CN106637175A - Surface passivation treatment method of martensite antibacterial stainless steel for surgical operating instrument - Google Patents
Surface passivation treatment method of martensite antibacterial stainless steel for surgical operating instrument Download PDFInfo
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- CN106637175A CN106637175A CN201611036157.5A CN201611036157A CN106637175A CN 106637175 A CN106637175 A CN 106637175A CN 201611036157 A CN201611036157 A CN 201611036157A CN 106637175 A CN106637175 A CN 106637175A
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- stainless steel
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/50—Treatment of iron or alloys based thereon
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Abstract
The invention discloses a surface passivation treatment method of martensite antibacterial stainless steel for a surgical operating instrument. The passivation treatment method comprises the steps that the antibacterial stainless steel surgical operation instrument is placed in a passivation solution, the passivation treatment temperature is set to be 85-95 DEG C, the passivation time is 0.2-0.5 h, then the instrument is washed with water, and the whole passivation process is finished. The passivation solution used in the surface passivation treatment method of the antibacterial stainless steel is formed by mixing raw materials including anhydrous cupric sulfate and a nitric acid aqueous solution. The passivation solution is prepared from, by weight, 1.5*10<-3>-2.5*10<-3> g/L of the anhydrous cupric sulfate, 25-35 g/L of nitric acid and the balance deionized water. By the adoption of the passivation treatment method, the effect that the antibacterial stainless steel surgical operation instrument has great corrosion resistance and antibacterial performance at the same time can be guaranteed.
Description
Technical field
The invention belongs to anti-bacteria stainless steel technical field of material surface treatment, and in particular to a kind of surgical operating instrument uses horse
The surface passivation treatment method of family name's build anti-bacteria stainless steel.
Background technology
Martensitic stain less steel, such as 2Cr13,3Cr13 and PH17-4 are adopted surgical operating instrument stainless steel more.Geneva
Build anti-bacteria stainless steel is the class biological function integration new material according to addition amount of copper on the basis of existing common stainless steel,
Its basic physicochemical property is suitable with common stainless steel.One outstanding advantages of martensitic stain less steel be with preferable intensity,
Can be used to be processed into the operating theater instruments that cutting guillotine style requires to have preferable hardness and wearability.But because it is used and is disappeared
Certain Korrosionsmedium is typically all contained in poison ring border, and in use, surgical operating instrument usually can corrode, and affect it
Performance.
In order to improve the corrosion resistance of surgical operating instrument stainless steel product, existing way often adopts chrome-faced
Treating method, this method for anti-bacteria stainless steel surgical operating instrument, have the shortcomings that two it is important：One is surface
The corrosion resisting property of the stainless steel material that although chromium plating greatly improve, but due to the appearance of chromium coating, block anti-bacteria stainless steel and resist
Bacterium element Cu ion is spread by surface to surrounding medium, that is to say, that anti-microbial property declines to a great extent；Two is traditional chromium plating work
Skill has that heavy metal Cr is exceeded and brings biological safety.
Another important processing method is surface passivation, and it can be prevented effectively from the exceeded safety wind for bringing of heavy metal Cr
Danger.But surface passivation is for anti-bacteria stainless steel, because its material surface defines the oxide layer of comparatively dense rich Cr, still
Copper diffusion in the passivation layer can be to a certain extent hindered, the anti-microbial property of material is reduced.
In sum, the invention provides a kind of surface passivation treatment method of anti-bacteria stainless steel, will to a great extent
The existing anti-corrosion and conflicting present situation of antibacterial is solved, for promoting anti-bacteria stainless steel this class material in surgical operating instrument
Application play a positive role.
The content of the invention
It is an object of the invention to provide surface passivating treatment side of the surgical operating instrument with martensite type anti-bacteria stainless steel
Method, to solve the problems, such as above-mentioned background technology in propose.
