CN1712553A - Magnesium surface treatment and product therefrom - Google Patents
Magnesium surface treatment and product therefrom Download PDFInfo
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- CN1712553A CN1712553A CN 200410027756 CN200410027756A CN1712553A CN 1712553 A CN1712553 A CN 1712553A CN 200410027756 CN200410027756 CN 200410027756 CN 200410027756 A CN200410027756 A CN 200410027756A CN 1712553 A CN1712553 A CN 1712553A
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Abstract
A surface dealing process of Mg alloy. First, cover a layer of Ti on Mg alloy. Second, fit the titanium nitride on the surface of Mg alloy with a layer of Ti.
Description
[technical field]
The invention relates to a kind of surface treatment method that is used for improving hardness, wear resistance and the erosion resistance of magnesium alloy and reach the prepared magnesium alloy product of method thus.
[technical background]
Advantage such as magnesium alloy has that light weight, normal temperature mechanicalness are good, electromagnetic wave shielding and anti-seismic performance are good, cause that in recent years industry member and academia pay close attention to greatly, particularly needing the Application Areas of weight reduction, as notebook computer shell and phone housing etc., though but magnesium alloy has above-mentioned advantage, but also be faced with the not good shortcoming of hardness, wear resistance and erosion resistance, thereby Application of Magnesium is restricted.
Owing to there is above-mentioned shortcoming, the spare part made from magnesium alloy often need improve its hardness and wear resistance by surface treatment or surfaction, the industry more options plate the method for a film at its outside surface, because this method does not have too big influence for the size of workpiece.
Titanium nitride (TiN) is a kind of thin-film material that very generally uses now, and it is celebrated with utmost point excellent abrasive, high strength, erosion resistance and good heat conductivity, and is widely used in cutter and the mould.So, if titanium nitride membrane is applied on the magnesium alloy, will overcome the shortcoming of magnesium alloy, thereby make magnesium alloy obtain to use more widely.
Though the use of titanium nitride membrane can overcome the shortcoming of magnesium alloy,, the tack of the two is not fine, if directly with titanium nitride membrane attached to Mg alloy surface, be subjected to external force to do the time spent, titanium nitride membrane is easy to come off from Mg alloy surface, does not reach the effect of use.
[summary of the invention]
The object of the present invention is to provide a kind of titanium nitride firmly to be plated in the magnesium alloy member surface, be used for improving the surface treatment method and the prepared magnesium alloy product of method thus of hardness, wear resistance and the erosion resistance of magnesium alloy.
Technical problem to be solved by this invention is achieved through the following technical solutions: surface treatment method of Mg alloy of the present invention and goods thereof mainly are to plate a titanium membrane middle layer earlier on a magnesium alloy member surface, and then titanium nitride is plated on this titanium film, thereby titanium nitride firmly is plated on the Mg alloy surface.
The invention has the advantages that and utilize intermediary titanium film that titanium nitride firmly is plated on the magnesium alloy member surface, make the magnesium alloy product of gained have the characteristic of magnesium alloy and titanium nitride.
[description of drawings]
Fig. 1 is the sputter schema of surface treatment method of Mg alloy of the present invention.
Fig. 2 is a magnesium alloy member pre-treatment schema in the surface treatment method of Mg alloy of the present invention.
[embodiment]
Please refer to Fig. 1 and Fig. 2, surface treatment method of Mg alloy of the present invention is to utilize intermediary titanium film that titanium nitride firmly is plated in the magnesium alloy member surface, and it may further comprise the steps:
Step 1, preparation machine and material
The present invention needs a magnetic control dc sputtering machine, a magnesium alloy member and a titanium metal target at least.This sputter machine comprises a vacuum system, a sputtering chamber, a magnetic control system, a gas input system and a cooling system, this vacuum system is to be used for air pressure in the sputtering chamber, and this sputtering chamber comprises a loading stage, a pre-sputter baffle plate, a negative electrode and a magnetic control dish.This magnetic control system is to be located in the magnetic control dish by a permanent magnet to form, and this permanent magnet forms a magnetic field to increase interparticle collision opportunity in this magnetic field near the magnetic control dish.This gas input system comprises a mass flow control device, is used for controlling the flow of input gas.This cooling system is used for cooling off target and magnetic control dish, damages because temperature is too high to avoid both.
