CN102605367A - Hard film, coated piece with hard film and manufacturing method of coated piece - Google Patents
Hard film, coated piece with hard film and manufacturing method of coated piece Download PDFInfo
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- CN102605367A CN102605367A CN2011100257303A CN201110025730A CN102605367A CN 102605367 A CN102605367 A CN 102605367A CN 2011100257303 A CN2011100257303 A CN 2011100257303A CN 201110025730 A CN201110025730 A CN 201110025730A CN 102605367 A CN102605367 A CN 102605367A
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Abstract
The invention discloses a hard film, a coated piece with the hard film and a manufacturing method of the coated piece. The hard film comprises titanium nitride layers and aluminum nitride layers which are alternatively arranged. The hard film has the following components in mass percent content of 46-46.6% of titanium, 25.6-26.2% of aluminum and 27.2-28.4% of nitride. The coated piece comprises a base material and the hard film formed on the base material. The manufacturing method of the coated piece comprises the following steps of: arranging the base material in a coating machine to alternatively deposit the titanium nitride layers and the aluminum nitride layers; and then arranging the deposited base material in a thermal treatment furnace for nitridation thermal treatment so as to obtain the coated piece. According to the coated piece with the hard film formed by the titanium nitride layers and the aluminum nitride layers, the hardness and the abrasion resistance of the coated piece can be greatly improved, and the preparation method is simple.
Description
Technical field
The invention relates to a kind of ganoine thin film, possess lining part, and the making method of this lining part of this ganoine thin film.
Background technology
Ganoine thin film is widely used in the surface of base materials such as wimet, rapid steel and pottery to produce the lining part of high firmness and high-wearing feature.Existing ganoine thin film mainly contains titanium nitride membrane, aluminium nitride film and titanium nitride/aluminium nitride AlN laminated film etc.Wherein, titanium nitride/aluminium nitride AlN laminated film is through the nanometer particle mutually mutual diffusion of titanium nitride layer with aln layer, and more single titanium nitride membrane, aluminium nitride film have higher hardness, and common titanium nitride/aluminium nitride AlN laminated film hardness can reach 40Gpa.
Generally replacing titanium nitride layer and aln layer on the base material on base material, to form titanium nitride/aluminium nitride AlN laminated film in the industry through the physical vapor deposition (PVD) method; In right this kind titanium nitride/aluminium nitride AlN laminated film; Titanium and aluminium are difficult to generate with the nitrogen complete reaction titanium nitride or the aluminium nitride AlN of chemical dosage ratio; Actual much other phases that contain in this laminated film are like Ti
2N, A1
2N and Ti, Al etc.In this laminated film; Usually the quality percentage composition of titanium is 47.2%-48.4%, and the quality percentage composition of aluminium is 26.8%-27.4%, and the quality percentage composition of nitrogen is 24.2-26%; The content of nitrogen is on the low side relatively, is difficult to improve preferably ganoine thin film whole hardness and wear resisting property.
Also have in the industry base material (like aluminium, titanium etc.) is handled the hardness that improves substrate surface through nitriding, this nitriding treatment process is mainly the nitriding of aura method.The nitriding of aura method is that base material is put into coating chamber; At a certain temperature; The principle of utilizing photoglow is directly beaten at substrate surface after with nitrogen-atoms ionization, generates the bigger nitride of hardness with the element reaction with the base material top layer, so increases the hardness and wear resistance ability of substrate surface.Yet it is limited, therefore limited to the raising of base material hardness that the IR of nitrogen is handled in this kind nitriding, has been formed with the situation of nitride hard layer for substrate surface, and the hardness of wanting further to improve through this kind nitriding method this hard layer has been difficult to realize.
Summary of the invention
In view of foregoing, be necessary to provide the ganoine thin film of a kind of high firmness, high abrasion resistance.
In addition, also be necessary to provide a kind of lining part that possesses above-mentioned ganoine thin film.
In addition, be necessary to provide a kind of making method of above-mentioned lining part.
A kind of ganoine thin film comprises the titanium nitride layer and the aln layer of alternately arranging, and the quality percentage composition of titanium is at 46-46.6% in the said ganoine thin film, and the quality percentage composition of aluminium is at 25.6-26.2%, and the quality percentage composition of nitrogen is at 27.2-28.4%.
A kind of lining part comprises base material and is formed at the ganoine thin film on the base material, and the quality percentage composition of titanium is at 46-46.6% in this ganoine thin film, and the quality percentage composition of aluminium is at 25.6-26.2%, and the quality percentage composition of nitrogen is at 27.2-28.4%.
