CN109487269A - A kind of preparation method of antibiotic property composite coating - Google Patents

A kind of preparation method of antibiotic property composite coating Download PDF

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Publication number
CN109487269A
CN109487269A CN201811405652.8A CN201811405652A CN109487269A CN 109487269 A CN109487269 A CN 109487269A CN 201811405652 A CN201811405652 A CN 201811405652A CN 109487269 A CN109487269 A CN 109487269A
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CN
China
Prior art keywords
coating
preparation
antibiotic property
composite coating
substrate surface
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811405652.8A
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Chinese (zh)
Inventor
曾晨光
李少军
许羽冬
陈诗浩
杨习锋
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Guangzhou Sun Shing Biotech Co ltd
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Guangzhou Sun Shing Biotech Co ltd
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Priority to CN201811405652.8A priority Critical patent/CN109487269A/en
Publication of CN109487269A publication Critical patent/CN109487269A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C26/00Coating not provided for in groups C23C2/00 - C23C24/00
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00Working by laser beam, e.g. welding, cutting or boring
    • B23K26/352Working by laser beam, e.g. welding, cutting or boring for surface treatment
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C28/00Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Plasma & Fusion (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The present invention provides a kind of preparation methods with antibiotic property composite coating, laser burn processing first is carried out to matrix surface, then silver nitrate solution is coated on substrate surface, it is irradiated again with ultraviolet lamp, nano-Ag particles are made to be attached to porous surface, and form silver coating, HA and silver powder are mixed again, and the HA/Ag solution that compound concentration is 1-100mg/mL is stirred, then the sample with HA/Ag coating is obtained in substrate surface with dip-coating method, air drying, Laser Cladding Treatment finally is carried out to the sample of acquisition, so that the HA/Ag coating on substrate surface is combined closely with substrate.

Description

A kind of preparation method of antibiotic property composite coating
Technical field
The present invention relates to a kind of antibiotic property carboxy apatite composite coatings, belong to medical bio field of ceramic coatings.
Background technique
Hydroxyapatite has the chemical composition and crystal structure similar with main mine substance in human body bone and tooth, is The main inorganic composition of body bone tissue is typical bioactive materials.But hydroxylapatite ceramic mechanical property is poor, Bending strength and fracture toughness index are below human body dense bone, it is difficult to use at human body carrying position.It (is closed in metals such as titaniums Gold) deposition hydroxylapatite ceramic coating can overcome the brittleness of hydroxyapatite body material on matrix, give full play to metal alloy High intensity and high tenacity, improve the bearing capacity of implant.Meanwhile the good biological activated energy of hydroxyapatite makes implant With the good combination of bone tissue.Using plasma spraying method, the hydroxyapatite coating layer prepared on the matrixes such as titanium alloy It is clinically one of most widely used artificial bone substitution material, is widely used in hip prosthesis and tooth root planting body etc..
For bone substitution material during implant surgery, infection caused by bacterium accounts for considerable proportion.Normal use is various anti- Raw element solves the problems, such as bacterium infection when operation, but increases bacterial antibiotic in the biomembrane that implant surface is formed Drug resistance causes antibiotic drug effect to reduce.In order to more efficiently prevent from infection, on bone implant material surface, load antibacterial agent is one Kind more effective method.Silver is a kind of most common inorganic antiseptic, has many advantages, such as efficient, safety, broad-spectrum antiseptic, wide It is general to be applied in antibacterial product.
However, it is attached in substrate in the adhesive force of hydroxyapatite and raising carboxy apatite composite coating to improve silver Put forth effort, still falls within a big technical problem.
Summary of the invention
The present invention provides a kind of preparation method with antibiotic property composite coating, comprising the following steps:
S1. laser burn processing is carried out to matrix surface, forms nanometer porous structure on surface;
S2. silver nitrate solution is coated on S1 treated substrate surface, then is irradiated with ultraviolet lamp, make nano silver Grain is attached to porous surface, and forms silver coating;
S3. HA and silver powder are mixed, and the HA/Ag solution that compound concentration is 1-100mg/mL is stirred, and is then used Dip-coating method obtains the sample with HA/Ag coating, air drying in substrate surface.
S4, Laser Cladding Treatment is carried out to the sample that step S3 is obtained, so that HA/Ag coating and substrate on substrate surface It combines closely.
Preferably, the processing of laser burn described in S1 is utilized in the mode of line laser punching.
Preferably, the concentration of silver nitrate solution described in S2 is 1-100mM.
Preferably, the mass ratio of HA and silver powder described in S3 are 1-20:1.
Preferably, the silver powder partial size is 20-100 μm, and the partial size of the HA powder is 10-100 μm.
Preferably, the substrate is titanium or its alloy.
The beneficial effects of the present invention are:
First, first coarse porous nanometer structure is formed, is conducive to subsequent by the way of laser burn in substrate surface Nano-Ag particles adhere to thereon;
Second, middle layer silver coating is increased as transition zone, is conducive to HA/Ag coating and is firmly adhered to thereon, further Improve the adhesive force of coating;
Third, HA/Ag coating are handled using laser melting coating, can be realized HA/Ag coating and the base on substrate surface Bottom is combined closely, and does not influence the anti-microbial property of coating.
Specific embodiment
Embodiment 1
A kind of preparation method with antibiotic property composite coating, comprising the following steps:
S1. laser burn processing is carried out to titanium alloy surface, forms nanometer porous structure on surface;
S2. 1mM silver nitrate solution is coated on S1 treated substrate surface, then the purple with wavelength 400nm, power 50W Outer lamp is irradiated, and so that nano-Ag particles is attached to porous surface, and form silver coating;
S3. HA and silver powder are mixed, and the HA/Ag solution that compound concentration is 1mg/mL is stirred, then with dipping Czochralski method obtains the sample with HA/Ag coating, air drying in substrate surface, and the silver powder partial size is 20 μm, the HA powder The partial size at end is 10 μm, and the mass ratio of the HA and silver powder is 1:1;
S4, Laser Cladding Treatment is carried out to the sample that step S3 is obtained, so that HA/Ag coating and substrate on substrate surface It combines closely.
Test shows that the HA/Ag coating anti-microbial property of titanium alloy surface is excellent, and adhesive force is high.
Embodiment 2
A kind of preparation method with antibiotic property composite coating, comprising the following steps:
S1. laser burn processing is carried out to titanium alloy surface, forms nanometer porous structure on surface;
S2. 50mM silver nitrate solution is coated on S1 treated substrate surface, then with wavelength 300nm, power 100W Ultraviolet lamp is irradiated, and so that nano-Ag particles is attached to porous surface, and form silver coating;
S3. HA and silver powder are mixed, and the HA/Ag solution that compound concentration is 50mg/mL is stirred, then with dipping Czochralski method obtains the sample with HA/Ag coating, air drying in substrate surface, and the silver powder partial size is 50 μm, the HA powder The partial size at end is 50 μm, and the mass ratio of the HA and silver powder is 10:1;
S4, Laser Cladding Treatment is carried out to the sample that step S3 is obtained, so that HA/Ag coating and substrate on substrate surface It combines closely.
Test shows that the HA/Ag coating anti-microbial property of titanium alloy surface is excellent, and adhesive force is high.
Embodiment 3
A kind of preparation method with antibiotic property composite coating, comprising the following steps:
S1. laser burn processing is carried out to titanium alloy surface, forms nanometer porous structure on surface;
S2. 100mM silver nitrate solution is coated on S1 treated substrate surface, then with wavelength 400nm, power 100W Ultraviolet lamp is irradiated, and so that nano-Ag particles is attached to porous surface, and form silver coating;
S3. HA and silver powder are mixed, and the HA/Ag solution that compound concentration is 100mg/mL is stirred, then with leaching Stain czochralski method obtains the sample with HA/Ag coating, air drying in substrate surface, and the silver powder partial size is 100 μm, the HA The partial size of powder is 100 μm, and the mass ratio of the HA and silver powder is 20:1;
S4, Laser Cladding Treatment is carried out to the sample that step S3 is obtained, so that HA/Ag coating and substrate on substrate surface It combines closely.
Test shows that the HA/Ag coating anti-microbial property of titanium alloy surface is excellent, and adhesive force is high.

