CN113278920A - DLC (diamond-like carbon) coating and preparation method thereof - Google Patents

DLC (diamond-like carbon) coating and preparation method thereof Download PDF

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Publication number
CN113278920A
CN113278920A CN202110364450.9A CN202110364450A CN113278920A CN 113278920 A CN113278920 A CN 113278920A CN 202110364450 A CN202110364450 A CN 202110364450A CN 113278920 A CN113278920 A CN 113278920A
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coating
substrate
dlc
transition layer
bottom layer
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韩秀全
李军明
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Qingdao denai Nano Technology Co.,Ltd.
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Yingmaidun Nano Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0664—Carbonitrides
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C14/3464—Sputtering using more than one target
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C14/3485—Sputtering using pulsed power to the target

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  • Engineering & Computer Science (AREA)
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  • Physical Vapour Deposition (AREA)

Abstract

The invention relates to the technical field of coating materials, in particular to a DLC (diamond-like carbon) coating and a preparation method thereof; the TiAlCN coating comprises a substrate, a TiN bottom layer covered on the substrate, a TiCN transition layer covered on the TiN bottom layer, and a TiAlCN coating covered on the TiCN transition layer; the DLC-like carbon coating prepared by the invention not only has good binding force, but also has good internal stress, wear resistance and hardness; so that the quality of the prepared DLC-like carbon coating is effectively improved.

