CN101070441A - Anti-bacterial carboxy apatite composite coating, its preparing method and use - Google Patents
Anti-bacterial carboxy apatite composite coating, its preparing method and use Download PDFInfo
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- CN101070441A CN101070441A CN 200710042106 CN200710042106A CN101070441A CN 101070441 A CN101070441 A CN 101070441A CN 200710042106 CN200710042106 CN 200710042106 CN 200710042106 A CN200710042106 A CN 200710042106A CN 101070441 A CN101070441 A CN 101070441A
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Abstract
This invention relates to one kind of the antibacterial hydroxyl apatite compound coat, the preparation method and the application, its characteristic is the related compound coat is composed of the metal silver powder and the hydroxyl apatite powder, the metal silver powder is treated as the antibacterial increase ingredient, the silver powder' quality accounts for 1-5% of the compound coat, the particle size of the silver powder is 20-100mum, the particle size of the hydroxyl apatite powder is 10-100mum. This invention making the compound coat is realized by using the spray technics of the vacuum plasma. The provided compound coat has an above 95% excellent antibacterial effect on the coliform, the green pus pseudomonad and the golden yellow staphylococcus, and the cytotoxic rank in vitro of the compound coat is zero, has no cytotoxicity.
Description
Technical field
The present invention relates to a kind of anti-bacterial carboxy apatite composite coating, preparation method and application, relate to preparation-antimicrobial form plasma spraying carboxy apatite composite coating, preparation and the application of an antibiotic bone substitution material or rather, belong to the medical bio field of ceramic coatings.
Background technology
Hydroxyapatite have with human body bone and tooth in similar chemical constitution and the crystalline structure of main mine material, be the main inorganic composition of body bone tissue, be typical biological active materials.But the hydroxylapatite ceramic mechanical property is relatively poor, and its bending strength and fracture toughness property index all are lower than the human body dense bone, is difficult to use at human body carrying position.The deposited hydroxyl apatite ceramic coating can overcome the fragility of hydroxyapatite body material on metals such as titanium (alloy) matrix, gives full play to the high strength and the high tenacity of metal alloy, improves the supporting capacity of implant.Simultaneously, the biological activated energy that hydroxyapatite is good makes implant and osseous tissue good binding.Using plasma spraying method, the hydroxyapatite coating layer for preparing on matrixes such as titanium alloy are one of most widely used clinically artificial bone replacement materials, have been widely used in hip prosthesis and tooth root planting body etc.
Bone substitution material is in the implant surgery process, and bacterial infection accounts for suitable ratio.Normal use various microbiotic, the problem of infectation of bacteria when solving operation, but increased the resistance of bacterial antibiotic at the microbial film that implant surface forms, cause the microbiotic drug effect to reduce.In order more effectively to protect from infection, loading antiseptic-germicide on the bone implant material surface is a kind of comparatively effective means.Silver is a kind of the most frequently used inorganic antiseptic, has advantages such as efficient, safety, broad-spectrum antimicrobial, is widely used in the antimicrobial prod.
The present invention is antiseptic-germicide with silver powder, and hydroxyapatite is a preparing carriers germ resistance biological coating.
Summary of the invention
Based on advantages such as efficient, the safety of good biological activity of hydroxyapatite and silver, broad-spectrum antimicrobials, the present invention adopts powder dry blending method to prepare the mixed powder of hydroxyapatite and silver, utilize the vacuum plasma spray technology, the blended powder is deposited on the metal base, thereby prepares hydroxyapatite bioactive coating with anti-microbial property.
Specific embodiment of the present invention is as follows: taking by weighing hydroxylapatite powder and the particle diameter that particle diameter is 10～100 μ m by a certain percentage is the silver powder of 20～100 μ m, and ball milling is done and mixed the mixed powder of making silver content 1-5wt% in 2 hours.Adopt vacuum plasma spray technology, under optimized parameters (table 1) condition mixed powder is being deposited on the metallic matrix (as titanium alloy) that cleans with sandblast.
