CN101314053A - 用于可植入假体的烧结涂层 - Google Patents
用于可植入假体的烧结涂层 Download PDFInfo
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- CN101314053A CN101314053A CNA200710305768XA CN200710305768A CN101314053A CN 101314053 A CN101314053 A CN 101314053A CN A200710305768X A CNA200710305768X A CN A200710305768XA CN 200710305768 A CN200710305768 A CN 200710305768A CN 101314053 A CN101314053 A CN 101314053A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F2/00—Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/002—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature
- B22F7/004—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature comprising at least one non-porous part
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Abstract
本发明涉及用于可植入假体的烧结涂层。具体而言,本发明尤其涉及具有承载着至少两层金属粒子层的外表面的制品,其中所述至少两层包括最外层和中间层;最外层基本由平均粒子尺寸为50到500微米的非球形金属粒子组成;中间层基本由平均粒子尺寸为50到500微米的大体为球形的金属粒子组成。在一些实施方案中,外表面具有约20%到约80%的体积孔隙率。
Description
技术领域
[001]本发明涉及用于可植入假体的烧结涂层,尤其涉及其中至少一层非球形金属粒子设置在球形金属粒子层之上的那些涂层。
背景技术
[002]有许多长久以来为部分骨替代植入体而探索的设计标准,包括(1)植入体应当持续到患者的生命而不丧失功能或者引发任何负面的过程反应(process response);(2)植入体应当恢复其所植入的骨的正常功能;并且(3)植入体应当能以商业规模生产。为满足上述标准,植入体不仅应当能承受所施加的通常具有波动性的负荷,而且植入体和骨之间的界面也应当能承受所述负荷需求。
[003]塑性水泥如聚甲基丙烯酸甲酯常用来将植入体固定到骨上以及改善植入体和骨之间的配合。植入体也具有多孔涂层,其与骨配合并引起骨向内生长,使得一段时间之后,假体与骨结构变成一个整体。典型的这种涂层公开在美国专利No.3855638;4206516;4156943;和4612160中。
[004]陶瓷涂层通常也具有良好的效果并且经常是特别理想的,这是由于骨和陶瓷材料例如氧化铝(Al2O3)之间的亲合力。典型的这种涂层公开在美国专利No.4145764和4483678中,它们尤其涉及了牙科植入体,以及美国专利No.4309488和4846837中,它们更广泛地公开了用于全身的可植入骨替代材料。
[005]其它研究工作在植入体上使用了高度回旋状的表面(convolutedSurface)。美国专利No.5368881和5658333揭示了使用非球形粉末来制造假体的粗糙表面。然而,已知这些表面几乎没有甚至没有相互连接的孔隙。
[006]在本领域中对具有改进性能的假体表面有不断的需求。
发明内容
[007]本发明的一个方面涉及具有载有至少两个金属粒子层的外表面的植入体和其它制品。在优选实施方案中,所述制品具有最外层以及设置在最外层和制品外表面之间的中间层。所述最外层基本上由平均粒子尺寸约50到500微米的非球形金属粒子组成。所述中间层基本上由平均粒子尺寸约50到500微米的大体上为球形的金属粒子组成。
