CN103317157A - Surface coating cutting tool - Google Patents
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- CN103317157A CN103317157A CN2013100874190A CN201310087419A CN103317157A CN 103317157 A CN103317157 A CN 103317157A CN 2013100874190 A CN2013100874190 A CN 2013100874190A CN 201310087419 A CN201310087419 A CN 201310087419A CN 103317157 A CN103317157 A CN 103317157A
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- Other Surface Treatments For Metallic Materials (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a surface coating cutting tool, which has a hard coating layer. The hard coating layer has excellent lubrication, blade breakage resistance and wear resistance during high-speed interrupted Ti alloy and stainless steel cutting processing operations, etc. The surface coating cutting tool has a tool substrate surface provided with a curing layer and further provided with an aluminum oxide layer having an average thickness ranging from 0.2 mu m to 5 mu m and further having relatively high smoothness. The aluminum oxide layer is composed of a base material and ball tissues dispersed inside the base material. The base material is composed of amorphous phases of the aluminum oxide. The ball tissues are composed of one or two of a needle crystalline phase and a plate-shaped crystalline phase and amorphous phase collecting bodies. The area proportion of the ball tissues inside the longitudinal section of the aluminum oxide layer is between 20- 60 area percent. The radius of an approximate circle ranges from 0.02 mu m to 0.5 mu m. The aluminum oxide base material contains 1-10 atom percent of chlorine.
Description
Technical field
The present invention relates to a kind of surface-coated cutting tool, because its hard coating layer possesses excellent lubricity, anti-cutter, the wearability of collapsing, the high speed interrupted cut that therefore is used for Ti alloy, stainless steel etc. adds man-hour, also can bring into play excellent abrasive through long-term use.
Background technology
In the past, known have by coating on tool base surface form the wearability raising that the hard film that is made of at least a above carbide of the 4a that is selected from periodic table, 5a, 6a family, nitride, carbonitride etc. is realized cutting element.
And, alpha-type aluminum oxide layer in hard film is because excellent heat stability, reactivity is lower and be high rigidity, therefore often forms the alpha-type aluminum oxide layer as the superficial layer coating of the hard film that is made of at least a above carbide of the 4a that is selected from above-mentioned periodic table, 5a, 6a family, nitride, carbonitride etc.
As the coating formation method of alumina layer, adopt chemical vapor deposition (CVD) method usually, but known in addition physical vapor deposition (PVD) method, sol-gal process arranged.
For example shown in patent documentation 1, proposition has following content, namely in order to avoid tool base, deterioration/the distortion of the characteristic of hard film, as the formation method at the alpha-type aluminum oxide layer of cryogenic conditions (below 1000 ℃), form on tool base surface by with the nitride of at least a element as necessary composition by physical vapor deposition (PVD) method, carbide, carbonitride, boride, nitrogen oxide, after the hard film that carbon nitrogen oxide constitutes, form the oxycompound layer by this hard film of oxidation, and by carrying out physical vapor deposition (PVD) at this oxycompound layer, evaporation forms as superficial layer, alumina layer based on the alpha type crystal structure of wearability and excellent heat resistance, wherein, described at least a element is selected from Al and 4a family, 5a family, 6a family and Si.
In addition, shown in patent documentation 2, propose to have following content, namely forming by physical vapor deposition (PVD) method evaporation in the surface-coated cutting tool of hard coating layer, constitute the 1st layer with (Ti, Al) N layer, and constitute the 2nd layer with alumina layer (preferred γ type alumina layer).
And, shown in patent documentation 3, proposition has following content, namely as having the manufacture method of the alumina-coated structure of mechanical characteristic, durability, by sol-gal process mother metal coat by crystal structure be the aluminium oxide of non crystalline structure or γ type or the 1st alumina layer that their mixture constitutes after, coat formation based on the 2nd alumina layer of γ type by sputter.
Patent documentation 1: the open 2004-124246 communique of Japan Patent
Patent documentation 2: the open 2007-75990 communique of Japan Patent
Patent documentation 3: the open 2006-205558 communique of Japan Patent
As hard coating layer, coat in the surface-coated cutting tool that forms alumina layer by the CVD method, when Ti alloy, stainless steel etc. are carried out machining, can enumerate the raising of the wearability in the rake face of coating instrument, but this is especially because the heat endurance of formed alpha-type aluminum oxide, non-reacted higher.
Propose to have by physical vapor deposition (PVD) method in the above-mentioned patent documentation 1 under cryogenic conditions, to form the alpha-type aluminum oxide layer, when but evaporation forms alumina layer, at first need the oxidation hard film and form the oxycompound layer on its surface, but the adhesiveness of oxycompound layer and alumina layer is insufficient, and not only there is alpha-type aluminum oxide as aluminium oxide, also there is γ type aluminium oxide, therefore fail to obtain sufficient hear resistance, its result exist can't bring into play in the long-term use can gratifying cutting ability problem.
In addition, in the above-mentioned patent documentation 2,3, there are the following problems, and namely formed aluminium oxide is γ type aluminium oxide, therefore lacks stability at high temperature, and can't bring into play gratifying cutting ability in high-speed cutting processing.
Summary of the invention
Therefore, the result that the inventor etc. have carried out further investigation for the alumina layer that forms excellent in abrasion resistance by sol-gal process on the tool base surface, find following content: in the amorphous phase aluminium oxide that constitutes the matrix that forms by sol-gal process, disperse distribution by the needle-like crystalline phase of amorphous phase and alpha-aluminium oxide, the congeries formation of tabular crystalline phase and the spheroidal structure of excellent in abrasion resistance, can obtain thus it is provided to and produce high heat and effect has the high speed interrupted cut of intermittence/impact load to add man-hour, lubricity to cutting edge, the anti-cutter that collapses, wearability is the surface-coated cutting tool of excellence also.
