CN112609155B - Wide-temperature-range self-lubricating nano-structure film material with high service life - Google Patents
Wide-temperature-range self-lubricating nano-structure film material with high service life Download PDFInfo
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
Abstract
The invention relates to the field of hard coating material preparation, in particular to a wide-temperature-range self-lubricating nano-structure film material with a high service life, wherein the nano-structure film is of a multi-element multi-layer structure and consists of three modulation layers; the modulation layer is a self-lubricating layer and has a nano-capsule structure, wherein the capsule core is C and Ag, and the capsule shell is amorphous Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The other modulation layer is a hard layer and is a face-centered cubic TiN; a gradient layer between the self-lubricating layer and the hard layer and made of amorphous Al 2 O 3 And face centered cubic TiN. The beneficial effects of the invention are as follows: the amorphous oxide shell wraps the lubricating component inner core, and the nanocapsule shell effectively avoids excessive consumption of the lubricating component; in order to avoid interlayer stripping in the wide temperature range friction service process, the abrasion resistance of the film is improved; the film material can obtain the highest hardness of 24GPa, has the friction coefficient approximately stabilized between 0.4 and 0.6 in the environment of room temperature and 900 ℃, and can be repeatedly used in the environment of room temperature and high temperature.
Description
Technical Field
The invention relates to the field of hard coating material preparation, in particular to wide-temperature-range self-lubricating hard Al with high service life in a room-temperature to high-temperature environment 2 O 3 -Ag-C/Al 2 O 3 -TiN/TiN nano structure film material and preparation method thereof.
Background
With the rapid development of the fields of engine start-stop, high-speed aircrafts, thermonuclear and the like, the related core components such as pistons, bearings, turbine blades and the like need to be in service for a long time in a wide temperature range from room temperature to high temperature, and the traditional lubricating grease is difficult to meet the performance requirement. For this reason, how to design and develop self-lubricating surface materials with a high service life in a wide temperature range using surface technology is an effective way to solve the above-mentioned problems, has become one of the leading directions in the field of tribology today.
Diversification is one of the main means for improving the comprehensive performance of film materials. Graphite (Carbon, C) has a lamellar structure, and the layers are connected by only van der waals force, and is a material with excellent room temperature lubrication performance. Silver (Ag) is a conventional medium temperature lubricating material, and it can generate a high temperature lubricating friction phase, i.e., a bimetallic oxide, under the action of friction pair at high temperature. Therefore, students at home and abroad add C, ag and the like into the hard nitride or oxide film to prepare a series of wide-temperature-range self-lubricating materials, and the design criteria of the materials are constructed. However, C is burnt under the condition of medium and high temperature, and Ag is excessively migrated and released under the condition of high temperature, so that the hard nitride or oxide-based film material containing C and Ag has short service life and is not reusable. In addition, the consumption of C and Ag leaves holes in the film, so that the mechanical properties are greatly reduced. How to utilize mature film preparation technology, prepare the hard film material with high service life and excellent wide-temperature-range self-lubricating performance through composition and structural design so as to avoid excessive consumption of lubricating components is a key for enabling the wide-temperature-range self-lubricating hard film material to have industrial application value.
Disclosure of Invention
Aiming at the problems, the invention is based on the slow release protection idea of the nanocapsules, and the film has excellent mechanical property and longer service life on the premise of ensuring the self-lubricating performance of C room temperature and Ag at medium and high temperature through component and structural design. The film material overcomes the defects of excessive consumption and single use of self-lubricating components in the existing wide-temperature-range self-lubricating film, can be prepared by various modes such as magnetron sputtering, multi-arc, ion plating and the like, and has higher production efficiency and industrial application value.
