CN107475686A - A kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane - Google Patents
A kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane Download PDFInfo
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- CN107475686A CN107475686A CN201710520551.4A CN201710520551A CN107475686A CN 107475686 A CN107475686 A CN 107475686A CN 201710520551 A CN201710520551 A CN 201710520551A CN 107475686 A CN107475686 A CN 107475686A
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/405—Oxides of refractory metals or yttrium
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- 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
- A61L27/02—Inorganic materials
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
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- 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
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
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- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/02—Methods for coating medical devices
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Abstract
A kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane, comprises the following steps, S1, using magnesium metal disk, by the use of sand paper, as substrate, then by substrate, 25~45min of ultrasound, naturally dry are standby in ethanol, acetone successively for surface polishing step by step；S2, step S1 is dried after substrate carry out ald, i.e., substrate surface zirconia ceramics coated film prepare complete.Its advantage is：Prepare the controllable nanometer zirconium oxide ceramic film of thickness in magnesium surface using atom deposition method so that the deposition compact of magnesium surface and uniformly；Furthermore the good biocompatibility of the material prepared using the method, that is, reduce its repulsion in human body, while have corrosion resistance；Preparation method is simple and easy, equipment investment is few, and consumption resource is few, safe.
Description
Technical field
It is specifically a kind of to be based on atomic layer deposition the present invention relates to nano material and the applied technical field of ceramic membrane
The preparation method of product zirconium oxide corrosion resistance ceramic membrane.
Background technology
With population increase, aging population getting worse, the injury such as traffic accident and athletic injury is taken place frequently, and sclerotin is dredged
Pine, Cranial defect and fracture often have generation.Be advantageous to the bio-medical material such as metal material, ceramic material of bone tissue reparation and have
The demand of machine/inorganic material is increasing.Wherein, metal material includes titanium-base alloy, stainless steel and cobalt-base alloys etc., due to
There is good toughness, higher intensity and chemical stability, be widely used in hard tissue repair and replace implant
Etc..
However, above-mentioned metal material is also having the drawbacks of certain in clinical practice, for example, because these metal materials are in people
Highly stable in body, after injured bone tissue returns to one's perfect health, these materials can not voluntarily degrade in vivo, so as to need secondary hand
Art takes out it from internal, had so both added the pain of patient or had increased the financial burden of patient.Magnesium-base metal is due to it
Excellent mechanical property, its tension and compression strength approach with people's bone, and it can degrade in human body, in recent years, by more
Carry out the concern of more researchers.But magnesium metal is more active, degradation speed in vivo is too fast, causes the bone tissue of injury
Not repair also, magnesium metal just loses intrinsic mechanical property, can not play a part of fixed and protect, and in degradation process
In, caused hydrogen and-OH can influence the growth of surrounding tissue cells, not reach certain clinical effectiveness.
The content of the invention
One of the object of the invention is a kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane, is used
To prepare the nano ceramic film with good corrosion energy.The second object of the present invention is to use technique for atomic layer deposition
Preparing zirconia ceramics coating makes it have good biocompatibility simultaneously.The third object of the present invention is to prepare thickness can
The nano coating of control is so as to controlling the corrosion rate of material.
One aspect of the present invention protects a kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane, bag
Include following steps：
S1, using magnesium metal disk, by the use of sand paper, surface polishing surpasses in ethanol, acetone successively as substrate, then by substrate step by step
25~45min of sound, naturally dry are standby；
S2, step S1 is dried after substrate carry out ald：Zirconium source is specially taken to be heated to 130-160 DEG C, so
Afterwards by the use of 30-40 DEG C of deionized water as O sources, depositing temperature is 200-250 DEG C, 100-400 circulation of progress, i.e. substrate surface
Prepared by zirconia ceramics coated film completes.
Preferably, in step S2, one cycle cleans 15-20s by four (dimethylamino) zirconium pulse 20-30ms, High Purity Nitrogen,
Deionized water pulse 100-150ms, High Purity Nitrogen cleaning 15-20s compositions；
In step S2, the zirconium source temperature is preferably to be heated to 150 DEG C；
The deionized water temperature is preferably to be heated to 35 DEG C；
The depositing temperature is preferably 250 DEG C；
The cycle-index is preferably 400；
The pulse of one cycle four (dimethylamino) zirconium be preferably 30ms, circulate deionized water burst length it is preferred
For 150ms；
The scavenging period of the High Purity Nitrogen is preferably 30s；
The material of surface deposited oxide zircon ceramic film prepared by second aspect of the present invention protection first aspect methods described.