Table 1 spray parameters scope
| Plasma gas Ar/slpm | 38～45 | Powder feeding rate/g/ |
10～30 |
| Plasma gas H 2/slpm | 7～16 | Vacuum tightness/mbar | 100～300 |
| Powder carrier gas Ar/slpm | 2.0 | Electric current/A | 550～650 |
| Spray distance/mm | 200～300 |
Slpm: standard liter/min
Prepared hydroxyapatite-silver-colored compound coating not only has good biological activity, but also has antibiotic resistance performance.The silver ions release test of compound coating in buffered soln shows that silver ions has certain slow-release function (Fig. 1).The closely connected method antibacterial tests of film finds that the antibiotic rate of compound coating increases (Fig. 2) with the increase of silver content.The vitro cytotoxicity test shows that significant cytotoxicity does not appear in the carboxy apatite composite coating that silver content is not more than 5wt%.The toxicity rank of the composite hydroxylapatite coating layer of the argentiferous 5wt% that the MTT colorimetry detects is 0, and the cell pattern is seen Fig. 3.Prepared compound coating to the antibiotic rate of intestinal bacteria, Pseudomonas aeruginosa and streptococcus aureus greater than 95% excellent antibiotic rate (seeing embodiment for details)
Description of drawings
The silver ions release concentration of hydroxyapatite coating layer in buffered soln of the different silver contents of Fig. 1.
The hydroxyapatite coating layer of the different silver contents of Fig. 2 is cultivated antibiotic rate behind the 24h to intestinal bacteria, Pseudomonas aeruginosa and streptococcus aureus.
Cellular form in hydroxyapatite coating layer (HA5) the vitro cytotoxicity test of Fig. 3 MTT colorimetry detection argentiferous 5wt%.
Bacterium colony photo behind Fig. 4 HA, HA1 and the HA3 test specimen surface 24h culturing bacterium.
Embodiment
Further illustrate characteristics of the present invention and effect below by embodiment.Limit the present invention absolutely not.
Embodiment 1:
Take by weighing the powder of 59.40 gram hydroxyapatites and 0.60 gram silver, taking by weighing 60 by 2: 2: 1 ratio again, to restrain diameters be the zirconia ball of 2mm, 3mm, 6mm, and in the ball milling bottle of packing into, ball milling is 2 hours on ball mill, makes the hydroxyapatite powder of argentiferous 1wt%.Adopt the vacuum plasma spray technology, with the spraying parameter of table 2, the spraying mixed powder is on the Ti-6Al-4V matrix that cleans with sandblast.The HA1 compound coating that makes of method is respectively 97%, 98% and 98% to the antibiotic rate of intestinal bacteria, Pseudomonas aeruginosa and streptococcus aureus thus.The bacterium colony photo is seen Fig. 4 behind the 24h culturing bacterium of test specimen surface.According to regulation among the standard GB 15979-1995 " product antibacterial and bactericidal property and stability test method ", bacteriostasis rate 〉=50% can report that product has bacteriostatic action, and the HA1 compound coating has good antibacterial effect to positive bacterias such as Gram-negative bacterias such as intestinal bacteria, Pseudomonas aeruginosa and streptococcus aureuses as can be known.The vitro cytotoxicity rank that the MTT colorimetry detects HA1 is 0, shows no cytotoxicity.
