CN112662996A - Stable load type nano composite cutter coating and preparation method thereof - Google Patents
Stable load type nano composite cutter coating and preparation method thereof Download PDFInfo
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Abstract
The application discloses a stable load type nano composite cutter coating and a preparation method thereof. The stable load type nano composite cutter coating comprises a CrN bonding layer, an AlTiN transition layer, an AlTiN/TiSiN supporting layer and a TiSiN functional layer which are sequentially deposited and loaded from inside to outside, wherein the CrN bonding layer is deposited and loaded to one side of the cutter after surface treatment; the coating with the structure improves the bonding strength between the hard coating and the substrate, and then improves the load performance of the coating and prolongs the service life of the cutter coating through surface treatment. The preparation method comprises the following steps: s1, bombarding and activating the surface of the cutter by metal ions; s2, depositing a CrN bonding layer on the activated surface of the cutter; s3, depositing an AlTiN transition layer on the surface of the CrN combination layer and then depositing an AlTiN/TiSiN supporting layer; and S4, finally, depositing a TiSiN functional layer on the surface of the AlTiN/TiSiN support layer to obtain the stable load type nano composite cutter coating. The preparation method has the advantages of simplicity, easiness in operation and wide application range.
Description
Technical Field
The invention belongs to the technical field of hard coatings, and particularly relates to a stable load type nano composite cutter coating and a preparation method thereof.
Background
The hard coat material is selected from simple metal nitride (carbide) coatings such as: TiN, CrN, TiC developed into nano multilayer coatings such as: TiAlN/TiN, TiAlN/AlCrSiN and the like, and has been widely applied in industries such as tools, molds, decoration and the like. When processing difficult-to-process materials with high hardness, high toughness and the like, the cutting force is large, the cutting temperature is high, and the cutter is seriously abraded, so that the cutting service life of the cutter is greatly influenced. Conventional machining uses cutting fluid to cool the tool to improve tool cutting life. However, the presence of many harmful substances in the cutting fluid causes environmental pollution. Dry cutting is the most environmentally friendly cutting method. However, the temperature of the cutter-chip interface can reach over 900 ℃ in a dry cutting state, which puts higher requirements on the high-temperature oxidation resistance of the cutter. The coated cutter combines the excellent wear resistance and oxidation resistance of the coating material and the good toughness of the base material, the cutting life of the cutter is obviously prolonged, and meanwhile, the processing precision and the processing efficiency of parts are greatly improved. Thanks to these advantages, the coating technology has developed rapidly.
In the prior art, the invention patent with the grant publication number of CN103789726B in China can be referred to, and the AlTiCrN/MoN nano multilayer coating firmly combined with the surface of a tool and the preparation method thereof are disclosed, wherein the multilayer coating comprises four layers from inside to outside on the surface of the tool, namely a Ti combining layer (2), a TiN gradient structural layer (3), an AlTiCrN supporting layer (4) and an AlTiCrN/MoN functional layer (5) in sequence; the method comprises the steps of pretreating and heating a tool matrix (1); plasma cleaning; evaporating a Ti bonding layer (2); evaporating a TiN gradient structure layer (3); the AlTiCrN support layer (4) and the AlTiCrN/MoN functional layer (5) are deposited in a sputtering mode.
In view of the above-mentioned related technologies, the applicant believes that the existing hard coating of the tool is prepared by a scheme of direct material plating and sputter deposition, and the bonding strength between the hard coating and the surface of the tool material is not high, so that the bonding load performance between the tool coating and the tool surface is not good, and the service life of the tool coating is reduced.
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 stably loaded nanocomposite tool coating, which improves the combined load performance between the tool coating and the tool surface and prolongs the service life of the tool coating.
The invention also provides a preparation method of the composite cutter coating, which has simple preparation steps and improves the preparation efficiency.
