CN102525826A - Preparation method for superhydrophilic micro-nano composite dental implant surface - Google Patents
Preparation method for superhydrophilic micro-nano composite dental implant surface Download PDFInfo
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- CN102525826A CN102525826A CN2012100174095A CN201210017409A CN102525826A CN 102525826 A CN102525826 A CN 102525826A CN 2012100174095 A CN2012100174095 A CN 2012100174095A CN 201210017409 A CN201210017409 A CN 201210017409A CN 102525826 A CN102525826 A CN 102525826A
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Abstract
The invention provides a preparation method for a superhydrophilic micro-nano composite dental implant surface. The preparation method comprises the following steps: coarsening the dental implant surface through sand blasting to obtain a large-sized fluctuant structure; performing acid-etching pretreatment to obtain a dental implant surface micro-scale composite structure; washing the treated implant with a large amount of water, so that one layer of holes of about 1 micron can be covered on the fluctuation of dozens of micro-scale of the implant surface; and performing secondary acid-etching to cover one layer of nano-scale particle structure on the micro-scale structure of the implant surface so as to form the implant surface with a micro-nano composite structure. The implant surface has a micro-nano multi-size composite structure and can obviously promote osseointegration of the dental implant.
Description
Technical field
The invention belongs to medical material manufacturing technology field, relate to a kind of method for preparing with the compound dental implant surface of ultra hydrophilic micro-nano.
Background technology
Bone integration (Osteointegration) theory that is proposed by professor Branemark is the core theory in tooth-planting field.Implantation body and surrounding bone tissue realize that synostosis is one of major criterion of estimating the plantation success or not.The surface texture of implantation body is one of most important factor that influences implant osseointegration.At present clinically, widely used implantation body all has rough surface, compares with the implantation body of smooth surface, and these implantation bodys have shown that all bone is integrated and secular clinical implantation body success rate fast.Therefore, the research and development of the implantation body of matsurface are one of the core directions in tooth implant field always.
Discover; The surface that micron rises and falls is to the facilitation that has of implant osseointegration; We discover; Further the nano level structure of etching can be given implant surface with ultra hydrophilic effect on micro-meter scale, and the surface of this Superhydrophilic can further promote the bone integration of implantation body.
Summary of the invention
The purpose of this invention is to provide the method for preparing of the compound dental implant surface of a kind of ultra hydrophilic micro-nano, realize through following steps:
(1) sandblast: slick titanium or titanium alloy sheet or titanium implant surface are carried out blasting treatment with 20-80 purpose corundum, aluminium oxide, white alumina, carborundum, green silicon carbide, pink aluminium oxide, shot-peening bead, the pill of aluminium, steel sand, steel ball, plastics sand, resin sand, Semen Juglandis sand, cerium oxide or zirconium oxide etc.; Blasting pressure is 4-8bar; Optimum pressure is 4-6bar; Wherein 40-60 order sand is best; The sandblast time is 10-600 second, and the wherein best sandblast time is 30-150 second;
(2) preparatory acid etching: titanium after the sandblast or titanium alloy sheet or titanium implant are distinguished supersound process 15min with acetone, ethanol and water successively, then, and reuse sulphuric acid (H
2SO
4) and the mixed solution of hydrochloric acid (HCl) handle, the processing time is 30 seconds-180 seconds, wherein the optimization process time is 50-80 second; Solution temperature is 90-110 ℃; Wherein optimum temperature is 99-103 a ℃ of solution, and wherein vitriolic mass concentration is 30%-80% in the mixed solution, and the mass concentration of hydrochloric acid is 1%-8%; Vitriolic optimum concentration range is 45%-55%, and the optimum concentration range of hydrochloric acid is 2.5-5%.Implantation body after the processing is directly with big water gaging flushing.Can in tens micron-sized fluctuatings of implant surface, cover the hole of about 1 micron of one deck like this;
(3) secondary acid etching: it is 98% H that the titanium behind acid etching or titanium alloy sheet or titanium implant surface are used mass concentration
2SO
4Solution and mass concentration are 30% H
2O
2Mixed acid solution handle, wherein concentration is 98% H in the mixed solution
2SO
4Solution and 30% H
2O
2The volume ratio of solution is 7:3-3:7, and wherein optimal proportion is 6:4-4:6; The temperature of mixed solution is 1-40 ℃, and optimum temperature is 20-30 ℃; The titanium implant surface processing time is 5-60min, and wherein Best Times is 10-40min.After handling like this, on implant surface micron order structure, cover the nano level grain structure of one deck again, formed the implant surface that contains micro-nano compound structure.
