CN1736493A - Method for preparing TiO2-HA biological medical nanometer structured film - Google Patents
Method for preparing TiO2-HA biological medical nanometer structured film Download PDFInfo
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- CN1736493A CN1736493A CN 200510028679 CN200510028679A CN1736493A CN 1736493 A CN1736493 A CN 1736493A CN 200510028679 CN200510028679 CN 200510028679 CN 200510028679 A CN200510028679 A CN 200510028679A CN 1736493 A CN1736493 A CN 1736493A
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Abstract
The invention discloses a making method of TiO2-HA biological medical nanostructure film in biological stock technique domain, wherein the ratio of TiO2 and HA is between 1:-9 and 9:1; The ratio of Ca and P is between 1.6:1 and 1.7:1; which comprises the following steps: cleaning, drying and fixing the medical implant base material; fixing the sputtering target material; drying the vacuum chamber; sputtering cleaning target material surface; passing the oxygen after steady sputtering cleaning; moving baffle; turning substrate; sputtering Ti/HA and Ti target in turn; sedimentating the TiO2-HA composite film; fetching the sample out of the vacuum chamber after sputtering. The invention adapts reaction magnetic sputtering technique to control the film component and particle dimension by adjusting the sputtering parameter and adding TiO2 ceramic component.
Description
Technical field
What the present invention relates to is a kind of preparation method of technical field of biological materials, specifically is a kind of TiO
2The preparation method of-HA biological medical nanometer structured film.
Background technology
Nowadays the biological implantation material that is used for hard tissue repair and replacement mainly still is Metal and Alloy, and wherein titanium alloy has intensity, toughness, corrosion resistance and good processability preferably, is a kind of more satisfactory interplantation material.But titanium implant belongs to bio-inert material, this back implant loose or dislocation that just causes implanting.Hydroxyapatite (Hydroxyapatite, be abbreviated as HA) be the main inanimate matter that constitutes human body hard tissue, have excellent biological compatibility and biological activity, therefore can titanium and alloy be core, the method of the composite implantation body of surface spraying hydroxyapatite, form good biological combination interface, guaranteed the biological affinity of implant surface on the one hand, guaranteed the high strength and the elasticity of implantation body on the one hand again.
K.De.Groot in 1987 have proposed to prepare with the plasma spray coating technology technology of hydroxyapatite coating layer, since then, the research of relevant plasma spray coating hydroxyapatite coating layer has had considerable progress, but long-term clinical discovery implantation body coating comes off from titanium and alloy surface thereof easily, finally causes graft failure.
Find that through literature search Journal of Thermal Spray Tech-nology " plasma spray technology magazine " the 9th phase 520-525 page or leaf had been published and has been entitled as " Characterizationof Plasma-Sprayed Hydroxyapatite/TiO in 2000 to prior art
2Composite coatings " " characterize plasma spray coating HA/TiO
2Composite coating " literary composition, introduced and utilized the plasma spray coating technology to prepare HA/TiO
2Composite coating, thereby the method for the bond strength of raising coating and titanio body storeroom.But, the main cause that causes coating shedding be the hydroxyapatite coating layer thicker (greater than 50 μ m) of plasma spraying preparation crystallization degree is low, porous, particle scale are big, be not resolved yet.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of TiO is provided
2The preparation method of-HA biological medical nanometer structured film.Utilize the reaction magnetocontrol sputtering technology and by in thin film, introducing TiO
2Ceramic component, the adhesive force of enhanced film and matrix Ti sill, the biological activity and the stability under the physiological environment condition of raising thin film.