The stable load type nano composite cutter coating according to the embodiment of the invention 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 stable load type nano composite cutter coating disclosed by the embodiment of the invention, a multilayer structure of a CrN bonding layer, an AlTiN transition layer, an AlTiN/TiSiN supporting layer and a TiSiN functional layer is adopted for coating, the coating structure of the multilayer structure is beneficial to reducing the internal stress of a hard coating and improving the bonding strength between the hard coating and a substrate, in addition, the coating of the multilayer structure has a template effect, and a superhard effect that the hardness of the coating is obviously improved can occur.
The load-stabilizing composite tool coating according to embodiments of the present invention may also have the following additional technical features:
according to one embodiment of the invention, the surface treatment step is: (1) sanding with abrasive paper to remove an oxide layer, washing, and etching the surface of the cutter; (2) and sanding the etched cutter, washing and drying to prepare the cutter surface treatment layer.
According to one embodiment of the present invention, the sanding process is performed by sequentially sanding 800#, 1200#, and 1500 #.
According to one embodiment of the invention, the etching process comprises: (1) taking two polished cutters as a cathode and an anode respectively, placing the two cutters in etching liquid, and etching at room temperature; (2) after the etching is finished, taking out the etching cutter, washing and drying to obtain an etched cutter; (3) and placing the etched cutter in a sanding device, sanding, washing and drying to obtain the surface treatment cutter.
According to one embodiment of the invention, the etching solution is prepared by stirring and mixing aluminum nitrate, palmitic acid and absolute ethyl alcohol according to a mass ratio of 1:5: 10.
According to one embodiment of the invention, the thickness of the CrN bonding layer is 0.2-0.3 μm, and the CrN bonding layer comprises 40-50% of Cr and 50-60% of N in atomic mass ratio.
According to one embodiment of the invention, the TiSiN functional layer comprises 5-10% of Si, 35-40% of Ti and 50-60% of N in atomic mass ratio.
The preparation method of the stable load type composite cutter coating according to the embodiment of the second aspect of the invention comprises the following steps: s1, placing the surface treatment cutter in a deposition vacuum chamber, vacuumizing to 30-50 Pa, heating to 375-425 ℃, carrying out heat preservation and preheating treatment, reducing the pressure to 2-5 Pa in a nitrogen atmosphere, and then bombarding and activating the surface of the cutter by metal ions; s2, after the surface of the cutter is activated, depositing a CrN bonding layer on the activated surface of the cutter in a nitrogen atmosphere; s3, after the CrN combination layer is deposited, depositing an AlTiN transition layer on the surface of the CrN combination layer by taking AlTi as a target material, and after the deposition is finished, depositing an AlTiN/TiSiN supporting layer on the surface of the AlTiN transition layer by taking TiSi and AlTi as target materials; s4, depositing a TiSiN functional layer on the surface of the AlTiN/TiSiN support layer by taking TiSi as a target material, and thus obtaining the stable load type nano composite cutter coating.
According to an embodiment of the invention, the thickness of the AlTiN/TiSiN supporting layer in the step S3 is 0.5-3.5 μm, the nitrogen flow rate for depositing the AlTiN/TiSiN supporting layer is 400-500 Sccm, and the substrate bias voltage is 40-60V.
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 stable-loading 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 stably loaded nanocomposite tool coatings according to embodiments of the present invention are described in detail below with reference to the accompanying 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, according to the stable load type nano composite tool coating provided by the embodiment of the invention, the multilayer structure of the CrN bonding layer, the AlTiN transition layer, the AlTiN/TiSiN supporting layer and the TiSiN functional layer is adopted for coating, the coating structure of the multilayer structure is beneficial to reducing the internal stress of the hard coating and improving the bonding strength between the hard coating and the substrate, in addition, the coating of the multilayer structure has a template effect, and a superhard effect that the hardness of the coating is obviously improved can occur.
