CN105002546A - Method for preparing wear-resisting biological ceramic film on surface of titanium alloy through micro-arc oxidation - Google Patents
Method for preparing wear-resisting biological ceramic film on surface of titanium alloy through micro-arc oxidation Download PDFInfo
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- CN105002546A CN105002546A CN201510481071.2A CN201510481071A CN105002546A CN 105002546 A CN105002546 A CN 105002546A CN 201510481071 A CN201510481071 A CN 201510481071A CN 105002546 A CN105002546 A CN 105002546A
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Abstract
The invention discloses a method for preparing wear-resisting biological ceramic film on surface of titanium alloy through micro-arc oxidation. The method comprises the steps of pretreatment, staged composite micro-arc oxidation and aftertreatment. According to the method for preparing wear-resisting biological ceramic film on the surface of the titanium alloy through the micro-arc oxidation, micro-size graphite particles are added in a lime acetate-phosphate base electrolyte system, the biological ceramic film with good wear-resisting performance is prepared, the electrolyte is prepared through lime acetate, EDTA-2Na, monopotassium phosphate and micro-size graphite powder, the concentration ratios of the lime acetate, the EDTA-2Na, the monopotassium phosphate and the micro-size graphite powder are 3.5:5.6:1.4:1 to 1.8:2.8:0.7:1. The method for preparing wear-resisting biological ceramic film on the surface of the titanium alloy through the micro-arc oxidation has the advantages that the wear-resisting performance of the micro-oxidation film is improved greatly, and the service life of an implant in a biological tissue can be improved effectively.
Description
Technical field
The invention belongs to metallurgical technology field, be specifically related to a kind of method preparing wear-resisting biological ceramics rete at titanium-alloy surface micro-arc oxidation.
Background technology
Along with the development of modern surgery technology and prosthetic designs, hip replacement (HA) has become the whole hip joint disease in latter stage for the treatment of effective ways the most.Compare conventional metals to polyethylene HA prosthese, metal-on-metal prosthesis (Metal-on-metal, MOM) is with its low wearing and tearing, and the advantages such as low dislocation attract the eyeball of numerous joint surgery doctors.As everyone knows, in MOM design, reactive protein plays a crucial role in metal friction layer, but still little to the understanding of the more basic substances of friction layer.Therefore, develop a kind of prosthetic material that can solve the problems of the technologies described above to be very important.
Summary of the invention
The object of the present invention is to provide a kind of method preparing wear-resisting biological ceramics rete at titanium-alloy surface micro-arc oxidation.
The object of the present invention is achieved like this, comprises pre-treatment, differential arc oxidation, post-processing step, specifically comprise:
A, pre-treatment: titanium alloy sample is carried out surface finish process to specimen surface no marking, dry for standby;
B, differential arc oxidation: hang pretreated titanium alloy sample in the electrolytic solution as anode, stainless steel electrolytic groove, as negative electrode, carries out differential arc oxidation;
C, aftertreatment: the sample deionized water after differential arc oxidation is cleaned, then through ultrasonic washing instrument cleaning, after drying, obtain the titanium material with wear-resisting biological ceramics rete.
The multidigit scientist of the U.S. and Germany constitutes a joint study group, and the structure of matter for MOM friction layer forms the research that runs an experiment, and discloses its research report in 2011 at Science magazine.This result of study confirms, reclaims containing graphite granule in the MOM-HA prosthese metal friction layer of patient, and this will contribute to the reason explaining the low wearing and tearing of MOM prosthese.
The present invention adds micron order graphite granule in lime acetate-phosphoric acid salt basis electrolyte system, prepares the biological stephanoporate ceramic film with excellent abrasive resistance.
Beneficial effect of the present invention:
1, the graphite granule added in the present invention has good oilness, and hardness is high, stable chemical nature, in differential arc oxidation film process, not easily with other ionic reaction.And the interpolation of graphite granule can suppress the propagation of tiny crack, improve membranous layer binding force.Therefore, compare with conventional differential arc oxidation, this rete has good abrasion resistance properties.
2, the graphite granule particle diameter that the present invention adds is 2.5 μm, and less than most of micropore size, therefore, graphite granule can be immersed in tight zone by melt passageway, said minuscule hole in blocking tight zone, thus improves the density of tight zone.When implant is implanted in organism, decrease the chance that the metal ion in titanium alloy substrate outwards dissociates, inhibit the possibility of tissue infection.
3, controllability of the present invention is high, is conducive to controlling, its graphite granule low price, and cost is low, and range of application is comparatively wide, can produce in batches.
