CN112663060A - Composite cutter coating and preparation method thereof - Google Patents
Composite cutter coating and preparation method thereof Download PDFInfo
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- CN112663060A CN112663060A CN202011377458.0A CN202011377458A CN112663060A CN 112663060 A CN112663060 A CN 112663060A CN 202011377458 A CN202011377458 A CN 202011377458A CN 112663060 A CN112663060 A CN 112663060A
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- 238000000034 method Methods 0.000 claims description 16
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
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- 239000011592 zinc chloride Substances 0.000 claims description 5
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- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
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Abstract
The application discloses a composite cutter coating and a preparation method thereof. The composite cutter coating is sequentially coated with an interface layer, a CrN bonding layer and an AlCrN coating layer from inside to outside, wherein the interface layer is prepared by drying and coating matrix gel liquid prepared by mixing nano molybdenum disulfide and citric acid solution. The preparation method comprises the following steps: s1, taking the cutter, polishing, washing, standing and airing to obtain a surface treatment cutter; s2, mixing the metal complex sol solution and the matrix gel solution, coating the mixture on the surface of a cutter, and heating and calcining the mixture to obtain an interface layer; s3, depositing a CrN bonding layer by taking Cr as a target material; and S4, depositing an AlCrN coating layer by taking AlCr as a target material to prepare the composite cutter coating. According to the preparation method, the Al element is added, so that compact Al and Cr oxides can be formed at high temperature, the stress intensity of the external force action part is effectively reduced, and the phenomenon of coating damage is reduced.
Description
Technical Field
The invention belongs to the technical field of hard coatings, and particularly relates to a composite cutter coating and a preparation method thereof.
Background
With the development of manufacturing industry, a hard coating enters a new stage of a multi-element multilayer coating from an initial simple binary coating, the technical scheme of the Cr-AlN coating formed by adding Al element into a CrN coating is obviously improved in hardness, high temperature resistance and wear resistance, and the performance of the AlCrN coating formed after the Al atom number content exceeds 50% is further improved with the improvement of the Al element content, so that the application field of the ternary coating is greatly widened, and the ternary coating is expected to become a typical representative of the current ternary nitride coating.
Because the AlCrN hard coating of the existing cutter and the surface of the cutter are directly loaded by adopting a deposition scheme, in the actual use process, when the metal and the coating are under the action of external force, the hard coating is easy to fall off due to the poor bearing performance of the coating and the low bonding strength between the hard coating and the metal under the action of the external force.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art.
In view of the above, the present invention provides a composite tool coating, which has high bonding strength with a substrate, excellent coating bearing performance, and high bonding strength between a hard coating and a metal under an external force.
The invention also provides a preparation method of the composite cutter coating, which has simple preparation steps and improves the preparation efficiency.
The preparation method of the copper-based powder metallurgy friction material comprises an interface layer, a CrN bonding layer and an AlCrN coating layer which are sequentially coated from inside to outside, wherein the interface layer is prepared by drying and coating matrix gel liquid prepared by mixing nano molybdenum disulfide and citric acid solution.
According to the composite cutter coating provided by the embodiment of the invention, an interface layer taking molybdenum disulfide as a main body is coated between the hard coating and the cutter surface so as to improve the bonding performance between the cutter surface and the deposited hard coating, and the molybdenum disulfide is deposited on the material surface through a sol deposition scheme.
The composite tool coating according to embodiments of the present invention may also have the following additional technical features:
according to an embodiment of the present invention, the interface layer further includes a metal complex sol solution, and the preparation step of the metal complex sol solution is: (1) adding polyvinyl alcohol into dimethyl sulfoxide, stirring and mixing, and collecting a mixed solution; (2) stirring and mixing the mixed solution, the metal complex and sodium bisulfate, and heating and preserving heat for reaction treatment under the nitrogen atmosphere to obtain a mixed solution; (3) adding the mixed solution into acetone, stirring, mixing, standing, aging, filtering, collecting precipitate, and adding the precipitate into metal ion solution to obtain metal complex sol solution.
According to one embodiment of the invention, the metal ion solution comprises: any one of ferric chloride solution, zinc chloride solution or aluminum chloride solution.
According to one embodiment of the invention, the metal complex is 3, 4-dihydroxyphenylalanine.
