CN102345103A - Preparation method of titanium modified layer on surface of magnesium and lithium alloy - Google Patents
Preparation method of titanium modified layer on surface of magnesium and lithium alloy Download PDFInfo
- Publication number
- CN102345103A CN102345103A CN2011102864974A CN201110286497A CN102345103A CN 102345103 A CN102345103 A CN 102345103A CN 2011102864974 A CN2011102864974 A CN 2011102864974A CN 201110286497 A CN201110286497 A CN 201110286497A CN 102345103 A CN102345103 A CN 102345103A
- Authority
- CN
- China
- Prior art keywords
- lithium alloy
- modified layer
- preparation
- magnesium lithium
- magnesium
- Prior art date
- 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
Links
Images
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a preparation method of a titanium modified layer on the surface of a magnesium and lithium alloy, and relates to a preparation method of an alloy titanium modified layer. The invention aims to solve the technical problem of poor corrosion resistance of the traditional magnesium and lithium alloy. The preparation method comprises the steps of: firstly, grinding the surface of the magnesium and lithium alloy by waterproof abrasive paper, then polishing, ultrasonically cleaning in acetone (analytically pure), ultrasonically cleaning in absolute ethyl alcohol, and drying; and secondly, placing a sample table in a vacuum chamber and connecting to the high-voltage pulse output end of a high-voltage pulse power supply, using a commercially pure titanium target as a magnetic control sputtering target material and connecting to the high-power pulse output end of a magnetic control sputtering power supply, then vacuumizing in the vacuum chamber, introducing high-purity argon when the vacuum degree is 4.0*10<-3>Pa, starting the high-voltage pulse power supply, then starting the magnetic control sputtering power supply, building in luminance and pre-ionizing through direct current, regulating working parameters, and carrying out ion injection and deposition, thereby obtaining the titanium modified layer on the surface of the magnesium and lithium alloy. According to the method disclosed by the invention, the titanium layer is formed on the surface of the magnesium alloy, and the surface hardness of the magnesium alloy is improved by about 40%.
Description
Technical field
The present invention relates to the preparation method of titanium alloy modified layer; Be specifically related to the preparation method of magnesium lithium alloy surface titanium modified layer.
Background technology
Magnesium lithium alloy is the lightest structural metallic materials, not only has high specific stiffness and good machinability, also has good magnetic shielding, performance such as shockproof.In communication electronic industry, military project and aerospace field, obtain increasingly extensive application.The corrosion stability difference is the principal element that the restriction magnesium lithium alloy is used.The chemical property of magnesium lithium alloy is more active than other magnesium alloy, and this is because Li itself is very active, simultaneously because Li has increased the chemically reactive of Mg in Mg.The Sensitivity of Stress Corrosion of magnesium lithium alloy in moist atmosphere is very big, and the normal temperature held also heavy corrosion can take place in atmosphere.Therefore effectively preventive means is the prerequisite that enlarges its application.Some process for protecting surface of Mg-Li alloy have in recent years been enumerated below.
Sharma has studied the chromic salt chemistry conversion film of magnesium lithium alloy, obtains the chromate film that thickness is 8～11 μ m.Han Yuchang etc. carry out Study on Electroless Nickel to the Mg-13Li-5Zn alloy; The result shows that the method that adopts chemical nickel plating can obtain even, the fine and close nickel-phosphorus alloy coating of one deck at the Mg-13Li-5Zn alloy surface, and this coating provides protection to a certain degree can for the Mg-13Li-5Zn alloy.Employing chemical gaseous phase depositing process (CVD) such as Yamauchi have prepared diamond-like coating (DLC) on the Mg-14Li alloy, this coating has been slowed down the lithium that takes off of Mg-14Li alloy.
Though above-mentioned these methods have improved the corrosion resisting property of magnesium lithium alloy to a certain extent; But these methods mostly relate to liquid; And the standard potential of Li is-3.045V; Electronegativity is also bigger than Mg; Therefore magnesium lithium alloy corrosion speed in electrolytic solution is exceedingly fast; Though can form coating on the magnesium lithium alloy surface through electrochemical method, also be accompanied by the quick corrosion of matrix alloy simultaneously.Therefore, above-mentioned these methods are ripe not enough.
Summary of the invention
The present invention will solve the technical problem that there is poor corrosion resistance in existing magnesium lithium alloy; And the preparation method of magnesium lithium alloy surface titanium modified layer is provided.
