CN103703165B - 控制合金颗粒的腐蚀速率的方法、具有受控腐蚀速率的合金颗粒和包含该颗粒的制品 - Google Patents
控制合金颗粒的腐蚀速率的方法、具有受控腐蚀速率的合金颗粒和包含该颗粒的制品 Download PDFInfo
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Abstract
一种复合颗粒，包含核，沉积在该核上的遮蔽层，并进一步包含在该遮蔽层与该核的界面处形成的层间区域，该层间区域具有低于该核的反应性，且该遮蔽层具有低于该层间区域的反应性，不同于该遮蔽层并沉积在该遮蔽层上的金属层，该金属层具有低于该核的反应性，和任选地，沉积在该金属层上的粘合金属层。
Description
相关申请的交叉引用
本申请要求2011年7月29日提交的美国申请号13/194271的权益，其通过引用以全文并入本文。
背景技术
某些井下作业涉及将元件在井下环境中的放置，在那里该元件发挥其作用，并随后将之移除。例如，诸如球/球座组件和压裂（frac）塞的元件是用于密封井眼中的下部区域以进行水力压裂过程（在本领域中也称为“液压破裂”）来破碎储集岩的不同区域的井下元件。在液压破裂操作后，随后移除球/球座或塞以使流体流至压裂的岩石或使流体从压裂的岩石流出。
球和/或球座以及压裂塞（frac plug）可以由可腐蚀材料形成，使得无需将它们完整地从井下环境中物理移除。以此方式，当涉及球/球座或压裂塞的操作完成时，该球、球座和/或压裂塞腐蚀掉。否则，井下制品可能不得不在井中停留比该操作所需更长的一段时间。
为了便利去除，此类元件可以由与周围的井下环境反应的材料形成，使得它们无需通过例如机械操作物理去除，而是可以在井下条件下腐蚀或溶解。但是，虽然可以通过调节合金组成来控制例如用于制备可腐蚀制品的合金的腐蚀速率，但控制井下制品的腐蚀速率的替代方式是需要的。
可腐蚀材料可包括在盐水电位序方面具有高活性的那些，如为腐蚀速率而调节的镁合金。已经发现，调节镁合金中痕量污染物的量可对此类合金的腐蚀速率具有显著影响（Song,G.和Atrens,A.,“Understanding Magnesium Corrosion:A Framework forImproved Alloy Performance”,Adv.Eng.Mater.2003,5(12)第837-858页）。例如，可以向镁中添加金属诸如镍、铁、铜、钙等以提高腐蚀速率，且可以添加其它金属例如锆、钇等以降低腐蚀速率。平衡此类添加剂的量以实现所需体腐蚀速率可以以此方式控制由该合金制成的制品的整体腐蚀；但是，这种方法需要多个批次的合金的制备，要求高的批次间再现性，和该合金中金属添加剂或污染物的准确的、可再现的控制。
因此仍然需要控制用于井下制品的镁合金的整体腐蚀速率，而无需合金组成的精细调节并具有改进的腐蚀控制。
发明概述
在一个实施方案中，通过复合颗粒克服现有技术的上述和其它缺陷，所述复合颗粒包含核、沉积在该核上的遮蔽层，并进一步包含在该遮蔽层与该核的界面处形成的层间区域，该层间区域具有低于该核的反应性，且该遮蔽层具有低于该层间区域的反应性，不同于该遮蔽层并沉积在该遮蔽层上的金属层，该金属层具有低于该核的反应性，以及任选地，沉积在该金属层上的粘合金属层。
在另一实施方案中，复合颗粒包含镁-铝合金核、包含沉积在该核上的含铝层的遮蔽层，并进一步包含层间区域，所述层间区域包含在该镁合金核与该含铝层之间的界面处形成的α-Mg和γ-Mg17Al12，并进一步包含氧化铝、氧化镁或包含这些氧化物的至少一种的组合的夹杂物，沉积在该遮蔽层上的金属层，该金属层包含Ni、Fe、Cu、Co、W、其合金或包含前述的至少一种的组合，沉积在该金属层上的含铝遮蔽层，以及任选地，含铝粘合金属层，其中该层间区域、遮蔽层、金属层和任选的粘合金属层彼此相互分散。