The preparation method of the composite cutter coating according to the second aspect of the invention comprises the following steps: s1, taking the cutter, polishing, washing, standing and airing to obtain a surface treatment cutter; s2, stirring and mixing the metal complex sol solution and the matrix gel solution, dispersing, collecting the modified dispersed gel solution, coating the modified dispersed gel solution on the surface of a surface treatment cutter, drying, heating, keeping warm, calcining, standing and cooling to room temperature to obtain an interface layer; s3, after the boundary layer is coated, placing the cutter coated by the boundary layer on a rotating frame, and depositing a CrN bonding layer by taking Cr as a target; and S4, after the CrN bonding layer is deposited, depositing an AlCrN coating layer by taking AlCr as a target material to prepare the composite cutter coating.
According to an embodiment of the present invention, the sanding process of step S1 is performed by using 800#, 1200# and 1500# sandpaper, respectively.
According to an embodiment of the present invention, the temperature-increasing, heating, and heat-preserving calcination step of step S2 is: heating to 150-180 ℃ at a speed of 3 ℃/min, carrying out heat preservation treatment for 3-5 h, then heating to 300-350 ℃ at a speed of 1 ℃/min, and carrying out heat preservation heating.
According to an embodiment of the present invention, the CrN bonding layer of step S3 is deposited to a thickness of 0.05-0.10 μm and at a deposition temperature of 480-550 ℃.
According to an embodiment of the invention, the AlCrN cladding layer of step S4 is deposited with a thickness of 3-5 μm and a deposition temperature of 480-500 ℃.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a flow chart of a method of making a composite tool coating according to an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
The following describes the preparation method of the copper-based powder metallurgy friction material according to the embodiment of the invention in detail with reference to the attached drawings.
First, a composite tool coating according to an embodiment of the present invention includes: the interface layer, the CrN bonding layer and the AlCrN coating layer are sequentially coated from inside to outside, the interface layer is prepared by drying and coating matrix gel liquid prepared by mixing nano molybdenum disulfide and citric acid solution.
Therefore, the coating layer is arranged between the hard coating and the surface of the cutter, the interface layer which takes molybdenum disulfide as a main body is coated, the bonding performance between the surface of the cutter and the deposited hard coating is improved, the molybdenum disulfide is deposited on the surface of the material through a sol deposition scheme, on one hand, the bonding strength between the sol material and the surface of the cutter material is higher, the bonding strength between the surface of the cutter and the coating can be obviously improved, on the other hand, the hard coating is under the action of external force, the molybdenum disulfide has good high bearing performance, the phenomenon of coating damage caused by stress concentration generated under the action of the external force can be reduced through the unloading effect of the high bearing performance of the molybdenum disulfide, the bonding strength between the AlCrN cutter coating and the surface of the cutter is effectively improved, and the shedding phenomenon of the AlCrN hard coating is reduced.
According to an embodiment of the present invention, the interface layer further includes a metal complex sol solution, and the preparation step of the metal complex sol solution is: (1) adding polyvinyl alcohol into dimethyl sulfoxide, stirring and mixing, and collecting a mixed solution; (2) stirring and mixing the mixed solution, the metal complex and sodium bisulfate, and heating and preserving heat for reaction treatment under the nitrogen atmosphere to obtain a mixed solution; (3) adding the mixed solution into acetone, stirring, mixing, standing, aging, filtering, collecting precipitate, and adding the precipitate into metal ion solution to obtain metal complex sol solution.
By adopting the technical scheme, the metal complex sol solution is modified and added, so that the bonding performance between the metal material and the gel material can be effectively improved, and on the basis, the high-bonding-property metal complex sol can effectively improve the bonding strength between the interface layer and the surface of the cutter, thereby improving the bonding strength between the AlCrN cutter coating and the surface of the cutter and reducing the shedding phenomenon of the AlCrN hard coating.
In some embodiments of the invention, the metal ion solution comprises: any one of ferric chloride solution, zinc chloride solution or aluminum chloride solution.
Therefore, by adopting the metal ion solution as the addition modification material, good sol performance can be effectively formed between the metal ion solution and the metal complex, the prepared sol material can effectively improve the density of the interface layer, so that the compactness of the interface layer is effectively improved, the interface layer can bear higher external pressure, and the shedding phenomenon of the AlCrN hard coating is reduced.