Description

DLC (diamond-like carbon) coating and preparation method thereof
Technical Field
The invention relates to the technical field of coating materials, in particular to a DLC (diamond-like carbon) coating and a preparation method thereof.
Background
A DLC-like diamond coating is a substance composed of carbon elements, similar in nature to diamond, and having a graphite atom composition structure. Diamond-like carbon (DLC) is an amorphous film and is widely used in surgical scissors, medical instruments, high-end door handles, and the like, which are in contact with the human body. The prior DLC film preparation methods are various, the carbon sources used by different preparation methods and the ion energy reaching the surface of a substrate are different, the structure and the performance of the deposited DLC film are greatly different, and the tribological performance is also different.
Although the diamond-like coating prepared by the patent document has certain wear resistance and binding force performance, the wear resistance and the binding force performance are relatively poor, the diamond-like coating does not have good hardness, and the function is relatively single, so that the performance and the quality of the prepared diamond-like coating are influenced.
Disclosure of Invention
Aiming at the defects in the prior art, the first purpose of the invention is to provide a DLC-like carbon coating, which not only has good bonding force, but also has good internal stress, wear resistance and hardness; so that the quality of the prepared DLC-like carbon coating is effectively improved.
In order to achieve the purpose, the invention provides the following technical scheme:
a DLC-like coating comprising a substrate and further comprising:
a TiN bottom layer covering the substrate, a TiCN transition layer covering the TiN bottom layer, and a TiAlCN coating covering the TiCN transition layer.
By adopting the technical scheme: according to the invention, the TiN bottom layer, the TiCN transition layer and the TiAlCN coating are used for forming the composite DLC-like carbon coating, so that the prepared composite DLC-like carbon coating has good wear resistance and hardness.
The invention is further configured to: the thickness of the TiN bottom layer is 200-600nm, the thickness of the TiCN transition layer is 120-200nm, and the thickness of the TiAlCN coating is 300-800 nm.
By adopting the technical scheme: the TiN bottom layer is coated on the substrate, so that the connection strength between the DLC-like carbon coating substrates is improved, the TiCN transition layer and the TiAlCN coating form multi-layer protection on the substrate, and the service life of the substrate is prolonged.
The second purpose of the invention is to provide a preparation method of DLC diamond-like coating, which comprises the following steps:
s1, preprocessing the surface of the substrate;
s2, preparing a TiN bottom layer on the pretreated substrate;
s3, further preparing a TiCN transition layer on the TiN bottom layer prepared in the S2;
s4, preparing TiAlCN coating on the TiCN transition layer prepared by the S3.
By adopting the technical scheme: the composite DLC-like diamond coating is composed of the TiN bottom layer, the TiCN transition layer and the TiAlCN coating, and compared with a single-layer structure, the composite DLC-like diamond coating can ensure that the substrate has good wear resistance, hardness and oxidation resistance.
The invention is further configured to: in step S1, the method for pre-treating the surface of the substrate is as follows:
preparing a cleaning solution; putting the matrix into the cleaning solution, heating the cleaning solution in a water bath and preserving the heat for 20 min; taking out the matrix from the cleaning solution, ultrasonically cleaning the matrix for 15min by acetone, and then washing the matrix by distilled water; by drying N2And drying the surface of the substrate by blowing.
By adopting the technical scheme: firstly, soaking a substrate by using a cleaning solution, then ultrasonically cleaning the substrate by using acetone to remove oil stains on the surface of the substrate, then washing the substrate by using distilled water, and using dry N2And drying is carried out, so that no residual water stain is left on the surface of the cleaned substrate, the subsequent separation of the substrate and the DLC-like carbon coating is avoided, and the binding force between the substrate and the DLC-like carbon coating is ensured.
The invention is further configured to: when the surface of the matrix is pretreated, the cleaning solution is heated to 80-90 ℃ in a water bath.
By adopting the technical scheme: the cleaning solution can better clean the oil stain on the surface of the matrix by heating the substrate to 80-90 ℃ in a water bath.
The invention is further configured to: in step S2, the method for preparing TiN underlayer on the pretreated substrate is:
