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EP-4739642-A1 - DOPED SUBSTANTIALLY SINGLE-PHASE RARE EARTH OXIDE-ZIRCONIA MATERIALS AND METHODS OF MAKING THE SAME

EP4739642A1EP 4739642 A1EP4739642 A1EP 4739642A1EP-4739642-A1

Abstract

New substantially single-phase polycrystalline materials are disclosed. The new substantially single-phase polycrystalline materials generally include from 0.01-20 mol. % zirconia, at least 80 mol. % of one or more rare earth oxides (REO), and 40 to 7000 ppm aluminum by weight, wherein the substantially single-phase polycrystalline material comprises at least 95 wt. % of a solid-solution of REO-zirconia as measured by x-ray diffraction. The new substantially single-phase polycrystalline materials may realize a high density, such as a density of at least 95% of theoretical density, or higher. The new substantially single-phase polycrystalline materials may be in the form of a semiconductor component, including those suited for use in a plasma chamber environment.

Inventors

  • LANDIN, STEVEN
  • HOOK, David Henry

Assignees

  • Coorstek Inc.

Dates

Publication Date
20260513
Application Date
20240625

Claims (20)

  1. 1. A substantially single-phase polycrystalline material comprising yttria (Y2O3) and zirconia (ZrCh), wherein the substantially single-phase polycrystalline material comprises from 0.01-20 mol. % zirconia and at least 80 mol. % yttria, and wherein the substantially single-phase polycrystalline material further comprises from 40 to 7000 ppm aluminum by weight, wherein the substantially single-phase polycrystalline material comprises at least 95 wt. % of a solid-solution of yttria-zirconia as measured by x-ray diffraction.
  2. 2. The substantially single-phase poly crystalline material of claim 1, comprising at least 100 ppm of aluminum, or at least 200 ppm of aluminum, or at least 250 ppm of aluminum, or at least 300 ppm of aluminum, or at least 350 ppm of aluminum, or at least 400 ppm of aluminum, or at least 450 ppm of aluminum, or at least 500 ppm of aluminum, or at least 550 ppm of aluminum, or at least 600 ppm of aluminum, or at least 650 ppm of aluminum, or at least 700 ppm of aluminum, or at least 750 ppm of aluminum, or at least 800 ppm of aluminum, or at least 850 ppm of aluminum, or at least 900 ppm of aluminum, or at least 1000 ppm of aluminum, or at least 1100 ppm of aluminum, or at least 1200 ppm of aluminum, or at least 1300 ppm of aluminum, or at least 1400 ppm of aluminum, or at least 1500 ppm of aluminum.
  3. 3. The substantially single-phase polycrystalline material of any of the preceding claims, comprising not greater than 6000 ppm of aluminum, or not greater than 5000 ppm of aluminum, or not greater than 4500 ppm of aluminum, or not greater than 4000 ppm of aluminum, or not greater than 3500 ppm of aluminum, or not greater than 3000 ppm of aluminum, or not greater than 2500 ppm of aluminum, or not greater than 2400 ppm of aluminum, or not greater than 2300 ppm of aluminum, or not greater than 2200 ppm of aluminum, or not greater than 2100 ppm of aluminum, or not greater than 2000 ppm of aluminum, or not greater than 1900 ppm of aluminum, or not greater than 1800 ppm of aluminum, or not greater than 1700 ppm of aluminum, or not greater than 1600 ppm of aluminum, or not greater than 1500 ppm of aluminum.
  4. 4. The substantially single-phase polycrystalline material of any of the preceding claims, wherein the substantially single-phase polycrystalline material realizes a density of at least 95% of its theoretical density, or at least 96% of its theoretical density, or at least 96.5% of its theoretical density, or at least 97% of its theoretical density, or at least 97.5% of its theoretical density, or at least 98% of its theoretical density, or at least 98.2% of its theoretical density, or at least 98.4% of its theoretical density, or at least 98.5% of its theoretical density, or at least 98.6% of its theoretical density, or at least 98.7% of its theoretical density, or at least 98.8% of its theoretical density, or at least 98.9% of its theoretical density, or at least 99.0% of its theoretical density, or at least 99.1% of its theoretical density, or at least 99.2% of its theoretical density, or at least 99.3% of its theoretical density, or at least 99.4% of its theoretical density, or at least 99.5% of its theoretical density, or at least 99.6% of its theoretical density, or at least 99.7% of its theoretical density, or at least 99.8% of its theoretical density, or at least 99.9% of its theoretical density.
  5. 5. The substantially single-phase poly crystalline material of any of the preceding claims, comprising at least 0.05 mol. % zirconia, or at least 0.10 mol. % zirconia, or at least 0.25 mol. % zirconia, or at least 0.50 mol. % zirconia, or at least 0.75 mol. % zirconia, or at least 1.0 mol. % zirconia, or at least 1.5 mol. % zirconia, or at least 2.0 mol. % zirconia, or at least 2.5 mol. % zirconia, or at least 3.0 mol. % zirconia, or at least 3.5 mol. % zirconia, or at least 4.0 mol. % zirconia, or at least 4.5 mol. % zirconia, or at least 5.0 mol. % zirconia, or at least 5.5 mol. % zirconia, or at least 6.0 mol. % zirconia, or at least 6.5 mol. % zirconia, or at least 7.0 mol. % zirconia, or at least 7.5 mol. % zirconia, or at least 8.0 mol. % zirconia, or at least 8.5 mol. % zirconia, or at least 9.0 mol. % zirconia, or at least 9.5 mol. % zirconia, or at least 10.0 mol. % zirconia.
  6. 6. The substantially single-phase polycrystalline material of any of the preceding claims, comprising not greater than 19.5 mol. % zirconia, or not greater than 19.0 mol. % zirconia, or not greater than 18.5 mol. % zirconia, or not greater than 18.0 mol. % zirconia, or not greater than 17.5 mol. % zirconia, or not greater than 17.0 mol. % zirconia, or not greater than 16.5 mol. % zirconia, or not greater than 16.0 mol. % zirconia, or not greater than 15.5 mol. % zirconia, or not greater than 15.0 mol. % zirconia, or not greater than 14.5 mol. % zirconia, or not greater than 14.0 mol. % zirconia, or not greater than 13.5 mol. % zirconia, or not greater than 13.0 mol. % zirconia, or not greater than 12.5 mol. % zirconia, or not greater than 12.0 mol. % zirconia, or not greater than 11.5 mol. % zirconia, or not greater than 11.0 mol. % zirconia, or not greater than 10.5 mol. % zirconia, or not greater than 10.0 mol. % zirconia.