Further, the metal complex is 3, 4-dihydroxyphenylalanine.
By adopting the technical scheme, as the 3, 4-dihydroxyphenylalanine is adopted for modification, the material has the capabilities of quick adhesion and chemical crosslinking solidification, and can be effectively adhered to the surface of a cutter material after being added into the sol, and meanwhile, the 3, 4-dihydroxyphenylalanine and metal ions also have good complexing capability, so that the compactness of an interface layer is effectively improved, and the shedding phenomenon of an AlCrN hard coating is improved.
In a second aspect, the present application provides a method of making a composite tool coating, the method comprising: s1, taking the cutter, polishing, washing, standing and airing to obtain a surface treatment cutter; s2, stirring and mixing the metal complex sol solution and the matrix gel solution, dispersing, collecting the modified dispersed gel solution, coating the modified dispersed gel solution on the surface of a surface treatment cutter, drying, heating, keeping warm, calcining, standing and cooling to room temperature to obtain an interface layer; s3, after the boundary layer is coated, placing the cutter coated by the boundary layer on a rotating frame, and depositing a CrN bonding layer by taking Cr as a target; and S4, after the CrN bonding layer is deposited, depositing an AlCrN coating layer by taking AlCr as a target material to prepare the composite cutter coating.
Therefore, the addition of Al element is adopted in the method, the coating crystal grains can be refined, the nitride lattice distortion is caused to form a strengthening effect, compact Al and Cr oxides can be formed at high temperature, the effect of protecting the internal coating is achieved, on the basis, the interface layer arranged between the surface of the cutter and the deposition coating is molybdenum disulfide, and due to the excellent structural performance, when the hard coating is acted by external force, the stress intensity of the external force action part is effectively reduced, so that the phenomenon that the hard coating is damaged due to stress concentration of the action part is reduced.
Alternatively, the sanding process in step S1 is performed by using 800#, 1200# and 1500# sandpaper, respectively.
The abrasive paper with multiple specifications is adopted for polishing, the oxide layer on the surface of the cutter can be thoroughly treated, and thus, the surface of the cutter and the interface layer can form direct contact and good bonding performance in the subsequent coating process.
In some embodiments of the present invention, the temperature-increasing, heating, and heat-preserving calcination step in step S2 is: heating to 150-180 ℃ at a speed of 3 ℃/min, carrying out heat preservation treatment for 3-5 h, then heating to 300-350 ℃ at a speed of 1 ℃/min, and carrying out heat preservation heating.
The scheme of temperature programming and heating calcination is adopted, the surface of the cutter is coated with the interface layer, the whole scheme is simple and feasible, the cost is lower, the operation steps are simple, the preparation cost is effectively reduced, and meanwhile, the interface layer and the surface of the cutter can effectively form a good coating load through high-temperature calcination treatment, so that the bonding performance of a subsequent coating and the surface of the cutter is improved.
In some embodiments of the present invention, the CrN bonding layer of step S3 is deposited to a thickness of 0.05-0.10 μm and at a deposition temperature of 480-550 ℃.
By adopting the technical scheme, the thickness of the CrN bonding layer is optimized, and the CrN bonding layer is used as a bonding layer with lower thickness and optimizes the thickness and size due to high hardness and low friction coefficient of CrN and small difference of physical and mechanical performance parameters of hard alloy, so that the structural effect of the whole coating caused by the excessively thick thickness of the bonding layer can be effectively reduced, the optimized CrN bonding layer can effectively improve the structural performance of a hard coating material, effectively embody the effects of high hardness and low friction coefficient of the hard coating material, and further improve the mechanical strength and mechanical performance of the coated coating after being bonded with the surface of a cutter.
According to an embodiment of the invention, the AlCrN cladding layer of step S4 is deposited with a thickness of 3-5 μm and a deposition temperature of 480-500 ℃.
By adopting the technical scheme, the AlCrN coating layer is arranged to be the outermost layer structure of the hard coating, and because the Al element is added into the coating, the addition of the Al element can refine coating crystal grains, simultaneously cause nitride crystal lattice distortion to form a strengthening effect, and can form compact Al and Cr oxides at high temperature, thereby having the function of protecting the internal coating, effectively improving the strength of the hard coating, enabling the hard coating to have excellent hardness performance, and further generating good impact resistance effect on the collision of high-hardness substances in use.
