CN103317157B - Surface-coated cutting tool - Google Patents
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- CN103317157B CN103317157B CN201310087419.0A CN201310087419A CN103317157B CN 103317157 B CN103317157 B CN 103317157B CN 201310087419 A CN201310087419 A CN 201310087419A CN 103317157 B CN103317157 B CN 103317157B
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- 238000005520 cutting process Methods 0.000 title claims abstract description 65
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 213
- 239000010410 layer Substances 0.000 claims abstract description 128
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- 239000011247 coating layer Substances 0.000 claims abstract description 16
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- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims description 32
- 238000000576 coating method Methods 0.000 claims description 27
- 239000011248 coating agent Substances 0.000 claims description 23
- 239000010936 titanium Substances 0.000 claims description 20
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- 239000000956 alloy Substances 0.000 claims description 8
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- 238000003754 machining Methods 0.000 abstract description 13
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- 238000000034 method Methods 0.000 description 59
- 230000008569 process Effects 0.000 description 38
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- 238000005240 physical vapour deposition Methods 0.000 description 22
- 239000000843 powder Substances 0.000 description 18
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 7
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- 239000000203 mixture Substances 0.000 description 6
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- 229910052758 niobium Inorganic materials 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910003178 Mo2C Inorganic materials 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
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- 150000004703 alkoxides Chemical group 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
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- OBROYCQXICMORW-UHFFFAOYSA-N tripropoxyalumane Chemical group [Al+3].CCC[O-].CCC[O-].CCC[O-] OBROYCQXICMORW-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Abstract
The present invention provides a kind of surface-coated cutting tool, and its hard coating layer plays the lubricity of excellence in the high rate intermittent machining of Ti alloy, rustless steel etc., resistance to collapses cutter, wearability.In the surface-coated cutting tool of the present invention, have on the tool base surface of cured layer on surface to possess and there is the average thickness of 0.2～5 μm and the higher alumina layer of flatness, this alumina layer is made up of substrate and the spheroidal structure that is dispersed in substrate, above-mentioned substrate is made up of the amorphous phase of aluminium oxide, and, above-mentioned spheroidal structure is made up of the congeries of one or both in needle-like crystalline phase and tabular crystalline phase and amorphous phase, the area ratio shared by spheroidal structure contained in the longitudinal section of alumina layer is 20～60 area %, and the radius of approximate circle is 0.02～0.5 μm, above-mentioned alumina host contains the chlorine of 1.0～10 atom %.
Description
Technical field
The present invention relates to a kind of surface-coated cutting tool, owing to its hard coating layer possesses the lubricity of excellence, resistance to collapses cutter, wearability, when thus be accordingly used in the high rate intermittent machining of Ti alloy, rustless steel etc., the most also can play the wearability of excellence.
Background technology
Conventionally, there is known realize the wearability raising of cutting element by forming, at tool base Surface coating, the hard film being made up of at least one above carbide of 4a, 5a, 6a race selected from periodic chart, nitride, carbonitride etc..
And, in hard film, alpha-type aluminum oxide layer is due to excellent heat stability, reactive relatively low and be high rigidity, therefore through frequently as by 4a, 5a, 6a race selected from above-mentioned periodic chart at least one more than carbide, the most surface layer of hard film that constitutes of nitride, carbonitride etc. is coated with and forms alpha-type aluminum oxide layer.
As the cladding forming method of alumina layer, generally use chemical vapor deposition (CVD) method, but the most known have physical vapor deposition (PVD) method, sol-gal process.
The most as Patent Document 1, propose there is following content, i.e. in order to avoid tool base, deterioration/the deformation of the characteristic of hard film, forming method as the alpha-type aluminum oxide layer at cryogenic conditions (less than 1000 DEG C), formed by the nitride using at least one element as essential component on tool base surface by physical vapor deposition (PVD) method, carbide, carbonitride, boride, nitrogen oxides, after the hard film that carbon nitrogen oxide is constituted, oxycompound layer is formed by aoxidizing this hard film, and by carrying out physical vapor deposition (PVD) on this oxycompound layer, evaporation is formed as most surface layer, based on wearability and the alumina layer of the alpha type crystal structure of excellent heat resistance, wherein, at least one element described is selected from Al and 4a race, 5a race, 6a race and Si.
Additionally, as shown in patent documentation 2, propose there is following content, i.e. in the surface-coated cutting tool being formed hard coating layer by physical vapor deposition (PVD) method evaporation, constituted the 1st layer with (Ti, Al) N shell, and constituted the 2nd layer with alumina layer (preferably γ type alumina layer).
And, as shown in patent documentation 3, propose there is following content, i.e. as the manufacture method of the alumina-coated structure with mechanical characteristic, durability, it is coated with on mother metal by sol-gal process and is non crystalline structure or the aluminium oxide of γ type by crystal structure or after the 1st alumina layer that their mixture is constituted, is coated with by sputtering and forms the 2nd alumina layer based on γ type.
Patent documentation 1: Japanese Patent Publication 2004-124246 publication
Patent documentation 2: Japanese Patent Publication 2007-75990 publication
Patent documentation 3: Japanese Patent Publication 2006-205558 publication
As hard coating layer, formed in the surface-coated cutting tool of alumina layer by CVD cladding, when Ti alloy, rustless steel etc. are carried out machining, can enumerate the raising of wearability in the rake face of coating tool, but this is especially because the heat stability of the alpha-type aluminum oxide formed, non-reacted higher.
Above-mentioned patent documentation 1 proposes to have form alpha-type aluminum oxide layer under cryogenic by physical vapor deposition (PVD) method, when but evaporation forms alumina layer, firstly the need of oxidation hard film and at its surface formation oxycompound layer, but oxycompound layer is insufficient with the adhesiveness of alumina layer, and alpha-type aluminum oxide is not only existed as aluminium oxide, there is also γ type aluminium oxide, thus failing to obtain sufficient thermostability, its result exists that cannot play in life-time service can the problem of cutting ability satisfactorily.
It addition, in above-mentioned patent documentation 2,3, there are the following problems, the aluminium oxide i.e. formed is γ type aluminium oxide, therefore lacks stability at high temperature, and cannot play gratifying cutting ability in high-speed cutting is processed.
