Summary of the invention
Technical problem to be solved by this invention is, provides a kind of surface roughness that can increase implant material, can not remain again the method for a large amount of harmful shot blasting particles.
And then another technical problem to be solved by this invention is, provide a kind of to human body and the environment liquid blasting treatment technology without harm, its may be used for processing implant material surface and can not the shot blasting particles of residual harmful.
In order to solve above-mentioned technical problem of the present invention, the present invention adopts following technical scheme:
According to an aspect of the present invention, provide a kind of surface at implant material to carry out the method for liquid blasting process, for increasing implant material surface roughness and reduce shot blasting particles remain, the method comprises:
With organic solvent and water cleaning implant material, and the implant material after cleaning is placed in drying baker dry; And
Liquid blasting process is carried out to this implant material surface, obtain the implant material that surface roughness increases, operating pressure wherein for the spray gun of atomizing of liquids mortar is 0.2 ~ 0.7MPa, and the distance between gun slot and surface to be processed is 3 ~ 25cm, and the blasting treatment time is 3 ~ 30 seconds.
According to further embodiment of the present invention, liquid mortar is the unit for uniform suspension comprising shot blasting particles and liquid flux.Preferred described shot blasting particles is selected from least one granule in aluminium sesquioxide, zirconium oxide, ceria, carborundum, titanium dioxide, insoluble phosphate, insoluble calcium phosphate and insoluble magnesium salt.Preferred described liquid flux is at least one solvent be selected from water, ethanol and acetone.
According to further embodiment of the present invention, described implant material is titanium, titanium alloy or polyether-ether-ketone.
According to further embodiment of the present invention, the roughness of the implant surface after liquid blasting process is 12 ~ 50 times of the roughness on the implant material surface after polishing.
According to further embodiment of the present invention, by scanning electron microscopic observation, the implant material surface after liquid blasting process is compared with the implant material surface through dry blasting process, and residual shot blasting particles significantly reduces.
According to another aspect of the present invention, provide a kind of implant material, it is made up of titanium, titanium alloy or polyether-ether-ketone, and by the implant material of method according to the present invention after liquid blasting process.
Carry out the method for liquid blasting process according to the surface at implant material of the present invention, and according to the implant material that the method obtains, have the following advantages:
1. adopt according to the titanium or titanium alloy material of liquid blasting technical finesse of the present invention or polyether-ether-ketone, the granule of its remained on surface significantly reduces, and maintains titanium or titanium alloy material or the good biocompatibility of polyether-ether-ketone simultaneously;
2. adopt liquid blasting treatment technology, be not easy to occur that dust granules flies away, to operator and environment without harm;
3. the titanium implant material after liquid blasting process, does not need to carry out the process such as acid etching, reduces potential hazardness;
4. the roughness through the titanium or titanium alloy surface of liquid blasting process apparently higher than untreated titanium or titanium alloy surface, but a little less than the titanium or titanium alloy material of dry blasting process;
5. method technique of the present invention is simple, does not need complicated chemical experiment through cleaning, the titanium material of liquid blasting process or the rough surface of polyetheretherketonematerials materials.
Detailed description of the invention
According to an aspect of the present invention, provide a kind of method of carrying out liquid blasting process on implant material surface, the method comprises: the implant material using sand papering cutting; With organic solvent and water cleaning, and the implant material after cleaning is placed in drying baker dry; And liquid blasting process is carried out to this material, obtain the implant material that surface roughness increases, operating pressure wherein for the spray gun of atomizing of liquids mortar is 0.2 ~ 0.7MPa, and the distance between gun slot and surface to be processed is 3 ~ 25cm, and the blasting treatment time is 3 ~ 30 seconds.Described spray gun is the spray gun commonly used in the art.Preferably the operating pressure of this spray gun is 0.3 ~ 0.6MPa, is more preferably 0.35 ~ 0.5MPa.Distance further preferably between gun slot and the surface of implant material to be processed is 3.5 ~ 22cm, is more preferably 4 ~ 18cm, is even more preferably 4 ~ 15cm.The time of liquid blasting process is generally 3 ~ 30 seconds, is preferably 3.5 ~ 25 seconds, more preferably 3.5 ~ 20 seconds, is even more preferably 3.5 ~ 15 seconds.
Implant material according to the inventive method process can be pure metallic titanium, comprises the titanium alloy material of Ti-6A1-4V, or polyether-ether-ketone (PEEK).From the viewpoint of the biocompatibility with bone structure, this implant material is preferably purity more than 99.8% and is suitable for use as the Titanium of such as oral implant material, is more preferably pure metallic titanium.
