CN103816569A - Method for treating medical implant material with gas-phase Ag nano-particles - Google Patents
Method for treating medical implant material with gas-phase Ag nano-particles Download PDFInfo
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- CN103816569A CN103816569A CN201410073837.9A CN201410073837A CN103816569A CN 103816569 A CN103816569 A CN 103816569A CN 201410073837 A CN201410073837 A CN 201410073837A CN 103816569 A CN103816569 A CN 103816569A
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 44
- 239000007943 implant Substances 0.000 title claims abstract description 30
- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000000151 deposition Methods 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000012567 medical material Substances 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000007747 plating Methods 0.000 abstract description 3
- 238000004544 sputter deposition Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 238000001771 vacuum deposition Methods 0.000 abstract 2
- 238000002513 implantation Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 230000000844 anti-bacterial effect Effects 0.000 description 8
- 229910001069 Ti alloy Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000012010 growth Effects 0.000 description 4
- 230000001954 sterilising effect Effects 0.000 description 4
- 238000004659 sterilization and disinfection Methods 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002070 germicidal effect Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 210000000963 osteoblast Anatomy 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Abstract
A method for treating a medical implant material with gas-phase Ag nano-particles comprises the following steps: 1) preparing the medical implant material, cleaning and drying the surface of the medical implant material, and sending the medical implant material into a vacuum deposition table; 2) generating an Ag nano-particle beam according to a beam clustering method, wherein the gas pressure of an Ag nano-particle generation chamber is 50 to 200 Pa, the degree of vacuum in the position of the vacuum deposition table is higher than 10<-2> Pa, the sizes of the generated Ag nano-particles are controlled by the supplying velocity of Ag vapor and the gas pressure of the generation chamber, and the coverage rate is controlled by deposition time; 3) depositing the Ag nano-particles, wherein the diameters of the Ag particles are controlled to be 5 to 100 nm, and the coverage rate is slightly lower than 30 percent. The combination degree of the Ag particles and the implant can be effectively adjusted and controlled by a beam technology; compared with a common plating formed through sputtering or chemical coating, the medical implant material is more wear-resistant, and can be used for a long time.
Description
Technical field
The present invention relates to medical material, propose a kind of useful implant medical material and manufacturing process thereof, realize strong anti-microbial property.
Background technology
The medical embedded materials such as artificial growth bone, tooth and joint such as titanium (alloy), magnesium alloy and hydroxyapatite have been obtained in current medical embedded field widely and have been applied because of its good mechanical property, biological stability, biocompatibility and processability.The hard material of these implantation must could be repaired position strong bonded with human body through the regular hour.During this period of time, the Growth of Cells (as osteoblast) that embedded material and human body are repaired position is exactly the emphasis that current medical embedded field is paid close attention to, wherein, gathering and the breeding of all anaerobe of implant, can cause that inflammation causes repairing failure, so antibacterial is one of link of greatest concern.Recently, people are carrying out the adjustment of pattern, component to the surface of embedded material by kinds of surface treatment technology, realize embedded material at the improvement of antibacterial and the many-sided performance of growth (as CN103143056A etc.) with it.
Nanometer Ag is processed and has been considered to anti-bacteria and grows and the effective ways of kill bacteria, and be considered to have broad-spectrum sterilization, germicidal efficiency high, be difficult for developing immunity to drugs, acting on the good characteristics such as stable.It should be noted that very much Ag nano-particle sterilization within a certain period of time has long-lasting, thus use that can be long-term.And due to the general unglazed photograph in position that implant is implanted, conventional TiO2 bactericidal effect is very poor, so people start to pay close attention to the coating effect of Ag nano-particle.Negative electrode (magnetic control) sputter and Cement Composite Treated by Plasma are the important method that obtains implant surfaces nanostructured.The simplest, on titanium or SiO2 substrate, cathodic sputtering spraying plating or magnetron sputtering directly just can obtain certain Ag nanostructured, but the size Control of this class nanostructured is subject to the impact of implantation body's pattern.This has realized implant surfaces preparation and certain bactericidal property of Ag nanostructured.In general the pattern of implantation body itself is comparatively coarse, and the atom of sputter spraying plating nanoscale pattern under the restriction of this preliminary structure is even not, the meticulous control of growing of the albumen that cannot realize expection.Also have, the method that people also adopt nanometer silver to mix is processed some medical materials, such as Chinese invention patent 201210050491.1,201120115265.8 and 201310187527.5 has just been introduced some about nanometer silver chemical method being blended in to the work that reaches bactericidal effect on medical material.
