CN101775634A - Method for preparing oxide nanotube array on surface of nickel-titanium shape memory alloy - Google Patents
Method for preparing oxide nanotube array on surface of nickel-titanium shape memory alloy Download PDFInfo
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- CN101775634A CN101775634A CN 201010127204 CN201010127204A CN101775634A CN 101775634 A CN101775634 A CN 101775634A CN 201010127204 CN201010127204 CN 201010127204 CN 201010127204 A CN201010127204 A CN 201010127204A CN 101775634 A CN101775634 A CN 101775634A
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- anodic oxidation
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Abstract
The invention relates to a method for preparing an oxide nanotube array on the surface of a nickel-titanium shape memory alloy, which belongs to the technical field of nanometer materials. The method comprises the following steps: firstly, using the nickel-titanium shape memory alloy as an anodic oxidation substrate to prepare an anodic oxidation medium, wherein the anodic oxidation medium comprises the components of ethylene glycol, ammonium sulfate, ammonium fluoride and glycerol or the components of ammonium fluoride and glycerol; and secondly, regulating the anodic oxidation voltage to 10 to 50V and performing oxidization to obtain the oxide nanotube array on the surface of the nickel-titanium shape memory alloy. The method can prepare oxide nanotube array on the surface of the nickel-titanium shape memory alloy; the prepared Ni-Ti-O oxide nanotubes have high orientation; the tube diameter of the oxide nanotubes can be controlled by regulating an anodic oxidation voltage; the length of the nanotubes can be controlled by regulating the anodic oxidation time; and the oxide nanotube array can significantly improve the corrosion resistance of the surface of the nickel-titanium shape memory alloy.
Description
Technical field
The present invention relates to a kind of preparation method of technical field of nano material, specifically is the preparation method of the oxide nanotube array on a kind of niti-shaped memorial alloy surface.
Background technology
NiTi alloy with shape memory effect and super elastic characteristics is a kind of important bio-medical material, has in fields such as orthopaedics and cardiovascular treatments widely to use.Because the solidity to corrosion and the biocompatibility of NiTi alloy are not ideal, so after in the NiTi alloy product implant into body, discharge toxic element Ni easily, produce potential safety hazard.For this reason, need carry out the performances such as solidity to corrosion, wear resistance and biocompatibility that surface modification improves implant surface to the NiTi alloy.Common surface modifying method comprises thermooxidizing, differential arc oxidation, Laser Surface Treatment, chemical passivation and anodic oxidation etc.
Find through literature search prior art, Cheng, F.T. wait to have delivered and be entitled as " Nature of oxide layer formed on NiTi by anodicoxidation in methanol " (zone of oxidation essence of NiTi alloy anodic oxidation preparation in methyl alcohol) literary composition 1516～1520 pages of " Materials letters " (material wall bulletin) 2005 the 59th phases, studied the heterogeneous microstructure of anodic oxide coating in the literary composition, but the technical scheme that the document discloses has only realized the anodic oxidation preparation of dense oxide coating or the irregular zone of oxidation of porous, can not the especially anodic oxidation preparation of oxide nanotube array of implementation rule porous oxide coatings.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the preparation method of the oxide nanotube array on a kind of niti-shaped memorial alloy surface is provided.Method of the present invention can go out oxide nanotube array in the niti-shaped memorial alloy surface preparation, the Ni-Ti-O oxide nano of preparation has height-oriented property, the caliber of oxide nano can be controlled by the size of regulating anodic oxidation voltage, and nanotube length can be controlled by adjusting anodizing time.
The present invention relates to the preparation method of the oxide nanotube array on a kind of niti-shaped memorial alloy surface, comprise the steps:
Step 1, getting niti-shaped memorial alloy is the anodic oxidation base material, preparation anodic oxidation medium;
The component of described anodic oxidation medium is ethylene glycol, ammonium sulfate, Neutral ammonium fluoride and glycerol; Perhaps be Neutral ammonium fluoride, glycerol;
Step 2, the scope of adjusting anodic oxidation voltage is 10V～50V, oxidation can obtain oxide nanotube array on the niti-shaped memorial alloy surface.