Namely, find following content: during the preparation alumina sol, handle as the low temperature maturation, carry out in the stirring and long-term maintenance that are lower than under the common temperature, the reaction speed that suppresses hydrolysis and polycondensation thus, when closely forming the alumina precursor that the combination by Al-O constitutes, can form more the octahedra AlO near corundum type structure
6Therefore this alumina sol is coated with as the superficial layer of tool base and dry, burn till, can form the superficial layer of the hard film that is constituted by following alumina layer, in the described alumina layer, be distributed with in the matrix of higher and lubricity, deposit resistance property, the anti-amorphous nickel/phosphorus/aluminium oxide that collapses the cutter excellence in flatness that congeries by the needle-like crystalline phase of amorphous phase and alpha-type aluminum oxide, tabular crystalline phase constitute and the spheroidal structure of excellent in abrasion resistance.
In addition, to form as the hard film of the basalis that contacts with the alumina layer of superficial layer in the metal ingredient of Al in this hard film shared contain proportional when being nitride epithelium more than the 40 atom %, uprise with the adhesion strength of the alumina layer of superficial layer, therefore preferred the peeling off of the alumina layer that causes such as the impact when suppressing to produce machining, the viewpoint such as damaged.
Namely, find following content: in the surface-coated cutting tool of the present invention, constitute the superficial layer of hard coating layer with alumina layer, and this alumina layer is by flatness, lubricity, deposit resistance property, the matrix of the anti-amorphous nickel/phosphorus/aluminium oxide that collapses the cutter excellence and dispersion is distributed in this matrix and the spheroidal structure of excellent in abrasion resistance constitutes, therefore the surface-coated cutting tool that possesses this hard coating layer is being used for the Ti alloy, high heat such as the generation of stainless steel etc. and to cutting edge effect has the high speed interrupted cut of intermittence/impact high load capacity to add man-hour, also can bring into play excellent abrasive through long-term use.
The present invention is based on above-mentioned opinion and finishes, it is characterized in that,
(1) a kind of surface-coated cutting tool, it forms hard coating layer in the tool base surface coating that is made of tungsten carbide base carbide alloy, base titanium carbonitride and forms, it is characterized in that,
(a) as the superficial layer of above-mentioned hard coating layer, possess the alumina layer of the average bed thickness with 0.2～5 μ m,
(b) above-mentioned alumina layer is made of matrix and the spheroidal structure that is dispersed in the matrix,
(c) above-mentioned matrix is made of the amorphous phase of aluminium oxide, and above-mentioned spheroidal structure is made of the congeries of one or both and amorphous phase in needle-like crystalline phase and the tabular crystalline phase.
(2) as described (1) described surface-coated cutting tool is characterized in that,
Spheroidal structure shared area ratio in above-mentioned alumina layer is 20～60 area %.
(3) as described (1) or (2) described surface-coated cutting tool is characterized in that,
The approximate radius of a circle of above-mentioned spheroidal structure is 0.02～0.5 μ m.
(4) as described (1) described surface-coated cutting tool is characterized in that,
The chlorine that contains 1.0～10 atom % in the above-mentioned alumina layer matrix.
(5) described (1) described surface-coated cutting tool, it forms hard coating layer in surface of the tool base that is made of tungsten carbide base carbide alloy coating and forms, it is characterized in that,
Be formed with the matrix surface cured layer of the average bed thickness with 0.5～3.0 μ m to depth direction from the surface of above-mentioned tool base, as be contained in this matrix surface cured layer in conjunction with the average content of the Co of phase metal less than 2.0 quality %.
(6) described (1) described surface-coated cutting tool, it forms hard coating layer in surface of the tool base that is made of tungsten carbide base carbide alloy coating and forms, it is characterized in that,
Be formed with the matrix surface cured layer of the average bed thickness with 0.5～3.0 μ m to depth direction from the surface of above-mentioned cermet tool matrix, as be contained in this matrix surface cured layer in conjunction with the total average content of the Co of phase metal and Ni less than 2.0 quality %.
According to surface-coated cutting tool of the present invention, it is to coat the instrument that forms by the aluminium oxide of sol-gal process film forming on the tool base surface, but formed above-mentioned alumina layer possesses excellent surface smoothing, lubricity, deposit resistance property, the anti-cutter that collapses, when to the cutting edge effect therefore used it for when producing high heat has in the high speed interrupted cut processing of the Ti alloy, stainless steel of intermittence/impact load etc., can not produce unusual damage such as collapse cutter, peel off and through the long-term performance excellent abrasive of using yet.
Description of drawings
Fig. 1 is expression with the photo of organizing of the longitudinal section of the alumina layer of tem observation instrument 2 of the present invention.
Fig. 2 be the expression alumina layer of observing instrument 2 of the present invention with SEM the cross section organize photo.
Fig. 3 be the expression alumina layer of observing instrument 2 of the present invention with SEM the surface organize photo.
The specific embodiment
Below, the present invention is described in detail.
In the surface-coated cutting tool of the present invention, possesses alumina layer by 0.2～5.0 μ m of sol-gal process film forming as the superficial layer of hard coating layer, but if the bed thickness of alumina layer is less than 0.2 μ m, the generation negligible amounts of ring-type tissue described later then, therefore can't bring into play sufficient abrasion resistance, on the other hand, if bed thickness surpasses 5.0 μ m, then easily produce peeling off of layer, therefore the bed thickness with alumina layer is decided to be 0.2～5.0 μ m.