The present invention is achieved by the following technical solutions, TiO of the present invention
2TiO in the-HA biological medical nanometer structured film
2: HA is 1: 9-9: between 1, Ca: P is 1.6: 1-1.7: between 1, film surface granule average dimension is between 20-80nm, and film thickness is between 20-200nm.Adopt the reaction magnetocontrol sputtering technology, and by in thin film, introducing TiO
2Ceramic component, the bond strength of raising thin film and titanium and alloy material thereof; By adjusting the sputter parameter and in thin film, adding TiO
2Ceramic component, control thin film composition and particle scale improve biological activity and the stability of thin film under typical physiological environment, and concrete steps are as follows:
(1) cleans, dries, fixes pending medical implant base material;
(2) fixing sputtering target material;
(3) baking vacuum chamber, the sputter clean target material surface;
(4) treat that sputter clean is stable after, aerating oxygen, regulate flow-rate ratio, total gas pressure and Ti/HA target sputtering power, Ti target power output, the underlayer temperature of argon flow amount, oxygen flow, argon and oxygen, remove plate washer, rotate substrate, react radio-frequency sputtering Ti/HA target and reaction d.c. sputtering Ti target in turn, coreaction sputters at depositing Ti O on the pending medical implant base material
2-HA laminated film;
(5) after sputtering sedimentation finishes, sample is taken out from vacuum chamber.
Described step (1), specifically: pending medical implant base material was successively inserted in acetone and the ethanol solution ultrasonic cleaning 15 minutes, use deionized water rinsing then, after the oven dry, be fixed on the sample base of magnetic control sputtering system vacuum chamber.
Described step (2), specifically: two titanium targets are separately fixed on two magnetron cathodes in the vacuum chamber, the HA target is placed on one of them titanium target, medical implant base material pending behind the cleaning, drying is fixed on the sample base of magnetic control sputtering system vacuum chamber, the magnetic field intensity in Ti/HA target and Ti target surface sputtering zone is respectively between 2500 Gauss's to 3000 gaussian sums, 2300 Gauss to 2500 Gausses, Ti/HA target surface is 60mm to 110mm to the distance of substrate, and Ti target target surface to the distance of substrate is 60mm to 90mm.
Described step (3), specifically: the baking vacuum chamber, treat that base vacuum is evacuated to 2 * 10
-3During Pa, feed argon, the Ti/HA target is carried out radio-frequency sputtering clean, the Ti target is carried out d.c. sputtering clean, block substrate with plate washer in the sputter clean process, guarantee that the composition that sputters from target material surface in the sputter clean process does not deposit on the substrate.
Described step (4), regulate argon flow amount between 10-45sccm, regulate oxygen flow between 5-30nm, regulate total gas pressure between 1-5Pa, the flow-rate ratio of regulating argon and oxygen is between 1: 3 to 8: 1, regulate Ti/HA target sputtering power between 50-150W, regulate the Ti target power output at 20-80W.Regulate underlayer temperature between 100-400 ℃.
Described step (5), specifically: after sputtering sedimentation finishes, or sample placed annealing furnace, in 400 degrees centigrade of air atmosphere or water vapour atmosphere, kept 5-10 hour, treat that annealing in process finishes after, sample is taken out from annealing furnace.
The present invention becomes film theory according to physical vapour deposition (PVD), selects suitable technological parameter and film forming post processing means, prepares nanostructured TiO at common medical pure titanium or titanium-aluminium alloy implantation material surface
2-HA bio-medical function laminated film.To the film surface composition, the sputtering power that the control of surface particles yardstick and grain size can be by regulating two magnetron cathode targets, air pressure, underlayer temperature and the subsequent anneal temperature controlling realized.Membrane analogy body fluid (Simulated Body Fluid) immersion test viewing film does not come off and peels off, the simulated body fluid pH value does not have significant change, show that the sample biological stability is good, osteoblast culture experiment viewing film has the characteristic that promotes that osteoblast adheres to, sprawls, breeds, and shows that sample has good biological activity.