The present invention provides a kind of method for preparing with ultra hydrophilic micro-nano composite plant surface; This method is come the alligatoring implant surface through sandblast; Obtain the relief fabric of large scale; Give implant surface micron order composite construction through preparatory acid etching then, give the implant surface micro-nano compound multiple dimensioned composite construction through the secondary acid etching at last, this surface can significantly promote the generation of implant osseointegration.
Description of drawings
Fig. 1 is the figuratrix of two groups of titanium sheets.
Fig. 2 is cell adhesion, the propagation situation of two groups of titanium sheets.
Fig. 3 is cell Bone Gla protein (OC) secretion situation on two groups of titanium sheets.
Fig. 4 is the interior torsion result of body with the titanium implant on two stack features surface, and RTQ represents the torque value size.
The specific embodiment
The present invention combines embodiment to be further described; Because the present invention can permanent implanted implant surface make up in all bodies; Thereby can realize the quick bone integration between implant and sclerous tissues; And improve plantation success rate at a specified future date, therefore, in other bodies on the permanent implanted implant surface with the constructed this coating of the present invention all within protection scope of the present invention.Embodiments of the invention are just explained characteristic of the present invention for better, and not exclusively comprise the content of protecting of this patent.
Embodiment one
Ganoid implantation body, evenly sprayed 1 minute under 5bar pressure with 40-60 order corundum, and the implantation body after the spraying uses acetone, ethanol and pure water respectively under ultrasonic situation, cleaned 15min, and a large amount of then pure water are cleaned, and nitrogen dries up.Obtain tens to tens microns macrorelief.
Implantation body after drying up directly puts into the mixed solution of ebullient sulphuric acid and hydrochloric acid, and wherein vitriolic mass concentration is 50%, and the mass concentration of hydrochloric acid is to take out after 3%, 60 second, cleans up with a large amount of pure water rapidly.Obtain about 1 micron pore space structure.
The implantation body that handles well is put into the H that volume ratio is 1:1
2SO
4(98%) and H
2O
2(30%) in the mixed solution, handled 30 minutes under the room temperature.Handle the back and directly use massive laundering, on original micron pore space structure, obtain nano level relief fabric, thereby obtain micro-nano composite plant surface.
Embodiment two
Ganoid implantation body, evenly sprayed 1 minute under 5bar pressure with 40-60 order corundum, and the implantation body after the spraying uses acetone, ethanol and pure water respectively under ultrasonic situation, cleaned 15min, and a large amount of then pure water are cleaned, and nitrogen dries up.Obtain tens to tens microns macrorelief.
Implantation body after drying up directly puts into the mixed solution of ebullient sulphuric acid and hydrochloric acid, and wherein vitriolic mass concentration is 50%, and the mass concentration of hydrochloric acid is to take out after 3%, 60 second, cleans up with a large amount of pure water rapidly.Obtain about 1 micron pore space structure.
The implantation body that handles well is put into the H that volume ratio is 6:4
2SO
4(98%) and H
2O
2(30%) in the mixed solution, handled 25 minutes under the room temperature.Handle the back and directly use massive laundering, on original micron pore space structure, obtain nano level relief fabric, thereby obtain micro-nano composite plant surface.
Embodiment three
Ganoid implantation body, evenly sprayed 1 minute under 5bar pressure with 40-60 order corundum, and the implantation body after the spraying uses acetone, ethanol and pure water respectively under ultrasonic situation, cleaned 15min, and a large amount of then pure water are cleaned, and nitrogen dries up.Obtain tens to tens microns macrorelief.
Implantation body after drying up directly puts into the mixed solution of ebullient sulphuric acid and hydrochloric acid, and wherein vitriolic mass concentration is 50%, and the mass concentration of hydrochloric acid is to take out after 3%, 60 second, cleans up with a large amount of pure water rapidly.Obtain about 1 micron pore space structure.
The implantation body that handles well is put into the H that volume ratio is 4:6
2SO
4(98%) and H
2O
2(30%) in the mixed solution, handled 30 minutes under the room temperature.Handle the back and directly use massive laundering, on original micron pore space structure, obtain nano level relief fabric, thereby obtain micro-nano composite plant surface.