In addition, above-mentioned alumina layer can be brought into play its performance in tool base by direct film forming, but the carbide alloy that will comprise titanium carbonitride is during as matrix, by in blanket of nitrogen, burning till, at the more higher carbonitride of at least a wearability that contains among Ti, Ta, Nb, the Zr of tool base near surface, thereby form the matrix surface cured layer, and improve the adhesion strength of alumina layer and tool base, can prolong life tools thus.The hardness of the hard alloy substrate after in addition, preferably this matrix surface cured layer forms with Vickers hardness (Hv) more than 2200 and below 2800.At this moment, by the more carbonitride that contains, near the matrix surface Co can reduce relatively, for example utilize scanning electron microscope (SEM) to carry out the cross-section of 0.5～3.0 μ m to depth direction from the surface, when in the scope of analyzing field of view 1 * 1 μ m, detecting conduct in conjunction with the content of the Co of phase metal by the quantitative analysis based on wavelength dispersion type x-ray spectrometry, if the content of Co is less than 2.0 quality %, then fully become the carbonitride of main cause of the surface cure of matrix, and wearability is further enhanced.
In addition, with base titanium carbonitride during as matrix, the atmosphere that reaches when keeping in maximum temperature that will heat up in sintering circuit is made as predetermined blanket of nitrogen, and keep midway or reduce pressure during cooling, compare during thus with enforcement clean burn knot operation in the blanket of nitrogen of constant pressure, the surface is more solidified.This be because, if in the operation of implementing under the constant nitrogen pressure till keeping with maximum temperature, then disperse to form the higher carbonitride of hardness equably in matrix inside, relative therewith, if heat up or keep midway before under than higher nitrogen pressure, handle, keep midway or begin to be made as in the blanket of nitrogen that is further depressurized during cooling and handle, then have only the most surperficial by denitrogenation of matrix, thus Ti or Nb etc. to Ni or Co metal in conjunction with the dissolving of phase and come to life to the diffusion of matrix surface internally, promote the formation of carbonitrides such as Ti or Nb on the surface, thereby form the matrix surface cured layer.The hardness of the cermet matrix after in addition, preferably this matrix surface cured layer forms with Vickers hardness (Hv) more than 2000 and below 2600.And, this moment is identical with above-mentioned hard substrate, near the matrix surface Ni and Co can reduce relatively, if will be as being made as less than 2.0 quality % in conjunction with the Ni of phase metal and the content of Co, then fully become the carbonitride of main cause of the surface cure of matrix, and wearability is further enhanced.
In addition, in surface-coated cutting tool of the present invention, can directly not form above-mentioned alumina layer 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, namely the hard film more than one deck at least that is made of nitride or the oxide of at least a above element that contains 4a, the 5a, 6a family and the Si that are selected from periodic table coats on the surface of this hard film afterwards and forms above-mentioned alumina layer.
In addition, when forming hard film by above-mentioned physical vapor deposition (PVD) method, at the hard film that contacts with alumina layer, from improving adhering viewpoint, be preferably formed that shared in the metal ingredient of this hard film to contain proportional be nitride epithelium (for example, TiAlN film, CrAlN film etc.) more than the 40 atom % in order to contain Al and Al in this hard film.
This be because, if shared in the metal ingredient of Al in hard film to contain proportional be nitride epithelium more than the 40 atom %, then form the higher oxide of alumina concentration at the interface of nitride epithelium and aluminium oxide epithelium, and this oxide becomes and has the effect that nitride epithelium and aluminium oxide epithelium are firmly adhered.
Constitute the alumina layer of superficial layer of surface-coated cutting tool of the present invention by sol-gal process film forming described later, its matrix is made of amorphous nickel/phosphorus/aluminium oxide thus, and forms the spheroidal structure that the congeries by amorphous phase and needle-like crystalline phase, tabular crystalline phase constitute in this matrix.
When utilizing scanning electron microscope (SEM) to observe alumina layer, as Fig. 1, Fig. 2, shown in Figure 3, above-mentioned spheroidal structure is viewed as the spherical congeries tissue of radius 0.02～0.5 μ m, in addition if further observe this spheroidal structure with transmission electron microscope (TEM), then it forms the congeries tissue of amorphous phase and needle-like crystalline phase, tabular crystalline phase as can be known.
And, if for example the scope of field of view 5 * 7 μ m in, obtain this spheroidal structure shared area ratio in alumina layer by SEM observation longitudinal section, account for 20～60 area % as can be known.
In addition, can be observed at spheroidal structure and interface as the aluminium oxide of matrix according to Fig. 1 and be formed with recess (white rings part among Fig. 1) in the mode around spheroidal structure.
The shape of spheroidal structure is exactly the complex tissue that each various in opposite directions direction is arranged originally, so the isotropism aspect is stronger, according to its stress dispersion effect, also helps stable wearability in applying the heavy cut of high load capacity.If above-mentioned spheroidal structure shared area ratio in alumina layer surpasses 60 area %, then fixedly the ratio of the matrix of spheroidal structure tails off, therefore the embrittlement tendency appears in alumina layer, and the ratio around the recess (with reference to figure 1) of spheroidal structure becomes big, therefore the load inhomogeneous to layer effect when machining might produce destruction.On the other hand, area ratio is during less than 20 area %, and the spheroidal structure that helps to improve wearability is less, so the wearability of alumina layer reduces.
Therefore, among the present invention, spheroidal structure shared area ratio in alumina layer is decided to be 20～60 area %.
With the radius of above-mentioned spheroidal structure as having when obtaining with the radius of a circle of the area equal areas of this spheroidal structure, if radius is less than 0.02 μ m, it is less that then the wearability in the alumina layer improves effect, on the other hand, then become thick tissue if radius surpasses 0.5 μ m, therefore easily become the starting point of be full of cracks and cause anti-reduction of collapsing cutter.
Therefore, the size with above-mentioned spheroidal structure is decided to be radius 0.02～0.5 μ m.
The alumina layer that constitutes the superficial layer of surface-coated cutting tool of the present invention can form by the following sol-gal process that illustrates.
The preparation of alumina sol:
By following formation alumina sol, namely at first, at aluminium-alcohol salt (for example, aluminium secondary butylate, aluminium propoxide) middle interpolation alcohol is (for example, ethanol, 1-butanols), further add (can add the alpha alumina particle of average grain diameter 10～300nm simultaneously) acid (for example, hydrochloric acid, nitric acid) afterwards, in the temperature range below 15～30 ℃, stir and the maturation carried out more than 12 hours is handled.
