Onyx coated workpiece and method of making same

Abstract

The application relates to an agate color coated workpiece and a preparation method thereof. The preparation method comprises the following steps: S1, depositing a transition layer on a base material by adopting a magnetron sputtering mode; S2, depositing a TiAlN intermediate layer on the transition layer in S1 by adopting the magnetron sputtering mode; and S3, depositing a TiAlSiN agate color coating layer on the TiAlN intermediate layer in S2 by adopting the magnetron sputtering mode. In step S3, the sputtering power of the Si target is controlled, so that the percentage of Si elements in the deposited TiAlSiN layer is 7%-8%. The application obtains a special agate color coated workpiece, and the workpiece has high hardness and wear resistance, and has a wider application prospect.

Description

Technical Field

[0001] This invention relates to the field of PVD sputtering technology, and in particular to an agate-colored coated workpiece and its preparation method. Background Technology

[0002] Physical vapor deposition (PVD) is a thin film preparation technology that uses physical methods to deposit materials onto a workpiece under vacuum conditions. It is widely used in surface treatment and thin film preparation. Magnetron sputtering is a type of PVD. General sputtering methods can be used to prepare various materials such as metals, semiconductors, and insulators, and have advantages such as simple equipment, easy control, large coating area, and strong adhesion.

[0003] Currently, the variety of coating colors available on the market cannot meet the needs of all customers, and it is not possible to produce coatings with vibrant colors.

[0004] Therefore, existing technologies need to be improved. Summary of the Invention

[0005] This invention provides an agate-colored coated workpiece and its preparation method, which fills the gap in the market for agate-colored coated workpieces, and also has better hardness and wear resistance than other colored film systems.

[0006] In a first aspect, the present invention provides a method for preparing an agate-colored coated workpiece, specifically including the following steps:

[0007] S1. A transition layer is deposited on the substrate material using magnetron sputtering.

[0008] S2. A TiAlN intermediate layer is deposited on the transition layer in S1 by magnetron sputtering.

[0009] S3. A TiAlSiN agate-colored coating is deposited on the TiAlN intermediate layer in S2 by magnetron sputtering.

[0010] In S3, the sputtering power of the Si target is controlled so that the percentage of Si element in the deposited TiAlSiN layer is 7%~8%.

[0011] In one implementation, S1 specifically includes: introducing Ar into the coating chamber until the gas pressure reaches 0.3~0.5Pa, setting the bias voltage to -50Pa, turning on the target, and depositing the transition layer.

[0012] In one implementation, in S1, the transition layer is a pure Ti layer.

[0013] In one implementation, S2 specifically includes the following steps:

[0014] S21. Introduce reactive gas N2 into the coating chamber, adjust the gas pressure to 0.41~0.43 Pa, and simultaneously turn on the Ti target and Al target. Deposit for 15~25 min to obtain the TiAlN intermediate layer.

[0015] S22. Continue to introduce reactive gas N2 into the coating chamber, adjust the gas pressure to 0.44~0.46 Pa, and simultaneously turn on the Ti target and Al target. Deposit for 25~35 min to obtain a dense TiAlN intermediate layer.

[0016] In one implementation, in S2, the current parameter of the Ti target is 30A and the current parameter of the Al target is 15A.

[0017] In one implementation, step S3 specifically includes the following steps: introducing reactive gas N2 into the coating chamber, adjusting the gas pressure to 0.46~0.50 Pa, simultaneously turning on the Ti target, Al target and Si target, depositing on the substrate material for 40~45 min to obtain a TiAlSiN agate-colored coating, and ending the coating process.

[0018] In one implementation, in S3, the current parameter of the Ti target is set to 10A, the current parameter of the Al target is set to 15A, and the current parameter of the Si target is set to 20A.

[0019] In one implementation, before S1, the process further includes: cleaning pretreatment, ultrasonic cleaning of the substrate material, vacuuming and heating of the coating chamber, introducing Ar into the coating chamber when the gas pressure in the coating chamber reaches 0.001 Pa, and performing arc bombardment rinsing on the substrate material when the gas pressure reaches -2 to 0 Pa and the bias voltage is set to -300 V.

