CN1213644A - Method of preparing antiseptic hydroxyl kietyoite cladding material - Google Patents
Method of preparing antiseptic hydroxyl kietyoite cladding material Download PDFInfo
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- CN1213644A CN1213644A CN 98120506 CN98120506A CN1213644A CN 1213644 A CN1213644 A CN 1213644A CN 98120506 CN98120506 CN 98120506 CN 98120506 A CN98120506 A CN 98120506A CN 1213644 A CN1213644 A CN 1213644A
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- energy
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- torr
- electric current
- ion beam
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- 239000000463 material Substances 0.000 title claims description 14
- 238000005253 cladding Methods 0.000 title claims description 11
- 230000002421 anti-septic effect Effects 0.000 title claims description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 title claims description 10
- 238000000034 method Methods 0.000 title claims description 7
- 238000004544 sputter deposition Methods 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims description 11
- 230000008021 deposition Effects 0.000 claims description 11
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 11
- 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 claims description 11
- 238000010884 ion-beam technique Methods 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 239000007943 implant Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 101710134784 Agnoprotein Proteins 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000010849 ion bombardment Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000007747 plating Methods 0.000 claims description 2
- 238000005477 sputtering target Methods 0.000 claims 1
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 abstract 3
- WHZWVUKPJBNTAK-UHFFFAOYSA-N hydroxy dihydrogen phosphite Chemical compound OOP(O)O WHZWVUKPJBNTAK-UHFFFAOYSA-N 0.000 abstract 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 230000000249 desinfective effect Effects 0.000 abstract 1
- 210000002540 macrophage Anatomy 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 210000000963 osteoblast Anatomy 0.000 abstract 1
- 231100000331 toxic Toxicity 0.000 abstract 1
- 230000002588 toxic effect Effects 0.000 abstract 1
- 208000015181 infectious disease Diseases 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 206010067268 Post procedural infection Diseases 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- -1 silver ions Chemical class 0.000 description 2
- 239000012890 simulated body fluid Substances 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 241000191963 Staphylococcus epidermidis Species 0.000 description 1
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000002924 anti-infective effect Effects 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
A process for preparing antibacterial coated layer os hydroxy phosphorite includes cleaning surface of specimen, sputtering hydroxy phosphorite layer on the cleaned surface, and immersing the coated specimen in 20-100 ppm solution of AgNO3 at ordinary temp for 24-48 hrs. The prepared specimen features high disinfecting rate up to 100% within 24 hrs, no toxic by-effect on macrophage and osteoblast, and better biocompatibility.
Description
The present invention relates to a kind of preparation method of antiseptic hydroxyl kietyoite cladding material, belong to medical material tech field.
The applicant had once applied for the Ion Beam Enhanced Deposit Technology deposited hydroxyl apatite in the patent (application number: 97120353.9) on medical implant surface in December, 1997, this invention has solved the weakness of conventional medical implant surface binding force of cladding material difference, but because the no antibiotic performance of coating itself, so face the danger of infection in actual applications.Hydroxyl apatite coating medically is being widely used, but infection problems fails to solve always.Postoperative infection in the medical implant process accounts for 22% of all kinds of infection summations at present, and only the U.S. causes the tens beautiful financial losses of not having every year.
The infection that bone implant material causes, its result must not cause the embedded material that infects is removed, and undergos surgery again, causes great misery and loss economically to patient.
In order to solve the postoperative infection problem, people use various microbiotic, but poor effect often, because the microbial film that forms at implant surface has increased the resistance of bacterial antibiotic.People recognize the antiseptic-germicide that must form high density on the bone implant material surface.
The objective of the invention is to propose a kind of preparation method of antiseptic hydroxyl kietyoite cladding material, experimental results demonstrate, hydroxyapatite has excellent biological compatibility, if the Ag ion is written in the hydroxyapatite, then has high stability, excellent biological compatibility and good antimicrobial property are by being written into silver ions to reach operation back sterilization, anti-infectious purpose in hydroxyl apatite coating.
The preparation method of the antiseptic hydroxyl kietyoite cladding material of the present invention's design comprises following each step:
(1) clean: electric current is 30～60mA, is the Ar ion beam bombardment substrate sample surface of 0.8～1.2KeV with energy, and bombardment time is 10～15 minutes, and background pressure is 5 * 10
-6Torr, in the working process, keeping steam partial pressure is 0～2 * 10
-4Torr, operating pressure are 0.5～2.5 * 10
-4Torr;
(2) make the interface: the hydroxyapatite sintered ceramic target with 50% is sputter, with electric current is 20～60mA, energy is the ion beam bombardment of 0.3～3.5KeV, in substrate sample surface sputtering film forming, be 1～3mA with electric current simultaneously, energy is the high energy Ar ion beam bombardment substrate sample surface of 24～30KeV, and sputtering time is 10～30 minutes;
(3) deposition growing: the sputter procedure in above-mentioned second step is proceeded, with electric current is that 40～100mA, energy are the ion beam bombardment of 3～3.5 KeV, continues spatter film forming, is 5～20mA with electric current simultaneously, energy is the energy Ar ion bombardment of 0.5～400eV, and sputtering time is 1～5 hour;
(4) behind the plated film 1 hour, the membrane sample in above-mentioned the 3rd step is taken out from vacuum, be heated to 380 ℃～420 ℃, annealed 0～4 hour in humidity greater than 70% damp atmosphere, can obtain possessing the sample of hydroxyl apatite coating;
(5) sample with the intact film of above-mentioned plating is placed on the AgNO that concentration is 20-100ppm
3In the solution, soaked 24-48 hour under the room temperature, be sample with antiseptic hydroxyl kietyoite cladding material.
