CN100338258C - 用磷酸钙涂覆基质的方法 - Google Patents
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Abstract
本发明涉及一种用于用磷酸钙涂覆基质的方法。用已知方法不可能用磷酸钙涂覆温度敏感的基质或颗粒,或者需要多个涂覆工步。用新的方法应该可以对所有材料,包括对颗粒进行方便的涂覆。按照本发明为了涂覆将基质放入磷酸钙凝胶内,并使涂有凝胶的基质干燥。接着去除没有附着在基质上的磷酸钙颗粒。按照本发明也可以将基质加入含磷酸钙的SiO2胶体溶液内。然后使混合物的不断地运动,去除溶剂,并通过胶态SiO2在基质表面上浓缩使基质涂有磷酸钙层。涂覆的基质可以用作骨替代材料,特别是如果是涂覆的颗粒的话。
Description
技术领域
本发明涉及一种用于用磷酸钙层涂覆一多孔的基质的方法。
背景技术
为了特别是用一种生物活性的磷酸钙层例如烃基磷灰石涂覆基质,采用等离子喷射法。但是如果基质由小的颗粒组成或者不耐热,那么这种方法便不适用。对于颗粒同样也不能采用磷酸钙的电化学沉积,即使颗粒是导电的。
在US-PS6,153,266中说明了一种用来形成磷酸钙涂层的方法,其中在第一步骤中将基质浸入含磷酸盐溶液中,溶液不含钙,接着将基质从溶液中取出、干燥并浸入一ph值为8并且含钙的第二溶液,在这种溶液内在基质表面上形成磷酸钙。这种该法的缺点首先是,涂覆用两个步骤进行。另一个缺点是,用两工步法不可能形成在希望范围内的层厚,因此对于厚涂层已知方法还要设置另一个步骤,在该步骤内将涂有磷酸钙层的基质浸入磷酸钙溶液内。
发明内容
本发明的目的是,消除已知方法的缺点,并用一个简单的方法形成具有所希望层厚的磷酸钙涂层。
按本发明这个目的通过这样的方法实现,在该方法中进行以下步骤:
a)将基质加入含SiO2的磷酸钙凝胶或胶体溶液内,
b)通过施加负压除去处于基质上的空气,
c)对基质-凝胶混合物进行通风,
d)使涂有凝胶的基质干燥,
e)使磷酸钙与涂覆的基质分离。
这里,“凝胶”理解为一种糊状液体。
也可以通过将基质放入含磷酸钙的二氧化硅胶体内并然后通过去除溶剂产生一无裂缝的涂膜而将磷酸钙涂层直接涂在基质表面上。
本发明方法的优点是,可以在一个步骤内用磷酸钙涂覆基质。因为层厚取决于磷酸钙凝胶或胶体溶液的浓度,可以通过调整浓度产生希望的层厚。此方法适用于涂覆大面积基质和颗粒。它与基质由何种材料制成无关。通过这样的方法来提高涂层在基质上的附着牢固性,即通过施加负压去除去基质上的气体(空气)。如果基质具有小孔,那么这种方法特别有利。这样便从小孔中去除空气,磷酸钙凝胶可以渗入小孔内。另一个优点是,可以通过合适的凝胶成份形成由不同的磷酸钙形式组成的层。这特别是对于生物活性层有重要意义。众所周知,涂层生物活性的程度随其在生理学环境中的不稳定性而增长。具有与烃基磷灰石相比高得多的可溶性的磷酸钙如透钙磷石(Bruschit)及三斜磷钙石(Monetit)特别是对于骨骼的愈合阶段具有特别重要的意义。如果为了改善基质与骨组织的结合的目的而应该采用涂覆的颗粒,那么凝胶由透钙磷石和/或三斜磷钙石或者由透钙磷石和/或三斜磷钙石与烃基磷灰石混合物组成。所述凝胶也可由一种硅胶和磷酸钙的混合物组成。此外可含有填料,如硫酸钙或起骨诱导(knocheninduzieren)的作用的成分因子。也可以通过例如混合在凝胶内的方法,在涂层内加入药品,如抗生素、加速骨生长或阻止骨分解的药品。
用本发明方法涂覆的基质特别适合于用作骨替代材料,以填补骨缺损或填补植入物和植入物装入其内的骨之间的缝隙,这被认为是另一个优点。为此目的优先采用生物相容的涂覆的基质颗粒。颗粒也可以用来将植入物固定在骨内。
具体实施方式
下面借助于例子对本发明作较详细的说明,但本发明并不局限于此。
例1:
在不断搅拌的情况下将磷酸溶液加入氢氧化钙溶液内。通过离心法浓缩由此形成的细的沉淀物,并将其从浮在上面的清的溶液中分离出来。在这样得到的磷酸钙凝胶内加入事先去油脂和清洗过的钛颗粒,并充分混和。将此混合物放入负压室内。在施加合适的负压的情况下从钛颗粒小孔中去除空气。在接下来的通风时,磷酸钙凝胶渗入小孔内。将涂覆的颗粒干燥、分开(vereinzeln)并通过筛分与落下的磷酸钙颗粒分离。磷酸钙的涂层厚度是可变的,可通过生成的凝胶的浓度调整。
例2:
任意的磷酸钙粉末与一种硅胶混合。在该凝胶内加入去脂和清洗过的钛颗粒并充分混和。和例1中一样去除钛颗粒小孔中的空气。以便在通风时使磷酸钙-二氧化硅-凝胶能够渗入小孔内。使涂覆的颗粒干燥、分开,并借助于气流与沉积的磷酸钙-二氧化硅颗粒分离。磷酸钙-硅酸盐涂层厚度可通过凝胶浓度调整。
