CN111491751B - 功能复合粒子及其制备方法 - Google Patents

功能复合粒子及其制备方法 Download PDF

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CN111491751B
CN111491751B CN201780093300.0A CN201780093300A CN111491751B CN 111491751 B CN111491751 B CN 111491751B CN 201780093300 A CN201780093300 A CN 201780093300A CN 111491751 B CN111491751 B CN 111491751B
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functional
metal
metal particles
particle
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CN111491751A (zh
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袁安素
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Jiaxing Ode Medical Technology Co ltd
Nashi New Materials Co ltd
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Jiaxing Ode Medical Technology Co ltd
Nashi New Materials Co ltd
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Abstract

一种功能复合粒子及其制备方法。所述功能复合粒子(10)包括：内核(11)，该内核(11)由功能金属粒子构成，具有外表面(111)；以及壳层(12)，该壳层(12)为生物可相容陶瓷材料构成的物理气相沉积PVD陶瓷层，壳层(12)附着在内核(11)的外表面(111)，其中，壳层(12)为结晶结构从而允许内核(11)中的功能金属粒子的离子态经由晶界(121)缓释至壳层(12)外。通过PVD工艺将生物可相容陶瓷材料包裹在具有特定功能的功能金属粒子外表面(111)以形成功能复合粒子(10)，该功能复合粒子(10)中的功能金属粒子的离子态经由壳层(12)的晶界(121)实现缓释，从而延长了功能金属粒子的作用时间。