The preparation method of magnesium lithium alloy surface titanium modified layer is undertaken by following step: one, use 240 successively
#, 600
#, 1000
#, 1500
#With 1000
#Liquid honing magnesium lithium alloy surface, analytical pure acetone ultrasonic cleaning is put in polishing more then, puts into the dehydrated alcohol ultrasonic cleaning then, dries up; Two, will place the high-voltage pulse output terminal that is attempted by high-voltage pulse power source on the sample table in the vacuum chamber through the magnesium lithium alloy that step 1 is handled; With purity is that the industrially pure titanium target of 99.9% (quality) is the high power pulse output terminal that magnetic control spattering target is attempted by the magnetron sputtering power supply; Vacuum chamber vacuumizes then, treats that vacuum tightness is 4.0 * 10
-3Feed high-purity argon gas during Pa, open high-voltage pulse power source, open the magnetron sputtering power supply then, through the preparatory ionization of direct current build-up of luminance, the re-adjustment working parameter carries out ion implantation and deposition, i.e. magnesium lithium alloy surface titanium modified layer; Wherein, the described working parameter of step 2: the ion implantation time is 15～35min, and galvanic current is 0.3～0.5A; Pulse current frequency is 50～52Hz, and the pulsed current pulsewidth is 200～210 μ s, and the pulsed current average is 0.03A; Air pressure is 0.5Pa, and bias voltage is 350～660V.
Through energy spectrum analysis and micro-hardness testing, the inventive method forms titanium layer at Mg alloy surface, and its surface hardness has improved about 40%.
Description of drawings
Fig. 1 is the ability spectrogram of the ion implantation titanium modified layer of test one magnesium lithium alloy; Fig. 2 is the ability spectrogram of the ion implantation titanium modified layer of test two magnesium lithium alloys.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of magnesium lithium alloy surface titanium modified layer is undertaken by following step in this embodiment: one, use 240 successively
#, 600
#, 1000
#, 1500
#With 1000
#Liquid honing magnesium lithium alloy surface, acetone analytical pure ultrasonic cleaning is put in polishing more then, puts into the dehydrated alcohol ultrasonic cleaning then, dries up; Two, will place the high-voltage pulse output terminal that is attempted by high-voltage pulse power source on the sample table in the vacuum chamber through the magnesium lithium alloy that step 1 is handled; With purity is that the industrially pure titanium target of 99.9% (quality) is the high power pulse output terminal that magnetic control spattering target is attempted by the magnetron sputtering power supply; Vacuum chamber vacuumizes then, treats that vacuum tightness is 4.0 * 10
-3Feed high-purity argon gas during Pa, open high-voltage pulse power source, open the magnetron sputtering power supply then, through the preparatory ionization of direct current build-up of luminance, the re-adjustment working parameter carries out ion implantation and deposition, i.e. magnesium lithium alloy surface titanium modified layer; Wherein, the described working parameter of step 2: the ion implantation time is 15～35min, and galvanic current is 0.3～0.5A; Pulse current frequency is 50～52Hz, and the pulsed current pulsewidth is 200～210 μ s, and the pulsed current average is 0.03A; Air pressure is 0.5Pa, and bias voltage is 350～660V.
Through energy spectrum analysis and micro-hardness testing, this embodiment method forms titanium layer at Mg alloy surface, and its surface hardness has improved about 40%.
Embodiment two: what this embodiment and embodiment one were different is: the time of the said ultrasonic cleaning of step 1 is that 10～30min, frequency of ultrasonic are 20kHz and hyperacoustic power 200w.Other step is identical with embodiment one with parameter.
Embodiment three: what this embodiment and embodiment two were different is: the time of the said ultrasonic cleaning of step 1 is 20min.Other step is identical with embodiment one or two with parameter.
Embodiment four: what this embodiment was different with one of embodiment one to three is: polish with the chromium trioxide lapping paste in the step 1.Other step is identical with one of embodiment one to three with parameter.
Embodiment five: what this embodiment was different with one of embodiment one to four is: the said ion implantation time of step 2 is 20～30min.Other step is identical with one of embodiment one to four with parameter.
Embodiment six: what this embodiment was different with one of embodiment one to four is: the said ion implantation time of step 2 is 25min.Other step is identical with one of embodiment one to four with parameter.
Embodiment seven: what this embodiment was different with one of embodiment one to six is: the said bias voltage of step 2 is 400～450V.Other step is identical with one of embodiment one to six with parameter.