[008]非球形金属粒子和球形金属粒子各自都可以独立地包含一种或多种金属,例如钴、铬、钼、钽和钛。在一些实施方案中,球形和非球形的金属粒子与其上设置它们的基材,即制品或至少它的外表面,具有相同的组成。在某些实施方案中,基材、球形金属粒子和非球形金属粒子包含钛,尽管在其它实施方案中它们包含钴和铬。
[009]基材可以包含一种或多种金属如钴、铬、钼、钽和钛。一些制品或假体使用与粒子组成不同的基材。在一些实施方案中,基材包含合金组合物(例如钛-6铝-4-钒)。
[010]在一些实施方案中,球形金属粒子层(多层)和非球形金属粒子层(多层)在基质之上有100微米到2.5mm的总厚度(combined thickness)。
[011]本发明还提供了制备本文所述涂层制品的方法。在某些实施方案中,该方法包括
提供基材;
在所述基材上设置一层或多层平均粒子尺寸约50-500微米的球形金属粒子层;
在所述至少一层或者多层球形金属粒子层上设置至少一层平均粒子尺寸为50-500微米的非球形金属粒子层;和
将所述粒子冶金烧结在基材上。
[0012]在一些方面,本发明涉及其中将金属粒子冶金烧结在固体金属基材表面上(或者植入体/制品表面上)的工艺。表面涂层可以产生高粗糙度、高孔隙的结构。在一些实施方案中,多孔涂层产生的体积孔隙率在约20%到约80%之间。在其它的实施方案中,孔隙率在约55%到约75%之间。
[013]本发明还涉及将本发明中的假体植入人体或动物体中的方法。所述植入通常包括将植入体放入骨内或骨附近。
附图说明
[0014]图1显示了髋部假体股骨部分的透视图。
[0015]图2显示了实施例1-4中所用-120+200目非球形粒子的扫描电子显微镜(SEM)图。
[0015]图3显示了实施例1-4中样品代表性区域在放大100倍下的SEM图。
[0016]图4显示了样品1-4的冶金制备的横截面光学显微照片。
[0017]图5显示了样品5-10的冶金法制备的横截面光学显微照片。
[0018]图6显示了样品11、15、19、23和27中的样品冶金制备的横截面光学显微照片。
具体实施方式
[0019]在本发明中,烧结金属涂层设置在基材上。特别地,所述涂层包含施加在基材至少一个表面上的对称粒子的第一部分和由非对称粒子制成并施加在涂层的所述第一部分上的涂层的第二部分。粒子层彼此冶金烧结并烧结在固体基材上。
[0020]本发明经涂布的表面适用于可植入的医疗器械。器械的植入通常包括将植入体放入骨中或骨附近。本发明的所述表面具有良好的粗糙度和孔隙性,使得器械较传统器械具有更优良的初始固定和更卓越的骨内生长。更优良的初始固定应该使得该器械的接受者更快地恢复。
[0021]可植入医疗器械包括可植入假体。例如本发明能应用到所有类型的可在体内任何位置结合到骨上的金属假体。可植入假体的例子包括面部骨、髋、膝或其它关节,以及牙科植入体。
[0022]通常,使用本领域公知的传统烧结技术将涂层施加在基材表面上(即制品或假体上,在一些实施方案中)。烧结可以在高温真空炉中进行。许多公司提供针对可以应用在本发明实践中的金属假体的涂布服务,包括Bio-Vac公司(Southfield,Mich.)、Hy-Vac Technologies公司(Detroit,Mich),和Astro Met,公司(Cincinnati,Ohio)。
[0023]在本发明中,涂层可通过一次或多次施加设置在表面上。第一粒子层(也可以称作粉末或珠粒)设置在基材表面上。这些第一粒子是球形的并且如果需要可以涂布多层。第二粒子层,非球形粒子,施加在第一粒子层上。第二粒子层如果需要也可以涂布为多层。
[0024]涂层包含生物相容性金属的烧结粒子,例如钴、铬、钼、钽、钛及其混合物。适合的金属例子包括纯钽、纯钛、钛合金(例如,Ti6Al4V;ASTM-F136),和钴-铬合金(例如,ASTM-F75)。在一些优选实施方案中,金属涂层和其下的假体具有相同的组成。
[0025]用在本发明中的一类粒子大体上为球形。也就是说,它们的横截面大体上是圆形。对于球形粒子来说,粒子直径(因此其尺寸)参照粒子表面上任意两点之间的最长弦来界定。这些球形粒子是金属的且粒子尺寸为50-500微米。在一些实施方案中,粒子尺寸为150-300微米。