Further, the surface treatment step is as follows: (1) sanding with abrasive paper to remove an oxide layer, washing, and etching the surface of the cutter; (2) and sanding the etched cutter, washing and drying to prepare the cutter surface treatment layer.
This application adopts abrasive paper to polish earlier and gets rid of the oxide layer, after the rethread sculpture is handled, the scheme of handling of sanding is handled the cutter surface, the cutter surface after abrasive paper is handled, the oxide layer is effectively got rid of, carry out the sculpture to it again, make its surface form anomalous pore structure, because these pore uniformity can not be good, lead to after the deposit of actual coating, CrN anchor coat structure is inhomogeneous, the CrN anchor coat mechanical properties who forms is not good, so to sand it and handle, through sanding processing back, make the structure on inhomogeneous sculpture surface become even smooth surface, through the sculpture pore of gomphosis in this even smooth surface, form good anchoring effect to the coating, improve the binding load performance on cutter coating and cutter surface, and prolong the life of cutter coating.
According to one embodiment of the present invention, the sanding process is performed by sequentially sanding 800#, 1200#, and 1500 #.
By adopting the technical scheme, the abrasive paper with multiple specifications is adopted for polishing, so that the oxide layer on the surface of the cutter can be thoroughly treated, a good etching effect can be formed in the subsequent etching process, and the improvement of the bonding performance of the subsequent coating and the surface of the cutter is facilitated.
According to one embodiment of the invention, the etching process comprises: (1) taking two polished cutters as a cathode and an anode respectively, placing the two cutters in etching liquid, and etching at room temperature; (2) after the etching is finished, taking out the etching cutter, washing and drying to obtain an etched cutter; (3) and placing the etched cutter in a sanding device, sanding, washing and drying to obtain the surface treatment cutter.
By adopting the technical scheme, the scheme of polishing the cutter after etching the cutter is characterized in that the etched pore channel formed on the surface of the cutter is trimmed through polishing treatment, so that the smoothness of the surface of the cutter is improved, and a good load effect can be formed on the surface of the cutter in the subsequent deposition process.
Further, the etching solution is prepared by stirring and mixing aluminum nitrate, palmitic acid and absolute ethyl alcohol according to the mass ratio of 1:5: 10.
As the application adopts the structure, Al ions in the aluminum nitrate exist in the form of Al3+ in the electrolyte, so that Al3+ is combined with palmitic acid and loaded on the surface of the cutter, and the structure is matched with a pore structure formed by etching, so that the roughness of the surface of the cutter is improved, the combination load performance of the cutter coating and the surface of the cutter is effectively improved, and the service life of the cutter coating is prolonged.
In some embodiments of the invention, the thickness of the CrN bonding layer is 0.2-0.3 μm, and the CrN bonding layer comprises 40-50% of Cr and 50-60% of N by atomic mass ratio.
Through adopting above-mentioned technical scheme, optimized CrN anchor coat thickness, made it both can form good boundary layer effect on transition layer and cutter surface, improved the bonding strength between the two, prevented the higher anchor coat of thickness simultaneously, influenced the structural effect of monolithic coating.
Further, the TiSiN functional layer comprises 5-10% of Si, 35-40% of Ti and 50-60% of N in atomic mass ratio.
Therefore, 5-10% of Si is added into the functional layer, and the Si element can remarkably improve the hardness and the high-temperature resistance of the coating material, so that the local nano hardness of the functional layer can reach more than 4000, and the high-temperature resistance can also reach 1100 ℃.
