CN203007383U - Antibacterial stainless steel with copper-cerium thin film contained on surface - Google Patents

Antibacterial stainless steel with copper-cerium thin film contained on surface Download PDF

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Publication number
CN203007383U
CN203007383U CN 201220561576 CN201220561576U CN203007383U CN 203007383 U CN203007383 U CN 203007383U CN 201220561576 CN201220561576 CN 201220561576 CN 201220561576 U CN201220561576 U CN 201220561576U CN 203007383 U CN203007383 U CN 203007383U
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stainless steel
cerium
copper
antibacterial
thin film
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徐晋勇
唐锋
唐炎
向家伟
蒋占四
张应红
高鹏
唐亮
高成
高波
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Guilin University of Electronic Technology
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Guilin University of Electronic Technology
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Abstract

The utility model discloses antibacterial stainless steel with a copper-cerium thin film contained on the surface. The antibacterial stainless steel comprises a stainless steel base material and an antibacterial layer, wherein the antibacterial layer is coated on the surface of the stainless steel through diffusion coating by using a magnetron sputtering technology. The antibacterial stainless steel is characterized in that the antibacterial layer with copper-cerium thin film is coated on the surface of the stainless steel base material through diffusion coating, and the thickness is 20 mu m. The antibacterial stainless steel with the copper-cerium thin film contained on the surface disclosed by the utility model is good in thin film compactness, controllable in thickness, and good in antimicrobial properties.