[0026]本发明中使用的其它粒子具有不规则的形状。这些粒子大体上是非球形的,例如,这些粒子可以具有形状不规则的截面。截面可以是不规则的,纵横比(aspect ratio)不等于1。为便于引用,不规则形状的粒子本文中称为“非球形粒子”。非球形粒子的直径(因此其尺寸)由粒子能通过的最小孔的直径来界定。这些非球形粒子是金属的且粒子尺寸为50-500微米。在一些实施方案中,粒子尺寸为150-300微米。
[0027]球形和非球形粒子可具有单峰的或至少双峰的粒子尺寸分布。当使用至少双峰的粒子时,可以通过混合至少两组不同平均直径的筛选粒子来获得所述粒子。
[0028]通常,对称的和不对称的烧结粒子的层具有最少100微米的总厚度。在一些实施方案中,层的总厚度(combined thickness)至多2.5mm。在其它实施方案中,层的总厚度至多2.0mm。层可以由对称粒子和不对称粒子的任意组合制成,只要将对称粒子施加到基材上且将非对称粒子施加到对称粒子上即可。也就是说,基材表面应当主要与对称粒子接触。在一些实施方案中,基材上对称粒子与不对称粒子的厚度比为90∶10、80∶20、70∶30、60∶40、50∶50、40∶60、30∶70、20∶80或10∶90。
[0029]带有涂层表面的植入体的重要质量是涂层与其下面基材之间的结合强度。在基材界面的本涂层的结合强度使其能承受相当大的负荷而涂层不会损坏。特别地,结合的拉伸强度大于骨水泥和金属表面之间的拉伸强度。在一些实施方案中,结合强度至少为4000psi。
[0030]给出下述定义以充分理解文中所用的术语。
[0031]本文所用的术语“中间层”是指设置在基材和外层之间的层。
[0032]“金属粒子”也称作“金属粉末”。在对称粒子的情况下,它们也可称为“珠粒”。
[0033]术语“假体”旨在意指躯体一部分的人造替代品。假体可以是功能性的、装饰性的、或者是两者的结合。这种假体的一个实例是图1中图示的髋假体的股骨部分。在该图中,假体植入体20可根据本发明加以改进。为了说明,假体植入体20是股骨部分,包括拟纳入到大腿骨的骨髓腔中的柄(stem)22。因此,柄22是将植入体牢固结合到骨上的支撑构件。可以认识到,在一些实施方案中,柄22的至少一部分表面可以依本发明加以改进。尽管所描述的实施例涉及的是股骨部分,但可以认识到,本发明可应用到可在体内任意位置连接到骨上的任何假体植入体。植入体20可以由通常用作假体目的的任何生物相容性金属和合金组成,包括钛、钴、铬、钽和不锈钢。假体的实例包括但不仅限于面部骨、髋、膝或其它关节和牙科植入体。
[0034]当谈到表面“承载(bear)”金属粒子时,所述粒子被固定到表面上。固定粒子的方法例如烧结,是本领域的技术人员已知的。
[0035]当谈到层“基本由特殊类型的粒子组成”时,是指该层的多数粒子是那种类型。通常该层中粒子的至少90%或95%或99%是指定的类型。
[036]在一些实施方案中,在各珠粒层之间可能不存在离散的阻挡。然而,在这种情况下,涂层最外部分(或外层)的粒子包含大部分不规则的粒子且邻近基材(或中间层)的涂层部分的大部分粒子为球形。
[037]术语“基本上球形的粒子”指任意两点之间的弦变化小于20%的粒子。
[038]术语“基本上非球形的粒子”指其形状使它们落在上述“基本上球形的粒子”定义之外的粒子。
[039]本文中所用的的术语“至少双峰的尺寸分布”意指粒子数目和粒子直径的关系图中有至少两个可辨的峰。这样的关系图可以通过筛分技术很容易地构造以构造出柱状图或通过简单计算和测量涂层假体的代表性部分的粒子来构造。本文中,粒子直径定义为粒子表面上任意两点之间最长的弦。
[040]本发明由下面的实施例举例说明,但本意不是限定发明。
实施例1-4
[041]实施例1-4用在-120+200目或75-125μm非球形粒子之下的-60+80目或175-250μm球形粒子来制备。非球形粒子的形态如图2所示。
[042]样品涂布在一个平坦表面上以便于随后的分析。
[043]扫描电子显微镜(SEM)在烧结样品上扫描。四个样品的微观结构相当相似,实施例2和4似乎本质上更“密闭(closed)”,很难看到这两个样品下面的珠粒。每个样品的显微照片显示在图3中。多孔的涂布样品被垂直于涂层和基材小心地剖开,安装,并按冶金制备以供形貌评估。截面的光学显微照片显示在图4中。对样品的体积孔隙率,整体厚度,和孔的平均截取长度进行评估,作为评价孔尺寸的指标。
实施例编号 | -60+80球形粒子涂层 | -120+200非球形粒子涂层 | 体积孔隙率(%) | 厚度(mm) | 平均截取长度(μm) |