A kind of making method of the part that is covered may further comprise the steps:
One base material is provided;
Base material is inserted alternating deposit titanium nitride layer and aln layer in the coating equipment;
The base material that then will deposit titanium nitride layer and aln layer is put into heat treatment furnace and is carried out nitrogenize thermal treatment; Make the ganoine thin film layer of abundant nitrogenize; Correspondingly make said lining part; The quality percentage composition of titanium is at 46-46.6% in the ganoine thin film, and the quality percentage composition of aluminium is at 25.6-26.2%, and the quality percentage composition of nitrogen is at 27.2-28.4%.
Ganoine thin film of the present invention by titanium nitride layer and aln layer alternating deposit and alternating deposit after nitrogenize thermal treatment process; The film that titanium nitride layer and aln layer alternating deposit form is compared to single titanium nitride layer or aln layer film; Through the nanometer particle mutually mutual diffusion of titanium nitride layer, make ganoine thin film possess higher hardness and wear resisting property with aln layer; Through the nitrogenize heat treatment process, improved the quality percentage composition of nitrogen element, can make the unreacted and complete nitrogenize of the incomplete metallics of nitrogenize on the film, the hardness of ganoine thin film further improves, and can bring up to 46-50GPa from 40Gpa generally.Correspondingly, the lining part that possesses this ganoine thin film possesses good hardness and wear resisting property.Make in the lining part, through earlier base material being carried out alternating deposit titanium nitride layer and aln layer, the base material that will form ganoine thin film is then put into heat treatment furnace and is carried out nitrogenize thermal treatment, and manufacture craft is simple.
Description of drawings
Fig. 1 is the cross-sectional schematic that preferred embodiment of the present invention possesses the lining part of ganoine thin film;
Fig. 2 is the making method schema of lining part shown in Figure 1;
Fig. 3 is the be covered structural representation of used coating equipment in the making processes of part of Fig. 1.
The main element nomenclature
Lining part 10
Base material 11
Ganoine thin film 12
Titanium nitride layer 121
Aln layer 122
Source of the gas passage 24
Embodiment
See also Fig. 1, preferred embodiment lining part 10 of the present invention comprises base material 11 and is formed on the ganoine thin film 12 on the base material 11.Said lining part 10 can be cutter, and the material of this base material 11 can be wimet, rapid steel etc.
Said ganoine thin film 12 is formed on the surface of this base material 11 through PVD plated film and nitrogenize thermal treatment, and the hardness of this ganoine thin film 12 is between 46-50Gp a.This ganoine thin film 12 comprises some aluminium nitride AlN (AlN) layer 121 and some titanium nitrides (TiN) layer 122; This several A lN layer 121 is alternately arranged with some TiN layers 122; The one deck that wherein contacts with base material 11 is a titanium nitride layer 122; These titanium nitride layer 122 thermal expansivity can not produce very big internal stress near base material 11 when temperature variation, be convenient to combine with base material 11 stable.The one deck that exposes to lining part 10 surfaces can be aln layer 121 or titanium nitride layer 122.All between 3～15 nanometers, the integral thickness of this ganoine thin film 12 is between 1～6 micron for the thickness of each titanium nitride layer 122 and each aln layer 121.In this ganoine thin film 12, the quality percentage composition of titanium is 46-46.6%, and the quality percentage composition of aluminium is 25.6-26.2%, and the quality percentage composition of nitrogen is 27.2-28.4%.
See also Fig. 2, the making method of this lining part 10 may further comprise the steps:
S1: a base material 11 is provided, and the material of base material 11 is a rapid steel in the present embodiment, and this base material 11 is carried out ultrasonic cleaning, to remove the greasy dirt on base material 11 surfaces, as adopting absolute ethyl alcohol or acetone base material 11 is carried out ultrasonic cleaning.
S2: carry out the PVD plated film in the coating equipment with inserting after base material 11 oven dry.In conjunction with consulting Fig. 3, a coating equipment 100 is provided, coating equipment 100 comprises a coating chamber 20 and is connected a vacuum pump 30 of coating chamber 20 that vacuum pump 30 is in order to vacuumize coating chamber 20.Be provided with pivoted frame and baffle plate (not shown), 2 first targets 22 and 2 second targets 23 in this coating chamber 20.Pivoted frame drives base material 11 along circular trace 21 revolution, base material 11 also rotation along track 21 revolution the time.Baffle plate is sputtered onto base material 11 in order to the particle of when cleaning target, isolating sputter, and it opens or closes through electronic control automatically.2 first targets 22 and 2 second targets 23 are about the centrosymmetry setting of track 21, and 2 first targets 22 relatively are arranged on the interior outside of track 21, and 2 second targets 23 relatively are arranged on the interior outside of track 21.The two ends of each first target 22 and each second target 23 are equipped with source of the gas passage 24, and gas gets into the surface that coating chamber 20 bombards corresponding target via this source of the gas passage 24, so that target material surface sputters particle.When base material 11 passed between 2 first targets 22 or 2 second targets 23, the particle that sputters on the target arrived base material 11 surfaces with sputter.