Application of the material on the bio-medical material of bone tissue reparation described in third aspect present invention protection second aspect.
A kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane, its advantage are：
The controllable nanometer zirconium oxide ceramic film of thickness is prepared in magnesium surface so that magnesium surface sinks using atom deposition method
Product is fine and close and uniform；Furthermore the good biocompatibility of the material prepared using the method, that is, reduce its repulsion in human body,
There is corrosion resistance simultaneously；Preparation method is simple and easy, equipment investment is few, and consumption resource is few, safe.
Brief description of the drawings
There is the surface of the magnesium alloy disk of the anticorrosive ceramic coating of zirconia nanopowder in the respectively embodiment 1,2 of Fig. 1,2
Shape appearance figure；
Fig. 3 is in the case of other conditions are constant in embodiment 1, and the deposition number of turns is obtained when being respectively 100,200,300,400
The electrochemical impedance figure of product；
Fig. 4 is for the magnesium alloy in embodiment 1 with the anticorrosive ceramic coating of zirconia nanopowder with pure magnesium sheet to cytoactive
The comparison diagram of influence.
Fig. 5, Fig. 6, Fig. 7 are respectively the cell morphology figure on pure magnesium sheet surface after cell culture 24 hours；
Fig. 8, Fig. 9, Figure 10 are respectively the cell of gained sample sample surfaces after cell culture 24 hours in embodiment 1
Shape appearance figure；
Figure 11 is the cell fluorescence figure on the pure magnesium sheet surface after cell culture 24 hours；
Figure 12 is the cell fluorescence figure of gained sample sample surfaces after cell culture 24 hours in embodiment 1；
Embodiment
To be best understood from the present invention, the present invention is done further described in detail with reference to the accompanying drawings and examples, still
The scope of protection of present invention is not limited to the scope of embodiment expression.
Embodiment one
S1, by magnesium metal disk with being beaten respectively with the sand paper that specification is 600#, 800#, 1200#, 2400# on polishing machine
Smooth mirror surface is milled to, as substrate, then by the substrate successively ultrasonic 30min in ethanol, acetone, to clean magnesium sheet surface
Debris, makes that its surface is clean, and then naturally dry is standby；
S2, step S1 is dried after substrate carry out ald：Zirconium source is specially taken to be heated to 150 DEG C, Ran Houyong
For 35 DEG C of deionized waters as O sources, depositing temperature is 250 DEG C, carries out 400 circulations, and one cycle is by four (dimethylamino) zirconiums
Pulse 30ms, High Purity Nitrogen clean 20s, deionized water pulse 150ms, High Purity Nitrogen cleaning 20s compositions, the i.e. oxidation in substrate surface
Prepared by zircon ceramic coated film completes.
In the case of above-mentioned other conditions are constant, only change the deposition number of turns, making the circulation number of turns into 100,200,300 respectively obtains
Product, and prepared product is carried out using impedance of the electrochemical workstation to sample when the above-mentioned deposition number of turns is 400
Test；
Its test condition is that interference voltage is 5mV, range of scanned frequencies 10-2Hz-105Hz, acquired results are used
The softwares of Zsimpwin 3.21 are fitted：Magnesium sheet with the modification of zirconia nanopowder ceramic coating is compared to pure magnesium sheet, electrochemistry
Impedance value greatly increases, and illustrates the magnesium sheet after modification, and corrosion resistance greatly increases, while the not synsedimentary number of turns, electrochemistry resistance
Anti- value is different, illustrates that its Corrosion Protection is different (as shown in Figure 3).
Embodiment two
It is with the difference of embodiment one：
In step S2, specially take zirconium source to be heated to 150 DEG C, be then by the use of 35 DEG C of deionized waters as O sources, depositing temperature
250 DEG C, 100 circulations are carried out, and one cycle is by four (dimethylamino) zirconium pulse 30ms, High Purity Nitrogen cleaning 20s, deionized water
Pulse 150ms, High Purity Nitrogen cleaning 20s compositions, i.e., prepare completion in the zirconia ceramics coated film of substrate surface.
Embodiment three
It is with the difference of embodiment one：
In step S2, specially take zirconium source to be heated to 150 DEG C, be then by the use of 35 DEG C of deionized waters as O sources, depositing temperature
200 DEG C, 200 circulations are carried out, and one cycle is by four (dimethylamino) zirconium pulse 30ms, High Purity Nitrogen cleaning 20s, deionized water
Pulse 150ms, High Purity Nitrogen cleaning 20s compositions, i.e., prepare completion in the zirconia ceramics coated film of substrate surface.