Description

功能复合粒子及其制备方法
技术领域
本发明涉及复合材料技术领域，特别涉及功能复合粒子及其制备方法。
背景技术
生物可相容陶瓷(Biocompatible ceramics)不仅具有陶瓷的力学相容性和稳定性，同时与生物组织之间具有亲和性和生物活性，可用于与人体或动物体相关的生物、医用、化学等领域。但是，单一的生物可相容陶瓷在实际应用中存在着一定的局限性。例如，当生物可相容陶瓷应用于人工关节时，容易引发细菌感染，更严重地，会导致骨骼局部的并发症。
将具有特定功能的金属粒子与生物可相容陶瓷结合是一种解决上述生物可相容陶瓷局限性的思路。例如，专利CN10293614A在陶瓷原料中掺入定量的金属银粉末，在常氧或增氧环境下烧结形成能够释放银离子的陶瓷，达到一定的抗菌作用。但是，在陶瓷的烧结过程中，过高的温度会使金属银很难处在固定位置，造成金属银与陶瓷材料在成品中分布不均匀，并且高温状态下的银也容易被环境中的氧气氧化，丧失银离子的抗菌作用。此外，金属银与陶瓷材料之间的结合力较弱，在具体的使用过程中，银离子的释放时间相对较短，难以达到持久的抗菌效果。
因此，现有的生物可相容陶瓷还有改进的空间。
发明内容
为改善现有生物可相容陶瓷的性能，提高其生物安全性和特定功能性，本发明的目的之一在于提供一种功能复合粒子及其制备方法。
根据本发明的一实施例，一种功能复合粒子，其包括内核和壳层，该内核由功能金属粒子构成并具有一外表面；该壳层为生物可相容陶瓷材料构成的物理气相沉积PVD陶瓷层，该壳层附着在该内核的外表面，其中，该壳层为结晶结构从而允许该内核中的功能金属粒子的离子态能通过晶界缓释至该壳层外。
本发明的另一实施例提供了功能复合粒子的制备方法，其包括如下步骤：采用蒸发冷凝工艺将由功能金属粒子组成的固体金属块体放入坩埚中，经由加热蒸发到真空物理气相沉积PVD工艺炉中冷凝；对冷凝状态下的功能金属粒子的外表面采用PVD工艺沉积由生物可相容陶瓷材料构成的PVD陶瓷层。
本发明的另一实施例还提供了功能复合粒子的用途，其中该功能复合粒子用于涂覆金属、布料、陶瓷或塑料的表面或植入在金属、布料、陶瓷或塑料中。
在本发明实施例中，通过物理气相沉积PVD工艺将生物可相容陶瓷材料包裹在具有特定功能的功能金属粒子外表面，形成功能复合粒子，一方面功能复合粒子的这种包覆结构可以避免功能金属粒子被外界的氧气氧化，另一方面，功能金属粒子的离子态可经由壳层的晶界实现缓释，从而延长了功能金属粒子的作用时间。
附图说明
图1所示是根据本发明一实施例的一功能复合粒子的金相图像；
图2所示是根据本发明一实施例的另一功能复合粒子的金相图像；
图3所示是图1所示的功能复合粒子的金相图像的局部放大图像；
图4所示是根据本发明一实施例的功能复合粒子的结构示意图。
具体实施方式
为更好的理解本发明的精神，以下结合附图和具体实施例对本发明实施例提供的功能复合粒子作进一步详细说明。根据以下说明及权利要求书，本发明实施例的优点和特征将更清楚。
需说明的是，图1-图3是使用电子显微镜拍摄得到的金相图像，图4中的示意图采用简化形式且使用非精准比例，仅用以方便、明晰地辅助说明本发明实施例。
具体地，图1所示是根据本发明一实施例的一功能复合粒子的金相图像。图2所示是根据本发明一实施例的另一功能复合粒子的金相图像。图3所示是图1所示的功能复合粒子的金相图像的局部放大图像。图4所示是根据本发明一实施例的功能复合粒子的结构示意图。
结合图1-图4，功能复合粒子10包括内核11和壳层12，其中内核11由功能金属粒子构成，具有外表面111。壳层12附着在内核11的外表面111上，是一种由生物可相容陶瓷材料构成的物理气相沉积PVD陶瓷层。
在本发明的一实施例中，内核11的功能金属粒子的粒径为5nm-5mm，壳层12为由Zr、Ti或Al构成的金属氧化物、金属氮化物中的一种或其混合物构成的生物可兼容陶瓷层，其厚度为5nm-50000nm，较佳为50nm-5000nm，表面硬度为1000HV-4500HV，较佳为3000HV-4000HV。
在本发明的一实施例中，壳层12为由ZrN、TiN、AlTiN或Al2O3构成的生物可相容陶瓷层。
在本发明的一实施例中，内核11的功能金属粒子是抗菌金属粒子，该抗菌金属粒子是Ag金属粒子、Zn金属粒子、Cu金属粒子或其混合物。
在本发明的另一实施例中，内核11的功能金属粒子是生长促进金属粒子，该生长促进金属粒子是Ca金属粒子、K金属粒子、Mg金属粒子或其混合物。
由图3和图4可看出，壳层12为结晶结构并具有晶界121，该晶界121为内核11中的功能金属粒子的离子态提供了通向壳层12外部的通道。在该功能复合粒子的使用过程中，由于壳层为结晶结构，内核11中的功能金属粒子会以离子态的形式经由晶界121缓慢释放到壳层12的外部。本发明提供的该功能复合粒子，包裹在内核11外表面111的壳层12可以有效阻止内核11中的功能金属粒子与外界的氧气接触，避免其过早地被氧化，另一方面，内核11中的功能金属粒子还可以通过壳层12的晶界121实现缓慢释放，延长了功能金属粒子的作用时间。