In addition, when adding alcohol, in order to improve film formation at low temp and the crystallinity that generates to realize by the nucleus that promotes when forming alumina layer, from making uniform colloidal sol viewpoint, preferred interpolation contains the alcohol that average grain diameter is the alpha alumina particle of 10～300nm in advance.In addition, this is because have following effect, namely when coating alpha alumina particle become the nuclear of the starting point that becomes crystal growth, and as the center in alumina layer favorable dispersibility ground form the spherical gathering organization of homogeneous diameter, but when interpolation contains alpha alumina particle pure, if the average grain diameter of alpha alumina particle is less than 10nm, then can not reach the critical nucleus size of the starting point that can become crystal growth, therefore can not produce the crystal growth from the alumina sol around the alpha alumina particle, cause from matrix isolatedly, after burning till, easily become the position more weak with the adhesion of on every side crystal grain.On the other hand, if average grain diameter surpasses 300nm, then be that the nucleus of starting point is excessively grown into oversize grain with the alpha alumina particle, cause in the reduction of film hardness and the film damagedly, therefore the average grain diameter with the alpha alumina particle that adds is made as 10～300nm.
In addition, if the alpha alumina particle content in the alcohol with respect to the alkoxide of aluminium oxide less than 0.5 quality %, then can't satisfy in film with the even required karyogenesis number of distribution nucleus more than certain density, cause crystallinity in the film according to the position and inhomogeneous, therefore when cutting, easily cause inordinate wear.If surpass 5 quality % with respect to aluminium-alcohol salt, then in alumina sol, easily produce the cohesion of alpha alumina particle, should cohesion portion when forming alumina layer form the oversize grain in the film, therefore preferably cause in the film damagedly, the addition of alpha alumina particle is made as the scope of 0.5～5 quality % with respect to aluminium-alcohol salt.
In addition, the concentration of the preferred acid of adding is 0.01～1.0N, and preferred acid is 0.1～2 times (capacity) with respect to the addition of alcohol.
In addition, when adding hydrochloric acid as acid, sneak into and residual chlorine in the final alumina host that forms, but metal reaction such as chlorine and iron also forms the higher chloride of lubricity, help the lubricity of alumina layer, the raising of deposit resistance property in the result thus, therefore allow the scope that contains 1.0～10 atom % as the concentration of the chlorine in the alumina layer.
Usually in the preparation of the alumina sol that carries out, stirring and the maturation about a few hours under this whipping temp carried out under 40～80 ℃ are handled, but among the present invention, carry out the stirring in 15～30 ℃ the temperature range and for example handle through the long low temperature maturation that reaches more than 12 hours.
Wherein, if the temperature when stirring and maintenance surpasses 30 ℃, then hydrolysis and polycondensation reaction meeting are carried out rapidly, therefore can closely not form presoma, and can not form alpha-aluminium oxide in as the firing process of subsequent handling, the temperature upper limit in the time of therefore will stirring and keep is made as 30 ℃.On the other hand, if the temperature when stirring and maintenance is less than 15 ℃, then can in alumina sol, form a plurality of Al-O joint portions of closely constructing in heterogeneity, but in order to form the spheroidal structure with size of the present invention, preferably in alumina sol, form minority Al-O joint portion closely locally.Temperature during therefore, with stirring and maintenance is made as easily and is hydrolyzed partly, 15～30 ℃ cryogenic temperature scope of polycondensation reaction.
In addition, with the maturation time be made as reach more than 12 hours be for a long time because, slowly promote hydrolysis at low temperatures, closely generate alumina precursor thus.
Dry/as to burn till:
The alumina sol of preparation in above-mentioned directly is coated on the surface of tool base or is coated on as the hard film surface that is formed at the basalis on tool base surface by physical vapor deposition (PVD) method, then carry out repeatedly more than 1 time 100～300 ℃, preferably the drying under 150～200 ℃ is handled, then, in 400～650 ℃ temperature range, burn till processing, coat thus and form alumina layer.
By the above-mentioned dry dry colloidal sol that forms aluminium oxide of handling, by the processing of then carrying out of burning till, form the amorphous phase of aluminium oxide as matrix on the hard film surface, disperseing simultaneously to distribute in matrix forms the spheroidal structure that the congeries by amorphous phase and needle-like crystalline phase, tabular crystalline phase constitute.
The thickness of above-mentioned alumina layer depends on coating thickness and the coating number of times of alumina sol, but if the thickness of the above-mentioned alumina layer that coating forms is less than 0.2 μ m, then can't be through the superior abrasion resistance of long-term use performance as surface-coated cutting tool, on the other hand, if thickness surpasses 5.0 μ m, then alumina layer easily produces and peels off, and therefore the thickness with above-mentioned alumina layer is made as 0.2～5.0 μ m.
In addition, the temperature range that drying is handled is decided to be 100～300 ℃, more preferably is decided to be 150～200 ℃, and the temperature range that will burn till processing is decided to be 400～650 ℃.About baking temperature, be because if then can't carry out abundant drying less than 100 ℃, if surpass 300 ℃ then the volume contraction of colloidal sol sharply carry out and produce be full of cracks etc., and epithelium easily produces and peels off etc.About firing temperature, be because if then can't form the effective crystallinity spheroidal structure of interrupted cut less than 400 ℃, it is therefore anti-that to collapse cutter insufficient, on the other hand, when burning till with the temperature that surpasses 650 ℃, the crystallization of thickization of spheroidal structure and matrix further carries out, so flatness, lubricity, deposit resistance property show and reduce tendency.
[embodiment 1]
Then, be specifically described by the present invention of embodiment.
