CN102031482A - Surface ion nitriding method for medical CoCrMo alloy - Google Patents
Surface ion nitriding method for medical CoCrMo alloy Download PDFInfo
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Abstract
The invention provides a surface ion nitriding method for a medical CoCrMo alloy. The method comprises the following steps of: firstly, polishing the surface of the CoCrMo alloy ground by waterproof abrasive paper, performing ultrasonic cleaning by using alcohol and deionized water, drying for later use; secondly, cleaning the CoCrMo alloy serving as a substrate with argon; and finally, forming a nitride ceramic layer on the surface of the CoCrMo alloy with pure NH3 (ammonia) serving as a gas source by ionic nitriding technology. The nitride layer consists of Cr2N (dichromium nitride) and CrN (chromium nitride) compounds with a compact nanostructure. The surface hardness of the CoCrMo alloy is improved to a certain degree. The nitride layer penetrates into the crystal boundary of the CoCrMo alloy and forms an interlaced net structure with the substrate. The method is simple in process and easy to popularize, effectively improves the wear resistance of the CoCrMo alloy, reduces the release of toxic Co (cobalt) and Cr (chromium) ions, solves the failure problem and has great application potential in the field of biomedicine and the like.
Description
Technical field
The present invention relates to a kind of surface ion nitriding method, especially a kind of preparation hard nitride ceramics layer, realization metallic surface potteryization of being applicable to is to improve the Medical C oCrMo(cobalt chrome molybdenum of its wear resistance and safety in utilization) the alloy surface ion nitriding method.
Background technology
CoCrMo(cobalt chrome molybdenum) alloy is to be the formed sosoloid of fundamental component with the cobalt.Chromium element more in the alloy can form thin and fine and close Cr at alloy surface
2O
3(chromic oxide) zone of oxidation, the corrosion-resistant and wear resistance of raising alloy.Though CoCrMo(cobalt chrome molybdenum) alloy is because of its excellent biological compatibility, corrosion-resistant and abrasion resistance properties, be widely used in the manufacturing of artificial hip and knee-joint prosthesis, but still had CoCrMo(cobalt chrome molybdenum clinically) wearing and tearing and the metal ion Co(cobalt of alloy), Cr(chromium) etc. the release problem.Long-term research behind the artificial joint replacement shows, the wear particle that the metal ion of these genotoxic potentials and wearing and tearing produce can spread by tissue migration, is to cause the bone dissolving of local interface, cause prosthese aseptic loosening, and then the major cause that causes the prosthetic replacement to fail.
Process for modifying surface can improve CoCrMo(cobalt chrome molybdenum) when alloy wear-resisting decreases performance, effectively reduce or stop the release of metal ion to the implanting prosthetic surrounding tissue.In the process for treating surface of having developed, it is ion implantation studying more, and nitrogen is ion implantation can be at CoCrMo(cobalt chrome molybdenum) alloy surface forms hard nitride input horizon, and improve wear resisting property and reduce the release of harmful ion.But the ion implantation thickness of nitrogen is limited, and the input horizon degree of depth under 50 ~ 100keV has only 0.1 ~ 0.2 μ m, and for the hip and the knee-joint prosthesis of load-bearing and frequent motion, the infiltration layer of this thickness is difficult to meet the demands.Because prosthese is under the effect of bearing load and friction, thin nitrogen ion implanted layer is worn easily, has finally caused CoCrMo(cobalt chrome molybdenum) alloy exposes out, and can not play effectively wear-resisting and prevent the effect that harmful ion discharges.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of Medical C oCrMo(cobalt chrome molybdenum) alloy surface ion nitriding method, by to Medical C oCrMo(cobalt chrome molybdenum) alloy surface carries out ion Plasma Nitriding Treatment, thereby obtain high rigidity and have certain thickness nitride ceramics layer, can significantly improve CoCrMo(cobalt chrome molybdenum) wearability and the safety in utilization of alloy prosthese, and then improve CoCrMo(cobalt chrome molybdenum) work-ing life of alloy prosthese.