在另一实施方案中，公开了对在含水电解质中的复合颗粒的调节腐蚀速率的方法，该复合颗粒具有核、沉积在该核上的遮蔽层，并进一步包含在该遮蔽层与该核的界面处形成的层间区域，该层间区域具有低于该核的反应性，且该遮蔽层具有低于该层间区域的反应性，与该遮蔽层不同并沉积在该遮蔽层上的金属层，该金属层具有低于该核的反应性，以及任选地，沉积在该金属层上的粘合金属层，该方法包括选择该金属层使得相对于遮蔽层该金属层的反应性越低，该腐蚀速率越高，并选择该遮蔽层与金属层的量、厚度或量和厚度使得相对于金属层该遮蔽层的量、厚度或量和厚度越小，该腐蚀速率越高。
附图概述
现在参照附图，其中相同元件在多幅图中标记为相同：
图1显示了具有多层结构的复合颗粒100a的横截面图（图1A）和具有相互分散的层的复合颗粒100b的横截面图（图1B）；
图2显示了具有多层结构的复合颗粒200a的横截面图（图2A）和具有相互分散的层的复合颗粒200b的横截面图（图2B）；及
图3显示了由复合颗粒310制备的示例性可腐蚀井下制品300的横截面图。
发明详述
本文中公开的是可对于制造可腐蚀制品有用的复合颗粒。该复合颗粒具有经涂覆的遮蔽层（例如铝）、高反应性材料（例如镁或镁合金）的核的多层结构。在该遮蔽层与该核的界面处可以形成且在不连续区域中存在金属间相，例如镁和铝的晶态金属化合物。包括该金属间区域的遮蔽层具有设置在其上的具有较低反应性（即比遮蔽层更惰性，尽管在反应性方面可与金属间相相比）的惰性材料层。可以在惰性材料层上方设置额外的粘合金属例如铝的层，以在模制时提供颗粒之间的粘合。该层间区域、遮蔽层、惰性材料层（当该惰性材料是金属时在本文中称为“金属层”）以及任选的粘合层被认为彼此相互分散，并形成在组成上不同的外壳，该外壳也与该核相互分散。
该惰性材料层（其相对于核材料具有较低的反应性）充当阴极，而由反应性比贵金属层更高的金属例如镁制成的核相对于该贵金属层是阳极的。包括金属间相的该遮蔽层相对于该核也是阴极的，但是相对于该贵金属层是阳极的。在电解质的存在下在相对阳极和相对阴极的材料之间发生电流放电循环（例如腐蚀）。通过相对于核和遮蔽层调节该贵金属层的组成，并通过调节该遮蔽层和贵金属层的量和/或厚度，调节该复合颗粒的腐蚀速率。
通过使用例如冷模制接着锻制将该颗粒压制并成形，将该复合颗粒成形为制品。
该核包括适于用在井下环境中的任何材料，如果该核在井下环境中相对于具有不同反应性的第二材料是可腐蚀的。在一个实施方案中，该复合颗粒由此包括含镁的核。含镁的核包括在腐蚀性环境（包括在井下一般会遇到的那些环境）中可腐蚀的任何此类合金，例如包括盐（即盐水）、或酸性或腐蚀性试剂例如硫化氢、盐酸或其它此类腐蚀性试剂的水性环境。适于使用的镁合金包括镁（Mg）与铝（Al）、镉（Cd）、钙（Ca）、钴（Co）、铜（Cu）、铁（Fe）、锰（Mn）、镍（Ni）、硅（Si）、银（Ag）、锶（Sr）、钍（Th）、锌（Zn）、锆（Zr）或包含这些元素的至少一种的组合的合金。特别有用的合金包括镁合金颗粒，其包括由与Ni、W、Co、Cu、Fe或其它金属合金化的镁制备的那些。可以以不同的量包括合金化或痕量元素以调节镁的腐蚀速率。例如，这些元素的四种（镉、钙、银和锌）对腐蚀速率具有轻度至中度的加速效应，而另外四种（铜、钴、铁和镍）对腐蚀具有更高的加速效应。包括上述合金化元素的不同组合以实现不同程度的耐腐蚀性的示例性的市售镁合金包括但不限于例如与铝、锶和锰合金化的镁，例如AJ62、AJ50x、AJ51x和AJ52x合金，以及与铝、锌和锰合金化的镁，包括AZ91 A-E合金。