putting the pretreated substrate into a sputtering chamber, wherein the temperature of the substrate is 300 ℃, the bias voltage of the substrate is-50V, and vacuumizing until the vacuum degree in the sputtering chamber reaches 1 x 10-3Pa; ar gas is introduced into the sputtering chamber with the flow rate of 30cm3Min, and adjusting the gas pressure in the sputtering chamberWhen the power is 1.0Pa, the pulse power frequency of the Ti target is 200kHz, the power is 600W, and the surface of the Ti target with the purity of 99.9 percent is pre-sputtered for 15min after glow discharge; keeping the flow of Ar constant, and introducing reaction gas N2The flow rate is 30cm3And/min, after the plasma treatment by the external voltage, depositing a TiN bottom layer on the substrate, wherein the deposition time is 90 min.
By adopting the technical scheme: in the invention, the vacuum degree in the sputtering chamber is pumped to 1 multiplied by 10-3Pa can ensure the purity of the TiN bottom layer, pre-sputtering the Ti target surface, removing impurities such as oxides on the Ti target surface and the like, and improving the binding force of the TiN bottom layer.
The invention is further configured to: in step S3, the method for further forming a TiCN transition layer on the TiN underlayer is as follows:
after the deposition of the TiN underlayer was completed, the gas pressure in the sputtering chamber was adjusted to 339X 10-3Pa, C target is connected with a direct current power supply, the frequency of the pulse power supply of the C target is 200kHz, the power is 200W, the deposition time is 60min, other conditions are kept unchanged, and a TiCN transition layer is deposited on the TiN bottom layer.
By adopting the technical scheme: the TiCN transition layer is deposited on the TiN bottom layer and can be used as a stress buffer zone, so that the internal stress of the DLC-like carbon coating is reduced, and the hardness of the DLC-like carbon coating is improved.
The invention is further configured to: in the step S4, the method for further forming the TiAlCN coating on the TiCN transition layer includes:
after the deposition of the TiCN transition layer is finished, the power of the C target is adjusted to be 450W, the Al target is connected with a direct current power supply, the power frequency is 200kHz, the power is 200W, and the Ar gas flow is 70cm3And/min, the deposition time is 120min, other conditions are kept unchanged, and the TiAlCN coating is deposited on the TiCN transition layer.
By adopting the technical scheme: connecting the Al target with a direct current power supply by adjusting the power of the C target to form a TiAlCN coating so as to sp3The content of the bond is higher, so that the TiAlCN coating has good hardness and wear resistance.
Advantageous effects
Compared with the known public technology, the technical scheme provided by the invention has the following beneficial effects:
1. the invention firstly uses cleaning fluid to soak the basal body, then uses acetone to carry out ultrasonic cleaning to remove the greasy dirt on the surface of the basal body, then uses distilled water to wash, and uses dry N2Blow-drying is carried out, so that no residual water stain is left on the surface of the cleaned substrate, the subsequent separation of the substrate and the DLC-like carbon coating is avoided, the binding force between the substrate and the DLC-like carbon coating is ensured, and the substrate is vacuumized until the vacuum degree in a sputtering chamber reaches 1 multiplied by 10-3Pa can ensure the purity of the TiN bottom layer, pre-sputtering the Ti target surface, removing impurities such as oxides on the Ti target surface, and improving the binding force of the TiN bottom layer, thereby improving the binding force between the DLC diamond-like coating and the substrate.
2. According to the invention, the TiN bottom layer, the TiCN transition layer and the TiAlCN coating form the composite DLC-like carbon coating, the TiCN transition layer is deposited on the TiN bottom layer, and the TiCN transition layer can be used as a stress buffer zone, so that the internal stress of the DLC-like carbon coating is reduced, the hardness of the DLC-like carbon coating is improved, and the prepared composite DLC-like carbon coating has good wear resistance and hardness.
3. According to the invention, the power of the C target is adjusted, the Al target is connected with a direct current power supply to form a TiAlCN coating, so that sp is3The content of the bond is higher, so that the TiAlCN coating has good hardness and wear resistance.
Drawings
FIG. 1 is a schematic structural view of a DLC-like carbon coating.
Illustration of the drawings:
10. a substrate; 11. a TiN bottom layer; 12. a TiCN transition layer; 13. and (4) TiAlCN coating.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be further described with reference to the following examples.
Example 1
A DLC-like coating comprising a substrate 10, further comprising:
a TiN underlayer 11 overlying the substrate 10, a TiCN transition layer 12 overlying the TiN underlayer 11, and a TiAlCN coating 13 overlying the TiCN transition layer 12.
The thickness of the TiN bottom layer 11 is 200-600nm, the thickness of the TiCN transition layer 12 is 120-200nm, and the thickness of the TiAlCN coating layer 13 is 300-800 nm.
A preparation method of a DLC diamond-like coating comprises the following steps:
s1, the surface of the substrate 10 is pretreated.
S2, preparing a TiN bottom layer 11 on the pretreated substrate 10.