Technical scheme: alloy surface ion nitriding method Medical C oCrMo(cobalt chrome molybdenum of the present invention) may further comprise the steps:
A, with Medical C oCrMo(cobalt chrome molybdenum) alloy surface polishes successively with the multiple waterproof abrasive paper of different model earlier, the method reduction CoCrMo(cobalt chrome molybdenum by mechanical polishing then) surfaceness of alloy is to 15nm;
B, the CoCrMo(cobalt chrome molybdenum after will polishing) alloy immerses ultrasonic cleaning in the spirit solvent, and to remove the alloy surface dirt, put into stoving oven afterwards and dry;
C, with dried Medical C oCrMo(cobalt chrome molybdenum) alloy puts into the reaction chamber of ion nitriding furnace, reaction chamber is vacuumized, when the air pressure of reaction chamber is lower than 0.1Pa, in reaction chamber, feed argon gas, to Medical C oCrMo(cobalt chrome molybdenum) alloy carries out sputter clean, cleaning is carried out in the process that reaction chamber heats up synchronously, after intensification reaches predetermined ion nitriding temperature, stops sputter clean;
Argon gas in d, the extraction reaction chamber feeds NH in reaction chamber
3(ammonia), control reaction chamber gaseous tension, ion nitriding temperature, sparking voltage, current density were incubated after 8 ~ 10 hours, and stove is chilled to 100 ℃ and comes out of the stove.
The multiple waterproof abrasive paper of described different model is respectively 180
#, 400
#, 800
#, 1200
#Waterproof abrasive paper; The time of ultrasonic cleaning is 10 ~ 20min in the described immersion spirit solvent; Described to put into the temperature that stoving oven dries be 60 ℃, and the time of oven dry is 10 hours; Described to Medical C oCrMo(cobalt chrome molybdenum) air pressure of reaction chamber was 90 ~ 150Pa when alloy carried out sputter clean, sparking voltage is 480 ~ 530V; Described feeding NH
3The reaction chamber gaseous tension is controlled at 400 ~ 500Pa when (ammonia), and the ion nitriding temperature is 750 ~ 850 ℃, and sparking voltage is 550 ~ 600V, and current density is 4 ~ 5mA/cm
2
Beneficial effect: owing to adopt such scheme, after the ion nitriding, CoCrMo(cobalt chrome molybdenum) alloy surface has formed nanostructure nitrogenize layer---the Cr with certain thickness densification
2The N(dichromium nitride) and the CrN(chromium nitride) the hard compounds layer, can effectively improve CoCrMo(cobalt chrome molybdenum) surface hardness of alloy.And nitride layer is deep into CoCrMo(cobalt chrome molybdenum) in the crystal boundary of alloy, form interlacing reticulated structure with matrix, this combination will inevitably be brought the good mechanical bonding properties.Therefore, after the ion nitriding, the high rigidity that certain thickness nitride layer had and with CoCrMo(cobalt chrome molybdenum) the netted combination of alloy substrate, after having guaranteed ion nitriding, Medical C oCrMo(cobalt chrome molybdenum) the obvious raising of the wearability of alloy prosthese and safety in utilization, reached the purpose of invention, and had the following advantages:
1. form interlacing reticulated structure feature between nitride ceramics layer of the present invention and the matrix, well solved nitride layer and CoCrMo(cobalt chrome molybdenum) bonding state problem between alloy;
2. nitride layer combines with the netted of matrix, can effectively improve CoCrMo(cobalt chrome molybdenum) supporting capacity and the abrasion resistance properties of alloy, reduce poisonous ionic and discharge;
3. preparation technology of the present invention is simple, and cost is low, is with a wide range of applications in fields such as bio-medicals.
Description of drawings
Fig. 1 is ion nitriding layer scanning electronic microscope of the present invention (SEM) photo.
Fig. 2 is profile scanning electron microscope (SEM) photo of nitride layer of the present invention and matrix bond.
Fig. 3 is X-ray diffraction (XRD) spectrogram that the present invention prepares nitride layer.
Fig. 4 is the microhardness histogram of the nitride layer for preparing of the present invention.
Fig. 5 is ion nitriding sample and the wear rate figure of untreated samples under the different experiments load-up condition that the present invention prepares.
Fig. 6 is scanning electronic microscope (SEM) the microscopic appearance photo on the eroded area surface of the ion nitriding sample for preparing of the present invention.
Fig. 7 is scanning electronic microscope (SEM) the microscopic appearance photo on eroded area surface that does not carry out the sample of ion Plasma Nitriding Treatment.