In a second aspect, the present application provides a method for preparing a stably-loaded nanocomposite tool coating, which comprises the following steps: s1, placing the surface treatment cutter in a deposition vacuum chamber, vacuumizing to 30-50 Pa, heating to 375-425 ℃, carrying out heat preservation and preheating treatment, reducing the pressure to 2-5 Pa in a nitrogen atmosphere, and then bombarding and activating the surface of the cutter by metal ions; s2, after the surface of the cutter is activated, depositing a CrN bonding layer on the activated surface of the cutter in a nitrogen atmosphere; s3, after the CrN combination layer is deposited, depositing an AlTiN transition layer on the surface of the CrN combination layer by taking AlTi as a target material, and after the deposition is finished, depositing an AlTiN/TiSiN supporting layer on the surface of the AlTiN transition layer by taking TiSi and AlTi as target materials; and S4, finally, depositing a TiSiN functional layer on the surface of the AlTiN/TiSiN support layer by taking TiSi as a target material to obtain the stable load type nano composite cutter coating.
Therefore, the coating is prepared by adopting a scheme of a multilayer structure, the advantages of component layers are integrated through the multilayer structure, so that the hardness, the initial performance, the high-temperature oxidation resistance and other performances of the coating are superior to those of a single layer, the deposition temperature and structure are optimized, the internal stress of the coating is reduced, the film-base bonding strength is improved, the bonding load performance of the cutter coating and the cutter surface is effectively improved, and the service life of the cutter coating is prolonged.
In some embodiments of the present invention, the thickness of the AlTiN/TiSiN supporting layer in step S3 is 0.5-3.5 μm, the nitrogen flow rate for depositing the AlTiN/TiSiN supporting layer is 400-500 Sccm, and the substrate bias is 40-60V.
The method optimizes the thickness preparation scheme of the supporting layer, so that the prepared AlTiN/TiSiN supporting layer is filled among the structures of the multilayer coating, the diffusion speed of external force and oxidation environment towards the inside of the coating and the diffusion speed of metal cations towards the outside under the action of the external force are delayed through the blocking effect of the supporting layer, the oxidation resistance and the falling resistance of the coating are improved, meanwhile, the optimized deposition conditions can effectively improve the ion energy and enhance the diffusion capacity, so that crystal nuclei growing faster preferentially nucleate, a compact columnar crystal structure is finally formed, the compact form of the whole coating is improved, and the service life of the cutter coating is prolonged.
In summary, the multilayer structure of a CrN combination layer, an AlTiN transition layer, an AlTiN/TiSiN support layer and a TiSiN functional layer is adopted for coating, the coating structure of the multilayer structure is beneficial to reducing the internal stress of a hard coating and improving the bonding strength between the hard coating and a base body, in addition, the coating of the multilayer structure has a template effect, a superhard effect that the hardness of the coating is obviously increased can occur, and on the basis, the surface of a cutter is subjected to surface treatment, so that the bonding strength between the CrN combination layer and the surface of the cutter is improved, the bonding load performance between the cutter coating and the surface of the cutter is effectively improved, and the service life of the cutter coating is prolonged.
The method comprises the steps of firstly polishing by using abrasive paper to remove an oxide layer, then carrying out etching treatment, and then carrying out sanding treatment on the surface of the cutter.
The etching liquid is adopted for etching treatment, wherein Al ions in the aluminum nitrate are dissociated in the electrolyte, combined with palmitic acid and loaded on the surface of the cutter, and the structure is matched with a pore structure formed by etching to improve the roughness of the surface of the cutter, so that the combined load performance of the cutter coating and the cutter surface is effectively improved, and the service life of the cutter coating is prolonged.
The stable load type nanocomposite cutter coating and the preparation method thereof according to the embodiment of the present invention will be described in detail with reference to the following specific embodiments.