图1-图4所示的功能复合粒子10的制备方法包括如下步骤：
采用蒸发冷凝工艺将由功能金属粒子组成的固体金属块体放入坩埚中，经由加热蒸发到真空物理气相沉积PVD工艺炉中冷凝以形成内核11，该内核11具有外表面111；
对冷凝状态下的功能金属粒子(内核11)的外表面111采用PVD工艺沉积由生物可相容陶瓷材料构成的PVD陶瓷层以形成壳层12，该壳层12为结晶结构并具有晶界121，并且允许内核11中的功能金属粒子的离子态经由晶界121缓释至壳层11外。
在本发明的一实施例中，功能金属粒子冷凝后的粒径受加热源加热功率的影响。在本发明的一实施例中，使用电子枪作为加热源来加热功能金属粒子组成的固体金属块体，电子枪的电流强度范围为60A-300A，较佳为150A-250A。
在本发明的一实施例中，采用PVD工艺形成PVD陶瓷层的步骤包括：在真空物理气相沉积PVD工艺炉中通入纯度为99.999％的氮气或氧气，在偏压为0V-1000V的条件下，打开包含生物可相容陶瓷材料的靶，弧电流为120A-200A，采用PVD工艺将冷凝状态下的功能金属粒子的外表面沉积PVD陶瓷层。
本发明实施例可通过常规的PVD设备采用常规的PVD工艺形成壳层12。
本发明实施例中功能金属粒子的种类不同，对应获得的功能复合粒子具有不同的功能性。例如，Ag金属粒子、Zn金属粒子、Cu金属粒子或其混合物对应于抗菌功能复合粒子；Ca金属粒子、K金属粒子、Mg金属粒子或其混合物对应于生长促进功能复合粒子。
功能复合粒子可以进一步涂覆在金属、布料(纯棉、无纺布等)、陶瓷或塑料的表面。举例来说，功能复合粒子可涂覆在骨科器械、人工支架或人工关节等金属产品的表面形成抗菌涂层或生长促进涂层；可涂覆在塑料产品表面形成抗菌涂层；亦可涂覆在无纺布表面形成抗菌涂层等。
此外，功能复合粒子还可以植入在金属、布料、陶瓷或塑料中，直接形成具有特定功能的产品。
以下结合本发明的部分更优选实施例对其作进一步说明。
实施例1
采用蒸发冷凝工艺将Ag金属块体放入坩埚中，经由电子枪以电流强度200A加热蒸发到真空物理气相沉积PVD工艺炉中冷凝；
在真空PVD工艺炉中通入纯度为99.999％的氮气，在偏压为80V-100V的条件下，打开包含Ti的靶，弧电流为120A-200A，采用PVD工艺将冷凝状态下的Ag金属粒子的外表面沉积TiN陶瓷层，从而形成如图1所示粒径d1为68nm的TiN-Ag复合粒子粉末。
实施例2
采用蒸发冷凝工艺将Cu金属块体放入坩埚中，经由电子枪以电流强度200A加热蒸发到真空物理气相沉积PVD工艺炉中冷凝；
在真空PVD工艺炉中通入纯度为99.999％的氮气，在偏压为80V-100V的条件下，打开包含Ti的靶，弧电流为120A-200A，采用PVD工艺将冷凝状态下的Cu金属粒子的外表面沉积TiN陶瓷层，从而形成如图2所示粒径d2为154nm的TiN-Cu复合粒子粉末。
实施例3
采用蒸发冷凝工艺将Zn金属块体放入坩埚中，经由电子枪以电流强度200A加热蒸发到真空物理气相沉积PVD工艺炉中冷凝；
在真空PVD工艺炉中通入纯度为99.999％的氧气，在偏压为80V-100V的条件下，打开包含Al的靶，弧电流为120A-200A，采用PVD工艺将冷凝状态下的Zn金属粒子的外表面沉积TiN陶瓷层，从而形成具有生长促进效果的TiN-Zn复合粒子粉末。
实施例4
采用蒸发冷凝工艺将Mg金属块体放入坩埚中，经由电子枪以电流强度200A加热蒸发到真空物理气相沉积PVD工艺炉中冷凝；
在真空PVD工艺炉中通入纯度为99.999％的氮气，在偏压为80V-100V的条件下，打开包含AlTi的混合物的靶，弧电流为120A-200A，采用PVD工艺将冷凝状态下的Mg金属粒子的外表面沉积AlTiN陶瓷层，从而形成具有生长促进效果的AlTiN-Mg复合粒子粉末。
分别将上述实施例1-2中获得的功能复合粒子涂覆在塑料制品的表面，作为以下抗菌效果实验的样品。同时，取另一相同的塑料制品，表面不涂覆功能复合材料，作为对照样。测试方法：参考ISO22196:2011。
实验数据请参见表一和表二。
表一
Figure BDA0002371923860000051
表二
Figure BDA0002371923860000052
注：表格中的抗菌活性值为样品相对于对照样的抗菌活性值。
由表1-2可知，相较于没有涂覆本发明实施例1-2提供的功能复合粒子的塑料，经涂覆的塑料显然具有更高的抗菌性能。
本发明实施例通过PVD工艺将生物可相容陶瓷材料包裹在具有特定功能的功能金属粒子外表面以形成功能复合粒子，该功能复合粒子中的功能金属粒子的离子态经由壳层的晶界实现缓释，从而延长了功能金属粒子的作用时间。
本发明的技术内容及技术特点已揭示如上，然而熟悉本领域的技术人员仍可能基于本发明的教示及揭示而作种种不背离本发明精神的替换及修饰。因此，本发明的保护范围应不限于实施例所揭示的内容，而应包括各种不背离本发明的替换及修饰，并为本专利申请权利要求书所涵盖。