Step 2, magnesium is closed magnesium alloy member carry out surperficial pre-treatment
The surperficial pre-treatment of magnesium alloy member is a step the most basic in the thin film deposition process, and its main purpose is in order to remove the foreign material such as grease, waste material and organism that the magnesium alloy member adhering on surface, the sticking power during with the raising plated film, the pin hole phenomenon of minimizing film.
The surperficial pre-treatment of the magnesium alloy member of surface treatment method of Mg alloy of the present invention may further comprise the steps: take off ester to clean → washing-→ pickling → washing → drying.
At first magnesium alloy member being taken off ester in advance cleans, grunge pollution thing with strong erosion acid removal of solvents magnesium alloy member surface, the keyed jointing of extensive damage oil stain and magnesium alloy member, then magnesium alloy member is led and taken off ester and clean, with the grunge pollution on retentivity solution removal magnesium alloy member surface, but must not damage magnesium alloy member surface itself.Next wash, with taking off ester solvent and polluting and thoroughly wash off with the magnesium alloy member remained on surface.Further wash magnesium alloy member then, adjust the reactivity on magnesium alloy member surface with acid solution, in and the remained on surface SOLUTION PROPERTIES.Then wash again, the acid solution and the pollutent of this magnesium alloy member remained on surface are washed off.The final drying magnesium alloy member, the carrying out of wait subsequent handling.
Step 3, at magnesium alloy member surface plating one titanium film
In magnetic control dc sputtering machine, the titanium target is installed in magnetic control dish top, magnesium alloy member is installed on the loading stage in the sputtering chamber, and to keep the distance between titanium target and magnesium alloy member be 15～50cm, and titanium target and magnesium alloy member separated with the pre-sputter baffle plate.Start vacuum system, the air pressure in the sputtering chamber is extracted into 3 * 10
-5～8 * 10
-5The vacuum tightness of Torr, the heating magnesium alloy member remains on about 300 ℃ the temperature of magnesium alloy member, is 99.999% argon gas by gas input system input purity, and be 4～7.5s.c.c.m by the flow of mass flow control device control argon gas, to keep having 2 * 10 in the sputtering chamber
-3～5 * 10
-3The vacuum tightness of Torr then for the negative electrode of sputter machine adds one 350～550V voltage, makes and forms a high-voltage electric field between titanium target and magnesium alloy member, in addition, because the effect of magnetic control system forms a magnetic field near the titanium target material surface.The free electron that is arranged in the argon gas body between titanium target and magnesium alloy under electric field action with the molecule and the atomic collision of argon gas body, and this equimolecular and atom are produced dissociate, ionization and reaction such as excite.The electronics that produces after dissociating is quickened by electric field again, further cause the ionization process of other molecule and atom, thereby produce more ion and electronics, so chain reaction will produce a large amount of ions and electronics, these ions and electronics quicken the back and the acquisition high-energy through electric field, and hit the titanium target, and the atom of titanium target material surface is knocked out and outwards sputter, and, owing to have magnetic field near the target material surface, the ion and the electronics that enter in the magnetic field are made corkscrew motion under electric field and magnetic field acting in conjunction, thereby further increase the interior argon molecules in this zone because of the Ionized chance of collision, thereby make more ionic bombardment titanium target and sputter more titanium atom.At this moment, owing to be provided with baffle plate between magnesium alloy member and titanium target, the titanium atom that comes out from target as sputter can not arrive the magnesium alloy member surface, at this moment, if titanium target material surface contains foreign material, then by said process can these foreign material being removed, just carry out pre-sputter to the titanium target.Titanizing target pre-sputter was removed baffle plate after 30 minutes, at this moment, the titanium atom that sputters out from titanium target material surface will be delivered to the magnesium alloy member surface, after these titanium atoms arrive the magnesium alloy member surface, owing to itself have higher kinetic energy, to bombard the magnesium alloy member surface, and further remove foreign material and the heating magnesium alloy member that after surperficial pre-treatment, still remains in the magnesium alloy member surface, thereby improve the tack on magnesium alloy member surface.Above-mentioned titanium atom can be the magnesium alloy member absorption again and deposits to the magnesium alloy member surface in the bombardment magnesium alloy member, thereby form a titanium film, this process is the sputter of magnesium alloy member, and sputter is after 60 minutes, and the magnesium alloy member surface will form the titanium film that a thickness is 0.2～0.5 μ m.