  7. 7. The substantially single-phase polycrystalline material of any of the preceding claims, comprising at least 81 mol. % yttria, or at least 82 mol. % yttria, or at least 83 mol. % yttria, or at least 84 mol. % yttria, or at least 85 mol. % yttria, or at least 86 mol. % yttria, or at least 87 mol. % yttria, or at least 88 mol. % yttria, or at least 89 mol. % yttria, or at least 90 mol. % yttria, or at least 91 mol. % yttria, or at least 92 mol. % yttria, or at least 93 mol. % yttria, or at least 94 mol. % yttria, or at least 95 mol. % yttria, or at least 96 mol. % yttria, or at least 97 mol. % yttria, or at least 98 mol. % yttria, or at least 99 mol. % yttria, or at least 99.5 mol. % yttria, or at least 99.75 mol. % yttria.
  8. 8. The substantially single-phase polycrystalline material of any of the preceding claims, wherein the substantially single-phase polycrystalline material comprises at least 96 wt. % of a solidsolution of yttria-zirconia, or at least at least 97 wt. % of a solid-solution of yttria-zirconia, or at least 98 wt. % of a solid-solution of yttria-zirconia, or at least 98.2 wt. % of a solid-solution of yttria-zirconia, or at least 98.4 wt. % of a solid-solution of yttria-zirconia, or at least 98.6 wt. % of a solid-solution of yttria-zirconia, or at least 98.8 wt. % of a solid-solution of yttria-zirconia, or at least 99.0 wt. % of a solid-solution of yttria-zirconia, or at least 99.2 wt. % of a solid-solution of yttria-zirconia, or at least 99.4 wt. % of a solid-solution of yttria-zirconia, or at least 99.5 wt. % of a solid-solution of yttria-zirconia, or at least 99.6 wt. % of a solid-solution of yttria-zirconia, or at least 99.7 wt. % of a solid-solution of yttria-zirconia, or at least 99.8 wt. % of a solid-solution of yttria-zirconia, or at least 99.9 wt. % of a solid-solution of yttria-zirconia.
  9. 9. The substantially single-phase polycrystalline material of any of the preceding claims, wherein the substantially single-phase polycrystalline material realizes an average grain size of not greater than 7 micrometers, or not greater than 6 micrometers, or not greater than 5 micrometers, or not greater than 4 micrometers, or not greater than 3.5 micrometers, or not greater than 3 micrometers, or not greater than 2.5 micrometers, or not greater than 2 micrometers, or not greater than 1.5 micrometers, or not greater than 1 micrometers, or not greater than 0.75 micrometers, or not greater than 0.5 micrometers.
  10. 10. The substantially single-phase poly crystalline material of claim 9, wherein a standard deviation of the grain size is not greater than twice the average grain size, or not greater than 150% of the average grain size, or not greater than 100% of the average grain size, or not greater than 80% of the average grain size, or not greater than 60% of the average grain size, or not greater than 50% of the average grain size, or not greater than 40% of the average grain size, or not greater than 30% of the average grain size, or not greater than 20% of the average grain size.
  11. 11. The substantially single-phase polycrystalline material of claim 9, wherein the substantially single-phase polycrystalline material realizes a maximum grain size, and wherein the maximum grain size is not more than 20 times larger than the average grain size, or not more than 15 times larger than the average grain size, or not more than 12 times larger than the average grain size, or not more than 10 times larger than the average grain size, or not more than 8 times larger than the average grain size, or not more than 7 times larger than the average grain size, or not more than 6 times larger than the average grain size, or not more than 5 times larger than the average grain size, or not more than 4 times larger than the average grain size.
  12. 12. The substantially single-phase polycrystalline material of any of the preceding claims, wherein the substantially single-phase polycrystalline materials realizes at least equivalent plasma etch resistance as compared to a baseline material, wherein the baseline material is a single-phase polycrystalline material comprising 90 mol. % yttria and 10 mol. % zirconia and with less than 5 ppm of aluminum.
  13. 13. A method comprising: (a) pressing a powder into a shaped component, wherein the powder comprises (i) 0.01-20 mol. % zirconia, (ii) at least 80 mol. % yttria, and (iii) from 40 to 7000 ppm of aluminum; (b) sintering the shaped component at a sintering temperature of from 1200-1800°C, thereby forming a sintered component, wherein the sintered component is polycrystalline, wherein the sintered component is substantially single-phase realizing at least 95 wt. % of a solid-solution of yttria-zirconia as measured by x-ray diffraction, and wherein the sintered component realizes a density of at least 95% of theoretical.
  14. 14. The method of claim 13, wherein the sintering is pressureless sintering.
  15. 15. The method of claim 13, wherein the sintering comprises sintering in air.
  16. 16. The method of claim 13, wherein the sintering temperature is not greater than 1750°C, or not greater than 1700°C, or not greater than 1680°C, or not greater than 1660°C, or not greater than 1640°C, or not greater than 1620°C, or not greater than 1600°C.
  17. 17. The method of claim 13, comprising, prior to the pressing step, formulating the powder.
  18. 18. The method of claim 17, wherein the formulating step comprises blending a yttria powder and a zirconia powder, thereby producing a powder blend.
  19. 19. The method of claim 18, wherein the formulating step comprising contacting the powder blend with a liquid phase material comprising aluminum.
  20. 20. The method of claim 19, wherein the liquid phase material is an aqueous aluminum-containing solution.