Claims (14)

1.一种功能复合粒子，其包括：
内核，所述内核由功能金属粒子构成，具有外表面；以及
壳层，所述壳层为生物可相容陶瓷材料构成的物理气相沉积PVD陶瓷层，所述壳层附着在所述内核的外表面，
其中，所述壳层为结晶结构从而允许所述内核中的功能金属粒子的离子态经由晶界缓释至所述壳层外。
2.根据权利要求1所述的功能复合粒子，其中所述功能金属粒子是抗菌金属粒子，所述抗菌金属粒子是Ag金属粒子、Zn金属粒子、Cu金属粒子或其混合物。
3.根据权利要求1所述的功能复合粒子，其中所述功能金属粒子是生长促进金属粒子，所述生长促进金属粒子是Ca金属粒子、K金属粒子、Mg金属粒子或其混合物。
4.根据权利要求1所述的功能复合粒子，其中所述功能金属粒子的粒径为5nm-5mm。
5.根据权利要求1所述的功能复合粒子，其中所述PVD陶瓷层为由Zr、Ti或Al构成的金属氧化物、金属氮化物中的一种或其混合物构成的生物可相容陶瓷层。
6.根据权利要求1所述的功能复合粒子，其中所述PVD陶瓷层为由ZrN、TiN、AlTiN或Al2O3构成的生物可相容陶瓷层。
7.根据权利要求1所述的功能复合粒子，其中所述PVD陶瓷层的厚度为5nm-50000nm，表面硬度为1000HV-4500HV。
8.一种功能复合粒子的制备方法，其包括如下步骤：
采用蒸发冷凝工艺将由功能金属粒子组成的固体金属块体放入坩埚中，经由加热蒸发到真空物理气相沉积PVD工艺炉中冷凝；
对冷凝状态下的功能金属粒子的外表面采用PVD工艺沉积由生物可相容陶瓷材料构成的PVD陶瓷层，其中所述PVD陶瓷层为结晶结构从而允许内核中的功能金属粒子的离子态经由晶界缓释至所述PVD陶瓷层外。
9.根据权利要求8所述的功能复合粒子的制备方法，其中所述功能金属粒子是抗菌金属粒子，所述抗菌金属粒子是Ag金属粒子、Zn金属粒子、Cu金属粒子或其混合物。
10.根据权利要求8所述的功能复合粒子的制备方法，其中所述功能金属粒子是生长促进金属粒子，所述生长促进金属粒子是Ca金属粒子、K金属粒子、Mg金属粒子或其混合物。
11.根据权利要求8所述的功能复合粒子的制备方法，其中所述PVD陶瓷层为由ZrN、TiN、AlTiN或Al2O3构成的生物可相容陶瓷层。
12.根据权利要求8所述的功能复合粒子的制备方法，其中藉由调整加热功率改变所述功能金属粒子冷凝后的粒径。
13.根据权利要求8所述的功能复合粒子的制备方法，其中采用PVD工艺形成所述PVD陶瓷层的步骤包括：在真空物理气相沉积PVD工艺炉中通入纯度为99.999％的氮气或氧气，在偏压为0V-1000V的条件下，打开包含生物可相容陶瓷材料的靶，弧电流为120A-200A，采用PVD工艺将冷凝状态下的所述功能金属粒子的外表面沉积所述PVD陶瓷层。
14.一种根据权利要求1-7中任一权利要求所述的功能复合粒子的用途，其用于涂覆金属、布料、陶瓷或塑料的表面或植入在金属、布料、陶瓷或塑料中。
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