Base material 11 surface coating processes are following: (1) provides first target 22 and second target 23, and cleans each target material surface.First target 22 is the titanium target, and second target 23 is the aluminium target.Cleaning process is following, and titanium target and aluminium target are placed respectively on the sputtering source of coating equipment 100, is evacuated to 3.0 * 10
-3Pa, the feeding flow is 500cm
3The high-purity argon gas of/s, regulate to be biased in-250～-350V, open titanium target and aluminium target, power is 3000～5000w, and argon gas bombards the surface of titanium target and aluminium target, and is so that titanium target and aluminium target surface cleaning is clean.When cleaning, pivoted frame does not rotate, and baffle plate is opened so that the particle and the base material 11 of sputter are isolated.(2) at base material 11 surperficial alternating deposit titanium nitride layers 122 and aln layer 121.The adjusting argon flow amount is 300cm
3/ s, the feeding flow is 70～130cm
3The nitrogen of/s; Regulate titanium target and aluminium target power output and be 3000～4000w, open pivoted frame base material 11 is rotated, regulate pivoted frame speed and be 2-5r/min (rev/min), depositing time is 30～120min.
So, will be at the titanium nitride layer 122 and aln layer 121 of base material 11 surperficial alternating deposit nanometer scale, the thickness of each titanium nitride layer 122 and each aln layer 121 is between 3～15 nanometers.Wherein, be titanium nitride layer 122 with base material 11 bonded one decks.Behind titanium nitride layer 122 and aln layer 121 alternating deposits, whole bed thickness is between 1～2.5 micron.At this moment, contain TiN, Ti in this titanium nitride layer 122
2Composition such as N and unreacted Ti contains AlN, Al in this aln layer 121
2N, and composition such as unreacted Al.Plated film is closed target electric current, bias voltage, air-flow etc. after finishing, and temperature drop is to room temperature in the chamber 20 to be coated, and taking-up is formed with the titanium nitride layer 122 of alternating deposit and the base material 11 of aln layer 121.
The principle of hardness that the alternating deposit of aln layer 121 and titanium nitride layer 122 can improve ganoine thin film 12 is following: in materialogy, whether a kind of metal or alloy hardness is big, from microcosmic, depends primarily on its inner dislocation and whether be easy to slippage.In general, the slippage of dislocation causes the slippage of metal inside particle aspect, and the repeatedly slippage of dislocation is accumulated, and on macroscopic aspect, just shows as plastic deformation of metal.The material of viscous deformation takes place more easily, and its ductility is good more, and hardness is low more; Otherwise, being not easy to take place the material of viscous deformation more, its ductility is poor more, and hardness is big more.Therefore, the hardness key of material depends on the complexity of the inner dislocation generation of material slippage.In the nanometer multi-layer horniness film 12 that aln layer 121 and titanium nitride layer 122 form, the thickness of each layer all is Nano grade (being several to tens particle thicknesses) in aln layer 121 and the titanium nitride layer 122.Because the lattice parameters of titanium nitride and aluminium nitride AlN etc. are inequality, therefore on titanium nitride and aluminium nitride AlN interface, exist the mispairing of atom, and the atom mispairing is the huge obstacle of dislocation glide, can cause material hardens (being the superlattice hardening effects); In addition; Because the thickness of aln layer 121 and titanium nitride layer 122 is all very thin; Therefore its inner dislocation only needs several atoms of slippage just can reach on the interface, is stopped and is fixed at the interface by the lattice misfit, thereby cause dislocation to be difficult to slide once more; Make the hardness of material increase greatly, thereby promote the integral hardness of ganoine thin film 12 greatly.
S3: have titanium nitride layer 122 to put into heat treatment furnace surperficial alternating deposit and carry out nitrogenize thermal treatment, so that not nitrogenize or the not titanium and the complete nitrogenize of aluminium of nitrogenize fully with the base material 11 of aln layer 121.
This kind nitrogenize heat treating method is that pending lining part is put into heat treatment furnace; Feed nitrogen; Air in the heat treatment furnace is discharged; Form nitrogen atmosphere, be heated to certain temperature then after, in nitrogen and the ganoine thin film unreacted metal or unreacted completely metal continue reaction and generate standard chemical metering ratio mutually.