将理解，具有大于上述示例性合金的腐蚀速率的合金也预期在本文中是有用的。例如，已经发现，当以小于或等于约0.5重量%、特别是小于或等于约0.4重量%且更特别小于或等于约0.3重量%的量包括时，镍可对于降低镁合金的耐腐蚀性（即提高腐蚀速率）是有用的，以提供可对于该可腐蚀井下制品有用的腐蚀速率。在另一实施方案中，该含镁的核包含镁-铝合金。
该镁合金核的粒度可以为约50至约150微米（μm），更特别为约60至约140微米，且更特别为约70至约130微米。有用的镁合金可以包括在200（93℃）下使用3重量%的KCl水溶液足以实现约0.1至约20mg/cm2/小时、特别地约1至约15mg/cm2/小时的镁合金核的腐蚀速率的上述元素和/或污染物的组合。
该复合颗粒包括遮蔽层。该遮蔽层通过在该核上沉积具有比该核反应性更低的材料来形成。在一个示例性实施方案中，该遮蔽层是沉积在该核上的含铝层。在一个实施方案中，该核是镁合金核，且该遮蔽层是含铝层。如本文中所用，“在……上”和“沉积在……上”指的是层可以与或不与施加该层的下方表面直接接触，除非另行规定为该层至少部分接触。要进一步理解的是，当对于方法使用时，“沉积”表示沉积的作用，而“沉积的”当在组合物或制品的上下文中使用时仅仅表示该层对基底的并置关系，并且不表示沉积的过程。该遮蔽层进一步包含在该核与遮蔽层的界面处形成的层间区域，其在组成上来自于该核与遮蔽层。在一个实施方案中，该层间区域在含镁的核与含铝遮蔽层的边界处形成，并且该层间区域包含金属间化合物。例如，镁-铝合金包括α-Mg相，且此外包括在Mg-Al合金中在晶界处聚积的γ-Mg17Al12金属间相。该金属间γ-Mg17Al12相通常以小于该Mg-Al合金的30重量%的量存在。取决于组成，还可以存在附加相，包括固溶体Al，以及其它金属间相，例如β-Mg2Al3。在含铝遮蔽层的沉积时，该γ-Mg17Al12相形成并在该遮蔽层与含Mg核的界面处聚积。热处理可以加速该层间区域的形成。例如，在低于共晶点的温度下（例如低于或等于约450℃，取决于合金组成，且只要不超过共晶点）加热约15分钟可以在该含Mg核与含Al层的界面处形成金属间相。该复合颗粒由此包括金属间化合物γ-Mg17Al12作为该层间区域的一部分。该层间区域在含Mg核与含Al层的整个接触面积上方或在接触面积的一部分上方形成。可以调整沉积方法和任何热处理，使得金属间相插在Mg合金核与含Al层的一部分接触表面之间。该遮蔽层进一步包括该核和/或遮蔽层所包含的一种或多种金属的氧化物。例如，当该核包含镁或镁-铝合金且该遮蔽层包含铝时，该遮蔽层任选地包括镁（如氧化镁）、铝（如氧化铝）或包含前述的至少一种的组合的氧化物。
该复合颗粒进一步包括不同于该遮蔽层并沉积在该遮蔽层上的金属层。基于由较低反应性（即更接近惰性金属）至高反应性（即较不接近惰性金属）的盐水电位序，该金属层相对于该核具有较低的反应性。在一个实施方案中，用于该金属层的金属当在电化学电池中用作阴极时允许形成氢。该金属层由此包含第6-11族的过渡金属。具体地，第6-11族的过渡金属包括Ni、Fe、Cu、Co、W、其合金或包含前述的至少一种的组合。
该复合颗粒任选包括沉积在该金属层上的粘合层。该粘合层包含促进复合颗粒之间粘合的材料。示例性粘合层包括铝或铝合金。在压制和锻制涂有该粘合层的复合颗粒以形成模制制品时，该颗粒经粘合层材料通过颗粒间接触彼此粘结以便向该制品进一步提供机械强度。
