CN104947096A - Preparation method of nickel-phosphorus-graphene oxide composite antibacterial coating - Google Patents
Preparation method of nickel-phosphorus-graphene oxide composite antibacterial coating Download PDFInfo
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Abstract
The invention discloses a preparation method of a nickel-phosphorus-graphene oxide composite antibacterial coating. The method comprises the steps that (1) polyethyleneimine modifies graphene oxide; (2), the modified graphene oxide is added into a chemical nickel-phosphorus plating solution to be magnetically stirred, and the temperature rises to 86 DEG C to 90 DEG C; and (4), a workpiece obtained after pretreatment such as oil removing and activation is added into a composite plating solution to react for 40 minutes to 120 minutes, and the nickel-phosphorus-graphene oxide composite antibacterial coating is obtained. A chemical composite plating method is adopted to prepare the nickel-phosphorus-graphene oxide composite antibacterial coating, and the method is simple in technology, convenient to operate and high in production efficiency; and the prepared nickel-phosphorus-graphene oxide composite antibacterial coating effectively reduces the bacterial adsorption and improves the antibacterial activity of chemically-plated nickel and phosphorus.
Description
Technical field
The present invention relates to a kind of preparation method of chemical composite plating, particularly a kind of preparation method of nickel phosphorus oxidation Graphene composite antibacterial coating.
Background technology
Extensively there is occurring in nature in microorganism, suppresses harmful microbe growth can improve environment for human survival and then improve the standard of living of people.Ni-P, as a kind of conventional material surface means, adds the inert particle that some have specific physico-chemical property in the plating solution, can comprise metal, semi-conductor or nonmetallic surface form the uniform composite deposite of thickness at differing materials.These property coating can meet different occasion needs, as wear resistant composite plating, corrosion-resistant coating and antimicrobial plating etc., make them all be with a wide range of applications in petroleum chemical industry, aircraft industry, daily living article and technical field of biological material etc.
Graphene is by the tightly packed bi-dimensional cellular shape crystalline network become of monolayer carbon atom, because of excellent physicochemical property, has broad application prospects in conduction, catalysis, photoabsorption, medicine, magneticmedium and novel material etc.Graphene after oxidation, a large amount of oxy radicals that its surface exists, the combination for other particle provides effective site.But graphene oxide is electronegative, when joining in the metal ion plating solution with positive charge, due to electrostatic interaction, graphene oxide is caused to be reunited, not can be uniformly dispersed in plating solution, cause forming uniform nickel phosphorus oxidation Graphene composite antibacterial coating.Therefore, using polyethylene imine beautify graphene oxide as the reinforcement improving anti-microbial property, the nickel phosphorus oxidation graphene composite material obtained is that the development of chemical nickel phosphorus plating multifunctional material opens new field.Both can widen the research field of chemical nickel phosphorus plating, and make again chemical nickel plating phosphorus composite material go a step further to practical application aspect is more advanced in years.Therefore, the research of a kind of preparation method of nickel phosphorus oxidation Graphene composite antibacterial coating has great importance to the preparation of novel antibacterial material and exploitation.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, provides a kind of technique simple, easy to operate, the preparation method of the nickel phosphorus oxidation Graphene composite antibacterial coating that production efficiency is high.
