CN1015995B - Method for ion deposition of (Ti, Al) N hard film on surface of aluminum alloy - Google Patents
Method for ion deposition of (Ti, Al) N hard film on surface of aluminum alloyInfo
- Publication number
- CN1015995B CN1015995B CN 87108177 CN87108177A CN1015995B CN 1015995 B CN1015995 B CN 1015995B CN 87108177 CN87108177 CN 87108177 CN 87108177 A CN87108177 A CN 87108177A CN 1015995 B CN1015995 B CN 1015995B
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- CN
- China
- Prior art keywords
- aluminum alloy
- film
- electric current
- aluminum
- deposition
- 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.)
- Expired
Links
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 56
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 41
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000008021 deposition Effects 0.000 title claims description 17
- 239000010936 titanium Substances 0.000 claims abstract description 41
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 24
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- 239000004411 aluminium Substances 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 14
- 229910045601 alloy Inorganic materials 0.000 claims description 12
- 229910004349 Ti-Al Inorganic materials 0.000 claims description 8
- 229910004692 Ti—Al Inorganic materials 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 4
- 238000000151 deposition Methods 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 13
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000007733 ion plating Methods 0.000 abstract description 3
- 239000011253 protective coating Substances 0.000 abstract 1
- 239000012495 reaction gas Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000010894 electron beam technology Methods 0.000 description 9
- 238000000576 coating method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 230000035882 stress Effects 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000004237 Crocus Nutrition 0.000 description 1
- 241000596148 Crocus Species 0.000 description 1
- 229910001060 Gray iron Inorganic materials 0.000 description 1
- 240000003936 Plumbago auriculata Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 229910002114 biscuit porcelain Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 206010025482 malaise Diseases 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000000191 radiation effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
The invention is a method for ion depositing a (Ti, Al) N hard film on an aluminum alloy surface. It adopts hollow cathode ion plating method to evaporate and ionize titanium and aluminum materials together, and introduces reaction gas N2Generating a (Ti, Al) N compound, and depositing on the surface of the aluminum alloy at a low temperature of about 200 ℃. The (Ti, Al) N film obtained by the method has high hardness, good wear resistance and corrosion resistance, compact structure and firm combination with a matrix. The method is a good method for generating an effective hard protective coating on the surface of the aluminum alloy.
Description
The present invention relates to the method that aluminum alloy surface is handled.
Usually, the method for aluminum alloy surface processing mainly contains japanning and anonizing.
The painted purpose is that metal and environment are completely cut off, so that play preservative activity, reduces but paint topped its thermal conductivity that can make on aluminium alloy.Wear-resisting effect simultaneously is also relatively poor.
Anonizing is by producing Al in aluminum alloy surface
2O
3Film shields, and this film makes the hardness of aluminum alloy surface can reach Hv=400-600, but the surface of this film is a porous, thus little to corrosion proof improvement, in addition, Al
2O
3Film has fragility, and thickness and hardness instability are also not obvious to the raising effect of aluminum alloy surface wear resistance and bite-resistant performance.
External is solve aluminium alloy ornamental, does work aspect physical vapor deposition, relates to the surface treatment of a kind of aluminum wrist-watch with the indication part as the clear 55-97469 of JP.The method of this processing is the watch hand surface of making at aluminum, and behind employing ion plating or the sputter plating Cr film, the Au film is plated in ion plating or sputter again.The purpose of handling mainly is to solve the ornamental of aluminium pointer and improve solidity to corrosion, does not consider the wear resistance on aluminum surface.
Handle at the lining of hard films, all be after adopting simple metal titanium evaporation, ionization among clear 52-7879 of JP and the clear 57-161058 of JP, feed reactant gases again and on steel substrate, generate TiC, TiN and Ti(C, N) film, owing to there is bigger internal stress, lacking toughness is so be unwell to hard coating as aluminum alloy material surface.Simultaneously, the temperature of using when handling among the clear 57-161058 of JP (550 ℃) is also higher, is not suitable for the metal of this low melting point of aluminum alloy materials (＜660 ℃), also makes alumina-base material produce serious thermal distortion during processing easily.
The purpose of this invention is to provide a kind of (Ti, Al) method of N hard coating that produces a kind of wear-resisting, anti-corrosion, good toughness in aluminum alloy surface.
The solution of the present invention is: adopt the hallow cathode deposition, HCD method, with titanium and aluminium co-evaporated and ionization, and feed reactant gases N
2(the low temperature deposit about 200 ℃ is in aluminum alloy surface for Ti, Al) N compound in the reaction generation.