所述层（遮蔽层、金属层和任选的粘合层）可以各自具有约0.05至约0.15微米、特别是约0.07至约0.13微米的平均厚度。在一个实施方案中，各层不完全覆盖在下方的层，并且层覆盖由此是不连续的。此外，当该层在另一层“上”时，可以存在层界面处的间隙空间。在一个实施方案中，该层间区域、遮蔽层、金属层和任选的粘合金属层彼此相互分散。如本文中所用的，“相互分散”指的是两个或多个相邻层以密切混合物形式相互渗透到彼此中或彼此相互渗透穿过，其中将理解两个（或更多个）相互分散的层因一个层互渗到相邻层中而具有平均组成梯度。
该核与遮蔽层、遮蔽层与金属层、和金属层与任选的粘合层各自由此相互部分接触，并且相互分散，使得该核、该遮蔽层与该金属层的组分存在于该复合颗粒的暴露表面处。
在一个实施方案中，该复合颗粒具有在200（93℃）下使用3重量%的KCl水溶液的约0.1至约20mg/cm2/小时、特别是约1至约15mg/cm2/小时的腐蚀速率。
在一个特定实施方案中，该遮蔽层是含铝层，该核是含镁核。在一个实施方案中，该遮蔽层包含铝。在另一个实施方案中，该遮蔽层除铝之外进一步包含氧化铝、氧化镁或包含这些氧化物的至少一种的组合的夹杂物。该遮蔽层进一步包括在该镁合金核与该第一含铝层之间的界面处形成的层间区域。在一个实施方案中，该层间区域包含γ-Mg17Al12。
还在一个特定实施方案中，该金属层在该遮蔽层上包含第6-11族过渡金属。该第6-11族过渡金属包括Ni、Fe、Cu、Co、W、其合金或包含前述的至少一种的组合。
任选地，在一个具体实施方案中，该粘合层是沉积在该金属层上的含铝层。
遮蔽层、金属层和粘合层在该核上的沉积不受特别限制。当遮蔽层和/或任选的粘合层包括铝或铝合金时，在一个示例性实施方案中，通过在将有机金属化合物，如三乙基铝（在50毫米汞柱下具有128-130℃的沸点）引入到含有镁合金核颗粒的流化床反应器中之后分解该有机金属化合物以沉积该遮蔽层，或将该有机金属化合物引入含有镁合金核/遮蔽层/金属层颗粒的反应器中以沉积该粘合层，在一个示例性实施方案中实现在镁合金核颗粒上均匀沉积铝层。通过在低于全部或部分复合颗粒的熔点的温度下的热处理，例如烧结和/或退火，和/或锻制由该复合颗粒模制的制品，在该Mg合金核与该遮蔽层的界面处进一步形成在这种情况下包括金属间化合物例如γ-Mg17Al12的该层间区域。
类似地，沉积均匀金属层也不受特别限制，并可以通过例如在将有机金属化合物引入含有涂有该遮蔽层的镁合金核颗粒的流化床反应器中之后分解该有机金属化合物（当金属层为镍时，例如羰基镍）来实现。
还可以使用物理混合法采用遮蔽层、金属层和任选的粘合层的材料涂覆该核。例如，通过低温研磨、球磨等将该核与该遮蔽层、金属层和任选的粘合层的一种或多种组分混合。以此方式，可以依次包括该遮蔽层、金属层和粘合层组分，或者可以同时包括两个层或所有三个层的组分。包括气相沉积与物理法的沉积法的组合也可用于提供该复合颗粒。但通过物理混合同时包括所有组分时，将理解，形成作为遮蔽层、金属层和粘合层组分的复合的单个层。
在另一实施方案中，该核包含第一核材料的内核和第二核材料的外核，内核材料具有比外核更低的反应性。内核是可用于在其上沉积高反应性材料例如镁的任何材料，没有限制。该内核由此可以是任何合适的低反应性材料，例如第6-11族过渡金属，包括Ni、Fe、Cu、Co、W、其合金或包含前述的至少一种的组合；金属氧化物，例如氧化铝、氧化硅、硅酸盐、铁氧化物、氧化钛、钨酸盐等；聚合物，包括酚聚合物；陶瓷；玻璃；或其它此类材料。在一个示例性实施方案中，该内核包含铝合金、镍、铁、氧化铝、氧化钛或氧化硅，外核包含如上文所述的镁或镁合金。使用任何合适的沉积法，例如在流化床反应器中金属镁或镁合金的物理气相沉积（PVD），在内核上沉积外核。随后采用如上所述的遮蔽层、金属层和任选的粘合层涂覆具有内核和外核的该核结构以形成该复合颗粒。