Example 1
Taking a cutter, respectively polishing with 800#, 1200# and 1500# abrasive paper, after the treatment is finished, washing with countless ethanol for 3 times, naturally drying and collecting to obtain a surface treatment cutter; stirring and mixing aluminum nitrate, palmitic acid and absolute ethyl alcohol according to a mass ratio of 1:5:10 to prepare etching liquid, taking two polished cutters as a positive pole and a negative pole respectively, placing the two cutters into the etching liquid, etching at room temperature, taking out the etching cutters after etching is finished, sequentially washing the etching cutters for 3 times by using acetone and deionized water, naturally drying the etching cutters to obtain etched cutters, placing the etched cutters into a sanding device, sanding, washing and drying to obtain surface treatment cutters; placing a surface treatment tool on a rotating frame, placing the rotating frame in a deposition vacuum chamber, starting cooling water and a mechanical pump, vacuumizing to 30Pa, heating to 375 ℃, keeping the temperature and preheating for 10min, introducing argon to remove air, reducing the pressure in the vacuum chamber to 2Pa, performing metal ion bombardment on the surface of the tool by adopting a Cr target under the matrix bias of-435V, activating the surface of the tool, performing CrN bonding layer deposition on the surface of the tool after the activation is completed, controlling the current of the Cr target to be 70A, the vacuum degree to be 1Pa, performing deposition treatment for 20min, sequentially depositing an AlTiN transition layer, the current of an AlTi target to be 200A, the vacuum degree to be 1Pa, performing deposition treatment for 20min, after the deposition is completed, taking TiSi and AlTi as targets, controlling the negative bias voltage to be 30V, the vacuum degree to be 1Pa, performing deposition treatment for 20min, controlling the nitrogen flow to be 400Sccm and the matrix bias to be 40V, preparing an AlTiN/TiSiN supporting layer, then depositing a TiSiN functional layer on the AlTiN/TiSiN supporting layer, using TiSi as a target material, controlling the negative bias voltage to be 30V and the vacuum degree to be 1Pa, and after deposition treatment is carried out for 20min, sequentially preparing a 0.2-mu m CrN layer, a 0.8-mu m AlTiN transition layer, a 0.5-mu m AlTiN/TiSiN supporting layer and a 0.8-mu m TiSiN functional layer, wherein the TiSiN functional layer comprises 5% of Si, 40% of Ti and 55% of N according to the atomic mass ratio, the thickness of the CrN bonding layer is 0.2 mu m, and the CrN bonding layer comprises 40% of Cr and 60% of N according to the atomic mass ratio, so as to prepare the stable load type nano composite cutter coating.
Example 2
Taking a cutter, respectively polishing by using 800#, 1200# and 1500# abrasive paper, after the treatment is finished, washing for 4 times by using countless ethanol, naturally drying and collecting to obtain a surface treatment cutter; stirring and mixing aluminum nitrate, palmitic acid and absolute ethyl alcohol according to a mass ratio of 1:5:10 to prepare etching liquid, taking two polished cutters as a positive pole and a negative pole respectively, placing the two cutters into the etching liquid, etching at room temperature, taking out the etching cutters after etching is finished, sequentially washing the etching cutters for 4 times by using acetone and deionized water, naturally drying the etching cutters to obtain etched cutters, placing the etched cutters into a sanding device, sanding, washing and drying to obtain surface treatment cutters; placing a surface treatment cutter on a rotating frame, placing the rotating frame in a deposition vacuum chamber, starting cooling water and a mechanical pump, vacuumizing to 40Pa, heating to 400 ℃, keeping the temperature and preheating for 12min, introducing argon to remove air, reducing the pressure in the vacuum chamber to 3Pa, performing metal ion bombardment on the surface of the cutter by adopting a Cr target under the matrix bias of-410V, activating the surface of the cutter, performing CrN bonding layer deposition on the surface of the cutter after the activation is completed, controlling the current of the Cr target to be 72A and the vacuum degree to be 1Pa, performing deposition treatment for 25min, sequentially depositing an AlTiN transition layer and an AlTi target to be 300A and the vacuum degree to be 1Pa, performing deposition treatment for 25min, after the deposition is completed, taking TiSi and AlTi as targets, controlling the negative bias voltage to be 100V and the vacuum degree to be 1Pa, performing deposition treatment for 25min, controlling the nitrogen flow to be 400Sccm and the matrix bias to be 40V, preparing an AlTiN/TiSiN supporting layer, then depositing a TiSiN functional layer on the AlTiN/TiSiN supporting layer, using TiSi as a target material, controlling the negative bias voltage to be 100V and the vacuum degree to be 2Pa, and after deposition treatment is carried out for 25min, sequentially preparing a 0.2-mu m CrN layer, a 1.6-mu m AlTiN transition layer, a 2.0-mu m AlTiN/TiSiN supporting layer and a 1.5-mu m TiSiN functional layer, wherein the TiSiN functional layer comprises 8% of Si, 37% of Ti and 55% of N according to the atomic mass ratio, the thickness of the CrN bonding layer is 0.2 mu m, and the CrN bonding layer comprises 45% of Cr and 55% of N according to the atomic mass ratio, so that the stable load type nano composite cutter coating can be prepared.