Table 2 spray parameters
| Plasma gas Ar/slpm | 40 | Powder feeding rate/g/ |
20 |
| Plasma gas H 2/slpm | 8 | Vacuum tightness/mbar | 100 |
| Powder carrier gas Ar/slpm | 2.0 | Electric current/A | 550 |
| Spray distance/mm | 280 |
Slpm: standard liter/min
Embodiment 2:
Adopt the carboxy apatite composite coating HA3 for preparing argentiferous 3wt% with top identical method.The HA3 compound coating is respectively 99%, 99% and 99% to the antibiotic rate of intestinal bacteria, Pseudomonas aeruginosa and streptococcus aureus.The bacterium colony photo is seen Fig. 4 behind the 24h culturing bacterium of test specimen surface.The result shows that the HA3 compound coating has better antibacterial effect to positive bacterias such as Gram-negative bacterias such as intestinal bacteria, Pseudomonas aeruginosa and streptococcus aureuses.The vitro cytotoxicity rank that the MTT colorimetry detects HA3 is 0, shows no cytotoxicity.
The preparation silver content is the carboxy apatite composite coating HA5 of 5wt%, and its preparation method is with embodiment 1, and antibacterial tests, toxicity test etc. are as Figure 1-3.
Claims (9)
1, a kind of anti-bacterial carboxy apatite composite coating is a matrix with Ti-6Al-4V, it is characterized in that described compound coating is made up of argent powder and hydroxyapatite powder; The argent powder is as antibiotic added ingredients, and the quality percentage composition of silver powder in compound coating is 1%-5%.
2, by the described anti-bacterial carboxy apatite composite coating of claim 1, the particle diameter that it is characterized in that described argent powder is 20-100 μ m.
, by the described anti-bacterial carboxy apatite composite coating of claim 1, the particle diameter that it is characterized in that described hydroxyapatite powder is 10-100 μ m.
4, preparation is characterized in that as the method for each described anti-bacterial carboxy apatite composite coating among the claim 1-3 preparation process is:
(a) hydroxyapatite powder and silver powder are mixed in proportion, do through ball milling and mix, the quality percentage composition of making silver powder is the mixed powder of 1-5%;
(b) adopt vacuum plasma spray coating technology, under the following processing parameter condition mixed powder is being deposited on the titanium alloy substrate that cleans with sandblast; Described spraying parameter is that plasma Ar gas flow is 38-45slpm, plasma H
2Gas flow is 7-16slpm, and powder carrier gas Ar gas flow is 2.0slpm, and powder feeding rate is 10-30g/min, and spraying vacuum tightness is 100-300mbar, and spray distance is 200-300mm; Slpm represents standard liter/min.
5, by the preparation method of the described anti-bacterial carboxy apatite composite coating of claim 4, use the grating zirconia ball when it is characterized in that argent powder and hydroxyapatite mixed powder ball milling, described zirconia ball diameter is respectively 2mm, 3mm and 6mm; Corresponding mass ratio is 2: 2: 1.
6, by the preparation method of the described anti-bacterial carboxy apatite composite coating of claim .4, electric current is 550A～650A when it is characterized in that spraying.
7, by the preparation method of the described anti-bacterial carboxy apatite composite coating of claim .4, it is characterized in that spraying parameter in the step (b) be plasma Ar airshed be 40 standards/minute; Plasma H
2Gas flow is 8 standard liter/min, and the mixed powder carrier gas flux is 2.0 standard liter/min, and powder feeding rate is 20g/min, and vacuum tightness is 100mbar, and spray distance is 280mm.
8, by the application of each described anti-bacterial carboxy apatite composite coating among the claim 1-3, it is characterized in that compound coating to the antibiotic rate of intestinal bacteria, Pseudomonas aeruginosa and streptococcus aureus greater than 95%, demonstrate excellent antibacterial effect.
