约18、约15至约20、约4至约11、约5至约9、约4至约8、或约7至约11nm中的任一者。
陶瓷表面改性材料(互连陶瓷网络)可以包括一种或多种金属氧化物和/或金属氢氧化物(和/或其水合物)。可包含在本文公开的陶瓷组合物中的金属的非限制性实例包括:锌、铝、锰、镁、铈、铜、钆、钨、锡、铅和钴。在一些实施方案中,陶瓷材料包括过渡金属、第II族元素、稀土元素(例如,镧、铈、钆、镨、钪、钇、钐或钕)、铝、锡或铅。在一些实施方案中,陶瓷材料包括两种或多种金属氧化物(例如,混合金属氧化物),包括但不限于锌、铝、锰、镁、铈、镨和钴。
在一些实施方案中,陶瓷表面改性材料(互连陶瓷网络)包括:锌和铝的氧化物和/或氢氧化物的混合物;ZnO和Al2O3的混合物,以及Zn-铝酸盐;包含含有Zn、Al和氧的任何/所有相的材料的混合物;锰和镁的氧化物和/或氢氧化物的混合物;氧化锰;氧化铝;混合金属锰氧化物和/或氢氧化物;镁和铝的氧化物和/或氢氧化物的混合物;镁、铈和铝的氧化物和/或氢氧化物的混合物;锌、钆和铝的氧化物和/或氢氧化物的混合物;钴和铝的氧化物和/或氢氧化物的混合物;锰和铝的氧化物和/或氢氧化物的混合物;铈和铝的氧化物和/或氢氧化物的混合物;铁和铝的氧化物和/或氢氧化物的混合物;钨和铝的氧化物和/或氢氧化物的混合物;锡和铝氧化物的混合物;氧化钨和/或氢氧化钨;氧化镁和/或氢氧化镁;氧化锰和/或氢氧化锰;氧化锡和/或氢氧化锡;或氧化锌和/或氢氧化锌。
在一些实施方案中,陶瓷材料的互连网络中的至少一种金属处于2+氧化态。
在一些实施方案中,陶瓷表面改性材料(互连陶瓷网络)包括锌、铝、锰、镁、铈、钆和钴的一种或多种氧化物和/或氢氧化物,并且基材是铝或铝合金。
在一些实施方案中,陶瓷表面改性材料(互连陶瓷网络)是超疏水的。在一些实施方案中,表面改性材料是高度疏水的。在一些实施方案中,与不包括陶瓷材料的基材相比,表面改性材料包括选自以下的一种或多种功能特性:润湿性、硬度、弹性、机械、电、压电、电磁、光学、粘附或热性质、微生物亲和力或耐受性、生物膜生长的改变、催化活性、渗透性、美学外观和耐腐蚀性。
在一些实施方案中,功能材料层(例如,顶层材料)沉积在陶瓷材料的互连网络上。此类材料的实例包括但不限于用于抗微生物功能的季铵基团、用于斥水性和烃亲和性的烷基链、用于防水和防油功能的全氟烷基、用于机械性能功能的聚合物、用于美学功能、光电功能或防腐功能的其他陶瓷。由此类材料赋予的功能的实例包括但不限于孔隙率、芯吸、排斥性和/或润湿行为的变化;复合材料(包括多孔材料和第二材料)的变化,以改变电/介电性能,改变机械性质如耐磨性、硬度、韧性、触感、弹性模量、屈服强度、屈服应力、杨氏模量、表面(压缩或拉伸)应力、拉伸强度、压缩强度和/或弹性;热性质如热扩散率、电导率、热膨胀系数、热界面应力、热各向异性的变化,以改变光学性质,诸如发射率、颜色、反射率和/或吸收系数,以改变化学性质,诸如腐蚀、催化、反应性、惰性、相容性、耐污性、离子泵阻塞、耐微生物性和/或微生物相容性、促进后续材料层的粘附以及/或作为生物催化的底物。
在一些实施方案中,与基材材料如聚合物或本文公开的任何基材材料相比,陶瓷表面改性材料(互连陶瓷网络)具有抗紫外线辐射降解性。
在一些实施方案中,陶瓷表面改性材料(互连陶瓷网络)包括约0.5微米至约20微米的厚度。在一些实施方案中,陶瓷材料包括约0.2微米至约25微米的厚度。在一些实施方案中,厚度为至少约0.2、0.5、1、2、3、4、5、6、7、8、9、10、11、12、13、14、15、16、17、18、19、20、21、22、23、24或25微米中的任一者。在一些实施方案中,厚度为约0.2至约0.5、约0.5至约1、约1至约5、约3至约7、约5至约10、约7至约15、约10至约15、约12至约18、约15至约20、约18至约25、约0.5至约15、约2至约10、约1至约10、约3至约13、约0.5至约15、约0.5至约5、约0.5至约10或约5至约15微米中的任一者。
在一些实施方案中,陶瓷表面改性材料(互连陶瓷网络)的特征在于约0°至约180°的水接触角。在其他实施方案中,水接触角小于约30度。在其他实施方案中,水接触角大于约150度。
在一些实施方案中,陶瓷表面改性材料(互连陶瓷网络)包括每平方米投影基材面积约1.1m2至约100m2的表面积。在一些实施方案中,陶瓷材料包括每平方米投影基材面积约10m2至约1500m2的表面积。在一些实施方案中,表面积为每平方米投影基材面积至少约10、50、100、150、200、250、300、350、400、450、500、550、600、650、700、750、800、850、900、950、1000、1050、1100、1150、1200、1250、1300、1350、1400、1450或1500m2中的任一者。在一些实施方案中,表面积为每平方米投影基材面积约10至约100、约50至约250、约150至约500、约250至约750、约500至约1000、约750至约1200、约1000至约1500、约70至约1000、约150至约800、约500至约900、或约500至约1000m2中的任一者。