Accompanying drawing explanation
Fig. 1 prepares the process flow sheet of abradable porous biological ceramics rete at titanium-alloy surface micro-arc oxidation.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
The method preparing wear-resisting biological ceramics rete at titanium-alloy surface micro-arc oxidation of the present invention, comprises pre-treatment, differential arc oxidation, post-processing step, specifically comprises:
A, pre-treatment: titanium alloy sample is carried out surface finish process to specimen surface no marking, dry for standby;
B, differential arc oxidation: hang pretreated titanium alloy sample in the electrolytic solution as anode, stainless steel electrolytic groove, as negative electrode, carries out differential arc oxidation;
C, aftertreatment: the sample deionized water after differential arc oxidation is cleaned, then through ultrasonic washing instrument cleaning, after drying, obtain the titanium material with wear-resisting biological ceramics rete.
The formula of the electrolytic solution described in step B is lime acetate, EDTA-2Na, potassium primary phosphate and micron order Graphite Powder 99, and its mass concentration ratio is 3.5:5.6:1.4:1 ~ 1.8:2.8:0.7:1.
The power parameter of described differential arc oxidation is: forward current is set as 10 ~ 25A/dm
2, negative current is 5 ~ 10A/dm
2, positive negative duty is 10 ~ 40%, and frequency is 400 ~ 900Hz, and positive negative pulse stuffing number is 1, and oxidization time is 5 ~ 20min.
The temperature of described electrolytic solution in compound micro-arc oxidation process all controls at 10 ~ 30 DEG C.
In micro-arc oxidation process, power supply used is the pulse power; Adopt constant current mode, power parameter is set as: forward current is set as 10 ~ 25A/dm
2, negative current is 5 ~ 10A/dm
2, positive negative duty is 10 ~ 40%, and frequency is 400 ~ 900Hz, and positive negative pulse stuffing number is 1, and oxidization time is 5 ~ 20min.In electrolyzer, the temperature of electrolytic solution is because there being recirculated water, keeps room temperature to get final product (namely 10 ~ 30 DEG C).
With embodiment, the present invention will be further described below:
Embodiment 1
A, pre-treatment: titanium alloy TC 4 is cut into cylindrical titanium material, punch, carry out surface finish process to specimen surface without obvious cut to titanium alloy above sample, and last deionization washing, dries naturally;
B, differential arc oxidation: hung in the electrolytic solution as anode by titanium alloy sample good for pre-treatment, stainless steel electrolytic groove is negative electrode, carries out differential arc oxidation stage by stage.Electrolyte prescription is: lime acetate: 176.18g, EDTA-2Na:279.18g, potassium primary phosphate 68.045g, micron order Graphite Powder 99: 25g, distilled water: 5L.Power parameter is: forward current is set as 10A/dm
2, negative current is 7A/dm
2, positive negative duty is 25%, and frequency is 450Hz, and positive negative pulse stuffing number is 1, and oxidization time is 5min.In electrolyzer, the temperature of electrolytic solution is because there being recirculated water, keeps room temperature.
C, the sample deionized water prepared by differential arc oxidation are cleaned, then are put in ultrasonic washing instrument and clean, final drying.
D, through friction wear testing machine test obtain, this embodiment gained combined oxidation rete abrasion loss is 20% of conventional differential arc oxidation film layer, through SEM observe obtaining, film surface has tiny crack to occur.
Embodiment 2
A, pre-treatment: titanium alloy TC 4 is cut into cylindrical titanium material, punch, carry out surface finish process to specimen surface without obvious cut to titanium alloy above sample, and last deionization washing, dries naturally;
B, differential arc oxidation: hung in the electrolytic solution as anode by titanium alloy sample good for pre-treatment, stainless steel electrolytic groove is negative electrode, carries out differential arc oxidation stage by stage.Electrolyte prescription is: lime acetate: 176.18g, EDTA-2Na:279.18g, potassium primary phosphate 68.045g, micron order Graphite Powder 99: 50g, distilled water: 5L.Power parameter is: forward current is set as 15A/dm
2, negative current is 7A/dm
2, positive negative duty is 40%, and frequency is 600Hz, and positive negative pulse stuffing number is 1, and oxidization time is 10min.In electrolyzer, the temperature of electrolytic solution is because there being recirculated water, keeps room temperature.
C, the sample deionized water prepared by differential arc oxidation are cleaned, then are put in ultrasonic washing instrument and clean, final drying.
D, through friction wear testing machine test obtain, this embodiment gained combined oxidation rete abrasion loss is 35.4% of conventional differential arc oxidation film layer.Observe through SEM and obtain, film surface has a little tiny crack to occur.