In summary, in the present application, an interface layer mainly composed of molybdenum disulfide is coated between a hard coating and a tool surface to improve the bonding performance between the tool surface and a deposited hard coating, and molybdenum disulfide is deposited on the material surface through a sol deposition scheme, so that on one hand, the bonding strength between a sol material and the tool material surface is high, and the bonding strength between the tool surface and the coating can be significantly improved, and on the other hand, under the action of an external force, the hard coating has a good high bearing performance due to the molybdenum disulfide, and the phenomenon of coating damage caused by stress concentration generated under the action of the external force can be reduced through the unloading effect of the high bearing performance of the molybdenum disulfide, so that the bonding strength between an AlCrN tool coating and the tool surface is effectively improved, and the phenomenon of shedding of the AlCrN hard coating is reduced.
By adopting the metal ion solution as the addition modification material, good sol performance can be effectively formed between the metal ion solution and the metal complex, and the prepared sol material can effectively improve the density of the interface layer, thereby effectively improving the compactness of the interface layer, enabling the interface layer to bear higher external pressure and further reducing the shedding phenomenon of the AlCrN hard coating.
By adding the Al element into the coating layer, the addition of the Al element can refine coating crystal grains, cause nitride lattice distortion and form a strengthening effect, and can form compact Al and Cr oxides at high temperature, so that the coating has the effect of protecting an internal coating, the strength of the hard coating is effectively improved, the hard coating has excellent hardness, and a good impact resistance effect can be generated on the collision of high-hardness substances in use.
The composite tool coating and the preparation method thereof according to the embodiments of the present invention will be described in detail with reference to specific embodiments.
Example 1
Adding polyvinyl alcohol into dimethyl sulfoxide according to a mass ratio of 1:25, stirring and mixing and collecting a mixed solution, adding the mixed solution into a three-neck flask, stirring and mixing, weighing 45 parts of the mixed solution, 3 parts of 3, 4-dihydroxyphenylalanine and 3 parts of sodium bisulfate respectively according to parts by weight, stirring and mixing, keeping the temperature at 75 ℃ under a nitrogen atmosphere for 20 hours, standing and cooling to room temperature, collecting the mixed solution, adding the mixed solution into acetone according to a volume ratio of 1:8, stirring and mixing, standing and aging, filtering and collecting precipitates, adding the precipitates to an iron chloride solution with a mass fraction of 5% according to a mass ratio of 1:10, placing the iron chloride solution into a beaker, stirring and mixing, and collecting a metal complex sol solution;
adding nano molybdenum disulfide into 1.3mol/L citric acid solution according to the mass ratio of 1:8, carrying out heat preservation reaction for 3 hours at 75 ℃, standing and cooling to room temperature to obtain matrix gel liquid, adding the metal complex sol liquid into the matrix gel liquid at room temperature, and carrying out ultrasonic dispersion for 10 minutes at 250W to obtain modified dispersed gel liquid;
taking a cutter, respectively polishing with 800#, 1200# and 1500# abrasive paper, after the treatment is finished, washing with absolute ethyl alcohol for 3 times, naturally drying and collecting to obtain a surface treatment cutter;
coating the modified dispersion gel liquid on the surface of a surface treatment cutter, drying the surface treatment cutter, placing the surface treatment cutter in a 100 ℃ oven for drying for 3h, heating to 150 ℃ at the speed of 3 ℃/min, carrying out heat preservation treatment for 3h, heating to 300 ℃ at the speed of 1 ℃/min, carrying out heat preservation heating, standing and cooling to room temperature to obtain a surface-coated modified cutter;
placing the surface-coated modified tool on a rotating frame, placing the rotating frame in a closed coating device, introducing nitrogen to remove air, vacuumizing to 65Pa, heating to 480 ℃, performing heat preservation treatment, performing deposition treatment under the arc current of 400A by taking Cr as a target material, depositing a 0.05-micron CrN bonding layer on the surface-coated modified tool, and then coating an AlCrN coating layer at 480 ℃ and the pressure of 65 to obtain the composite tool coating.