Embodiment eight: what this embodiment was different with one of embodiment one to six is: the said bias voltage of step 2 is 650V.Other step is identical with one of embodiment one to six with parameter.
Adopt following verification experimental verification effect of the present invention:
Test one: the preparation method of magnesium lithium alloy surface titanium modified layer is undertaken by following step:
One, uses 240 successively
#, 600
#, 1000
#, 1500
#With 1000
#Liquid honing magnesium lithium alloy surface, acetone (analytical pure) ultrasonic cleaning 10min is put in polishing more then, and frequency 20kHz and power 200w put into dehydrated alcohol ultrasonic cleaning 10min then, and frequency 20kHz and power 200w use drier;
Two, will place the high-voltage pulse output terminal that is attempted by high-voltage pulse power source on the sample table in the vacuum chamber through the magnesium lithium alloy that step 1 is handled; With purity is that the industrially pure titanium target of 99.9% (quality) is the high power pulse output terminal that magnetic control spattering target is attempted by the magnetron sputtering power supply; Vacuum chamber vacuumizes then, treats that vacuum tightness is 4.0 * 10
-3Feed high-purity argon gas during Pa; (and the magnitude of voltage of regulating high-voltage pulse power source output pulse is 0.5～100kv to open high-voltage pulse power source; Pulse-repetition is 0～1000Hz; Pulsewidth is 0～50 μ s); Open the magnetron sputtering power supply then; Through the preparatory ionization of direct current build-up of luminance, the re-adjustment working parameter carries out ion implantation and deposition, i.e. magnesium lithium alloy surface titanium modified layer; Wherein, the described working parameter of step 2: time 15min, direct current 0.3A, pulse current frequency 50Hz, pulsed current pulsewidth 200 μ s, pulsed current average 0.03A, air pressure 0.5Pa, bias voltage 650V.
The ion implantation titanium modified layer of testing a magnesium lithium alloy is carried out energy spectrum analysis (seeing accompanying drawing 1), and the result shows that alloy surface forms titanium layer.Utilize micro Vickers to measure matrix of samples and microhardness of coating, the result shows that the average hardness through ion implantation and sedimentary sample has improved about 40%.
Test two: the preparation method of magnesium lithium alloy surface titanium modified layer is undertaken by following step:
Before the preparation titanium modified layer, sample is through 240
#, 600
#, 1000
#, 1500
#, 2000
#Waterproof abrasive paper is polished successively, polishes with the chromium trioxide lapping paste then.Matrix after handling is put into acetone (analytical pure) use ultrasonic cleaning 10min, frequency is 20kHz, and power is 200w, removes the spot on surface, puts into raw spirit ultrasonic cleaning 10min then, with blower sample is dried up and puts into the sample chamber.Rete prepare process in corresponding gas be argon gas (99.99%).Test use magnetic control spattering target is 99.9% industrially pure titanium target.
Pending workpiece is placed on the sample table in the vacuum chamber, and workpiece connects the high-voltage pulse output terminal of high-voltage pulse power source, and the magnetron sputtering target source on the vacuum chamber of being installed in connects the high power pulse output terminal of magnetron sputtering power supply.Vacuum chamber is vacuumized, treat that vacuum tightness is 4.0 * 10
-3During Pa, feed high-purity argon gas.The pulse synchronization matching set is controlled the magnetron sputtering power work according to the high pressure synchronous triggering signal of high-voltage pulse power source output.Open high-voltage pulse power source, and the magnitude of voltage of regulating high-voltage pulse power source output pulse is 0.5～100kv, pulse-repetition is 0～1000Hz, and pulsewidth is 0～50 μ s.Open the magnetron sputtering power supply; Earlier through the preparatory ionization of direct current build-up of luminance; Regulate required processing parameter; The magnitude of voltage of magnetron sputtering power supply output pulse is 300～2500V; Pulsewidth is 0～100 μ s; The phase differential of control high-voltage pulse power source output voltage and magnetron sputtering power supply output pulse is-1000～1000 μ s, carries out ion implantation and deposition.
Working parameter: time 35min, direct current 0.5A, pulse current frequency 52Hz, pulsed current pulsewidth 210 μ s, pulsed current average 0.03A, air pressure 0.5Pa, bias voltage 660V.