在一些实施方案中,陶瓷材料(互连陶瓷网络)包括每克陶瓷材料约15m2至约1500m2的表面积。在一些实施方案中,表面积为每克陶瓷材料至少约15、50、100、150、200、250、300、350、400、450、500、550、600、650、700、750、800、850、900、950、1000、1050、1100、1150、1200、1250、1300、1350、1400、1450或1500m2中的任一者。在一些实施方案中,表面积为每克陶瓷材料约15至约100、约50至约250、约150至约500、约250至约750、约500至约1000、约750至约1200、约1000至约1500、约50至约700、约75至约600、约150至约650、或约250至约700m2中的任一者。
基材
在其上施加或沉积包括如本文所述的互连陶瓷网络的多孔陶瓷材料的基材可以由适用于结构或功能特性或功能应用的任何材料组成,例如,在诸如热交换器的装置中。在一些实施方案中,基材是铝或含有铝(例如,铝合金)、铁合金、锌、锌合金、铜、铜合金、镍合金、镍、钛合金、钛、含钴-铬的合金、玻璃、聚合物、共聚物、天然材料(例如,含纤维素的天然材料)或塑料。
在一些实施方案中,基材包括金属,并且如本文所述的陶瓷表面改性材料中的原生金属不同于基材中的原生金属。原生金属是占基材或陶瓷材料中总金属的至少约50%、60%、70%、80%、90%或95%的金属,例如如通过基于原子金属的x射线衍射所测定。基材原生金属的实例包括但不限于铝、铁、铜、锌、镍、钛和镁。陶瓷原生金属的实例包括但不限于锌、铝、锰、镁、铈、铜、钆、钨、锡、铅和钴。
在一些实施方案中,基材包括能够在允许基材金属局部溶解的反应条件下反应(例如溶解)的金属,并且基材金属被掺入到基材改性材料中,诸如陶瓷材料,例如无粘结剂多孔陶瓷材料。例如,铝基材可以提供铝(例如,Al2+),当陶瓷材料沉积在基材上时,铝掺入到陶瓷材料中。
在一些实施方案中,基材是颗粒、粉末、挤出物、球粒、薄片或叶状(例如,双叶、三叶、四叶等)结构。在一些实施方案中,基材是金属颗粒、粉末、挤出物、球粒、薄片或叶状结构,其中沉积的无粘合剂互连陶瓷网络沉积在基材的表面上。
在一些实施方案中,基材是陶瓷材料。在一些实施方案中,基材包括陶瓷材料。在一些实施方案中,陶瓷材料是氧化物陶瓷、非氧化物陶瓷或其组合。在一些实施方案中,陶瓷材料包括氧化物陶瓷、非氧化物陶瓷或其组合。在一些实施方案中,陶瓷材料由一种或多种氧化物陶瓷、一种或多种非氧化物陶瓷或其组合组成。在一些实施方案中,陶瓷材料由一种或多种氧化物陶瓷组成。在一些实施方案中,陶瓷材料由一种或多种非氧化物陶瓷组成。在一些实施方案中,陶瓷材料包括氧化物陶瓷。在一些实施方案中,氧化物陶瓷是氧化物、氢氧化物、混合氧化物/氢氧化物、铝酸盐、硅酸盐、钛酸盐、锆酸盐、钨酸盐或其混合物。在一些实施方案中,其中氧化物陶瓷是混合氧化物/氢氧化物,氧化物:氢氧化物的比率是混合氧化物/氢氧化物的水合程度的函数。在一些实施方案中,氧化物陶瓷是氧化铝(aluminum oxide/alumina)、氧化硅(二氧化硅)、二氧化硅-氧化铝、氧化铈(二氧化铈)、氧化钇(yttrium oxide/yttria)、氧化钛(二氧化钛)、氧化锆(zirconium oxide/zirconia)、二氧化铪(hafnium oxide/hafnia)、氧化钼、氧化钨、氧化锡或其组合。在一些实施方案中,氧化物陶瓷是氧化铝、二氧化硅或二氧化硅-氧化铝。在一些实施方案中,氧化物陶瓷是氧化铝。在一些实施方案中,氧化物陶瓷是二氧化硅。在一些实施方案中,氧化物陶瓷是二氧化硅-氧化铝。在一些实施方案中,氧化物陶瓷是二氧化钛、氧化锆、氧化铪或其组合。在一些实施方案中,氧化物陶瓷是二氧化钛。在一些实施方案中,氧化物陶瓷是氧化锆。在一些实施方案中,氧化物陶瓷包括碱金属氧化物/氢氧化物、碱土金属氧化物/氢氧化物或其组合。在一些实施方案中,氧化物陶瓷包括氧化钠/氢氧化钠或氧化钾/氢氧化钾。在一些实施方案中,氧化物陶瓷包括氧化二钾。在一些实施方案中,氧化物陶瓷包括氧化二钠。在一些实施方案中,氧化物陶瓷是氧化镁(magnesium oxide/magnesia)或氧化钙。在一些实施方案中,氧化物陶瓷是氧化镁。在一些实施方案中,氧化物陶瓷是铝酸镁或铝酸钙。在一些实施方案中,氧化物陶瓷是碱金属硅酸盐、硅酸镁、硅酸钙、硅酸铝、硅酸锆或其组合。在一些实施方案中,氧化物陶瓷是钛酸镁或钛酸铝。在一些实施方案中,氧化物陶瓷是锆酸铝、锆酸镁或锆酸钙。在一些实施方案中,氧化物陶瓷是沸石。在一些实施方案中,陶瓷材料包括非氧化物陶瓷。在一些实施方案中,非氧化物陶瓷是碳化物、氮化物或氧氮化物。在一些实施方案中,非氧化物陶瓷是氮化物陶瓷或碳化物陶瓷。在一些实施方案中,非氧化物陶瓷是氮化硼、氮化铝、氮化硅、碳化硼、碳化硅、碳化钛、碳化钨、碳化钼或其组合。在一些实施方案中,非氧化物陶瓷是硅铝氧氮化物。
在一些实施方案中,基材包括陶瓷材料。在一些实施方案中,陶瓷材料包括氧化物陶瓷。在一些实施方案中,氧化物陶瓷包括硫酸化的氧化物。在一些实施方案中,硫酸化的氧化物是硫酸化的二氧化钛、硫酸化的氧化锆或硫酸化的氧化锡。