The present invention has obvious progress, at the deficiencies in the prior art part, by introduce TiO in thin film
2Improve the bond strength of thin film and matrix material, by adjusting sputter parameter control film surface HA granule and TiO
2Particulate yardstick improves biological activity and the stability of thin film under typical physiological environment, has very big application potential.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
To polish medical implant Ti base material and successively insert in acetone and the ethanol solution ultrasonic cleaning 10 minutes, use deionized water rinsing then, dry for standby.Two titanium targets are separately fixed on two magnetron cathodes in the vacuum chamber, and the HA target is placed on one of them titanium target.Medical implant base material pending behind the cleaning, drying is fixed on the sample base of magnetic control sputtering system vacuum chamber.The magnetic field intensity in Ti/HA target and Ti target surface sputtering zone is respectively 2800 gaussian sums, 2400 Gausses, and Ti/HA target surface is 60mm to the distance of substrate, and Ti target target surface to the distance of substrate is 60mm.Toast vacuum chamber before the preparation earlier, treat that base vacuum is evacuated to 2 * 10
-3After Pa is following, feed argon, respectively Ti/HA and Ti target are carried out radio-frequency sputtering and d.c. sputtering cleaning, block substrate with plate washer in the sputter clean process, guarantee that the composition that sputters from target material surface in the sputter clean process does not deposit on the substrate.After treating that sputter clean is stable, aerating oxygen, regulate argon flow amount to 45sccm, oxygen flow to 10sccm, the reaction d.c. sputtering power of total gas pressure to the reaction radio-frequency sputtering power of 4Pa, Ti/HA target to 150W, Ti target is to 50W, underlayer temperature to 400 ℃, sputtering sedimentation TiO
2-HA laminated film.In the sputter procedure, rotate substrate, reactive sputtering Ti/HA target and Ti target in turn at every turn to 5 seconds that were sputtered to of Ti/HA target and Ti target, are divided into other to Ti/HA target and the sputter of Ti target 60 minutes.Sputtering sedimentation takes out sample after finishing from vacuum chamber.
AFM result shows that film surface granule average dimension is about 45nm.AES result shows film thickness 55nm, TiO in the thin film
2: HA is about 2: 5, Ca: P is about 1.65: 1.With sample simulated body fluid (SBF) soak one week the back viewing film do not come off and peel off, the simulated body fluid pH value does not have significant change, shows that the sample biological stability is good.The osteoblast culture experiment shows that sample has good biological activity.
Embodiment 2
To polish medical implant Ti base material and successively insert in acetone and the ethanol solution ultrasonic cleaning 10 minutes, use deionized water rinsing then, dry for standby.Two titanium targets are separately fixed on very aerial two magnetron cathodes, and the HA target is placed on one of them titanium target.Medical implant base material pending behind the cleaning, drying is fixed on the sample base of magnetic control sputtering system vacuum chamber.The magnetic field intensity in Ti/HA target and Ti target surface sputtering zone is respectively 2800 gaussian sums, 2400 Gausses, and Ti/HA target surface is 60mm to the distance of substrate, and Ti target target surface to the distance of substrate is 60mm.Toast vacuum chamber before the preparation earlier, treat that base vacuum is evacuated to 2 * 10
-3After Pa is following, feed argon, respectively Ti/HA and Ti target are carried out radio-frequency sputtering and d.c. sputtering cleaning, block substrate with plate washer in the sputter clean process, guarantee that the composition that sputters from target material surface in the sputter clean process does not deposit on the substrate.After treating that sputter clean is stable, aerating oxygen, regulate argon flow amount to 10sccm, oxygen flow to 30sccm, the reaction d.c. sputtering power of total gas pressure to the reaction radio-frequency sputtering power of 2Pa, Ti/HA target to 100W, Ti target is to 40W, underlayer temperature to 300 ℃, sputtering sedimentation TiO
2-HA laminated film.In the sputter procedure, rotate substrate, reactive sputtering Ti/HA target and Ti target in turn at every turn to 5 seconds that were sputtered to of Ti/HA target and Ti target, are divided into other to Ti/HA target and the sputter of Ti target 60 minutes.Sputtering sedimentation takes out sample after finishing from vacuum chamber.