Technical scheme: in order to realize foregoing invention object, the technical solution used in the present invention is as follows:
A preparation method for nickel phosphorus oxidation Graphene composite antibacterial coating, comprises the following steps:
1) graphene oxide getting 0.05 ~ 0.1g adds in deionized water, in ice-water bath ultrasonic 20 ~ 40 minutes, obtains the single-layer graphene oxide dispersion soln that graphene oxide concentration is 1.5 ~ 2.5g/L;
2) polymine getting 0.1 ~ 0.8g adds in single-layer graphene oxide dispersion soln, and 60 ~ 80 DEG C are reacted 15 ~ 24 hours; By its under 8000 ~ 10000rpm centrifugal 10 ~ 20 minutes after reaction terminates, then use washed with de-ionized water; Suspension is put into dialysis tubing dialysis after 3 days, obtain the graphene oxide of polyethylene imine beautify;
3) graphene dispersing solution will modified, adds in chemical plating fluid and is made into the chemical composite plating bath that concentration is 0.1 ~ 0.5g/L, ultrasonic disperse 5 ~ 10 minutes, magnetic agitation 30 ~ 60 minutes;
4) by the workpiece after fuel-displaced activating pretreatment, the composite plating bath putting into 86 ~ 90 DEG C carries out Ni-P 40 ~ 120 minutes, namely obtains nickel phosphorus oxidation Graphene composite antibacterial coating;
Wherein, the consisting of of often liter of chemical nickel plating phosphor bath: 20 ~ 30g NiSO
46H
2o, 15 ~ 20g Na
3c
6h
5o
72H
2o, 25 ~ 30g NaH
2pO
22H
2o, 15 ~ 20g CH
3cOONa3H
2o, 1 ~ 2ppm (CH
2) CS; Each component is joined in deionized water and dissolves, and regulate pH to obtain with dilute sulphuric acid and sodium hydroxide.
Described graphene oxide is micron order, and its diameter is 0.5 ~ 2 micron.
Described single-layer graphene oxide dispersion soln, the concentration range preferentially choosing graphene oxide is 2 ~ 2.5g/L.
Described polyethylene imine beautify graphene oxide liquid mixture, the concentration range preferentially choosing polymine is 10 ~ 12.5g/L.
Described chemical nickel phosphorus plating composite plating bath, preferentially choosing pH scope is 4.6 ~ 4.8.
Described chemical nickel phosphorus plating composite plating bath, preferentially choosing plating temperature scope is 87 ~ 88 DEG C.
The present invention adopts polyethylene imine beautify graphene oxide, prevents the mutual reunion between graphene oxide in containing the plating solution of metal ion, realizes the preparation of nickel phosphorus oxidation Graphene composite antibacterial coating.Prepared composite deposite is a kind of excellent anti-biotic material.
Beneficial effect: compared with prior art, the preparation method of nickel phosphorus oxidation Graphene composite antibacterial coating of the present invention, achieves the dispersed of graphene oxide, effectively prevent the reunion of graphene oxide in chemical plating fluid.Prepared nickel phosphorus oxidation Graphene composite antibacterial coating, be positioned over containing in staphylococcus glucose coccus and colibacillary bacterium liquid, antibiotic rate can reach 96% and 97% respectively, and fungistatic effect is remarkable.
Accompanying drawing explanation
Fig. 1 is the bacteriostasis rate result of nickel phosphorus oxidation Graphene composite antibacterial coating for gram-positive microorganism streptococcus aureus (Staphylococcus aureus); Wherein, a is the antibiotic rate of nickel-phosphorus chemical plating for gram-positive microorganism streptococcus aureus; B is the bacteriostasis rate of antibacterial composite material in embodiment 1; C is the antibiotic rate of antimicrobial plating in embodiment 2; D is the antibiotic rate of antimicrobial plating in embodiment 3;
Fig. 2 is the bacteriostasis rate result of nickel phosphorus oxidation Graphene composite antibacterial coating for Gram-negative bacteria intestinal bacteria (Escherichia coli); Wherein, a is the antibiotic rate of nickel-phosphorus chemical plating for gram-positive microorganism streptococcus aureus; B is the bacteriostasis rate of antibacterial composite material in embodiment 1; C is the antibiotic rate of antimicrobial plating in embodiment 2; D is the antibiotic rate of antimicrobial plating in embodiment 3.
Fig. 3 is the infrared spectrogram of the polyethylene imine beautify graphene oxide prepared by embodiment 3;
Fig. 4 is the x-ray photoelectron spectrogram of the nickel phosphorus oxidation Graphene composite antibacterial coating prepared by embodiment 3;
Fig. 5 is the stereoscan photograph figure of nickel-phosphorus chemical plating and the nickel phosphorus oxidation Graphene composite antibacterial coating prepared by embodiment 3.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, but the present invention is not by the restriction of these examples of implementation.