在一些实施方案中,基材包括陶瓷材料。在一些实施方案中,陶瓷材料包括氧化物陶瓷。在一些实施方案中,氧化物陶瓷包括碱金属卤化物、碱土金属卤化物或其组合。在一些实施方案中,氧化物陶瓷包括氯化钠、氯化钾、溴化钾、氯化钙、氯化镁或其组合。在一些实施方案中,氧化物陶瓷包括氯化镁。
在一些实施方案中,形成基材。在一些实施方案中,基材是成形的陶瓷材料。在一些实施方案中,成形的陶瓷材料是球粒、球形、环、圆柱体、蜂窝、三叶或四叶的形式。在一些实施方案中,成形的陶瓷材料是球粒的形式。在一些实施方案中,成形的陶瓷材料是球形的形式。在一些实施方案中,成形的陶瓷材料是环的形式。在一些实施方案中,成形的陶瓷材料是圆柱体的形式。在一些实施方案中,成形的陶瓷材料是蜂窝的形式。在一些实施方案中,成形的陶瓷材料是三叶的形式。在一些实施方案中,成形的陶瓷材料是四叶的形式。在一些实施方案中,成形的陶瓷材料是挤出物。在一些实施方案中,挤出物具有约0.5mm至约5mm的直径、约0.5mm至约4mm的直径、约0.5mm至约3mm的直径、约0.5mm至约2mm的直径、约0.5mm至约1mm的直径、约1mm至约5mm的直径、约1mm至约4mm的直径、约1mm至约3mm的直径或约1mm至约2mm的直径。在一些实施方案中,成形的陶瓷材料处于无规或松散的堆积构造,诸如鞍形、螺旋形填料或拉西环(Raschig rings)。在一些实施方案中,成形的陶瓷材料为网状构造,在一些实施方案中,成形的陶瓷材料为结构化填料构造。
金属氧化物的转化
本文提供了由于陶瓷表面改性(例如,多孔金属氧化物和/或氢氧化物陶瓷表面改性,例如,多孔金属氧化物和/或氢氧化物陶瓷的互连网络)的化学转化而形成的产物。本文所述的转化产物赋予基材一种或多种性质,这些性质可以与原始陶瓷表面改性所赋予的性质相同或不同。转化产物提供的益处具有广泛的适用性。形成的产物是原始金属氧化物和/或氢氧化物陶瓷材料的改性物,包括但不限于金属氧化物/氢氧化物、金属磷酸盐、金属碳酸盐、金属硫酸盐、金属硼酸盐、金属钨酸盐、金属钼酸盐、金属钛酸盐、金属锡酸盐、金属硅酸盐或金属钒酸盐。
在一些实施方案中,与不包括转化的相同陶瓷材料相比,该转化可以赋予额外的耐腐蚀性,使表面等电点或零电荷点偏移,保护免受酸或碱影响,调节光学性质以吸收、反射或发射不同频率,抑制膜等离子体ATP酶,提供铁电性质,增加电容或改善介电性能,调节电阻的温度系数,增加热稳定性,赋予压电性质,增加表面积,有助于吸附,在某些化学反应后改变颜色,增加抗紫外线(UV)性并且/或者赋予假电容性质。
在一个实施方案中,该转化降低基材对腐蚀的敏感性。在一个非限制性实例中,通过惰性金属磷酸盐或金属碳酸盐阻挡层保护基材免受腐蚀性环境和/或化学品的影响。该保护层可以以两种主要方式起作用以防止腐蚀和/或基材的电导率降低。主要的保护是物理的,惰性阻挡层防止腐蚀性物质侵蚀基材并降低电导率。金属磷酸盐层的次要功能是作为牺牲元素与腐蚀性物质反应而不是与基材反应。
用途的应用
在一些实施方案中,改性的基材是涂覆的制品,并且在涂覆时或安装到系统诸如热交换器、反应器或蒸馏塔中后使用。在其他实施方案中,涂覆的基材可以用作添加剂,诸如改性颗粒、粉末、挤出物或薄片,例如在热糊或聚合物-陶瓷复合材料中。在其他实施方案中,改性的基材可以被加工成块状部件,诸如通过烧结(例如,激光烧结)、熔铸、注射成型或涂覆基材或涂覆基材的复合物的3-D打印(例如,熔融沉积成型(FDM)3-D打印)。在一些实施方案中,涂覆的基材是表面改性的陶瓷颗粒、粉末、挤出物、球粒、薄片或叶状结构,其被烧结在一起(例如,使用激光烧结)形成金属-陶瓷复合材料。在一些实施方案中,诸如反应器或蒸馏填料,改性的基材可以形成为结构形状,诸如但不限于鞍形,并随后结合(例如,烧结)成系统中使用的更大部件。在一些实施方案中,改性的基材可以形成为结构形状,该结构形状用作填充系统中使用的较大部件的模具。在一些实施方案中,该金属-陶瓷复合材料包括氧化镁和氧化铝。在其他实施方案中,烧结(例如,激光烧结、单轴热压、热等静压)、熔铸或注射成型改性颗粒、粉末、挤出物、球粒或薄片产生陶瓷整料。在一些实施方案中,该陶瓷整料的理论密度大于约80%、大于约90%、或大于约95%。在一些实施方案中,该陶瓷整料包括镁-铝尖晶石、钛酸铝、锌-铝尖晶石,或者包括硅、铝、镁、锆、钛或钙。
在一些实施方案中,对陶瓷改性的金属颗粒、粉末、挤出物、球粒或薄片进行后加工产生光学透明的整料。在一些实施方案中,该整料可以用作屏幕或窗口。在一些实施方案中,对陶瓷改性的金属颗粒、粉末、挤出物、球粒或薄片进行后加工产生相对于不含陶瓷的固体金属具有增加的屈服强度、韧性和/或硬度的金属-陶瓷复合材料。
在一些实施方案中,在后处理的陶瓷-金属复合材料中,陶瓷形成贯穿整料固体的互连网络。在一些实施方案中,在烧结(例如,激光烧结)、铸造(例如,熔铸)或模制(例如,注射成型)期间,金属基材颗粒、粉末、挤出物或薄片在多孔互连陶瓷涂层内或穿过多孔互连陶瓷涂层熔融和流动,从而产生固体物体。在一些实施方案中,该后加工可以产生网状制造零件。在其他实施方案中,可以将涂覆的颗粒、粉末或挤出物熔铸成膜。在一些实施方案中,膜是光学透明的。