Embodiment
Embodiment one, with 180
#, 400
#, 800
#, 1200
#The waterproof abrasive paper Medical C oCrMo(cobalt chrome molybdenum of polishing successively) alloy surface, method by mechanical polishing reduces CoCrMo(cobalt chrome molybdenum then) surfaceness of alloy is to 15nm, polishing back spirit solvent ultrasonic cleaning CoCrMo(cobalt chrome molybdenum) alloy, scavenging period 15min, to remove the alloy surface dirt, in 60 ℃ stoving oven, dried 10 hours again, standby; With dried Medical C oCrMo(cobalt chrome molybdenum) alloy puts into the reaction chamber of ion nitriding furnace, reaction chamber is vacuumized (air pressure of reaction chamber is lower than 0.1Pa), in reaction chamber, feed argon gas then, alloy is carried out sputter clean, the air pressure of reaction chamber is 120Pa during cleaning, and sparking voltage is 500V, cleans in the process that reaction chamber heats up and carries out synchronously, intensification stops sputter clean after reaching predetermined ion nitriding temperature; After the sputter clean, extract the argon gas (reaction chamber air pressure is lower than 0.1Pa) in the reaction chamber out,, adopt pure NH
3(ammonia) is source of the gas, feeds NH in reaction chamber
3(ammonia), the reaction chamber gaseous tension is controlled at 450Pa, and the ion nitriding temperature is 800 ℃, and sparking voltage is 575V, and current density is 4.5mA/cm
2, being incubated after 9 hours, stove is chilled to 100 ℃ and comes out of the stove.
Behind the above-mentioned ion nitriding technology, Medical C oCrMo(cobalt chrome molybdenum) alloy surface has formed the nitride ceramics layer with fine and close nanostructure, and it is spherical that particle is, and arranges even compact, and particle size is less than 120nm(such as Fig. 1); The thickness of nitride layer is about 18 μ m, and nitride layer is deep into CoCrMo(cobalt chrome molybdenum) in the crystal boundary of alloy, form interlacing reticulated structure with matrix, this combination will inevitably be brought good mechanical performance (Fig. 2); The XRD interpretation of result shows that the nitride layer hard compounds after the ion nitriding is the CrN(chromium nitride mutually) and Cr
2The N(dichromium nitride) phase (Fig. 3); The hardness of nitride layer is 980.6HV
0.05, be CoCrMo(cobalt chrome molybdenum) and 2.8 times (Fig. 4) of alloy rigidity; CoCrMo(cobalt chrome molybdenum with the same terms ion Plasma Nitriding Treatment) alloy pin sample (radius 4mm) is a friction pair, under 2.5MPa, 5.5MPa and 8.5MPa load, 25% calf serum solution is lubricated, the wear rate of ion nitriding sample significantly reduces, 2.5MPa under the load, wear rate only is 1.26 * 10
-8Mg (Nm)
-1, the abrasion resistance properties ratio CoCrMo(cobalt chrome molybdenum that is untreated) and alloy improved 4 times (Fig. 5); The polishing scratch surface (Fig. 6) of sample slight localized delamination phenomenon only occurred with respect to untreated sample (Fig. 7) after the ion nitriding, and it is lighter to wear and tear, and polishing scratch is more shallow, shows that wear resistance is significantly improved.
Embodiment two, with Medical C oCrMo(cobalt chrome molybdenum) alloy surface is with 180
#, 400
#, 800
#, 1200
#Waterproof abrasive paper polish successively, method by mechanical polishing reduces CoCrMo(cobalt chrome molybdenum then) surfaceness of alloy is to 15nm, after the polishing with CoCrMo(cobalt chrome molybdenum) alloy immerses ultrasonic cleaning 10min in the spirit solvent, to remove the alloy surface dirt, in 60 ℃ stoving oven, dried 10 hours again, standby.With dried Medical C oCrMo(cobalt chrome molybdenum) alloy puts into the reaction chamber of ion nitriding furnace, reaction chamber is vacuumized, when the air pressure of reaction chamber is lower than 0.1Pa, in reaction chamber, feed argon gas, alloy is carried out sputter clean, clean in the process that reaction chamber heats up and carry out synchronously, the air pressure of reaction chamber is 90Pa during cleaning, sparking voltage is 480V, heats up after the ion nitriding temperature that reaches predetermined, stops sputter clean; To Medical C oCrMo(cobalt chrome molybdenum) after alloy sputter cleans, extract the argon gas (reaction chamber air pressure is lower than 0.1Pa) in the reaction chamber out,, adopt pure NH
3(ammonia) is source of the gas, feeds NH in reaction chamber
3(ammonia), the reaction chamber gaseous tension is controlled at 400Pa, and the ion nitriding temperature is 750 ℃, and sparking voltage is 550V, and current density is 4mA/cm
2, being incubated after 8 hours, stove is chilled to 100 ℃ and comes out of the stove.
