CN104726836A - Titanium metal material surface modifying method and modified titanium metal material - Google Patents
Titanium metal material surface modifying method and modified titanium metal material Download PDFInfo
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Abstract
The invention discloses a titanium metal material surface modifying method and a modified titanium metal material obtained through the method. The method is characterized in that zinc ions and magnesium ions are co-implanted to the surface of a titanium metal material through a plasma immersion ion implantation technology in order to improve the biological activity of the medical titanium metal material. The modified titanium metal material has the characteristics of improved corrosion resistance, good cell spreading performance and increased cell proliferation rate, can promote ossification differentiation of rBMSCs, and has an ossification promotion effect.
Description
Technical field
The invention belongs to medical material tech field, be specifically related to the titanium metal material of a kind of method that surface modification is carried out to titanium metal material and the modification obtained.
Background technology
Surface modification (Surface modification) refers to and processes the surface of material and a kind of technology that its performance is changed, as carburizing (or nitriding), shot-peening, laser treatment, ion implantation, top coat method, anodic oxidation, chemical vapour deposition, physical vapor deposition etc.Wherein, plasma immersion and ion implantation (PIII) technology is the process for modifying surface that is a kind of novel, cheap, non-line-of-sight grown up in the last few years.This technology is by direct for workpiece to be implanted submergence in the plasma, and a series of negative potential pulse is applied relative to vacuum-chamber wall on workpiece, at this moment, just around workpiece, form a plasma sheath constantly expanded/bounce back, electronics at the flows by action of plasma sheath current potential to vacuum-chamber wall, and ion is under the effect of plasma sheath current potential, is accelerated from all directions and is injected into the surface of workpiece, thus realizing the surface modification of material.PIII technology has larger advantage to abnormal workpieces process and batch processing, and this technology has been widely used in the surface modification of the materials such as metal, pottery, semi-conductor and polymkeric substance now.
Titanium or titanium alloy is because having good mechanical property and biocompatibility and being widely used as the embedded material of orthopaedics and dentistry.But Long-term clinical is followed the tracks of and fundamental research finds, the biological activity of titanium or titanium alloy implantation material surface is still not ideal enough, causes implant Integrated implant ability more weak, is combined not strong with surrounding tissue.How to improve the biological activity of medical titanium metal material, improve the Integrated implant ability of implant, become one of focus of embedded material research.
Zinc, as one of required trace element of body vital movement, plays an important role to the hundreds of protein structure of maintenance and function.Zinc participates in various kinds of cell process in cell, such as DNA synthesis, enzymic activity and cell fission (The Journal of Nutrition2000,130:1500-1508.) etc.Research shows, zinc can reach by improving cell proliferation, alkaline phosphatase activities and collagen protein synthesis the effect (Nutrition Research and Practice2010,4:356-361.) promoting skeletonization.Therefore, zine ion Implanted Titanium and alloy surface thereof significantly can improve the biological activity (Acta Biomaterialia2010,6:962-968) of embedded material, thus promote propagation, the differentiation of cell.But the effect of zine ion to cell is mainly manifested in cell and material interactional later stage, the interaction (such as adhere to and sprawl) of cell in early days and between material is poor, need to improve.
Magnesium, as the important element of needed by human, is the cofactor of hundreds of enzyme system.To bioprocess such as protein synthesis, nucleotide metabolism that body weight for humans is wanted, there is positive effect.Magnesium is in cell growth process; be not only cell and energy support is provided; promote protein synthesis; and can promote cell proliferation and can have obvious promoter action to cell Attachment with sprawling, cell growth process is carried out positive protection and is prevented various influence factor to the damage of cell.Research shows, magnesium ion has vital role (Int.J.Oral Maxillofac.Implants2005,20:349 – 359.) to bone remodeling.Magnesium ion injected bio-medical surface of metal titanium by ion implantation technique and can promote that cell is in the early stage response (Biomaterials2006,7:1728-1734.) of implant surfaces, improves the biological activity of embedded material.But magnesium ion is not very desirable to cell and the interaction in material later stage.
Summary of the invention
Single ionic injection is only carried out in the surface that the present invention is based on titanium metal material in prior art, namely only inject zinc or only inject magnesium, the technical problem that its biological activity is still still inadequate, object is to provide a kind of method of titanium metal material being carried out to surface modification newly, method of the present invention is that zine ion and magnesium ion are injected into titanium metal material surface by using plasma immersion ion implantttion technique altogether, obtain the titanium metal material of common note zinc-magnesium modification, thus the biological activity of medical titanium metal material can be improved.