在一些实施方案中,可以选择基材粒度来确定后加工的零件中金属与陶瓷的比率。在一些实施方案中,这可以产生金属-陶瓷复合材料。在其他实施方案中,这可以产生陶瓷。在其他实施方案中,后加工的零件是超过约10%的陶瓷、超过约20%的陶瓷、超过约30%的陶瓷、超过约40%的陶瓷、超过约50%的陶瓷、超过约60%的陶瓷、超过约70%的陶瓷、超过约80%的陶瓷、超过约90%的陶瓷、超过约95%的陶瓷、超过约99%的陶瓷。
在一些实施方案中,包括陶瓷表面改性的零件可以在比其他制造技术更低的温度下加工。在一些加工技术中,基材熔融并与多孔陶瓷涂层反应。在一些实施方案中,该反应形成耐火材料。在一些实施方案中,陶瓷涂层调节基材的光学性质,从而导致后加工改善。
以下实施例旨在说明而非限制本发明。
实施例
如以下实施例中所述的多孔陶瓷材料施加到其上的基材或组件通常经历从以下开始的过程:(a)表面准备或清洁,随后(b)结构化陶瓷沉积,以及(c)另一陶瓷层的沉积或沉积的结构化陶瓷层的转化。
(a)表面准备和清洁步骤:在下面的实施例中,如下制备表面。将金属基材或组件用异丙醇(IPA)和毛巾罐式清洁或擦拭以去除任何残留的油。接着,在20℃的标称室温下将部件浸没在pH>10的苛性蚀刻浴中,直到观察到表面变暗,或约15分钟。然后将基材或组件在水中漂洗以去除任何残留的苛性碱或松散粘附的材料。接着,将部件浸没在pH低于3和温度为20℃的硝酸溶液中,以去除污迹、蚀刻反应产物、金属间化合物和表面氧化物,或酸洗基材,从而露出清洁的表面。产生清洁表面的其他表面制备技术是适当的并且是适用的。将聚合物和纤维素基材在毛巾上用异丙醇罐式清洗或擦拭以去除任何残余物。
(b)结构化陶瓷沉积:除非另有说明,否则以下实施例中的结构化陶瓷沉积被认为是连续的。通过部分化学暴露和/或通过使用掩蔽剂进行选择性覆盖。然后将基材或组件置于含有20-500mM金属硝酸盐和类似量的胺(诸如乙二胺、六亚甲基四胺或脲)的结构化陶瓷沉积浴中,并使其在基材插入之前在30℃-90℃的反应温度下反应。将组件保持在浴中,直到浊度降至100NTU以下,或者保持约5分钟至约90分钟。将基材或组件取出、沥干、冲洗并放入烘箱中以在大约100℃-800℃下干燥和/或煅烧几个小时。然后使部件冷却至室温。
(c)第二陶瓷的沉积或沉积的结构化陶瓷的转化:除非另有说明,否则在后加工步骤之前,干燥(b)中产生的结构陶瓷,诸如转化沉积的陶瓷或沉积用第二材料部分或完全填充多孔互连陶瓷网络的第二陶瓷。除非另有说明,否则施加和后续处理之间的加工时间少于24小时。
实施例1
通过转化如上所述在基板板上制备的金属(镁)氧化物互连陶瓷表面改性物,产生磷酸盐基腐蚀保护层。将先前用氧化镁结构化的陶瓷表面(使用硝酸镁和六亚甲基四胺)改性的3003铝合金基材浸入含水磷酸盐转化浴中。磷酸盐转化发生在50℃至90℃之间加热的加热水溶液中。该溶液需要三种主要组分:A=磷酸盐源,B=缓冲物质,C=催化剂。组分A可以是浓度不超过0.250M的磷酸或碱式磷酸盐。组分B可以是适当的缓冲剂,诸如浓度不超过0.150M的乙酸及其共轭碱盐或柠檬酸及其共轭碱盐。组分C是浓度不超过0.1M的锡酸盐,诸如六氢锡酸盐。必须以此方式选择组分A、B和C的适当组合,以获得6至8.5的pH。
测试这些板在中性3.5%NaCl溶液中的电化学阻抗,其中发现阻抗平均比未转化的表面改性的阻抗高一个数量级。在根据ASTM G85 A3的酸性盐雾测试中对样品和未转化的样品一起进行评估94小时。与未转化的表面改性的样品相比,在磷酸盐样品上观察到的点蚀的量减少。经由X射线荧光(XRF)观察到的转化后的化学组成显示出磷含量从0%增加至30±7%,并且锡含量从0%增加至0.5±0.2%。傅立叶变换红外(FTIR)光谱学表明存在P-O键。
实施例2
通过转化如上所述在基材上制备的金属氧化物互连陶瓷表面改性物,产生碳酸盐基腐蚀保护层。将先前用氧化镁结构化的陶瓷改性的铝合金基材浸入含水碳酸盐转化浴中。碳酸盐转化发生在50℃和90℃之间的加热水溶液中。该溶液需要一种包含碳酸盐源的组分。这可以是碳酸盐,诸如碳酸钾、碳酸氢钠、碳酸氢铵,或者是在溶液中产生碳酸的来源,诸如鼓泡的二氧化碳。碳酸盐浓度在0.01M和1M之间,并且最佳浸渍时间为600至1500分钟。
在一个特定情况下,制备125mM的NaHCO3于去离子(DI)水中的碳酸化溶液,并加热至80℃并平衡1小时。将具有氧化镁结构化沉积物的基材浸入碳酸化溶液中16小时,并添加水以保持液位。取出样品并干燥。
使用SEM观察来自碳酸盐基转化的表面结构变化。通过1408cm-1处的强IR透射峰证实了表面上碳酸盐化合物的存在。
还在根据ASTM G85 A3的酸性盐雾测试中对样品和未转化的样品一起进行评估94小时。与裸板基材材料相比,观察到的点蚀量减少。
当使用X射线衍射(XRD)分析样品时,样品中的化合物包括氢氧化镁、氢氧化铝和含碳酸盐的矿物水滑石。
实施例3
通过将如上所述在基材上制备的互连金属氧化物陶瓷结构的陶瓷转化成磷酸钙的形式,产生羟基磷灰石、磷酸八钙、磷酸三钙腐蚀保护层。将表面改性的基材浸入含有钙盐诸如氯化钙或硝酸钙、磷酸盐诸如磷酸氢钾和螯合剂/络合剂诸如尿素、六亚甲基四胺或乙二胺四乙酸的水浴中。所有组分的浓度范围为0.01M至1M。转化发生在50℃至90℃的加热水溶液中,浸渍时间为60至1500分钟。在浸渍后,在200℃至600℃的温度下进行热退火60至1500分钟。