该复合颗粒通常具有约50至约150微米（μm）、更特别约60至约140μm的粒度。
在另一实施方案中，公开了调节复合颗粒或由此制备的制品的腐蚀速率的方法。在一个实施方案中，通过选择金属层组成以具有所需反应性来实现该调节，其中金属层相对于遮蔽层（以及通过定义，相对于该核与层间区域）的反应性越低，腐蚀速率越快；并且相反，金属层相对于遮蔽层的反应性越高，腐蚀速率越慢。作为替代或补充，在一个实施方案中，通过对金属层的任何给定的量和/或厚度提高该遮蔽层的量和/或厚度来实现调节。进一步要理解，通过该核、层间区域、遮蔽层和金属层的相互分散程度实现对腐蚀速率的附加控制，其中这些层的相互分散程度越高，腐蚀速率越大，且相反，层的相互分散程度越低，腐蚀速率越慢。因此，本文中所使用的量和厚度相关之处在于，以基于复合颗粒重量的重量百分比表示的层的量越高，该厚度越大。
该复合颗粒的表面包括相互分散的层的阳极和阴极区域。将理解，“阳极区域”和“阴极区域”是基于相互分散的材料的相对反应性的相对术语。例如，如上所述，镁（来自该核）相对于层间区域的阴极金属间化合物（γ-Mg17Al12）和来自层间区域/遮蔽层的阴极铝是阳极的，并且相对于来自阴极金属层的镍是阳极的。类似地，金属间化合物（γ-Mg17Al12）相对于来自该遮蔽层的阴极铝是阳极的，相对于来自阴极金属层的镍是阳极的；且来自遮蔽层的铝相对于来自该金属层的镍是阳极的。
以此方式，在将复合颗粒（和由该复合颗粒制成的任何制品）的表面暴露于电解质时，发生多种局部腐蚀机制，其中发生阳极和阴极区域的反转。例如，在暴露的阳极核材料（例如镁）被腐蚀后，此前为阴极的材料（例如金属间化合物或遮蔽层中的铝）变成阳极的，并且通过与更阴极的金属层（例如，其包括镍等）的相互作用被腐蚀。当该表面腐蚀并暴露更阳极的核材料例如镁时，情况再次逆转，铝或金属间化合物对该核材料变成阴极的。
当腐蚀在电解质流体（水、盐水等）的存在下在阳极与阴极区域之间的表面上的局部区域中发展时，这些区域（在本文中称为微电池）可以在该复合颗粒表面上方向外腐蚀，并与其它微电池连接以形成更大的腐蚀区域，当其它阳极材料例如镁（来自该核）或金属间γ-Mg17Al12（来自该层间区域/遮蔽层）暴露时，该腐蚀区域又与其它腐蚀区域等连接。在这些区域腐蚀之后，来自该核的新的下方的阳极材料暴露于该电解质。在腐蚀时，这些相互分散的层由此可以变得对该电解质流体可渗透。这允许电解质流体渗透到腐蚀表面中以渗入和侵蚀该层，并且重复该过程，直到可腐蚀材料被消耗。将理解，金属氧化物在核/遮蔽层界面处的存在还通过充当惰性屏障降低了界面处该核的腐蚀速率，并由此影响了微电池的相对阳极/阴极特性（例如，当在镁核与金属间化合物之间存在氧化铝和/或氧化镁时，该金属间化合物与该核隔绝，并相对于该金属层将是阳极的）。以此方式，金属氧化物夹杂物的存在影响了复合颗粒的整体腐蚀速率。
当该核包含内核和外核（其中外核为阳极的）时，腐蚀会发展直到仅剩下内核。由此暴露的内核不再具有复合颗粒的结构完整性与粘结性，并以颗粒的悬浮体形式分散到周围的流体中，并可以以此方式除去。
因此，在一个实施方案中，调节复合颗粒中的腐蚀速率的方法包括选择该金属层使得该金属层相对于该遮蔽层的反应性越低，该腐蚀速率越高。在另一实施方案中，调节复合颗粒中的腐蚀速率的方法包括选择该遮蔽层与该金属层的量、厚度或者量和厚度使得该遮蔽层的量、厚度或者量和厚度相对于该金属层越小，该腐蚀速率越高。该层间区域、遮蔽层、金属层和任选的粘合金属层彼此相互分散，并具有如上所述的组成。