Wherein, described common injection refers to that excitation pulse zinc cathode arc and pulse magnesium cathodic arc plasma source carry out plasma immersion and ion implantation simultaneously.
The processing parameter of described plasma immersion ion implantation technique is preferably: vacuum chamber temperature is 20 ~ 60 DEG C, and background vacuum is 3 × 10
-3~ 4 × 10
-3pa, injecting voltage is-10 ~-40kV, and frequency is 5 ~ 9Hz, and pulsewidth is 50 ~ 450 μ s, and injection length is 0.5 ~ 2.0h altogether.
Described zinc negative electrode is preferably pure zinc negative electrode; Described magnesium negative electrode is preferably pure magnesium negative electrode.
Described titanium metal material be pure titanium as the pure titanium after sandblasting acid treatment, or titanium alloy.
Another object of the present invention is to the titanium metal material of the modification providing a kind of method of the present invention to obtain, wherein, the titanium metal material surface of described modification is injected with zine ion and magnesium ion simultaneously, and namely titanium metal material of the present invention is the titanium metal material of common note zinc-magnesium modification.
The titanium metal material of described modification be pure titanium as the pure titanium after sandblasting acid treatment, or titanium alloy.
Positive progressive effect of the present invention is: the present invention adopts PIII technology zine ion and magnesium ion to be injected into altogether titanium metal material surface to carry out surface modification and obtain the titanium metal material of common note zinc-magnesium modification, its corrosion resistance nature is improved, be conducive to cell Attachment and sprawl, and on cell proliferation and differentiation have good promoter action.Cytoskeleton coloration result confirms, cell is titanium metal material surface spreading better than other materials surface of modification of the present invention; Cell proliferation experiment result confirms, the titanium metal material superficial cell proliferation rate of modification of the present invention is higher than other materials surface; Alkaline phosphatase activities experimental result confirms, the titanium metal material of modification of the present invention can promote rBMSCs cell Osteoblast Differentiation, illustrates that the titanium metal material of modification of the present invention has and promotes skeletonization effect.
Accompanying drawing explanation
Figure 1A ~ 1D is respectively unmodified, note zinc modification, note magnesium-modified and note the scanning electron microscope diagram on titanium metal material surface of zinc-magnesium modification altogether;
Fig. 2 is the contact angle of titanium metal material, wherein, Ti represents unmodified, and Zn-PIII represents note zinc modification, Mg-PIII represents that note is magnesium-modified, and Zn/Mg-PIII represents the modification of common note zinc-magnesium;
Fig. 3 is the corrosion potential figure of titanium metal material, wherein, Zn-PIII represents note zinc modification, and Mg-PIII represents that note is magnesium-modified, and Zn/Mg-PIII represents the modification of common note zinc-magnesium;
Fig. 4 is the cell Attachment of titanium metal material and the Olympus fluorescent microscopy images sprawled, wherein, Ti represents unmodified, Zn-PIII represents note zinc modification, Mg-PIII represents that note is magnesium-modified, Zn/Mg-PIII represents the modification of common note zinc-magnesium, and 1h, 4h and 24h represent cultivation 1 hour, 4 hours and the 24 little results observed constantly respectively;
Fig. 5 is the cell proliferation rate figure of titanium metal material, wherein, Ti represents unmodified, and Zn-PIII represents note zinc modification, Mg-PIII represents that note is magnesium-modified, and Zn/Mg-PIII represents the modification of common note zinc-magnesium;
Fig. 6 is the electron scanning micrograph of the superficial cell pattern of titanium metal material, wherein, Ti represents unmodified, and Zn-PIII represents note zinc modification, Mg-PIII represents that note is magnesium-modified, and Zn/Mg-PIII represents the modification of common note zinc-magnesium;
Fig. 7 A is the Olympus fluorescent microscopy images after the dyeing of the 7th day titanium metal material surface alkalinty Phosphoric acid esterase, and wherein, Ti represents unmodified, Zn-PIII represents note zinc modification, and Mg-PIII represents that note is magnesium-modified, and Zn/Mg-PIII represents the modification of common note zinc-magnesium;
Fig. 7 B is the 7th day titanium metal material surface alkalinty phosphatase activity figure, wherein, Ti represents unmodified, and Zn-PIII represents note zinc modification, Mg-PIII represents that note is magnesium-modified, and Zn/Mg-PIII represents the modification of common note zinc-magnesium;
Fig. 8 A is the Olympus fluorescent microscopy images after titanium metal material surface alkalinty Phosphoric acid esterase dyeing in the 14th day, wherein, Ti represents unmodified, and Zn-PIII represents note zinc modification, Mg-PIII represents that note is magnesium-modified, and Zn/Mg-PIII represents common note zinc-magnesium modification;
Fig. 8 B is the 14th day titanium metal material surface alkalinty phosphatase activity figure, wherein, Ti represents unmodified, and Zn-PIII represents note zinc modification, Mg-PIII represents that note is magnesium-modified, and Zn/Mg-PIII represents the modification of common note zinc-magnesium.