According to the preferred implementation of the inventive method, the described liquid mortar for liquid blasting process of the present invention is the unit for uniform suspension comprising shot blasting particles and liquid flux.Further preferably described shot blasting particles is 5 ~ 30% of described liquid mortar weight, is more preferably 5.5 ~ 21%.According to further preferred embodiment, described shot blasting particles is selected from least one granule in aluminium sesquioxide, zirconium oxide, ceria, carborundum, titanium dioxide, insoluble phosphate, insoluble calcium phosphate and insoluble magnesium salt.More preferably described shot blasting particles is aluminium sesquioxide.According to the further preferred embodiment of the inventive method, the mean diameter of described shot blasting particles is 30 ~ 450 μm, is preferably 35 ~ 300 μm, is more preferably 80 ~ 300 μm.Further preferably, described liquid flux is at least one solvent be selected from water, ethanol and acetone.
According to the preferred embodiment of the present invention, the height of the implant material after cutting is 0.5 ~ 5mm, and diameter is 5 ~ 50mm.According to further preferred embodiment, the present invention uses No. 80, GB respectively, the sand paper of No. 400 and No. 800 is polished.Preferably, the roughness on the surface of the implant material after polishing is 0.1 ~ 0.55 μm.According to further preferred embodiment of the present invention, the roughness on the implant material surface after liquid blasting process is 12 ~ 50 times of the roughness on the implant material surface after polishing.More preferably, the roughness on the titanium surface after liquid blasting process is 12 ~ 50 times of the roughness on the titanium surface after polishing.
According to another aspect of the present invention, provide a kind of implant material, it is by the material with the surface roughness of increase obtained after liquid blasting disposal methods according to the present invention.The surface roughness of described increase refers to the surface roughness of increase compared with the surface with untreated implant material or the material after polishing.From the viewpoint of being suitable for implant material, the surface roughness of preferred described increase is 1.0 ~ 4.5 μm, is more preferably within the scope of 1.0 ~ 3.5 μm, most preferably is within the scope of 1.2 ~ 3.0 μm.Wherein, pass through scanning electron microscopic observation, implant surface after liquid blasting process is compared with the surface of the implant material through dry blasting process, and residual shot blasting particles significantly reduces, and the implant surface even after liquid blasting process does not have the residual of shot blasting particles.Further preferably, be within the scope of 1.0 ~ 3.5 μm by the surface roughness with the material of the surface roughness of increase obtained behind the surface of liquid blasting disposal methods titanium according to the present invention or titanium alloy material, be more preferably within the scope of 1.2 ~ 3.0 μm, be even more preferably 1.2 ~ 2.75 μm.Further, pass through scanning electron microscopic observation, titanium after liquid blasting process or the surface of titanium alloy material are with compared with the titanium of dry blasting process or the surface of titanium alloy material, residual shot blasting particles significantly reduces, and the titanium even after liquid blasting process or the surface of titanium alloy material do not have the residual of shot blasting particles.
Implant material after liquid blasting disposal methods of the present invention, its surface roughness increases, and improves the bonded area of implant material and osseous tissue.Described surface roughness refers to that normally used roughmeter carries out roughness test to the sample that above three kinds of processing methods obtain, and the roughness of the sample of dry blasting process is 15 ~ 50 times of the sample of a grinding process; The roughness of the sample of liquid blasting process is 12 ~ 50 times of the sample of a grinding process.
Have a large amount of particle residue through scanning electron microscope (SEM) display sample after traditional dry blasting process, EDX power spectrum display particle elements remains more; And according to almost not having particle residue or residual particles obviously to reduce after liquid blasting process of the present invention, and EDX power spectrum display particle elements remains considerably less.
Embodiment
Embodiment 1: liquid blasting process titanium implant material surface
First, it is 15mm that pure titanium material is cut into diameter, is highly the sample of 1mm.Then use No. 80, GB successively, the SiC sand paper of No. 400 and No. 800 carries out polishing 8 minutes.Sample after polishing is placed in turn acetone, ethanol cleaning 15 minutes, is then placed in the drying baker of 40 DEG C dry 8 hours.
Utilize roughmeter (TR200, Times Group Co., Beijing) surface roughness of pure titanium sample under room temperature condition after test polishing, its Ra value is 0.114 ± 0.0154 μm, utilize scanning electron microscope (SEM) to observe surface, EDX power spectrum display surface titanium elements accounts for 100%.
