CN106756744B - A kind of processing and treating method on medical 316L stainless steel surface - Google Patents

A kind of processing and treating method on medical 316L stainless steel surface Download PDF

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CN106756744B
CN106756744B CN201611164513.1A CN201611164513A CN106756744B CN 106756744 B CN106756744 B CN 106756744B CN 201611164513 A CN201611164513 A CN 201611164513A CN 106756744 B CN106756744 B CN 106756744B
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stainless steel
316l stainless
parts
steel surface
made
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CN201611164513.1A
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CN106756744A (en
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洪功正
潘永刚
蔡永波
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安徽宝恒新材料科技有限公司
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Abstract

The invention belongs to medical stainless steel manufacturing fields, more particularly to a kind of processing and treating method on medical 316L stainless steel surface, it is impregnated 2-3 hours the following steps are included: 316L stainless steel is placed in soak by (1), it takes out, it is put into the ethanol solution that volume fraction is 70%, it is cleaned after ultrasonic treatment 10min, then with distilled water;(2) by modified hydroxylapatite obtained plasma jet Flashmelt;(3) by the 316L stainless steel surface of modified hydroxylapatite spraying after steeping after melting;(4) until modified hydroxylapatite is after the solidification of 316L stainless steel surface, using ultraviolet light irradiation 10min, obtained medical 316L stainless steel.Using method provided by the invention, it can make 316L stainless steel obtained that there is excellent chemical stability, corrosion resistance and antibiotic property, greatly improve the quality of 316L stainless steel.

Description

A kind of processing and treating method on medical 316L stainless steel surface

Technical field

The invention belongs to medical stainless steel manufacturing fields, and in particular to a kind of working process on medical 316L stainless steel surface Method.

Background technique

Stainless steel is using earliest a kind of biomaterial, and in medical stainless steel material, austenitic stainless steel is good because of its Good mechanical performance, corrosion resistance and cheap price, and be widely applied.Wherein 316L stainless steel is due to good biology Compatibility, mechanical property, workability and resistance to corrosion in body fluid performance and be widely used in hard tissue repair and alternative materials.As Bone implant material, in Long-term clinical in use, being still difficult to avoid that some problem and shortage, as 316LSS itself does not have biology Activity, anti-microbial property difference etc. are a kind of embedding bone for connecting property of machinery between planting body and bone after implantation as artificial joint material Integration, rather than strong chemical bonding;Bacterium infection is inevitable complication in Implant, although disappearing by stringent Poison and sterile working, the infection rate for still suffering from 0.5~3% exist.If purposely introduced on the surface of the material with special The surface texture of property, design is conducive to the interaction for adjusting histocyte and storeroom and the surface with anti-microbial property is tied Structure makes 316LSS that there is treatment to repair and pre- aseptic function.A kind of currently used 316L stainless steel surface processing technique It is plasma spraying process, the powder of spraying is hydroxyapatite, but hydroxy apatite powder is in plasma in pyrolytic coating Flame acts on lower thermodynamic instability and undergoes phase transition, generate amorphous state and be thermally decomposed into other synthos, makes its bioactivity It is affected.In addition, the thermal expansion coefficient of hydroxyapatite and 316LSS are mismatched, cause between hydroxyapatite and matrix Binding force is also not good enough, the phenomenon that disbonding clinically usually occurs, significantly limits the service life of coating.Therefore It is badly in need of a kind of scientific and effective 316LSS process for treating surface.

Summary of the invention

To solve the above-mentioned problems, the present invention provides a kind of processing and treating method on medical 316L stainless steel surface.

The present invention is achieved by the following technical solutions.