Embodiment four
Ganoid implantation body, evenly sprayed 2 minutes under 4bar pressure with 40-60 order corundum, and the implantation body after the spraying uses acetone, ethanol and pure water respectively under ultrasonic situation, cleaned 15min, and a large amount of then pure water are cleaned, and nitrogen dries up.Obtain tens to tens microns macrorelief.
Implantation body after drying up directly puts into the sulphuric acid of 95 ° of C and the mixed solution of hydrochloric acid, and wherein vitriolic mass concentration is 50%, and the mass concentration of hydrochloric acid is to take out after 3%, 80 second, cleans up with a large amount of pure water rapidly.Obtain about 1 micron pore space structure.
The implantation body that handles well is put into the H that volume ratio is 1:1
2SO
4(98%) and H
2O
2(30%) in the mixed solution, handled 30 minutes under the room temperature.Handle the back and directly use massive laundering, on original micron pore space structure, obtain nano level relief fabric, thereby obtain micro-nano composite plant surface.
Embodiment five
Ganoid implantation body, evenly sprayed 2 minutes under 4bar pressure with 40-60 order corundum, and the implantation body after the spraying uses acetone, ethanol and pure water respectively under ultrasonic situation, cleaned 15min, and a large amount of then pure water are cleaned, and nitrogen dries up.Obtain tens to tens microns macrorelief.
Implantation body after drying up directly puts into the mixed solution of ebullient sulphuric acid and hydrochloric acid, and wherein vitriolic mass concentration is 60%, and the mass concentration of hydrochloric acid is to take out after 2.5%, 55 second, cleans up with a large amount of pure water rapidly.Obtain about 1 micron pore space structure.
The implantation body that handles well is put into the H that volume ratio is 1:1
2SO
4(98%) and H
2O
2(30%) in the mixed solution, handled 30 minutes under the room temperature.Handle the back and directly use massive laundering, on original micron pore space structure, obtain nano level relief fabric, thereby obtain micro-nano composite plant surface.
Embodiment six
Ganoid implantation body, evenly sprayed 2 minutes under 4bar pressure with 40-60 order corundum, and the implantation body after the spraying uses acetone, ethanol and pure water respectively under ultrasonic situation, cleaned 15min, and a large amount of then pure water are cleaned, and nitrogen dries up.Obtain tens to tens microns macrorelief.
Implantation body after drying up directly puts into the sulphuric acid of 102 ° of C and the mixed solution of hydrochloric acid, and wherein vitriolic mass concentration is 50%, and the mass concentration of hydrochloric acid is to take out after 4%, 60 second, cleans up with a large amount of pure water rapidly.Obtain about 1 micron pore space structure.
The implantation body that handles well is put into the H that volume ratio is 1:1
2SO
4(98%) and H
2O
2(30%) in the mixed solution, handled 30 minutes under the room temperature.Handle the back and directly use massive laundering, on original micron pore space structure, obtain nano level relief fabric, thereby obtain micro-nano composite plant surface.
Embodiment seven
Ganoid implantation body, evenly sprayed 1 minute under 6bar pressure with 40-60 order corundum, and the implantation body after the spraying uses acetone, ethanol and pure water respectively under ultrasonic situation, cleaned 15min, and a large amount of then pure water are cleaned, and nitrogen dries up.Obtain tens to tens microns macrorelief.
Implantation body after drying up directly puts into the mixed solution of ebullient sulphuric acid and hydrochloric acid, and wherein vitriolic mass concentration is 45%, and the mass concentration of hydrochloric acid is to take out after 5%, 60 second, cleans up with a large amount of pure water rapidly.Obtain about 1 micron pore space structure.
The implantation body that handles well is put into the H that volume ratio is 1:1
2SO
4(98%) and H
2O
2(30%) in the mixed solution, handled 30 minutes under the room temperature.Handle the back and directly use massive laundering, on original micron pore space structure, obtain nano level relief fabric, thereby obtain micro-nano composite plant surface.
Embodiment eight
Ganoid implantation body, evenly sprayed 1 minute under 6bar pressure with 40-60 order corundum, and the implantation body after the spraying uses acetone, ethanol and pure water respectively under ultrasonic situation, cleaned 15min, and a large amount of then pure water are cleaned, and nitrogen dries up.Obtain tens to tens microns macrorelief.
Implantation body after drying up directly puts into the mixed solution of ebullient sulphuric acid and hydrochloric acid, and wherein vitriolic mass concentration is 65%, and the mass concentration of hydrochloric acid is to take out after 2%, 60 second, cleans up with a large amount of pure water rapidly.Obtain about 1 micron pore space structure.