S3, a TiCN transition layer 12 was further formed on the TiN underlayer 11 obtained in the above-mentioned S2.
S4, a TiAlCN coating layer 13 is further prepared on the TiCN transition layer 12 prepared by the S3.
The method for pretreating the surface of the substrate 10 comprises the following steps:
preparing a cleaning solution; putting the matrix 10 into the cleaning solution, heating the cleaning solution in a water bath and preserving the temperature for 20 min; taking out the matrix 10 from the cleaning solution, ultrasonically cleaning the matrix for 15min by acetone, and then washing the matrix 10 by distilled water; by drying N2The surface of the substrate 10 is blow-dried.
In the pretreatment of the surface of the substrate 10, the cleaning solution was heated to 80 ℃ in a water bath.
The method for preparing the TiN bottom layer 11 on the pretreated substrate 10 comprises the following steps:
putting the pretreated matrix 10 into a sputtering chamber, wherein the temperature of the matrix 10 is 300 ℃, the bias voltage of the matrix 10 is minus 50V, and vacuumizing is carried out until the vacuum degree in the sputtering chamber reaches 1 multiplied by 10-3Pa; ar gas is introduced into the sputtering chamber with the flow rate of 30cm3Min, adjusting the air pressure in the sputtering chamber to 1.0Pa, the pulse power frequency of the Ti target to 200kHz, the power to 600W, and performing glow discharge on the Ti target with the purity of 99.9 percentPre-sputtering the dough for 15 min; keeping the flow of Ar constant, and introducing reaction gas N2The flow rate is 30cm3And/min, after the plasma formation of the external voltage, depositing a TiN bottom layer on the substrate 10, wherein the deposition time is 90 min.
The method for further preparing the TiCN transition layer 12 on the TiN bottom layer 11 comprises the following steps:
after the deposition of the TiN underlayer 11 was completed, the gas pressure in the sputtering chamber was adjusted to 339X 10-3Pa, C target is connected with a direct current power supply, the frequency of the pulse power supply of the C target is 200kHz, the power is 200W, the deposition time is 60min, other conditions are kept unchanged, and a TiCN transition layer 12 is deposited on the TiN bottom layer 11.
The method for further preparing the TiAlCN coating 13 on the TiCN transition layer 12 comprises the following steps:
after the deposition of the TiCN transition layer 12 is finished, the power of the C target is adjusted to 450W, the Al target is connected with a direct current power supply, the power frequency is 200kHz, the power is 200W, and the Ar gas flow is 70cm3And/min, the deposition time is 120min, other conditions are kept unchanged, and the TiAlCN coating 13 is deposited on the TiCN transition layer 12.
Example 2
The DLC diamond-like coating and the preparation method provided in this example are substantially the same as in example 1, with the main difference being: when the surface of the matrix 10 is pretreated, the cleaning solution is heated to 90 ℃ in a water bath;
comparative example 1
The DLC diamond-like coating and the preparation method provided in this example are substantially the same as in example 1, with the main differences: the surface of the substrate 10 is not pretreated;
comparative example 2
The DLC diamond-like coating and the preparation method provided in this example are substantially the same as in example 1, with the main difference being: the TiN bottom layer 11 is not covered;
comparative example 3
The DLC diamond-like coating and the preparation method provided in this example are substantially the same as in example 1, with the main difference being: no TiCN transition layer 12 is coated;
comparative example 4
The DLC diamond-like coating and the preparation method provided in this example are substantially the same as in example 1, with the main difference being: no TiAlCN coating 13 is coated;
performance testing
Taking the DLC-like carbon coatings prepared in the embodiments 1-2 and the comparative examples 1-4, and detecting the related performance of the prepared DLC-like carbon coatings, wherein the detection method comprises the following steps:
1. respectively detecting the binding force of each DLC diamond-like coating according to the national standard GB/T5270-;
TABLE 1
Figure BDA0003006849230000091
2. Respectively detecting the internal stress of each DLC diamond-like coating according to the national standard GB/T31566-2005, and recording the obtained data in a table 2;
3. the hardness of each DLC diamond-like coating is detected according to the national standard GB/T9790-;
4. the wear resistance of each DLC diamond-like coating is respectively detected according to the national standard GB/T11379-2008, and the obtained data is recorded in a table 2;
TABLE 2
Figure BDA0003006849230000092
Figure BDA0003006849230000101
By analyzing the relevant data in the tables, the DLC diamond-like coating prepared by the method has good bonding force and good internal stress; but also enhances the hardness and wear resistance of the coating. Therefore, the DLC diamond-like carbon coating and the preparation method thereof have wider market prospect and are more suitable for popularization.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.