A kind of processing and treating method on medical 316L stainless steel surface, comprising the following steps:

(1) 316L stainless steel is placed in soak and is impregnated 2-3 hours, taken out, it is molten to be put into the ethyl alcohol that volume fraction is 70% In liquid, cleaned after ultrasonic treatment 10min, then with distilled water;

(2) by modified hydroxylapatite obtained plasma jet Flashmelt;

(3) by the 316L stainless steel surface of modified hydroxylapatite spraying after steeping after melting;

(4) wait until that modified hydroxylapatite after the solidification of 316L stainless steel surface, irradiates 10min using ultraviolet light, is made Medical 316L stainless steel;

Above-mentioned soak is made of the component of following parts by weight: two 1-3 parts of molybdic acid hydrate sodium, ethylenediamine base propanesulfonate 12-16 parts, 0.6-0.8 parts of benzyltrimethylammonium bromide, 2-4 parts of Imazalil sulfate, bis- 0.5-0.7 parts of bromo- 1- propyl alcohol of 2,3-, 60-70 parts of distilled water;

Above-mentioned modified hydroxylapatite is made of following methods :(a) by weight, by 20-25 parts of four water-calcium nitrates, 3-5 parts of calcium chloride, 40-45 parts of dehydrated alcohols, 0.1-0.3 parts of ethylene thiourea mixing, stir evenly spare;(b) by weight, After 10-12 parts of phosphorus pentoxides, 0.1-0.3 parts of phosphorus powders, 1-2 parts of carbon disulfide, 24-26 parts of dehydrated alcohols are mixed, stirring is equal It is even spare;(c) natural after the ratio mixing of 3-5:1 by the resulting mixture of step (a) and the resulting mixture of step (b) After placing 48-50 hours, white gels are made, after white gels are dried, is crushed to 200-220 mesh, modified modified hydroxyl is made Base apatite;

Specifically, the soak in above-mentioned steps (1) is made of following methods: distilled water being heated to 80 DEG C, is used The revolving speed of 300r/min persistently stirs, and two molybdic acid hydrate sodium, ethylenediamine base propane sulfonic acid are successively then added thereto every 3min Sodium, benzyltrimethylammonium bromide, Imazalil sulfate, the bromo- 1- propyl alcohol of 2,3- bis- after the completion of charging, continue to stir 5min, be made Soak.

Specifically, the frequency of above-mentioned ultrasonic wave is 50KHz, and uitraviolet intensity is 90 μ W/cm2

From the above technical scheme, it can be seen that the beneficial effects of the present invention are:

Using method provided by the invention, it can make 316L stainless steel obtained that there is excellent chemical stability, anti-corruption Corrosion and antibiotic property improve the thermodynamic stability of hydroxy apatite powder and the adhesion strength in stainless steel surface, greatly Ground improves the quality of 316L stainless steel.Wherein, two molybdic acid hydrate sodium in soak and the collaboration of ethylenediamine base propanesulfonate are made With can effectively remove some intractable spots such as grease of stainless steel surface, have to the bacterium of stainless steel surface relatively strong Inhibiting effect, and can and benzyltrimethylammonium bromide, Imazalil sulfate, the bromo- 1- propyl alcohol of 2,3- bis- synergistic effect, promoted The activity of metal surface increases the adhesion strength of plasma liquid and stainless steel surface, so that coating is not easy to take off during use It falls;Modified hydroxylapatite joined calcium chloride and phosphorus powder during preparation, can promote the yield and purity of product, greatly The generation of ground reduction impurity;Ethylene thiourea can accelerate the speed of synthetic reaction and change with carbon disulfide synergistic effect, promotion Property hydroxyapatite thermal stability dislike and bioactivity, and the chemical stability of coating can also be promoted, so that coating makes It is not easily to fall off during, therefore it is greatly improved the service life and anti-microbial property of medical 316L stainless steel obtained.

Specific embodiment

In order to enable those skilled in the art to be further understood that feature and technology contents of the invention, please referring to following has Close detailed description of the invention.