This nitrogenize thermal treatment practical implementation process is put into the heat treatment furnace of good seal with the base material that plated ganoine thin film 12 11, and continual feeding nitrogen is all discharged the air in the heat treatment furnace in stove, forms the atmosphere of nitrogen, begins heating.
Embodiment 1
When the ganoine thin film thickness of preparation is the 1-1.5 micron; Under heat treatment furnace and atmospheric pressure environment that ambient atmosphere is communicated with, in the heating heat treatment furnace TR between 515 to 525 degrees centigrade, (if with isolated from atmosphere; Heat treatment furnace is under the environment that has only nitrogen of sealing; Then TR is between 533 to 546 degree), heat treatment time is 5-10 minute, under this kind temperature and time; Unreacted metal or unreacted metal reaction completely generates TiN and AlN fully in nitrogen and the ganoine thin film.And this moment, atom superlattice effect was the most obvious, thereby the hardness of ganoine thin film can significantly improve.
Scope and time to thermal treatment temp in this nitrogenize heat treatment process require very high; Owing in nitridation process, be full of nitrogen in the heat treatment furnace in the cavity, under certain thermal treatment temp, (be the 500-800 degree generally, to rapid steel; To wimet is more than 700 degree) activated nitrogen atom can generate a large amount of nitride with substrate surface atom (even surperficial certain thickness is with lower area) reaction; When temperature was too high, these nitride gatherings were grown up, and form needle-like or bar-shaped fragility phase; Though cause substrate surface firmly but extremely crisp easily, and then cause declining to a great extent of surface abrasion resistance.Simultaneously, because the crystallization of base material and recrystallization temperature and heat-treatment temperature range all have overlapping, processing can cause declining to a great extent of base material mechanical property accidentally, loses more than gain.If heat-up time is long, can significantly reduce the hardness of ganoine thin film, because the further mutual diffusion of the particle meeting interface between obscuring layer and the layer gradually, thereby make superlattice effect disappearance between layer and the layer, cause the hardness of ganoine thin film to decline to a great extent.
Embodiment 2
When the ganoine thin film thickness of preparation was the 1.5-3 micron, under the atmospheric pressure environment, TR was that heat treatment time is 15-20 minute between 515 to 525 degree.Under this kind temperature and time, titanium, aluminium (are Ti completely for unreacted titanium, aluminium or unreacted in nitrogen and the ganoine thin film
2N, Al
2N etc.) reaction generates TiN and AlN fully.And this moment, atom superlattice effect was obvious, thereby the hardness of ganoine thin film can significantly improve.
Embodiment 3
When the ganoine thin film thickness of preparation was the 3-6 micron, under the atmospheric pressure environment, TR was between 515 to 525 degrees centigrade, and heat treatment time is 20-25 minute.Under this kind temperature and time, unreacted metal or unreacted metal reaction completely generates TiN and AlN fully in nitrogen and the ganoine thin film.And this moment, atom superlattice effect was obvious, thereby the hardness of ganoine thin film can significantly improve.
Close the heat treatment furnace power supply then, and continue to feed nitrogen, reduce to room temperature until furnace temperature, so, the titanium of nitrogenize or not complete nitrogenize and aluminium do not obtain said ganoine thin film 12 with complete nitrogenize, correspondingly, make said lining part 10.In this process; Because the film integral of titanium nitride layer 122 and aln layer 121 alternating deposits is than having the atom gap between each particle in thin and the film; Thereby nitrogen not only can with the titanium nitride layer 122 on top layer or the particle reaction of aln layer 121; Also can further see through the particle reaction of atom gap and other titanium nitride layers 122 or aln layer 121; So that not nitrogenize or the not titanium and the complete nitrogenize of aluminium of nitrogenize fully generate titanium nitride and aluminum nitride particle, fully with the hardness and wear resistance ability that improves ganoine thin film 12 integral body greatly.In addition, in nitridation process, the titanium nitride layer 122 of Nano grade and aln layer 121 are under higher temperature, and the mutual diffusion of trace also can take place particle, also makes titanium nitride layer 122 and the bonding force of aln layer 121 at the bonding interface place further increase.