Summary of the invention
Therefore, the present inventor etc. are for the result conducted in-depth research at the alumina layer of tool base surface formation excellent in abrasion resistance by sol-gal process, find following content: dispersed and distributed is by the needle-like crystalline phase of amorphous phase and alpha-aluminium oxide in the amorphous alumina constituting the substrate formed by sol-gal process, the congeries of tabular crystalline phase are constituted and the spheroidal structure of excellent in abrasion resistance, when thus can obtain being provided to produce high heat and have the high rate intermittent machining of intermittence/impact load to cutting edge effect, lubricity, resistance to collapse cutter, the surface-coated cutting tool that wearability is also excellent.
I.e., find following content: when preparing alumina sol, process as low temperature maturation, carry out less than the stirring at common temperature and long-term holding, thus suppression hydrolysis and the response speed of polycondensation, when closely forming the alumina precursor being bonded by Al-O, it is possible to formed more close to the octahedra AlO of corundum type structure6Therefore using this alumina sol as tool base surface layer come coated and dried, burn till, the surface layer of the hard film being made up of following alumina layer can be formed, in described alumina layer, in and lubricity higher in flatness, deposit resistance property, the resistance to substrate collapsing the excellent amorphous nickel/phosphorus/aluminium oxide of cutter, dispersed and distributed has and is made up of and the spheroidal structure of excellent in abrasion resistance the needle-like crystalline phase of amorphous phase and alpha-type aluminum oxide, the congeries of tabular crystalline phase.
Additionally, using as the hard film of the basal layer contacted with the alumina layer of surface layer be formed as shared in Al metal ingredient in this hard film nitride epithelium that content ratio is 40 more than atom % time, uprise with the adhesion strength of the alumina layer of surface layer, therefore in the viewpoints such as the stripping of alumina layer suppressing the impact etc. during generation machining to cause, defect preferably.
I.e., find following content: in the surface-coated cutting tool of the present invention, the surface layer of hard coating layer is constituted with alumina layer, and this alumina layer is by flatness, lubricity, deposit resistance property, the resistance to substrate collapsing the excellent amorphous nickel/phosphorus/aluminium oxide of cutter and dispersed and distributed are in this substrate and the spheroidal structure of excellent in abrasion resistance is constituted, therefore possesses the surface-coated cutting tool of this hard coating layer for Ti alloy, when producing high heat and cutting edge effect had the high rate intermittent machining of intermittence/impact high load capacity of rustless steel etc., the most also the wearability of excellence can be played.
The present invention completes based on above-mentioned opinion, it is characterised in that
(1) a kind of surface-coated cutting tool, it forms hard coating layer at the tool base Surface coating being made up of tungsten carbide base carbide alloy or base titanium carbonitride and forms, it is characterised in that
A (), as the surface layer of above-mentioned hard coating layer, possesses the alumina layer of the average thickness with 0.2～5 μm,
B () above-mentioned alumina layer is made up of substrate and the spheroidal structure that is dispersed in substrate,
C () above-mentioned substrate is made up of the amorphous phase of aluminium oxide, and above-mentioned spheroidal structure is made up of the congeries of one or both in needle-like crystalline phase and tabular crystalline phase and amorphous phase.
(2) surface-coated cutting tool as described in described (1), it is characterised in that
The area ratio shared by spheroidal structure contained in the longitudinal section of above-mentioned alumina layer is 20～60 area %.
(3) surface-coated cutting tool as described in described (1) or (2), it is characterised in that
The radius of the approximate circle of above-mentioned spheroidal structure is 0.02～0.5 μm.
(4) surface-coated cutting tool as described in described (1), it is characterised in that
Above-mentioned alumina layer substrate contains the chlorine of 1.0～10 atom %.
(5) described surface-coated cutting tool described in (1), it forms hard coating layer at the Surface coating of the tool base being made up of tungsten carbide base carbide alloy and forms, it is characterised in that
The matrix surface cured layer of the average thickness with 0.5～3.0 μm it is formed with to depth direction, as the average content of Co of the combination phase metal being contained in this matrix surface cured layer less than 2.0 mass % from the surface of above-mentioned tool base.
(6) described surface-coated cutting tool described in (1), it forms hard coating layer at the Surface coating of the tool base being made up of tungsten carbide base carbide alloy and forms, it is characterised in that
The matrix surface cured layer of the average thickness with 0.5～3.0 μm it is formed with to depth direction, as the total average content of Co and Ni of the combination phase metal being contained in this matrix surface cured layer less than 2.0 mass % from the surface of above-mentioned cermet tool matrix.
Surface-coated cutting tool according to the present invention, it is to form the instrument by the aluminium oxide of sol-gal process film forming at tool base Surface coating, but the above-mentioned alumina layer formed possesses the surface smoothness of excellence, lubricity, deposit resistance property, resistance to collapses cutter, when cutting edge effect being had in the high rate intermittent machining of the Ti alloy of intermittence/impact load, rustless steel etc. while therefore using it for producing high heat, also will not produce and collapse the Abnormal damage such as cutter, stripping and play the wearability of excellence by long-term use.
Accompanying drawing explanation
Fig. 1 is the macrograph representing the longitudinal section with the alumina layer of tem observation inventive article 2.
Fig. 2 is the macrograph in the cross section representing the alumina layer observing inventive article 2 with SEM.
Fig. 3 is the macrograph on the surface representing the alumina layer observing inventive article 2 with SEM.
Detailed description of the invention
Hereinafter, the present invention is described in detail.
In the surface-coated cutting tool of the present invention, surface layer as hard coating layer possesses the alumina layer of by sol-gal process film forming 0.2～5.0 μm, if but the thickness of alumina layer is less than 0.2 μm, the generation negligible amounts of annular tissue the most described later, therefore sufficient wearability cannot be played, on the other hand, if thickness is more than 5.0 μm, then it is easily generated the stripping of layer, therefore the thickness of alumina layer is set to 0.2～5.0 μm.