For achieving the above object, the present invention is employed the following technical solutions：Surgical operating instrument is stainless with martensite type antibacterial
The surface passivation treatment method of steel, its deactivating process for the treatment of is：
Anti-bacteria stainless steel surgical operating instrument is put in above-mentioned passivating solution, Passivation Treatment temperature is set as 85～95 DEG C,
Passivation time is 0.2～0.5h, is washed afterwards, i.e., whole passivating process terminates.
Preferably, the passivating solution used in the surface passivation treatment method of the anti-bacteria stainless steel be with anhydrous cupric sulfate and
Aqueous solution of nitric acid is mixed for raw material.
Preferably, the proportioning of the passivating solution is count by weight percentage：Anhydrous cupric sulfate：1.5×10-3～2.5 ×
10-3g/L；Nitric acid：25～35g/L；Deionized water：Complementary amount g/L.
The invention has the advantages that：
1st, deactivating process for the treatment of of the present invention can cause anti-bacteria stainless steel material to improve material on the premise of antibacterial functions are kept
The corrosion resistance of material, can improve anti-bacteria stainless steel material widely using in medical field.
2nd, deactivating process for the treatment of of the present invention not only has long-acting antibacterial functions, and is bio-safety.
Description of the drawings
Fig. 1 is the passivation parameter and passivating solution composition schematic diagram of the embodiment of the present invention and comparative example；
Fig. 2 is the performance test experimental result schematic diagram of the embodiment of the present invention and comparative example anti-bacteria stainless steel.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment 1：
This specific embodiment is employed the following technical solutions：The surgical operating instrument surface of martensite type anti-bacteria stainless steel
Deactivating process for the treatment of is：Anti-bacteria stainless steel surgical operating instrument is put in above-mentioned passivating solution, Passivation Treatment temperature is set as 85
DEG C, passivation time is 0.2h, is washed afterwards, i.e., whole passivating process terminates.
The proportioning of the passivating solution is count by weight percentage：Anhydrous cupric sulfate：1.5×10-3g/L；Nitric acid：25g/L；
Deionized water：Complementary amount g/L.
Embodiment 2：
This specific embodiment is employed the following technical solutions：The surgical operating instrument surface of martensite type anti-bacteria stainless steel
Deactivating process for the treatment of is：Anti-bacteria stainless steel surgical operating instrument is put in above-mentioned passivating solution, Passivation Treatment temperature is set as 90
DEG C, passivation time is 0.3h, is washed afterwards, i.e., whole passivating process terminates.
The proportioning of the passivating solution is count by weight percentage：Anhydrous cupric sulfate：2.0×10-3g/L；Nitric acid：30g/L；
Deionized water：Complementary amount g/L.
Embodiment 3：
This specific embodiment is employed the following technical solutions：The surgical operating instrument surface of martensite type anti-bacteria stainless steel
Deactivating process for the treatment of is：Anti-bacteria stainless steel surgical operating instrument is put in above-mentioned passivating solution, Passivation Treatment temperature is set as 95
DEG C, passivation time is 0.5h, is washed afterwards, i.e., whole passivating process terminates.
The proportioning of the passivating solution is count by weight percentage：Anhydrous cupric sulfate：2.5×10-3g/L；Nitric acid：35g/L；
Deionized water：Complementary amount g/L.
The passivation membrane component that deactivating process for the treatment of of the present invention is formed includes the oxide of Cu and Cr, the wherein oxide of Cr
Presence ensure that effective corrosion resisting property, when the material after Passivation Treatment is contacted with solution medium, the oxide of copper-rich
Release antibacterial copper ion can be partly dissolved again participates in killing bacteria process.Therefore the Passivation Treatment can ensure outside anti-bacteria stainless steel
Section's operating theater instruments has good anti-corrosion and anti-microbial property simultaneously.