AFM result shows that film surface granule average dimension is about 40nm.AES result shows that film thickness is 40nm, TiO in the thin film
2: HA is about 1: 2, Ca: P is about 1.7: 1.With sample simulated body fluid (SBF) soak one week the back viewing film do not come off and peel off, the simulated body fluid pH value does not have significant change, shows that the sample biological stability is good.The osteoblast culture experiment shows that sample has good biological activity.
Embodiment 3
To polish medical implant Ti base material and successively insert in acetone and the ethanol solution ultrasonic cleaning 10 minutes, use deionized water rinsing then, dry for standby.Two titanium targets are separately fixed on two magnetron cathodes in the vacuum chamber, and the HA target is placed on one of them titanium target.Medical implant base material pending behind the cleaning, drying is fixed on the sample base of magnetic control sputtering system vacuum chamber.The magnetic field intensity in Ti/HA target and Ti target surface sputtering zone is respectively 2800 gaussian sums, 2400 Gausses, and Ti/HA target surface is 110mm to the distance of substrate, and Ti target target surface to the distance of substrate is 60mm.Toast vacuum chamber before the preparation earlier, treat that base vacuum is evacuated to 2 * 10
-3After Pa is following, feed argon, respectively Ti/HA and Ti target are carried out radio-frequency sputtering and d.c. sputtering cleaning, block substrate with plate washer in the sputter clean process, guarantee that the composition that sputters from target material surface in the sputter clean process does not deposit on the substrate.After treating that sputter clean is stable, aerating oxygen, regulate argon flow amount to 40sccm, oxygen flow to 5sccm, the reaction d.c. sputtering power of total gas pressure to the reaction radio-frequency sputtering power of 3Pa, Ti/HA target to 50W, Ti target is to 80W, underlayer temperature to 400 ℃, sputtering sedimentation TiO
2-HA laminated film.In the sputter procedure, rotate substrate, reactive sputtering Ti/HA target and Ti target to 5 seconds that were sputtered to of Ti/HA target and Ti target, are divided into other to Ti/HA target and Ti target sputter 180 clocks at every turn in turn.Sputtering sedimentation takes out sample after finishing from vacuum chamber, place annealing furnace, is 400 ℃ in temperature, and annealing is 8 hours under the water vapour atmosphere.
AFM result shows that film surface granule average dimension is about 50nm.AES result shows that film thickness is 200nm, TiO in the thin film
2: HA is about 9: 1, Ca: P is about 1.67: 1.With sample simulated body fluid (SBF) soak one week the back viewing film do not come off and peel off, the simulated body fluid pH value does not have significant change, shows that the sample biological stability is good.The osteoblast culture experiment shows that sample has good biological activity.
Embodiment 4
To polish medical implant Ti base material and successively insert in acetone and the ethanol solution ultrasonic cleaning 10 minutes, use deionized water rinsing then, dry for standby.Two titanium targets are separately fixed on two magnetron cathodes in the vacuum chamber, and the HA target is placed on one of them titanium target.Medical implant base material pending behind the cleaning, drying is fixed on the sample base of magnetic control sputtering system vacuum chamber.The magnetic field intensity in Ti/HA target and Ti target surface sputtering zone is respectively 2800 gaussian sums, 2400 Gausses, and Ti/HA target surface is 80mm to the distance of substrate, and Ti target target surface to the distance of substrate is 60mm.Toast vacuum chamber before the preparation earlier, treat that base vacuum is evacuated to 2 * 10
-3After Pa is following, feed argon, respectively Ti/HA and Ti target are carried out radio-frequency sputtering and d.c. sputtering cleaning, block substrate with plate washer in the sputter clean process, guarantee that the composition that sputters from target material surface in the sputter clean process does not deposit on the substrate.After treating that sputter clean is stable, aerating oxygen, regulate argon flow amount to 30sccm, oxygen flow to 5sccm, the reaction d.c. sputtering power of total gas pressure to the reaction radio-frequency sputtering power of 2Pa, Ti/HA target to 150W, Ti target is to 60W, underlayer temperature to 200 ℃, sputtering sedimentation TiO
2-HA laminated film.In the sputter procedure, rotate substrate, reactive sputtering Ti/HA target and Ti target in turn at every turn to 5 seconds that were sputtered to of Ti/HA target and Ti target, are divided into other to Ti/HA target and the sputter of Ti target 60 minutes.Sputtering sedimentation takes out sample after finishing from vacuum chamber, place annealing furnace, is 400 ℃ in temperature, and annealing is 10 hours under the water vapour atmosphere.