在另一实施方案中，一种制品包含以粉末或其它合适形式如预压缩丸粒形式提供的该复合颗粒。可以通过压缩或以其它方式成型该复合颗粒以形成具有合适形状的制品由该复合颗粒制备制品。例如，在约40至约80ksi（约275至约550MPa）下使用等静压机通过冷压将该复合颗粒模制或压缩成所需形状，接着锻制或烧结和机加工以提供具有所需形状与尺寸的制品。如本文中公开的那样，在低于该组分熔点的温度下进行锻制或烧结。
因此，成形制品的方法包括模制该复合颗粒并锻制该模制制品。
由此制备的制品称为受控电解材料（CEM）制品，并在井下条件下是有用的。制品包括例如球、球座、压裂塞或其它此类井下制品。但是，应当理解的是，尽管公开了这些制品，对于粉末形式的该复合颗粒存在其它用途。例如，该复合颗粒可以包括在非金属的基质中，并可以以涂层（例如涂料、粉末涂层等）形式施加到表面上，其中在水的存在下，且优选在水加电解质的存在下发生受控电解过程。此类过程可以包括用于海事应用如钻架、船壳或船体、水下工具或其它此类应用的涂层。此类电解材料可以提供牺牲层以缓解或防止下面的金属层的腐蚀，或者可以防止例如海洋生物粘结到涂有该复合颗粒的水下表面上。
本文中描述了一种示例性用途。图1以示意性横截面显示了复合颗粒100a和100b的不同结构变体。在图1A中，该复合颗粒100a包括核110；包括金属间区域121（重虚线）和包围该金属间区域的铝层122的遮蔽层120；金属层130，和任选地，充当粘合层的第二铝层140。可以包括这种粘合层140以便当压缩在一起以形成成形制品时促进颗粒的粘合。将理解，该层当显示为不连续的核-壳层时还可以在界面处相互混合和/或该层在施加它们的表面上可以是不连续的，使得核110实际上与遮蔽层120和/或金属层130和/或粘合层140接触。
在图1B中，复合颗粒100b具有核110和相互分散的层150，该层150包括层间区域、遮蔽层、金属层和任选的粘合层的组分（在图1B中没有单独显示）。将理解，这种相互分散的结构可以来自于如图1A中所描述的不连续的核-壳结构，并且其中通过热处理（例如烧结）提高相互分散；或者该相互分散的结构可以来自于形成该颗粒的物理方法（例如低温研磨或球磨），或通过在层形成期间将超过一个层的前体材料包括到流化床反应器中。该相互分散的层150与同等地遍及相互分散层150分布的不同层（层间区域、遮蔽层、金属层）的组分均匀地相互分散，或者例如以梯度不均匀地分布，其中该组成由相互分散的层150与核110的界面处的主要为层间区域的组成改变为相互分散层150外表面处的主要为粘合层的组成。
类似于图1，图2显示了复合颗粒200a和200b的不同结构变体的横截面图。在图2A中，该复合颗粒200a包括核210，所述核210包含内核211和外核212；遮蔽层220，其包括金属间区域221（重虚线）和包围该金属间区域的铝层222；金属层230，以及任选地，充当粘合层的第二铝层240。如在图1A中那样，将理解，该层当显示为不连续的核-壳层时还可以在界面处相互混合和/或该层在施加它们的表面上可以是不连续的。
在图2B中，复合颗粒200b具有包含内核211和外核212的核210，以及包括层间区域、遮蔽层、金属层与任选的粘合层的组分（在图2B中未单独显示）的相互分散的层250。如在图1B中那样，将理解，此类相互分散的结构可以来自于不连续的核-壳结构、来自于研磨以形成该颗粒、或通过在层形成期间将超过一个层的前体材料包括到流化床反应器中。同样如图1B中，相互分散的层250的组成均分分布，或不均匀分布，例如以梯度形式。
在图3中，作为示例性制品，显示球体300。在图3中，球体300由复合颗粒310组成。在冷压以形成球体300期间，将粉末状复合颗粒310压缩和成形以形成具有间隙空间320的球状球体300，其中，通过锻制和/或烧结进一步减少间隙空间320的体积，以将压制后约20%的自由体积减少至锻制/烧结后的小于约5%、特别是小于约3%、更特别小于约1%。当与球座（未显示）结合使用并安置在球座中以防止流体流过该球/球座时，球体300形成用于隔离例如位于球/球座组件下方的压裂区的井下密封。