1 | 1 | 3 | 49.2 | 0.64 | 127.8 |
2 | 1 | 4 | 52.8 | 0.66 | 120.2 |
3 | 2 | 2 | 45.2 | 0.74 | 143.4 |
4 | 2 | 3 | 53.1 | 0.89 | 108.2 |
[044]定性来说,本工艺生产的涂层较传统微珠多孔涂层粗糙得多。和传统使用的珠粒多孔涂层相比,细小的粉末使整体的孔尺寸更小,体积孔隙率没有显著增加。
实施例5-10
[0045]实施例5-10采用-60+80目球形粒子和-50+60目、-60+80目、-70+80和/或-80+100目的非球形粒子制备。该粉末显示出与初始粉末相似的形态,只是尺寸上更大。样品涂布在一个平坦表面上以便于随后的分析。样品按下面表格中所示加以涂布,涂层按顺序从左至右施加。带多孔涂层的烧结样品垂直于涂层和基材小心地剖面,安装,并冶金制备以供形态评估。所选剖面的光学显微照片显示在图5中。对样品的体积孔隙率和总厚度进行评估。
实施例编号 | -60+80球形粒子涂层 | -60+80非球形粒子涂层 | -50+60非球形粒子涂层 | -70+80非球形粒子涂层 | -80+100非球形粒子涂层 | 体积孔隙率(%) | 厚度(mm) |
5 | 1 | 2 | 1 | 63.2 | 0.86 | ||
6 | 1 | 2 | 1 | 59.2 | 1.02 | ||
7 | 1 | 2 | 57.0 | 1.02 | |||
8 | 1 | 2 | 55.5 | 0.81 | |||
9 | 1 | 2 | 60.4 | 0.81 | |||
10 | 1 | 2 | 1 | 57.1 | 1.37 |
[0046]对实施例5-10的粗糙度定性评估表明粒子尺寸越大,涂层的总体粗糙度越大。初始体积孔隙率结果也表明粒子越大,孔隙率越高,至少与前面用在实施例1-4中的-120+200目的粒子相比是这样。
实施例11-30
[0047]实施例11-30用-60+80目球形粒子和在-50+80目内不同尺寸分布的非球形粒子制备。该粉末显示出与初始粉末相似的形态。样品涂布在一个平坦表面上以便于随后的分析。样品按下面表格中所示加以涂布,球形粒子施加到金属基材上且非球形粒子施加在球形粒子之上。带多孔涂层的烧结样品垂直于涂层和基质小心地剖面,安装,并冶金制备以供形态评估。代表性剖面的光学显微照片显示在图6中。对样品的体积孔隙率、总厚度和孔的平均截取长度(average pore intercept length)进行评价。
概括地说,本发明具体体现在以下方面:
1、假体,具有承载至少两层金属粒子层的外表面,其中:
所述的至少两层之一是最外层,基本上由平均粒子尺寸为50到500微米的大体上非球形的金属粒子组成;和
所述至少两层中的至少一层是中间层,其设置于所述最外层和所述外表面之间且基本由平均粒子尺寸为50到500微米的大体球形的金属粒子组成。
2、方面1中的所述假体,其中球形金属粒子的平均粒子尺寸为150-300微米。
3、方面1中的所述假体,其中非球形金属粒子的平均粒子尺寸为150-300微米。
4、方面1中的所述假体,其中所述非球形金属粒子包含钴、铬、钼、钽和钛中的一种或多种。
5、方面1中的所述假体,其中所述球形金属粒子包含钴、铬、钼、钽和钛中的一种或多种。
6、方面1中的所述假体,其中所述表面、所述球形金属粒子和所述非球形金属粒子包含钛。
7、方面1中的所述假体,其中所述表面、所述球形金属粒子和所述非球形金属粒子包含钴和铬。
8、方面1中的所述假体,其中所述表面、所述球形金属粒子和所述非球形金属粒子包含钽。
9、方面1中的所述假体,其中球形金属粒子层和非球形金属粒子层的总厚度为100微米到2.5毫米。
10、方面1中的所述假体,其中所述外表面的体积孔隙率在约20%到约80%之间。
11、一种制品,具有承载至少两层金属粒子层的外表面,其中:
所述至少两层包含最外层和中间层;
所述最外层基本由平均粒子尺寸为50到500微米的非球形金属粒子组成;和
所述中间层基本由平均粒子尺寸为50到500微米的大体球形的金属粒子组成。
12、方面11中所述的制品,其中球形金属粒子平均粒子尺寸为150-300微米和非球形金属粒子平均粒子尺寸为150-300微米。