(a1) as material powder, prepare the middle grain WC powder of particulate WC powder, average grain diameter 2～3 μ m of average grain diameter 0.8 μ m, all have TiCN powder, ZrC powder, TaC powder, NbC powder, a Cr of the average grain diameter of 1～3 μ m
3C
2Powder and Co powder, these material powders are fitted in the predetermined cooperation shown in the table 1 to be formed, further add paraffin and in acetone ball milling mixed 24 hours, after the drying under reduced pressure, pressure punch forming with 98MPa is the pressed compact of reservation shape, and in the vacuum of 5Pa, with 1400 ℃ of conditions that kept 1 hour this pressed compact is carried out vacuum-sintering, after the sintering cutting portion is imposed the cutting edge reconditioning processing of R:0.05mm, make the WC base cemented carbide tool base A processed with blade shapes of in ISOCNMG120408, stipulating thus, B, C, D, E(is called hard substrate A, B, C, D, E).Wherein, at hard substrate D, in the blanket of nitrogen of 3.3kPa, carry out the cooling that keeps after 1 hour till 1320 ℃ with 1400 ℃, at hard substrate E, in the blanket of nitrogen of 2kPa, carry out the cooling that keeps after 1 hour till 1320 ℃ with 1400 ℃, thus matrix surface is cured processing.
(b1) then, with the above-mentioned hard substrate A chemical evaporation plating device of packing into, utilize the membrance casting condition shown in the table 2 to be pre-formed the Ti compound layer that is constituted by the TiCN layer of the TiN layer that possesses the granular crystal tissue with the thickness shown in the table 4 and longitudinal growth crystalline structure (below, represent with l-TiCN) as basalis.And for above-mentioned hard substrate B, the arc ion plating apparatus of one of the physical vapor deposition device of also packing into as basalis, coats the Ti that forms by the thickness 2.0 μ m shown in the table 4 by physical vapor deposition
0.5Al
0.5N layer or Al
0.7Cr
0.3The hard film that the N layer constitutes.In addition, for above-mentioned hard substrate C, D, E, implement special surface and coat processing.
(c1) on the other hand, carry out for the preparation that coats the alumina sol that forms alumina layer by sol-gal process the most surperficial following of hard film.
Aluminium-alcohol salt at the scheduled volume shown in the table 3 is the ethanol that adds the scheduled volume that is shown in table 3 equally in the aluminium secondary butylate as alcohol, stirs under 20 ℃ in thermostat, and adds the hydrochloric acid of the water that has been added with scheduled volume by dripping down through 1 hour.
(d1) with its as shown in table 3 in thermostat, remaining like that under 20 ℃ the state, continue to stir more than 12 hours, and handled 24 hours with 20 ℃ of low temperature maturations, prepare alumina sol thus.
Becoming following mode with final solution composition with mol ratio adjusts.
(aluminium secondary butylate): (water): (ethanol): (hydrochloric acid)=1:(80～120): 20:(0.1～1)
(e1) then, above-mentioned alumina sol is coated on the Ti that is formed at above-mentioned hard substrate B by the described Ti compound layer that is formed at above-mentioned hard substrate A by the chemical vapor deposition method, by physical vapor deposition
0.5Al
0.5N layer, Al
0.7Cr
0.3Reaching the special surface of enforcement on the hard film that the N layer constitutes coats on hard substrate C, the D of processing.
(f1) then, the drying of the predetermined condition shown in the above-mentioned alumina sol that has been coated with carry out table 3 is handled, and be coated with repeatedly with drying after, in atmosphere with 600 ℃ of processing of burning till of carrying out 1 hour, form alumina layer of the present invention (namely in the most surperficial coating, in the matrix that is constituted mutually by amorphous nickel/phosphorus/aluminium oxide, be distributed with the alumina layer of the spheroidal structure that the congeries by amorphous phase and needle-like crystalline phase, tabular crystalline phase constitute), make surface-coated cutting tool 1 of the present invention, 2,3,4 thus, 5(is called instrument 1 of the present invention, 2,3,4,5).
At the invention described above instrument 1～5, the result who observes the longitudinal section of alumina layer with scanning electron microscope (SEM) can confirm, its matrix is made of amorphous phase, on the other hand, the spheroidal structure that is distributed in the matrix is made of the congeries of one or both and amorphous phase in needle-like crystalline phase and the tabular crystalline phase.Utilize transmission electron microscope (TEM) to analyze the result of its matrix and spheroidal structure respectively by the SEAD method for the affirmation of amorphous phase, its matrix obtains dizzy master drawing case, and spheroidal structure obtains electronics ray diffraction diagram case and dizzy master drawing case clearly.
The longitudinal section TEM photo of the alumina layer of instrument 2 of the present invention is shown as an example among Fig. 1, among Fig. 2 and Fig. 3 this instrument 2 of the present invention is illustrated surface and the section S EM photo of its alumina layer in addition.Can confirm that according to Fig. 2, Fig. 3 the spheroidal structure that is scattered in the amorphous nickel/phosphorus/aluminium oxide layer is made of the congeries of amorphous phase and needle-like crystalline phase, tabular crystalline phase.
For the invention described above instrument 1～5, observe spheroidal structure shared area ratio and mean radius of spheroidal structure in the longitudinal section of alumina layer by scanning electron microscope with 50,000 times visual field, at its result, be assumed to be the plane and come 5 area ratios of measuring spheroidal structure, and the approximate radius of a circle when 5 mensuration is calculated the area of this spheroidal structure as the area of a circle, and with its mean value as average-size.
In addition, content about the Co that sneaks into the cl concn that remains in the alumina layer matrix and hard substrate surface, wavelength dispersion type x-ray spectrometry quantitative analysis alumina layer by utilizing scanning electron microscope (SEM) or the longitudinal section of hard substrate are observed in the visual field, and adopt its mean value.Cl concn in the alumina layer matrix carries out 5 mensuration with point analysis, and the surface analysis of analysis field of view 1 * 1 μ m in the scope of Co content utilization 0.5～3.0 μ m from substrate surface to depth direction on hard substrate surface carries out 5 visual fields and measures.