Description

A kind of anti-bacteria stainless steel of copper-cerium-containing surface film
Technical field
The utility model relates to anti-bacteria stainless steel, particularly utilizes magnetron sputtering method to prepare the anti-bacteria stainless steel of copper-cerium-containing surface film.
Background technology
Stainless steel has good mechanical property and erosion resistance, and it is one of most widely used ferrous materials, is widely used in each industrial circle.And a lot of special dimensions not only require stainless steel attractive in appearance such as articles for daily use such as medical and health industry, food service industry, sanitary equipment, kitchen tools, for stainless germ resistance, certain requirement are arranged also, and the research of anti-bacteria stainless steel technology is risen thereupon.At present, the stainless steel antiseptic-germicide is take copper or silver as main, anti-bacteria stainless steel can be divided into whole anti-bacteria stainless steel and stainless steel with antibacterial surface according to the distributing position of antiseptic elements.Wherein in whole anti-bacteria stainless steel, antiseptic elements is distributed among stainless steel substrate, all needs to carry out ageing treatment in preparation process and makes copper separate out mutually with ε-Cu, can reach antibacterial effect preferably.Stainless steel with antibacterial surface all will carry out ageing treatment after adding copper.
The preparation method of anti-bacteria stainless steel has:
" a kind of anti-bacteria stainless steel of surface containing cerium " (publication number CN202054884U) discloses with the surperficial method that contains the anti-bacteria stainless steel of cerium alloy layer of two brightness plasma permeating technology preparations, the part processing parameter is: source voltage 900 ~ 1100V, cathode voltage 500 ~ 600V, temperature: 800 ~ 850 oC。Because simple substance cerium fusing point is lower, be in molten state during plating, must be placed in plumbago crucible, and very easily oxidation, cause certain difficulty to test operation.
" a kind of anti-bacteria stainless steel of copper-cerium-containing surface " (publication number CN 202054883 U) disclose the method for preparing the anti-bacteria stainless steel of copper-cerium-containing surface alloy layer with two brightness plasma permeating technology, the part processing parameter is: source voltage 900V, cathode voltage 550V, 820 ~ 860 ℃ of plating temperature, soaking time 3.5 hours.This technique can obtain more stable copper cerium alloy layer, but long processing time, and power consumption is larger, and has the high temperature deformation problem when processing sheet workpiece.
(publication number CN 101717920 A) disclose a kind of method of utilizing magnetron sputtering method to prepare composite Ag-Ti oxide antibacterial film " to utilize magnetron sputtering method to prepare the method for composite Ag-Ti oxide antibacterial film ".
" a kind of antibacterial makrolon film that utilizes the magnetron sputtering technique preparation " (publication number CN 102011095 A) disclose a kind of method of utilizing magnetron sputtering method to prepare the antibacterial makrolon film.
Above-mentioned two kinds of anti-bacteria stainless steels that utilize the magnetron sputtering method preparation are all take silver as antiseptic elements, and cost is expensive.
Advantages such as sputter rate is high owing to having, the workpiece to be plated temperature is low, film adhesion good for magnetron sputtering, pollution-free and become gradually the focus of top coat research.But so far, yet there are no the report that adopts magnetron sputtering technique to prepare the anti-bacteria stainless steel of copper-cerium-containing surface film.
Summary of the invention
The purpose of this utility model is to provide a kind of anti-bacteria stainless steel that utilizes magnetron sputtering method to prepare the copper-cerium-containing surface film, this stainless steel has good germ resistance, and the original mechanical property of maintenance matrix, the anti-bacteria stainless steel that preparation cost oozes silver than preparation is low, preparation time is short, need not ageing treatment, pollution-free.
A kind of anti-bacteria stainless steel of copper-cerium-containing surface film, comprise stainless steel substrate and adopt the magnetron sputtering technique plating at the antibiotic layer of stainless steel surface, unlike the prior art be: the antibiotic layer of plating cupric, cerium film on austenite or Martensite Stainless Steel base material, thickness are 20 μ m.
A kind of method of utilizing magnetron sputtering method to prepare the anti-bacteria stainless steel of copper-cerium-containing surface film comprises the following steps:
(1) target is chosen
Choose purity and be 99.9% block copper cerium alloy as magnetic control spattering target 1, Cu, Ce mass ratio are 4:1, choose purity and be 99.9% pure iron as magnetic control spattering target 2;
(2) substrate processing
Substrate is cleaned with ultrasonic wave and acetone successively, put into magnetron sputtering chamber after polishing;
(3) bombardment preheating
The vacuum tightness of sputtering chamber is less than 2 * 10 -5Pa passes into argon gas, and sputtering pressure is adjusted to 1.5 ~ 5Pa, opens the negative bias power supply, transfers to 400 ~ 800V scope, workpiece is carried out the ion bombardment aura clean, and opens simultaneously well heater to workpiece preheating to be plated, and preheating temperature is 200 ℃, warm up time 10 ~ 20min;
(4) spatter film forming
Target voltage transfers to 200 ~ 500V, and sputtering current is 0.3 ~ 0.5A constant current, substrate is carried out recirculated water cooling process, and target is 70 ~ 90mm to the distance of substrate, and sputter prepares film through 1 ~ 2h.
The anti-bacteria stainless steel of the utility model preparation is after tested:
1, antibacterial ability test:
Stainless steel A ', M ' after stainless steel A, M, T and processing that magnetron sputtering processes, the sample that T ' makes respectively 5 * 5cm will do not carried out, wherein untreated contrast steel adopts 00Cr18Ni10 austenitic stainless steel, 1Cr13 Martensite Stainless Steel and 0Cr13 ferritic stainless steel.The experiment microorganism is adopted intestinal bacteria, streptococcus aureus.Experimental procedure is as follows:
After the stainless steel of copper-cerium-containing film is cleaned with ethanol with the contrast steel 120 ℃ of lower autoclavings 25 minutes.
It is 10 that postvaccinal bacterial classification is diluted to concentration with PBS liquid (0.03mol/l, PH=7.2, disodium hydrogen phosphate,anhydrous 2.83g, potassium primary phosphate 1.36g, distilled water 1000ml) 5Standardized solution, and 0.5ml bacterium liquid is evenly dripped to sample and contrast stainless steel surface, cover with the aseptic plastic film respectively.
The surface is scribbled the sample of bacterium liquid and contrast stainless steel, and to put into 35 ℃, humidity be effect 24 hours in 90% incubator.