Behind the above-mentioned ion nitriding technology, Medical C oCrMo(cobalt chrome molybdenum) alloy surface has formed the nitride ceramics layer with fine and close nanostructure, and particle is spherical and arranges even compact, and size is less than 100nm; The thickness of nitride layer is about 16 μ m, and nitride layer is deep into CoCrMo(cobalt chrome molybdenum) in the crystal boundary of alloy, form interlacing reticulated structure with matrix; The XRD interpretation of result shows the also formation CrN(chromium nitride after the ion nitriding) and Cr
2The N(dichromium nitride) hard compounds phase; The hardness of nitride layer is 930.3HV
0.05Carry out the frictional experiment of the same terms with embodiment one, obtain similar result, wear rate obviously reduces, and some slight localized delamination phenomenons only appear in the polishing scratch surface, and it is lighter to wear and tear.
Embodiment three, with Medical C oCrMo(cobalt chrome molybdenum) alloy surface is earlier with 180
#, 400
#, 800
#, 1200
#Waterproof abrasive paper polish successively, method by mechanical polishing reduces CoCrMo(cobalt chrome molybdenum then) surfaceness of alloy is to 15nm, after the polishing with CoCrMo(cobalt chrome molybdenum) alloy immerses ultrasonic cleaning 20min in the spirit solvent, to remove the alloy surface dirt, in 60 ℃ stoving oven, dried 10 hours again, standby; With dried Medical C oCrMo(cobalt chrome molybdenum) alloy puts into the reaction chamber of ion nitriding furnace, reaction chamber is vacuumized, when the air pressure of reaction chamber is lower than 0.1Pa, in reaction chamber, feed argon gas, alloy is carried out sputter clean, clean in the process that reaction chamber heats up and carry out synchronously, the air pressure of reaction chamber is 150Pa during cleaning, sparking voltage is 530V, heats up after the ion nitriding temperature that reaches predetermined, stops sputter clean; To Medical C oCrMo(cobalt chrome molybdenum) after alloy sputter cleans, extract the argon gas (reaction chamber air pressure is lower than 0.1Pa) in the reaction chamber out,, adopt pure NH
3(ammonia) is source of the gas, feeds NH in reaction chamber
3(ammonia), the reaction chamber gaseous tension is controlled at 500Pa, and the ion nitriding temperature is 850 ℃, and sparking voltage is 600V, and current density is 5mA/cm
2, being incubated after 10 hours, stove is chilled to 100 ℃ and comes out of the stove.
Behind the above-mentioned ion nitriding technology, Medical C oCrMo(cobalt chrome molybdenum) alloy surface has formed the nitride ceramics layer of fine and close nanostructure, and it is spherical that particle is, and arranges evenly, and size is less than 130nm; The thickness of nitride layer is about 20 μ m, nitride layer and CoCrMo(cobalt chrome molybdenum) alloy substrate forms interlacing reticulated structure, the XRD interpretation of result shows that the nitride layer hard compounds after the ion nitriding is the CrN(chromium nitride mutually) and Cr
2The N(dichromium nitride) phase; The hardness of nitride layer is 940.5HV
0.05, carry out the frictional experiment of the same terms with embodiment one, can obtain similar result, wear rate obviously reduces, and some slight localized delamination phenomenons only appear in the polishing scratch surface, and it is lighter to wear and tear.
Claims (6)
1. Medical C oCrMo alloy surface ion nitriding method is characterized in that may further comprise the steps:
A, with Medical C oCrMo(cobalt chrome molybdenum) alloy surface polishes successively with the multiple waterproof abrasive paper of different model earlier, the method reduction CoCrMo(cobalt chrome molybdenum by mechanical polishing then) surfaceness of alloy is to 15nm;
B, the CoCrMo(cobalt chrome molybdenum after will polishing) alloy immerses ultrasonic cleaning in the spirit solvent, and to remove the alloy surface dirt, put into stoving oven afterwards and dry;
C, with dried Medical C oCrMo(cobalt chrome molybdenum) alloy puts into the reaction chamber of ion nitriding furnace, reaction chamber is vacuumized, when the air pressure of reaction chamber is lower than 0.1Pa, in reaction chamber, feed argon gas, to Medical C oCrMo(cobalt chrome molybdenum) alloy carries out sputter clean, cleaning is carried out in the process that reaction chamber heats up synchronously, after intensification reaches predetermined ion nitriding temperature, stops sputter clean;
Argon gas in d, the extraction reaction chamber feeds NH in reaction chamber
3(ammonia), control reaction chamber gaseous tension, ion nitriding temperature, sparking voltage, current density were incubated after 8 ~ 10 hours, and stove is chilled to 100 ℃ and comes out of the stove.