Step 4, form one deck titanium nitride membrane on magnesium alloy member surface
Plate titanium film Hou on the magnesium alloy member surface, making the gas input system import purity simultaneously is 99.999% argon gas and nitrogen, and the flow of control argon gas and nitrogen is respectively 1～2s.c.c.m and 3～6s.c.c.m, and has 1 * 10 in the maintenance sputtering chamber
-3～3 * 10
-3The vacuum tightness of Torr.The atom of titanium target material surface is outwards sputter owing to continue to be bombarded, the titanium atom that sputters out contacts with nitrogen and chemical reaction takes place forms titanium nitride and deposit on the titanium film of magnesium alloy member, thereby on the titanium film, form the titanium nitride film, when sputter stopped sputter after 2 hours, magnesium alloy member will form a thickness on the basis of titanium plated film be the titanium nitride membrane of 1～3 μ m, can take out this magnesium alloy member after the cooling.In the above-mentioned sputter process, cooling system can be taken away permanent magnet and the unnecessary heat of titanium target in the magnetic control dish when the sputter machine is worked, and unlikelyly damages owing to system temperature is too high.
By the formed magnesium alloy product of aforesaid method have not only that light weight, normal temperature mechanicalness are good, the characteristic of magnesium alloy such as electromagnetic wave shielding and anti-seismic performance are good, and has a characteristic of utmost point excellent abrasive, high strength, erosion resistance and good titanium nitrides such as heat conductivity, in addition, it is golden yellow that titanium nitride is, thickness by the control titanium nitride membrane can make the magnesium alloy product surface present the outward appearance of different golden colors from shallow to deep.
The present invention also can clean the magnesium alloy member surface by argon ion earlier before titanizing, because of after this process, can make the magnesium alloy member surface produce the better plated film of sticking power.
In addition, because sputter can be realized splendid sedimentation effect, the control of large-sized deposit thickness, accurate Composition Control and lower manufacturing cost simultaneously, so, adopt jet-plating method to come titanizing and titanium nitride in the preferred embodiment of the invention described above.But,, also can adopt other film coating method, as electricity slurry ion plating method or electric arc vapour deposition method if when other film coating method can be realized same effect of the present invention.
Claims (10)
1. a surface treatment method of Mg alloy is used for titanium nitride firmly is plated in a magnesium alloy member surface, and it may further comprise the steps:
At magnesium alloy member surface plating one platinum/titanium metal thin film;
On the titanium film, form the titanium nitride film.
2. surface treatment method of Mg alloy as claimed in claim 1 is characterized in that: described surface treatment method of Mg alloy also comprises a surperficial pre-treatment step, promptly earlier magnesium alloy member is carried out treating processess such as surperficial degreasing, pickling and washing before titanizing.
3. surface treatment method of Mg alloy as claimed in claim 1, it is characterized in that: described surface treatment method of Mg alloy carries out in a chamber, be placed with magnesium alloy member and titanium target in this chamber, have the voltage of 350～550V between this titanium target and magnesium alloy member.
4. surface treatment method of Mg alloy as claimed in claim 3, it is characterized in that: during titanizing, in chamber, import argon gas, be positioned at the argon gas ionization under effect of electric field between magnesium alloy member and titanium target, the argon ion bombardment titanium target that produces and sputter titanium atom forms this titanium film thereby titanium atom transmits and deposit to the magnesium alloy member surface.
5. surface treatment method of Mg alloy as claimed in claim 4, it is characterized in that: after the titanium film forms, in chamber, import argon gas and nitrogen simultaneously, the titanium target still is subjected to the argon gas ion bombardment and continues to sputter titanium atom, titanium atom and nitrogen generation chemical reaction and form titanium nitride and deposit to the titanium film surface, thus this titanium nitride membrane formed.
6. surface treatment method of Mg alloy as claimed in claim 3 is characterized in that: before the titanizing, the air pressure in the chamber is extracted into 3 * 10
-5～8 * 10
-5The vacuum tightness of Torr.