Placed 48 hours in the incubator of 35 ℃ with dull and stereotyped agar culture method, calculate at last the bacterium number on the plastics plate, calculate sterilizing rate.Antibacterial experiment the results are shown in Table 1.
Wherein the calculation formula of sterilizing rate is:
Figure DEST_PATH_58956DEST_PATH_IMAGE002
Above-mentioned contrast stainless steel aerobic plate count is the viable count after the contrast stainless steel carries out antibacterial experiment, and the anti-bacteria stainless steel aerobic plate count refers to the viable count after anti-bacteria stainless steel carries out antibacterial experiment.The results are shown in Table 1.
The method also can be used for the viable count after stainless steel carries out antibacterial experiment.
2, Durability of antimicrobial effect test:
Use model MMS-2A frictional testing machines to carry out the sliding frictional wear test to the anti-bacteria stainless steel of preparation with the contrast steel of testing in 2.Rub(bing)test power: 1000N; The sliding friction time: 20min.The results are shown in Table 1.
3, mechanical property experiment:
To be cut into through the anti-bacteria stainless steel of antimicrobial treatment tension specimen (stretching gauge length 12mm, thick 1mm).Al2O3 sand paper with 600 granularities carries out mechanical polishing.Take with the private of MTS-810 point and carry out tension test in protracted test machine, room temperature, air, rate of extension is 2 * 10 -3s -1, obtain following mechanical property, see Table 2.
Table 1 stainless-steel antibacterial can synopsis
Figure DEST_PATH_DEST_PATH_IMAGE004A
In table ++ represent sterilizing rate more than 99% ,+represent more than 90% ,-represent sterilizing rate more than 80%,--the expression sterilizing rate is more than 50%, and zero expression sterilizing rate is lower than 50%.
Table 2 anti-bacteria stainless steel mechanical property synopsis
The stainless steel sequence number σb(N/ mm 2 δ(%)
A’ 550 45
A 520 45
M’ 580 16
M 540 25
T’ 460 22
T 490 24
Compared with prior art, the beneficial effects of the utility model are:
1, preparation technology is simple, and sputter temperature is lower than 500 ℃, and workpiece high temperature deformation can not occur, is specially adapted to sheet workpiece;
2, adopt the copper cerium alloy as target, can be not oxidized in the short period of time in air, avoided using the simple substance cerium to do the very easily problem of oxidation of target;
3, the stainless steel surface copper-cerium-containing film of the utility model preparation, have good antibacterial effect, and copper, Ce elements consumption are few, and is little on the original mechanical property impact of stainless steel;
4, anti-bacteria stainless steel to add copper, silver as main, is compared with silver at present, and copper cerium alloy cost is lower.And the stainless steel of merely making antiseptic-germicide with copper need just can reach antibacterial effect preferably through ageing treatment; Good antibacterial effect be can reach and the anti-bacteria stainless steel of the utility model take the copper cerium as antiseptic-germicide need not ageing treatment in whole preparation process, time and cost saved.
Description of drawings
Fig. 1 is the structural representation of the anti-bacteria stainless steel of the utility model copper-cerium-containing surface film.
In figure: 1. the antibacterial film of stainless steel base 2. copper-cerium-containings.
Embodiment
Embodiment 1:
Prepare the austenite antimicrobial stainless steel of copper-cerium-containing surface film with magnetron sputtering method, comprise the following steps:
(1) target is chosen
Choose purity and be 99.9% block copper cerium alloy as magnetic control spattering target 1, Cu, Ce mass ratio are 4:1, choose purity and be 99.9% pure iron as magnetic control spattering target 2;
(2) substrate processing
Choose the 00Cr18Ni10 austenitic stainless steel as substrate, substrate is cleaned with ultrasonic wave and acetone successively, put into magnetron sputtering chamber after polishing;
(3) bombardment preheating
The vacuum tightness of sputtering chamber is less than 2 * 10 -5Pa passes into purity and is 99.99% argon gas, and sputtering pressure is adjusted to 2.5Pa, open the negative bias power supply, transfer to 400 ~ 800V scope, workpiece is carried out the ion bombardment aura clean, open simultaneously well heater to workpiece preheating to be plated, preheating temperature is 200 ℃, warm up time 15min;
(4) spatter film forming
Target 1 voltage transfers to 200V, target 2 voltage 500V, and sputtering current is the 0.3A constant current, substrate is carried out recirculated water cooling process, target is 90mm to the distance of substrate, sputtering time 1h, making film thickness is 20 μ m.
Embodiment 2:
Prepare the Martensite Stainless Steel of copper-cerium-containing surface film with magnetron sputtering method, comprise the following steps:
(1) target is chosen identical with embodiment 1;
(2) substrate processing
Choose the 1Cr13 Martensite Stainless Steel as substrate, substrate is cleaned with ultrasonic wave and acetone successively, put into magnetron sputtering chamber after polishing;
(3) bombardment preheating
The vacuum tightness of sputtering chamber is less than 2 * 10 -5Pa passes into purity and is 99.99% argon gas, and sputtering pressure is adjusted to 2.5Pa, open the negative bias power supply, transfer to 400 ~ 800V scope, workpiece is carried out the ion bombardment aura clean, open simultaneously well heater to workpiece preheating to be plated, preheating temperature is 200 ℃, warm up time 15min;
(4) spatter film forming
Target 1 voltage transfers to 300V, target 2 voltage 500V, and sputtering current is the 0.4A constant current, substrate is carried out recirculated water cooling process, target is 90mm to the distance of substrate, sputtering time 1h, making film thickness is 20 μ m.
Embodiment 3:
Prepare the ferritic stainless steel of copper-cerium-containing surface film with magnetron sputtering method, comprise the following steps:
(1) target is chosen identical with embodiment 1;
(2) substrate processing
Choose the 0Cr13 Martensite Stainless Steel as substrate, substrate is cleaned with ultrasonic wave and acetone successively, put into magnetron sputtering chamber after polishing;
(3) bombardment preheating
The vacuum tightness of sputtering chamber is less than 2 * 10 -5Pa passes into purity and is 99.99% argon gas, and sputtering pressure is adjusted to 2.5Pa, open the negative bias power supply, transfer to 400 ~ 800V scope, workpiece is carried out the ion bombardment aura clean, open simultaneously well heater to workpiece preheating to be plated, preheating temperature is 200 ℃, warm up time 15min;
(4) spatter film forming
Target 1 voltage transfers to 300V, target 2 voltage 500V, and sputtering current is the 0.3A constant current, substrate is carried out recirculated water cooling process, target is 80mm to the distance of substrate, sputtering time 1h, making film thickness is 20 μ m.