Embodiment
Embodiment 1
The pure titanium sheet of 10mm × 10mm × 1mm will be of a size of through nitration mixture (HF:HNO
3: H
2o=1:5:4, volume ratio) clean 10min after, use alcohol, deionized water and ultrapure water ultrasonic cleaning clean successively, clean 10 ~ 20min, seasoning is stand-by at every turn.Using plasma immersion ion injects (PIII) technology and zinc and magnesium ion is injected into altogether pure titanium surface, concrete technology parameter is as shown in table 1, simultaneously only inject separately zine ion with same processing parameter and only inject separately magnesium ion to pure titanium surface in contrast, obtain respectively the modification of note zinc-magnesium, note zinc modification, note magnesium-modified titanium metal material.As shown in Figure 1, contact angle as shown in Figure 2 for their scanning electronic microscope pattern.
The processing parameter of table 1PIII technology
Note: target represents the titanium metal material in sample table, pulsed arc represents zinc plasma source and Mg plasmas source.
As seen from Figure 1, titanium metal material and the unmodified titanium metal material surface of the common note zinc-magnesium modification that embodiment 1 obtains have no significant difference, note zinc modification and the magnesium-modified titanium metal material surface of note also have no difference, all visible more shallow hole, surface with minute protrusions.
As seen from Figure 2, the contact angle of titanium metal material and the contact angle of unmodified titanium metal material of the common note zinc-magnesium modification that embodiment 1 obtains have no significant difference, be 101.89 ± 1.86 °, the contact angle of the titanium metal material that note zinc modification is magnesium-modified with note also has no difference.
Embodiment 2
The pure titanium sheet of 10mm × 10mm × 1mm will be of a size of through nitration mixture (HF:HNO
3: H
2o=1:5:4, volume ratio) clean 10min after, use alcohol, deionized water and ultrapure water ultrasonic cleaning clean successively, clean 10 ~ 20min, seasoning is stand-by at every turn.Using plasma immersion ion injects (PIII) technology and zinc and magnesium ion is injected into altogether pure titanium surface, concrete technology parameter is as shown in table 2, simultaneously only inject separately zine ion with same processing parameter and only inject separately magnesium ion to pure titanium surface in contrast, obtain respectively the modification of note zinc-magnesium, note zinc modification, note magnesium-modified titanium metal material.
The processing parameter of table 2PIII technology
Note: target represents the titanium metal material in sample table, pulsed arc represents zinc plasma source and Mg plasmas source.
Embodiment 3
The pure titanium sheet of 10mm × 10mm × 1mm will be of a size of through nitration mixture (HF:HNO
3: H
2o=1:5:4, volume ratio) clean 10min after, use alcohol, deionized water and ultrapure water ultrasonic cleaning clean successively, clean 10 ~ 20min, seasoning is stand-by at every turn.Using plasma immersion ion injects (PIII) technology and zinc and magnesium ion is injected into altogether pure titanium surface, concrete technology parameter is as shown in table 3, simultaneously only inject separately zine ion with same processing parameter and only inject separately magnesium ion to pure titanium surface in contrast, obtain respectively the modification of note zinc-magnesium, note zinc modification, note magnesium-modified titanium metal material.
The processing parameter of table 3PIII technology
Note: target represents the titanium metal material in sample table, pulsed arc represents zinc plasma source and Mg plasmas source.
Effect example 1
Corrosion resistant performance test is carried out to the titanium metal material of the modification that embodiment 1 obtains and unmodified titanium metal material (i.e. pure titanium sheet): working electrode is titanium metal material test sample, be graphite rod to electrode, reference electrode is mercurous chloride electrode, utilize electrochemical workstation (using instrument for Shanghai occasion China CHI760C), the corrosion resistant performance of titanium metal material is tested, test voltage is-0.7V ~-0.1V, and result is as shown in Fig. 3.
As seen from Figure 3; the titanium metal material of note zinc modification is relatively unmodified; corrosion potential offsets to negative direction; note magnesium-modified titanium metal material for unmodified; corrosion potential offsets to positive dirction; note the titanium metal material of zinc-magnesium modification altogether for unmodified; corrosion potential also offsets to positive dirction; show that the corrosion resistance nature of the titanium metal material of common note zinc-magnesium modification is enhanced; this is because the zinc noted altogether in the titanium metal material of zinc-magnesium modification is corroded as anode, titanium substrate obtains protection.