The ion implantation titanium modified layer of magnesium lithium alloy is carried out energy spectrum analysis (seeing accompanying drawing 2), and the result shows that alloy surface forms titanium layer.Utilize micro Vickers to measure matrix of samples and microhardness of coating, the result shows that the average hardness through ion implantation and sedimentary sample has improved about 42%.
Claims (8)
1. the preparation method of magnesium lithium alloy surface titanium modified layer is characterized in that the preparation method of magnesium lithium alloy surface titanium modified layer is undertaken by following step:
One, uses 240 successively
#, 600
#, 1000
#, 1500
#With 1000
#Liquid honing magnesium lithium alloy surface, analytical pure acetone ultrasonic cleaning is put in polishing more then, puts into the dehydrated alcohol ultrasonic cleaning then, dries up;
Two, will place the high-voltage pulse output terminal that is attempted by high-voltage pulse power source on the sample table in the vacuum chamber through the magnesium lithium alloy that step 1 is handled; With the industrially pure titanium target is the high power pulse output terminal that magnetic control spattering target is attempted by the magnetron sputtering power supply; Vacuum chamber vacuumizes then, treats that vacuum tightness is 4.0 * 10
-3Feed high-purity argon gas during Pa, open high-voltage pulse power source, open the magnetron sputtering power supply then, through the preparatory ionization of direct current build-up of luminance, the re-adjustment working parameter carries out ion implantation and deposition, i.e. magnesium lithium alloy surface titanium modified layer; Wherein, the described working parameter of step 2: the ion implantation time is 15～35min, and galvanic current is 0.3～0.5A; Pulse current frequency is 50～52Hz, and the pulsed current pulsewidth is 200～210 μ s, and the pulsed current average is 0.03A; Air pressure is 0.5Pa, and bias voltage is 350～660V.
2. according to the preparation method of the said magnesium lithium alloy of claim 1 surface titanium modified layer, the time that it is characterized in that the said ultrasonic cleaning of step 1 is that 10～30min, frequency of ultrasonic are 20kHz and hyperacoustic power 200w.
3. according to the preparation method of the said magnesium lithium alloy of claim 2 surface titanium modified layer, the time that it is characterized in that the said ultrasonic cleaning of step 1 is 20min.
4. according to the preparation method of claim 1,2 or 3 said magnesium lithium alloy surface titanium modified layer, it is characterized in that polishing with the chromium trioxide lapping paste in the step 1.
5. according to the preparation method of the said magnesium lithium alloy of claim 4 surface titanium modified layer, it is characterized in that the said ion implantation time of step 2 is 20～30min.
6. according to the preparation method of the said magnesium lithium alloy of claim 4 surface titanium modified layer, it is characterized in that the said ion implantation time of step 2 is 25min.
7. according to the preparation method of the said magnesium lithium alloy of claim 5 surface titanium modified layer, it is characterized in that the said bias voltage of step 2 is 400～450V.
8. according to the preparation method of the said magnesium lithium alloy of claim 5 surface titanium modified layer, it is characterized in that the said bias voltage of step 2 is 650V.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102864974A CN102345103A (en) | 2011-09-23 | 2011-09-23 | Preparation method of titanium modified layer on surface of magnesium and lithium alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102864974A CN102345103A (en) | 2011-09-23 | 2011-09-23 | Preparation method of titanium modified layer on surface of magnesium and lithium alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102345103A true CN102345103A (en) | 2012-02-08 |
Family
ID=45544168
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102864974A Pending CN102345103A (en) | 2011-09-23 | 2011-09-23 | Preparation method of titanium modified layer on surface of magnesium and lithium alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102345103A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526174A (en) * | 2013-09-27 | 2014-01-22 | 南京工程学院 | Surface modification method for delaying degradation rate of biomedical magnesium alloy |
| CN103924202A (en) * | 2014-04-03 | 2014-07-16 | 西南交通大学 | Metal support surface modification method |
| CN109440065A (en) * | 2018-11-09 | 2019-03-08 | 南昌大学 | A kind of preparation method of Mg alloy surface tungsten molybdenum nanoscale anticorrosion film |