Embodiment 1
The graphene oxide getting 0.05g adds in deionized water, in ice-water bath ultrasonic 20 minutes, obtains the single-layer graphene oxide dispersion soln that graphene oxide concentration is 1g/L; The polymine getting 0.1g adds in single-layer graphene oxide dispersion soln, and 60 DEG C are reacted 15 hours; By its under 8000rpm centrifugal 10 minutes after reaction terminates, then use washed with de-ionized water 3 times; Suspension is put into dialysis tubing dialysis after 3 days, obtain polyethylene imine beautify graphene oxide; Chemical nickel plating phosphor bath, often liter by 20g NiSO
46H
2o, 15g Na
3c
6h
5o
72H
2o, 25g NaH
2pO
22H
2o, 15g CH
3cOONa3H
2o, 1ppm (CH
2) CS joins in deionized water and dissolve, and regulate pH4.8 to obtain with dilute sulphuric acid and sodium hydroxide.The graphene dispersing solution will modified again, adds in chemical plating fluid and is made into the chemical composite plating bath that concentration is 0.1g/L, and through ultrasonic disperse 5 minutes, magnetic agitation obtained for 60 minutes; By pretreated workpiece such as fuel-displaced activation, the composite plating bath putting into 86 DEG C carries out Ni-P 40 minutes, namely obtains nickel phosphorus oxidation Graphene composite antibacterial coating.
Anti-microbial property test is carried out to nickel phosphorus oxidation Graphene composite antibacterial coating, specific as follows:
The solid medium cultivating intestinal bacteria employing is trypticase soy agar substratum (TSA), substratum consists of: pancreatic digest of casein 15.0g/L, soyflour papain digestion thing 5.0g/L, sodium-chlor 5.0g/L, agar 15.0g/L, pH value 7.2, high pressure steam 121 DEG C of sterilizings, after 20 minutes, are down flat plate.The staphylococcus glucose coccus of freezen protective is got and strain Escherichia coli is inoculated on TSA culture plate respectively with disinfection inoculation ring, be placed in incubator 37 DEG C of constant temperature culture 24 hours, divide with disinfection inoculation ring picking colony in the aseptic Erlenmeyer flask being clipped to the pancreas peptone soybean broth substratum (TSB) filling 100mL sterilizing, substratum consists of: pancreatic digest of casein 15.0g/L, soyflour papain digestion thing 5.0g/L, sodium-chlor 5.0g/L, pH value 7.2, high pressure steam 121 DEG C of sterilizings 20 minutes.Turbidimetry measurement is adopted to make its bacterial concentration 5 × 10
7about CFU/mL, thermal agitation makes it mix.The Composite Coatings workpiece of 2cm × 2cm is placed in bacterium liquid, and at rotating speed, to be 20rpm and temperature be cultivates 1 hour in 37 DEG C of incubators.
Composite Coatings workpiece is taken out, after aseptic deionized water clean surface, puts into 10 milliliters of sterile beaker and carry out supersound process 5 minutes.Getting 100 μ L suspension adopts the dull and stereotyped method of stepwise dilution painting to count the bacterium alive be adsorbed on workpiece respectively, and bacteriostasis rate is by following formulae discovery: R(%)=(N
blank-N
sample)/N
blank× 100%, wherein, N
blankand N
samplebe respectively the colony number being adsorbed on nickel-phosphorus chemical plating and nickel phosphorus oxidation Graphene composite antibacterial coating.
Nickel-phosphorus chemical plating and nickel phosphorus oxidation Graphene composite antibacterial coating to the bacteriostasis rate result of staphylococcus glucose coccus, as shown in Figure 1.The bacteriostasis rate (Fig. 1-a) can finding out nickel phosphorus oxidation Graphene composite antibacterial coating in embodiment 1 is 58%, has good suppression staphylococcus glucose coccus effect.
Nickel-phosphorus chemical plating and nickel phosphorus oxidation Graphene composite antibacterial coating to colibacillary bacteriostasis rate result, as shown in Figure 2.The bacteriostasis rate (Fig. 2-a) can finding out nickel phosphorus oxidation Graphene composite antibacterial coating in embodiment 1 is 61%, has superior suppression intestinal bacteria effect.