Adopt the medical embedded matter sample of the present invention's preparation to reach antibiotic purpose fully, sample soaks the Ag that just can make after 4 hours in the simulated body fluid in simulated body fluid
-Concentration reaches 20ppm, keeps Ag in a week
-Concentration is about 25ppm; 10
-5Electron microscopic observation after soaking in the bacterium liquid of/ml concentration shows that the thalline adhesive rate of sample significantly reduces than the sample that does not carry silver; Sample reached 100% to the sterilizing rate of intestinal bacteria, streptococcus aureus, staphylococcus epidermidis, Pseudomonas aeruginosa etc. in 24 hours.
Cell experiment shows that sample has no side effect to scavenger cell, scleroblast etc., and showing as the sample surfaces cell of handling does not have phenomenons such as aggegation, distortion, and in well attached, the abundant stretching, extension of sample surfaces, normal breeding.More than the existing excellent biological compatibility of sample of explanation the present invention preparation possesses anti-microbial property completely again.
Introduce embodiments of the invention below:
Embodiment 1 adopts the listed parameter plated film of following table, and at 400+20 ℃, humidity was not less than in 70% the air annealing 2 hours, just can obtain degree of crystallinity near 100% hydroxyapatite film.
| Substrate sample | The Ti-6Al-4V alloy | |
| Background pressure | 5×10 -6Torr (torr) | |
| Steam partial pressure | 1.2×10 -4Torr (torr) | |
| Operating pressure | 1.8×10 -4Torr (torr) | |
| Ionic fluid cleans | (1.0keV kiloelectron volt), 50mA (milliampere), 12min (minute) | |
| Make the interface | The high energy bombardment | 28keV (kiloelectron volt), 2mA (milliampere), |
| Make the interface | Sputter | (3.5keV kiloelectron volt) 45mA (milliampere), |
| Make the interface | Time | 30min (minute) |
| Deposition growing | The low energy bombardment | Do not have |
| Deposition growing | Sputter | (3.25keV kiloelectron volt), 60mA (milliampere), |
| Deposition growing | Time | 3hr (hour) |
| Aftertreatment | 400 ± 20 ℃, 2hr (hour) | |
Above-mentioned sample is immersed in the AgNO that concentration is 20ppm
3In the solution, soak time is 48 hours, and sample promptly has antiseptic hydroxyl kietyoite cladding material.Embodiment 2
Above-mentioned sample is immersed in the AgNO that concentration is 50ppm
3In the solution, soak time is 30 hours, and sample promptly has antiseptic hydroxyl kietyoite cladding material.Embodiment 3
| Substrate sample | Al 2O 3Pottery | |
| Background pressure | 5×10 -6Torr (torr) | |
| Steam partial pressure | Do not have | |
| Operating pressure | 2.2×10 -4Torr (torr) | |
| Ionic fluid cleans | (1.0keV kiloelectron volt), 50mA (milliampere), 12min (branch) | |
| Make the interface | The high energy bombardment | 30keV (kiloelectron volt), 2mA (milliampere), |
| Make the interface | Sputter | (3.25keV kiloelectron volt), 45mA (milliampere), |
| Make the interface | Time | 15min (minute) |
| Deposition growing | The low energy bombardment | 150eV (electron-volt), 10mA (milliampere) |
| Deposition growing | Sputter | (3.25keV kiloelectron volt), 90mA (milliampere), |
| Deposition growing | Time | 2.5hr (hour) |
| Aftertreatment | 400 ± 20 ℃, 2hr (hour) |
| Substrate sample | Ultra high molecular polyethylene | |
| Background pressure | 5×10 -6Torr (torr) | |
| Steam partial pressure | 1.2×10 -4Torr (torr) | |
| Operating pressure | 2.2×10 -4Torr (torr) | |
| Ionic fluid cleans | (1.0keV kiloelectron volt), 30mA (milliampere), 5min (minute) | |
| Make the interface | The high energy bombardment | 25keV (kiloelectron volt), 1mA (milliampere), |
| Make the interface | Sputter | (3.25keV kiloelectron volt), 30mA (milliampere), |
| Make the interface | Time | 10min (minute) |
| Deposition growing | The low energy bombardment | 150eV (electron-volt), 10mA (milliampere) |
| Deposition growing | Sputter | (3.25keV kiloelectron volt), 50mA (milliampere), |
| Deposition growing | Time | 3hr (hour) |
| Aftertreatment | Do not have | |
Above-mentioned sample is immersed in the AgNO that concentration is 100ppm
3In the solution, soak time is 24 hours, and sample promptly has antiseptic hydroxyl kietyoite cladding material.