实施例4
羟基磷灰石、磷酸八钙、磷酸三钙腐蚀保护层通过将包含磷酸钙的互连陶瓷直接沉积到基材上而形成。将基材浸入含有钙盐诸如氯化钙或硝酸钙、磷酸盐诸如磷酸氢钾和螯合剂/络合剂诸如尿素、六亚甲基四胺或乙二胺四乙酸的水浴中。所有组分的浓度范围为0.025M至1M。转化发生在50℃至90℃的加热水溶液中,浸渍时间为60至1500分钟。在浸渍后,在200℃至600℃的温度下进行热退火60至1500分钟。
实施例5
混合金属陶瓷表面改性通过转化如上所述在基材上制备的互连金属氧化物结构陶瓷而产生。将表面改性的基材浸入含水转化浴中,以引入另一种金属的阴离子形式。阴离子用作腐蚀抑制源。阴离子源是某些含氧阴离子的盐,诸如锡酸钠、钨酸钠、钼酸钠,或磷酸氧阴离子盐,诸如磷钨酸钠或磷钼酸钠。水溶液可以包含缓冲剂以稳定溶液中的离子和表面改性。缓冲剂可以包括柠檬酸体系、磷酸体系、碳酸盐体系、乙酸盐体系或普通的生物缓冲剂,诸如三(羟甲基)氨基甲烷(Tris)或3-(N-吗啉代)丙磺酸(MOPS)。溶液组分的浓度为0.01M至1M。浸渍在50℃和90℃之间的温度下进行,浸渍时间为5至1500分钟。在浸渍后,在200℃至600℃的温度下进行热退火60至1500分钟。
实施例6
混合金属陶瓷表面改性通过转化如上所述在基材上制备的互连氧化镁陶瓷表面改性而产生。将表面改性的基材浸入包含钼酸钠的含水转化浴中,以引入阴离子形式的钼。钼酸钠在灌注在陶瓷基体内中时起腐蚀抑制剂的作用。钼酸钠以0.01M至500mM,通常约100mM的浓度存在于溶液中,并且保持在范围为20℃至90℃,通常约20℃的温度下。浸渍时间为60至1500分钟,通常为约120分钟。在转化步骤后,在流动的去离子水中彻底冲洗样品,以从表面去除任何溶液。然后将样品在20℃至105℃之间的温度下干燥。在20℃和80℃的转化浴温度下转化后进行的EDS和XRF测量显示了材料的表面上存在钼。当通过扫描电子显微镜(SEM)观察时,互连氧化镁表面改性和互连钼转化的氧化镁表面改性的结构是相似的。
实施例7
混合金属陶瓷表面改性通过转化如上所述在基材上制备的氧化镁互连陶瓷表面改性而产生。将表面改性的基材浸入包含钼酸钠的含水转化浴中,以引入阴离子形式的钼。钼酸钠在灌注在陶瓷基体内中时起腐蚀抑制剂的作用。钼酸钠以0.01M至500mM,通常约100mM的浓度存在于溶液中并且保持在范围为20℃至90℃,通常约20℃的温度下。浸渍时间为60至1500分钟,通常为约120分钟。在转化步骤后,在流动的去离子水中彻底冲洗样品,以从表面去除任何溶液。然后,样品在400℃至600℃之间的温度下热退火60至1500分钟,通常约120分钟。在20℃和80℃转化后进行的EDS和XRF测量显示在材料的表面上存在钼。在转化步骤之前用EDS和XRF进行的测量没有识别出材料表面上的钼。当用SEM观察时,氧化镁表面改性和互连的钼转化的氧化镁表面改性的互连结构是类似的。
实施例8
混合金属陶瓷表面改性通过转化如上所述在基材上制备的互连氧化镁结构化的陶瓷表面改性而产生。将表面改性的基材浸入其中引入阴离子形式的锡的水性转化物中。阴离子用作腐蚀抑制源。将锡酸钠添加到水浴中。通过添加1M硝酸,将溶液的pH控制在7至13之间,通常为约8至9。任选添加缓冲剂以帮助维持溶液的pH并稳定溶液中的离子。溶液组分的浓度为0.01M至1M,通常为约100mM。浸渍在20℃和90℃之间,通常为20℃的温度下进行,浸渍时间为5至1500分钟,通常为约900分钟。在浸渍后,用去离子水彻底冲洗样品,以从表面去除任何水溶液。使样品在15℃至105℃之间的温度下干燥。在干燥样品后,用EDS和XRF对其进行分析,其中在20℃和80℃下转化浴暴露的陶瓷结构中鉴定出锡。此外,当在浸入锡酸钠浴之前和之后使用SEM成像时,陶瓷表面改性的互连结构是类似的。
实施例9
通过将铝基材上的互连的氧化镁结构化陶瓷表面改性转化为铝基材上的混合锡和氧化镁表面改性来产生混合金属陶瓷表面改性。如上所述制备互连的结构化氧化镁表面改性的基材。在该步骤结束时,互连的氧化镁表面改性的铝基材的表面呈现白色。然后将互连的镁表面改性的基材浸入0.005至1M,通常约100mM的锡酸钠溶液中。添加1M硝酸,将溶液的pH控制在7至13之间,通常为约pH 12。任选添加缓冲剂以帮助维持溶液的pH并稳定溶液中的离子。将溶液的温度控制在15℃和90℃之间,通常为约20℃,浸渍时间在60分钟和1500分钟之间,通常为约120分钟。取出后,用去离子水轻轻冲洗样品以清洁溶液表面。任选的热退火步骤在200℃和600℃之间,通常约400℃的温度下进行60至1500分钟,通常约120分钟。在20℃和80℃转化步骤结束时,混合金属陶瓷表面改性的外观是银色金属。在热退火步骤结束时,表面的颜色变成深灰色。在转化步骤之后,通过能量色散X射线光谱(EDS)在20℃下处理的样品表面的原子组成为1.31%Mg、17.65%Sn、3.17%Al、77.53%O和痕量钠。在80℃下通过EDS处理的样品表面的原子组成是14.1%Sn、85.0%O和痕量的Al、Mg和Na。两个样品的表面相互连接,并表现出通过SEM成像测定的纳米级粗糙度。
实施例10