Cluster Beam, also be nano-particle line, that a kind of magnetron sputtering/gas phase cohesion/difference multiple technologies such as bleed of utilizing coordinate the nano-particle line producing, its nano-particle produces in gas phase, and its size can be by the condition control that produces line, and nano-particle line can be deposited to easily substrate surface required substrate is carried out to nanometer processing (Wang Guanghou, " Cluster Physics ", Shanghai science tech publishing house, 2003).So the metal/non-metal nano-particle that utilizes Cluster Beam can produce the size (1-200nm) of various gas phases is used for the modification of medical implantation body.This class is operated in open source literature not yet to be reported.This method is with different in implant surfaces formation nanostructured traditionally, and nano-particle forms in-flight in gas phase, so the nanotopography that implant forms can be by line technology controlling and process.In addition, this type nano granular is generally charged, improves its effect kinetic energy and greatly improves the bond strength of nano-particle thereby can add certain voltage, improves the anti-wear performance of artificial implant.This class formation is controlled, Ag nano-antibacterial and anti-wear performance improve the key performance that medical embedded material is paid close attention to just.
Summary of the invention:
The present invention seeks to, propose the method for the medical implant material of a kind of gas phase Ag nano-particle processing, this class medical material material can be titanium, titanium alloy, magnesium alloy, can be also the insulation Artificial Intervention materials such as hydroxyapatite.The Ag nano-particle layer that surface attachment is grown by gas phase nano particle deposition, the characteristic size of this nanostructured is between 5-100nm, can play the effect of sterilization in a short time, propose the better medical embedded material of a kind of Ag nano-particle fixed performance, make the sterilization anti-microbial property of medical embedded material more permanent.
Technical scheme of the present invention is: the method for the implant medical material of gas phase Ag nano-particle processing, and its step is as follows:
1) prepare medical embedded material, and medical embedded material surface is carried out sending into vacuum moulding machine platform after cleaning, drying;
2) adopt the method for Cluster Beam to produce Ag nano-particle line; Wherein the air pressure of Ag nano-particle generating chamber is in 50～200Pa left and right, and vacuum moulding machine platform place vacuum is better than 10
-2pa.The Ag nanoparticle size producing can be by the air pressure control of the delivery rate of Ag steam, generating chamber, and coverage rate can be controlled by the time depositing;
3) deposition Ag nano-particle, Ag particle diameter, between 5-100nm, reaches the coverage rate a little less than 30%; Especially lower than 20% coverage rate, Ag particle diameter is between 15-60nm;
Further, the present invention can, to medical embedded material surface Dc bias, reach kinetic energy more than every atom 1eV in nano-particle, realizes effectively adhering to anti-wear performance of Ag granule and improves.
For insulation medical implant material, can adopt at the same time beam bombardment, improve the adhesion effect of Ag nano-particle and medical material.Insulation medical implant material can be to be also placed on electric conductor while adding Dc bias, applies Dc bias on electric conductor.
The invention has the beneficial effects as follows, the coverage rate of Ag granule is less than 30%, so do not affect effective combination of implant and human body.The combination degree of Ag granule and implant can effectively regulate by line technique, more wear-resisting than the coating of general sputter or chemistry coating, the permanent use that can guarantee to implant medical material.This material can have the antibacterial effect and the anti-wear performance that are enough to guarantee the firm growth of implant, and also easily controls in technique.
The specific embodiment
Illustrate that by the following examples the present invention implants preparation and the beneficial effect of medical material.
