Method for preparing a protective coating on a surface of key components and parts of IC devices based on plasma spraying technology and cold spraying technology

20220275518 · 2022-09-01

    Inventors

    Cpc classification

    International classification

    Abstract

    Through the plasma spraying technology and the cold spraying high-speed deposition technology, an evenly distributed protective coating is formed on the surface of a plasma etching chamber. The protective coating, having a double-layer composite structure, includes a metal+Y.sub.2O.sub.3 coating as a metal+Y.sub.2O.sub.3 transition layer deposited by plasma spraying as a lower layer of the double-layer composite structure, and a high-purity Y.sub.2O.sub.3 ceramic coating coated on the metal+Y.sub.2O.sub.3 transition layer as an upper layer of the double-layer composite structure, the metal+Y.sub.2O.sub.3 transition layer is configured to reduce the difference in expansion coefficient between the Y.sub.2O.sub.3 ceramic coating and the metal substrate, and enhance the bonding force between the Y.sub.2O.sub.3 ceramic coating and the metal substrate; the high-purity Y.sub.2O.sub.3 ceramic coating is formed by depositing Y.sub.2O.sub.3 ceramic powders on the metal+Y.sub.2O.sub.3 transition layer at high speed through cold spraying high-speed deposition.

    Claims

    1. A method for preparing a protective coating on a surface of key components and parts of an IC (integrated circuit) device based on plasma spraying technology and cold spraying technology, wherein: the method adopts the plasma spraying technology and cold spraying high-speed deposition technology to form an evenly distributed protective coating on a surface of a plasma etching chamber of the IC device; the protective coating, having a double-layer composite structure, comprises a metal+Y.sub.2O.sub.3 transition layer deposited by plasma spraying as a lower layer of the double-layer composite structure, and a high-purity Y.sub.2O.sub.3 ceramic coating coated on the metal+Y.sub.2O.sub.3 transition layer as an upper layer of the double-layer composite structure, the high-purity Y.sub.2O.sub.3 ceramic coating is formed by depositing Y.sub.2O.sub.3 ceramic powders on the metal+Y.sub.2O.sub.3 transition layer at high speed through cold spraying high-speed deposition; the method comprises steps of drying metal powders and Y.sub.2O.sub.3 powders, respectively, and then obtaining a metal+Y.sub.2O.sub.3 layer by depositing the metal and Y.sub.2O.sub.3 powders on a substrate at high speed through supersonic plasma spraying technology, and then depositing high-purity Y.sub.2O.sub.3 powders on the metal+Y.sub.2O.sub.3 layer through cold spraying high-throughout deposition technology, so as to obtain the protective coating through controlling process parameters.

    2. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 1, wherein the method comprises steps of: (1) drying metal powders to be sprayed and Y.sub.2O.sub.3 powders to be sprayed, respectively, wherein a purity of the metal powders and the Y.sub.2O.sub.3 powders is above 99.9 wt. %; (2) preparing a metal+Y.sub.2O.sub.3 transition layer on a substrate through plasma spraying technology, which comprises: placing the dried metal and Y.sub.2O.sub.3 powders into a powder feeder of a plasma spraying device, obtaining mixed powders after evenly mixing the dried metal and Y.sub.2O.sub.3 powders, melting and depositing the mixed powders on an inner surface of a plasma etching chamber through the plasma spraying technology, so as to obtain the metal+Y.sub.2O.sub.3 transition layer; and (3) depositing a high-purity Y.sub.2O.sub.3 coating through cold spraying high-speed deposition technology, which is specifically embodied as depositing high-purity Y.sub.2O.sub.3 powders through the cold spraying high-speed deposition technology on the metal+Y.sub.2O.sub.3 transition layer obtained by the step (2), so as to obtain the high-purity Y.sub.2O.sub.3 coating, whereby, a (metal+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite protective coating is obtained.