The technical idea of the invention is as follows: the related nano-structure film is a multi-element multi-layer structure and is composed of three modulation layers. A modulation layer is a self-lubricating layer and has a nano-capsule structure, wherein the capsuleThe core is room temperature, medium temperature self-lubricating components C and Ag, and the capsule shell is amorphous Al with excellent high-temperature heat stability 2 O 3 The modulation layer has the self-lubricating function at the temperature of the medium temperature, and meanwhile, the capsule shell can avoid excessive consumption of lubricating components; the other modulating layer is a hard layer and is crystalline TiN so as to ensure the integral mechanical property of the film, and in the service process, the modulating layer and Ag in the self-lubricating layer undergo a tribochemical reaction to generate high-temperature self-lubricating friction phase Ag z Ti y O x The method comprises the steps of carrying out a first treatment on the surface of the A gradient layer between the self-lubricating layer and the hard layer and made of amorphous Al 2 O 3 And crystalline TiN, avoid the interlaminar stripping of the film in the in-service process. The content of C, ag, al and O in the self-lubricating layer is 1-20at%, 1-30at%, 5-90at% and 8-85at%, respectively; the Al, ti and O contents in the gradient layer are respectively 10-30at%, 30-80at% and 10-40at%; the hard layer contains 45-55at%, 45-55at% and 0-10at%, respectively. The three modulation layers are used as minimum units and are prepared under the pure Ar atmosphere by means of magnetron sputtering, multiple arcs, ion plating and the like. Controlling the thickness of the capsule shell in the lubricating layer to be 10-50nm and the diameter of the capsule core to be 5-20nm; the Al content in the gradient layer is between 10 and 30 at%; the modulation ratio of the lubricating layer, the gradient layer and the hard layer is controlled to be (1-1.5) (0.1-0.8) (1-5), the modulation period is between 10-500 nm, and the total thickness of the film is 1-5 mu m. The film material can obtain the highest hardness of 24GPa, has the friction coefficient approximately stabilized between 0.4 and 0.6 under the environment of room temperature and 900 ℃, and can be repeatedly used for multiple times.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
preparation of Al based on hard matrix surface 2 O 3 -Ag-C/Al 2 O 3 -a method of TiN/TiN nanostructured thin film material comprising the steps of:
step one: mirror-treating the hard matrix, and placing in a film forming device such as magnetron sputtering, multi-arc, ion plating, etc., wherein Al is preset in the film forming cabin 2 O 3 Target, ag target, C target, and TiN target. If the number of targets in the membrane-forming chamber is limited, silver-carbon composites, for example, can be usedAnd (5) a gold target. The distance between the target and the substrate is adjusted according to the requirement in the preparation process; step two: the background vacuum degree of the vacuum chamber is better than 6.0 multiplied by 10 -4 Ar with purity of 99.999% is introduced into the vacuum chamber after Pa 2 And (3) arcing, wherein a hard alloy or ceramic matrix surface substrate and an ion area are isolated by a baffle plate before a film is deposited. After the baffle plate is isolated, firstly opening Al 2 O 3 Targets, ag target, C target and TiN target, each target was pre-sputtered for 10min to remove oxide impurities on the target surface. The fixed sputtering air pressure is 0.3-0.8 Pa, and Al is fixed when the self-lubricating layer is deposited 2 O 3 Target, ag target, C target 150, 40 and 80W, while TiN target is turned off, preparation of amorphous Al 2 O 3 Wrapped Ag and C; fixing Al while depositing the gradient layer 2 O 3 Target and TiN targets 150, 150W, while closing Ag target, C target, preparation of amorphous Al from crystalline TiN 2 O 3 TiN/Al of two-phase constitution 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the At the time of depositing the hard layer, the TiN target 150W is turned off at the same time as Al 2 O 3 Targets, ag targets and C targets, and preparing TiN with higher crystallinity. Three modulation layer materials with different thicknesses are precisely deposited by reasonably controlling the sputtering time of each target, and finally the wide-temperature-range self-lubricating hard nano-structure film material with the total thickness of 1-5 mu m and high service life is prepared.
The beneficial effects of the invention are as follows:
1. the self-lubricating layer is designed based on the design idea of the nanocapsules, the amorphous oxide shell wraps the lubricating component inner core, and the nanocapsule shell effectively avoids excessive consumption of the lubricating component; in order to avoid interlayer peeling in the wide temperature range friction service process, the abrasion resistance of the film is improved, a gradient layer is designed, and interlayer peeling between a lubricating layer and a hard layer caused by the difference of thermal expansion coefficients is relieved; the hard layer is designed for ensuring the overall mechanical property of the self-lubricating film.