7. surface treatment method of Mg alloy as claimed in claim 6 is characterized in that: during titanizing, the argon flow amount of input is 4～7.5s.c.c.m, has 2 * 10 in the chamber
-3～5 * 10
-3The vacuum tightness of Torr.
8. surface treatment method of Mg alloy as claimed in claim 5 is characterized in that: during titanium-nitride, the argon flow amount of input is that 1～2s.c.c.m and nitrogen flow are 3～6s.c.c.m, has 1 * 10 in the chamber
-3～3 * 10
-3The vacuum tightness of Torr.
9. surface treatment method of Mg alloy as claimed in claim 3 is characterized in that: this chamber is degree of the spattering chamber of a sputter machine.
10. magnesium alloy product that makes by the described surface treatment method of Mg alloy of claim 1 comprises:
One magnesium alloy layer;
The titanium nitride layer;
One is positioned at the titanium coating between magnesium alloy layer and titanium nitride layer.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410027756 CN1712553A (en) | 2004-06-15 | 2004-06-15 | Magnesium surface treatment and product therefrom |
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|---|---|---|---|
| CN 200410027756 CN1712553A (en) | 2004-06-15 | 2004-06-15 | Magnesium surface treatment and product therefrom |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101728241B (en) * | 2008-10-10 | 2012-07-04 | 台湾积体电路制造股份有限公司 | Method for reducing the peeling of film deposited on technique external member |
| CN101422977B (en) * | 2007-10-30 | 2012-07-04 | 比亚迪股份有限公司 | Filming material and preparation method thereof |
| CN102534487A (en) * | 2010-12-30 | 2012-07-04 | 鸿富锦精密工业（深圳）有限公司 | Coated piece with hard coating and preparation method thereof |
| CN101444983B (en) * | 2007-11-27 | 2012-07-04 | 比亚迪股份有限公司 | Coating material and preparation method thereof |
| CN101623943B (en) * | 2008-07-07 | 2012-09-05 | 比亚迪股份有限公司 | Coating material and preparation method thereof |
| CN104195517A (en) * | 2014-08-29 | 2014-12-10 | 南京工程学院 | Method for reducing residual stress of surface coating of biological medical magnesium alloy |
| CN104213091A (en) * | 2014-08-29 | 2014-12-17 | 南京工程学院 | Method for improving bonding property of magnetron sputtering TiN coating on biomedical magnesium alloy surface |
| CN106943627A (en) * | 2017-02-15 | 2017-07-14 | 北京华钽生物科技开发有限公司 | High-biocompatibility fiber |
-
2004
- 2004-06-15 CN CN 200410027756 patent/CN1712553A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422977B (en) * | 2007-10-30 | 2012-07-04 | 比亚迪股份有限公司 | Filming material and preparation method thereof |
| CN101444983B (en) * | 2007-11-27 | 2012-07-04 | 比亚迪股份有限公司 | Coating material and preparation method thereof |
| CN101623943B (en) * | 2008-07-07 | 2012-09-05 | 比亚迪股份有限公司 | Coating material and preparation method thereof |
| CN101728241B (en) * | 2008-10-10 | 2012-07-04 | 台湾积体电路制造股份有限公司 | Method for reducing the peeling of film deposited on technique external member |
| CN102534487A (en) * | 2010-12-30 | 2012-07-04 | 鸿富锦精密工业（深圳）有限公司 | Coated piece with hard coating and preparation method thereof |
| CN104195517A (en) * | 2014-08-29 | 2014-12-10 | 南京工程学院 | Method for reducing residual stress of surface coating of biological medical magnesium alloy |
| CN104213091A (en) * | 2014-08-29 | 2014-12-17 | 南京工程学院 | Method for improving bonding property of magnetron sputtering TiN coating on biomedical magnesium alloy surface |
| CN104213091B (en) * | 2014-08-29 | 2017-04-12 | 南京工程学院 | Method for improving bonding property of magnetron sputtering TiN coating on biomedical magnesium alloy surface |
| CN106943627A (en) * | 2017-02-15 | 2017-07-14 | 北京华钽生物科技开发有限公司 | High-biocompatibility fiber |
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