In the surface passivation treatment method passivating solution of surgical operating instrument of the invention with martensite type anti-bacteria stainless steel,
Anhydrous cupric sulfate is antimicrobial chemical reagent important in passivating solution, this effect of common-sense antiseptic solution in this passivating process
It is：Salpeter solution preferentially can generate Cr with the Cr element reactions in steel as matrix material2O3, in certain density copper sulphate
Copper ion is deposited in the passivating film of rich Cr by Brownian movement, and combines to form CuO with oxygen.When with extraneous solution medium environment
During contact, the CuO in passivating film resolves into first Cu ions, discharges participation sterilized.Because passivating film is all the time in metastable
State, the Cu ion concentrations in anti-bacteria stainless steel surface C u ion solubility and passivating film keep basically identical.Make according to the conservation of mass
With when Cu ions occur mass transfer in passivation film on stainless steel surface, the copper ion on stainless steel base is continuous according to concentration gradient
Cu ions are supplemented in passivating film and keeps balance.Therefore in the present invention addition and follow-up passivation temperature of anhydrous cupric sulfate and
The reasonable selection of passivation time, the antibacterial passivation layer that can cause anti-bacteria stainless steel keeps stable, is conducive to its Long-Time Service, carries
High durability.Therefore, the design of the copper-bath in salpeter solution is just particularly important, when more than 2.5 × 10-3During g/L,
Can cause excessive Cu ions are enriched with anti-bacteria stainless steel passivation layer and bio-safety performance is affected；But less than 1.5 × 10-3g/L
When, but due in anti-bacteria stainless steel passivation layer Cu concentration it is relatively low and affect the stability of its anti-microbial property and passivating film.
The Passivation Treatment temperature of the present invention is set as 85～95 DEG C, and passivation time is 0.2～0.5h, is to take into account resisting for optimization
Bacterium performance and corrosion resisting property；Because too low passivation temperature can extend passivation time, production efficiency is reduced；Too high passivation temperature
The volatilization of passivating solution can be brought, passivation effect is affected.Passivation time is selected on the basis of passivation temperature, due to passivating process
The formation of passivating film was formed in the short period, and longer passivation time can not increase the compactness and copper of film in film
Deposited concentration.But the time is too short, more stable passivation effect can not be reached again.
Referring to Fig. 1, Fig. 2, passivation process of this specific embodiment to anti-bacteria stainless steel surgical operating instrument, implement
Example and comparative example are using 2Cr13Cu anti-bacteria stainless steels as experiment material.Anti-bacteria stainless steel operating theater instruments is placed and Fig. 1 institutes
In the passivating solution of row, using passivation temperature and passivation time described in Fig. 1.
1st, anti-microbial property detection
According to " JIS Z 2801-2000《Antibacterial fabricated product-antibiotic property test method and antibacterial effect》、GB/
T2591-2003《Antibiotic plastic anti-microbial property experimental technique and antibacterial effect》" etc. correlation standard, quantitative test Fig. 1 institutes
Show the medical stainless steel after passivating method process to the sterilization after frequent infectious bacteria (Escherichia coli, staphylococcus aureus) effect
Rate.In-vitro antibacterial performance test results are shown in Fig. 2, and the computing formula of wherein sterilizing rate is：Sterilizing rate (%)=[(control sample is lived
Bacterium number-Passivation Treatment stainless steel viable count)/control sample viable count] × 100%, control sample viable count is at general passivation
Managing carries out the viable count after Bacteria Culture on stainless steel sample, Passivation Treatment stainless steel viable count is referred on Passivation Treatment stainless steel
Carry out the viable count after Bacteria Culture.
2nd, decay resistance
According to stainless steel pitting potential measuring method (national standard：GB/T 17899-1999) to the embodiment of the present invention and
Comparative example stainless steel carries out anodic polarization curves test, and test result is shown in Fig. 2.