Effect example 2
The titanium metal material of modification embodiment 1 obtained and unmodified titanium metal material (i.e. pure titanium sheet) carry out cell Attachment as sample and sprawl experiment: density, after 75% alcohol sterilizing 2h, is 5 × 10 by sample
4the cell suspending liquid 1mL of individual/mL is inoculated in sample surfaces, after cultivating certain hour, cleans sample 2 times with PBS, carry out penetrating with triton after the fixing 10min of 4% paraformaldehyde (PFA), with FITC transfect cell skeleton, DAPI contaminates core, in fluorescence microscopy Microscopic observation, result as shown in Figure 4.
As seen from Figure 4, cell presents the form that spheroidal is not sprawled substantially when 1h is cultivated on titanium metal material surface, the sample surfaces of note zinc modification is compared unmodified surface spreading and must be got well, noting magnesium-modified sample surfaces cell sprawls well, and the sample surfaces cell noting zinc-magnesium modification is altogether sprawled also better; When cultivating 4h, cell is all better sprawled on all titanium metal material surfaces, and the surface of metal titanium noting zinc-magnesium modification altogether compares other surface sprawling advantageously in cell; After cultivating 24h, cell is all sprawled very well, and skeleton is clear, and has a large amount of Actin muscle.
Effect example 3
The titanium metal material of modification embodiment 1 obtained and unmodified titanium metal material (i.e. pure titanium sheet) carry out scleroblast (MC3T3-E1) proliferation experiment as sample: density, after 75% alcohol sterilizing 2h, is 5 × 10 by sample
4the cell suspending liquid 1mL of individual/mL is inoculated in sample surfaces, after cultivating certain hour (1 day, 4 days, 7 days), sample is cleaned 2 times with PBS, what add that 0.5mL contains 10% ALMA indigo plant cultivates 4h further without phenol red medium, then get 100 μ L test the absorbance at 570nm and 600nm wavelength place and calculate cell proliferation rate by reagent specification sheets, result as shown in Figure 5 and Figure 6.
As seen from Figure 5, the titanium metal material superficial cell proliferation rate of 1 day post-modification is cultivated a little more than unmodified; Cultivate the titanium metal material superficial cell proliferation rate noting zinc-magnesium modification for 4 days afterwards altogether and note zinc sample a little more than titanium with independent; Cultivate within 7 days, note zinc-magnesium modification afterwards altogether titanium metal material superficial cell proliferation rate still higher than other samples, illustrate that the titanium metal material surface that the present invention puts into the modification of common note zinc-magnesium can promote osteoblastic proliferation.
As seen from Figure 6, it is better than unmodified that the titanium metal material superficial cell cultivating 1 day post-modification is sprawled, visible a large amount of filopodia; When cultivating 4 days and 7 days, cell is sprawled completely on titanium metal material surface and is had two confluent monolayer cells to cover material surface.
Effect example 4
The titanium metal material of modification embodiment 1 obtained and unmodified titanium metal material (i.e. pure titanium sheet) carry out stem cell alkaline phosphatase activities (ALP) experiment as sample: density, after 75% alcohol sterilizing 2h, is 1.0 × 10 by sample
4individual/mL (7 days) and 0.5 × 10
4the cell suspending liquid 1mL of individual/mL (14 days) is inoculated in sample surfaces, after cultivating certain hour, sample is cleaned 2 times with PBS, sample is immersed in lysate and preserves 40min in 4 DEG C, then cell being preserved 30min in 37 DEG C from sample surfaces wash-out and p-nitrophenyl phosphate, characterizing alkaline phosphatase expression of enzymes by testing it in the absorbancy at 405nm wavelength place.Detect total protein of cell amount by BCA protein method, by calculate with μM/μ g total protein characterizes alkaline phosphatase activities, result is as shown in Figure 7 and Figure 8.
From Fig. 7 A, find that the titanium metal material surface alkalinty Phosphoric acid esterase expression ratio of note zinc modification is unmodified by dyeing will get well, note magnesium-modified titanium metal material surface alkalinty Phosphoric acid esterase express also good than unmodified, and the titanium metal material surface alkalinty Phosphoric acid esterase expression ratio noting zinc-magnesium altogether unmodified, note zinc modification, note magnesium-modified 3 kinds and all will get well.This result is also confirmed further by quantitative result (shown in Fig. 7 B).