低温(<100℃)热致变色活性表面改性通过转化如上所述在基材上制备的互连氧化镁结构化陶瓷表面改性来产生。在热退火步骤后,氧化镁结构化表面改性的颜色是白色的。将表面改性的基材浸入含水转化浴中,以将原始陶瓷金属氧化物转化为含有热致变色活性金属氧化物的混合金属氧化物。浸渍浴包含浓度在10和200mM之间,通常约100mM的偏钒酸钠水溶液。将水溶液通过添加1M硝酸保持在pH 3-7,并任选地含有缓冲剂,诸如柠檬酸体系、磷酸体系、碳酸盐体系、乙酸盐体系或普通的生物缓冲剂诸如tris或MOPS。在pH给药后,溶液变成亮橙色,表明存在十钒酸根离子。所有组分的浓度范围为0.01M至200mM。转化发生在保持在20℃至90℃之间,通常为20℃的水溶液中,浸渍时间为60至1500分钟,通常为约120分钟。在浸渍后,用去离子水彻底冲洗样品,并使样品干燥。在20℃和80℃下将基材从浸渍浴中取出后,表面的颜色为黄橙色,表明在表面上存在钒化合物。EDS显示在20℃下处理的表面的原子组成为23.7%Al、9.6%Mg、12.1%V和54.6%O。此外,表面的FTIR分析指示存在十钒酸根离子(V10O28 6-)和聚合阴离子[V3O8]n n-,诸如V6O16 2-。在812cm-1处观察到十钒酸根阴离子的反对称拉伸,在957cm-1、1025cm-1处观察到十钒酸根离子或末端VO3单元的对称拉伸。这些FTIR峰不存在于在含钒盐的浴中处理之前分析的样品中。当通过SEM观察时,该表面在结构上类似于未转化的互连氧化镁结构化陶瓷。
实施例11
低温(<100℃)热致变色活性表面改性通过转化如上所述在基材上制备的互连氧化镁结构化陶瓷表面改性来产生。在热退火步骤后,氧化镁表面改性的颜色是白色的。将表面改性的基材浸入含水转化浴中,以将原始陶瓷金属氧化物转化为含有热致变色活性金属氧化物的混合金属氧化物。浸渍浴含有所需金属的盐,诸如氯化钒或原钒酸钠。水溶液通过添加1M硝酸保持在pH3-7,并任选地含有缓冲剂,诸如柠檬酸体系、磷酸体系、碳酸盐体系、乙酸盐体系或普通的生物缓冲剂诸如tris或MOPS。在pH给药后,溶液变成亮橙色,表明存在十钒酸根离子。所有组分的浓度范围为0.01M至1M,通常为约100mM。转化发生在保持在20℃至90℃之间,通常为20℃的水溶液中,浸渍时间为60至1500分钟,通常为约120分钟。在浸渍后,用去离子水彻底冲洗样品,并将样品在400℃下烘烤60分钟。在20℃和60℃下将基材从浸渍浴中取出后,表面的颜色为黄橙色,表明在表面上存在钒化合物。在烘烤步骤之后,样品在材料表面上仍具有一些橙色,表明在表面上存在钒化合物。XRF分析显示样品中存在钒。此外,SEM分析显示钒转化的氧化镁的表面结构类似于未转化的氧化镁-两个表面都是相互连接的。
实施例12
发光陶瓷表面改性是通过转化如上所述在基材上制备的金属氧化物结构化陶瓷表面改性而产生的。将表面改性的基材浸入含水转化浴中以引入发光或将金属氧化物转化成发光化合物。水溶液可以包含发光源,诸如硝酸铕或奎宁。所有组分的浓度范围为0.01M至1M。转化发生在50℃至90℃的加热水溶液中,浸渍时间为60至1500分钟。在浸渍后,在100℃至600℃的温度下进行热退火60至1500分钟。
实施例13
通过转化如上所述在基材上制备的互连金属氧化物结构化的陶瓷表面改性来产生碳酸盐基腐蚀保护层。将先前用互连氧化镁结构化表面改性剂改性的铝合金基材浸入并保持在含有UV光源的室中,该光源在70℃下具有295-340nm的光和1-2W/m2/nm的辐照度。该室装有与环境CO2平衡的水。样品在室内保持500小时。
在根据ASTM G85 A3的酸性盐雾测试中对样品和未转化的样品一起进行评估94小时。与未转化的表面改性样品相比,观察到的点蚀缺陷数量减少。
实施例14
如上所述,将氧化镁互连多孔陶瓷表面改性剂施加到最大尺寸小于1cm的铝颗粒、粉末、薄片或挤出物上。选择涂层厚度和粒度,使得铝镁比大于2比1。然后通过熔融铝基材并使其流过多孔陶瓷涂层,使用烧结、铸造或模制对这些颗粒、粉末、薄片或挤出物进行后加工而形成整料或网状物体,从而产生相对于铝强度增加的陶瓷-金属复合材料。
实施例15
如上所述,将互连氧化镁结构化陶瓷表面改性剂施加到最大尺寸小于1cm的铝颗粒、粉末、薄片或挤出物上。选择涂层厚度和粒度,使得铝镁比为约2比1。然后通过熔融铝基材并使其流过多孔陶瓷涂层,使用烧结、铸造或模制对这些颗粒、粉末、薄片或挤出物进行后加工而形成整料或网状物体,从而由于熔融铝与化学计量量的氧化镁反应而形成尖晶石整料。使用铝颗粒上的二氧化钛涂层重复该过程以产生钛酸铝。
实施例16
如上所述,将互连氧化镁多孔陶瓷表面改性剂施加到最大尺寸小于1cm的铝颗粒、粉末、薄片或挤出物上。氧化镁层相对于未涂覆的铝提供电绝缘特性。然后将改性的粉末、薄片、颗粒或挤出物添加到树脂或粘结剂中,以产生具有电绝缘特性的导热糊剂。
实施例17