3rd, Evaluation of Biocompatibility
According to GB GBT16886.5-2003 BiologicalEvaluationofMedicalDevice, to embodiment and comparative example stainless steel pair
L929 (l cell) was evaluated in the cytotoxicity of 1-7 days.Cell is higher with respect to the rate of increase and cytotoxicity
Rating value is less, and bio-safety performance is more excellent.As a result Fig. 2 is seen.
The stainless-steel antibacterial energy after embodiment of the present invention 1-3 Passivation Treatment, resistance to is can be seen that from the result of Fig. 2
Corrosion energy and bio-safety performance are respectively provided with good performance.And comparative example is compared to embodiment, in different performance
There is deficiency.
Analyze by more than, passivating solution, passivation time and the temperature for only specifying in the present invention reaches a conjunction
Reason scope, cooperates between them, and surgical operating instrument martensite type anti-bacteria stainless steel could be caused to possess corrosion proof
Meanwhile, but also with good anti-microbial property and biological safety.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (1)
1. the surgical operating instrument surface passivation treatment method of martensite type anti-bacteria stainless steel, it is characterised in that：Passivation Treatment
Method is：Anti-bacteria stainless steel surgical operating instrument is put in above-mentioned passivating solution, Passivation Treatment temperature is set as 85～95 DEG C, blunt
The change time is 0.2～0.5h, is washed afterwards, i.e., whole passivating process terminates；
Passivating solution used in the surface passivation treatment method of the anti-bacteria stainless steel is with anhydrous cupric sulfate and aqueous solution of nitric acid
Mix for raw material；
The proportioning of the passivating solution is count by weight percentage：Anhydrous cupric sulfate：1.5×10-3～2.5 × 10-3g/L；Nitric acid：
25～35g/L；Deionized water：Complementary amount g/L.
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| CN201611036157.5A CN106637175B (en) | 2016-11-09 | 2016-11-09 | The surface passivation treatment method of surgical operating instrument martensite type anti-bacteria stainless steel |
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| CN201611036157.5A CN106637175B (en) | 2016-11-09 | 2016-11-09 | The surface passivation treatment method of surgical operating instrument martensite type anti-bacteria stainless steel |
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| CN106637175A true CN106637175A (en) | 2017-05-10 |
| CN106637175B CN106637175B (en) | 2019-02-22 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326012A (en) * | 2000-05-29 | 2001-12-12 | 北京科技大学 | Passivation technique for filming on surface of stainless steel |
| US20100132844A1 (en) * | 2007-03-05 | 2010-06-03 | Poligrat Gmbh | Method for the thermochemical passivation of stainless steel |
| CN202054883U (en) * | 2011-03-24 | 2011-11-30 | 桂林电子科技大学 | Antibacterial stainless steel containing copper and cerium on surface |
| CN104593761A (en) * | 2015-01-14 | 2015-05-06 | 中国科学院金属研究所 | Surface antibacterial passivation solution for medical stainless steel with biosafety and passivation process |
| CN105088092A (en) * | 2014-05-23 | 2015-11-25 | 中国科学院金属研究所 | Novel medical antibacterial stainless steel |
-
2016
- 2016-11-09 CN CN201611036157.5A patent/CN106637175B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326012A (en) * | 2000-05-29 | 2001-12-12 | 北京科技大学 | Passivation technique for filming on surface of stainless steel |
| US20100132844A1 (en) * | 2007-03-05 | 2010-06-03 | Poligrat Gmbh | Method for the thermochemical passivation of stainless steel |
| CN202054883U (en) * | 2011-03-24 | 2011-11-30 | 桂林电子科技大学 | Antibacterial stainless steel containing copper and cerium on surface |
| CN105088092A (en) * | 2014-05-23 | 2015-11-25 | 中国科学院金属研究所 | Novel medical antibacterial stainless steel |
| CN104593761A (en) * | 2015-01-14 | 2015-05-06 | 中国科学院金属研究所 | Surface antibacterial passivation solution for medical stainless steel with biosafety and passivation process |
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