[0020] In one implementation, before S1, a mixed solution of potassium permanganate and hydrogen peroxide is used as the cleaning solution, and the substrate material to be coated is placed in an ultrasonic cleaner for 15-25 minutes.

[0021] Secondly, the present invention also provides an agate-colored coated workpiece, which is made by the preparation method of the agate-colored coated workpiece described in any one of the above-mentioned methods.

[0022] Beneficial effects: This invention uses magnetron sputtering technology to prepare agate-colored coated workpieces, and continues to deposit a TiAlN intermediate layer on the transition layer to enhance the bonding force between the agate-colored coated workpiece and the transition layer, so that the TiAlSiN agate-colored layer can be better deposited on the substrate material. At the same time, this invention also adjusts the proportion of each element in TiAlSiN agate color, increases the silicon content, enhances the wear resistance of the agate-colored coated workpiece, and provides a colorful and wear-resistant agate-colored coated workpiece that meets user needs. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of the product obtained in an embodiment of the present invention after a 48-hour abrasion resistance test;

[0024] Figure 2 This is a schematic diagram from another angle showing the product obtained in an embodiment of the present invention after undergoing a 48-hour abrasion resistance test;

[0025] Figure 3 This is a schematic diagram of the product obtained in the comparative example of the present invention after a 48-hour abrasion resistance test;

[0026] Figure 4 This is a schematic diagram from another angle showing the product obtained in the comparative example of this invention after undergoing a 48-hour abrasion resistance test. Detailed Implementation

[0027] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. Additional aspects and advantages of this 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. It should be understood that the following description is merely illustrative and not intended to limit the invention.

[0028] As used herein, the terms “comprising,” “including,” “having,” “containing,” or any other variation thereof are intended to cover non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not necessarily limited to those elements, but may include other elements not expressly listed or elements inherent to such composition, step, method, article, or apparatus.

[0029] When a quantity, concentration, or other value or parameter is expressed as a range, a preferred range, or a range defined by a series of upper and lower preferred values, this should be understood as specifically disclosing all ranges formed by any pair of any upper or preferred value with any lower or preferred value, regardless of whether the range is disclosed individually. For example, when the range “1 to 5” is disclosed, the described range should be interpreted as including the ranges “1 to 4”, “1 to 3”, “1 to 2”, “1 to 2 and 4 to 5”, “1 to 3 and 5”, etc. When numerical ranges are described herein, unless otherwise stated, the range is intended to include its endpoints and all integers and fractions within that range.

[0030] Furthermore, the technical features involved in the various embodiments of the present invention can be combined with each other as long as they do not conflict with each other.

[0031] In one embodiment of the present invention, a method for preparing an agate-colored coated workpiece is provided, comprising the following steps:

[0032] S1. A transition layer is deposited on the substrate material using magnetron sputtering.

[0033] S2. An intermediate layer is deposited on the transition layer using magnetron sputtering.

[0034] S3. A TiAlSiN agate-colored coating was deposited using magnetron sputtering.

[0035] In S3, the sputtering power of the Si target is controlled so that the percentage of Si element in the deposited TiAlSiN agate-colored coating is 7%~8%.

[0036] By adopting the above technical solution, this invention uses magnetron sputtering technology to deposit a TiAlSiN agate-colored coating on a substrate material. In this technology, the magnetron sputtering instrument emits electrons and applies an electric field to them. Ar and N2 are then introduced into the coating chamber. Argon atoms and electrons collide under the action of the electric field, ionizing a large number of argon ions. The argon ions are accelerated under the action of the electric field to bombard the Ti, Al, and Si targets located in the magnetron sputtering coating machine, sputtering a large number of titanium, aluminum, and silicon atoms. At the same time, nitrogen molecules also collide with electrons under the action of the electric field, ionizing a large number of nitrogen atoms. Titanium, aluminum, silicon, and nitrogen atoms are deposited on the substrate material to complete the coating.