2. Medical C oCrMo alloy surface ion nitriding method according to claim 1 is characterized in that: the multiple waterproof abrasive paper of described different model is respectively 180
#, 400
#, 800
#, 1200
#Waterproof abrasive paper.
3. Medical C oCrMo alloy surface ion nitriding method according to claim 1 is characterized in that: the time of ultrasonic cleaning is 10 ~ 20min in the described immersion spirit solvent.
4. Medical C oCrMo alloy surface ion nitriding method according to claim 1 is characterized in that: described to put into the temperature that stoving oven dries be 60 ℃, and the time of oven dry is 10 hours.
5. Medical C oCrMo alloy surface ion nitriding method according to claim 1 is characterized in that: described to Medical C oCrMo(cobalt chrome molybdenum) air pressure of reaction chamber was 90 ~ 150Pa when alloy carried out sputter clean, sparking voltage is 480 ~ 530V.
6. Medical C oCrMo alloy surface ion nitriding method according to claim 1 is characterized in that: described feeding NH
3The reaction chamber gaseous tension is controlled at 400 ~ 500Pa when (ammonia), and the ion nitriding temperature is 750 ~ 850 ℃, and sparking voltage is 550 ~ 600V, and current density is 4 ~ 5mA/cm
2
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560329A (en) * | 2011-12-23 | 2012-07-11 | 中国矿业大学 | Technology for preparing micropore ceramic on surface of medical titanium alloy artificial joint handle |
| CN103014599A (en) * | 2012-12-09 | 2013-04-03 | 常州大学 | Treatment process of composite surface of austenitic stainless steel |
| CN104372341A (en) * | 2014-10-11 | 2015-02-25 | 桂林市口腔医院 | Surface strengthening method for cobalt chromium alloy or pure titanium denture support |
| CN105695923A (en) * | 2016-02-25 | 2016-06-22 | 重庆跃进机械厂有限公司 | Ionic nitriding machining method for steel air valve |
| CN108691003A (en) * | 2018-06-12 | 2018-10-23 | 常州大学 | A method of improving cobalt-base alloys surface comprehensive performance |
-
2010
- 2010-11-24 CN CN 201010555638 patent/CN102031482A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 《Surface & Coatings Technology》 20061231 Orhan Oztürk等 "Metal ion release from nitrogen ion implanted CoCrMo orthopedic implant material" 5687-5697 1-6 第200卷, 2 * |
| 《Surface & Coatings Technology》 20081231 A. Celik等 "Effects of plasma nitriding on mechanical and tribological properties of CoCrMo alloy" 2433-2438 1-6 第202卷, 2 * |
| 《功能材料》 20100820 李嫱等 "CoCrMo 合金氮化处理后粗糙度对超高分子量聚乙烯摩擦磨损性能的影响" 1324-1326，1331 1-6 第41卷, 第8期 2 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560329A (en) * | 2011-12-23 | 2012-07-11 | 中国矿业大学 | Technology for preparing micropore ceramic on surface of medical titanium alloy artificial joint handle |
| CN103014599A (en) * | 2012-12-09 | 2013-04-03 | 常州大学 | Treatment process of composite surface of austenitic stainless steel |
| CN104372341A (en) * | 2014-10-11 | 2015-02-25 | 桂林市口腔医院 | Surface strengthening method for cobalt chromium alloy or pure titanium denture support |
| CN105695923A (en) * | 2016-02-25 | 2016-06-22 | 重庆跃进机械厂有限公司 | Ionic nitriding machining method for steel air valve |
| CN105695923B (en) * | 2016-02-25 | 2017-12-12 | 重庆跃进机械厂有限公司 | A kind of processing method of steel air valve ionic nitriding |
| CN108691003A (en) * | 2018-06-12 | 2018-10-23 | 常州大学 | A method of improving cobalt-base alloys surface comprehensive performance |
| CN108691003B (en) * | 2018-06-12 | 2020-06-26 | 常州大学 | Method for improving comprehensive performance of cobalt-based alloy surface |
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Application publication date: 20110427 |