In addition, utilize the result of the average bed thickness of scanning electron microscope cross-section determination alumina layer simultaneously, all show in fact identical with target bed thickness mean value (mean values at 5 places).
Measurement result shown in the table 4.
[comparative example 1]
For relatively, make surface-coated cutting tool with following manufacture method.
Namely for tool base A, B, C, D, the E of described (a1), the operation by described (b1) forms hard film, and prepares alumina sol by the operation (reference table 3) of described (c1).
(in addition, do not carry out formation according to the hard film of described (b1) operation for tool base C, D, E.）
Then, replace the operation of described (d1), in thermostat, remain and continue under 40 ℃ the state to stir 12 hours, and 40 ℃ of following maturations 24 hours, prepare alumina sol thus.
Then, similarly above-mentioned alumina sol is coated on by the Ti that is formed at hard substrate A, B with described (e1)
0.5Al
0.5N layer, Al
0.7Cr
0.3On the hard film that the N layer constitutes and implement special surface and coat on the hard substrate C, the D that handle, the E.
Then, similarly the above-mentioned alumina sol that has been coated with being carried out drying with described (f1) handles, and be coated with repeatedly and dry the processing after, in atmosphere with 600 ℃ of processing of burning till of carrying out 1 hour, form alumina layer in the most surperficial coating, the surface-coated cutting tool 1,2,3,4,5, the 6(that make comparative example thus are called comparative example instrument 1,2,3,4,5,6).
[embodiment 2]
For reference, make surface-coated cutting tool with following manufacture method.
That is, for tool base A, the B of described (a1), (in addition, for tool base C, D, E, do not carry out the formation according to the hard film of described (b1) operation by the operation formation of described (b1).) hard film, operation (reference table 3) preparation solution composition by described (c1) is different from the alumina sol of embodiment 1, and the operation by described (e1) will be coated on respectively on hard substrate A, B, C, D, the E by the colloidal sol that the operation (reference table 3) of described (d1) has been implemented low temperature maturation processing.
Then, similarly the above-mentioned alumina sol that has been coated with being carried out drying with described (f1) handles, and be coated with repeatedly and dry the processing after, in atmosphere with 600 ℃ of processing of burning till of carrying out 1 hour, coat the formation alumina layer on the surface, make surface-coated cutting tool 6～17(of the present invention thus and be called instrument 6～17 of the present invention).
At above-mentioned comparative example instrument 1～6, instrument of the present invention 6～17, the results verification that utilizes scanning electron microscope (SEM) and transmission electron microscope (TEM) to observe alumina layer arrives, the comparative example instrument has the membrane tissue of no spheroidal structure, instrument 6～17 of the present invention has spheroidal structure, but for having the membrane tissue of the spheroidal structure size different with instrument of the present invention 1～5, area occupation ratio, concentration of residual chlorine.And confirm, spheroidal structure is made of the congeries of amorphous phase and needle-like crystalline phase, tabular crystalline phase.
At the invention described above instrument 6～17, observe spheroidal structure shared area ratio and mean radius of spheroidal structure in the longitudinal section of alumina layer by scanning electron microscope with 50,000 times visual field, at its result, be assumed to be the plane and come 5 area ratios of measuring spheroidal structure, and the approximate radius of a circle when 5 mensuration is calculated the area of this spheroidal structure as the area of a circle, and with its mean value as average-size.
Measurement result shown in the table 4.
Then, for the invention described above instrument 1～17 and comparative example instrument 1～6, carry out the wet type high speed interrupted cut processing experiment of Ti alloy with following condition.
Carry out wet type high speed interrupted cut processing experiment (common cutting speed is respectively 80m/min.) afterwards with following condition, the state of wear of each instrument is observed, and measure the wear of the tool flank amount.
Workpiece: on the length direction of Ti-6Al-4V alloy (HB250) with the pole that uniformly-spaced is formed with 4 pods,
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, the TiCN(for preparing all to have the average grain diameter of 0.5～2 μ m is TiC/TiN=50/50 with the mass ratio) powder, Mo
2The C powder, the NbC powder, the TaC powder, WC powder, Co powder and Ni powder, these are fitted in the predetermined cooperation shown in the table 5 forms, carry out 24 hours wet mixed with ball milling, pressure punch forming with 98MPa after dry is pressed compact, in the blanket of nitrogen of 1.3kPa with temperature: 1540 ℃ of conditions that kept 1 hour are carried out sintering to this pressed compact, after the sintering blade part branch is imposed the cutting edge reconditioning processing of R:0.07mm, make the TiCN based ceramic metal tool base F processed of the blade shapes with iso standard CNMG120408 thus, G, H, I, J(is called cermet matrix F, G, H, I, J).Wherein, for tool base I, in the blanket of nitrogen of 1.3kPa, programming rate is made as 2 ℃/min, is warming up to 1540 ℃ and keep being made as after 30 minutes the vacuum of 13Pa from room temperature, and keep lowering the temperature after 30 minutes and carrying out surface cure with 1540 ℃.For tool base J, the nitrogen pressure during with sintering is made as different with tool base I, is made as the constant surface cure that carries out in the blanket of nitrogen of 13Pa.
(b2) then, with the above-mentioned hard substrate F chemical evaporation plating device of packing into, as basalis, utilize the membrance casting condition shown in the table 2 to be pre-formed the Ti compound layer that the l-TiCN layer by the TiN layer that possesses the granular crystal tissue with the thickness shown in the table 7 and longitudinal growth crystalline structure constitutes.In addition, for above-mentioned hard substrate G, the arc ion plating apparatus of one of the physical vapor deposition device of also packing into as basalis, coats the Ti that forms by the thickness 2.0 μ m shown in the table 7 by physical vapor deposition
0.5Al
0.5N layer or Al
0.7Cr
0.3The hard film that the N layer constitutes.