2. The film material can obtain the highest hardness of 24GPa, has the friction coefficient approximately stabilized between 0.4 and 0.6 in the environment of room temperature and 900 ℃, and can be repeatedly used in the environment of room temperature and high temperature.
Description of the drawings:
FIG. 1, al 2 O 3 -Ag-C modulation layer transmission electron micrographs;
FIG. 2, al 2 O 3 -TiN modulation layer transmission electron microscopy;
FIG. 3, a transmission electron micrograph of a TiN modulation layer;
FIG. 4, average friction coefficient and wear rate of five-cycle service of a multilayer film with a modulation period of 95nm, wherein the thickness of the self-lubricating layer is 30nm, the thickness of the gradient layer is 5nm, the thickness of the hard layer is 60nm, and the modulation ratio of the three modulation layers is 6:1:12.
Detailed Description
In order to enable those skilled in the art to better understand the technical solution of the present invention, the technical solution of the present invention is further described below with reference to examples.
Example 1:
preparation of Al based on hard matrix surface 2 O 3 -Ag-C/Al 2 O 3 -a method of TiN/TiN nanostructured films comprising the steps of: al (Al) 2 O 3 -Ag-C/Al 2 O 3 The preparation of the TiN/TiN film is completed on a high-vacuum multi-target magnetron sputtering device, namely a magnetron sputtering instrument which is provided with three sputtering targets, the three sputtering targets are respectively arranged on three water-cooled target brackets, and three stainless steel baffles are respectively arranged in front of the three targets and are automatically controlled by a computer; al (Al) 2 O 3 The targets (the purity is 99.95%), the Ag-C alloy targets (the purity is 99.9%) and the TiN targets (the purity is 99.5%) are respectively arranged on the independent radio frequency cathodes, and the diameters of the targets are 75mm;
step one: mirror surface treatment of the hard alloy surface substrate, ultrasonic cleaning with absolute ethyl alcohol and acetone for 15min, hot air drying, and loading onto rotatable substrate rack inside film making cabin of composite high vacuum multi-target magnetron sputtering equipment, with preset Al inside film making cabin 2 O 3 The position of the target, ag-C alloy target and TiN target, and the surface substrate of the hard alloy or ceramic matrix is connected with Al 2 O 3 The distance between the target, the Ag-C alloy target and the TiNl target is fixed at 80cm;
step two: to compound high vacuum multi-target magnetron sputtering equipmentThe vacuum pumping operation is carried out on the film making cabin, and the background vacuum degree of the vacuum chamber is better than 6.0 multiplied by 10 -4 Ar with purity of 99.999% is introduced into the vacuum chamber after Pa 2 Striking an arc;
step three: isolating the surface substrate of the hard alloy or ceramic matrix from the ion region by a baffle plate before depositing the film;
step four: after the baffle plate is isolated, al is opened 2 O 3 Targets, ag-C alloy targets and TiN targets, each target being pre-sputtered for 10min to remove impurities from the target surface;
step five: and rotating the baffle plate, and pre-sputtering a 200nm Ag-C transition layer on the surface substrate of the hard matrix to enhance the film base binding force. Then the baffle plate is removed, the fixed sputtering air pressure is 0.3Pa, the substrate is heated to 300 ℃, and when the self-lubricating layer is deposited, al is fixed 2 O 3 Target, ag target, C target 150, 40 and 80W, while TiN target is turned off, preparation of amorphous Al 2 O 3 The deposition time of the wrapped Ag and C is 380s; fixing Al while depositing the gradient layer 2 O 3 Target and TiN targets 150, 150W, while closing Ag target, C target, preparation of amorphous Al from crystalline TiN 2 O 3 TiN/Al of two-phase constitution 2 O 3 The deposition time is 90s; at the time of depositing the hard layer, the TiN target 150W is turned off at the same time as Al 2 O 3 The target, ag target and C target are used for preparing TiN with higher crystallinity, and the deposition time is 300s. The above-described deposition of the modulation layer was then reciprocally cycled 90 times. At the moment, the thickness of the self-lubricating layer is 30nm, the thickness of the gradient layer is 5nm, the thickness of the hard layer is 60nm, the modulation ratio of the three modulation layers is 6:1:12, and the modulation period is 95nm. The film hardness was 24GPa. After 30 minutes of circumferential friction test, the friction coefficients of room temperature, 300 ℃, 600 ℃ and 800 ℃ are approximately stabilized at 0.5, the friction test is circulated for five times, and the film is not worn through, so that the service life of the wide temperature range is prolonged.