Handling object is that artificial tooth is made up of a titanium alloy implantation body and an outer hat.The titanium alloy implantation body of inner core is soaked 20 minutes in acetone, and dry up and rear implantation body is packed into cluster deposition table with dry nitrogen.Reach 10-4Pa when above at system vacuum degree, pass into Ar gas, flow 40sccm, thus obtaining the cluster generation chamber air pressure of 80Pa, sputtering power maintains 20W.The air pressure of Ag nano-particle generating chamber (Ag being heated to 400-500 degree Celsius by crucible) is in 80Pa left and right, and vacuum moulding machine platform place vacuum is better than 10
-2pa.The Ag nanoparticle size producing can be by the air pressure control of the delivery rate of Ag steam, generating chamber, and coverage rate (surface coverage Ag nano-particle accounts for the long-pending ratio of all surfaces) can be controlled 15-20% by the time depositing; Further scheme, apply employing beam bombardment: under these conditions, the present invention is contained in implantation body's material in a deposition table that applies 10000V voltage, deposits 1 minute simultaneously, the titanium alloy implantation body that can form Ag nano-particle coating, its coverage rate is lower than 20-25%.
Contrast applies 10000V voltage and does not execute alive coating, rap with hand hammer, the Ag nano-particle coating that discovery applies 10000V voltage is very firm, and do not apply be vulnerable to damage, the present invention in use Ag nano-particle and medical adhesion property is obviously better than the product of prior art, and can conveniently control the amount of Ag nanometer.
Adopted after Ag nano-particle coating, in implantation body, bactericidal effect is obvious, and bacterial growth is subject to stronger inhibition.
Claims (4)
1. the method for the implant medical material of gas phase Ag nano-particle processing, is characterized in that step is as follows:
1) prepare medical embedded material, and medical embedded material surface is carried out sending into vacuum moulding machine platform after cleaning, drying;
2) adopt the method for Cluster Beam to produce Ag nano-particle line; Wherein the air pressure of Ag nano-particle generating chamber is at 50～200Pa, and vacuum moulding machine platform place vacuum is better than 10
-2pa; The Ag nanoparticle size producing is by the delivery rate of Ag steam, the air pressure control of generating chamber, and coverage rate was controlled by the time depositing;
3) deposition Ag nano-particle, Ag particle diameter, between 5-100nm, reaches the coverage rate a little less than 30%.
2. the method for the implant medical material of gas phase Ag nano-particle according to claim 1 processing, is characterized in that depositing Ag nano-particle lower than 20% coverage rate, and Ag particle diameter is between 15-60nm.
3. the method for the implant medical material of gas phase Ag nano-particle according to claim 1 processing, it is characterized in that in implant medical material surface Dc bias, reach kinetic energy more than every atom 1eV in nano-particle, realize effectively adhering to anti-wear performance of Ag granule and improve.
4. the method for the implant medical material of gas phase Ag nano-particle according to claim 1 processing, is characterized in that, insulation medical embedded material is adopted to beam bombardment simultaneously, improving the adhesive force of Ag nano-particle and medical material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410073837.9A CN103816569B (en) | 2014-02-28 | 2014-02-28 | The method of the implant medical material of a kind of gas phase Ag nano particle processing |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410073837.9A CN103816569B (en) | 2014-02-28 | 2014-02-28 | The method of the implant medical material of a kind of gas phase Ag nano particle processing |
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| CN103816569A true CN103816569A (en) | 2014-05-28 |
| CN103816569B CN103816569B (en) | 2016-05-11 |
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| CN201410073837.9A Expired - Fee Related CN103816569B (en) | 2014-02-28 | 2014-02-28 | The method of the implant medical material of a kind of gas phase Ag nano particle processing |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119802A (en) * | 2016-08-01 | 2016-11-16 | 宋凤麒 | A kind of elementide line for organic nanometer processing method and apparatus |
| CN107739939A (en) * | 2017-10-26 | 2018-02-27 | 中南大学 | A kind of Biological magnesium alloy with anti-microbial property and preparation method thereof |
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| US5984905A (en) * | 1994-07-11 | 1999-11-16 | Southwest Research Institute | Non-irritating antimicrobial coating for medical implants and a process for preparing same |
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| CN107739939A (en) * | 2017-10-26 | 2018-02-27 | 中南大学 | A kind of Biological magnesium alloy with anti-microbial property and preparation method thereof |
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| Publication number | Publication date |
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| CN103816569B (en) | 2016-05-11 |
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