CN107140599A - A kind of pattern surface preparation method with anti-microbial property - Google Patents
A kind of pattern surface preparation method with anti-microbial property Download PDFInfo
- Publication number
- CN107140599A CN107140599A CN201710284286.4A CN201710284286A CN107140599A CN 107140599 A CN107140599 A CN 107140599A CN 201710284286 A CN201710284286 A CN 201710284286A CN 107140599 A CN107140599 A CN 107140599A
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- China
- Prior art keywords
- micro
- yardstick
- pattern surface
- topological structure
- pattern
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00214—Processes for the simultaneaous manufacturing of a network or an array of similar microstructural devices
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
Abstract
The present invention discloses a kind of pattern surface preparation method with anti-microbial property, and key step includes：First prepared in silicon material substrate with it is micro-/receive the framework of yardstick topological structure；Then, prepare pure titanium pattern surface or prepare titanium dioxide pattern surface.The pattern surface that the present invention is prepared provides one kind independent of chemical composition or drug ingedient, the simple non-pesticide application strategy for producing anti-microbial property by physical pattern and its dimensional effect, because obtaining antibacterial effect not against antibiotic etc, patient can be prevented effectively from and produce drug anaphylaxis, the body burden of patient is significantly reduced.
Description
Technical field
There is antibacterial the invention belongs to biomimetic engineering and bio-medical engineering material preparing technical field, more particularly to one kind
The pattern surface preparation method of performance.
Background technology
In recent years, the problem of an aging population is increasingly highlighted, and the orthopaedics illness such as hip joint, diseases of knee joint and intervertebral disease is got over
To annoying the daily life of the elderly more.In view of the ever-increasing requirements of health care of the people so that artificial
Extensive concern of the orthopaedics implant such as joint replacement surgery surgical medical by more and more families and society.However, such hand
Art still suffers from a certain proportion of postoperative infection, and infection can cause surgery to fail, or even the serious consequence such as patient death.Cause
This, it would be highly desirable to develop a kind of new and effective Anti-infective bone surgical implant.But it is extremely challenging, due to orthopaedics implant infection
Mainly it is attributed to biomembrane to be formed on its surface, moreover biomembrane once forms extremely difficult elimination, so how effectively to prevent life
It is one of biomedical boundary problem to be resolved that thing film is formed on orthopaedics implant surface.Biomembrane is formed as bacterium
Caused in the adhesion of orthopaedics implant material surface, breeding, perch.Bacterium is orthopaedics implant surface in the adhesion of material surface
The formation of biomembrane and the first step of Subsequent infection are also a crucial step.Therefore, make orthopaedics implant surface that there is antibacterial to glue
Attached performance and bactericidal property are the available strategies for preventing biofilm formation.
In view of biomembrane can protect bacterium allow its from antibiotic injury so that orthopaedics implant infection be difficult to individually according to
By antibiotic therapy；Again because the bacterium of more and more species generates the resistance to the action of a drug to common antibiotics, its drug effect is by significantly
Weaken；It is again very long plus the construction cycle of antibiotics；Then orthopaedics implant surface is obtained with non-pesticide application strategy good
Antibacterial adhesion and bactericidal property gradually paid close attention to by scientific research personnel.
The content of the invention
It is an object of the invention to overcome prior art deficiency, there is provided a kind of pattern surface system with anti-microbial property
Preparation Method.
The technical scheme is that a kind of pattern surface preparation method with anti-microbial property, including following step
Suddenly：
Step (1)：Prepared in silicon material substrate with it is micro-/receive the framework of yardstick topological structure；
Step (2)：Pattern surface is prepared, including：Prepare pure titanium pattern surface or prepare the micro- figure of titanium dioxide
Shape surface；
Micro-/yardstick of receiving refers to the range scale from ten microns to ten nanometers in the step (1)；
It is micro- in the step (1)/to receive yardstick topological structure, including：It is micro-/to receive the columnar arrays of yardstick, array of protrusions, pit
Array or groove array.
The pure titanium pattern surface for preparing in the step (2) is to use magnetron sputtering method, pure titanium is deposited on described
In step (1) have it is micro-/receive yardstick topological structure framework on form pure titanium microthin coating.
In the step (2) prepare titanium dioxide pattern surface be first with it is micro-/receive yardstick topological structure
Pure titanium microthin coating is deposited on framework, titanium dioxide microthin coating is turned into by oxidation processes.
It is to use photoetching process to prepare micro-/framework of yardstick topological structure received in the step (1) in silicon material substrate,
Its technique includes following 14 steps：Photomask design, thermal oxidation method growth silica coating, one layer of hexamethyl two of deposition
Silazane, coating photoresist, prebake conditions, ultraviolet exposure imaging, postexposure bake, development, eventually it is roasting, remove residual photoresist,
Silicon dioxide layer, etching silicon base are etched, photoresist layer is removed and removes silicon dioxide layer.