AFM result shows that film surface granule average dimension is about 40nm.AES result shows that film thickness is 60nm, TiO in the thin film
2: HA is about 3: 2, Ca: P is about 1.67: 1.With sample simulated body fluid (SBF) soak one week the back viewing film do not come off and peel off, the simulated body fluid pH value does not have significant change, shows that the sample biological stability is good.Cell culture experiments shows that sample has good biological activity.
Embodiment 5
To polish medical implant Ti base material and successively insert in acetone and the ethanol solution ultrasonic cleaning 10 minutes, use deionized water rinsing then, dry for standby.Two titanium targets are separately fixed on two magnetron cathodes in the vacuum chamber, and the HA target is placed on one of them titanium target.Medical implant base material pending behind the cleaning, drying is fixed on the sample base of magnetic control sputtering system vacuum chamber.The magnetic field intensity in Ti/HA target and Ti target surface sputtering zone is respectively 2800 gaussian sums, 2400 Gausses, and Ti/HA target surface is 60mm to the distance of substrate, and Ti target target surface to the distance of substrate is 60mm.Toast vacuum chamber before the preparation earlier, treat that base vacuum is evacuated to 2 * 10
-3After Pa is following, feed argon, respectively Ti/HA and Ti target are carried out radio-frequency sputtering and d.c. sputtering cleaning, block substrate with plate washer in the sputter clean process, guarantee that the composition that sputters from target material surface in the sputter clean process does not deposit on the substrate.After treating that sputter clean is stable, aerating oxygen, regulate argon flow amount to 20sccm, oxygen flow to 30sccm, the reaction d.c. sputtering power of total gas pressure to the reaction radio-frequency sputtering power of 5Pa, Ti/HA target to 80W, Ti target is to 60W, underlayer temperature to 100 ℃, sputtering sedimentation TiO
2-HA laminated film.In the sputter procedure, rotate substrate, reactive sputtering Ti/HA target and Ti target in turn at every turn to 5 seconds that were sputtered to of Ti/HA target and Ti target, are divided into other to Ti/HA target and the sputter of Ti target 60 minutes.Sputtering sedimentation takes out sample after finishing from vacuum chamber, place annealing furnace, is 400 ℃ in temperature, and annealing is 5 hours under the air atmosphere.
AFM result shows that film surface granule average dimension is about 80nm.AES result shows that film thickness is 60nm, TiO in the thin film
2: HA is about 5: 2, Ca: P is about 1.6: 1.With sample simulated body fluid (SBF) soak one week the back viewing film do not come off and peel off, the simulated body fluid pH value does not have significant change, shows that the sample biological stability is good.The osteoblast culture experiment shows that sample has good biological activity.