Embodiment 1

A kind of processing and treating method on medical 316L stainless steel surface, comprising the following steps:

(1) 316L stainless steel is placed in soak and is impregnated 2 hours, taken out, be put into the ethanol solution that volume fraction is 70% In, it is cleaned after ultrasonic treatment 10min, then with distilled water;

(2) by modified hydroxylapatite obtained plasma jet Flashmelt;

(3) by the 316L stainless steel surface of modified hydroxylapatite spraying after steeping after melting;

(4) wait until that modified hydroxylapatite after the solidification of 316L stainless steel surface, irradiates 10min using ultraviolet light, is made Medical 316L stainless steel;

Above-mentioned soak is made of the component of following parts by weight: two 1-3 parts of molybdic acid hydrate sodium, ethylenediamine base propanesulfonate 12 Part, 0.6 part of benzyltrimethylammonium bromide, 2 parts of Imazalil sulfate, bis- 0.5 part of bromo- 1- propyl alcohol of 2,3-, 60 parts of distilled water;

Above-mentioned modified hydroxylapatite is made of following methods :(a) by weight, by 20 parts of four water-calcium nitrates, 3 parts Calcium chloride, 40 parts of dehydrated alcohols, 0.1 part of ethylene thiourea mixing, stir evenly spare;(b) by weight, 10 part five is aoxidized After two phosphorus, 0.1 part of phosphorus powder, 1 part of carbon disulfide, 24 parts of dehydrated alcohol mixing, stir evenly spare;(c) step (a) is resulting After placing 48 hours naturally, white gels are made after the ratio mixing of 3:1 in mixture and the resulting mixture of step (b), After white gels are dried, 200 mesh are crushed to, modified modified hydroxyapatite is made;

Specifically, the soak in above-mentioned steps (1) is made of following methods: distilled water being heated to 80 DEG C, is used The revolving speed of 300r/min persistently stirs, and two molybdic acid hydrate sodium, ethylenediamine base propane sulfonic acid are successively then added thereto every 3min Sodium, benzyltrimethylammonium bromide, Imazalil sulfate, the bromo- 1- propyl alcohol of 2,3- bis- after the completion of charging, continue to stir 5min, be made Soak.

Specifically, the frequency of above-mentioned ultrasonic wave is 50KHz, and uitraviolet intensity is 90 μ W/cm2

Embodiment 2

A kind of processing and treating method on medical 316L stainless steel surface, comprising the following steps:

(1) 316L stainless steel is placed in soak and is impregnated 2.5 hours, taken out, it is molten to be put into the ethyl alcohol that volume fraction is 70% In liquid, cleaned after ultrasonic treatment 10min, then with distilled water;

(2) by modified hydroxylapatite obtained plasma jet Flashmelt;

(3) by the 316L stainless steel surface of modified hydroxylapatite spraying after steeping after melting;

(4) wait until that modified hydroxylapatite after the solidification of 316L stainless steel surface, irradiates 10min using ultraviolet light, is made Medical 316L stainless steel;

Above-mentioned soak is made of the component of following parts by weight: two 2 parts of molybdic acid hydrate sodium, ethylenediamine base propanesulfonate 14 Part, 0.7 part of benzyltrimethylammonium bromide, 3 parts of Imazalil sulfate, bis- 0.6 part of bromo- 1- propyl alcohol of 2,3-, 65 parts of distilled water;

Above-mentioned modified hydroxylapatite is made of following methods :(a) by weight, by 23 parts of four water-calcium nitrates, 4 parts Calcium chloride, 43 parts of dehydrated alcohols, 0.2 part of ethylene thiourea mixing, stir evenly spare;(b) by weight, 11 part five is aoxidized After two phosphorus, 0.2 part of phosphorus powder, 1 part of carbon disulfide, 25 parts of dehydrated alcohol mixing, stir evenly spare;(c) step (a) is resulting After placing 49 hours naturally, white gels are made after the ratio mixing of 4:1 in mixture and the resulting mixture of step (b), After white gels are dried, 210 mesh are crushed to, modified modified hydroxyapatite is made;

Specifically, the soak in above-mentioned steps (1) is made of following methods: distilled water being heated to 80 DEG C, is used The revolving speed of 300r/min persistently stirs, and two molybdic acid hydrate sodium, ethylenediamine base propane sulfonic acid are successively then added thereto every 3min Sodium, benzyltrimethylammonium bromide, Imazalil sulfate, the bromo- 1- propyl alcohol of 2,3- bis- after the completion of charging, continue to stir 5min, be made Soak.