Additionally, above-mentioned alumina layer can play its performance by direct formation of film at surface in tool base, but using comprise titanium carbonitride hard alloy as matrix time, by burning till in blanket of nitrogen, at the more carbonitride higher containing at least one wearability in Ti, Ta, Nb, Zr of tool base near surface, thus form matrix surface cured layer, and improve the adhesion strength of alumina layer and tool base, it is possible to extend life tools.Additionally, it is preferred that this matrix surface cured layer formed after the hardness of hard alloy substrate with Vickers hardness (Hv) more than 2200 and less than 2800.Now, by more containing carbonitride, Co near matrix surface can reduce relatively, scanning electron microscope (SEM) is such as utilized to carry out the cross-section of 0.5～3.0 μm to depth direction from surface, when detecting the content as the Co combining phase metal by quantitative analysis based on wavelength-dispersion type x-ray spectrometry in the range of analysis field of view 1 × 1 μm, if the content of Co is less than 2.0 mass %, then it is sufficiently formed the carbonitride of the main cause of the surface cure becoming matrix, and wearability is further enhanced.
Additionally, during using base titanium carbonitride as matrix, atmosphere when heating up and keep in maximum temperature in sintering circuit is set to predetermined blanket of nitrogen, and reduce pressure when the midway kept or cooling, thus compared with when the blanket of nitrogen of constant pressure is implemented full sintering circuit, it is possible to make surface more solidify.This is because, if implementing the operation till keeping with maximum temperature under constant nitrogen pressure, then it is uniformly dispersed forming the carbonitride that hardness is higher at intrinsic silicon, on the other hand, if processing under higher nitrogen pressure before the midway heated up or keep, start the blanket of nitrogen being set to be further depressurized processes when the midway kept or cooling, then only has the most surface of matrix by denitrogenation, thus Ti or Nb etc. to the dissolving of Ni or Co metal bound phase and come to life from inside to the diffusion of matrix surface, the formation of the carbonitrides such as Ti or Nb is promoted on surface, thus form matrix surface cured layer.Additionally, it is preferred that this matrix surface cured layer formed after the hardness of metal-ceramic matrix with Vickers hardness (Hv) more than 2000 and less than 2600.And, now identical with above-mentioned hard substrate, Ni and Co near matrix surface can reduce relatively, if the content as Ni and Co combining phase metal is set to less than 2.0 mass %, then it is sufficiently formed the carbonitride of the main cause of the surface cure becoming matrix, and wearability is further enhanced.
Additionally, in the surface-coated cutting tool of the present invention, above-mentioned alumina layer can not be directly formed on the surface of tool base, but form hard film well known by persons skilled in the art by physical vapor deposition (PVD) method, chemical vapor deposition (CVD) method or sol-gal process, the hard film more than at least one of which being i.e. made up of the nitride containing at least one the above element selected from 4a, 5a, 6a race of periodic chart and Si or oxide, the Surface coating at this hard film forms above-mentioned alumina layer afterwards.
Additionally, when forming hard film by above-mentioned physical vapor deposition (PVD) method, for the hard film contacted with alumina layer, from the viewpoint of improving adhesiveness, it is preferably formed in this hard film the nitride epithelium (such as, TiAlN film, CrAlN film etc.) that content ratio be 40 atom %s more than shared in the metal ingredient of this hard film containing Al and Al.
This is because, if the nitride epithelium that content ratio is 40 more than atom % shared in the metal ingredient that Al is in hard film, then form, with the interface of aluminium oxide epithelium, the oxide that alumina concentration is higher at nitride epithelium, and this oxide becomes have the effect making nitride epithelium and aluminium oxide epithelium firmly adhere.
Constitute the alumina layer of surface layer of the surface-coated cutting tool of the present invention by sol-gal process film forming described later, thus its substrate is made up of amorphous nickel/phosphorus/aluminium oxide, and forms the spheroidal structure being made up of the congeries of amorphous phase and needle-like crystalline phase, tabular crystalline phase in this substrate.
When utilizing scanning electron microscope (SEM) to observe alumina layer, as shown in Figure 1, Figure 2, Figure 3 shows, above-mentioned spheroidal structure is viewed as the spherical congeries tissue of radius 0.02～0.5 μm, if additionally further looking at this spheroidal structure with transmission electron microscope (TEM), then understand it and be formed as amorphous phase and needle-like crystalline phase, the congeries tissue of tabular crystalline phase.
And, if such as observing longitudinal section by SEM in the range of field of view 5 × 7 μm to obtain the area ratio that this spheroidal structure is shared in alumina layer, it is known that account for 20～60 area %.
It addition, can be observed to be formed with recess (white rings part in Fig. 1) at the interface of spheroidal structure with the aluminium oxide as substrate in the way of cincture spheroidal structure according to Fig. 1.
The shape of spheroidal structure is exactly the complex tissue of the most various each directions arrangement originally, and therefore isotropism aspect is relatively strong, according to its stress dispersion effect, also contributes to stable wearability in the heavy cut applying high load capacity.If the area ratio shared by the above-mentioned spheroidal structure contained in the longitudinal section of alumina layer is more than 60 area %, the ratio of the substrate then fixing spheroidal structure tails off, therefore embrittlement tendency occurs in alumina layer, and the ratio around the recess (with reference to Fig. 1) of spheroidal structure becomes big, the load uneven to layer effect when machining, destroys it is therefore possible to produce.On the other hand, when area ratio is less than 20 area %, the spheroidal structure being favorably improved wearability is less, and therefore the wearability of alumina layer reduces.
Therefore, in the present invention, the area ratio that spheroidal structure is shared in alumina layer is set to 20～60 area %.
During using the radius of above-mentioned spheroidal structure as the radius of the circle of the area equation area having with this spheroidal structure to obtain, if radius is less than 0.02 μm, then the raising of the wearability in alumina layer effect is less, on the other hand, if radius is more than 0.5 μm, become thick tissue, the most easily become the starting point of be full of cracks and cause the resistance to reduction collapsing cutter.
Therefore, above-mentioned spheroidal structure is dimensioned to radius 0.02～0.5 μm.
The alumina layer of the surface layer constituting the surface-coated cutting tool of the present invention can be formed by sol-gal process described below.
