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CN-122013109-A - Preparation method of yttrium oxide-zirconium oxide composite coating

CN122013109ACN 122013109 ACN122013109 ACN 122013109ACN-122013109-A

Abstract

The invention discloses a preparation method of an yttrium oxide-zirconium oxide composite coating, which comprises the following steps of S11, mounting a cleaned and dried glass substrate on a rotary substrate table in a coating cavity, introducing argon plasma into the coating cavity to bombard and clean the surface of the glass substrate, S12, introducing argon and oxygen into the coating cavity, and simultaneously starting an yttrium target and a zirconium target to perform magnetron sputtering so as to deposit and form the yttrium oxide-zirconium oxide composite coating on the surface of the glass substrate in reciprocating rotary motion. According to the invention, a charge compensation effect is introduced through Zr 4+ doping so as to reduce the concentration of oxygen vacancies in the coating, thereby improving the visible light transmittance and chemical stability of the coating. Meanwhile, the invention breaks the growth of the columnar crystal of the yttrium oxide through the formation of the zirconium oxide, thereby optimizing the microstructure of the coating and ensuring that the coating has good etching resistance.

Inventors

  • XIAO SHU
  • CHEN YINTING
  • FENG ZIQING
  • CHEN RUIXUE
  • Yuan Haihang
  • HUANG HANRUI
  • LI QIANG

Assignees

  • 华南理工大学
  • 广东钇芯微半导体技术有限公司

Dates

Publication Date
20260512
Application Date
20260409

Claims (10)

  1. 1. The preparation method of the yttrium oxide-zirconium oxide composite coating is characterized by comprising the following steps of: Step S11, mounting the cleaned and dried glass substrate on a rotary substrate stand in a coating cavity, and introducing argon plasma into the coating cavity to bombard and clean the surface of the glass substrate; And S12, introducing argon and oxygen into the film coating cavity, and simultaneously starting an yttrium target and a zirconium target to perform magnetron sputtering so as to deposit and form a yttrium oxide-zirconium oxide composite coating on the surface of the glass substrate in reciprocating rotary motion, wherein the flow ratio of the argon to the oxygen is 12:1, the sputtering power of the yttrium target is 200-500W, and the sputtering power of the zirconium target is 20-60W.
  2. 2. The method for producing a yttria-zirconia composite coating according to claim 1, wherein prior to step S11, the method further comprises: and placing the glass substrate in an alcohol solution for ultrasonic cleaning, and then drying, wherein the ultrasonic cleaning time is 5-30 min.
  3. 3. The method for producing a yttria-zirconia composite coating according to claim 1, wherein in step S11, a pulse bias power supply for applying a negative bias voltage to the glass substrate and a heating device for heating the glass substrate are provided on the rotating base.
  4. 4. The method for preparing a yttria-zirconia composite coating according to claim 3, wherein the voltage range of the pulse bias power supply is 50-200 v, and the heating temperature range of the heating device is 0-300 ℃.
  5. 5. The method for preparing a yttria-zirconia composite coating according to claim 3, wherein the rotating base frame has a reciprocating rotation angle of 30-120 degrees, a rotation speed of 1-5 rpm and a reciprocating period of 50-200 times.
  6. 6. The method of claim 1, wherein in step S11, the gas ion source is a linear anode ion source, the argon flow is 5-30 sccm, the voltage adjustable range is 800-1200 v, and the bombardment time is 5-30 min.
  7. 7. The method for producing a yttria-zirconia composite coating according to claim 1, wherein in step S12, the flow rate of argon is 20 to 40sccm, the flow rate of oxygen is 1 to 10sccm, the sputtering voltage range of the yttrium target is 100 to 500v, and the sputtering voltage range of the zirconium target is 200 to 400v.
  8. 8. The method for preparing a yttria-zirconia composite coating according to claim 1, wherein in step S12, a magnetron sputtering rectangular cathode is adopted as a yttrium target sputtering cathode, the area is (1-5) ×10 5 mm 3 , and a pulse direct current power supply is adopted; the zirconium target sputtering cathode adopts a magnetron sputtering circular cathode, the area is (5-8) multiplied by 10 3 mm 2 , and a direct current power supply is adopted.
  9. 9. The method for preparing the yttrium oxide-zirconium oxide composite coating according to claim 8, wherein the distances between the yttrium target sputtering cathode and the zirconium target sputtering cathode and the surface of the glass substrate to be coated are 50-300 mm.
  10. 10. The method for producing a yttria-zirconia composite coating according to any one of claims 1 to 9, wherein the total thickness of the yttria-zirconia composite coating is 1 to 10 μm.