Beneficial effect
1. the pattern surface that the present invention is prepared provide it is a kind of independent of chemical composition or drug ingedient, merely
The non-pesticide application strategy of anti-microbial property is produced by physical pattern and its dimensional effect；
2. the present invention can be prevented effectively from patient and produce medicine mistake due to obtaining antibacterial effect not against antibiotic etc
Quick reaction, significantly reduces the body burden of patient；
3. the method for the present invention prepares the pattern surface of pure titanium, titanium dioxide biomaterial, not only with antibacterial
Performance, and ensure that good biocompatibility.
Brief description of the drawings
Fig. 1 be three kinds prepared with silicon material substrate it is micro-/receive the columnar arrays topological structure schematic diagram of yardstick：
(a), experimental comparison group；
(b), width=spacing=5 micron；
(c), width=spacing=10 micron；
(d), width=spacing=1 micron.
Embodiment
Below by specific embodiments and the drawings, the present invention is further illustrated.Embodiments of the invention be in order that
Those skilled in the art more fully understands the present invention, does not make any limitation to the present invention.
Embodiment：The step of a kind of pattern surface preparation method with anti-microbial property, this method, is specific as follows：
Step (1)：Prepared in silicon material substrate with it is micro-/receive the framework of yardstick topological structure, micro-/yardstick of receiving refers to
Range scale from ten microns to ten nanometers, micro-/yardstick topological structure of receiving includes：It is micro-/receive yardstick columnar arrays, projection battle array
Row, pit array or groove array；
It is to use photoetching process to prepare micro-/framework of yardstick topological structure received in the step (1) in silicon material substrate,
Concrete technology step is as follows：
S1, photomask design：With L-Edit (Tanner Research, Inc.) software carry out it is micro-/receive yardstick column battle array
Row, array of protrusions, pit array or the corresponding photomask design of groove array；
S2, thermal oxidation method growth silica coating：With " wet oxidation ", silicon chip is aoxidized in diffusion furnace,
Finally obtaining a layer thickness on silicon chip isSilicon dioxide layer；
S3, one layer of HMDS (HMDS) of deposition：Purpose is for strengthening the adhesion of photoresist and silicon chip surface
Intensity；
S4, coating photoresist：From positive photoresist (AZ HiR 1075), whirl coating rotating speed is 4000rpm, final to obtain
Photoresist coating thickness be about
S5, prebake conditions：The silicon chip for having had been coated with photoresist is placed in oven and toasts 60s at 90 DEG C, it is therefore an objective to is removed
The adhesion strength of solvent and stress, enhancing photoresist and silicon chip surface；
S6, ultraviolet exposure imaging：Purpose is by the pattern transfer on photomask to photoresist；
S7, postexposure bake：By being placed in by the silicon chip of ultraviolet exposure in oven 60s is toasted at 110 DEG C；
S8, development：Developed in the way of spraying FHD-5 developer solutions to silicon chip surface, so as to obtain photoresist pattern；
S9, end are roasting：Silicon chip after development is placed in oven and toasts 60s at 120 DEG C, it is therefore an objective to photoetching is further enhanced
The adhesion strength of glue and silicon chip surface, and ensure that photoresist pattern will not be deformed；
S10, removal residual photoresist：The unnecessary photoresist that left behind after developing procedure is gone with oxygen plasma
Remove；
S11, etching silicon dioxide layer：It is saturating with " silica dry etching method " (AOE-advanced oxideetch) etching
The silicon dioxide layer of silicon chip surface, so that pattern is transferred into silicon dioxide layer from photoresist layer；
S12, etching silicon base：Silicon chip is etched with " silicon dry etching method " (DRIE-Deep reactive-ion etching)
Silicon substrate material, so that pattern is transferred in silicon base from the silicon dioxide layer of silicon chip surface；
S13, removal photoresist layer：
S13-1, first, silicon chip Jing Guo " etching silicon base " process is handled with oxygen plasma
20min, to remove most photoresist layers；
S13-2, then, treated silicon chip is immersed 120 DEG C of H2SO4+H2O2Solution bath 10min,
Further remove photoetching glue residua；
S14, removal silicon dioxide layer：By silicon chip immersion BOE (buffered Jing Guo " removal photoresist layer " process
Oxide etching) solution 3~5min, to remove the silicon dioxide layer of silicon chip surface, so far, silicon material substrate micro/nono chi
The framework of degree topological structure has prepared completion.
Be as shown in Figure 1 three kinds prepared with silicon material substrate it is micro-/receive the columnar arrays topological structure schematic diagram of yardstick.
Step (2)：Preparing pattern surface includes：Prepare pure titanium pattern surface or prepare titanium dioxide micrographics
Change surface；
A, prepare pure titanium pattern surface：Using magnetron sputtering method, target is used as by 99.99% pure titanium dish of purity
Material, in the vacuum environment (3 × 10 of room temperature-7Torr in), with constant radio frequency power 100W magnetron sputtering plating 300s, pure titanium is sunk
Product forms microthin coating in having of preparing of above-mentioned steps (1) on micro-/framework for receiving yardstick topological structure, and then obtains pure titanium
Pattern surface.Because microthin coating will not change the pattern of silicon frame, therefore the pattern on pure titanium pattern surface can refer to
The pattern of corresponding silicon frame shown in Fig. 1.