Example 3
Taking a cutter, respectively polishing with 800#, 1200# and 1500# abrasive paper, after the treatment is finished, washing with countless ethanol for 5 times, naturally drying and collecting to obtain a surface treatment cutter; stirring and mixing aluminum nitrate, palmitic acid and absolute ethyl alcohol according to a mass ratio of 1:5:10 to prepare etching liquid, taking two polished cutters as a positive pole and a negative pole respectively, placing the two cutters into the etching liquid, etching at room temperature, taking out the etching cutters after etching is finished, sequentially washing the etching cutters for 5 times by using acetone and deionized water, naturally drying the etching cutters to obtain etched cutters, placing the etched cutters into a sanding device, sanding, washing and drying to obtain surface treatment cutters; placing a surface treatment tool on a rotating frame, placing the rotating frame in a deposition vacuum chamber, starting cooling water and a mechanical pump, vacuumizing to 50Pa, heating to 425 ℃, keeping the temperature and preheating for 15min, introducing argon to remove air, reducing the pressure in the vacuum chamber to 5Pa, performing metal ion bombardment on the surface of the tool by adopting a Cr target under the bias of a-400V matrix, activating the surface of the tool, performing CrN bonding layer deposition on the surface of the tool after the activation is completed, controlling the current of the Cr target to be 75A, the vacuum degree to be 2Pa, performing deposition treatment for 30min, sequentially depositing an AlTiN transition layer and the current of an AlTi target to be 400A, the vacuum degree to be 2Pa and performing deposition treatment for 30min, after the deposition is completed, taking TiSi and AlTi as targets, controlling the negative bias voltage to be 200V, the vacuum degree to be 2Pa, performing deposition treatment for 30min, controlling the nitrogen flow to be 400Sccm and the matrix bias to be 40V, preparing an AlTiN/TiSiN supporting layer, then depositing a TiSiN functional layer on the AlTiN/TiSiN supporting layer, using TiSi as a target material, controlling the negative bias voltage to be 200V and the vacuum degree to be 2Pa, and after deposition treatment is carried out for 30min, sequentially preparing a 0.3-mu m CrN layer, a 2.6-mu m AlTiN transition layer, a 3.5-mu m AlTiN/TiSiN supporting layer and a 2.8-mu m TiSiN functional layer, wherein the TiSiN functional layer comprises 10% of Si, 40% of Ti and 50% of N according to the atomic mass ratio, the thickness of the CrN bonding layer is 0.3 mu m, and the CrN bonding layer comprises 50% of Cr and 50% of N according to the atomic mass ratio, so as to prepare the stable load type nano composite cutter coating.
Example 4
In example 4, a deposition process was performed using a nitrogen flow of 450sccm and a substrate bias of 50V instead of the deposition conditions in example 1 when depositing the AlTiN/TiSiN support layer, and the remaining conditions and component ratios were the same as in example 1.