13、方面11中所述的制品,其中所述非球形金属粒子和球形金属粒子各自包含钴、铬、钼、钽和钛中的一种或多种。
14、方面11中所述的制品,其中所述基材、所述球形金属粒子和所述非球形金属粒子包含钛。
15、方面11中所述的制品,其中所述基材、所述球形金属粒子和所述非球形金属粒子包含钴和铬。
16、方面11中所述的制品,其中所述基材、所述球形金属粒子和所述非球形金属粒子包含钽。
17、方面11中所述的制品,其中球形金属粒子层和非球形金属粒子层在所述基材上的总厚度为100微米到2.5毫米。
18、方面11中所述的制品,其中外表面的体积孔隙率在约20%到约80%之间。
19、一种方法,包括:
提供基材;
在所述基材上施加一层或多层大体为球形的金属粒子涂层,所述球形金属粒子平均粒子尺寸为50到500微米;
在所述球形金属粒子上施加一层或多层另外的涂层,所述另外的涂层包含平均粒子尺寸为50到500微米的非球形金属粒子;和
将所述粒子冶金烧结在所述基材上。
20、方面19中所述的方法,其中球形金属粒子的平均粒子尺寸为150-300微米和非球形金属粒子的平均粒子尺寸为150-300微米。
21、方面19中所述的方法,其中非球形金属粒子和球形金属粒子各自都包含钴、铬、钼、钽和钛中的一种或多种。
22、方面19中所述的方法,其中该基材、球形金属粒子和非球形金属粒子各自包含钛。
23、方面19中所述的方法,其中该基材、球形金属粒子和非球形金属粒子各自包含钴和铬。
24、方面19中所述的方法,其中该基材、球形金属粒子和非球形金属粒子各自包含钽。
25、方面19中所述的方法,其中球形金属粒子层和非球形金属粒子层的总厚度为100微米到2.5毫米。
26、在将假体植入人体或动物体中与骨接触的方法中,改进之处包括与所述骨接触的所述假体的至少一部分具有承载着至少两层金属粒子层的表面,其中:
所述至少两层包含最外层和中间层;
所述最外层基本由平均粒子尺寸为50到500微米的非球形金属粒子组成;和
所述中间层基本由平均粒子尺寸为50到500微米的大体球形金属粒子组成。
27、方面26中所述的方法,其中球形金属粒子的平均粒子尺寸为150-300微米和非球形金属粒子的平均粒子尺寸为150-300微米。
28、如方面26中所述的方法,其中非球形金属粒子和球形金属粒子各自都包含钴、铬、钼、钽和钛中的一种或多种。
[0048]在之前的详细说明中,参照具体的实施方案已经对概念进行了说明。很多方面和实施方案前面已做了阐述并只是作为典型示例而非限定。阅读了本说明书后,本领域的技术人员能认识到其它方面和实施方案在不脱离本发明范围的情况下也是可行的。此外,本领域普通技术人员能认识到,在不脱离如下所列权利要求限定的本发明范围的情况下,可进行各种改进和改变。因此,说明书和附图认为是示例而非限制意思,且所有这种修改都包括在本发明的范围之内。
[0049]上文已经就具体实施方案对益处、其它优势、和问题的解决方案进行了阐述。然而,益处、优势、问题的解决方案以及可以使这些发生或者使其变得更显著的任何技术特征都不应理解成是任何或所有权利要求的关键、必需,或必要的特征。
[0050]可以认识到,某些技术特征,为清楚起见,在单独实施方案中进行了说明,但也可以在单一实施方案中组合出现。反过来,为简洁起见,在一个实施方案内容中进行阐述的各种特征,也可以单独地或者组合地提供。此外,对范围内数值的引用包括该范围内的每一个值。
Claims (10)
1、假体,具有承载着至少两层金属粒子的外表面,其中:
所述至少两层中的一层是最外层,其基本上由平均粒子尺寸为50到500微米的大体为非球形的金属粒子组成;和
所述至少两层中的至少一层是中间层,其设置在所述最外层和所述外表面之间且基本由平均粒子尺寸为50到500微米的大体为球形的金属粒子组成。
2、如权利要求1所述的假体,其中所述球形金属粒子的平均粒子尺寸为150-300微米。
3、如权利要求1所述的假体,其中所述非球形金属粒子的平均粒子尺寸为150-300微米。
4、如权利要求1所述的假体,其中所述非球形金属粒子包含钴、铬、钼、钽和钛中的一种或多种。
5、如权利要求1所述的假体,其中所述球形金属粒子包含钴、铬、钼、钽和钛中的一种或多种。
6、如权利要求1所述的假体,其中所述表面、所述球形金属粒子和所述非球形金属粒子包含钛。