Example 2
Adding polyvinyl alcohol into dimethyl sulfoxide according to a mass ratio of 1:25, stirring and mixing and collecting a mixed solution, adding the mixed solution into a three-neck flask, stirring and mixing, weighing 47 parts of the mixed solution, 4 parts of 3, 4-dihydroxyphenylalanine and 4 parts of sodium bisulfate respectively according to parts by weight, stirring and mixing, keeping the temperature at 77 ℃ under a nitrogen atmosphere for reaction for 22 hours, standing and cooling to room temperature, collecting the mixed solution, adding the mixed solution into acetone according to a volume ratio of 1:8, stirring and mixing, standing and aging, filtering and collecting precipitates, adding the precipitates to an iron chloride solution with a mass fraction of 5% according to a mass ratio of 1:10, placing the iron chloride solution into a beaker, stirring and mixing, and collecting a metal complex sol solution;
adding nano molybdenum disulfide into 1.3mol/L citric acid solution according to the mass ratio of 1:8, carrying out heat preservation reaction for 4 hours at the temperature of 80 ℃, standing and cooling to room temperature to obtain matrix gel liquid, adding the metal complex sol liquid into the matrix gel liquid at the room temperature, and carrying out ultrasonic dispersion for 12 minutes at 275W to obtain modified dispersed gel liquid;
taking a cutter, respectively polishing with 800#, 1200# and 1500# abrasive paper, after the treatment is finished, washing with absolute ethyl alcohol for 4 times, naturally drying and collecting to obtain a surface treatment cutter;
coating the modified dispersion gel liquid on the surface of a surface treatment cutter, drying the surface treatment cutter in a 105 ℃ oven for 4h, heating to 165 ℃ at the speed of 3 ℃/min, carrying out heat preservation treatment for 4h, heating to 325 ℃ at the speed of 1 ℃/min, carrying out heat preservation heating, standing and cooling to room temperature to obtain a surface-coated modified cutter;
placing the surface-coated modified tool on a rotating frame, placing the rotating frame in a closed coating device, introducing nitrogen to remove air, vacuumizing to 72Pa, heating to 525 ℃, performing heat preservation treatment, depositing under the condition that the arc current is 450A, depositing a 0.07-micron CrN bonding layer on the surface-coated modified tool, and performing secondary deposition treatment on a 4-micron AlCrN coating layer under the condition that the arc current is 450A and the temperature is 490 ℃, the pressure is 72Pa and the pressure is 72 AlCr is used as a target material to prepare the composite tool coating.
Example 3
Adding polyvinyl alcohol into dimethyl sulfoxide according to a mass ratio of 1:25, stirring and mixing and collecting a mixed solution, adding the mixed solution into a three-neck flask, stirring and mixing, weighing 50 parts of the mixed solution, 5 parts of 3, 4-dihydroxyphenylalanine and 5 parts of sodium bisulfate respectively according to parts by weight, stirring and mixing, keeping the temperature at 80 ℃ under a nitrogen atmosphere for 24 hours, standing and cooling to room temperature, collecting the mixed solution, adding the mixed solution into acetone according to a volume ratio of 1:8, stirring and mixing, standing and aging, filtering and collecting precipitates, adding the precipitates to an iron chloride solution with a mass fraction of 5% according to a mass ratio of 1:10, placing the iron chloride solution into a beaker, stirring and mixing, and collecting a metal complex sol solution;
adding nano molybdenum disulfide into 1.3mol/L citric acid solution according to the mass ratio of 1:8, carrying out heat preservation reaction for 5 hours at 85 ℃, standing and cooling to room temperature to obtain matrix gel liquid, adding the metal complex sol liquid into the matrix gel liquid at room temperature, and carrying out ultrasonic dispersion for 15min at 300W to obtain modified dispersed gel liquid;
taking a cutter, respectively polishing with 800#, 1200# and 1500# abrasive paper, after the treatment is finished, washing with absolute ethyl alcohol for 5 times, naturally drying and collecting to obtain a surface treatment cutter;
coating the modified dispersion gel liquid on the surface of a surface treatment cutter, drying the surface treatment cutter, placing the surface treatment cutter in a 110 ℃ oven for drying for 5h, heating to 180 ℃ at the speed of 3 ℃/min, carrying out heat preservation treatment for 5h, heating to 350 ℃ at the speed of 1 ℃/min, carrying out heat preservation heating, standing and cooling to room temperature to obtain a surface-coated modified cutter;
placing the surface-coated modified cutter on a rotating frame, placing the rotating frame in a closed coating device, introducing nitrogen to remove air, vacuumizing to 80Pa, heating to 550 ℃, performing heat preservation treatment, performing deposition treatment under the arc current of 500A by taking Cr as a target material, depositing a 0.10 mu m CrN bonding layer on the surface-coated modified cutter, performing secondary deposition treatment on a 5 mu m AlCrN coating layer under the arc current of 500A by taking AlCr as the target material at 500 ℃ and 80Pa, and preparing the composite cutter coating.