Embodiment 6
To polish medical implant Ti base material and successively insert in acetone and the ethanol solution ultrasonic cleaning 10 minutes, use deionized water rinsing then, dry for standby.Two titanium targets are separately fixed on very aerial two magnetron cathodes, and the HA target is placed on one of them titanium target.Medical implant base material pending behind the cleaning, drying is fixed on the sample base of magnetic control sputtering system vacuum chamber.The magnetic field intensity in Ti/HA target and Ti target surface sputtering zone is respectively 2800 gaussian sums, 2400 Gausses, and Ti/HA target surface is 60mm to the distance of substrate, and Ti target target surface to the distance of substrate is 90mm.Toast vacuum chamber before the preparation earlier, treat that base vacuum is evacuated to 2 * 10
-3After Pa is following, feed argon, respectively Ti/HA and Ti target are carried out radio-frequency sputtering and d.c. sputtering cleaning, block substrate with plate washer in the sputter clean process, guarantee that the composition that sputters from target material surface in the sputter clean process does not deposit on the substrate.After treating that sputter clean is stable, aerating oxygen, regulate argon flow amount to 15sccm, oxygen flow to 15sccm, the reaction d.c. sputtering power of total gas pressure to the reaction radio-frequency sputtering power of 1Pa, Ti/HA target to 150W, Ti target is to 20W, underlayer temperature to 400 ℃, sputtering sedimentation TiO
2-HA laminated film.In the sputter procedure, rotate substrate, reactive sputtering Ti/HA target and Ti target in turn at every turn to 5 seconds that were sputtered to of Ti/HA target and Ti target, are divided into other to Ti/HA target and the sputter of Ti target 40 minutes.Sputtering sedimentation takes out sample after finishing from vacuum chamber.
AFM result shows that film surface granule average dimension is about 20nm.AES result shows that film thickness is 20nm, TiO in the thin film
2: HA is about 1: 9, Ca: P is about 1.7: 1.With sample simulated body fluid (SBF) soak one week the back viewing film do not come off and peel off, the simulated body fluid pH value does not have significant change, shows that the sample biological stability is good.The osteoblast culture experiment shows that sample has good biological activity.
Claims (10)
1. TiO
2The preparation method of-HA biological medical nanometer structured film is characterized in that, TiO in the described thin film
2: HA is 1: 9-9: between 1, Ca: P is 1.6: 1-1.7: between 1, adopt the reaction magnetocontrol sputtering technology, and by in thin film, introducing TiO
2Ceramic component, the bond strength of raising thin film and titanium and alloy material thereof; By adjusting the sputter parameter and in thin film, adding TiO
2Ceramic component, control thin film composition and particle scale improve biological activity and the stability of thin film under typical physiological environment, and concrete steps are as follows:
(1) cleans, dries, fixes pending medical implant base material;
(2) fixing sputtering target material;
(3) baking vacuum chamber, the sputter clean target material surface;
(4) treat that sputter clean is stable after, aerating oxygen, regulate flow-rate ratio, total gas pressure and Ti/HA target sputtering power, Ti target power output, the underlayer temperature of argon flow amount, oxygen flow, argon and oxygen, remove plate washer, rotate substrate, react radio-frequency sputtering Ti/HA target and reaction d.c. sputtering Ti target in turn, coreaction sputters at depositing Ti O on the pending medical implant base material
2-HA laminated film;
(5) after sputtering sedimentation finishes, sample is taken out from vacuum chamber.
2. TiO according to claim 1
2The preparation method of-HA biological medical nanometer structured film, it is characterized in that, described step (1), specifically: pending medical implant base material was successively inserted in acetone and the ethanol solution ultrasonic cleaning 15 minutes, use deionized water rinsing then, after the oven dry, be fixed on the sample base of magnetic control sputtering system vacuum chamber.
3. TiO according to claim 1
2The preparation method of-HA biological medical nanometer structured film, it is characterized in that, described step (2), specifically: two titanium targets are separately fixed on two magnetron cathodes in the vacuum chamber, the HA target is placed on one of them titanium target, medical implant base material pending behind the cleaning, drying is fixed on the sample base of magnetic control sputtering system vacuum chamber, measures the magnetic field intensity in Ti/HA target and Ti target surface sputtering zone, regulate Ti/HA target surface, Ti target target surface distance to substrate.
4. TiO according to claim 3
2The preparation method of-HA biological medical nanometer structured film is characterized in that, the magnetic field intensity in Ti/HA target and Ti target surface sputtering zone is respectively between 2500 Gauss's to 3000 gaussian sums, 2300 Gauss to 2500 Gausses.