[0037] Meanwhile, this invention changes the proportion of each element in the TiAlSiN agate-colored coating, increasing the silicon content to 7%~8%. Silicon atoms can form covalent bonds with nitrogen atoms, forming a large number of Si-N-Si hard grid structures, thereby greatly enhancing the wear resistance of the coating.

[0038] Preferably, step S1 specifically includes the following steps: introducing Ar into the coating chamber until the gas pressure reaches 0.3~0.5Pa, setting the bias voltage to -50Pa, turning on the target material, and depositing the transition layer.

[0039] By employing the above technical solution, argon gas is first introduced into the coating chamber. Through glow discharge of the argon gas, high-energy argon ions are generated. These high-energy argon ions bombard the substrate material at high speed under the influence of a magnetic field, cleaning away any adhering substances on the substrate material surface. Furthermore, this invention also deposits a transition layer between the coating and the substrate material, allowing the TiAlSiN agate-colored coating to be deposited more effectively on the substrate material, thus improving the coating deposition quality.

[0040] Preferably, step S2 specifically includes the following steps:

[0041] S21. Introduce reactive gas N2 into the coating chamber, adjust the gas pressure to 0.40~0.44Pa, and simultaneously turn on the Ti target and Al target to obtain the intermediate layer (TiAlN layer).

[0042] S22. Continue to introduce reactive gas N2 into the coating chamber, adjust the gas pressure to 0.40~0.44Pa, and simultaneously turn on the Ti target and Al target to obtain a dense intermediate layer (TiAlN layer).

[0043] By adopting the above technical solution, the present invention also deposits a TiAlN intermediate layer between the transition layer (pure Ti layer) and the TiAlSiN agate-colored coating. The intermediate layer can effectively alleviate the contradiction of insufficient coating adhesion caused by the mismatch of physical properties such as elastic modulus between coatings, and improve the interlayer adhesion.

[0044] Preferably, step S3 specifically includes the following steps: introducing reactive gas N2 into the coating chamber, adjusting the gas pressure to 0.46~0.50 Pa, and simultaneously turning on the Ti target, Al target and Si target to obtain a TiAlSiN agate-colored coating.

[0045] By adopting the above technical solution, under the deposition conditions, the deposited TiAlSiN layer has ultra-high hardness and wear resistance, which improves the quality of the coating and extends the service life of the coated product.

[0046] Preferably, in step S1, a pair of Ti targets, a pair of Al targets, and a pair of Si targets are provided in the coating chamber. The Ti targets and Si targets are placed at one end of the coating chamber in a target-to-target configuration, and the Al targets are placed at the other end of the coating chamber in a target-to-target configuration.

[0047] By adopting the above technical solution, three pairs of targets are placed in specific positions, which enables better deposition of the intermediate layer (TiAlN layer), resulting in stable coating color, uniform film thickness, and stable optical effect on the substrate material surface.

[0048] Preferably, the substrate material is pretreated by cleaning before the transition layer is deposited on the surface of the substrate material in step S1.

[0049] By adopting the above technical solution, the present invention further improves the quality of coating by cleaning and pre-treating the substrate material before coating, thereby breaking the adsorption of pollutants on the workpiece surface, allowing the pollutants to peel off from the workpiece surface, completing the cleaning of the workpiece, and improving the coating effect on the workpiece.

[0050] Preferably, the cleaning pretreatment includes the following steps: first, ultrasonic cleaning of the substrate material, then vacuuming and heating the coating chamber; when the gas pressure in the coating chamber reaches 0.001 Pa, Ar is introduced into the coating chamber; when the gas pressure reaches -2 to 0 Pa and the bias voltage is set to -300 V, ion cleaning of the substrate material is performed.