Example 4
In example 4, a zinc chloride solution was used in place of the iron chloride solution in example 1, and the other conditions and component ratios were the same as in example 1.
Example 5
In example 5, an aluminum chloride solution was used in place of the ferric chloride solution in example 1, and the other conditions and component ratios were the same as in example 1.
Performance test
The performance tests of examples 1 to 5 were respectively carried out, and the coating film-substrate bonding force, the frictional wear performance of the coating, the micro-hardness of the coating and the bonding strength between the coating and the substrate of the cutter coating prepared in examples 1 to 5 were tested.
Detection method/test method
(1) Bonding strength: the bonding force of the hard coating is represented by adopting a Rockwell indentation method, the load of a hardness tester is 150kg, the loading time is 15s, the grade of the film-substrate bonding force can be qualitatively judged through the indentation morphology of the film surface, and the judgment standard is the German VDI3198 standard. In the experiment, the indentation method adopts LC-200R type Rockwell hardness tester equipment of Japanese FT, then the appearance of the Rockwell indentation is represented by a high-power scanning electron microscope and a Smartzoom5 three-dimensional digital microscope of Zeiss, and the combination grade HF is judged by combining the existing standard through the crack or film falling condition in the middle or around the indentation.
(2) Coating film-based bonding force: measured by adopting a WS-2005 type coating adhesive force automatic scratch tester, the scratch length is 4mm, and the test load is 70N; the measurement mode is as follows: acoustic signals, friction; the operation mode is as follows: carrying out dynamic loading; scratching mode: and (6) repeatedly scratching. Comprehensively judging the film-base binding force of the coating by acoustic emission signals, friction curves and the position of the coating laceration in each test, testing each coating four times, and taking the average value of the test results of the four times;
(3) the frictional wear performance of the coating is as follows: an HSR-2M reciprocating/rotating friction abrasion tester is adopted to carry out a dry friction abrasion test on the coating, the friction form adopts a reciprocating type, the specification of the sensor is 1-10N, and a friction pair adopts Si3N4 ceramic balls with the diameter of 4mm and the reciprocating length of 5 mm. The measured parameters include friction coefficient and friction force, heating range of the sample heating furnace: the temperature is between room temperature and 300 ℃, and the highest temperature is set to be 250 ℃ when the paint is used;
(4) microhardness of coating: the microhardness of the coating was measured using a microhardness tester of the HXD-1000TMD type. Test parameters are as follows: a diamond regular quadrangular pyramid pressure head of 136 degrees, a load of 50g and a loading time of 10 s. Firstly, loading on a test piece according to test parameters, unloading the load after the loading is finished, then measuring the length of a diagonal line of the test piece under an optical microscope, and finally calculating the microhardness of the test piece according to a Vickers hardness calculation formula.
The specific detection results are shown in the following table 1:
TABLE 1 Performance test Table
Referring to table 1 for comparison of performance tests, it can be found that:
comparing the performances of the examples 1 to 3, wherein the comprehensive comparison of microhardness, coating film-base binding force, friction coefficient and binding strength shows that the performance of the example 3 is the best, and the average friction coefficient and microhardness all affect the service performance of the tool coating, and it can also be said that the service life of the coating and the binding strength with the base layer of the example 3 are the best in the examples 1 to 3, because the proportion of the materials added in the example 3 is the highest, and the technical scheme of the application is reflected from the side surface.
Comparing the performances of examples 1 and 4-5, as different metal ion solutions are used in examples 4-5, compared with the performance test data in table 1, the aluminum chloride solution used in example 5 has the best performance, because the aluminum chloride solution used in the technical scheme of the present application is modified by adding Al element, and the aluminum chloride solution used in the interface layer is prepared as the raw material, the bonding performance between the interface layer and the coating layer can be effectively improved, so that the bonding strength of the interface layer is further improved, and the performance of example 5 is the best, and meanwhile, the zinc chloride solution in example 4 has higher activity, and also can effectively improve the bonding strength between the interface layer and the coating layer and the base material, so compared with example 1, the performance of example 1 is also higher than that of example 1.