(c2) on the other hand, carry out for the preparation that coats the alumina sol that forms alumina layer by sol-gal process the most surperficial following of hard film.
Aluminium-alcohol salt at the scheduled volume shown in the table 6 is in the aluminium isopropoxide, add the 1-butanols of the scheduled volume of the alpha alumina particle that contains the predetermined mean particle diameter shown in the table 6 as alcohol, in thermostat, under 20 ℃, stir, and add the water-reducible nitric acid with scheduled volume by dripping down through 1 hour.
(d2) it is remained in thermostat under 20 ℃ the state, continue to stir 12 hours, and handled 24 hours 20 ℃ of following low temperature maturations, prepare alumina sol thus.
In addition, the amount that makes an addition to the water in this colloidal sol is 1:(80～120 with respect to the ratio that is contained in the aluminium oxide in the alumina sol in above-mentioned).
(e2) then, above-mentioned alumina sol is coated on the Ti that is formed at above-mentioned cermet matrix G by the described Ti compound layer that is formed at above-mentioned cermet matrix F by the chemical vapor deposition method, by physical vapor deposition
0.5Al
0.5N layer, Al
0.7Cr
0.3Reaching the special surface of enforcement on the hard film that the N layer constitutes coats on cermet matrix H, the I of processing.
(f2) then, to the above-mentioned alumina sol that has been coated with, the drying of the predetermined condition shown in carry out table 6 is handled, and be coated with repeatedly with drying after, in atmosphere with 600 ℃ of processing of burning till of carrying out 1 hour, coat formation alumina layer of the present invention on the surface (namely, in the matrix that is constituted mutually by amorphous nickel/phosphorus/aluminium oxide, be distributed with the alumina layer of the spheroidal structure that the congeries by amorphous phase and needle-like crystalline phase, tabular crystalline phase constitute), make surface-coated cutting tool 18～22(of the present invention thus and be called instrument 18～22 of the present invention).
At the invention described above instrument 18～22, the results verification of observing the longitudinal section of alumina layer by scanning electron microscope (SEM) arrives, its matrix is made of mutually amorphous nickel/phosphorus/aluminium oxide, on the other hand, the spheroidal structure that is distributed in the matrix is made of the congeries of amorphous phase and needle-like crystalline phase, tabular crystalline phase.
At the invention described above instrument 18～22, observe spheroidal structure shared area ratio and mean radius of spheroidal structure in the longitudinal section of alumina layer by scanning electron microscope with 50,000 times visual field, at its result, be assumed to be the plane and come 5 area ratios of measuring spheroidal structure, and the approximate radius of a circle when 5 mensuration is calculated the area of this spheroidal structure as the area of a circle, and with its mean value as average-size.
Measurement result shown in the table 7.
[comparative example 2]
For relatively, utilize the surface-coated cutting tool 7～12(of above-mentioned tool base F, G, H, I, J manufacturing comparative example to be called comparative example instrument 7～12).
That is, the operation by above-mentioned (b2) forms the Ti compound layer at cermet matrix F, and G forms Ti at the cermet matrix
0.5Al
0.5N layer and Al
0.7Cr
0.3The N layer, the operation by above-mentioned (c2) prepares alumina sol.
Then, in the operation of described (d2), in thermostat, remain under 40 ℃ the state, continue to stir 12 hours, and with 40 ℃ of maturations 24 hours, prepare alumina sol thus.
Then, above-mentioned alumina sol is coated on the hard film that is formed at cermet matrix F, G and does not implement special surface and coat cermet matrix H, I, the J that handles.
Then, similarly the above-mentioned alumina sol that has been coated with being carried out drying with above-mentioned (f2) handles, and be coated with repeatedly and dry the processing after, in atmosphere with 600 ℃ of processing of burning till of carrying out 1 hour, form alumina layer in the most surperficial coating, the surface-coated cutting tool 7～12(that makes comparative example thus is called comparative example instrument 7～12).
[embodiment 4]
For reference, make surface-coated cutting tool with following manufacture method.
Namely, tool base F, G, H, I, J for described (a2), operation by described (b2) forms hard film, operation by described (c2) prepares the alumina sol that solution composition is different from embodiment 3, and the operation by described (e2) will be implemented the colloidal sol that the low temperature maturation handles by the operation of described (d2) and be coated on tool base F, G, H, I, the J.
Then, similarly the above-mentioned alumina sol that has been coated with being carried out drying with described (f2) handles, and be coated with repeatedly and dry the processing after, in atmosphere with 600 ℃ of processing of burning till of carrying out 1 hour, form alumina layer in the most surperficial coating, make surface-coated cutting tool 23～28(of the present invention thus and be called instrument 23～28 of the present invention).
At above-mentioned comparative example instrument 7～12, the invention described above instrument 23～28, the results verification of observing alumina layer with scanning electron microscope (SEM) and transmission electron microscope (TEM) arrives, the comparative example instrument is the membrane tissue of no spheroidal structure, instrument 23～28 of the present invention contains spheroidal structure, but for having the membrane tissue of the spheroidal structure size that is different from instrument 18～22 of the present invention, area occupation ratio, concentration of residual chlorine.
For the invention described above instrument 23～28, observe spheroidal structure shared area ratio and mean radius of spheroidal structure in the longitudinal section of alumina layer by scanning electron microscope with 50,000 times visual field, at its result, be assumed to be the plane and come 5 area ratios of measuring spheroidal structure, and the approximate radius of a circle when 5 mensuration is calculated the area of this spheroidal structure as the area of a circle, and with its mean value as average-size.Measurement result shown in the table 7.
Then, to the invention described above instrument 18～28 and comparative example instrument 7～12, carry out stainless wet type high speed interrupted cut processing experiment with following condition.