Example 2
Unlike example 1, the following is: when the self-lubricating layer is deposited, the deposition time is 760s; when the gradient layer is deposited, the deposition time is 90s; in depositing the hard layer, the deposition time was 300s. The above-described deposition of the modulation layer was then reciprocally cycled 90 times. At the moment, the thickness of the self-lubricating layer is between 60 and 5nm, the thickness of the gradient layer is between 60 and 60nm, the modulation ratio of the three modulation layers is 12:1:12, and the modulation period is 125nm. The film hardness was 22GPa. After 30 minutes of circumferential friction test, the friction coefficients of room temperature, 300 ℃, 600 ℃ and 800 ℃ are approximately stabilized at 0.4, the friction test is circulated for five times, and the film is not worn through, so that the service life of the wide temperature range is prolonged.
Example 3
Unlike example 1, the following is: when the self-lubricating layer is deposited, the deposition time is 760s; when the gradient layer is deposited, the deposition time is 90s; in depositing the hard layer, the deposition time was 150s. The above-described deposition of the modulation layer was then reciprocally cycled 90 times. At the moment, the thickness of the self-lubricating layer is 60nm, the thickness of the gradient layer is 5nm, the thickness of the hard layer is 30nm, the modulation ratio of the three modulation layers is 12:1:6, and the modulation period is 125nm. The film hardness was 17GPa. After 30 minutes of circumferential friction test, the friction coefficients of room temperature, 300 ℃, 600 ℃ and 800 ℃ are approximately stabilized at 0.3, the friction test is circulated for five times, and the film is not worn through, so that the service life of the wide temperature range is prolonged.
The film preparation mode related to the patent is not limited to magnetron sputtering, and can be obtained by multiple film preparation modes such as multi-arc and ion plating. In addition, it is worth pointing out that the design concept of the nanocapsule for preventing noble metal migration and diffusion can also be applied to the fields of microelectronics, semiconductors and the like. The modulation layer material related to the patent can also be independently used as a hard composite film material.
It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. Wide-temperature-range self-lubricating nanometer with high service lifeThe structural film material is characterized in that the related nano-structural film is of a multi-element multi-layer structure and is composed of three modulation layers; the modulation layer is a self-lubricating layer and has a nano-capsule structure, wherein the capsule core is C and Ag, and the capsule shell is amorphous Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The other modulating layer is a hard layer and is crystalline TiN; a gradient layer between the self-lubricating layer and the hard layer and made of amorphous Al 2 O 3 And crystalline TiN.
2. The wide temperature range self-lubricating nanostructured thin film material with high service life according to claim 1, wherein Al 2 O 3 -Ag-C/Al 2 O 3 The combination of the three modulation layers of TiN/TiN is set for the minimum unit period, and the modulation period is 10-500 nm.
3. The wide temperature range self-lubricating nanostructured thin film material with high service life according to claim 1, wherein the content of C, ag, al and O in the self-lubricating layer is 1-20 at%, 1-30 at%, 5-90 at% and 8-85 at%, respectively; the Al, ti and O contents in the gradient layer are 10-30 at%, 30-80 at% and 10-40 at% respectively; the hard layer contains 45-55 at%, 45-55 at% and 0-10 at% of Ti, N and O, respectively.