Example 5
In example 5, a deposition process was performed using a nitrogen flow rate of 500sccm and a substrate bias of 60V instead of the deposition conditions in example 1 while depositing the AlTiN/TiSiN support layer, and the remaining conditions and component ratios were the same as in example 1. Specific deposition conditions are shown in table 1 below:
TABLE 1 EXAMPLES 1-5 Nitrogen and substrate bias summary Table Performance test for deposition of AlTiN/TiSiN support layers
And respectively testing the performances of the cutter coatings prepared in the embodiments 1 to 5, and testing the coating film-substrate binding force, the frictional wear performance of the coating, the microhardness of the coating and the indentation morphology of the coating of the cutter coatings prepared in the embodiments 1 to 5.
Detection method/test method
(1) 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;
(3) 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
Referring to the comparison of the performance tests of table 2, it can be found that:
comparing the performances of the examples 1 to 3, wherein the microhardness, the bonding force performance and the friction coefficient of the example 3 are optimal, and the friction coefficient can significantly affect the service life of the whole coating, so that the ratio of the materials added in the example 3 is the highest, and the performance can also achieve the optimal technical effect, which indicates that the technical scheme of the application can be implemented.
Comparing the performances of the embodiment 1 and the embodiments 4 to 5, the embodiment 4 to 5 adopt different deposition conditions, which shows that the optimized deposition conditions of the present application can effectively improve ion energy and enhance diffusion capability, so that the crystal nucleus growing faster preferentially nucleates to finally form a compact columnar crystal structure, and the compact form of the whole coating is improved, thereby prolonging the service life of the cutter coating.
Comparative example
Comparative examples 1 to 3
In comparative examples 1 to 3, the surface of the cutter was not treated, and the coating was directly deposited, 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 only adopt etching treatment to the surface of the cutter, and the coating is deposited without sanding treatment, and the rest conditions and the component ratio are the same as those in examples 1 to 3.
Comparative examples 7 to 9
Comparative examples 7 to 9 only treated the surface of the cutter by sanding, and the coating was deposited without etching, 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 0.8. mu.m, and the remaining conditions and the component ratios were the same as in examples 1 to 3.
Comparative examples 13 to 15
Comparative examples 13 to 15 were prepared by depositing a CrN bonding layer, an AlTiN transition layer and a TiSiN functional layer in this order from the inside to the outside, and the other conditions and the component ratios were the same as those in examples 1 to 3.
Performance test
And respectively testing the coating film-base binding force, the frictional wear performance, the microhardness and the indentation morphology of the coating of the cutter coating prepared in the comparative examples 1-15.
Detection method/test method
(1) 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;
(3) 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 test results are shown in the following table 3:
TABLE 3 Performance test Table
The performance test table of table 3 was analyzed as follows:
comparing the comparative examples 1-3 with the examples 1-3, the structural performance and the coating film-substrate binding force of the tool without surface treatment in the comparative example are remarkably reduced in the test process, which shows that the tool after surface treatment can form good anchoring effect on the coating by embedding etched pore channels in the uniform and smooth surface after surface treatment, thereby effectively improving the binding load performance of the tool coating and the tool surface and prolonging the service life of the tool coating.
Comparing the comparative examples 4-6 with the examples 1-3, the deposition is carried out without sanding treatment in the comparative examples, and the performance is slightly reduced, which shows that the smoothness of the surface of the cutter is improved by trimming the etched pore channel formed on the surface of the cutter, and good load effect can be formed on the surface of the cutter in the subsequent deposition process by sanding treatment.
Comparing the comparative examples 7-9 with the examples 1-3, the deposition effect and the service life of the deposited coating are obviously reduced without etching treatment in the comparative examples, which shows that the etching treatment can not only improve the structural performance of the material, but also the Al ions in the aluminum nitrate are combined with palmitic acid and loaded on the surface of the cutter, and the structure is matched with the pore structure formed by etching to improve the roughness of the surface of the cutter, thereby effectively improving the combined loading performance of the cutter coating and the cutter surface and prolonging the service life of the cutter coating.