[0051] By adopting the above technical solution, this invention further improves the coating quality by ultrasonically cleaning the substrate material before coating. The ultrasonic cleaning machine in this technology can convert the acoustic energy of the high-power ultrasonic frequency source into mechanical vibration. The ultrasonic waves are radiated into the cleaning liquid in the tank through the cleaning tank wall. Due to the radiation of the ultrasonic waves, the cleaning liquid in the tank will generate microbubbles and maintain vibration, thereby destroying the adsorption of contaminants on the surface of the workpiece and causing the contaminants to peel off from the surface of the workpiece, thus completing the cleaning of the workpiece. In order to further clean the substrate material, this invention also performs ion cleaning on the substrate material. Since a high-frequency alternating electric field is formed in the coating chamber, the oxygen or argon gas in the coating chamber will form plasma under the action of the alternating electric field. Under the dual action of the chemical reaction of the plasma and repeated physical bombardment, the contaminants on the surface of the substrate material are transformed into ions or gaseous substances and discharged from the coating chamber, thus completing the cleaning of the substrate material and allowing the subsequently deposited film layer to better adhere to the surface of the substrate material.

[0052] Preferably, in step S11, the ion cleaning of the substrate material is performed by arc bombardment cleaning.

[0053] By adopting the above technical solution, the present invention also performs arc bombardment cleaning on the substrate material. By applying a high-voltage electric field to the gas in the coating chamber, the gas ion beam bombards the substrate material. The bombardment energy can be transferred to the lattice atoms of the substrate material, thereby destroying the lattice structure of the substrate material, increasing the micro-roughness of the substrate material, and completely exposing the surface atoms of the substrate material, thus improving the atomic polarizability. In this way, when depositing a coating on the substrate material, the distance between the transition layer and the surface atoms of the substrate material will be reduced, and the contact area between the transition layer and the surface of the substrate material will be increased, significantly enhancing the mechanical locking force between the two, thereby significantly improving the adhesion between the transition layer and the substrate material, so that the prepared TiAlSiN layer can be better deposited on the surface of the substrate material.

[0054] Preferably, in step S12, a pure Ti layer is used as the transition layer.

[0055] By adopting the above technical solution, the present invention uses a pure Ti layer as a transition layer between the substrate material and the TiAlSiN layer. Ti can reduce the residual stress between the substrate material and the coating, enhance the bonding force between the TiAlSiN layer and the substrate material, and enable the TiAlSiN layer to be deposited more tightly on the substrate material, thereby further improving the deposition effect.

[0056] Example

[0057] A method for preparing an agate-colored coated workpiece includes the following steps:

[0058] Cleaning pretreatment: First, use a mixed solution of potassium permanganate and hydrogen peroxide as the cleaning solution. Place the substrate material to be coated in an ultrasonic cleaner for 20 minutes.

[0059] S1. First, use a degreasing and dewaxing solution as the cleaning agent. Place the substrate material to be coated in an ultrasonic cleaner for 20 minutes. Then, place the Ti and Si targets in a target-to-target configuration at one end of the coating chamber, and place the Al target in a target-to-target configuration at the other end of the coating chamber away from the Ti and Si targets. Then, use a vacuum pump to evacuate the coating chamber until the pressure reaches 0.001 Pa. Heat the coating chamber and maintain the temperature at 150°C. Then, introduce argon gas into the coating chamber so that when the pressure reaches 0.4 Pa, the bias voltage parameter is set to -300 V. Then, start the intermediate frequency coating power supply, set the current parameter of the Ti target to 30 A, and sputter the substrate material for 20 minutes to obtain a transition layer (pure Ti layer).

[0060] S2. Introduce N2 into the coating chamber and adjust the gas pressure until it stabilizes at 0.42 Pa. Simultaneously turn on the Ti target and Al target, set the current parameter of the Ti target to 30 A and the current parameter of the Al target to 15 A, and deposit the substrate material for 20 min to obtain the intermediate layer (TiAlN layer). Continue to introduce N2 into the coating chamber and adjust the gas pressure until it stabilizes at 0.45 Pa, and deposit the substrate material for 30 min to obtain the dense intermediate layer (TiAlN layer).

[0061] S3. Continue to introduce N2 into the coating chamber, adjust the gas pressure until it stabilizes at 0.42 Pa, then adjust it to stabilize at 0.48 Pa. Simultaneously turn on the Ti target, Al target, and Si target. The current parameters for the Ti target are set to 10 A, the Al target to 15 A, and the Si target to 20 A. Deposit on the substrate material for 42 min to obtain a TiAlSiN agate-colored coating, and end the coating process. The percentage of Si element in the TiAlSiN layer is controlled to be between 7% and 8%, and the Si element content in the obtained TiAlSiN layer is 7.6%.