Example IV
It is with the difference of embodiment one：
In step S2,
Specially take zirconium source to be heated to 150 DEG C, be then 200 DEG C by the use of 35 DEG C of deionized waters as O sources, depositing temperature, enter
300 circulations of row, and one cycle is by four (dimethylamino) zirconium pulse 20ms, High Purity Nitrogen cleaning 20s, deionized water pulse
100ms, High Purity Nitrogen cleaning 20s compositions, i.e., prepare completion in the zirconia ceramics coated film of substrate surface.
The surface topography of the sample in embodiment one, two is detected by SEM, by Fig. 1,2 can be with
Draw, the zirconia coating of ald is molecular by nanoparticle, and with once adding for the deposition number of turns, nano-particle can become
Obtain more even compact.
External biological experiment (control is wherein used as using pure magnesium sheet) is carried out to sample prepared by embodiment 1, is specially：
Cytoactive tests concrete operations：1ml mouse bone-forming cells, i.e. MC3CT3 are taken, to pure magnesium and the gained sample of embodiment 1
Product are cultivated, incubation time 1,3,7 days, and the cell liquid after processing is detected with ELIASA to it, and absorbing wavelength is
490nm.As seen from Figure 4, relative to pure magnesium sheet, the cytoactive for the magnesium sheet modified by the zirconium oxide of ald is obvious
Increase；
Cellscan concrete operations：1ml mouse bone-forming cells are taken, culture 1 is carried out to pure magnesium and the gained sample of embodiment 1
My god, after processing, cell morphology is observed with electron microscope.From Fig. 5, Fig. 6, Fig. 7, pure magnesium metal due to corrosion and
Crackle be present, make cell rupture；From Fig. 8, Fig. 9, Figure 10, on the sample of embodiment 1, cell is sprawled well, and intact.
Thus illustrate that the magnesium metal after zirconia ceramics modification is more suitable for cell growth, there is good biocompatibility.
The concrete operations of cell fluorescence figure：1ml mouse bone-forming cells are taken, pure magnesium and the gained sample of embodiment 1 are trained
Support 1 day, after cell dyeing, it is observed with fluorescence microscope.Comparison diagram 11, Figure 12 can be seen that pure magnesium sheet surface
Cell roll up, without drawout, and cell quantity is less (such as Figure 11), and zirconia ceramics modification after magnesium based metal
Cell growth is good, sprawls completely, and feeler is obvious, and cell quantity is more compared to the magnesium sheet of no modification (such as Figure 12).
Illustrate that the magnesium metal after zirconia ceramics modification is more suitable for cell growth, there is good biocompatibility.
Therefore cell growth is better on the gained sample of embodiment 1, then draws, technique for atomic layer deposition prepares oxidation
Zircon ceramic coating has good biocompatibility, when the bio-medical material as bone tissue reparation, inserts in human body,
Before wound healing, magnesium metal can keep original mechanical property.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (4)
1. a kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane, it is characterised in that：Including as follows
Step
S1, using magnesium metal disk, by the use of sand paper, surface polishing is as substrate step by step, then by substrate successively ultrasonic 25 in ethanol, acetone
~45min, naturally dry are standby；
S2, step S1 is dried after substrate carry out ald：Zirconium source is specially taken to be heated to 130-160 DEG C, Ran Houyong
For 30-40 DEG C of deionized water as O sources, depositing temperature is 200-250 DEG C, carries out 100-400 circulation, the i.e. oxidation of substrate surface
Prepared by zircon ceramic coated film completes.
2. method according to claim 1, it is characterised in that：In step S2, one cycle is by four (dimethylamino) zirconium pulses
20-30ms, High Purity Nitrogen cleaning 15-20s, deionized water pulse 100-150ms, High Purity Nitrogen cleaning 15-20s are formed.
3. the material of surface deposited oxide zircon ceramic film prepared by claim 1~2 methods described.
4. application of the material described in claim 3 on the bio-medical material of bone tissue reparation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113636868A (en) * | 2021-08-19 | 2021-11-12 | 北京大学口腔医学院 | Surface coating method of zirconia ceramic implant material and application thereof |
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| US20160060758A1 (en) * | 2014-08-29 | 2016-03-03 | University Of Maryland, College Park | Protective coated object and method of coating an object |
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| CN101003889A (en) * | 2007-02-05 | 2007-07-25 | 陈鸿文 | Surface process technique for artificial joint, bone lamella, and bone nail coated by Nano diamond |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113636868A (en) * | 2021-08-19 | 2021-11-12 | 北京大学口腔医学院 | Surface coating method of zirconia ceramic implant material and application thereof |
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Application publication date: 20171215 |