The weight proportion of above-mentioned co-evaporated and ionized titanium, aluminium material is respectively the 90-95%(titanium) and 5-10%(aluminium).
Be no more than 200 ℃ for making, in coating process, adopt minor arc electric current, working vacuum degree and three processing parameters of baking electric current are carried out Comprehensive Control by the alloy matrix aluminum temperature of plated film.
For making rete and aluminium alloy that firm bonding force be arranged and making the film layer structure densification, the present invention changes the focus level of the ionization level and the electron beam spot of furnace gas by the polarity in the magnetic field of change magnetic field focus coil generation.
Figure one is aluminum alloy surface (Ti, Al) N film and a Ti-Al alloy middle layer synoptic diagram.
Figure two is dual mode sketches of stove internal magnetic field polar contribution.
Figure three is aluminum alloy surface (Ti, Al) ultimate analysis curves of N film.
Figure four is grinding defect morphologies of the TiN of aluminum alloy surface.
Figure five is aluminum alloy surface (Ti, Al) grinding defect morphologies of N.
Below the present invention is further explained in detail:
Said employing hallow cathode deposition, HCD method among the present invention program is to say that the equipment that adopts is the hallow cathode deposition, HCD device. The titanium of said common evaporation and ionization, aluminium material are to put in the crucible of hallow cathode deposition, HCD device by the above-mentioned proportioning that provides, the method for its placement be the titanium material in the above, the aluminium material is below. Under the effect of the electron beam that the hollow cathode electron gun produces, with the pure titanium material fusing on upper strata, rear dependence titanium liquation makes rapidly the aluminium fusing earlier. In evaporate process, the stirring action that produces under the focus coil magnetic fields by electron beam makes the Ti-Al liquation keep evenly mixing. When titanium, aluminium material after fusing evaporation under the vacuum, in the situation that does not pass into reacting gas, apply-30 at workpiece～-back bias voltage of 50v, first evaporation 3-5 minute, obtaining one deck Ti-Al alloy intermediate layer 2 on the alloy matrix aluminum 1 and between (Ti, Al) N film 3 with this. In order to increase the adhesion of (Ti, Al) N film and alloy matrix aluminum.
The said control range that three technological parameters are comprehensively controlled in front is: minor arc electric current 80-130A, working vacuum degree 6.67 * 10-2～6.67×10
-1Pa, baking electric current 0-80A, the principle of control is: in the incipient stage, formed the Ti-Al alloy intermediate layer stage in namely evaporation 3-5 minute, can carry out under higher vacuum, this moment, the minor arc electric current can be opened more greatly. After the incipient stage, because the thermoradiation efficiency of liquation in the continuous bombardment effect of ion and the crucible, can cause workpiece temperature that the trend of rising is arranged, should turn down the minor arc electric current this moment, but for keeping the plasma discharge state in the stove, vacuum can be reduced, in order to again keep the stable of the interior work of stove. The baking electric current will progressively reduce in deposition, can all turn off in the interstage of deposition, only relies on the thermoradiation efficiency of liquation in the bombardment effect of ion and the crucible just can keep workpiece temperature about 200 ℃.
Figure two is for two kinds of different stove internal magnetic field polarity distribution mode schematic diagrames that change furnace gas ionization level and electron beam spot focus level. Wherein polarity of the magnetic field is that NS-NS distributes among the figure two (a), two polarity of the magnetic fields that coil 5,6 produces that the electron beam 7 that this kind distribution mode is launched electron gun 4 focuses on, and meeting is so that big to the beam spot focussing force, and the bundle spot is little, the energy density height. Melting capacity to metal in the crucible 8 is big like this, and the result makes titanium, aluminium material will melt rapidly in the incipient stage. Melt at titanium, aluminium material, and after workpiece had deposited one deck Ti-Al alloy intermediate layer 2, the polarity of the magnetic field that (a) mode among the figure two can be converted to (b) mode distributed. (b) polarity of the magnetic field of mode is that NS-SN distributes, and this kind mode is little to the Electron Beam Focusing effect of electron gun 4 emissions, and the bundle spot is big, and energy density is low, but the ionization level of furnace gas is increased. After titanium and aluminium be melt into one, become titanium-molten aluminium alloy, its fusing point was far below the fusing point of pure titanium, and utilize the low beam bombardment of energy density also to be enough to keep evaporation this moment. At this moment the electron beam of large beam spot is conducive to improve the ionization level of furnace gas, so that the quality of depositional coating improves; The speed of deposition also improves, thereby has shortened the needed time of deposition, and the temperature of workpiece also is unlikely rising. The change of polarity of the magnetic field realizes by two-way knife switch of adjunction in focus circuit among the figure two.