Claims (1)
1, a kind of preparation method of reinforced ion beam-deposited hydroxyl apatite coating of medical implant is characterized in that this method comprises following each step:
(1) clean: electric current is 30～60mA, is the Ar ion beam bombardment substrate sample surface of 0.8～1.2KeV with energy, and bombardment time is 10～15 minutes, and background pressure is 5 * 10
-6Torr, in the working process, keeping steam partial pressure is 0～2 * 10
-4Torr, operating pressure are 0.5～2.5 * 10
-4Torr;
(2) make the interface: the hydroxyapatite sintered ceramic target with 50% is a sputtering target, with electric current is 20～60mA, energy is the ion beam bombardment of 0.3～3.5KeV, in substrate sample surface sputtering film forming, be 1～3mA with electric current simultaneously, energy is the high energy Ar ion beam bombardment substrate sample surface of 24～30KeV, and sputtering time is 10～30 minutes;
(3) deposition growing: the sputter procedure in above-mentioned second step is proceeded, with electric current is that 40～100mA, energy are the ion beam bombardment of 3～3.5KeV, continues spatter film forming, is 5～20mA with electric current simultaneously, energy is the energy Ar ion bombardment of 0.5～400eV, and sputtering time is 1～5 hour:
(4) behind the plated film 1 hour, the membrane sample in above-mentioned the 3rd step is taken out from vacuum, be heated to 380 ℃～420 ℃, annealed 0～4 hour in humidity greater than 70% damp atmosphere, can obtain possessing the sample of hydroxyl apatite coating;
It is characterized in that also comprising:
(5) sample with the intact film of above-mentioned plating is placed on the AgNO that concentration is 20-100ppm
3In the solution, soaked 24-48 hour under the room temperature, be sample with antiseptic hydroxyl kietyoite cladding material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98120506 CN1059874C (en) | 1998-10-16 | 1998-10-16 | Method of preparing antiseptic hydroxyl kietyoite cladding material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98120506 CN1059874C (en) | 1998-10-16 | 1998-10-16 | Method of preparing antiseptic hydroxyl kietyoite cladding material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1213644A true CN1213644A (en) | 1999-04-14 |
| CN1059874C CN1059874C (en) | 2000-12-27 |
Family
ID=5226777
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98120506 Expired - Fee Related CN1059874C (en) | 1998-10-16 | 1998-10-16 | Method of preparing antiseptic hydroxyl kietyoite cladding material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1059874C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306999C (en) * | 2002-12-27 | 2007-03-28 | 富士通株式会社 | Method for forming photocatalyst apatite film |
| WO2009030149A1 (en) * | 2007-08-27 | 2009-03-12 | Tao Zhang | Metallic-base antiseptic patch, its preformed body, its preparing method using magnetron sputtering and its use |
| CN101879331A (en) * | 2010-06-26 | 2010-11-10 | 上海交通大学 | Preparation method of amino-terminated hyperbranched polybenzimidazole composite film |
| CN104131325A (en) * | 2014-07-18 | 2014-11-05 | 中国兵器工业第五二研究所 | Preparation method of titanium oxide nano-tube array-silver composite coating material |
| CN113197689A (en) * | 2021-05-08 | 2021-08-03 | 山东恒泰医疗器械有限公司 | Dental implant abutment for inhibiting adhesion of dental bacteria and surface treatment method thereof |
-
1998
- 1998-10-16 CN CN 98120506 patent/CN1059874C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306999C (en) * | 2002-12-27 | 2007-03-28 | 富士通株式会社 | Method for forming photocatalyst apatite film |
| WO2009030149A1 (en) * | 2007-08-27 | 2009-03-12 | Tao Zhang | Metallic-base antiseptic patch, its preformed body, its preparing method using magnetron sputtering and its use |
| CN101879331A (en) * | 2010-06-26 | 2010-11-10 | 上海交通大学 | Preparation method of amino-terminated hyperbranched polybenzimidazole composite film |
| CN101879331B (en) * | 2010-06-26 | 2013-03-20 | 上海交通大学 | Preparation method of amino-terminated hyperbranched polybenzimidazole composite film |
| CN104131325A (en) * | 2014-07-18 | 2014-11-05 | 中国兵器工业第五二研究所 | Preparation method of titanium oxide nano-tube array-silver composite coating material |
| CN113197689A (en) * | 2021-05-08 | 2021-08-03 | 山东恒泰医疗器械有限公司 | Dental implant abutment for inhibiting adhesion of dental bacteria and surface treatment method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1059874C (en) | 2000-12-27 |
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