    3-6. (canceled)

    7. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 1, wherein a porosity of the protective coating is below 2%, an interface bonding strength of the protective coating and the substrate is in a range of 20 to 100 MPa, and a thickness of the protective coating is in a range of 10 to 400 μm.

    8. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 1, wherein the metal powders are at least one member selected from a group consisting of aluminum powders and yttrium powders.

    9. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 2, wherein the metal powders are at least one member selected from a group consisting of aluminum powders and yttrium powders.

    10. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 1, wherein a particle size of the metal powders and the Y.sub.2O.sub.3 powders is in a range of 1-50 μm.

    11. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 2, wherein a particle size of the metal powders and the Y.sub.2O.sub.3 powders is in a range of 1-50 μm.

    12. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 1, wherein the mixed powders are directly sprayed on the inner surface of the plasma etching chamber through supersonic plasma spraying technology, and simultaneously plasma spraying parameters are controlled, wherein main working gas used in the plasma spraying technology is argon, secondary working gas is hydrogen, powder feeding gas is nitrogen, and gas flow rates thereof are in a range of 10-80 mL/min, 5-220 mL/min and 5-80 mL/min, respectively; a spraying distance is in a range of 10-100 mm, so that the mixed powders are deposited on the inner surface of the plasma etching chamber, so as to obtain the evenly distributed metal+Y.sub.2O.sub.3 protective coating.

    13. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 2, wherein the mixed powders are directly sprayed on the inner surface of the plasma etching chamber through supersonic plasma spraying technology, and simultaneously plasma spraying parameters are controlled, wherein main working gas used in the plasma spraying technology is argon, secondary working gas is hydrogen, powder feeding gas is nitrogen, and gas flow rates thereof are in a range of 10-80 mL/min, 5-220 mL/min and 5-80 mL/min, respectively; a spraying distance is in a range of 10-100 mm, so that the mixed powders are deposited on the inner surface of the plasma etching chamber, so as to obtain the evenly distributed metal+Y.sub.2O.sub.3 protective coating.

    14. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 1, wherein the high-purity Y.sub.2O.sub.3 powders are deposited on the metal+Y.sub.2O.sub.3 transition layer obtained by the step (2) through the cold spraying high-speed deposition technology, and simultaneously cold spraying parameters are controlled, wherein compressed air is used as working gas, a temperature of the compressed air is in a range of 200 to 700° C., a pressure of the compressed air is in a range of 1.5 to 3.0 MPa, and a spraying distance is in a range of 10 to 60 mm, so that the high-purity Y.sub.2O.sub.3 powders are deposited on the metal+Y.sub.2O.sub.3 transition layer, so as to obtain the evenly distributed high-purity Y.sub.2O.sub.3 coating.

    15. The method for preparing the protective coating on the surface of the key components and parts of the IC device based on the plasma spraying technology and the cold spraying technology according to claim 2, wherein the high-purity Y.sub.2O.sub.3 powders are deposited on the metal+Y.sub.2O.sub.3 transition layer obtained by the step (2) through the cold spraying high-speed deposition technology, and simultaneously cold spraying parameters are controlled, wherein compressed air is used as working gas, a temperature of the compressed air is in a range of 200 to 700° C., a pressure of the compressed air is in a range of 1.5 to 3.0 MPa, and a spraying distance is in a range of 10 to 60 mm, so that the high-purity Y.sub.2O.sub.3 powders are deposited on the metal+Y.sub.2O.sub.3 transition layer, so as to obtain the evenly distributed high-purity Y.sub.2O.sub.3 coating.

    Description

    BRIEF DESCRIPTION OF THE DRAWINGS

    [0028] The drawing is a schematic diagram of a (metal+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating.

    [0029] In the drawing, 1: substrate; 2: metal+Y.sub.2O.sub.3 transition layer; 3: high-purity Y.sub.2O.sub.3 coating.

    DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT

    [0030] In the specific embodiments provided by the present invention, metal powders and Y.sub.2O.sub.3 powders are mixed in accordance with a weight ratio in a range of (0.1-5):1. After the mixture is dried, micron mixed powders with a particle size in a range of 1-50 μm are obtained. The above-mentioned micron mixed powders and high-purity Y.sub.2O.sub.3 powders are preheated by heated compressed air and then deposited on an inner surface of a plasma etching chamber by plasma spraying technology or cold spraying technology in order of priority, so that a protective coating is obtained on the inner surface of the plasma etching chamber. The plasma spraying technology is specifically described as follows: when the main working gas is argon, the secondary working gas is hydrogen, and the powder feeding gas is nitrogen, gas flow rates thereof are in a range of 10-80 mL/min, 5-220 mL/min and 5-80 mL/min, respectively; a spraying distance is in a range of 10-100 mm. The cold spraying technology is specifically described as follows: the compressed air is used as working gas, a temperature of the compressed air is in a range of 200−700° C., a pressure of the compressed air is in a range of 1.5-3.0 MPa, and a spraying distance is in a range of 10-60 mm.

    [0031] The present invention is further detailed described in combination with embodiments as follows.

    First Embodiment

    [0032] According to the first embodiment of the present invention, a method for preparing a protective coating on a 6061 aluminum alloy substrate for protecting an inner surface of a plasma etching chamber of an IC (integrated circuit) device comprises steps of:

    [0033] (1) weighing 20 g of pure Al powders and 160 g of pure Y.sub.2O.sub.3 powders, mixing the pure Al powders with the Y.sub.2O.sub.3 powders, obtaining mixed micron (Al+Y.sub.2O.sub.3) powders after drying, weighing 300 g of high-purity Y.sub.2O.sub.3 powders with a purity of 99.99 wt. %, and drying the high-purity Y.sub.2O.sub.3 powders;

    [0034] (2) preparing a (Al+Y.sub.2O.sub.3) coating with a thickness of 150 μm as a (Al+Y.sub.2O.sub.3) transition layer on the 6061 aluminum alloy substrate through plasma spraying technology by taking the mixed micron (Al+Y.sub.2O.sub.3) powders obtained by the step (1) as a raw material; and

    [0035] (3) depositing a high-purity Y.sub.2O.sub.3 coating with a thickness of 180 μm on the (Al+Y.sub.2O.sub.3) transition layer obtained by the step (2) through cold spraying high-speed deposition technology by taking the dried high-purity Y.sub.2O.sub.3 powders obtained by the step (1) as a raw material, so that a (Al+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating as the protective coating is obtained.

    [0036] In the step (2) of preparing the (Al+Y.sub.2O.sub.3) transition layer through plasma spraying technology, main working gas is argon, secondary working gas is hydrogen, powder feeding gas is nitrogen, and gas flow rates thereof are 30 mL/min, 220 mL/min and 30 mL/min, respectively; a spraying distance is 80 mm.

    [0037] In the step (3) of depositing the high-purity Y.sub.2O.sub.3 coating through cold spraying high-speed deposition technology, compressed air is used as working gas, a temperature of the compressed air is 500° C., a pressure of the compressed air is 2.0 MPa, and a spraying distance is 20 mm.

    [0038] As shown in the drawing, a metal+Y.sub.2O.sub.3 transition layer 2 is coated on a substrate 1 through plasma spraying technology, a high-purity Y.sub.2O.sub.3 coating 3 is coated on the metal+Y.sub.2O.sub.3 transition layer 2 through cold spraying high-speed deposition technology. The (Al+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating provided by the first embodiment has a porosity of 2.0% and an interface bonding strength between a ceramic coating and the substrate is 45 MPa.