The implantation body that handles well is put into the H that volume ratio is 1:1
2SO
4(98%) and H
2O
2(30%) in the mixed solution, handled 30 minutes under the room temperature.Handle the back and directly use massive laundering, on original micron pore space structure, obtain nano level relief fabric, thereby obtain micro-nano composite plant surface.
Embodiment nine
Ganoid implantation body, evenly sprayed 1 minute under 6bar pressure with 40-60 order corundum, and the implantation body after the spraying uses acetone, ethanol and pure water respectively under ultrasonic situation, cleaned 15min, and a large amount of then pure water are cleaned, and nitrogen dries up.Obtain tens to tens microns macrorelief.
Implantation body after drying up directly puts into the mixed solution of ebullient sulphuric acid and hydrochloric acid, and wherein vitriolic mass concentration is 50%, and the mass concentration of hydrochloric acid is to take out after 3%, 70 second, cleans up with a large amount of pure water rapidly.Obtain about 1 micron pore space structure.
The implantation body that handles well is put into the H that volume ratio is 1:1
2SO
4(98%) and H
2O
2(30%) in the mixed solution, handled 30 minutes under the room temperature.Handle the back and directly use massive laundering, on original micron pore space structure, obtain nano level relief fabric, thereby obtain micro-nano composite plant surface.
Embodiment ten
The implant surface that obtains among nine top embodiment is all carried out contact angle to be characterized; Every group of 5 samples, each sample five test positions that get on independently carry out the static contact angle test, and the result gets the meansigma methods of several groups of data; Discover that their contact angle all is 0.Show that these nine kinds of surfaces all have Superhydrophilic.
Embodiment 11
Electronic scanner microscope is carried out on surface among the embodiment one observe, the result is referring to Fig. 1, A among the figure: the acid etching group of sandblast+in advance, and B is the partial enlarged drawing of figure A; C: sandblast+preparatory acid etching+secondary acid etching group, D is the partial enlarged drawing of figure C.
Embodiment 12
Resulting micro-nano composite surface is to the influence of MC3T3 cell adhesion, propagation behavior among the embodiment one.Research shows, the adhesion of the acid etching group of sandblast+in advance is than sandblast+the adhesion situation of acid etching+secondary acid etching group is poor in advance, and at 1 hour, putting with 7 days testing time in 3 days all had statistical significance.The result is referring to Fig. 2.
Embodiment 13
The influence that resulting micro-nano composite surface is expressed MC3T3 cell Bone Gla protein (OC) among the embodiment one.The result finds, the OC of the acid etching group of sandblast+in advance during two weeks excretory amount be less than the amount of acid etching+secondary acid etching group of sandblast+in advance, statistical significance is arranged.The result is referring to Fig. 3.
Test in embodiment ten limbs
New zealand rabbit is as laboratory animal, implants biological effect in the body that implantation body is used to estimate the implantation body after coating modified at the bilateral femur distal end of bull rabbit.Respectively 2,4 and 8 weeks after implantation body implants, adopt portable digital torsional test appearance to analyze the adhesion (RTQ value) of implantation body and osseous tissue.The torque value size is represented the adhesion size.Experimental result shows, each time point after implantation body implants, and implantation body's synosteosis power of experimental group is greater than matched group.(" * " represent P 0.05, experimental group and the contrast between difference have statistical significance).The result is referring to Fig. 4.
Claims (4)
1. the method for preparing of the compound dental implant surface of ultra hydrophilic micro-nano is characterized in that, realizes through following steps:
(1) sandblast: slick titanium or titanium alloy sheet or titanium implant surface are carried out blasting treatment with 20-80 purpose corundum, aluminium oxide, white alumina, carborundum, green silicon carbide, pink aluminium oxide, shot-peening bead, the pill of aluminium, steel sand, steel ball, plastics sand, resin sand, Semen Juglandis sand, cerium oxide or zirconium oxide; Blasting pressure is 4-8bar, and the sandblast time is 10-600 second;
(2) preparatory acid etching: titanium after the sandblast or titanium alloy sheet or titanium implant are distinguished supersound process 15 minutes with acetone, ethanol and water successively; Then, the mixed solution of reuse sulphuric acid and hydrochloric acid is handled, and the processing time is 30 seconds-180 seconds; Solution temperature is 90-110 ℃; Wherein vitriolic mass concentration is 30%-80% in the mixed solution, and the mass concentration of hydrochloric acid is 1%-8%, and titanium after the processing or titanium alloy sheet or tooth implant are directly with big water gaging flushing;
(3) secondary acid etching: it is 98% H that the titanium behind acid etching or titanium alloy sheet or titanium implant surface are used mass concentration
2SO
4Solution and mass concentration are 30% H
2O
2Mixed acid solution handle, wherein concentration is 98% H in the mixed solution
2SO
4Solution and 30% H
2O
2The volume ratio of solution is 7:3-3:7, and the temperature of mixed solution is 1-40 ℃, and the surface treatment time is 5-60 minute.