The preparation of alumina sol:
By forming alumina sol as follows, first, at aluminium-alcohol salt (such as, aluminium secondary butylate, Aluminum tripropoxide) middle interpolation alcohol is (such as, ethanol, n-butyl alcohol), after further adding (alpha alumina particle of mean diameter 10～300nm can be added) acid (such as, hydrochloric acid, nitric acid), within the scope of the temperature less than 15～30 DEG C, it is stirred and carries out the maturation process of more than 12 hours simultaneously.
During it addition, add alcohol, in order to improve by promoting that the nucleus when forming alumina layer generates the film formation at low temp and crystallinity realized, from making uniform colloidal sol viewpoint, preferably add the alcohol in advance containing the alpha alumina particle that mean diameter is 10～300nm.Additionally, this is because have the effect that, i.e. when coating, alpha alumina particle becomes the core of the starting point becoming crystal growth, and as center spherical gathering organization of favorable dispersibility landform uniformly diameter in alumina layer, but when adding the alcohol containing alpha alumina particle, if the mean diameter of alpha alumina particle is less than 10nm, then it is not up to the critical nucleus size of the starting point that can become crystal growth, thus without producing the crystal growth from the alumina sol around alpha alumina particle, cause isolating from substrate, the position that the adhesion of crystal grain with surrounding is more weak is easily become after burning till.On the other hand, if mean diameter is more than 300nm, then the nucleus with alpha alumina particle as starting point excessively grows into oversize grain, causes defect in the reduction of film hardness and film, therefore the mean diameter of the alpha alumina particle added is set to 10～300nm.
Additionally, if the alpha alumina particle content in alcohol relative to the alkoxide of aluminium oxide less than 0.5 mass %, then cannot meet in order in film more than certain density to be uniformly distributed the karyogenesis number needed for nucleus, cause the crystallinity in film uneven according to position, therefore easily cause inordinate wear when cutting.If relative to aluminium-alcohol salt more than 5 mass %, in alumina sol, then it is easily generated the cohesion of alpha alumina particle, when forming alumina layer, this cohesion portion is formed as the oversize grain in film, cause defect in film, the most preferably the addition of alpha alumina particle is set to relative to aluminium-alcohol salt the scope of 0.5～5 mass %.
Additionally, it is preferred that the concentration of the acid added is 0.01～1.0N, preferred acid is 0.1～2 times (capacity) relative to the addition of alcohol.
Additionally, when adding hydrochloric acid as acid, the alumina host ultimately formed is mixed into and residual chlorine, but the metal reactions such as chlorine and ferrum also form the chloride that lubricity is higher, thus contributing to the raising of the lubricity of alumina layer, deposit resistance property in result, therefore the concentration as the chlorine in alumina layer allows the scope containing 1.0～10 atom %.
In the preparation of the alumina sol generally carried out, carry out the stirring at 40～80 DEG C and the maturation about a few hours under this whipping temp processes, but in the present invention, carry out the stirring in the temperature range of 15～30 DEG C and such as process through the long low temperature maturation up to more than 12 hours.
Wherein, if temperature when stirring and holding is more than 30 DEG C, then hydrolysis and polycondensation reaction can be carried out, rapidly thus without closely forming presoma, and alpha-aluminium oxide will not be formed in as the firing process of subsequent handling, therefore temperature upper limit when stirring and holding is set to 30 DEG C.On the other hand, if temperature when stirring and holding is less than 15 DEG C, then can form multiple Al-O joint portion closely constructed in alumina sol in heterogeneity, but in order to form the spheroidal structure of the size with the present invention, in alumina sol, preferably form minority close Al-O joint portion locally.Therefore, the temperature by stirring and when keeping be set to easily locally to be hydrolyzed, the cryogenic temperature scope of 15～30 DEG C of polycondensation reaction.
It addition, be set to the maturation time, up to more than 12 hours be because for a long time, the most slowly promote hydrolysis, the most closely generate alumina precursor.
Be dried/burn till:
The alumina sol of above-mentioned middle preparation is coated directly onto the surface of tool base or is coated on the hard film surface as the basal layer being formed at tool base surface by physical vapor deposition (PVD) method, then be repeated more than 1 time at 100～300 DEG C, the preferably dried at 150～200 DEG C, then, carrying out burning till process in the temperature range of 400～650 DEG C, thus cladding forms alumina layer.
The dry colloidal sol of aluminium oxide is formed by above-mentioned dried, process is burnt till by then carry out, form the amorphous phase of aluminium oxide as substrate on hard film surface, in substrate, dispersed and distributed forms the spheroidal structure being made up of the congeries of amorphous phase and needle-like crystalline phase, tabular crystalline phase simultaneously.
The thickness of above-mentioned alumina layer depends on coating thickness and the application frequency of alumina sol, if but the thickness of the above-mentioned alumina layer of cladding formation is less than 0.2 μm, then cannot play the superior abrasion resistance as surface-coated cutting tool by long-term use, on the other hand, if thickness is more than 5.0 μm, then alumina layer is easily generated stripping, and therefore the thickness of above-mentioned alumina layer is set to 0.2～5.0 μm.
It addition, the temperature range of dried is set to 100～300 DEG C, more preferably it is set to 150～200 DEG C, and the temperature range burning till process is set to 400～650 DEG C.About baking temperature, if being because less than 100 DEG C, cannot be carried out fully being dried, if more than 300 DEG C, the volume contraction of colloidal sol drastically carries out and produces be full of cracks etc., and epithelium is easily generated stripping etc..About firing temperature, if being because less than 400 DEG C, crystallinity spheroidal structure effective to interrupted cut cannot be formed, it is the most resistance to that to collapse cutter insufficient, on the other hand, when burning till with the temperature more than 650 DEG C, the coarsening of spheroidal structure and the crystallization of substrate are carried out further, and therefore flatness, lubricity, deposit resistance property display reduce tendency.
[embodiment 1]
Then, by embodiment, the present invention is specifically described.