Comparing this application comparative example 10 ~ 12 with embodiment 1 ~ 3 again, improving the thickness of bonding layer in the comparative example, lead to the material property to descend to some extent, this demonstrates the bonding layer thickness of optimizing among the technical scheme of this application, both can form good boundary layer effect on transition layer and cutter surface, improves bonding strength between the two, prevents the higher bonding layer of thickness simultaneously, influences the structural effect of whole coating.
Comparing the comparative examples 13-15 with the examples 1-3, the performance of the coating is reduced because the supporting layer is not deposited in the comparative examples, which shows that the phenomena of internal diffusion of external force and oxidation environment into the coating and external diffusion of metal cations are delayed by the deposition treatment of the supporting layer, the oxidation resistance and the anti-falling performance of the coating are improved, and the service life of the cutter coating is prolonged.
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 stable-load type nano composite cutter coating is characterized by comprising a CrN bonding layer, an AlTiN transition layer, an AlTiN/TiSiN supporting layer and a TiSiN functional layer which are sequentially deposited and loaded from inside to outside, wherein the CrN bonding layer is deposited and loaded to one side of a cutter after surface treatment.
2. The tool coating of claim 1, wherein the surface treatment step is:
(1) sanding with abrasive paper to remove an oxide layer, washing, and etching the surface of the cutter;
(2) and sanding the etched cutter, washing and drying to prepare the cutter surface treatment layer.
3. The tool coating of claim 2, wherein the sanding process is a 800#, a 1200# and a 1500# sanding process in sequence.
4. The tool coating of claim 3, wherein the etching process comprises:
(1) taking two polished cutters as a cathode and an anode respectively, placing the two cutters in etching liquid, and etching at room temperature;
(2) after the etching is finished, taking out the etching cutter, washing and drying to obtain an etched cutter;
(3) and placing the etched cutter in a sanding device, sanding, washing and drying to obtain the surface treatment cutter.
5. The stable load type nanometer composite cutter coating according to claim 4, wherein the etching solution is prepared by stirring and mixing aluminum nitrate, palmitic acid and absolute ethyl alcohol according to a mass ratio of 1:5: 10.
6. The stably-loaded nanocomposite tool coating according to claim 4, wherein the CrN bonding layer has a thickness of 0.2 to 0.3 μm and comprises 40 to 50% Cr and 50 to 60% N by atomic mass ratio.
7. The stably-loaded nanocomposite tool coating according to claim 4, wherein the TiSiN functional layer comprises, by atomic mass, 5-10% Si, 35-40% Ti and 50-60% N.
8. A preparation method of a stable load type nanometer composite cutter coating is characterized by comprising the following steps:
s1, placing the surface treatment cutter in a deposition vacuum chamber, vacuumizing to 30-50 Pa, heating to 375-425 ℃, carrying out heat preservation and preheating treatment, reducing the pressure to 2-5 Pa in a nitrogen atmosphere, and then bombarding and activating the surface of the cutter by metal ions;
s2, after the surface of the cutter is activated, depositing a CrN bonding layer on the activated surface of the cutter in a nitrogen atmosphere;
s3, after the CrN combination layer is deposited, depositing an AlTiN transition layer on the surface of the CrN combination layer by taking AlTi as a target material, and after the deposition is finished, depositing an AlTiN/TiSiN supporting layer on the surface of the AlTiN transition layer by taking TiSi and AlTi as target materials;
s4, depositing a TiSiN functional layer on the surface of the AlTiN/TiSiN support layer by taking TiSi as a target material, and thus obtaining the stable load type nano composite cutter coating.
9. The method for preparing a stable load type nano composite cutter coating according to claim 8, wherein the thickness of the AlTiN/TiSiN supporting layer in the step S3 is 0.5-3.5 μm, the nitrogen flow rate for depositing the AlTiN/TiSiN supporting layer is 400-500 Sccm, and the substrate bias voltage is 40-60V.
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