Embodiment 2
The graphene oxide getting 0.08g adds in deionized water, in ice-water bath ultrasonic 20 minutes, obtains the single-layer graphene oxide dispersion soln that graphene oxide concentration is 1g/L; The polymine getting 0.2g adds in single-layer graphene oxide dispersion soln, and 60 DEG C are reacted 15 hours; By its under 8000rpm centrifugal 10 minutes after reaction terminates, then use washed with de-ionized water 3 times; Suspension is put into dialysis tubing dialysis after 3 days, obtain polyethylene imine beautify graphene oxide; Chemical nickel plating phosphor bath, often liter by 20g NiSO
46H
2o, 15g Na
3c
6h
5o
72H
2o, 25g NaH
2pO
22H
2o, 15g CH
3cOONa3H
2o, 2ppm (CH
2) CS joins in deionized water and dissolve, and regulate pH=4.8 to obtain with dilute sulphuric acid and sodium hydroxide.The graphene dispersing solution will modified again, adds in chemical plating fluid and is made into the chemical composite plating bath that concentration is 0.2g/L, and through ultrasonic disperse 5 minutes, magnetic agitation obtained for 60 minutes; By pretreated workpiece such as fuel-displaced activation, the composite plating bath putting into 86 DEG C carries out Ni-P 60 minutes, namely obtains nickel phosphorus oxidation Graphene composite antibacterial coating.Performance test methods is with embodiment 1, and wherein, the bacteriostasis rate (Fig. 1-b) suppressing staphylococcus glucose coccus is 85%, suppresses colibacillary bacteriostasis rate (Fig. 2-b) to be 86%.
Embodiment 3
The graphene oxide getting 0.08g adds in deionized water, in ice-water bath ultrasonic 20 minutes, obtains the single-layer graphene oxide dispersion soln that graphene oxide concentration is 1.5g/L; The polymine getting 0.5g adds in single-layer graphene oxide dispersion soln, and 60 DEG C are reacted 24 hours; By its under 10000rpm centrifugal 10 minutes after reaction terminates, then use washed with de-ionized water 3 times; Suspension is put into dialysis tubing dialysis after 3 days, obtain polyethylene imine beautify graphene oxide; Chemical nickel plating phosphor bath, often liter by 30g NiSO
46H
2o, 20g Na
3c
6h
5o
72H
2o, 30g NaH
2pO
22H
2o, 20g CH
3cOONa3H
2o, 1ppm (CH
2) CS joins in deionized water and dissolve, and regulate pH=4.8 to obtain with dilute sulphuric acid and sodium hydroxide.The graphene dispersing solution will modified again, adds in chemical plating fluid and is made into the chemical composite plating bath that concentration is 0.3g/L, and through ultrasonic disperse 5 minutes, magnetic agitation obtained for 60 minutes; By pretreated workpiece such as fuel-displaced activation, the composite plating bath putting into 88 DEG C carries out Ni-P 60 minutes, namely obtains nickel phosphorus oxidation Graphene composite antibacterial coating.Performance test methods is with embodiment 1, and wherein, the bacteriostasis rate (Fig. 1-c) suppressing staphylococcus glucose coccus is 95%, suppresses colibacillary bacteriostasis rate (Fig. 2-c) to be 94%.
Embodiment 4
The graphene oxide getting 0.08g adds in deionized water, in ice-water bath ultrasonic 20 minutes, obtains the single-layer graphene oxide dispersion soln that graphene oxide concentration is 4g/L; The polymine getting 0.8g adds in single-layer graphene oxide dispersion soln, and 60 DEG C are reacted 24 hours; By its under 10000rpm centrifugal 10 minutes after reaction terminates, then use washed with de-ionized water 3 times; Suspension is put into dialysis tubing dialysis after 3 days, obtain polyethylene imine beautify graphene oxide; Chemical nickel plating phosphor bath, often liter by 25g NiSO
46H
2o, 18g Na
3c
6h
5o
72H
2o, 30g NaH
2pO
22H
2o, 18g CH
3cOONa3H
2o, 1ppm (CH
2) CS joins in deionized water and dissolve, and regulate pH=4.8 to obtain with dilute sulphuric acid and sodium hydroxide.The graphene dispersing solution will modified again, adds in chemical plating fluid and is made into the chemical composite plating bath that concentration is 0.4g/L, and through ultrasonic disperse 5 minutes, magnetic agitation obtained for 60 minutes; By pretreated workpiece such as fuel-displaced activation, the composite plating bath putting into 88 DEG C carries out Ni-P 60 minutes, namely obtains nickel phosphorus oxidation Graphene composite antibacterial coating.Performance test methods is with embodiment 1, and wherein, the bacteriostasis rate (Fig. 1-c) suppressing staphylococcus glucose coccus is 96%, suppresses colibacillary bacteriostasis rate (Fig. 2-c) to be 97%.
