CN103695707B - A kind of titanium silver alloy nanotube for surgical fixator tool and preparation method thereof - Google Patents
A kind of titanium silver alloy nanotube for surgical fixator tool and preparation method thereof Download PDFInfo
- Publication number
- CN103695707B CN103695707B CN201310489824.5A CN201310489824A CN103695707B CN 103695707 B CN103695707 B CN 103695707B CN 201310489824 A CN201310489824 A CN 201310489824A CN 103695707 B CN103695707 B CN 103695707B
- Authority
- CN
- China
- Prior art keywords
- titanium
- silver
- nanotube
- silver alloy
- anodic oxidation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Materials For Medical Uses (AREA)
Abstract
The invention belongs to medical instruments field, be specifically related to a kind of titanium silver alloy nanotube for surgical fixator tool and preparation method thereof.For the titanium silver alloy nanotube of surgical fixator tool, by weight percentage, silver content is 1-5%, and surplus is titanium; The caliber of nanotube is between 20-100nm, and pipe range is 1-50 μm.Its preparation method first adopts scorification to synthesize titanium silver alloys in high temperature furnace, then two step anodic oxidation treatment are carried out to titanium silver alloys, finally dry under 400-500 DEG C of condition in retort furnace, control heat-up rate 2 ~ 4 DEG C/min, obtain titanium silver alloy nanotube.Titanium silver alloy nanotube pattern surgical fixator tool of the present invention, adds the anti-microbial property of surgery anchor apparatus, and selected materials silver and titanium abundance, price is low, is easy to promote.
Description
Technical field
The invention belongs to medical instruments field, be specifically related to a kind of titanium silver alloy nanotube for surgical fixator tool and preparation method thereof.
Background technology
Skeletal diseases and the quality of wound to health and lives have far-reaching influence.Skeletal diseases creates tremendous influence to quality of life with to society.On the whole, the health care expenditures of 10% and skeletal diseases closely bound up (as joint replacement, fracture fixation etc.) is had every year at least.Along with the development of society, the biomaterial that increasing orthopaedics is relevant is applied to clinical, as joint prosthesis, and spinal fusion, fracture fixation apparatus (comprising internal fixtion, extenal fixation) etc.At least millions of patient in the annual whole world about needs hip joint or knee prosthesis.Although have passed through strict sterilizing and sterile procedure when implanting surgical fixator tool, medical implant infects the principal element remaining and implant Internal implant failure.Therefore reduce surgery, the infection problems that especially orthopaedics and emergency department's fixed apparatus are relevant is extremely important.
Unfortunately, still lack clinically at present and effectively make surgical fixator tool self have to avoid bacteriological infection method, current surgical fixator tool self does not have anti-microbial property, and the infection rate that especially external fixation device is relevant is up to 30%-50%.Therefore the antibacterial ability improving current surgical fixator tool is extremely important.Titania nanotube has nano-tube array and the bio-compatibility of high-sequential, and one of the most attractive nano material is at present applied on surgical fixator tool, is the positive thinking solving external application fixed apparatus infection problems.
Summary of the invention
For prior art Problems existing, the invention provides a kind of titanium silver alloy nanotube for surgical fixator tool and preparation method thereof, object is surface topography by changing surgical fixator tool and composition, reaches anti-bacteria and adheres to, the effect of kill bacteria.
Titanium silver alloy nanotube for surgical fixator tool of the present invention, its composition is 1-5% silver by weight percentage, and surplus is titanium, and nanotube caliber is between 20-100nm, and length is 1-20 μm.
The preparation method of the above-mentioned silver-colored titanium alloy nano pipe for surgical fixator tool carries out according to following steps:
(1) prepare burden according to weight percent 1-5% silver, 95-99% titanium, adopt scorification to synthesize titanium silver alloys in high temperature furnace;
(2) two step anodic oxidation treatment are carried out to titanium silver alloys, with ethylene glycol and the NH accounting for ethylene glycol weight 0.5%
4f is as the anodised electrolytic solution of the first step, and oxidization time is 2-20 hour, and oxidation voltage is 20-60V; In the first step anodic oxidation electrolyte, add the HF accounting for electrolyte weight 0.75%, oxidization time is 2-20 hours, and oxidation voltage is that 20V-60V carries out second step anodic oxidation;
(3) the titanium silver alloys after two step anodic oxidation treatment is dried under 400-500 DEG C of condition in retort furnace, control heat-up rate 2 ~ 4 DEG C/min, obtain titanium silver alloy nanotube.