5. TiO according to claim 3
2The preparation method of-HA biological medical nanometer structured film is characterized in that, Ti/HA target surface is 60mm to 110mm to the distance of substrate, and Ti target target surface to the distance of substrate is 60mm to 90mm.
6. TiO according to claim 1
2The preparation method of-HA biological medical nanometer structured film is characterized in that, described step (3), specifically: the baking vacuum chamber, treat that base vacuum is evacuated to 2 * 10
-3During Pa, feed argon, the Ti/HA target is carried out radio-frequency sputtering clean, the Ti target is carried out d.c. sputtering clean, block substrate with plate washer in the sputter clean process, guarantee that the composition that sputters from target material surface in the sputter clean process does not deposit on the substrate.
7. TiO according to claim 1
2The preparation method of-HA biological medical nanometer structured film is characterized in that, described step (4), regulate argon flow amount between 10-45sccm, regulate oxygen flow between 5-30sccm, the flow-rate ratio of argon and oxygen is between 1: 3 to 8: 1, and total gas pressure is between 1-5Pa.
8. according to claim 1 or 7 described TiO
2The preparation method of-HA biological medical nanometer structured film is characterized in that, described step (4), and Ti/HA target sputtering power is between 50-150W, and the Ti target power output is at 20-80W, regulates underlayer temperature between 100-400 ℃.
9. TiO according to claim 1
2The preparation method of-HA biological medical nanometer structured film is characterized in that, after sputtering sedimentation finishes, or sample placed annealing furnace, in 400 degrees centigrade of air atmosphere or water vapour atmosphere, kept 5-10 hour, treat that annealing in process finishes after, sample is taken out from annealing furnace.
10. TiO according to claim 1
2The preparation method of-HA biological medical nanometer structured film is characterized in that, film surface granule average dimension is between 20-80nm, and film thickness is between 20-200nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103993315A (en) * | 2014-06-05 | 2014-08-20 | 山东大学 | Process for preparing Ca/P-TiO2 composite biofilm |
| CN106924811A (en) * | 2017-03-24 | 2017-07-07 | 纳狮新材料股份有限公司 | Composite coating joint prosthesis and preparation method thereof |
| EP3292877A1 (en) * | 2016-09-09 | 2018-03-14 | Universität Basel | Implant or osteosynthesis and method for producing the same |
| CN110079765A (en) * | 2012-06-29 | 2019-08-02 | 西门子公司 | The method for preparing polycrystalline ceramics film |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1118587C (en) * | 2000-12-07 | 2003-08-20 | 杉杉集团有限公司 | Process for preparing hydrophobic rutile film by reinforced and magnetically controlled DC sputtering |
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2005
- 2005-08-11 CN CNB2005100286796A patent/CN100413545C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079765A (en) * | 2012-06-29 | 2019-08-02 | 西门子公司 | The method for preparing polycrystalline ceramics film |
| CN110079765B (en) * | 2012-06-29 | 2021-08-17 | 西门子公司 | Method for producing polycrystalline ceramic membranes |
| CN103993315A (en) * | 2014-06-05 | 2014-08-20 | 山东大学 | Process for preparing Ca/P-TiO2 composite biofilm |
| CN103993315B (en) * | 2014-06-05 | 2016-03-23 | 山东大学 | A kind of CaP-TiO 2the preparation technology of compound bio film |
| EP3292877A1 (en) * | 2016-09-09 | 2018-03-14 | Universität Basel | Implant or osteosynthesis and method for producing the same |
| WO2018046655A1 (en) * | 2016-09-09 | 2018-03-15 | Universität Basel | Implant or osteosynthesis device and method for the production thereof |
| CN106924811A (en) * | 2017-03-24 | 2017-07-07 | 纳狮新材料股份有限公司 | Composite coating joint prosthesis and preparation method thereof |
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| CN100413545C (en) | 2008-08-27 |
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