互连氧化镁多孔陶瓷表面改性应用于钎焊铝热交换器。然后将热交换器置于浴中,以将表面改性部分转化为碳酸盐基腐蚀保护层。这是通过转化如上所述在热交换器上制备的结构化金属氧化物陶瓷表面改性而产生的。将先前用结构化氧化镁表面改性剂改性的钎焊铝热交换器浸入含水碳酸盐转化浴中。碳酸盐转化发生在50℃和90℃之间的加热水溶液中。该溶液需要一种包含碳酸盐源的组分。这可以是碳酸盐,诸如碳酸钾、碳酸氢钠、碳酸氢铵,或者是在溶液中产生碳酸的来源,诸如鼓泡的二氧化碳。碳酸盐浓度在0.01M和1M之间,通常为约100mM,并且最佳浸渍时间为600至1500分钟。在完全转化为碳酸盐之前去除热交换器,得到包含含碳酸盐的陶瓷和金属氢氧化物的表面。然后对该热交换器进行ASTMG85-A3盐雾测试,并且得到与未涂覆的热交换器相比,在1000小时时具有平均较少的盐累积和腐蚀产物的表面。
实施例18
如上所述,将互连氧化锌多孔陶瓷表面改性剂沉积在3003Al基材上。然后将互连氧化锌改性的3003铝合金基材置于含有如上所述的硝酸锰盐和络合剂(诸如六亚甲基四胺)的第二沉积浴中,在约50℃至80℃的温度下持续约10分钟至约90分钟。这产生氧化锰填充的氧化锌多孔陶瓷网络。通过EDS分析证实了锌和锰的存在,并表明互连材料的表面含有氧化锌和氧化锰两者。
实施例19
产生如上所述的互连结构化氧化锰改性的铝面板。然后,通过溅射、ALD或者将金属盐溶液或金属颗粒悬浮液浇注到孔隙中,用另一种陶瓷材料填充改性的面板。这产生陶瓷填充的互连陶瓷网络。第一陶瓷和第二陶瓷可以是相同或不同的陶瓷材料。
实施例20
清洁的4006铝箔基材涂覆有基于镁、铈和铝的氧化物的混合物的互连结构化陶瓷表面。氪BET表面积测量表明,表面积为约200平方米/平方米投影基材表面积。
实施例21
清洁的4006铝箔基材涂覆有基于氧化镁和氧化铝的混合物的互连结构化陶瓷表面。然后使用十六烷基膦酸于异丙醇中的稀释溶液将表面官能化,类似于实施例16中的程序。氮BET表面积测量表明表面积为300至500平方米/平方米投影基材表面积,并且陶瓷材料的质量比表面积为150至200m2/g。水银孔隙率测定法表明存在双峰孔径分布,孔径集中在约5nm和约30nm处。BJH测量表明直径小于2.7nm的孔隙的体积实际上为零。这表明最小的孔隙直径为2.7nm。在部分填充表面官能化之前和之后通过BJH吸附测量确定的孔径分布显示在图1A-1B中。此外,水银孔隙度测定法表明该材料相对于块状氧化物材料具有52%至69%的孔隙率。
实施例22-陶瓷-陶瓷复合材料
混合金属互连陶瓷表面改性是通过转化如上所述在1mm厚的3003铝合金基材上制备的结构化氧化镁陶瓷表面改性而产生的。然后将基材置于金属丝架上,并在650℃和1800℃之间进行热处理条件。在这些条件下,基材熔融,但陶瓷表面改性剂不熔融。熔融的基材通过陶瓷表面改性的孔隙流入金属丝架下面的排水盘中。在样品冷却后,存在两种状态,一种状态仅包含表面改性,并且该状态保持在一起,因为陶瓷表面改性是互连的。其他状态包含表面改性和由于表面张力而被保持的固化基材。当基材达到其熔点时,它填充陶瓷表面改性的孔隙。在进一步加热后,基材被氧化成氧化铝,产生互连的氧化镁和氧化铝结构化陶瓷材料。这产生了互连的氧化铝-氧化镁复合材料。
实施例23
如上所述,混合金属陶瓷表面改性通过转化在纤维素基材诸如乙酸纤维素上制备的互连结构化金属氧化物陶瓷表面改性而产生。将表面改性的基材浸入含水转化浴中,以引入另一种金属的阴离子形式。将表面改性的基材浸入含水转化浴中,以将原始陶瓷金属氧化物转化为含有热致变色活性金属氧化物的混合金属氧化物。浸渍浴含有所需金属的盐,诸如氯化钒或原钒酸钠。水溶液通过添加1M硝酸保持在pH 3-7,并且可含有缓冲剂,诸如柠檬酸体系、磷酸体系、碳酸盐体系、乙酸盐体系或普通的生物缓冲剂诸如tris或MOPS。所有组分的浓度范围为0.01M至1M,通常为约100mM。转化发生在保持在20℃至90℃之间,通常约70℃的水溶液中,浸渍时间为60至1500分钟,通常为约90分钟。在浸渍步骤之后,用去离子水彻底冲洗溶液并使其干燥。
尽管出于清楚理解的目的,已经通过说明和实施例的方式相当详细地描述了前述发明,但是对于本领域技术人员显而易见的是,在不脱离本发明的精神和范围的情况下,可以实施某些改变和修改。因此,该描述不应被解释为限制本发明的范围。
本文所引用的所有出版物、专利和专利申请均出于所有目的以引用的方式整体并入本文中,并且并入的程度如同每个单独的出版物、专利或专利申请被具体地和单独地以引用的方式并入本文中一般。
Claims (39)
1.一种组合物,其包含多孔陶瓷材料,所述多孔陶瓷材料包括与基材接触的互连陶瓷网络。
2.根据权利要求1所述的组合物,其中所述多孔陶瓷材料是无粘合剂陶瓷材料。
3.根据权利要求1所述的组合物,其中所述基材和所述陶瓷材料各自包含原生金属,并且其中所述陶瓷材料中的所述原生金属不同于所述基材中的所述原生金属。
4.根据权利要求1所述的组合物,其中所述基材上的所述互连陶瓷网络包含约1微米至约100微米的厚度。
5.根据权利要求1所述的组合物,其中至少约20质量%的陶瓷内容物是互连的。
6.根据权利要求1所述的组合物,其中所述互连陶瓷网络大于约10平方微米。
7.根据权利要求1所述的组合物,其中所述组合物包含与所述基材接触的多个互连陶瓷网络。
8.根据权利要求7所述的组合物,其中所述多个互连陶瓷网络内的互连陶瓷网络的中值面积大于约10平方微米。
9.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料包括稀土元素、过渡金属元素、碱土金属元素或铝。