2. the method for preparing of the compound dental implant surface of a kind of ultra hydrophilic micro-nano according to claim 1; It is characterized in that; Step (1) is middle with 40-60 purpose corundum, aluminium oxide, white alumina, carborundum, green silicon carbide, pink aluminium oxide, shot-peening bead, the pill of aluminium, steel sand, steel ball, plastics sand, resin sand, Semen Juglandis sand, cerium oxide or zirconium oxide sandblast; Blasting pressure is 4-6bar, and the sandblast time is 30-150 second.
3. the method for preparing of the compound dental implant surface of a kind of ultra hydrophilic micro-nano according to claim 1; It is characterized in that; The mixed solution processing time of reuse sulphuric acid and hydrochloric acid is 50-80 second in the step (2); Solution temperature is 99-103 ℃, and wherein vitriolic mass concentration is 45%-55% in the mixed solution, and the mass concentration of hydrochloric acid is 2.5-5%.
4. the method for preparing of the compound dental implant surface of a kind of ultra hydrophilic micro-nano according to claim 1 is characterized in that, concentration is 98% H in the middle mixed solution of step (3)
2SO
4Solution and 30% H
2O
2The volume ratio of solution is 6:4-4:6, and the temperature of mixed solution is 20-30 ℃, and the surface treatment time is 10-40 minute.
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| CN102912349A (en) * | 2012-10-19 | 2013-02-06 | 浙江大学 | Preparation method of titanium implant surface with micro-nano composite structure |
| CN103006339A (en) * | 2012-12-13 | 2013-04-03 | 大连理工（营口）新材料工程中心有限公司 | Preparation method of multilevel cellular structure for medical pure titanium implant surface |
| CN103341210A (en) * | 2013-05-14 | 2013-10-09 | 中国人民解放军第四军医大学 | Preparation method of anti-osteoporotic micro/nano biomimetic coating of bone implant |
| CN103981523A (en) * | 2014-04-28 | 2014-08-13 | 大连大学 | Surface sand-blasting and acid-etching treatment method of super-hydrophilic Ti6Ai7Ni |
| CN104975335A (en) * | 2015-06-04 | 2015-10-14 | 西北有色金属研究院 | Preparation method of composite coating on surface of titanium alloy dental implant |
| CN105441960A (en) * | 2014-08-22 | 2016-03-30 | 广州中国科学院先进技术研究所 | Method for constructing micrometer/nanometer hierarchical structure with super hydrophilicity on surface of titanium dental implant |
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| CN104451684B (en) * | 2014-09-27 | 2017-02-15 | 浙江大学 | Method for constructing surface of bionic multifunctional titanium-based implant |
| CN106890357A (en) * | 2017-01-11 | 2017-06-27 | 浙江大学 | One kind stabilization and high performance implant surface preparation method |
| CN107345300A (en) * | 2017-06-01 | 2017-11-14 | 成都贝施美生物科技有限公司 | Planting body double acid-etching technique |
| CN107447216A (en) * | 2017-08-08 | 2017-12-08 | 江苏创英医疗器械有限公司 | A kind of dental implant surface processing method and equipment |
| CN107662133A (en) * | 2017-07-27 | 2018-02-06 | 芜湖微云机器人有限公司 | A kind of surface processing technology for dental implant |
| CN108158676A (en) * | 2017-12-22 | 2018-06-15 | 大连三生科技发展有限公司 | A kind of preparation method on the quick osseo-integrated implant surface of concrete dynamic modulus |
| CN108578700A (en) * | 2018-04-25 | 2018-09-28 | 中国人民解放军总医院 | A kind of drug targets for diabetic's implant osseointegration |
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| CN113529158A (en) * | 2021-07-28 | 2021-10-22 | 西北有色金属研究院 | Process for preparing porous structure on surface of TC4 titanium alloy by electrochemical dealloying method |
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