Compared with prior art, feature of the present invention and beneficial effect are:
Technical scheme of the present invention is that the surface topography and composition by changing surgical fixator tool reaches anti-bacteria adhesion, the effect of kill bacteria.Because silver ions has natural anti-microbial effect.And on the cell walls that antibacterial mechanisms mainly relies on electrostatic attraction to be adsorbed on negative charge, the cytolemma penetrating bacterium infiltrates cell, and DNA in bacterium inclusion is in conjunction with the propagation of anti-bacteria, and can combine with the sulfydryl on many enzymes, the transhipment of interference electron transport chain, cause bacterial death, many experiment in vitro all confirm that metal ion can reduce adhesion and the growth of bacterium.
The Titanium copper alloy nanotube pattern surgical fixator tool of this reality invention, adds the anti-microbial property of surgical fixator tool, and selected materials copper and titanium abundance, price is low, is easy to promote.
Accompanying drawing explanation
Fig. 1 is titanium silver alloy nanotube prepared by the embodiment of the present invention 1;
Fig. 2 is titanium silver alloy nanotube prepared by the embodiment of the present invention 2;
Fig. 3 is that the titanium silver alloy nanotube prepared of the embodiment of the present invention 1 and common titanium nanotube and business titanium metal carry out antibacterial experiment effect contrast figure;
Fig. 4 be the embodiment of the present invention 1 prepare titanium silver alloy nanotube and business titanium metal carry out antibacterial experiment metallic surface bacterial growth situation comparison diagram;
Fig. 5 is that the titanium silver alloy nanotube prepared of the embodiment of the present invention 2 and common titanium nanotube and business titanium metal carry out antibacterial experiment effect contrast figure.
Embodiment
Embodiment 1
The titanium silver alloy nanotube for surgical fixator tool of the present embodiment, by weight percentage, silver content is 3%, and surplus is titanium; The caliber of nanotube is 40nm, and pipe range is 20 μm.
The preparation method of the above-mentioned silver-colored titanium alloy nano pipe for surgical fixator tool carries out according to following steps:
(1) prepare burden according to weight percent 3% silver medal, 97% titanium, adopt scorification to synthesize silver-colored titanium alloy in high temperature furnace;
(2) two step anodic oxidation treatment are carried out to silver-colored titanium alloy, with ethylene glycol and the NH accounting for ethylene glycol weight 0.5%
4f is as the anodised electrolytic solution of the first step, and oxidization time is 2 hours, and oxidation voltage is 20V; In the first step anodic oxidation electrolyte, add the HF accounting for electrolyte weight 0.75%, oxidization time is 2 hours, and oxidation voltage is that 20V carries out second step anodic oxidation;
(3) dried under 400 DEG C of conditions in retort furnace by the titanium silver alloys after two step anodic oxidation treatment, control heat-up rate 2 DEG C/min, obtain titanium silver alloy nanotube, its pattern as shown in Figure 1.
Antibacterial experiment is done to the titanium silver alloy nanotube prepared:
Experimental technique: according to 10
7/ ml prepares S. aureus L-forms bacterium liquid, adopts LIVE/DEAD Baclight TM staining kit (containing SYTO-9 and PI) that SYTO9 and PI two pipe staining agent is used 2.5mL sterilizing deionized water dissolving respectively, and then equal proportion mixing, as staining agent.
During experiment, S. aureus L-forms bacterium liquid and staining agent are mixed and is layered on titanium silver nanotube tinsel and common titanium metal nanotube tinsel and business titanium metal plate respectively afterwards, lucifuge adopts the burnt electric Microscopic observation bacterial colony of copolymerization to be formed and antibacterial situation after 15 minutes, as shown in Figure 3, show that titanium silver alloy nanotube of the present invention compares with business titanium metal the adhesion greatly reducing bacterium with common titanium metal nanotube, and have good sterilising effect.