虽然已经显示和描述了一个或多个实施方案，但可以不偏离本发明的精神与范围而对其进行修改和替换。因此，要理解，通过解释而非限制的方式描述了本发明。
本文中公开的所有范围包括端点，该端点可以相互独立地组合。本文中所用后缀“（s）”意在包括其修饰的术语的单数与复数，由此包括至少一个该术语（例如，着色剂(s)包括至少一种着色剂）。“任选的”或“任选地”指的是随后描述的事件或情况可能发生或可能不发生，并且该描述包括其中该事件发生的例子和其中该情况没有发生的例子。本文中所用的“组合”包括共混物、混合物、合金、反应产物等。所有参考文献经引用并入本文。
在描述本发明的上下文中（尤其在下面的权利要求书中）使用术语“一个”和“该”以及类似所指对象应解释为覆盖单数和复数，除非在本文中另行说明或与上下文明显矛盾。此外，还要注意，术语“第一”、“第二”等在本文中不表示任何次序、数量或重要性，而是用于区分一个元素与另一个元素。与数量结合使用的修饰词“约”包括所述值，并具有上下文所指示的含义（例如，其包括与特定量的测量相关的误差程度）。
Claims (21)
1.一种复合颗粒，包含：
核，
沉积在该核上的遮蔽层，并进一步包含在该遮蔽层与该核的界面处形成的层间区域，该层间区域具有低于该核的反应性，且该遮蔽层具有低于该层间区域的反应性，
不同于该遮蔽层并沉积在该遮蔽层上的金属层，该金属层具有低于该核的反应性，和
任选地，沉积在该金属层上的粘合金属层，
其中所述核、遮蔽层、金属层和任选的粘合金属层是不连续的。
2.权利要求1的复合颗粒，其中该核包含镁，该遮蔽层包含铝，以及任选地，铝、镁或包含前述的至少一种的组合的氧化物，并且该层间区域包含金属间化合物。
3.权利要求2的复合颗粒，其中该金属间化合物是γ-Mg17Al12。
4.权利要求1的复合颗粒，其中该金属层包含第6-11族过渡金属。
5.权利要求4的复合颗粒，其中第6-11族过渡金属包含Ni、Fe、Cu、Co、W、其合金或包含前述的至少一种的组合。
6.权利要求1的复合颗粒，其中该核包含第一核材料的内核和第二核材料的外核，该内核材料具有比外核更低的活性。
7.权利要求6的复合颗粒，其中该内核包含铝，且该外核包含镁。
8.权利要求1的复合颗粒，其中该核包含镁-铝合金。
9.权利要求1的复合颗粒，其中该核与遮蔽层、遮蔽层与金属层、和金属层与任选的粘合金属层各自相互部分接触，使得该核、遮蔽层与金属层的组分存在于该复合颗粒的暴露表面处。
10.权利要求1的复合颗粒，其中该层间区域、遮蔽层、金属层和任选的粘合金属层彼此相互分散。
11.权利要求1的复合颗粒，其中该遮蔽层相对于该核是阴极的，且相对于该金属层是阳极的。
12.一种复合颗粒，包含：
镁-铝合金核，
包含沉积在该核上的含铝层的遮蔽层，进一步包含在该镁-铝合金核与该含铝层之间界面处形成的包含γ-Mg17Al12的层间区域，并进一步包含氧化铝、氧化镁或包含这些氧化物的至少一种的组合的夹杂物，
沉积在该遮蔽层上的金属层，该金属层包含Ni、Fe、Cu、Co、W、其合金或包含前述的至少一种的组合，
沉积在该金属层上的含铝遮蔽层，和
任选地，含铝粘合金属层，
其中，该层间区域、遮蔽层、金属层和任选的粘合金属层彼此相互分散。
13.调节复合颗粒在含水电解质中的腐蚀速率的方法，所述复合颗粒具有：
核，
沉积在该核上的遮蔽层，并进一步包含在该遮蔽层与该核的界面处形成的层间区域，该层间区域具有低于该核的反应性，且该遮蔽层具有低于该层间区域的反应性，