Comparative example
Comparative examples 1 to 3
In comparative examples 1 to 3, the tool surface was not coated with an interface layer but was directly coated with a coating layer, and the other conditions and the component ratios were the same as in examples 1 to 3.
Comparative examples 4 to 6
Comparative examples 4 to 6 were coated without an interface layer prepared from a metal complex sol solution, and the other conditions and component ratios were the same as in examples 1 to 3.
Comparative examples 7 to 9
Comparative examples 7 to 9 in the preparation of AlCrN clad layers by deposition, the deposition thickness was controlled to 2 μm, and the other conditions and the component ratios were the same as in examples 1 to 3.
Comparative examples 10 to 12
Comparative examples 10 to 12 when a CrN bonding layer was deposited, the thickness of the deposited CrN bonding layer was 0.2. mu.m, and the remaining conditions and the component ratios were the same as those in examples 1 to 3.
Performance test
And respectively testing the cutter coatings prepared in the comparative examples 1-12, and specifically testing the coating film-substrate binding force, the frictional wear performance of the coating, the microhardness of the coating and the binding strength between the coating and the substrate.
Detection method/test method
(1) Bonding strength: for comparative example 1-12, the bonding force of the hard coating is represented by adopting a Rockwell indentation method, the load of a hardness tester is 150kg, the loading time is 15s, the grade of the film-based bonding force of the film can be qualitatively judged according to the indentation morphology of the surface of the film, and the judgment standard is the German VDI3198 standard. In the experiment, the indentation method adopts LC-200R type Rockwell hardness tester equipment of Japanese FT, then the appearance of the Rockwell indentation is represented by a high-power scanning electron microscope and a Smartzoom5 three-dimensional digital microscope of Zeiss, and the combination grade HF is judged by combining the existing standard through the crack or film falling condition in the middle or around the indentation.
(2) Coating film-based bonding force: measured by adopting a WS-2005 type coating adhesive force automatic scratch tester, the scratch length is 4mm, and the test load is 70N; the measurement mode is as follows: acoustic signals, friction; the operation mode is as follows: carrying out dynamic loading; scratching mode: and (6) repeatedly scratching. Comprehensively judging the film-base binding force of the coating by acoustic emission signals, friction curves and the position of the coating laceration in each test, testing each coating four times, and taking the average value of the test results of the four times;
(2) the frictional wear performance of the coating is as follows: an HSR-2M reciprocating/rotating friction abrasion tester is adopted to carry out a dry friction abrasion test on the coating, the friction form adopts a reciprocating type, the specification of the sensor is 1-10N, and a friction pair adopts Si3N4 ceramic balls with the diameter of 4mm and the reciprocating length of 5 mm. The measured parameters include friction coefficient and friction force, heating range of the sample heating furnace: the temperature is between room temperature and 300 ℃, and the highest temperature is set to be 250 ℃ when the paint is used;
(4) microhardness of coating: the microhardness of the coating was measured using a microhardness tester of the HXD-1000TMD type. Test parameters are as follows: a diamond regular quadrangular pyramid pressure head of 136 degrees, a load of 50g and a loading time of 10 s. Firstly, loading on a test piece according to test parameters, unloading the load after the loading is finished, then measuring the length of a diagonal line of the test piece under an optical microscope, and finally calculating the microhardness of the test piece according to a Vickers hardness calculation formula.
The specific detection results are shown in the following table 2:
TABLE 2 Performance test Table
The performance test table of table 2 was analyzed as follows:
comparing the comparative examples 1-3 with the examples 1-3, the microhardness and the bonding force performance of the hard coating of the cutter, which is prepared without adopting the interface layer, in the comparative examples are obviously reduced, which shows that the interface layer adopted by the method can obviously improve the bonding strength between the surface of the cutter and the hard coating, so that the phenomenon of coating damage caused by stress concentration generated under the action of external force is reduced under the action of the high-bearing-performance unloading force of molybdenum disulfide on the hard coating under the action of the external force, thereby effectively improving the bonding strength between the AlCrN cutter coating and the surface of the cutter and reducing the shedding phenomenon of the AlCrN hard coating.
