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A method for preparing metal-ceramic nanocomposite films by solid-state dewetting
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A nano-composite and de-wetting technology, applied in metal material coating process, vacuum evaporation plating, coating and other directions, can solve the problems of very sensitive, deterioration, etc., to achieve improved friction and wear resistance, high repeatability, high yield effect
Active Publication Date: 2020-01-03
JILIN UNIV
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It is worth noting that in this system, the ductile metal phase must meet the phase separation criterion, that is, it cannot be miscible with TMN (C), which is limited to some soft metals (Cu, Ag, Au), such as ZrN / Cu, nc-WC / a-C(Al) and TMC(N) / noble metal(Ag,Au) systems, etc. Although the introduction of soft ductile metals can improve the toughness of TMN(C)-based films, the hardness of soft metals content is very sensitive and often shows significant deterioration
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Embodiment 1
[0027] 1) Clean and dry the substrate; specifically: clean and dry the substrate, the specific method is: place the substrate in an acetone solution for ultrasonic cleaning for 20 to 25 minutes; then put the substrate in alcohol Ultrasonic cleaning in medium for 20-25 minutes; finally, ultrasonically clean the substrate in deionized water for 20-25 minutes, take it out and place it in a drying oven at 40-60°C for 1-1.5 hours.
[0028] 2) Using magnetron sputtering equipment, put the cleaned and dried substrate into the vacuum chamber of the magnetron sputtering device, adjust the deposition angle to 0°, and the distance between the target and the substrate to be 12cm. The bias voltage is adjusted to -250V, and the cavity is evacuated to 3×10 -4 Below Pa. Adjust the working pressure of the vacuum chamber to 0.8Pa.
[0029] 3) Pass in the sputtering gas argon; set the gas flow rate of argon to 60 sccm; 0.5A. Regulate the preset deposition thickness ratio of ceramics and meta...
Embodiment 2
[0033] Step 1), 2) are identical with embodiment 1.
[0034] 3) Introduce the sputtering gas argon; set the gas flow rate of argon to 60 sccm; 0.5A. Regulate the preset deposition thickness ratio of ceramics and metals in an alternate unit to be 5:1, and the total sputtering time is 60 minutes.
[0035] 4) After the sputtering is finished, take out the sample for use.
[0036] 5) The TEM and HRTEM tests of the prepared sample confirmed that the characteristics of the disordered nanocomposite film appeared in the film prepared in this example. Therefore, the experimental parameters need to be further adjusted.
Embodiment 3
[0038] Step 1), 2) are identical with embodiment 1.
[0039] 3) Introduce the sputtering gas argon; set the gas flow rate of argon to 60 sccm; 0.5A. Regulate the preset deposition thickness ratio of ceramics and metals in an alternate unit to be 5:1, and the total sputtering time is 60 minutes.
[0040] 4) After the sputtering is finished, take out the sample for use.
[0041] 5) XRD is carried out to the prepared sample, and after the TEM test of the cross section, it is confirmed that this embodiment has successfully prepared a thin film of an ordered nanocomposite structure with a specific Ta layer wrapping TaC nanoparticles, such as figure 2 shown. The samples were subjected to mechanical tests, and the Ta-TaC nanocomposite film showed excellent properties of superhardness (~41GPa) and high toughness.
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Abstract
The invention provides a method for preparing a metal-ceramic nanometer composite thin film through solid dewetting and belongs to the technical field of functional film material preparation. A magnetron sputtering layered deposition technology is adopted, metal and ceramic serve as metal sources correspondingly, and Ar serves as sputtering gas. By adopting a continuous solid dewetting method, themetal and ceramic are alternately led into high-temperature layered deposition, the preset deposition thickness ratio of the ceramic to the metal in an alternating unit is regulated, and a continuously-wrapped nanometer composite structure thin film is prepared. According to the method, a traditional co-sputtering deposition mode controlled by phase separation in the preparation process of the metal-ceramic nanometer composite thin film is broken through, and selection of ductile metal, particularly comprising hard metal mixed and fused with the ceramic, is widened. The method has the advantages that the technique is simple, cost is low, repeatability is high, the production rate is high, and large-batch industrial production can be achieved. In the preparation process, by-products are not generated, environmental friendliness is facilitated, and prepared samples have ultra-hard and high-toughness excellent performance.
Description
technical field [0001] The invention belongs to the technical field of preparation of functional membrane materials, and in particular relates to a method for preparing metal-ceramic nanocomposite thin films by solid-state dewetting. Background technique [0002] Transition metal nitride / carbide TMN(C) with high hardness has been widely used in engineering applications including cutting tools, anti-friction and anti-scratch films. However, their inherently low toughness usually leads to automatic failure once cracks appear, which undoubtedly drives the rapid development of "tough and high-toughness films". At present, some successful strategies have been applied to improve the toughness of ceramic films, mainly including the introduction of ductile phases, the construction of nanocomposite structures, phase transition toughening and the introduction of appropriate compressive stress. Among them, the introduction of ductile metal phases to construct TMN(C)-based nanocomposit...
Claims
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