不同于该遮蔽层并沉积在该遮蔽层上的金属层，该金属层具有低于该核的反应性，和
任选地，沉积在该金属层上的粘合金属层；
该方法包括选择该金属层使得相对于该遮蔽层该金属层的活性越低，腐蚀速率越高，和
选择该遮蔽层与金属层的量、厚度或量和厚度，使得相对于该金属层该遮蔽层的量、厚度或量和厚度越低，腐蚀速率越高。
14.权利要求13的方法，其中该层间区域、遮蔽层、金属层和任选的粘合金属层彼此相互分散。
15.权利要求13的方法，其中该核包含镁，该遮蔽层包含铝、以及氧化铝、氧化镁或包含前述氧化物的至少一种的组合的夹杂物，并且该层间区域包含γ-Mg17Al12。
16.权利要求13的方法，其中该金属层包含第6-11族过渡金属。
17.权利要求16的方法，其中该金属层包含Ni、Fe、Cu、Co、W、其合金或包含前述的至少一种的组合。
18.形成制品的方法，包括模制权利要求1的复合颗粒，并锻制该模制制品。
19.包含权利要求1的复合颗粒的制品。
20.权利要求19的制品，其中该制品包括球、球座或压裂塞。
21.包含权利要求1的复合颗粒的涂层。
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|---|---|---|---|
| US13/194,271 US9643250B2 (en) | 2011-07-29 | 2011-07-29 | Method of controlling the corrosion rate of alloy particles, alloy particle with controlled corrosion rate, and articles comprising the particle |
| US13/194,271 | 2011-07-29 | ||
| PCT/US2012/047163 WO2013019409A2 (en) | 2011-07-29 | 2012-07-18 | Method of controlling the corrosion rate of alloy particles, alloy particle with controlled corrosion rate, and articles comprising the particle |
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| EP (1) | EP2737108B1 (zh) |
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| DK2737108T3 (da) | 2019-11-04 |
| AU2012290564B2 (en) | 2017-02-16 |
| WO2013019409A2 (en) | 2013-02-07 |
| US20130029886A1 (en) | 2013-01-31 |
| BR112014001466A2 (pt) | 2017-02-21 |
| EP2737108B1 (en) | 2019-08-21 |
| EP2737108A4 (en) | 2015-08-05 |
| US9643250B2 (en) | 2017-05-09 |
| US20160207106A1 (en) | 2016-07-21 |
| CN103703165A (zh) | 2014-04-02 |
| US10092953B2 (en) | 2018-10-09 |
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