Comparing comparative examples 4-6 with examples 1-3, the comparative examples do not adopt metal complex sol solution to add, so that the performance of the comparative examples is reduced, the bonding performance of the interface layer and the surface of the cutter is poor, and the method proves that the adhesion can be effectively carried out on the surface of the cutter material, so that the compactness performance of the interface layer is effectively improved, and the shedding phenomenon of the AlCrN hard coating is improved.
Comparing the comparative examples 7-9 with the examples 1-3, the deposition thickness is controlled to be 2 μm when the AlCrN coating layer is prepared by deposition in the comparative examples, and the hardness of the AlCrN coating layer is obviously reduced in the actual use process due to the reduction of the thickness of the AlCrN coating layer, which shows that the optimization of the thickness of the AlCrN can effectively improve the strength of the hard coating layer and enable the hard coating layer to have excellent hardness performance, so that good impact resistance effect can be generated on the collision of high-hardness substances in use.
Comparing the comparative examples 10-12 with the examples 1-3, the thickness of the bonding layer is increased in the comparative examples, so that the material performance is reduced, which shows that the optimized bonding layer thickness in the technical scheme effectively reduces the structural effect of the whole coating caused by the excessively thick bonding layer thickness, so that the optimized CrN bonding layer not only can effectively improve the structural performance of the hard coating material, but also effectively embodies the effects of high hardness and low friction coefficient.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (9)
1. The composite cutter coating is characterized by comprising an interface layer, a CrN bonding layer and an AlCrN coating layer which are sequentially coated from inside to outside, wherein the interface layer is prepared by drying and coating matrix gel liquid prepared by mixing nano molybdenum disulfide and citric acid solution.
2. The composite cutter coating of claim 1, wherein the interface layer further comprises a metal complex sol solution, and the metal complex sol solution is prepared by the steps of:
(1) adding polyvinyl alcohol into dimethyl sulfoxide, stirring and mixing, and collecting a mixed solution;
(2) stirring and mixing the mixed solution, the metal complex and sodium bisulfate, and heating and preserving heat for reaction treatment under the nitrogen atmosphere to obtain a mixed solution;
(3) adding the mixed solution into acetone, stirring, mixing, standing, aging, filtering, collecting precipitate, and adding the precipitate into metal ion solution to obtain metal complex sol solution.
3. The composite tool coating of claim 2, wherein the metal ion solution comprises: any one of ferric chloride solution, zinc chloride solution or aluminum chloride solution.
4. The composite tool coating of claim 2 wherein the metal complex is 3, 4-dihydroxyphenylalanine.
5. A preparation method of a composite cutter coating is characterized by comprising the following steps:
s1, taking the cutter, polishing, washing, standing and airing to obtain a surface treatment cutter;
s2, stirring and mixing the metal complex sol solution and the matrix gel solution, dispersing, collecting the modified dispersed gel solution, coating the modified dispersed gel solution on the surface of a surface treatment cutter, drying, heating, keeping warm, calcining, standing and cooling to room temperature to obtain an interface layer;
s3, after the boundary layer is coated, placing the cutter coated by the boundary layer on a rotating frame, and depositing a CrN bonding layer by taking Cr as a target;
and S4, after the CrN bonding layer is deposited, depositing an AlCrN coating layer by taking AlCr as a target material to prepare the composite cutter coating.
6. The method of claim 5, wherein the step S1 is performed by using 800#, 1200# and 1500# sandpaper.
7. The method for preparing the composite cutter coating according to claim 5, wherein the step of heating, keeping warm and calcining in the step S2 comprises the following steps: heating to 150-180 ℃ at a speed of 3 ℃/min, carrying out heat preservation treatment for 3-5 h, then heating to 300-350 ℃ at a speed of 1 ℃/min, and carrying out heat preservation heating.
8. The method for preparing the composite tool coating according to claim 5, wherein the CrN bonding layer of step S3 is deposited at a thickness of 0.05-0.10 μm and a deposition temperature of 480-550 ℃.
9. The method for preparing the composite cutter coating according to claim 5, wherein the AlCrN coating layer of step S4 is deposited at a deposition thickness of 3-5 μm and a deposition temperature of 480-500 ℃.
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