    Second Embodiment

    [0039] According to the second embodiment of the present invention, a method for preparing a protective coating on a 6061 aluminum alloy substrate for protecting an inner surface of a plasma etching chamber of an IC (integrated circuit) device comprises steps of:

    [0040] (1) weighing 70 g of pure Al powders and 150 g of Y.sub.2O.sub.3 powders, mixing the pure Al powders with the Y.sub.2O.sub.3 powders, obtaining mixed micron (Al+Y.sub.2O.sub.3) powders after drying, weighing 200 g of high-purity Y.sub.2O.sub.3 powders with a purity of 99.99 wt. %, and drying the high-purity Y.sub.2O.sub.3 powders;

    [0041] (2) preparing a (Al+Y.sub.2O.sub.3) coating with a thickness of 120 μm as a (Al+Y.sub.2O.sub.3) transition layer on the 6061 aluminum alloy substrate through plasma spraying technology by taking the mixed micron (Al+Y.sub.2O.sub.3) powders obtained by the step (1) as a raw material; and

    [0042] (3) depositing a high-purity Y.sub.2O.sub.3 coating with a thickness of 170 μm on the (Al+Y.sub.2O.sub.3) transition layer obtained by the step (2) through cold spraying high-throughput deposition technology by taking the dried high-purity Y.sub.2O.sub.3 powders obtained by the step (1) as a raw material, so that a (Al+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating as the protective coating is obtained.

    [0043] In the step (2) of preparing the (Al+Y.sub.2O.sub.3) transition layer through plasma spraying technology, main working gas is argon, secondary working gas is hydrogen, powder feeding gas is nitrogen, and gas flow rates thereof are 25 mL/min, 200 mL/min and 30 mL/min, respectively; a spraying distance is 90 mm.

    [0044] In the step (3) of depositing the high-purity Y.sub.2O.sub.3 coating through cold spraying high-throughput deposition technology, compressed air is used as working gas, a temperature of the compressed air is 550° C., a pressure of the compressed air is 2.2 MPa, and a spraying distance is 20 mm.

    [0045] As shown in the drawing, a metal+Y.sub.2O.sub.3 transition layer 2 is coated on a substrate 1 through plasma spraying technology, a high-purity Y.sub.2O.sub.3 coating 3 is coated on the metal+Y.sub.2O.sub.3 transition layer 2 through cold spraying high-throughput deposition technology. The (Al+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating provided by the second embodiment has a porosity of 1.8% and an interface bonding strength between a ceramic coating and the substrate is 60 MPa.

    Third Embodiment

    [0046] According to the third embodiment of the present invention, a method for preparing a protective coating on a 6061 aluminum alloy substrate for protecting an inner surface of a plasma etching chamber of an IC (integrated circuit) device comprises steps of:

    [0047] (1) weighing 40 g of pure Al powders and 120 g of Y.sub.2O.sub.3 powders, mixing the pure Al powders with the Y.sub.2O.sub.3 powders, obtaining mixed micron (Al+Y.sub.2O.sub.3) powders after drying, weighing 400 g of high-purity Y.sub.2O.sub.3 powders with a purity of 99.99 wt. %, and drying the high-purity Y.sub.2O.sub.3 powders;

    [0048] (2) preparing a (Al+Y.sub.2O.sub.3) coating with a thickness of 160 μm as a (Al+Y.sub.2O.sub.3) transition layer on the 6061 aluminum alloy substrate through plasma spraying technology by taking the mixed micron (Al+Y.sub.2O.sub.3) powders obtained by the step (1) as a raw material; and

    [0049] (3) depositing a high-purity Y.sub.2O.sub.3 coating with a thickness of 180 μm on the (Al+Y.sub.2O.sub.3) transition layer obtained by the step (2) through cold spraying high-speed deposition technology by taking the dried high-purity Y.sub.2O.sub.3 powders obtained by the step (1) as a raw material, so that a (Al+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating as the protective coating is obtained.

    [0050] In the step (2) of preparing the (Al+Y.sub.2O.sub.3) transition layer through plasma spraying technology, main working gas is argon, secondary working gas is hydrogen, powder feeding gas is nitrogen, and gas flow rates thereof are 30 mL/min, 180 mL/min and 25 mL/min, respectively; a spraying distance is 100 mm.