Specifically, the frequency of above-mentioned ultrasonic wave is 50KHz, and uitraviolet intensity is 90 μ W/cm2

Embodiment 3

A kind of processing and treating method on medical 316L stainless steel surface, comprising the following steps:

(1) 316L stainless steel is placed in soak and is impregnated 3 hours, taken out, be put into the ethanol solution that volume fraction is 70% In, it is cleaned after ultrasonic treatment 10min, then with distilled water;

(2) by modified hydroxylapatite obtained plasma jet Flashmelt;

(3) by the 316L stainless steel surface of modified hydroxylapatite spraying after steeping after melting;

(4) wait until that modified hydroxylapatite after the solidification of 316L stainless steel surface, irradiates 10min using ultraviolet light, is made Medical 316L stainless steel;

Above-mentioned soak is made of the component of following parts by weight: two 3 parts of molybdic acid hydrate sodium, ethylenediamine base propanesulfonate 16 Part, 0.8 part of benzyltrimethylammonium bromide, 4 parts of Imazalil sulfate, bis- 0.7 part of bromo- 1- propyl alcohol of 2,3-, 70 parts of distilled water;

Above-mentioned modified hydroxylapatite is made of following methods :(a) by weight, by 25 parts of four water-calcium nitrates, 5 parts Calcium chloride, 45 parts of dehydrated alcohols, 0.3 part of ethylene thiourea mixing, stir evenly spare;(b) by weight, 12 part five is aoxidized After two phosphorus, 0.3 part of phosphorus powder, 2 parts of carbon disulfide, 26 parts of dehydrated alcohol mixing, stir evenly spare;(c) step (a) is resulting After placing 50 hours naturally, white gels are made after the ratio mixing of 5:1 in mixture and the resulting mixture of step (b), After white gels are dried, 220 mesh are crushed to, modified modified hydroxyapatite is made;

Specifically, the soak in above-mentioned steps (1) is made of following methods: distilled water being heated to 80 DEG C, is used The revolving speed of 300r/min persistently stirs, and two molybdic acid hydrate sodium, ethylenediamine base propane sulfonic acid are successively then added thereto every 3min Sodium, benzyltrimethylammonium bromide, Imazalil sulfate, the bromo- 1- propyl alcohol of 2,3- bis- after the completion of charging, continue to stir 5min, be made Soak.

Specifically, the frequency of above-mentioned ultrasonic wave is 50KHz, and uitraviolet intensity is 90 μ W/cm2

Common medical 316L stainless steel commercially available in 316L stainless steel made from embodiment 1,2,3 and comparative example is carried out rotten Corrosion test, the CHI660E electrochemical workstation developed using Shanghai Chen Hua Instrument Ltd. measure embodiment and comparative example The dynamic potential polarization curve and electrochemical impedance spectroscopy of middle 316L stainless steel.First by test sample with naked before electrochemical corrosion test The copper conductor of dew reserves 1cm around fixing and being sealed with epoxy resin to non-working surface2Work area, will before test sample Sample ultrasonic cleaning 5min in deionized water, is then dried up in cold wind with hair dryer.Pt electrode (1cm × 1cm) conduct Auxiliary electrode, saturated calomel electrode are reference electrode.Etchant solution selects Stimulated body fluid, the proportion tool of Stimulated body fluid Body is as follows:

NaCl(8.0g) + Na2HPO4(0.2g) + KH2PO4(0.2g) + KCl (0.2g) + 1LH2O

(1) electrochemical impedance spectroscopy is tested

Initial potential is set as open circuit potential, and frequency range is set as 1 × 103 Hz-1×10-3 Hz;To measured friendship Flow impedance spectrum is fitted analysis using Zsimp Win V3.20 impedance software.