In the step 1, the component and the content of described anodic oxidation medium are specially: volume fraction is 1.0～10% ethylene glycol, the ammonium sulfate of 0～1.0M, and the Neutral ammonium fluoride of 0.05～1.0M, surplus is a glycerol.
In the step 1, the component and the content of described anodic oxidation medium are specially: the Neutral ammonium fluoride of 0.1～2wt%, surplus are glycerol.
Compared with prior art, the present invention has following beneficial effect: method of the present invention can go out oxide nanotube array in the niti-shaped memorial alloy surface preparation, the Ni-Ti-O oxide nano of preparation has height-oriented property, the caliber of oxide nano can be controlled by the size of regulating anodic oxidation voltage, and nanotube length can be controlled by adjusting anodizing time.The Ni-Ti-O oxide nanotube array can obviously improve the niti-shaped memorial alloy surface solidity to corrosion, have performances such as excellent biological compatibility and medicament slow release.
Embodiment
Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment 1
Step 1 is got niti-shaped memorial alloy sheet material, polishes, polishes with abrasive paper for metallograph, with alcohol wash and dry, obtains the anodic oxidation base material; Preparation anodic oxidation medium, the component of described medium is: 5% (volume fraction) ethylene glycol, (NH of 0.15M
4)
2SO
4, 0.2M NH
4F, surplus is a glycerol;
Step 2, the adjustment anodic oxidation voltage is 20V, oxidization time 1.5 hours, taking out and obtain the nanotube diameter from anodizing tank is 30～40nm, nanotube length is the Ni-Ti-O nano-tube array of 200nm.
Embodiment 2
Step 1 is got niti-shaped memorial alloy sheet material, polishes, polishes with abrasive paper for metallograph, with alcohol wash and dry, obtains the anodic oxidation base material; Preparation anodic oxidation medium, the component of described medium is: 1% (volume fraction) ethylene glycol, (NH of 0M
4)
2SO
4, 0.05M NH
4F, surplus is a glycerol;
Step 2, the adjustment anodic oxidation voltage is 10V, oxidization time 1.5 hours takes out and obtains the Ni-Ti-O nano-tube array of nanotube diameter less than 30nm from anodizing tank.
Embodiment 3
Step 1 is got niti-shaped memorial alloy sheet material, polishes, polishes with abrasive paper for metallograph, with alcohol wash and dry, obtains the anodic oxidation base material; Preparation anodic oxidation medium, the component of described medium is: 10% (volume fraction) ethylene glycol, (NH of 1M
4)
2SO
4, 1M NH
4F, surplus is a glycerol;
Step 2, the adjustment anodic oxidation voltage is 50V, oxidization time 1.5 hours takes out and obtains the Ni-Ti-O nano-tube array of nanotube diameter less than 100nm from anodizing tank.
Embodiment 4
Step 1 is got niti-shaped memorial alloy sheet material, polishes, polishes with abrasive paper for metallograph, with alcohol wash and dry, obtains the anodic oxidation base material; Preparation anodic oxidation medium, the component of described medium is: the NH of 0.5wt%
4F, surplus is a glycerol;
Step 2, the adjustment anodic oxidation voltage is 20V, oxidization time 1.5 hours takes out and obtains the Ni-Ti-O nano-tube array that the nanotube diameter is about 20nm from anodizing tank.
Embodiment 5
Step 1 is got niti-shaped memorial alloy sheet material, polishes, polishes with abrasive paper for metallograph, with alcohol wash and dry, obtains the anodic oxidation base material; Preparation anodic oxidation medium, the component of described medium is: the NH of 0.1wt%
4F, surplus is a glycerol;
Step 2, the adjustment anodic oxidation voltage is 50V, oxidization time 1.5 hours takes out and obtains the Ni-Ti-O nano-tube array of nanotube diameter less than 100nm from anodizing tank.