Claims (1)

1. the anti-bacteria stainless steel of a copper-cerium-containing surface film, comprise stainless steel substrate and adopt the magnetron sputtering technique plating at the antibiotic layer of stainless steel surface, it is characterized in that: the antibiotic layer of plating cupric, cerium film on austenite or Martensite Stainless Steel base material, thickness are 20 μ m.
CN 201220561576 2012-10-30 2012-10-30 Antibacterial stainless steel with copper-cerium thin film contained on surface Expired - Fee Related CN203007383U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105239068A (en) * 2015-11-17 2016-01-13 广西中医药大学 Stainless steel material modified through ruthenium complex and preparation method and application thereof
CN107299320A (en) * 2015-11-16 2017-10-27 王贝 A kind of anti-bacteria stainless steel
CN108329515A (en) * 2018-03-21 2018-07-27 安徽江淮汽车集团股份有限公司 A kind of preparation method of antibacterial agent

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107299320A (en) * 2015-11-16 2017-10-27 王贝 A kind of anti-bacteria stainless steel
CN107299320B (en) * 2015-11-16 2018-12-25 佛山市钿汇不锈钢有限公司 A kind of anti-bacteria stainless steel
CN105239068A (en) * 2015-11-17 2016-01-13 广西中医药大学 Stainless steel material modified through ruthenium complex and preparation method and application thereof
CN105239068B (en) * 2015-11-17 2017-11-03 广西中医药大学 Stainless steel material of ruthenium complex modification and preparation method thereof and purposes
CN108329515A (en) * 2018-03-21 2018-07-27 安徽江淮汽车集团股份有限公司 A kind of preparation method of antibacterial agent

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