7、如权利要求1所述的假体,其中所述表面、所述球形金属粒子和所述非球形金属粒子包含钴和铬。
8、如权利要求1所述的假体,其中所述表面、所述球形金属粒子和所述非球形金属粒子包含钽。
9、如权利要求1所述的假体,其中所述球形金属粒子层和非球形金属粒子层的总厚度为100微米到2.5毫米。
10、如权利要求1所述的假体,其中所述外层具有约20%到约80%的体积孔隙率。
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EP (1) | EP1997524B1 (zh) |
JP (1) | JP5179169B2 (zh) |
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- 2007-12-29 DE DE602007004956T patent/DE602007004956D1/de active Active
- 2007-12-29 ES ES07255083T patent/ES2340961T3/es active Active
- 2007-12-29 EP EP07255083A patent/EP1997524B1/en active Active
- 2007-12-29 DK DK07255083.3T patent/DK1997524T3/da active
- 2007-12-29 AT AT07255083T patent/ATE458505T1/de active
- 2007-12-29 CN CN200710305768XA patent/CN101314053B/zh active Active
- 2007-12-31 AU AU2007254712A patent/AU2007254712B2/en active Active
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102639084A (zh) * | 2009-10-22 | 2012-08-15 | 德普伊国际有限公司 | 医用植入装置 |
CN102639084B (zh) * | 2009-10-22 | 2015-04-01 | 德普伊国际有限公司 | 医用植入装置 |
CN110084814A (zh) * | 2019-05-13 | 2019-08-02 | 苏州微创关节医疗科技有限公司 | 表面涂层测量方法、装置、计算机设备和存储介质 |
CN110084814B (zh) * | 2019-05-13 | 2021-11-02 | 苏州微创关节医疗科技有限公司 | 表面涂层测量方法、装置、计算机设备和存储介质 |
CN116036385A (zh) * | 2023-03-31 | 2023-05-02 | 艾柯医疗器械(北京)股份有限公司 | 一种自膨式编织植入物及其制备方法及包含其的血流导向系统 |
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EP1997524B1 (en) | 2010-02-24 |
AU2007254712A1 (en) | 2008-12-18 |
JP2008296005A (ja) | 2008-12-11 |
CN101314053B (zh) | 2013-05-08 |
JP5179169B2 (ja) | 2013-04-10 |
AU2007254712B2 (en) | 2013-04-04 |
EP1997524A1 (en) | 2008-12-03 |
DE602007004956D1 (de) | 2010-04-08 |
ATE458505T1 (de) | 2010-03-15 |
DK1997524T3 (da) | 2010-05-31 |
ES2340961T3 (es) | 2010-06-11 |
ZA200800058B (en) | 2009-09-30 |
US20080300682A1 (en) | 2008-12-04 |
US8066770B2 (en) | 2011-11-29 |
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