Utilize double faced adhesive tape or fixation clamps are pasted by the sample after above-mentioned polishing or are fixed on blasting treatment workbench, liquid blasting process is carried out to pure titanium.Wherein, by percentage by weight, to be the water of 75% and the particle diameter of 25% be sandblasting slurry that the aluminium sesquioxide sand grains of 250-300 μm forms, and this sandblasting slurry is sprayed by lance head, and operating pressure is 0.45MPa, and the working time is 10 seconds, and operating distance is 5cm.
Utilize roughmeter (TR200, Times Group Co., Beijing) to test the surface roughness of the implant material obtained at ambient temperature, Ra value is 1.813 ± 0.084 μm.It is less that SEM shows aluminium sesquioxide residual particles, and EDX power spectrum display surface titanium elements atomic percent is 83.32%, and aluminium element accounts for 4.99%, and oxygen element accounts for 11.69%.
Embodiment 2: the pure titanium implant material surface of liquid blasting process
First, it is 15mm that pure titanium material is cut into diameter, is highly the sample of 1mm.Then use No. 80, GB successively, the SiC sand paper of No. 400 and No. 800 carries out polishing 8 minutes.Sample after polishing is placed in turn acetone, ethanol cleaning 15 minutes, is then placed in the drying baker of 40 DEG C dry 8 hours.
Utilize roughmeter (TR200, Times Group Co., Beijing) surface roughness of pure titanium implant material at ambient temperature after test polishing, its Ra value is 0.114 ± 0.0154 μm, utilize scanning electron microscope (SEM) to observe surface, EDX power spectrum display surface titanium elements accounts for 100%.
Utilize double faced adhesive tape or fixation clamps are pasted by the sample after above-mentioned polishing or are fixed on blasting treatment workbench, liquid blasting process is carried out to titanium.Wherein, the aluminium sesquioxide sand grains that sandblasting slurry is 250-300 μm by the water of percentage by weight 80% and the particle diameter of 20% forms, and this sandblasting slurry is sprayed by lance head, and operating pressure is 0.45MPa, and the working time is 10 seconds, and operating distance is 5cm.
Utilize roughmeter (TR200, Times Group Co., Beijing) to test the surface roughness of the implant material obtained at ambient temperature, Ra value is 1.783 ± 0.084 μm.It is less that SEM shows aluminium sesquioxide residual particles, and EDX power spectrum display surface titanium elements atomic percent is 85.31%, and aluminium element accounts for 4.78%, and oxygen element accounts for 10.91%.
Comparative example 3: the pure titanium implant material of dry blasting process
First, according to the method for embodiment 1 or 2, pure titanium being cut into diameter is 15mm, is highly the sample of 1mm, and uses the SiC sand papering of No. 80, GB, No. 400 and No. 800 successively.Then sample is placed in turn acetone, ethanol ultrasonic cleaning 15 minutes, is then placed in the drying baker of 40 DEG C dry 8 hours.
Utilize double faced adhesive tape or fixation clamps are pasted by sample or are fixed on sand spraying work table, dry blasting process is carried out to titanium sample.Wherein, shot blasting particles to be diameter the be aluminium sesquioxide of 250-300 μm, operating pressure is 0.6Mpa, and the working time is 10 seconds, and operating distance is 5cm.
Sample after dry blasting process to be placed in ethanol and deionized water ultrasonic cleaning successively 15 minutes, to be then placed in drying baker dry 2 hours;
Roughmeter is utilized to test the roughness of the sample surfaces obtained, obtaining surface roughness Ra value is 2.151 ± 0.271 μm, scanning electron microscope (SEM) is utilized to observe surface, find that there is more aluminium sesquioxide particle residue on surface, EDX power spectrum display surface titanium elements atomic percent is 34.41%, aluminium element accounts for 22.91%, and oxygen element accounts for 42.68%.
By above embodiment 1-2 and comparative example 1 known, liquid blasting processing method according to the present invention is compared with traditional dry blasting processing method, the shot blasting particles considerably reduced on implant material surface remains, and similarly can increase the surface roughness of implant material simultaneously.
Above specific embodiment is only the preferred embodiment describing the inventive method; the operating pressure of the liquid blasting technology that it uses, working time and operating distance to change; all equivalent transformations carried out according to the principle of the invention, all should not get rid of outside protection scope of the present invention.