Antibacterial observation is carried out to the titanium silver alloy nanotube prepared:
Titanium silver nanotube tinsel and business titanium metal plate is adopted to test respectively.The tinsel of 1cm × 1cm is placed in 12 orifice plates, washs 2 times with PBS liquid, at tinsel surface seeding S. aureus L-forms, be placed in incubator cultivate 6 hours (37 DEG C, 5% CO
2, 20% O
2).Took out tinsel respectively at the 6th, 24 hour, solution removed by aspiration, PBS cleans 2 times, carries out PBS cleaning again after adopting the pentanedial liquid of 2.5% fixing.Adopt scanning electron microscopic observation metallic surface biofilm load to generate situation, as shown in Figure 4, display titanium silver alloy nanotube and business titanium metal plate, compare the adhesion greatly reducing bacterium, and have good sterilising effect result; Bacterium is bacterial multiplication on business titanium metal, and ne ar is good, and bacterium is poor adhesion in titanium silver alloy nanotube, and ne ar distortion, inclusion breaks.
Embodiment 2
The silver-colored titanium alloy nano pipe for surgical fixator tool of the present embodiment, by weight percentage, silver content is 5%, and surplus is titanium; The caliber of nanotube is 100nm, and pipe range is 50 μm, and its pattern as shown in Figure 2.
The preparation method of the above-mentioned silver-colored titanium alloy nano pipe for surgical fixator tool carries out according to following steps:
(1) prepare burden according to weight percent 5% silver medal, 95% titanium, adopt scorification to synthesize silver-colored titanium alloy in high temperature furnace;
(2) two step anodic oxidation treatment are carried out to silver-colored titanium alloy, with ethylene glycol and the NH accounting for ethylene glycol weight 0.5%
4f is as the anodised electrolytic solution of the first step, and oxidization time is 10 hours, and oxidation voltage is 60V; In the first step anodic oxidation electrolyte, add the HF accounting for electrolyte weight 0.75%, oxidization time is 10 hours, and oxidation voltage is that 60V carries out second step anodic oxidation;
(3) the titanium silver alloys after two step anodic oxidation treatment is dried under 500 DEG C of conditions in retort furnace, control heat-up rate 3 DEG C/min, obtain titanium silver alloy nanotube.
Antibacterial experiment is done to the titanium silver alloy nanotube prepared:
Experimental technique: according to 10
7/ ml prepares S. aureus L-forms bacterium liquid, adopts LIVE/DEAD Baclight TM staining kit (containing SYTO-9 and PI) that SYTO9 and PI two pipe staining agent is used 2.5mL sterilizing deionized water dissolving respectively, and then equal proportion mixing, as staining agent.
During experiment, S. aureus L-forms bacterium liquid and staining agent are mixed and is layered on titanium silver nanotube tinsel and common titanium nanotube tinsel and business titanium metal plate respectively afterwards, lucifuge adopts the burnt electric Microscopic observation bacterial colony of copolymerization to be formed and antibacterial situation after 15 minutes, as shown in Figure 5, show that titanium silver alloy nanotube of the present invention compares with business titanium metal the adhesion greatly reducing bacterium with common titanium metal nanotube, and have good sterilising effect.
Embodiment 3
The silver-colored titanium alloy nano pipe for surgical fixator tool of the present embodiment, by weight percentage, silver content is 1%, and surplus is titanium; The caliber of nanotube is 20nm, and pipe range is 1 μm.
The preparation method of the above-mentioned silver-colored titanium alloy nano pipe for surgical fixator tool carries out according to following steps:
(1) prepare burden according to weight percent 1% silver medal, 99% titanium, adopt scorification to synthesize silver-colored titanium alloy in high temperature furnace;
(2) two step anodic oxidation treatment are carried out to silver-colored titanium alloy, with ethylene glycol and the NH accounting for ethylene glycol weight 0.5%
4f is as the anodised electrolytic solution of the first step, and oxidization time is 20 hours, and oxidation voltage is 40V; In the first step anodic oxidation electrolyte, add the HF accounting for electrolyte weight 0.75%, oxidization time is 20 hours, and oxidation voltage is that 40V carries out second step anodic oxidation;
(3) the titanium silver alloys after two step anodic oxidation treatment is dried under 450 DEG C of conditions in retort furnace, control heat-up rate 4 DEG C/min, obtain titanium silver alloy nanotube.