9, by the application of each described anti-bacterial carboxy apatite composite coating in the claim 8, the vitro cytotoxicity rank that it is characterized in that compound coating is 0, no cytotoxicity.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417741A (en) * | 2011-05-24 | 2012-04-18 | 周君琳 | Design and preparation of iodine antibacterial hydroxyapatite coating titanium and titanium alloy implants |
| CN102677125A (en) * | 2012-06-13 | 2012-09-19 | 西北有色金属研究院 | Preparation method of active antibacterial composite coating on surface of titanium and titanium alloy medical instrument |
| CN103027077A (en) * | 2011-09-29 | 2013-04-10 | 钱陈慧贤 | Antibacterial product containing ceramic and silver mixed powder and preparation method of antibacterial product |
| CN103981519A (en) * | 2014-05-30 | 2014-08-13 | 山东大学 | Method for laser cladding of wollastonite-based bioactive ceramic coating on surface of titanium alloy |
| CN104127914A (en) * | 2014-07-29 | 2014-11-05 | 复旦大学附属华山医院 | Preparation method of HAp blended silver and copper antibacterial composite coating |
| CN104388874A (en) * | 2014-10-14 | 2015-03-04 | 中国科学院上海硅酸盐研究所 | Silver doped alumina ceramic coating and its making method |
| CN107638591A (en) * | 2016-07-20 | 2018-01-30 | 中国科学院上海硅酸盐研究所 | A kind of good ceria doped hydroxyapatite coating of biological antioxidant performance and its application |
| CN111334746A (en) * | 2020-04-26 | 2020-06-26 | 广州珈鹏科技有限公司 | Biological ceramic coating with antibacterial activity and preparation method thereof |
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| CN1267006C (en) * | 2002-09-06 | 2006-08-02 | 清华大学 | Silver-carried fluor apatite antimicrobials and its preparation method |
| TW200510065A (en) * | 2003-09-11 | 2005-03-16 | Ryuzaburo Hanawa | Anti-contaminant coating material |
| KR20060056093A (en) * | 2004-11-19 | 2006-05-24 | 학교법인연세대학교 | Silver incorporated calcium phosphate film and method for preparing the same |
| CN100336450C (en) * | 2005-09-22 | 2007-09-12 | 上海交通大学 | Prepn process of nanometer composite silver carrying hydroxyapatite/titania disinfectant |
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2007
- 2007-06-15 CN CNB2007100421068A patent/CN100549109C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417741A (en) * | 2011-05-24 | 2012-04-18 | 周君琳 | Design and preparation of iodine antibacterial hydroxyapatite coating titanium and titanium alloy implants |
| CN103027077A (en) * | 2011-09-29 | 2013-04-10 | 钱陈慧贤 | Antibacterial product containing ceramic and silver mixed powder and preparation method of antibacterial product |
| CN102677125A (en) * | 2012-06-13 | 2012-09-19 | 西北有色金属研究院 | Preparation method of active antibacterial composite coating on surface of titanium and titanium alloy medical instrument |
| CN102677125B (en) * | 2012-06-13 | 2014-12-17 | 西北有色金属研究院 | Preparation method of active antibacterial composite coating on surface of titanium and titanium alloy medical instrument |
| CN103981519A (en) * | 2014-05-30 | 2014-08-13 | 山东大学 | Method for laser cladding of wollastonite-based bioactive ceramic coating on surface of titanium alloy |
| CN104127914A (en) * | 2014-07-29 | 2014-11-05 | 复旦大学附属华山医院 | Preparation method of HAp blended silver and copper antibacterial composite coating |
| CN104388874A (en) * | 2014-10-14 | 2015-03-04 | 中国科学院上海硅酸盐研究所 | Silver doped alumina ceramic coating and its making method |
| CN107638591A (en) * | 2016-07-20 | 2018-01-30 | 中国科学院上海硅酸盐研究所 | A kind of good ceria doped hydroxyapatite coating of biological antioxidant performance and its application |
| CN107638591B (en) * | 2016-07-20 | 2019-12-17 | 中国科学院上海硅酸盐研究所 | Ceria-doped hydroxyapatite coating with good biological oxidation resistance and application thereof |
| CN111334746A (en) * | 2020-04-26 | 2020-06-26 | 广州珈鹏科技有限公司 | Biological ceramic coating with antibacterial activity and preparation method thereof |
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