B, prepare titanium dioxide pattern surface：By the sample on the pure titanium pattern surface of above-mentioned preparation at 700 DEG C
Lower heat treatment 1h, makes pure titanium microthin coating be oxidized into titanium dioxide microthin coating, and then obtain titanium dioxide pattern table
Face.Because microthin coating will not change the pattern of silicon frame, therefore the pattern on titanium dioxide pattern surface can refer to shown in Fig. 1
Corresponding silicon frame pattern.
It should be appreciated that embodiment and example discussed herein simply to illustrate that, to those skilled in the art
For, it can be improved or be converted, and all these modifications and variations should all belong to the protection of appended claims of the present invention
Scope.
Claims (4)
1. a kind of pattern surface preparation method with anti-microbial property, it is characterised in that comprise the following steps：
Step (1)：Prepared in silicon material substrate with it is micro-/receive the framework of yardstick topological structure；
Step (2)：Pattern surface is prepared, including：Prepare pure titanium pattern surface or prepare titanium dioxide pattern
Surface；
Micro-/yardstick of receiving refers to the range scale from ten microns to ten nanometers in the step (1)；
It is micro- in the step (1)/to receive yardstick topological structure, including：It is micro-/to receive columnar arrays, array of protrusions, the pit array of yardstick
Or groove array.
2. according to the method described in claim 1, it is characterised in that prepare pure titanium pattern surface in the step (2)
To use magnetron sputtering method, by pure titanium be deposited in the step (1) have it is micro-/receive yardstick topological structure framework on formed
Pure titanium microthin coating.
3. according to the method described in claim 1, it is characterised in that prepare titanium dioxide pattern in the step (2)
Surface is first to deposit pure titanium microthin coating on micro-/framework for receiving yardstick topological structure, and dioxy is turned into by oxidation processes
Change titanium microthin coating.
4. according to the method described in claim 1, it is characterised in that prepared in the step (1) in silicon material substrate it is micro-/
The framework of yardstick topological structure received is to use photoetching process, and its technique includes following 14 steps：Photomask design, thermal oxidation method
Grow silica coating, one layer of HMDS of deposition, coating photoresist, prebake conditions, ultraviolet exposure imaging, exposure
Toast, develop afterwards, eventually it is roasting, remove residual photoresist, etching silicon dioxide layer, etching silicon base, remove photoresist layer and removal
Silicon dioxide layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710284286.4A CN107140599A (en) | 2017-04-26 | 2017-04-26 | A kind of pattern surface preparation method with anti-microbial property |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710284286.4A CN107140599A (en) | 2017-04-26 | 2017-04-26 | A kind of pattern surface preparation method with anti-microbial property |
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| Publication Number | Publication Date |
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| CN107140599A true CN107140599A (en) | 2017-09-08 |
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| CN201710284286.4A Pending CN107140599A (en) | 2017-04-26 | 2017-04-26 | A kind of pattern surface preparation method with anti-microbial property |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113004448A (en) * | 2021-03-04 | 2021-06-22 | 佛山科学技术学院 | Preparation method of antibacterial and bactericidal functional surface |
| TWI800027B (en) * | 2020-10-12 | 2023-04-21 | 南韓商Ｕｔｉ有限公司 | Method of manufacturing antibacterial cover window, and antibacterial cover window manufactured thereby |
Citations (3)
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|---|---|---|---|---|
| US20100303722A1 (en) * | 2006-06-23 | 2010-12-02 | Sungho Jin | Articles comprising large-surface-area bio-compatible materials and methods for making and using them |
| CN102732882A (en) * | 2012-07-13 | 2012-10-17 | 东南大学 | Artificial joint with micro-nano graded topological surface structure and preparation method of artificial joint |
| US20150290358A1 (en) * | 2010-07-06 | 2015-10-15 | The Regents Of The University Of California | Inorganically surface-modified polymers and methods for making and using them |
-
2017
- 2017-04-26 CN CN201710284286.4A patent/CN107140599A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100303722A1 (en) * | 2006-06-23 | 2010-12-02 | Sungho Jin | Articles comprising large-surface-area bio-compatible materials and methods for making and using them |
| US20150290358A1 (en) * | 2010-07-06 | 2015-10-15 | The Regents Of The University Of California | Inorganically surface-modified polymers and methods for making and using them |
| CN102732882A (en) * | 2012-07-13 | 2012-10-17 | 东南大学 | Artificial joint with micro-nano graded topological surface structure and preparation method of artificial joint |
Non-Patent Citations (1)
| Title |
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| YONGHUI DING, ET AL.: "Effects of microtopographic patterns on platelet adhesion and activation on titanium oxide surfaces", 《JOURNAL OF BIOMEDICAL MATERIALS RESEARCH PART A》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI800027B (en) * | 2020-10-12 | 2023-04-21 | 南韓商Ｕｔｉ有限公司 | Method of manufacturing antibacterial cover window, and antibacterial cover window manufactured thereby |
| CN113004448A (en) * | 2021-03-04 | 2021-06-22 | 佛山科学技术学院 | Preparation method of antibacterial and bactericidal functional surface |
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Application publication date: 20170908 |