Description

Preparation method of yttrium oxide-zirconium oxide composite coating Technical Field The invention relates to the technical field of material surface treatment, in particular to a preparation method of an yttrium oxide-zirconium oxide composite coating. Background At present, with the development of the semiconductor integrated circuit industry toward miniaturization, the high-density plasma environment in the dry etching process has put very high protection requirements on parts in the reaction chamber. Especially, for the optical window and transparent protective cover plate responsible for process monitoring, not only the extremely strong chemical corrosion resistance is needed to prevent the wafer from being polluted by impurity particles, but also the excellent optical transmittance is needed to be maintained to ensure the accuracy of spectrum monitoring. Yttria films are recognized as the first protective material against fluorine-based or chlorine-based plasma attack by virtue of its extremely low standard free energy of formation and excellent thermodynamic stability. However, when the yttrium oxide film is prepared by adopting the existing physical vapor deposition technologies such as magnetron sputtering and the like, a significant technical bottleneck is still faced. On one hand, high-energy particle bombardment and anoxic environment in the deposition process are very easy to induce high-concentration oxygen vacancies in the coating, and the vacancies can form deep energy level defect states and absorption centers in a forbidden band, so that the coating is light yellow, the transparency is obviously reduced, and the use standard of a precision optical component is difficult to meet, on the other hand, a pure yttrium oxide film tends to grow in a columnar crystal, the structure at the crystal boundary is loose and has micropores, corrosive plasmas are very easy to permeate inwards along a crystal boundary channel and accelerate etching, and the compactness and the service life of the coating are severely limited. Disclosure of Invention Based on the above, the invention aims to provide a preparation method of an yttrium oxide-zirconium oxide composite coating, which is used for improving the visible light transmittance and the etching resistance of the coating, so as to prolong the service life of semiconductor equipment parts (such as an observation window) in a high-energy plasma environment. A preparation method of an yttrium oxide-zirconium oxide composite coating comprises the following steps: Step S11, mounting the cleaned and dried glass substrate on a rotary substrate stand in a coating cavity, and introducing argon plasma into the coating cavity to bombard and clean the surface of the glass substrate; And S12, introducing argon and oxygen into the film coating cavity, and simultaneously starting an yttrium target and a zirconium target to perform magnetron sputtering so as to deposit and form a yttrium oxide-zirconium oxide composite coating on the surface of the glass substrate in reciprocating rotary motion, wherein the flow ratio of the argon to the oxygen is 12:1, the sputtering power of the yttrium target is 200-500W, and the sputtering power of the zirconium target is 20-60W. Preferably, before step S11, the preparation method further includes: and placing the glass substrate in an alcohol solution for ultrasonic cleaning, and then drying, wherein the ultrasonic cleaning time is 5-30 min. Preferably, in step S11, the rotating base is provided with a pulse bias power supply for applying a negative bias voltage to the glass substrate, and a heating device for heating the glass substrate. Preferably, the voltage range of the pulse bias power supply is 50-200V, and the heating temperature range of the heating device is 0-300 ℃. Preferably, the reciprocating rotation angle of the rotary base frame is 30-120 degrees, the rotating speed is 1-5 rpm, and the reciprocating period is 50-200 times. Preferably, in step S11, the gas ion source is a linear anode ion source, the argon flow is 5-30 sccm, the voltage adjustable range is 800-1200V, and the bombardment time is 5-30 min. Preferably, in step S12, the flow rate of argon is 20-40 sccm, the flow rate of oxygen is 1-10 sccm, the sputtering voltage range of the yttrium target is 100-500 v, and the sputtering voltage range of the zirconium target is 200-400 v. Preferably, in step S12, the yttrium target sputtering cathode is a magnetron sputtering rectangular cathode, the area is (1-5) ×10 5mm3, and a pulse dc power supply is used; the zirconium target sputtering cathode adopts a magnetron sputtering circular cathode, the area is (5-8) multiplied by 10 3mm2, and a direct current power supply is adopted. Preferably, the distances between the yttrium target sputtering cathode and the zirconium target sputtering cathode and the surface of the glass substrate to be coated are 50-300 mm. Preferably, the total thickness of the yttria-zirconia co