Embodiment 6
Step 1 is got niti-shaped memorial alloy sheet material, polishes, polishes with abrasive paper for metallograph, with alcohol wash and dry, obtains the anodic oxidation base material; Step 2, preparation anodic oxidation medium, the component of described medium is: the NH of 2wt%
4F, surplus is a glycerol;
Step 2, the adjustment anodic oxidation voltage is 10V, oxidization time 1.5 hours takes out and obtains the Ni-Ti-O nano-tube array of nanotube diameter less than 20nm from anodizing tank.
Claims (3)
1. the preparation method of the oxide nanotube array on a niti-shaped memorial alloy surface is characterized in that, comprises the steps:
Step 1, getting niti-shaped memorial alloy is the anodic oxidation base material, preparation anodic oxidation medium;
The component of described anodic oxidation medium is ethylene glycol, ammonium sulfate, Neutral ammonium fluoride and glycerol; Perhaps be Neutral ammonium fluoride, glycerol;
Step 2, the scope of adjusting anodic oxidation voltage is 10V～50V, oxidation can obtain oxide nanotube array on the niti-shaped memorial alloy surface.
2. the preparation method of the oxide nanotube array on niti-shaped memorial alloy according to claim 1 surface, it is characterized in that, in the step 1, the component and the content of described anodic oxidation medium are specially: volume fraction is 1.0～10% ethylene glycol, the ammonium sulfate of 0～1.0M, 0.05 the Neutral ammonium fluoride of～1.0M, surplus are glycerol.
3. the preparation method of the oxide nanotube array on niti-shaped memorial alloy according to claim 1 surface, it is characterized in that, in the step 1, the component and the weight percent of described anodic oxidation medium are specially: the Neutral ammonium fluoride of 0.1～2wt%, surplus are glycerol.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013004560A1 (en) | 2011-07-06 | 2013-01-10 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Method for producing p-type semiconducting tio2 nanotubes |
| CN104404602A (en) * | 2014-11-18 | 2015-03-11 | 上海交通大学 | Preparation method of NiTi shape memory alloy with porous surface |
| CN104532321A (en) * | 2014-12-19 | 2015-04-22 | 浙江工业大学 | Method for oxidizing anode of titanium-aluminum alloy in fluoride-added ethylene glycol solution |
| CN106456310A (en) * | 2014-06-24 | 2017-02-22 | 加利福尼亚大学董事会 | Nickel titanium oxide coated articles |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884630A (en) * | 2006-06-01 | 2006-12-27 | 厦门大学 | High length-diameter ratio titania nanometer tube array preparation method |
| CN101514471A (en) * | 2009-02-27 | 2009-08-26 | 哈尔滨工业大学 | Method for preparing TiO2 nanotube array film |
-
2010
- 2010-03-19 CN CN 201010127204 patent/CN101775634A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884630A (en) * | 2006-06-01 | 2006-12-27 | 厦门大学 | High length-diameter ratio titania nanometer tube array preparation method |
| CN101514471A (en) * | 2009-02-27 | 2009-08-26 | 哈尔滨工业大学 | Method for preparing TiO2 nanotube array film |
Non-Patent Citations (1)
| Title |
|---|
| 《physical status solidi》 20060606 Jan M. Macak Smooth anodic TiO2 nanotubes:annealing and structure 67-69 1-3 第203卷, 第10期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013004560A1 (en) | 2011-07-06 | 2013-01-10 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Method for producing p-type semiconducting tio2 nanotubes |
| DE102011106685A1 (en) | 2011-07-06 | 2013-01-10 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Process for producing P-semiconducting TiO 2 nanotubes |
| CN106456310A (en) * | 2014-06-24 | 2017-02-22 | 加利福尼亚大学董事会 | Nickel titanium oxide coated articles |
| CN104404602A (en) * | 2014-11-18 | 2015-03-11 | 上海交通大学 | Preparation method of NiTi shape memory alloy with porous surface |
| CN104404602B (en) * | 2014-11-18 | 2017-01-25 | 上海交通大学 | Preparation method of NiTi shape memory alloy with porous surface |
| CN104532321A (en) * | 2014-12-19 | 2015-04-22 | 浙江工业大学 | Method for oxidizing anode of titanium-aluminum alloy in fluoride-added ethylene glycol solution |
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