(a1) as material powder, prepare the microgranule WC powder of mean diameter 0.8 μm, the middle grain WC powder of mean diameter 2～3 μm, be respectively provided with the TiCN powder of the mean diameter of 1～3 μm, ZrC powder, TaC powder, NbC powder, Cr3C2Powder and Co powder, these material powders are fitted in the predetermined cooperation composition shown in table 1, addition paraffin in acetone ball milling mixing 24 hours further, after drying under reduced pressure, pressed compact with the pressure punch forming of 98MPa as reservation shape, and with 1400 DEG C of conditions kept 1 hour, this pressed compact is carried out vacuum-sintering in the vacuum of 5Pa, after sintering, cutting portion is imposed the cutting edge reconditioning processing of R:0.05mm, thus manufacture and there is WC base cemented carbide tool base A of the blade shapes of regulation in ISO CNMG120408, B, C, D, E (referred to as hard substrate A, B, C, D, E).Wherein, for hard substrate D, the blanket of nitrogen of 3.3kPa being carried out with 1400 DEG C of coolings kept after 1 hour to 1320 DEG C, for hard substrate E, the blanket of nitrogen of 2kPa being carried out with 1400 DEG C of coolings kept after 1 hour to 1320 DEG C, thus matrix surface is carried out cured.
(b1) then, above-mentioned hard substrate A is loaded chemical evaporation plating device, the membrance casting condition shown in table 2 is utilized to be pre-formed the Ti compound layer being made up of the TiCN layer (following, to represent) of the TiN layer and longitudinal growth crystalline structure possessing the granular crystal tissue with the thickness shown in table 4 with l-TiCN as basal layer.Further, for above-mentioned hard substrate B, it is also loaded onto the arc ion plating apparatus of one of physical vapor deposition device, as basal layer, is formed the Ti of thickness 2.0 μm as shown in Table 4 by physical vapor deposition cladding0.5Al0.5N shell or Al0.7Cr0.3The hard film that N shell is constituted.It addition, for above-mentioned hard substrate C, D, E, special Surface coating is not carried out and processes.
(c1) on the other hand, the most surface at hard film is carried out as follows the preparation of the alumina sol for being formed alumina layer by sol-gal process cladding.
In the aluminium-alcohol salt i.e. aluminium secondary butylate of the scheduled volume shown in table 3, add the ethanol of the scheduled volume being also illustrated in table 3 as alcohol, be stirred at 20 DEG C in temperature chamber, and by the hydrochloric acid adding the water being added with scheduled volume that dripped down through 1 hour.
(d1) when it being remained 20 DEG C the most like that in temperature chamber, continuously stirred more than 12 hours, and process 24 hours with 20 DEG C of low temperature maturations, thus prepare alumina sol.
Become such a way with final solution composition with mol ratio to be adjusted.
(aluminium secondary butylate): (water): (ethanol): (hydrochloric acid)=1:(80～120): 20:(0.1～1)
(e1) then, above-mentioned alumina sol is coated on by being formed at the described Ti compound layer of above-mentioned hard substrate A by chemical vapor deposition method, being formed at the Ti of above-mentioned hard substrate B by physical vapor deposition0.5Al0.5N shell, Al0.7Cr0.3N shell constitute hard film on and be not carried out special Surface coating process hard substrate C, D on.
(f1) then, the above-mentioned alumina sol having been coated with is carried out the dried of the predetermined condition shown in table 3, and after coating being repeated and being dried, in an atmosphere with 600 DEG C carry out 1 hour burn till process, the alumina layer of the present invention is formed (i.e. in most surface cladding, in the substrate being made up of mutually amorphous nickel/phosphorus/aluminium oxide, dispersed and distributed has by amorphous phase and needle-like crystalline phase, the alumina layer of the spheroidal structure that the congeries of tabular crystalline phase are constituted), thus manufacture the surface-coated cutting tool 1 of the present invention, 2, 3, 4, 5 (referred to as inventive article 1, 2, 3, 4, 5).
For the invention described above instrument 1～5, can confirm that by the result of the longitudinal section of scanning electron microscope (SEM) observation alumina layer, its substrate is made up of amorphous phase, on the other hand, dispersed and distributed spheroidal structure in substrate is made up of the congeries of one or both in needle-like crystalline phase and tabular crystalline phase and amorphous phase.Confirmation for amorphous phase utilizes transmission electron microscope (TEM) to analyze the result of its substrate and spheroidal structure respectively by SEAD method, its substrate obtains dizzy master drawing case, and spheroidal structure obtains electric wire diffraction pattern and dizzy master drawing case clearly.
As the longitudinal section TEM photo of an alumina layer exemplifying inventive article 2 in Fig. 1, Fig. 2 and Fig. 3 additionally illustrates to this inventive article 2 surface and the cross section SEM photograph of its alumina layer.Can confirm that according to Fig. 2, Fig. 3, the spheroidal structure being scattered in amorphous oxide aluminium lamination is made up of the congeries of amorphous phase and needle-like crystalline phase, tabular crystalline phase.
For the invention described above instrument 1～5, spheroidal structure area ratio shared in the longitudinal section of alumina layer and the mean radius of spheroidal structure is observed with the visual field of 50,000 times by scanning electron microscope, for its result, it is assumed to be plane and carrys out 5 area ratios measuring spheroidal structure, and 5 measure using the area of this spheroidal structure as the area of a circle calculate time the radius of approximate circle, and be averaged value as average-size.
Additionally, content about the Co being mixed into the cl concn remained in alumina layer substrate and hard substrate surface, by in the observation visual field, longitudinal section of the wavelength-dispersion type X-ray spectrum quantitative analysis alumina layer or hard substrate that utilize scanning electron microscope (SEM), and use its meansigma methods.Cl concn point analysis in alumina layer substrate carries out 5 mensuration, and the Co content on hard substrate surface utilizes and carries out 5 visual field mensuration from substrate surface to the surface analysis of analysis field of view 1 × 1 μm in the range of depth direction 0.5～3.0 μm.
It addition, utilize the result of the average thickness of scanning electron microscope cross-section determination alumina layer simultaneously, all show actually identical with target thickness meansigma methods (meansigma methodss at 5).
Measurement result shown in table 4.
[comparative example 1]
In order to compare, manufacture surface-coated cutting tool by following manufacture method.
I.e. for tool base A, B, C, D, the E of described (a1), form hard film by the operation of described (b1), and prepare alumina sol by the operation (reference table 3) of described (c1).