Carry out wet type high speed interrupted cut test (common cutting speed is 100m/min) with following condition and afterwards, the state of wear of each instrument is observed, and measure the wear of the tool flank amount.
On the length direction of workpiece: JISSUS304 with the pole that uniformly-spaced is formed with 4 pods,
Cutting speed: 160m/min,
Cutting depth: 1.2mm,
Feed speed: 0.22mm/rev.,
Cutting time: 5 minutes.
[table 5]
[table 6]
[table 7]
From the result shown in the table 4,7 as can be known, in the surface-coated cutting tool 1～5 of the present invention, 18～22, be formed with aluminium oxide by sol-gal process in the coating of tool base surface, this alumina layer possesses excellent surface smoothing, lubricity, deposit resistance property, therefore when using it in the high speed interrupted cut processing of Ti alloy, stainless steel etc., can not produce yet and collapse cutter, unusual damage such as peel off, and use performance excellent abrasive, smear metal to discharge property through long-term.
Relative therewith, the surface-coated cutting tool 1～12 of the clear and definite comparative example that in the alumina layer on surface, does not contain spheroidal structure as can be known and only constituted by matrix organization, can't bear the greater impact of interrupted cut, especially be easy to generate near the small cutter that collapses of cutting edge reconditioning portion, and owing to only be made of amorphous phase, so high temperature hardness is insufficient, the bigger heating that produces during owing to high-speed cutting, the crescent hollow abrasion heighten degree arrives service life at short notice.
And, instrument 6～17 of the present invention, 23～28 contains the crystallinity spheroidal structure in the alumina layer on surface, therefore do not find the carrying out of rapid crescent hollow abrasion, but because the size of spheroidal structure or the be full of cracks that recess causes, produce sometimes that near the cutting edge reconditioning portion small collapsed cutter or owing to the surface cure layer that does not have tool base causes the wear of the tool flank heighten degree, but compare with the surface-coated cutting tool 1～12 of comparative example, show excellent abrasive, can say to obtain long lifetime life tools.
In addition, among the described embodiment, utilize the instrument of blade shapes to estimate the performance of hard coating layer, but also can obtain same result certainly with drill bit, slotting cutter etc.
Utilizability on the industry
According to surface-coated cutting tool of the present invention, coating is formed with aluminium oxide on the surface by sol-gal process, this alumina layer possesses excellent surface smoothing, lubricity, deposit resistance property, the anti-cutter that collapses, therefore the high speed interrupted cut of using it for Ti alloy, stainless steel etc. adds man-hour, can not produce yet and collapse cutter, unusual damage such as peel off, and use performance excellent abrasive and smear metal to discharge property through long-term, long lifetime that can the implementation tool life-span, the effect in the use is bigger.
Claims (6)
1. surface-coated cutting tool, its coating on the tool base surface that is made of tungsten carbide base carbide alloy, base titanium carbonitride forms hard coating layer and forms, it is characterized in that,
(a) as the superficial layer of above-mentioned hard coating layer, possess the alumina layer of the average bed thickness with 0.2～5 μ m,
(b) above-mentioned alumina layer is made of matrix and the spheroidal structure that is dispersed in the matrix,
(c) above-mentioned matrix is made of the amorphous phase of aluminium oxide, and above-mentioned spheroidal structure is made of the congeries of one or both and amorphous phase in needle-like crystalline phase and the tabular crystalline phase.
2. surface-coated cutting tool according to claim 1 is characterized in that,
Spheroidal structure shared area ratio in above-mentioned alumina layer is 20～60 area %.
3. surface-coated cutting tool according to claim 1 and 2 is characterized in that,
The approximate radius of a circle of above-mentioned spheroidal structure is 0.02～0.5 μ m.
4. surface-coated cutting tool according to claim 1 is characterized in that,
The chlorine that contains 1.0～10 atom % in the above-mentioned alumina layer matrix.
5. surface-coated cutting tool according to claim 1, its surface in the tool base that is made of tungsten carbide base carbide alloy coat and form hard coating layer and form, it is characterized in that,
Formed the matrix surface cured layer of the average bed thickness with 0.5～3.0 μ m to depth direction from the surface of above-mentioned tool base, as be contained in this matrix surface cured layer in conjunction with the average content of the Co of phase metal less than 2.0 quality %.
6. surface-coated cutting tool according to claim 1, its surface in the tool base that is made of base titanium carbonitride coat and form hard coating layer and form, it is characterized in that,
Formed the matrix surface cured layer of the average bed thickness with 0.5～3.0 μ m to depth direction from the surface of above-mentioned tool base, as be contained in this matrix surface cured layer in conjunction with the total average content of the Co of phase metal and Ni less than 2.0 quality %.
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| 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 |
| WO2010050225A1 (en) * | 2008-10-29 | 2010-05-06 | 川研ファインケミカル株式会社 | 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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- 2012-03-21 JP JP2012063413A patent/JP5876755B2/en active Active
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| US4801510A (en) * | 1987-09-02 | 1989-01-31 | Kennametal Inc. | Alumina coated silcon carbide whisker-alumina composition |
| 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 |
| US6338894B1 (en) * | 2000-05-31 | 2002-01-15 | Mitsubishi Materials Corporation | Coated cemented carbide cutting tool member and process for producing the same |
| CN1748917A (en) * | 2004-06-30 | 2006-03-22 | 三菱综合材料株式会社 | Surface-coated cermet cutting tool |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107980013A (en) * | 2016-08-24 | 2018-05-01 | 住友电工硬质合金株式会社 | Surface-coated cutting tool and its manufacture method |
| CN107980013B (en) * | 2016-08-24 | 2019-07-05 | 住友电工硬质合金株式会社 | Surface-coated cutting tool and its manufacturing method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103317157B (en) | 2016-08-03 |
| JP5876755B2 (en) | 2016-03-02 |
| JP2013193171A (en) | 2013-09-30 |
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