例3:
在一种烷氧基硅烷(例如TEOS)的水解产物的亲水胶体中加入任意一种磷酸钙粉末,并通过搅拌使其均匀分布。接着在继续搅拌的情况下在这种胶体溶液内加入一种任意颗粒大小的钛粉末或颗粒,在充分混和后开始在不断运动的情况下仔细地蒸馏掉溶剂。涂覆完成的特征是,实现了钛颗粒的可倾倒性,并直接在基质表面上形成一无裂纹的薄膜。最后将涂覆的基质在到150℃的多个级中进行热处理。
Claims (11)
1.用于用一磷酸钙层涂覆一基质的方法,其特征为,进行以下步骤:
f)将基质加入含SiO2的磷酸钙凝胶或胶体内,
g)通过施加负压除去处于基质上的空气,
h)对基质-凝胶混合物进行通风,
i)使涂有凝胶的基质干燥,
j)使磷酸钙颗粒与涂覆的基质分离。
2.按权利要求1所述的方法,其特征为:通过改变SiO2凝胶或胶体溶液的浓度确定涂层厚度。
3.按权利要求1所述的方法,其特征为:采用含小孔的基质。
4.按权利要求1所述的方法,其特征为:磷酸钙凝胶由透钙磷石和/或三斜磷钙石或透钙磷石和/或三斜磷钙石与烃基磷灰石的混合物组成。
5.按权利要求1所述的方法,其特征为:胶体溶液包含烃基磷灰石和/或β-磷酸三钙。
6.按权利要求1至5之一项所述的方法,其特征为:磷酸钙凝胶或胶体溶液包含骨诱导成分因子。
7.按权利要求1至5之一项所述的方法,其特征为:磷酸钙凝胶或胶体溶液包含药品。
8.按权利要求1的方法涂覆的基质。
9.按权利要求8所述的基质,其特征为:它由生物相容的基质颗粒组成。
10.按权利要求8所述的基质用作骨替代材料。
11.按权利要求8所述的基质用来将植入物固定在骨内。
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Application Number | Priority Date | Filing Date | Title |
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DE10161827A DE10161827A1 (de) | 2001-12-15 | 2001-12-15 | Verfahren zur Beschichtung eines Substrats mit Calciumphosphat |
DE10161827.1 | 2001-12-15 |
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CN1636080A CN1636080A (zh) | 2005-07-06 |
CN100338258C true CN100338258C (zh) | 2007-09-19 |
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EP (1) | EP1579028B1 (zh) |
JP (1) | JP4192101B2 (zh) |
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CA (1) | CA2470036C (zh) |
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US6558426B1 (en) | 2000-11-28 | 2003-05-06 | Medidea, Llc | Multiple-cam, posterior-stabilized knee prosthesis |
JP4493290B2 (ja) * | 2003-06-23 | 2010-06-30 | 菊治 山下 | 人工生体材料及びその製造方法 |
DE602005023509D1 (de) | 2004-11-16 | 2010-10-21 | 3M Innovative Properties Co | Dentalfüllstoffe, verfahren, zusammensetzungen mit einem caseinat |
JP5362991B2 (ja) | 2004-11-16 | 2013-12-11 | スリーエム イノベイティブ プロパティズ カンパニー | リン酸塩を含む歯科用充填剤および組成物 |
KR20070086324A (ko) | 2004-11-16 | 2007-08-27 | 쓰리엠 이노베이티브 프로퍼티즈 컴파니 | 칼슘과 인을 방출하는 유리를 함유한 치과용 조성물 |