(it addition, do not carry out the formation of the hard film according to described (b1) operation for tool base C, D, E.)
Then, replace the operation of described (d1), in temperature chamber, remain when 40 DEG C continuously stirred 12 hours, and maturation 24 hours at 40 DEG C, thus prepare alumina sol.
Then, in the same manner as described (e1), above-mentioned alumina sol is coated on and is formed from the Ti of hard substrate A, B0.5Al0.5N shell, Al0.7Cr0.3N shell constitute hard film on and be not carried out special Surface coating process hard substrate C, D, E on.
Then, in the same manner as described (f1), the above-mentioned alumina sol having been coated with is dried process, and after coating and dried are repeated, in an atmosphere with 600 DEG C carry out 1 hour burn till process, form alumina layer in most surface cladding, thus manufacture the surface-coated cutting tool 1,2,3,4,5,6 (referred to as comparative example instrument 1,2,3,4,5,6) of comparative example.
[embodiment 2]
For reference, manufacture surface-coated cutting tool by following manufacture method.
That is, for tool base A, the B of described (a1), formed by the operation of described (b1) and (it addition, for tool base C, D, E, do not carry out the formation of hard film according to described (b1) operation.) hard film, prepare solution composition by the operation (reference table 3) of described (c1) and be different from the alumina sol of embodiment 1, by the operation of described (e1), the colloidal sol being implemented low temperature maturation process by the operation (reference table 3) of described (d1) is respectively coated on hard substrate A, B, C, D, E.
Then, in the same manner as described (f1), the above-mentioned alumina sol having been coated with is dried process, and after coating and dried are repeated, in an atmosphere with 600 DEG C carry out 1 hour burn till process, form alumina layer at Surface coating, thus manufacture the surface-coated cutting tool 6～17 (referred to as inventive article 6～17) of the present invention.
For above-mentioned comparative example instrument 1～6, inventive article 6～17, the results verification utilizing scanning electron microscope (SEM) and transmission electron microscope (TEM) to observe alumina layer arrives, comparative example instrument has the membrane tissue without spheroidal structure, inventive article 6～17 has a spheroidal structure, but for having the spheroidal structure size different from inventive article 1～5, area occupation ratio, the membrane tissue of concentration of residual chlorine.And confirm, spheroidal structure is made up of the congeries of amorphous phase and needle-like crystalline phase, tabular crystalline phase.
For the invention described above instrument 6～17, spheroidal structure area ratio shared in the longitudinal section of alumina layer and the mean radius of spheroidal structure is observed with the visual field of 50,000 times by scanning electron microscope, for its result, it is assumed to be plane and carrys out 5 area ratios measuring spheroidal structure, and 5 measure using the area of this spheroidal structure as the area of a circle calculate time the radius of approximate circle, and be averaged value as average-size.
Measurement result shown in table 4.
Then, for the invention described above instrument 1～17 and comparative example instrument 1～6, the wet type high rate intermittent machining test of Ti alloy is carried out with following condition.
After carrying out wet type high rate intermittent machining test (common cutting speed is respectively 80m/min.) with following condition, the state of wear of each instrument is observed, and measures tool flank wear.
Workpiece: on the length direction of Ti-6Al-4V alloy (HB250) be formed at equal intervals 4 pods pole,
Cutting speed: 120m/min.,
Cutting depth: 1.5mm,
Feed speed: 0.22mm/rev.,
Cutting time: 5 minutes.
The results are shown in table 4.
[table 1]
[table 2]
[table 3]
[table 4]
[embodiment 3]
(a2) as material powder, prepare to be respectively provided with TiCN (with mass ratio as the TiC/TiN=50/50) powder of mean diameter of 0.5～2 μm, Mo2C powder, NbC powder, TaC powder, WC powder, Co powder and Ni powder, these are fitted in the predetermined cooperation composition shown in table 5, 24 hours wet mixed are carried out with ball milling, with the pressure punch forming of 98MPa as pressed compact after being dried, with temperature in the blanket of nitrogen of 1.3kPa: this pressed compact is sintered by 1540 DEG C of conditions kept 1 hour, after sintering, blade part is given and process with the cutting edge reconditioning of R:0.07mm, thus manufacture TiCN based ceramic metal tool base F of the blade shapes with iso standard CNMG120408, G, H, I, J (referred to as metal-ceramic matrix F, G, H, I, J).Wherein, for tool base I, in the blanket of nitrogen of 1.3kPa, will heat up speed and be set to 2 DEG C/min, from room temperature to 1540 DEG C the vacuum that is set to 13Pa after keeping 30 minutes, and lower the temperature and carry out surface cure after keeping 30 minutes with 1540 DEG C.For tool base J, nitrogen pressure during sintering is set to different from tool base I, is set to constant carry out surface cure in the blanket of nitrogen of 13Pa.
(b2) then, above-mentioned hard substrate F is loaded chemical evaporation plating device, as basal layer, the membrance casting condition shown in table 2 is utilized to be pre-formed the Ti compound layer being made up of the l-TiCN layer of the TiN layer possessing the granular crystal tissue with the thickness shown in table 7 and longitudinal growth crystalline structure.It addition, for above-mentioned hard substrate G, be also loaded onto the arc ion plating apparatus of one of physical vapor deposition device, as basal layer, formed the Ti of thickness 2.0 μm as shown in Table 7 by physical vapor deposition cladding0.5Al0.5N shell or Al0.7Cr0.3The hard film that N shell is constituted.
(c2) on the other hand, the most surface at hard film is carried out as follows the preparation of the alumina sol for being formed alumina layer by sol-gal process cladding.
In the aluminium-alcohol salt i.e. aluminum isopropylate. of the scheduled volume shown in table 6, the n-butyl alcohol of the scheduled volume of the alpha alumina particle containing the predetermined mean particle diameter shown in table 6 is added as alcohol, temperature chamber is stirred at 20 DEG C, and by the water-reducible nitric acid of the interpolation scheduled volume that dripped down through 1 hour.
(d2) when it being remained 20 DEG C in temperature chamber, continuously stirred 12 hours, and at 20 DEG C, low temperature maturation processes 24 hours, thus prepares alumina sol.