10.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料包括氧化物、氢氧化物或层状双氢氧化物。
11.根据权利要求10所述的组合物,其中所述氧化物、氢氧化物或层状双氢氧化物包括铁、铝、镁、铈、锌、锰、钛、铬、钒、锆、镍、钴、铜、银、钽、钨、硅、磷、钙、钡、锡或铕。
12.根据权利要求11所述的组合物,其中所述多孔陶瓷材料包括磷酸盐、碳酸盐、钛酸盐、铝酸盐、锆酸盐、氟铝酸盐、硅酸盐、硫化物、钒酸盐、钨酸盐、锡酸盐或硫酸盐。
13.根据权利要求1至8中任一项所述的组合物,其中所述基材包括铝合金、镁合金、钢合金、镍合金、钛合金、聚合物、纤维素材料、多糖或玻璃。
14.根据权利要求13所述的组合物,其中所述基材包括选自木材、人造丝和棉的纤维素材料。
15.根据权利要求14所述的组合物,其中所述基材是颗粒、粉末、挤出物、薄片或叶状结构。
16.根据权利要求15所述的组合物,其中所述基材包括小于约5mm的最大尺寸。
17.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料主要是结晶的。
18.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料包括每平方米投影基材面积约10m2至约1500m2的表面积。
19.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料包括每克陶瓷材料约15m2至约1500m2的表面积。
20.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料包括约2nm至约20nm的平均孔径。
21.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料包括具有多峰孔径分布的孔隙。
22.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料包括至多约50微米的厚度。
23.根据权利要求22所述的组合物,其中所述多孔陶瓷材料包括约0.2微米至约25微米的厚度。
24.根据权利要求22所述的组合物,其中所述多孔陶瓷材料包括大于约10%的孔隙率。
25.根据权利要求24所述的组合物,其中所述多孔陶瓷材料包括约30%至约95%的孔隙率。
26.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料包括如通过压汞孔隙率测定法测定的约100mm3/g至约7500mm3/g的空隙体积。
27.根据权利要求1至8中任一项所述的组合物,其中所述多孔陶瓷材料包括部分或完全填充有气体、液体或固体物质或其组合的可及孔隙体积。
28.根据权利要求27所述的组合物,其中所述多孔陶瓷材料包括部分或完全填充有第二陶瓷材料的孔隙。
29.根据权利要求28所述的组合物,其中所述第二陶瓷材料在组成上不同于所述互连陶瓷网络中的所述陶瓷。
30.根据权利要求29所述的组合物,其中所述互连陶瓷网络包括氢氧化物、氧化物或层状双氢氧化物,并且所述第二陶瓷材料包括磷酸盐、碳酸盐、硅酸盐、硫酸盐、钛酸盐、钨酸盐、锆酸盐、钒酸盐、锡酸盐、锌酸盐或铝酸盐。
31.根据权利要求28至30中任一项所述的组合物,其中所述互连陶瓷网络和第二陶瓷材料各自包含原生金属,并且其中所述互连陶瓷网络的原生金属和所述第二陶瓷材料的原生金属是相同的。
32.根据权利要求28至30中任一项所述的组合物,其包含所述互连陶瓷网络与第二陶瓷材料之间的界面,其中所述界面包含梯度。
33.根据权利要求32所述的组合物,其中所述梯度包括磷、碳、硅、硫、钨、钛、钒、锰、镁、锌、锡、锆或铝的梯度。
34.一种金属-陶瓷复合材料或聚合物-陶瓷复合材料,其包括基材的组件,其中所述基材中的每个用多孔陶瓷材料改性,所述多孔陶瓷材料包括与所述基材接触的互连陶瓷网络。
35.根据权利要求34所述的金属-陶瓷复合材料或聚合物-陶瓷复合材料,其中所述陶瓷改性基材的组件包括颗粒、粉末、薄片或挤出物,其各自包含小于约5mm的最大尺寸。
36.一种制造表面改性基材的方法,
其中包含互连陶瓷网络的多孔陶瓷材料沉积在金属或聚合物基材上,所述基材为金属或聚合物颗粒、粉末、挤出物或薄片的形式,从而产生表面改性的金属或聚合物基材,
其中所述表面改性的金属或聚合物基材被模制、铸造或烧结成整料或网状陶瓷或金属-陶瓷或聚合物-陶瓷复合材料部件
其中所述金属或聚合物基材芯包括比所述互连陶瓷网络更低的熔点,并且所述陶瓷足够多孔以芯吸熔融金属或聚合物和/或与所述熔融金属或聚合物反应。
37.根据权利要求36所述的制造方法,其中所述金属颗粒、粉末、挤出物或薄片包含铝、铝合金、镁、镁合金、锌、锌合金、钙或钙合金。
38.根据权利要求36所述的制造方法,其中所述聚合物颗粒、粉末、挤出物或薄片包括聚烯烃、聚酯、聚苯乙烯、聚酰胺、热塑性淀粉、丙烯酸或聚碳酸酯。
39.根据权利要求37或38所述的制造方法,其中所述陶瓷包括氧化镁、氧化钛、氧化锌、氧化锰、氧化锆、二氧化硅或碳酸钙。
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