Show that titanium silver alloy nanotube of the present invention compares with business titanium metal the adhesion greatly reducing bacterium with common titanium nanotube through antibacterial tests, and have good sterilising effect.
Claims (1)
1., for a preparation method for the titanium silver alloy nanotube of surgical fixator tool, by weight percentage, silver content is 1-5% to the composition of titanium silver alloy nanotube, and surplus is titanium; The caliber of nanotube is between 20-100nm, and pipe range is 1-50 μm, it is characterized in that carrying out according to following steps:
(1) prepare burden according to weight percent 1-5% silver, 95-99% titanium, adopt scorification to synthesize silver-colored titanium alloy in high temperature furnace;
(2) two step anodic oxidation treatment are carried out to silver-colored titanium alloy, with ethylene glycol and the NH accounting for ethylene glycol weight 0.5%
4f is as the anodised electrolytic solution of the first step, and oxidization time is 2-20 hour, and oxidation voltage is 20-60V; In the first step anodic oxidation electrolyte, add the HF accounting for electrolyte weight 0.75%, oxidization time is 2-20 hours, and oxidation voltage is that 20V-60V carries out second step anodic oxidation;
(3) the titanium silver alloys after two step anodic oxidation treatment is dried under 400-500 DEG C of condition in retort furnace, control heat-up rate 2 ~ 4 DEG C/min, obtain titanium silver alloy nanotube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310489824.5A CN103695707B (en) | 2013-10-18 | 2013-10-18 | A kind of titanium silver alloy nanotube for surgical fixator tool and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310489824.5A CN103695707B (en) | 2013-10-18 | 2013-10-18 | A kind of titanium silver alloy nanotube for surgical fixator tool and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103695707A CN103695707A (en) | 2014-04-02 |
| CN103695707B true CN103695707B (en) | 2015-08-19 |
Family
ID=50357366
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310489824.5A Expired - Fee Related CN103695707B (en) | 2013-10-18 | 2013-10-18 | A kind of titanium silver alloy nanotube for surgical fixator tool and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103695707B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106038274A (en) * | 2016-06-30 | 2016-10-26 | 江苏凯邦医疗器械有限公司 | Cannula-type acupuncture needle |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739886B (en) * | 2017-10-11 | 2019-02-15 | 白希壮 | A kind of titanium silver alloy and preparation method thereof for orthopaedics implant |
| CN107747076A (en) * | 2017-11-15 | 2018-03-02 | 成都测迪森生物科技有限公司 | A kind of method for strengthening titanium alloy and carboxyl polymer cementability |
| CN107794408A (en) * | 2017-11-15 | 2018-03-13 | 成都测迪森生物科技有限公司 | A kind of support titanium alloy material |
| CN108300898B (en) * | 2018-01-29 | 2020-08-25 | 东北大学 | Low-modulus silver-containing anti-infection titanium alloy |
| CN108300897B (en) * | 2018-01-29 | 2020-12-15 | 东北大学 | Low-modulus silver-containing anti-infection medical titanium alloy |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011008778A2 (en) * | 2009-07-14 | 2011-01-20 | University Of Massachusetts | Metal and metal oxide structures and preparation thereof |
| CN103046056B (en) * | 2012-12-21 | 2014-11-26 | 太原理工大学 | Method for preparing Ag-Ti-O antibacterial nanotube film on surface of titanium alloy |
| CN103110981B (en) * | 2013-01-10 | 2014-06-04 | 内蒙金属材料研究所 | Method for preparing antibacterial active titanium oxide nanotube array composite coating material |
-
2013
- 2013-10-18 CN CN201310489824.5A patent/CN103695707B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106038274A (en) * | 2016-06-30 | 2016-10-26 | 江苏凯邦医疗器械有限公司 | Cannula-type acupuncture needle |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103695707A (en) | 2014-04-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ehrensberger et al. | Cathodic voltage-controlled electrical stimulation of titanium implants as treatment for methicillin-resistant Staphylococcus aureus periprosthetic infections | |