Claims (6)

1. a kind of preparation method of antibiotic property composite coating, which comprises the following steps:
S1. laser burn processing is carried out to matrix surface, forms nanometer porous structure on surface;
S2. silver nitrate solution is coated on S1 treated substrate surface, then is irradiated with ultraviolet lamp, keep nano-Ag particles attached In porous surface;
S3. HA and silver powder are mixed, and the HA/Ag solution that compound concentration is 1-100mg/mL is stirred, then with dipping Czochralski method obtains the sample with HA/Ag coating, air drying in substrate surface.
S4, Laser Cladding Treatment is carried out to the sample that step S3 is obtained, so that the HA/Ag coating and substrate on substrate surface are close In conjunction with.
2. a kind of preparation method of composite coating with antibiotic property according to claim 1, which is characterized in that described in S1 Laser burn processing is utilized in the mode of line laser punching.
3. a kind of preparation method of composite coating with antibiotic property according to claim 1, which is characterized in that described in S2 The concentration of silver nitrate solution is 1-100mM.
4. a kind of preparation method of composite coating with antibiotic property according to claim 1, which is characterized in that described in S3 HA and the mass ratio of silver powder are 1-20:1.
5. a kind of preparation method of composite coating with antibiotic property according to claim 1, which is characterized in that the silver Powder diameter is 20-100 μm, and the partial size of the HA powder is 10-100 μm.
6. a kind of preparation method of composite coating with antibiotic property according to claim 1, which is characterized in that the base Bottom is titanium or its alloy.
CN201811405652.8A 2018-11-23 2018-11-23 A kind of preparation method of antibiotic property composite coating Pending CN109487269A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111334746A (en) * 2020-04-26 2020-06-26 广州珈鹏科技有限公司 Biological ceramic coating with antibacterial activity and preparation method thereof
CN113088958A (en) * 2021-03-09 2021-07-09 中南大学 Gradient composite bioactive ceramic coating material and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104127911A (en) * 2014-07-21 2014-11-05 华中科技大学 Preparation method of biological composite material using titanium alloy as implant

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104127911A (en) * 2014-07-21 2014-11-05 华中科技大学 Preparation method of biological composite material using titanium alloy as implant

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
XIANGMEI LIU 等: ""Laser fabrication of Ag-HA nanocomposites on Ti6Al4V implant for enhancing bioactivity and antibacterial capability"", 《MATERIALS SCIENCE AND ENGINEERING C》 *
刘榕芳等: "两步法电沉积制备HA/ Ag复合涂层", 《应用化学》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111334746A (en) * 2020-04-26 2020-06-26 广州珈鹏科技有限公司 Biological ceramic coating with antibacterial activity and preparation method thereof
CN113088958A (en) * 2021-03-09 2021-07-09 中南大学 Gradient composite bioactive ceramic coating material and preparation method thereof
CN113088958B (en) * 2021-03-09 2021-12-28 中南大学 Gradient composite bioactive ceramic coating material and preparation method thereof

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Application publication date: 20190319

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