| CN113811106A (en) * | 2020-06-11 | 2021-12-17 | 维达力实业（赤壁）有限公司 | Preparation method of shell, shell and application |
| CN114481074A (en) * | 2022-04-06 | 2022-05-13 | 中南大学湘雅医院 | Magnesium alloy surface coating material and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101067200A (en) * | 2007-06-01 | 2007-11-07 | 哈尔滨工程大学 | Method for producing magnesium-lithium alloy titanium anticorrosion coating |
-
2011
- 2011-09-23 CN CN2011102864974A patent/CN102345103A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101067200A (en) * | 2007-06-01 | 2007-11-07 | 哈尔滨工程大学 | Method for producing magnesium-lithium alloy titanium anticorrosion coating |
Non-Patent Citations (2)
| Title |
|---|
| 李俊刚等: "镁锂合金表面处理技术研究现状及展望", 《材料保护》, vol. 44, no. 7, 31 July 2011 (2011-07-31), pages 38 - 41 * |
| 高福毅: "磁控溅射法在镁锂合金表面制备防腐涂层的研究", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》, no. 4, 15 April 2011 (2011-04-15), pages 22 - 25 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526174A (en) * | 2013-09-27 | 2014-01-22 | 南京工程学院 | Surface modification method for delaying degradation rate of biomedical magnesium alloy |
| CN103924202A (en) * | 2014-04-03 | 2014-07-16 | 西南交通大学 | Metal support surface modification method |
| CN109440065A (en) * | 2018-11-09 | 2019-03-08 | 南昌大学 | A kind of preparation method of Mg alloy surface tungsten molybdenum nanoscale anticorrosion film |
| CN109440065B (en) * | 2018-11-09 | 2020-07-14 | 南昌大学 | Preparation method of nano-scale corrosion-resistant molybdenum-tungsten film on surface of magnesium alloy |
| CN113811106A (en) * | 2020-06-11 | 2021-12-17 | 维达力实业（赤壁）有限公司 | Preparation method of shell, shell and application |
| CN113811106B (en) * | 2020-06-11 | 2023-06-27 | 维达力科技股份有限公司 | Shell preparation method, shell and application |
| CN114481074A (en) * | 2022-04-06 | 2022-05-13 | 中南大学湘雅医院 | Magnesium alloy surface coating material and application thereof |
| CN114481074B (en) * | 2022-04-06 | 2022-06-17 | 中南大学湘雅医院 | Magnesium alloy surface coating material and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102345103A (en) | Preparation method of titanium modified layer on surface of magnesium and lithium alloy | |
| CN102492924A (en) | Autologous ion bombardment assisted electron beam evaporation device, and method for coating film by using same | |
| CN103243305A (en) | Secondary electron emission film preparation method | |
| CN106435494A (en) | Method for improving electrical performance of positive electrode collector electrode of lithium battery | |
| CN108165943B (en) | TiB with structural gradient2Method for producing a coating | |
| US20200091497A1 (en) | Electrode plate and surface treatment method thereof | |
| CN106803570B (en) | A kind of lithium battery SiCO- carbon nano-tube coextruded film electrode | |
| CN108203813A (en) | A kind of preparation method of in-situ preparation graphene | |
| CN105529172A (en) | Surface protection method for samarium-cobalt magnet workpiece | |
| CN102094177A (en) | Production method for sputtering aluminum foil on surface of plastic | |
| CN108998769A (en) | A kind of two-part pulsed magnetron sputtering method | |
| CN201793721U (en) | Vacuum electronic gun coating machine | |
| CN112126961A (en) | Micro-arc oxidation surface treatment method for aluminum alloy workpiece | |
| EP2107592A3 (en) | Apparatus for mass-producing sulicon-based thin film and method for mass-producing silicon-based thin film | |
| CN204661820U (en) | A kind of PVD vaccum ion coater | |
| CN103774092B (en) | It is a kind of to prepare conductive and corrosion-resistant finishes method in Mg alloy surface | |
| CN102330057A (en) | Method for preparing metal ruthenium film for hard semiconductor component | |
| CN108796493B (en) | Hole sealing modification method for cold spraying coating on surface of light metal | |
| CN102945894A (en) | Preparation method of aluminum oxide passivation film and back electrode of crystalline silicon solar cell | |
| CN101445906A (en) | Method for preparing platinum coating layers on the surfaces of titanium and titanium alloy | |
| CN211256073U (en) | Device for preparing low-oxygen-content easily-oxidized film by ion plating in non-ultrahigh vacuum environment | |
| US10053769B2 (en) | Target preparation | |
| CN102242346A (en) | Device and process for growing TiAlN film on surface of aluminum alloy in situ | |
| CN113506887A (en) | Method for preparing TiCxNy coating on surface of stainless steel and application | |
| JPS6196721A (en) | Film forming method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120208 |