This ganoine thin film 12 is processed by nitrogenize thermal treatment behind titanium nitride layer 122 and aln layer 121 alternating deposits and the alternating deposit; Compared to single titanium nitride layer or aln layer film; The titanium nitride layer 122 of this alternating deposit and aln layer 121 are because the superlattice hardening effect makes ganoine thin film possess higher hardness and wear resisting property; Further; Through back nitrogenize heat treatment process, improved the quality percentage composition of nitrogen element, can make the unreacted and complete nitrogenize of the incomplete metallics of nitrogenize on the film; The hardness of ganoine thin film further improves, and can bring up to 46-50GPa from 40Gpa generally.Correspondingly, the lining part 10 that possesses this ganoine thin film 12 possesses good hardness and wear resisting property.In addition; In nitridation process; Particle generation mutual diffusion between aln layer 121, titanium nitride layer 122 and the base material 11, thus make titanium nitride layer 122 and the bonding force of aln layer 121 increase greatly at the bonding surface place, and the bonding force between titanium nitride layer 122 and the base material 11 strengthens.
Claims (10)
1. ganoine thin film; Comprise the titanium nitride layer and the aln layer of alternately arranging; It is characterized in that: the quality percentage composition of titanium is at 46-46.6% in the said ganoine thin film, and the quality percentage composition of aluminium is at 25.6-26.2%, and the quality percentage composition of nitrogen is at 27.2-28.4%.
2. ganoine thin film as claimed in claim 1 is characterized in that: all between 3～15 nanometers, the integral thickness of this ganoine thin film is between 1～6 micron for the thickness of each said titanium nitride layer and each said aln layer.
3. ganoine thin film as claimed in claim 1 is characterized in that: the hardness of said ganoine thin film is between 46-50Gpa.
One kind the lining part; Comprise base material and be formed at the ganoine thin film on the base material; It is characterized in that: the quality percentage composition of titanium is at 46-46.6% in the said ganoine thin film, and the quality percentage composition of aluminium is at 25.6-26.2%, and the quality percentage composition of nitrogen is at 27.2-28.4%.
5. lining part as claimed in claim 3 is characterized in that: said base material is a rapid steel, and what contact with base material in the ganoine thin film is titanium nitride layer.
6. lining part as claimed in claim 3 is characterized in that: all between 3～15 nanometers, the integral thickness of this ganoine thin film is between 1～6 micron for the thickness of each said titanium nitride layer and each said aln layer.
7. the making method of the part that is covered may further comprise the steps:
One base material is provided;
On this base material, replace titanium nitride layer and aln layer through the sputter coating mode;
The base material that deposits titanium nitride layer and aln layer is put into heat treatment furnace carry out nitrogenize thermal treatment; On base material, make the ganoine thin film layer; The quality percentage composition of titanium is at 46-46.6% in the ganoine thin film; The quality percentage composition of aluminium is at 25.6-26.2%, and the quality percentage composition of nitrogen is at 27.2-28.4%.
8. the making method of lining part as claimed in claim 7 is characterized in that: said ganoine thin film thickness is the 1-1.5 micron, atmospheric pressure environment, and TR is between 515 to 525 degrees centigrade in the heat treatment furnace, and heat treatment time is 5-10 minute.
9. the making method of lining part as claimed in claim 7 is characterized in that: ganoine thin film thickness is the 1.5-3 micron, atmospheric pressure environment, and TR is between 515 to 525 degrees centigrade in the heat treatment furnace, heat treatment time is 15-20 minute.
10. the making method of lining part as claimed in claim 7 is characterized in that: ganoine thin film thickness is the 3-6 micron, and TR is that under the atmospheric pressure environment, heat treatment time is 20-25 minute between 515 to 525 degree.
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| CN2011100257303A CN102605367A (en) | 2011-01-24 | 2011-01-24 | Hard film, coated piece with hard film and manufacturing method of coated piece |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105463456A (en) * | 2014-09-30 | 2016-04-06 | 钴碳化钨硬质合金公司 | Multilayer structured coatings for cutting tools |
| CN111394710A (en) * | 2020-05-26 | 2020-07-10 | 阳江市金彪马实业有限公司 | Preparation process of titanium nitride coating stainless steel knife |
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| CN101671812A (en) * | 2009-09-30 | 2010-03-17 | 株洲钻石切削刀具股份有限公司 | Heat treatment method of Ti-Al-N coating on hard alloy substrate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463456A (en) * | 2014-09-30 | 2016-04-06 | 钴碳化钨硬质合金公司 | Multilayer structured coatings for cutting tools |
| CN105463456B (en) * | 2014-09-30 | 2019-08-20 | 钴碳化钨硬质合金公司 | Multilayer structured coating for cutting element |
| US10570521B2 (en) | 2014-09-30 | 2020-02-25 | Kennametal Inc. | Multilayer structured coatings for cutting tools |
| CN111394710A (en) * | 2020-05-26 | 2020-07-10 | 阳江市金彪马实业有限公司 | Preparation process of titanium nitride coating stainless steel knife |
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Application publication date: 20120725 |