Performance test is carried out to nickel phosphorus oxidation Graphene composite antibacterial coating, specific as follows:
1) examination of infrared spectrum
The infrared spectrogram of the graphene oxide of graphene oxide and polyethylene imine beautify, as shown in Figure 3.In figure, a is the infrared spectrogram of graphene oxide; B is the infrared spectrogram of the graphene oxide of polyethylene imine beautify.The graphene oxide of polyethylene imine beautify is 1633cm in wave number as we can see from the figure
-1time there is the absorption peak of amido linkage, confirm that the amino of polymine and the carboxyl reaction of graphene oxide generate amido linkage.
2) x-ray photoelectron spectroscopy (XPS) test
The x-ray photoelectron spectroscopy figure of nickel phosphorus oxidation Graphene composite antibacterial coating, as shown in Figure 4.The combination of Ni in 2p region can be 855.81eV as we can see from the figure, the combination of P in 2p region can be 129.07eV, the combination of C in 1s region can be 284.81eV, the combination of O in 1s region can be 531.61eV, the combination of N in 1s region can be 400.27eV, shows that the graphene oxide of polyethylene imine beautify successfully joins among nickel-phosphorus composite deposit.
3) scanning electron microscope (SEM) test
Nickel-phosphorus chemical plating and nickel phosphorus oxidation Graphene composite antibacterial coating SEM photo, as shown in Figure 5.Nickel-phosphorus chemical plating presents clearly crystalline structure, when the graphene oxide of polyethylene imine beautify joins in nickel-phosphorus coating, interrupted the formation of well-regulated crystalline structure, nickel phosphorus oxidation Graphene composite antibacterial coating layer reveals the apparent form of more all even densification.
Claims (7)
1. a preparation method for nickel phosphorus oxidation Graphene composite antibacterial coating, is characterized in that, comprise the following steps:
1) graphene oxide getting 0.05 ~ 0.1g adds in deionized water, in ice-water bath ultrasonic 20 ~ 40 minutes, obtains the single-layer graphene oxide dispersion soln that graphene oxide concentration is 1.5 ~ 2.5g/L;
2) polymine getting 0.1 ~ 0.8g adds in single-layer graphene oxide dispersion soln, and 60 ~ 80 DEG C are reacted 15 ~ 24 hours; By its under 8000 ~ 10000rpm centrifugal 10 ~ 20 minutes after reaction terminates, then use washed with de-ionized water; Suspension is put into dialysis tubing dialysis after 3 days, obtain the graphene oxide of polyethylene imine beautify;
3) graphene dispersing solution will modified, adds in chemical plating fluid and is made into the chemical composite plating bath that concentration is 0.1 ~ 0.5g/L, ultrasonic disperse 5 ~ 10 minutes, magnetic agitation 30 ~ 60 minutes;
4) by the workpiece after fuel-displaced activating pretreatment, the composite plating bath putting into 86 ~ 90 DEG C carries out Ni-P 40 ~ 120 minutes, namely obtains nickel phosphorus oxidation Graphene composite antibacterial coating;
Wherein, the consisting of of often liter of chemical nickel plating phosphor bath: 20 ~ 30g NiSO
46H
2o, 15 ~ 20g Na
3c
6h
5o
72H
2o, 25 ~ 30g NaH
2pO
22H
2o, 15 ~ 20g CH
3cOONa3H
2o, 1 ~ 2ppm (CH
2) CS; Each component is joined in deionized water and dissolves, and regulate pH to obtain with dilute sulphuric acid and sodium hydroxide.