Claims (8)

1. A DLC-like coating comprising a substrate, characterized in that it further comprises:
a TiN bottom layer covering the substrate, a TiCN transition layer covering the TiN bottom layer, and a TiAlCN coating covering the TiCN transition layer.
2. A DLC-like coating according to claim 1, characterised in that: the thickness of the TiN bottom layer is 200-600nm, the thickness of the TiCN transition layer is 120-200nm, and the thickness of the TiAlCN coating is 300-800 nm.
3. A preparation method of a DLC diamond-like coating is characterized by comprising the following steps:
s1, preprocessing the surface of the substrate;
s2, preparing a TiN bottom layer on the pretreated substrate;
s3, further preparing a TiCN transition layer on the TiN bottom layer prepared in the S2;
s4, preparing TiAlCN coating on the TiCN transition layer prepared by the S3.
4. The method for preparing DLC-like carbon coating according to claim 3, wherein said step S1, the method for pre-treating the surface of said substrate is:
preparing a cleaning solution; putting the matrix into the cleaning solution, heating the cleaning solution in a water bath and preserving the heat for 20 min; taking out the matrix from the cleaning solution, ultrasonic cleaning with acetone for 15min, and distillingWashing the matrix with water; by drying N2And drying the surface of the substrate by blowing.
5. The method of preparing a DLC-like carbon coating as claimed in claim 4, wherein: when the surface of the matrix is pretreated, the cleaning solution is heated to 80-90 ℃ in a water bath.
6. A method of producing a DLC-like coating according to claim 3, characterised in that: in step S2, the method for preparing TiN underlayer on the pretreated substrate is:
putting the pretreated substrate into a sputtering chamber, wherein the temperature of the substrate is 300 ℃, the bias voltage of the substrate is-50V, and vacuumizing until the vacuum degree in the sputtering chamber reaches 1 x 10-3Pa; ar gas is introduced into the sputtering chamber with the flow rate of 30cm3Min, adjusting the air pressure in the sputtering chamber to 1.0Pa, adjusting the frequency of a Ti target pulse power supply to 200kHz and the power to 600W, and pre-sputtering the surface of the Ti target with the purity of 99.9 percent for 15min after glow discharge; keeping the flow of Ar constant, and introducing reaction gas N2The flow rate is 30cm3And/min, after the plasma treatment by the external voltage, depositing a TiN bottom layer on the substrate, wherein the deposition time is 90 min.
7. A method of producing a DLC-like coating according to claim 3, characterised in that: in step S3, the method for further forming a TiCN transition layer on the TiN underlayer is as follows:
after the deposition of the TiN underlayer was completed, the gas pressure in the sputtering chamber was adjusted to 339X 10-3Pa, C target is connected with a direct current power supply, the frequency of the pulse power supply of the C target is 200kHz, the power is 200W, the deposition time is 60min, other conditions are kept unchanged, and a TiCN transition layer is deposited on the TiN bottom layer.
8. A method of producing a DLC-like coating according to claim 3, characterised in that: in the step S4, the method for further forming the TiAlCN coating on the TiCN transition layer includes:
after the deposition of TiCN transition layerThen, the power of the C target is adjusted to 450W, the Al target is connected with a direct current power supply, the power frequency is 200kHz, the power is 200W, and the Ar gas flow is 70cm3And/min, the deposition time is 120min, other conditions are kept unchanged, and the TiAlCN coating is deposited on the TiCN transition layer.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020136933A1 (en) * 1996-09-03 2002-09-26 Hans Braendle Method for manufacturing a workpiece with wear-protective coating
CN104846332A (en) * 2015-04-17 2015-08-19 岭南师范学院 Superlubricity multilayer nano composite coating and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020136933A1 (en) * 1996-09-03 2002-09-26 Hans Braendle Method for manufacturing a workpiece with wear-protective coating
CN104846332A (en) * 2015-04-17 2015-08-19 岭南师范学院 Superlubricity multilayer nano composite coating and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
YUQIAO ZENG.ET.AL.: "Superhard TiAlCN coatings prepared by radio frequency magnetron sputtering", 《THIN SOLID FILMS》 *
刘红: "《工程材料》", 30 April 2019, 北京理工大学出版社 *
阮勇等: "《硅MEMS工艺与设备基础》", 31 December 2018, 国防工业出版社 *

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