It addition, the amount of the water made an addition in this colloidal sol is 1:(80～120 relative to the ratio of the aluminium oxide being contained in alumina sol in above-mentioned).
(e2) then, above-mentioned alumina sol is coated on by being formed at the described Ti compound layer of above-mentioned metal-ceramic matrix F by chemical vapor deposition method, being formed at the Ti of above-mentioned metal-ceramic matrix G by physical vapor deposition0.5Al0.5N shell, Al0.7Cr0.3N shell constitute hard film on and be not carried out special Surface coating process metal-ceramic matrix H, I on.
(f2) then, to the above-mentioned alumina sol having been coated with, carry out the dried of the predetermined condition shown in table 6, and after coating being repeated and being dried, in an atmosphere with 600 DEG C carry out 1 hour burn till process, the alumina layer of the present invention is formed (i.e. at Surface coating, in the substrate being made up of mutually amorphous nickel/phosphorus/aluminium oxide, dispersed and distributed has the alumina layer of the spheroidal structure being made up of the congeries of amorphous phase and needle-like crystalline phase, tabular crystalline phase), thus manufacture the surface-coated cutting tool 18～22 (referred to as inventive article 18～22) of the present invention.
For the invention described above instrument 18～22, arrived by the results verification of the longitudinal section of scanning electron microscope (SEM) observation alumina layer, its substrate is made up of mutually amorphous nickel/phosphorus/aluminium oxide, on the other hand, dispersed and distributed spheroidal structure in substrate is made up of the congeries of amorphous phase and needle-like crystalline phase, tabular crystalline phase.
For the invention described above instrument 18～22, spheroidal structure area ratio shared in the longitudinal section of alumina layer and the mean radius of spheroidal structure is observed with the visual field of 50,000 times by scanning electron microscope, for its result, it is assumed to be plane and carrys out 5 area ratios measuring spheroidal structure, and 5 measure using the area of this spheroidal structure as the area of a circle calculate time the radius of approximate circle, and be averaged value as average-size.
Measurement result shown in table 7.
[comparative example 2]
In order to compare, above-mentioned tool base F, G, H, I, J is utilized to manufacture the surface-coated cutting tool 7～12 (referred to as comparative example instrument 7～12) of comparative example.
That is, on metal-ceramic matrix F, form Ti compound layer by the operation of above-mentioned (b2), metal-ceramic matrix G is formed Ti0.5Al0.5N shell and Al0.7Cr0.3N shell, prepares alumina sol by the operation of above-mentioned (c2).
Then, in the operation of described (d2), temperature chamber remains 40 DEG C, continuously stirred 12 hours, and with 40 DEG C of maturations 24 hours, thus prepare alumina sol.
Then, above-mentioned alumina sol is coated on be formed on the hard film of metal-ceramic matrix F, G and be not carried out special Surface coating process metal-ceramic matrix H, I, J.
Then, in the same manner as above-mentioned (f2), the above-mentioned alumina sol having been coated with is dried process, and after coating and dried are repeated, in an atmosphere with 600 DEG C carry out 1 hour burn till process, form alumina layer in most surface cladding, thus manufacture the surface-coated cutting tool 7～12 (referred to as comparative example instrument 7～12) of comparative example.
[embodiment 4]
For reference, manufacture surface-coated cutting tool by following manufacture method.
I.e., tool base F, G, H, I, J for described (a2), hard film is formed by the operation of described (b2), prepare solution composition by the operation of described (c2) and be different from the alumina sol of embodiment 3, by the operation of described (e2), the colloidal sol being implemented low temperature maturation process by the operation of described (d2) is coated on tool base F, G, H, I, J.
Then, in the same manner as described (f2), the above-mentioned alumina sol having been coated with is dried process, and after coating and dried are repeated, in an atmosphere with 600 DEG C carry out 1 hour burn till process, form alumina layer in most surface cladding, thus manufacture the surface-coated cutting tool 23～28 (referred to as inventive article 23～28) of the present invention.
For above-mentioned comparative example instrument 7～12, the invention described above instrument 23～28, the results verification observing alumina layer with scanning electron microscope (SEM) and transmission electron microscope (TEM) arrives, comparative example instrument is the membrane tissue without spheroidal structure, inventive article 23～28 is containing spheroidal structure, but is different from the spheroidal structure size of inventive article 18～22, area occupation ratio, the membrane tissue of concentration of residual chlorine for having.
For the invention described above instrument 23～28, spheroidal structure area ratio shared in the longitudinal section of alumina layer and the mean radius of spheroidal structure is observed with the visual field of 50,000 times by scanning electron microscope, for its result, it is assumed to be plane and carrys out 5 area ratios measuring spheroidal structure, and 5 measure using the area of this spheroidal structure as the area of a circle calculate time the radius of approximate circle, and be averaged value as average-size.Measurement result shown in table 7.
Then, to the invention described above instrument 18～28 and comparative example instrument 7～12, the test of stainless wet type high rate intermittent machining is carried out with following condition.
After carrying out wet type high rate intermittent cutting test (common cutting speed is as 100m/min) with following condition, the state of wear of each instrument is observed, and measures tool flank wear.
Workpiece: on the length direction of JIS SUS304 be formed at equal intervals 4 pods pole,
Cutting speed: 160m/min,
Cutting depth: 1.2mm,
Feed speed: 0.22mm/rev.,
Cutting time: 5 minutes.
[table 5]
[table 6]
[table 7]
Knowable to the result shown in table 4,7, in the surface-coated cutting tool 1～5,18～22 of the present invention, it is formed with aluminium oxide at tool base Surface coating by sol-gal process, this alumina layer possesses the surface smoothness of excellence, lubricity, deposit resistance property, when therefore using it in the high rate intermittent machining of Ti alloy, rustless steel etc., also will not produce and collapse the Abnormal damage such as cutter, stripping, and play the wearability of excellence, chip discharge by long-term use.