4. The wide temperature range self-lubricating nano-structured film material with high service life as claimed in claim 1, wherein the thickness of the capsule shell in the self-lubricating layer is controlled to be 10-50nm, and the diameter of the capsule core is controlled to be 5-20nm.
5. The wide-temperature-range self-lubricating nanostructured thin film material with a high service life according to claim 1, wherein the modulation ratio of the self-lubricating layer, the gradient layer and the hard layer is controlled to be (1-1.5): (0.1-0.8): (1-5).
6. The wide temperature range self-lubricating nanostructured thin film material with high service life according to claim 1, wherein the total thickness of the thin film is 1-5 μm.
7. A wide temperature range self-lubricating nanostructured thin film material having a high service life according to any of claims 1 to 6, prepared by the method of:
step one: mirror surface treatment of the hard alloy surface substrate, ultrasonic cleaning with absolute ethyl alcohol and acetone for 15min, hot air drying, and loading onto rotatable substrate rack inside film making cabin of composite high vacuum multi-target magnetron sputtering equipment, with preset Al inside film making cabin 2 O 3 The position of the target, ag-C alloy target and TiN target, and the surface substrate of the hard alloy or ceramic matrix is connected with Al 2 O 3 The distance between the target, the Ag-C alloy target and the TiN target is fixed at 80cm;
step two: vacuum pumping operation is carried out on a film making cabin of the composite high-vacuum multi-target magnetron sputtering equipment, and the background vacuum degree of a vacuum chamber is better than 6.0 multiplied by 10 -4 After Pa, introducing Ar with purity of 99.999% into a vacuum chamber for arcing;
step three: isolating the surface substrate of the hard alloy or ceramic matrix from the ion region by a baffle plate before depositing the film;
step four: after the baffle plate is isolated, al is opened 2 O 3 Targets, ag-C alloy targets and TiN targets, each target being pre-sputtered for 10min to remove impurities from the target surface;
step five: removing the baffle plate, fixing the sputtering air pressure to be 0.3Pa, heating the substrate to 300 ℃, and respectively fixing Al when the self-lubricating layer is deposited 2 O 3 Target, ag target, C target 150W, 40W and 80W, while TiN target is turned off, preparation of amorphous Al 2 O 3 The deposition time of the wrapped Ag and C is 380s; during the deposition of the gradient layer, al is fixed separately 2 O 3 The targets and TiN targets 150W, while closing the Ag target and the C target, to prepare a metal alloy composed of crystalline TiN and amorphous Al 2 O 3 TiN/Al of two-phase constitution 2 O 3 The deposition time is 90s; at the time of depositing the hard layer, the TiN target 150W is turned off at the same time as Al 2 O 3 Preparing TiN by using a target, an Ag target and a C target, wherein the deposition time is 300s;
step six: the above-described process of depositing the modulation layer is then reciprocally cycled several times.
8. The wide temperature range self-lubricating nanostructured thin film material with high service life according to claim 7, wherein after step four, the baffle is rotated first, the Ag-C alloy target is operated, a 200nm Ag-C transition layer is pre-sputtered on the hard base surface substrate, and then step five is performed.
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| JP2004217973A (en) * | 2003-01-14 | 2004-08-05 | Gunze Ltd | Thin film, and thin film production method |
| CN102277018A (en) * | 2011-07-20 | 2011-12-14 | 合肥工业大学 | High-temperature self-lubricating wear-resistant powder coating |
| GB2513867A (en) * | 2013-05-07 | 2014-11-12 | Mahle Int Gmbh | Sliding engine component |
| WO2015120893A1 (en) * | 2014-02-13 | 2015-08-20 | Mimsi Materials Ab | Method of coating a substrate so as to provide a controlled in-plane compositional modulation |
| CN110878407A (en) * | 2019-10-31 | 2020-03-13 | 江苏科技大学 | Ta-Ag-N/VN multilayer film material with abnormal hardness increasing effect and preparation method thereof |
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| 磁控溅射高温固体自润滑涂层的研究与进展;陈亚军;郁佳琪;赵婕宇;王付胜;;材料导报(第03期);全文 * |
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