CA2587556A1 (en) | 2004-11-16 | 2006-05-26 | 3M Innovative Properties Company | Dental fillers including a phosphorus containing surface treatment, and compositions and methods thereof |
KR100930279B1 (ko) * | 2007-06-20 | 2009-12-09 | 재단법인서울대학교산학협력재단 | 인산칼슘 극초박막 및 그의 제조법 |
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- 2002-12-06 US US10/498,732 patent/US7344749B2/en not_active Expired - Fee Related
- 2002-12-06 CA CA2470036A patent/CA2470036C/en not_active Expired - Fee Related
- 2002-12-06 CN CNB028251245A patent/CN100338258C/zh not_active Expired - Fee Related
- 2002-12-06 WO PCT/EP2002/013819 patent/WO2003052164A2/de active IP Right Grant
- 2002-12-06 AU AU2002361980A patent/AU2002361980B2/en not_active Ceased
- 2002-12-06 DE DE50211899T patent/DE50211899D1/de not_active Expired - Lifetime
- 2002-12-06 EP EP02796576A patent/EP1579028B1/de not_active Expired - Lifetime
- 2002-12-06 AT AT02796576T patent/ATE389043T1/de not_active IP Right Cessation
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EP0322250A1 (en) * | 1987-12-23 | 1989-06-28 | Sumitomo Chemical Company, Limited | Coating liquor containing hydroxyapatite and method for forming hydroxyapatite coating film using the same |
US5849569A (en) * | 1993-05-18 | 1998-12-15 | Millenium Biologix, Inc. | Assessment of bone cell activity |
CN1195336A (zh) * | 1995-09-01 | 1998-10-07 | 米列姆·贝尔罗吉克公司 | 特别适于维持骨细胞活性的人造稳定的磷酸钙相组合物 |
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WO2003052164A2 (de) | 2003-06-26 |
DE50211899D1 (de) | 2008-04-24 |
CA2470036C (en) | 2010-05-04 |
ATE389043T1 (de) | 2008-03-15 |
AU2002361980B2 (en) | 2007-05-10 |
US7344749B2 (en) | 2008-03-18 |
CN1636080A (zh) | 2005-07-06 |
CA2470036A1 (en) | 2003-06-26 |
DE10161827A1 (de) | 2003-06-26 |
EP1579028B1 (de) | 2008-03-12 |
JP2005519186A (ja) | 2005-06-30 |
JP4192101B2 (ja) | 2008-12-03 |
AU2002361980A1 (en) | 2003-06-30 |
US20050069629A1 (en) | 2005-03-31 |
WO2003052164A3 (de) | 2005-07-14 |
EP1579028A2 (de) | 2005-09-28 |
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