[0062] Comparative Example

[0063] The difference from the example is that a TiON film system (TiAlON coating) is deposited on the substrate material using magnetron sputtering technology.

[0064] Performance testing

[0065] The coating products prepared in the examples and comparative examples were tested for abrasion resistance according to ISO 23160 standard.

[0066] Test method: Place a 4L grinding stone in a clean vibrating dish, then slowly add 24ml of grinding liquid to the dish. Start the vibrating dish and wait for the grinding liquid to be evenly distributed on the dish. Then slowly add 800ml of water. After a small amount of grinding liquid foam remains around the central cylinder of the dish, place the product to be tested in the dish and conduct tests for 24 hours and 48 hours.

[0067] Test results: such as Figures 1-4 As shown, Figure 1 This is a schematic diagram of the product obtained in an embodiment of the present invention after a 48-hour abrasion resistance test. Figure 2 This is a schematic diagram from another angle showing the product obtained in an embodiment of the present invention after undergoing a 48-hour abrasion resistance test. Figure 3 This is a schematic diagram of the product obtained in the comparative example of this invention after a 48-hour abrasion resistance test. Figure 4 This is a schematic diagram from another angle showing the product obtained in the comparative example of the present invention after a 48-hour abrasion resistance test. The product prepared in the example can withstand the 48-hour test without the surface coating peeling off; the product prepared in the comparative example can withstand the 24-hour test but not the 48-hour test, after which the surface coating peels off.

[0068] The above description is merely a preferred embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural or procedural transformations made based on the content of the present invention's specification and drawings, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. A method for preparing an agate-colored coated workpiece, characterized in that, Specifically, the following steps are included: S1. A transition layer is deposited on the substrate material using magnetron sputtering. S2. A TiAlN intermediate layer is deposited on the transition layer in S1 by magnetron sputtering. S3. A TiAlSiN agate-colored coating is deposited on the TiAlN intermediate layer in S2 by magnetron sputtering. In step S3, the sputtering power of the Si target is controlled so that the percentage of Si element in the deposited TiAlSiN layer is 7% to 8%. In S1, the specific steps include: introducing Ar into the coating chamber until the pressure reaches 0.3~0.5Pa, setting the bias voltage to -300V, turning on the target, and depositing the transition layer. In S1, the transition layer is a pure Ti layer. S2 specifically includes the following steps: S21. Introduce reactive gas N2 into the coating chamber, adjust the gas pressure to 0.41~0.43 Pa, and simultaneously turn on the Ti target and Al target. Deposit for 15~25 min to obtain the TiAlN intermediate layer. S22. Continue to introduce reactive gas N2 into the coating chamber, adjust the gas pressure to 0.44~0.46Pa, and simultaneously turn on the Ti target and Al target. Deposit for 25~35 minutes to obtain a dense TiAlN intermediate layer. Before S1, a mixed solution of potassium permanganate and hydrogen peroxide is used as the cleaning solution. The substrate material to be coated is placed in an ultrasonic cleaner and cleaned for 15-25 minutes. In S3, the specific steps include: introducing reactive gas N2 into the coating chamber, adjusting the gas pressure to 0.46~0.50 Pa, simultaneously turning on the Ti target, Al target and Si target, depositing on the substrate material for 40~45 min to obtain a TiAlSiN agate-colored coating, and ending the coating process; in S3, the current parameter of the Ti target is set to 10 A, the current parameter of the Al target is set to 15 A, and the current parameter of the Si target is set to 20 A.

2. The method for preparing an agate-colored coated workpiece according to claim 1, characterized in that, In S2, the current parameter of the Ti target is 30A, and the current parameter of the Al target is 15A.

3. An agate-colored coated workpiece, characterized in that, It is made using the preparation method of the agate-colored coated workpiece according to any one of claims 1 to 2.

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