From Fig. 8 A, find that the titanium metal material surface alkalinty Phosphoric acid esterase expression ratio of note zinc modification is unmodified good by dyeing, note magnesium-modified titanium metal material surface alkalinty Phosphoric acid esterase expression ratio unmodified good, the titanium metal material surface alkalinty Phosphoric acid esterase expression ratio noting zinc-magnesium is altogether unmodified, note zinc modification, to note three kinds of magnesium-modified materials all good.This result is also confirmed further by quantitative result (as shown in Figure 8 B).And can find, the result of the 7th day and the 14th day result have similar rule, illustrate that the titanium metal material obtained through modification of the present invention significantly can promote the alkaline phosphatase activities of stem cell.
Claims (7)
1. titanium metal material is carried out to a method for surface modification, it is characterized in that, zine ion and magnesium ion are injected into titanium metal material surface by using plasma immersion ion implantttion technique altogether.
2. the method for claim 1, is characterized in that, described common injection refers to that excitation pulse zinc cathode arc and pulse magnesium cathodic arc plasma source carry out plasma immersion and ion implantation simultaneously.
3. the method for claim 1, is characterized in that: the processing parameter of described plasma immersion ion implantation technique is: vacuum chamber temperature is 20 ~ 60 DEG C, and background vacuum is 3 × 10
-3~ 4 × 10
-3pa, injecting voltage is-10 ~-40kV, and frequency is 5 ~ 9Hz, and pulsewidth is 50 ~ 450 μ s, and injection length is 0.5 ~ 2.0h altogether.
4. method as claimed in claim 2, is characterized in that: described zinc negative electrode is pure zinc negative electrode; Described magnesium negative electrode is pure magnesium negative electrode.
5. the method for claim 1, is characterized in that: described titanium metal material is pure titanium or titanium alloy.
6. the titanium metal material of modification that obtains of method according to claim 1, it is characterized in that, the titanium metal material surface of described modification is injected with zine ion and magnesium ion altogether.
7. material as claimed in claim 6, the titanium metal material of described modification is pure titanium or titanium alloy.
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| CN107304472A (en) * | 2016-04-18 | 2017-10-31 | 中国科学院上海硅酸盐研究所 | Have medical titanium-based composite coat of Bone Defect Repari function and anti-microbial property and preparation method thereof concurrently |
| CN107469150A (en) * | 2017-08-07 | 2017-12-15 | 北京大学口腔医学院 | A kind of implantation material for forming built-in electric field and preparation method thereof |
| CN107557715A (en) * | 2017-07-27 | 2018-01-09 | 芜湖微云机器人有限公司 | Improved bioactive metal titanium implant surface modification technology |
| CN107802886A (en) * | 2017-12-12 | 2018-03-16 | 成都育芽科技有限公司 | A kind of 3D printing titanium alloy artificial bone material and preparation method |
| CN107829123A (en) * | 2017-10-09 | 2018-03-23 | 深圳市中科摩方科技有限公司 | A kind of aluminium alloy of surface duplex coating and its preparation method and application |
| CN108838405A (en) * | 2018-07-16 | 2018-11-20 | 刘建光 | A kind of medical artificial tooth |
| CN111876707A (en) * | 2020-08-04 | 2020-11-03 | 安徽理工大学 | Modification method of titanium alloy with bone regeneration promoting and antibacterial functions and modified titanium alloy |
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| CN107304472A (en) * | 2016-04-18 | 2017-10-31 | 中国科学院上海硅酸盐研究所 | Have medical titanium-based composite coat of Bone Defect Repari function and anti-microbial property and preparation method thereof concurrently |
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| CN107469150A (en) * | 2017-08-07 | 2017-12-15 | 北京大学口腔医学院 | A kind of implantation material for forming built-in electric field and preparation method thereof |
| CN107829123A (en) * | 2017-10-09 | 2018-03-23 | 深圳市中科摩方科技有限公司 | A kind of aluminium alloy of surface duplex coating and its preparation method and application |
| CN107802886A (en) * | 2017-12-12 | 2018-03-16 | 成都育芽科技有限公司 | A kind of 3D printing titanium alloy artificial bone material and preparation method |
| CN108838405A (en) * | 2018-07-16 | 2018-11-20 | 刘建光 | A kind of medical artificial tooth |
| CN111876707A (en) * | 2020-08-04 | 2020-11-03 | 安徽理工大学 | Modification method of titanium alloy with bone regeneration promoting and antibacterial functions and modified titanium alloy |
| CN111876707B (en) * | 2020-08-04 | 2021-11-19 | 安徽理工大学 | Modification method of titanium alloy with bone regeneration promoting and antibacterial functions and modified titanium alloy |
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