2. the preparation method of nickel phosphorus oxidation Graphene composite antibacterial coating according to claim 1, it is characterized in that: described graphene oxide is micron order, diameter is 0.5 ~ 2 micron.
3. the preparation method of nickel phosphorus oxidation Graphene composite antibacterial coating according to claim 1, is characterized in that: the concentration of described single-layer graphene oxide dispersion soln is 2 ~ 2.5g/L.
4. the preparation method of nickel phosphorus oxidation Graphene composite antibacterial coating according to claim 1, is characterized in that: the concentration of described graphene oxide in chemical composite plating bath is 0.3 ~ 0.4g/L.
5. the preparation method of nickel phosphorus oxidation Graphene composite antibacterial coating according to claim 1, is characterized in that: the pH of described chemical composite plating bath is 4.5 ~ 5.0.
6. the preparation method of nickel phosphorus oxidation Graphene composite antibacterial coating according to claim 1, is characterized in that: the Ni-P time is 60 ~ 80 minutes.
7. the nickel phosphorus oxidation Graphene composite antibacterial coating obtained by the preparation method of the nickel phosphorus oxidation Graphene composite antibacterial coating described in claim 1-6 any one.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109207984A (en) * | 2018-08-20 | 2019-01-15 | 中国科学院金属研究所 | The preparation method of corrosion resistant antibiotic anti-biofouling multifunctional metal-base protective coating |
| CN109487247A (en) * | 2017-09-12 | 2019-03-19 | 欣兴电子股份有限公司 | Chemical nickel plating graphene composite material layer and its manufacturing method |
| CN115300482A (en) * | 2022-08-17 | 2022-11-08 | 山东大学 | Bovine serum albumin coated chlorhexidine loaded nickel phosphide nano-capsule, preparation method and antibacterial application thereof |
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| CN103833231A (en) * | 2014-03-06 | 2014-06-04 | 上海应用技术学院 | Glass with graphene oxide nickel-phosphorus composite coating and preparation method of glass |
| CN104313552A (en) * | 2014-10-22 | 2015-01-28 | 湖南元素密码石墨烯研究院（有限合伙） | Preparation method of chemical nickel-graphene antirust coating |
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2015
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Patent Citations (4)
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| CN103833231A (en) * | 2014-03-06 | 2014-06-04 | 上海应用技术学院 | Glass with graphene oxide nickel-phosphorus composite coating and preparation method of glass |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109487247A (en) * | 2017-09-12 | 2019-03-19 | 欣兴电子股份有限公司 | Chemical nickel plating graphene composite material layer and its manufacturing method |
| CN109207984A (en) * | 2018-08-20 | 2019-01-15 | 中国科学院金属研究所 | The preparation method of corrosion resistant antibiotic anti-biofouling multifunctional metal-base protective coating |
| CN115300482A (en) * | 2022-08-17 | 2022-11-08 | 山东大学 | Bovine serum albumin coated chlorhexidine loaded nickel phosphide nano-capsule, preparation method and antibacterial application thereof |
| CN115300482B (en) * | 2022-08-17 | 2023-11-28 | 山东大学 | Bovine serum albumin coated chlorhexidine loaded nickel phosphide nanocapsule, preparation method and antibacterial application thereof |
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Application publication date: 20150930 Assignee: NANJING QIUPU BIOLOGICAL TECHNOLOGY CO.,LTD. Assignor: Nanjing Forestry University Contract record no.: 2019320000114 Denomination of invention: Preparation method of nickel-phosphorus-graphene oxide composite antibacterial coating Granted publication date: 20170718 License type: Common License Record date: 20190424 Application publication date: 20150930 Assignee: KELEIBOSHI ENVIRONMENTAL PROTECTION TECHNOLOGY (SUZHOU) CO.,LTD. Assignor: Nanjing Forestry University Contract record no.: 2019320000111 Denomination of invention: Preparation method of nickel-phosphorus-graphene oxide composite antibacterial coating Granted publication date: 20170718 License type: Common License Record date: 20190423 |
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