    [0051] In the step (3) of depositing the high-purity Y.sub.2O.sub.3 coating through cold spraying high-speed deposition technology, compressed air is used as working gas, a temperature of the compressed air is 600° C., a pressure of the compressed air is 2.3 MPa, and a spraying distance is 20 mm.

    [0052] As shown in the drawing, a metal+Y.sub.2O.sub.3 transition layer 2 is coated on a substrate 1 through plasma spraying technology, a high-purity Y.sub.2O.sub.3 coating 3 is coated on the metal+Y.sub.2O.sub.3 transition layer 2 through cold spraying high-speed deposition technology. The (Al+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating provided by the third embodiment has a porosity of 1.7% and an interface bonding strength between a ceramic coating and the substrate is 55 MPa.

    Fourth Embodiment

    [0053] According to the fourth embodiment of the present invention, a method for preparing a protective coating on a 6061 aluminum alloy substrate for protecting an inner surface of a plasma etching chamber of an IC (integrated circuit) device comprises steps of:

    [0054] (1) weighing 40 g of pure Y powders and 120 g of Y.sub.2O.sub.3 powders, mixing the pure Y powders with the Y.sub.2O.sub.3 powders, obtaining mixed micron (Y+Y.sub.2O.sub.3) powders after drying, weighing 400 g of high-purity Y.sub.2O.sub.3 powders with a purity of 99.99 wt. %, and drying the high-purity Y.sub.2O.sub.3 powders;

    [0055] (2) preparing a (Y+Y.sub.2O.sub.3) coating with a thickness of 120 μm as a (Y+Y.sub.2O.sub.3) transition layer on the 6061 aluminum alloy substrate through plasma spraying technology by taking the mixed micron (Y+Y.sub.2O.sub.3) powders obtained by the step (1) as a raw material; and

    [0056] (3) depositing a high-purity Y.sub.2O.sub.3 coating with a thickness of 180 μm on the (Y+Y.sub.2O.sub.3) transition layer obtained by the step (2) through cold spraying high-speed deposition technology by taking the dried high-purity Y.sub.2O.sub.3 powders obtained by the step (1) as a raw material, so that a (Y+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating as the protective coating is obtained.

    [0057] In the step (2) of preparing the (Y+Y.sub.2O.sub.3) transition layer through supersonic plasma spraying technology, main working gas is argon, secondary working gas is hydrogen, powder feeding gas is nitrogen, and gas flow rates thereof are 30 mL/min, 180 mL/min and 25 mL/min, respectively; a spraying distance is 100 mm.

    [0058] In the step (3) of depositing the high-purity Y.sub.2O.sub.3 coating through cold spraying deposition technology, compressed air is used as working gas, a temperature of the compressed air is 650° C., a pressure of the compressed air is 2.3 MPa, and a spraying distance is 20 mm.

    [0059] As shown in the drawing, a metal+Y.sub.2O.sub.3 transition layer 2 is coated on a substrate 1 through plasma spraying technology, a high-purity Y.sub.2O.sub.3 coating 3 is coated on the metal+Y.sub.2O.sub.3 transition layer 2 through cold spraying deposition technology. The (Y+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating provided by the fourth embodiment has a porosity of 1.5% and an interface bonding strength between a ceramic coating and the substrate is 35 MPa.

    [0060] The results of the above embodiments show that, in the method for preparing the protective coating on the inner surface of the plasma etching chamber of the IC device, the plasma spraying technology and the cold spraying high-speed deposition technology are used to prepare the (metal+Y.sub.2O.sub.3)/Y.sub.2O.sub.3 composite coating. The coating, which is well bonded to the substrate, has the porosity of less than 2%, the interface bonding strength in a range of 30-80 MPa, and the thickness in a range of 100-400 μm. The coating is able to reduce the corrosion of corrosive gas to the etching chamber and the pollution of the plasma to the chip, and improve the service life of the plasma etching chamber in the process of producing the chip.

    [0061] The above are detailed embodiments and specific operation processes based on the technical solutions provided by the present invention, but the protective scope of the present invention is not limited to the above embodiments.