On the other hand, it is clear that the surface-coated cutting tool 1～12 of the comparative example not containing spheroidal structure in the alumina layer on surface and be only made up of matrix organization, the greater impact of interrupted cut cannot be born, it is particularly susceptible produce near cutting edge reconditioning portion small and collapses cutter, and owing to being only made up of amorphous phase, therefore high temperature hardness is insufficient, due to the bigger heating produced during high-speed cutting, crescent hollow abrasion degree is deepened, and arrives service life at short notice.
And, inventive article 6～17,23～28 contains crystallinity spheroidal structure in the alumina layer on surface, therefore the carrying out of crescent hollow abrasion drastically is not found, but the be full of cracks caused due to size or the recess of spheroidal structure, produce near cutting edge reconditioning portion sometimes small collapses cutter or owing to not having the surface solidified layer of tool base to cause wear of the tool flank degree to deepen, but compared with the surface-coated cutting tool 1～12 of comparative example, the wearability that display is excellent, can say that life tools obtain long lifetime.
It addition, in described embodiment, utilize the instrument of blade shapes to have rated the performance of hard coating layer, but certainly also can get same result with drill bit, slotting cutter etc..
Industrial applicability
Surface-coated cutting tool according to the present invention, it is formed with aluminium oxide at Surface coating by sol-gal process, this alumina layer possesses the surface smoothness of excellence, lubricity, deposit resistance property, resistance to collapses cutter, when therefore using it for the high rate intermittent machining of Ti alloy, rustless steel etc., also will not produce and collapse the Abnormal damage such as cutter, stripping, and play wearability and the chip discharge of excellence by long-term use, it is possible to the long lifetime in implementation tool life-span, the effect used is bigger.
Claims (6)
1. a surface-coated cutting tool, it forms hard coating layer at the Surface coating of the tool base being made up of tungsten carbide base carbide alloy or base titanium carbonitride and forms, it is characterised in that
A (), as the surface layer of above-mentioned hard coating layer, possesses the alumina layer of the average thickness with 0.2～5 μm,
B () above-mentioned alumina layer is made up of substrate and the spheroidal structure that is dispersed in substrate,
C () above-mentioned substrate is made up of the amorphous phase of aluminium oxide, and above-mentioned spheroidal structure is made up of the congeries of one or both in needle-like crystalline phase and tabular crystalline phase and amorphous phase.
Surface-coated cutting tool the most according to claim 1, it is characterised in that
The area ratio shared by spheroidal structure contained in the longitudinal section of above-mentioned alumina layer is 20～60 area %.
Surface-coated cutting tool the most according to claim 1 and 2, it is characterised in that
The radius of the approximate circle of above-mentioned spheroidal structure is 0.02～0.5 μm.
Surface-coated cutting tool the most according to claim 1, it is characterised in that
Above-mentioned alumina layer substrate contains the chlorine of 1.0～10 atom %.
Surface-coated cutting tool the most according to claim 1, it forms hard coating layer at the Surface coating of the tool base being made up of tungsten carbide base carbide alloy and forms, it is characterised in that
The matrix surface cured layer of the average thickness with 0.5～3.0 μm is defined to depth direction, as the average content of Co of the combination phase metal being contained in this matrix surface cured layer less than 2.0 mass % from the surface of above-mentioned tool base.
Surface-coated cutting tool the most according to claim 1, it forms hard coating layer at the Surface coating of the tool base being made up of base titanium carbonitride and forms, it is characterised in that
The matrix surface cured layer of the average thickness with 0.5～3.0 μm is defined to depth direction, as the total average content of Co and Ni of the combination phase metal being contained in this matrix surface cured layer less than 2.0 mass % from the surface of above-mentioned tool base.
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| JP7256978B2 (en) * | 2017-09-29 | 2023-04-13 | 三菱マテリアル株式会社 | A surface-coated cutting tool with a hard coating layer that exhibits excellent adhesion resistance and abnormal damage resistance. |
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| JP2009172748A (en) * | 2007-12-28 | 2009-08-06 | Mitsubishi Materials Corp | Surface-coated cutting tool with hard coating layer having excellent wear resistance |
| CN102069453A (en) * | 2009-11-24 | 2011-05-25 | 陈荣方 | Sharpener trimmer with protection film and forming method of protection film |
| CN102268661A (en) * | 2011-07-04 | 2011-12-07 | 成都理工大学 | Method for preparing Al2O3/TiC composite coating hard alloy |
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| ATE119583T1 (en) * | 1991-03-27 | 1995-03-15 | Krupp Widia Gmbh | COMPOSITE BODY, USE OF THE COMPOSITE BODY AND METHOD FOR PRODUCING IT. |
| US20070154713A1 (en) * | 2005-12-30 | 2007-07-05 | 3M Innovative Properties Company | Ceramic cutting tools and cutting tool inserts, and methods of making the same |
| US20110206919A1 (en) * | 2008-10-29 | 2011-08-25 | Kawaken Fine Chemicals Co., Ltd. | Porous alumina free-standing film, alumina sol and methods for producing same |
| DE102009001675A1 (en) * | 2009-03-19 | 2010-09-23 | Eberhard-Karls-Universität Tübingen | cutting tool |
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| US4820663A (en) * | 1987-09-02 | 1989-04-11 | Kennametal Inc. | Whisker reinforced ceramic and a method of clad/hot isostatic pressing same |
| CN1194015A (en) * | 1995-09-01 | 1998-09-23 | 桑德维克公司 | Coated turning insert |
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| CN1807685A (en) * | 2005-12-09 | 2006-07-26 | 浙江工业大学 | Nano coating process for metal surface |
| JP2009172748A (en) * | 2007-12-28 | 2009-08-06 | Mitsubishi Materials Corp | Surface-coated cutting tool with hard coating layer having excellent wear resistance |
| CN102069453A (en) * | 2009-11-24 | 2011-05-25 | 陈荣方 | Sharpener trimmer with protection film and forming method of protection film |
| CN102268661A (en) * | 2011-07-04 | 2011-12-07 | 成都理工大学 | Method for preparing Al2O3/TiC composite coating hard alloy |
Also Published As
| Publication number | Publication date |
|---|---|
| JP5876755B2 (en) | 2016-03-02 |
| CN103317157A (en) | 2013-09-25 |
| JP2013193171A (en) | 2013-09-30 |
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