Embodiment 3
A, pre-treatment: titanium alloy TC 4 is cut into cylindrical titanium material, punch, carry out surface finish process to specimen surface without obvious cut to titanium alloy above sample, and last deionization washing, dries naturally;
B, differential arc oxidation: hung in the electrolytic solution as anode by titanium alloy sample good for pre-treatment, stainless steel electrolytic groove is negative electrode, carries out differential arc oxidation stage by stage.Electrolyte prescription is: lime acetate: 176.18g, EDTA-2Na:279.18g, potassium primary phosphate 68.045g, micron order Graphite Powder 99: 100g, distilled water: 5L.Power parameter is: forward current is set as 25A/dm
2, negative current is 10A/dm
2, positive negative duty is 40%, and frequency is 900Hz, and positive negative pulse stuffing number is 1, and oxidization time is 20min.In electrolyzer, the temperature of electrolytic solution is because there being recirculated water, keeps room temperature.
C, the sample deionized water prepared by differential arc oxidation are cleaned, then are put in ultrasonic washing instrument and clean, final drying.
D, through friction wear testing machine test obtain, this embodiment gained combined oxidation rete abrasion loss is 53% of conventional differential arc oxidation film layer.Observe through SEM and obtain, film surface has a small amount of tiny crack to occur.
Claims (4)
1. prepare a method for wear-resisting biological ceramics rete at titanium-alloy surface micro-arc oxidation, it is characterized in that comprising pre-treatment, differential arc oxidation, post-processing step, specifically comprise:
A, pre-treatment: titanium alloy sample is carried out surface finish process to specimen surface no marking, dry for standby;
B, differential arc oxidation: hang pretreated titanium alloy sample in the electrolytic solution as anode, stainless steel electrolytic groove, as negative electrode, carries out differential arc oxidation;
C, aftertreatment: the sample deionized water after differential arc oxidation is cleaned, then through ultrasonic washing instrument cleaning, after drying, obtain the titanium material with wear-resisting biological ceramics rete.
2. the method preparing wear-resisting biological ceramics rete at titanium-alloy surface micro-arc oxidation according to claim 1, it is characterized in that the formula of the electrolytic solution described in step B is lime acetate, EDTA-2Na, potassium primary phosphate and micron order Graphite Powder 99, its mass concentration ratio is 3.5:5.6:1.4:1 ~ 1.8:2.8:0.7:1.
3. the method preparing wear-resisting biological ceramics rete at titanium-alloy surface micro-arc oxidation according to claim 1, is characterized in that the power parameter of described differential arc oxidation is: forward current is set as 10 ~ 25A/dm
2, negative current is 5 ~ 10A/dm
2, positive negative duty is 10 ~ 40%, and frequency is 400 ~ 900Hz, and positive negative pulse stuffing number is 1, and oxidization time is 5 ~ 20min.
4. the method preparing wear-resisting biological ceramics rete at titanium-alloy surface micro-arc oxidation according to claim 1, is characterized in that the temperature of described electrolytic solution in compound micro-arc oxidation process all controls at 10 ~ 30 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106222726A (en) * | 2016-09-06 | 2016-12-14 | 南京航空航天大学 | A kind of titanium and alloy surface friction composite coating wear-resisting, low and preparation method thereof thereof |
| CN107115005A (en) * | 2017-03-20 | 2017-09-01 | 武汉苏泊尔炊具有限公司 | Differential arc oxidation non-stick pan and preparation method thereof |
| CN109371444A (en) * | 2018-12-03 | 2019-02-22 | 北京市辐射中心 | Carburizing/oxidation/diamond-like deposition composite film method is quickly prepared for titanium alloy surface |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106222726A (en) * | 2016-09-06 | 2016-12-14 | 南京航空航天大学 | A kind of titanium and alloy surface friction composite coating wear-resisting, low and preparation method thereof thereof |
| CN106222726B (en) * | 2016-09-06 | 2019-02-01 | 南京航空航天大学 | A kind of titanium and its alloy surface is wear-resisting, low friction composite coating and preparation method thereof |
| CN107115005A (en) * | 2017-03-20 | 2017-09-01 | 武汉苏泊尔炊具有限公司 | Differential arc oxidation non-stick pan and preparation method thereof |
| CN109371444A (en) * | 2018-12-03 | 2019-02-22 | 北京市辐射中心 | Carburizing/oxidation/diamond-like deposition composite film method is quickly prepared for titanium alloy surface |
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Application publication date: 20151028 |