The present invention's good effect compared with prior art is:
The present invention realize (Ti, Al) N film and alloy matrix aluminum be in conjunction with firmly, compact structure.
2. method sedimentation velocity of the present invention is fast, as long as 40-45 minute can reach about 5 μ m.Figure three is the surface-element analytic curve through technology of the present invention institute coatings.
3. sedimentary (Ti, Al) N film hardness height improve the wear resistance of aluminum alloy surface greatly through the present invention.Table 1 is the result of microhardness value and wearing test.The condition of wearing test is that last sample is grey cast iron (HT20-40), and following sample is an aluminium alloy, and positive pressure 75kg with No. 30 engine oil lubrication, wore and tore one hour.
4.(Ti Al) Al in the N film can make its internal stress reduce.Table 2 is rete internal stress and the relation that adds the aluminium amount.
The internal stress of table 2 rete and the relation that adds the Al amount
The kind stress σ of film (*
10
3Mpa）
Pure TiN film-74.48
(Al, Al) the N film-61.33 that add 5%Al
(Ti, Al) the N film-46.97 that add 10%Al
5. compare (Ti, Al) good toughness of N coating with TiN coating.Under identical abrasive conditions, the abrasive dust of TiN is brittle and scales off, and (Ti, Al) abrasive dust of N film is tiny free particle disengaging, shown in figure four and figure five.
6. energy-conservation, the water saving, nuisanceless of technological process of the present invention, labor condition is good.
Be specific embodiments of the invention below:
Utilize the present invention can the cast aluminium alloy of the different trades mark and electrician with fine aluminium material surface carry out ion deposition (Ti, Al) N film, deposition on the Jiefang brand piston of automobile that broadly representative material ZL108 cast aluminium is made (Ti, Al) the concrete technology of N film is as follows:
(1) the pure A1 of 95% Ti material (trade mark TA1) and 5% is expected to put into the plumbago crucible of hallow cathode deposition, HCD device after weighing, charging method as previously mentioned.
(2) workpiece to be plated is strict cleans.In trieline, use ultrasonic cleaning five minutes earlier, clean with acetone again and dry, in the vacuum oven of packing into immediately then with crocus cloth.
(3) close upper furnace door, open mechanical pump, diffusion pump, make the interior vacuum tightness of stove be evacuated to 6.67 * 10
-3More than the Pa.
(4) feed argon gas, make in the stove vacuum tightness reduce to 6.67pa, apply-negative high voltage of 1.5kv sputter clean 15-20 minute on the workpiece.
(5) close argon gas,, make the interior vacuum tightness of stove return to 6.67 * 10 again to vacuumizing in the stove
-3Behind the pa, connect the baking electric current, baking is 20-30 minute under condition of high vacuum degree, and the baking electric current is approximately 100-120A.Storing temperature must not surpass the aging temp (＜300 ℃) of cast aluminium alloy.During baking, start the rotation motor of work rest, workpiece is rotated, the homogeneity of workpiece temperature during with the assurance baking.After baking finishes, the baking electric current falls to 80A.
(6) after workpiece is cooled to 200 ℃, feed argon gas, vacuum tightness is reduced to 6.67 * 10pa, the electron beam gun that ignites, the about 220V of striking voltage, the about 12A of electric current.Open the minor arc electric current then rapidly, regulate minor arc voltage power 65V, the minor arc electric current is about about 120A.Make the interior vacuum tightness of stove rise to 6.67 * 10
-2Behind the pa, make the minor arc voltage and current return to above-mentioned numerical value once more, close the striking electric current.At this moment, the polarity of crucible magnetic field focus coil adopts as (a) mode among the figure two, and metal charge melts rapidly.
(7) treat that metal charge melts fully after, open the baffle plate of crucible top, deposition one deck Ti-Al alloy layer on workpiece, depositing time is about 3 minutes.Add-30V negative bias on the workpiece this moment, and workpiece remains rotation, and the baking electric current will progressively reduce, and makes workpiece temperature be no more than 200 ℃.
(8) depositing Ti-Al alloy layer by switching the two-way knife switch in the crucible magnetic focusing circuit, became (b) mode to the polarity in crucible magnetic field (a) mode from figure two after 3 minutes.Feed highly purified reactant gases N
2(99.99%), make the interior working vacuum degree of stove become 9 * 10
-2Exoelectrical reaction at this moment, takes place in the stove rapidly in pa, can observe the aura of bisque beauty from the viewing window.