| CN103695707B (en) | A kind of titanium silver alloy nanotube for surgical fixator tool and preparation method thereof | |
| Zhang et al. | Improved antibacterial activity and biocompatibility on vancomycin-loaded TiO2 nanotubes: in vivo and in vitro studies | |
| Ercan et al. | Decreased Staphylococcus aureus biofilm growth on anodized nanotubular titanium and the effect of electrical stimulation | |
| CN103695706B (en) | A kind of Titanium copper alloy nanotube for surgical fixator tool and preparation method thereof | |
| Ercan et al. | Diameter of titanium nanotubes influences anti-bacterial efficacy | |
| Schaer et al. | Hydrophobic polycationic coatings that inhibit biofilms and support bone healing during infection | |
| He et al. | Antibacterial ability and osteogenic activity of porous Sr/Ag-containing TiO2 coatings | |
| ES2414635T3 (en) | Medical part and method of manufacturing it | |
| Shivaram et al. | Mechanical degradation of TiO2 nanotubes with and without nanoparticulate silver coating | |
| Guan et al. | Long-lasting bactericidal activity through selective physical puncture and controlled ions release of polydopamine and silver nanoparticles–loaded TiO2 nanorods in vitro and in vivo | |
| Shi et al. | An effective self-powered strategy to endow titanium implant surface with associated activity of anti-biofilm and osteogenesis | |
| CN102371005B (en) | Zinc-doped porous nano-titanium oxide coating and its preparation method | |
| CN107661544A (en) | Antibacterial facilitates porous orthopaedics implant of bone complex function and preparation method thereof | |
| Dias-Netipanyj et al. | Effect of crystalline phases of titania nanotube arrays on adipose derived stem cell adhesion and proliferation | |
| Ehrensberger et al. | Electrochemical methods to enhance osseointegrated prostheses | |
| US9353453B2 (en) | Metal substrate modified with silicon based biomimetic treatment having antibacterial property for the osteointegration thereof | |
| CN103242551B (en) | Method for injecting titanium ions to modify surface of polyether-ether-ketone | |
| Wang et al. | Osteogenic and antiseptic nanocoating by in situ chitosan regulated electrochemical deposition for promoting osseointegration | |
| Dauben et al. | A novel in vitro system for comparative analyses of bone cells and bacteria under electrical stimulation | |
| Beltrán-Partida et al. | Disinfection of titanium dioxide nanotubes using super-oxidized water decrease bacterial viability without disrupting osteoblast behavior | |
| CN105506586A (en) | Method for preparing degradable magnesium cage implant with antibacterial and anti-corrosion graphene/apatite composite coating | |
| CN112107739A (en) | Bionic material with physical sterilization and cell adhesion promotion functions and manufacturing method | |
| Liu et al. | Biocompatibility evaluation of antibacterial Ti–Ag alloys with nanotubular coatings | |
| CN104264204A (en) | Method for directly preparing micro-arc oxidation ceramic membrane containing zinc oxide on surface of magnesium alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| CB03 | Change of inventor or designer information |
Inventor after: Bai Xizhuang Inventor after: Niu Ping Inventor after: Xue Xiangxin Inventor after: Tian Ang Inventor after: You Junhua Inventor after: Sun Yu Inventor after: Zhang Hangzhou Inventor after: Wang Lin Inventor after: Ali Inventor before: Bai Xizhuang Inventor before: Niu Ping Inventor before: Sun Yu Inventor before: Zhang Hangzhou Inventor before: Xue Xiangxin Inventor before: Tian Ang Inventor before: Wang Lin Inventor before: Ali Inventor before: You Junhua |
|
| COR | Change of bibliographic data | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20150923 Address after: 110001 No. 92 Heping District, Liaoning, Shenyang Patentee after: CHINA MEDICAL University Patentee after: Northeastern University Patentee after: SHENYANG University OF TECHNOLOGY Address before: 110001 No. 92 Heping District, Liaoning, Shenyang Patentee before: CHINA MEDICAL University |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150819 Termination date: 20211018 |