(2) dynamic potential polarization curve is tested

Sample impregnates to the laggard action potential polarization curve test of 30min in Stimulated body fluid, scanning range is- 1V-1V, scanning speed 1mV/s.

Test result is as shown in table 1:

1 316L stainless steel surface corrosion resistance test result of table

Project Corrosion potential/V Corrosion electric current density/A.cm-2 Breakdown voltage Embodiment 1 -0.297 8.30×10-8 0.783 Embodiment 2 -0.293 8.06×10-8 0.801 Embodiment 3 -0.286 7.97×10-8 0.810 Comparative example -0.325 9.48×10-7 0.690

As shown in Table 1,316L stainless steel obtained has stronger corrosion resistance, coating in human body fluid in the present invention It is higher with the conjugation of stainless steel surface, it is not easily to fall off, it is greatly improved the quality of 316L stainless steel.

Certainly, the above description is not a limitation of the present invention, and the present invention is also not limited to the example above, the art Those of ordinary skill, within the essential scope of the present invention, variation, change, addition or the replacement made all should belong to the present invention Protection scope.

Claims (3)

1. a kind of processing and treating method on medical 316L stainless steel surface, which comprises the following steps:
(1) 316L stainless steel is placed in soak and is impregnated 2-3 hours, taken out, be put into the ethanol solution that volume fraction is 70% In, it is cleaned after ultrasonic treatment 10min, then with distilled water;
(2) by modified hydroxylapatite obtained plasma jet Flashmelt;
(3) by the 316L stainless steel surface of modified hydroxylapatite spraying after steeping after melting;
(4) wait until that modified hydroxylapatite after the solidification of 316L stainless steel surface, irradiates 10min using ultraviolet light, is made medical 316L stainless steel;
Above-mentioned soak is made of the component of following parts by weight: two 1-3 parts of molybdic acid hydrate sodium, ethylenediamine base propanesulfonate 12-16 Part, 0.6-0.8 parts of benzyltrimethylammonium bromide, 2-4 parts of Imazalil sulfate, bis- 0.5-0.7 parts of bromo- 1- propyl alcohol of 2,3-, distillation 60-70 parts of water;
Above-mentioned modified hydroxylapatite is made of following methods :(a) by weight, by 20-25 parts of four water-calcium nitrates, 3-5 Part calcium chloride, 40-45 parts of dehydrated alcohols, 0.1-0.3 parts of ethylene thioureas mixing, stir evenly spare;(b) by weight, will After 10-12 parts of phosphorus pentoxides, 0.1-0.3 parts of phosphorus powders, 1-2 parts of carbon disulfide, 24-26 parts of dehydrated alcohol mixing, stir evenly It is spare;(c) the resulting mixture of step (a) and the resulting mixture of step (b) are put naturally after the ratio mixing of 3-5:1 After setting 48-50 hours, white gels are made, after white gels are dried, is crushed to 200-220 mesh, modified modified hydroxyl is made Apatite.
2. a kind of processing and treating method on medical 316L stainless steel surface according to claim 1, which is characterized in that on The soak stated in step (1) is made of following methods: distilled water being heated to 80 DEG C, is continued using the revolving speed of 300r/min Stirring, is then successively added two molybdic acid hydrate sodium, ethylenediamine base propanesulfonate, benzyl trimethyl bromination every 3min thereto Ammonium, Imazalil sulfate, the bromo- 1- propyl alcohol of 2,3- bis- after the completion of charging, continue to stir 5min, soak are made.
3. a kind of processing and treating method on medical 316L stainless steel surface according to claim 1, which is characterized in that on The frequency for stating ultrasonic wave is 50KHz, and uitraviolet intensity is 90 μ W/cm2
CN201611164513.1A 2016-12-16 2016-12-16 A kind of processing and treating method on medical 316L stainless steel surface CN106756744B (en)

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