(9) for 200 ℃ of the temperature maintenance that make workpiece, along with the carrying out of handling, as when finding that workpiece temperature has rising, can turn down the minor arc electric current, and increase argon gas feeding amount, and reduce vacuum tightness, can continue to keep plasma discharge state in the stove like this, the minor arc electric current can progressively be reduced to 80A, and the working vacuum degree can progressively be adjusted to 6.67 * 10
-1Pa.The baking electric current can reduce to 0, and it is constant that only need utilize the thermal radiation effect of ion bombardment and crucible inner melt just can keep workpiece temperature this moment.
(10) depositing time is 40 minutes, workpiece is rotated, and apply-negative bias of 30V, and the thickness of settled layer is about about 5 μ m.
(11) after deposition finishes, turn down minor arc electric current and voltage after, cut off main arc power source, the electron beam gun blow-out.Close argon gas (Ar) and nitrogen (N
2), vacuum tightness in the stove is evacuated to 6.67 * 10
-3The above cooling of pa.At this moment, workpiece still need keep rotating.
(12) treat that workpiece is chilled to below 80 ℃ after, can come out of the stove.
The microhardness of table 1 specimen surface, thickness and wear test result
Experimental condition wear extent (mg) microhardness (HV0.01) thickness (μ m)
No coating 7.55 450～500＊-
Pure TiN film 4.0 1,967 5.8
Add (Ti, Al) N film 2.37 1,952 6.2 that 2.5%Al forms
Add (Ti, Al) N film 0.35 1,973 6.0 that 5%Al forms
Add (Ti, Al) N film 0.70 1,530 5.6 that 10%AL forms
Add (Ti, Al) N film 4.47 760～980 that 35%Al forms＊5.5
* hardness is inhomogeneous.
Claims (2)
1, a kind of method in aluminum alloy surface ion deposition (Ti, Al) N hard films, adopt hallow cathode deposition, HCD, it is characterized in that: with weight ratio is 90-95% titanium and 5-10% aluminium co-evaporated and ionization, first evaporation 3-5 minute generation one deck Ti-Al alloy middle layer on alloy matrix aluminum; Then feed reactant gases N
2(the low temperature deposit about 200 ℃ is in aluminum alloy surface for Ti, Al) N compound in the reaction generation.
2, according to claim 1 a kind of at aluminum alloy surface ion deposition (Ti, Al) method of N hard films, it is characterized in that said about 200 ℃ low temperature takes the processing parameter Comprehensive Control to realize, each parameter control scope: minor arc electric current 80-130A, working vacuum degree 6.67 * 10
-2-6.67 * 10
-1Pa, baking electric current 0-80A.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87108177 CN1015995B (en) | 1987-12-18 | 1987-12-18 | Method for ion deposition of (Ti, Al) N hard film on surface of aluminum alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87108177 CN1015995B (en) | 1987-12-18 | 1987-12-18 | Method for ion deposition of (Ti, Al) N hard film on surface of aluminum alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1033655A CN1033655A (en) | 1989-07-05 |
| CN1015995B true CN1015995B (en) | 1992-03-25 |
Family
ID=4816389
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87108177 Expired CN1015995B (en) | 1987-12-18 | 1987-12-18 | Method for ion deposition of (Ti, Al) N hard film on surface of aluminum alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1015995B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304627C (en) * | 2004-04-30 | 2007-03-14 | 麦桥 | Surface antibiotic, wearable stainless steel products and its production method |
| CN101979703B (en) * | 2010-11-10 | 2013-01-16 | 范文波 | Method for performing surface treatment on golf head by aluminium -titanium nitride composite coating |
| CN108103548B (en) * | 2018-03-02 | 2023-09-19 | 安徽尚德科技有限公司 | High wear-resisting aluminum alloy intermediate plate |
| CN113046677B (en) * | 2021-03-12 | 2023-05-26 | 昆明理工大学 | Flaky ceramic/aluminum alloy composite material and preparation method thereof |
| CN114481024A (en) * | 2021-12-29 | 2022-05-13 | 江苏佳搏实业发展集团有限公司 | High-performance aluminum alloy die ceramic coating and preparation method thereof |
| CN114606461B (en) * | 2022-04-18 | 2023-02-28 | 东莞理工学院 | Preparation method of Al-Ti-C-N nanocrystalline and application of Al-Ti-C-N nanocrystalline in aluminum alloy |
-
1987
- 1987-12-18 CN CN 87108177 patent/CN1015995B/en not_active Expired
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| Publication number | Publication date |
|---|---|
| CN1033655A (en) | 1989-07-05 |
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