Description

DOPED SUBSTANTIALLY SINGLE-PHASE RARE EARTH OXIDE-ZIRCONIA MATERIALS AND METHODS OF MAKING THE SAME CROSS-REFERENCE TO RELATED APPLICATION [001] This patent application claims priority to U.S. Provisional Patent Application No. 63/525,069, entitled, “DOPED SUBSTANTIALLY SINGLE-PHASE YTTRIA-ZIRCONIA MATERIALS AND METHODS OF MAKING THE SAME,” filed on July 5, 2023, which application is incorporated herein by reference in its entirety. BACKGROUND [002] Corrosion and erosion resistance are critical properties for apparatus components and liners used in semiconductor processing chambers, where corrosive environments are present. Examples of corrosive plasma environments include plasmas used for cleaning of processing apparatus and plasmas used to etch semiconductor substrates. Yttrium oxide ceramics may realize plasma resistance properties, but yttrium oxide generally exhibits weak mechanical properties that limits its applications for general use in semiconductor processing components. SUMMARY OF THE DISCLOSURE [003] Broadly, the present patent application relates to new substantially single-phase polycrystalline materials having improved properties. In one approach, the new substantially single-phase polycrystalline materials generally include: (A) one or more rare earth oxide (“REO”) materials and (B) zirconia (ZrO ). In one embodiment, the new materials may comprise a solid solution of REO-zirconia, wherein zirconium periodically substitutes for the REO material on the REO lattice. The new substantially single-phase polycrystalline materials generally include at least 80 mol. % of the one or more REO materials and from 0.01 to 20 mol. % zirconia. The new single-phase polycrystalline materials also generally include from 40 to 7000 ppm by weight of aluminum. In one embodiment, the one or more REO materials comprise one or more oxides of the Lanthanide series of elements. In one embodiment, the one or more REO materials at least include yttrium oxide (yttria). In another embodiment, the one or more REO materials at least include ytterbium oxide (ytterbia). In another embodiment, the one or more REO materials at least include both yttrium oxide and ytterbium oxide. Other combinations of REO materials may be used. In one embodiment, at least one rare earth sesquioxide having the formula RE2O3 (e.g., Y2O3, Yb2O3, Gd2O3, Er2O3, and Dy2O3, among others) is used as a REO material. For purposes of illustration, reference is now made to yttria-zirconia materials. It is to be appreciated that the yttria-zirconia disclosures herein generally apply to other REO-zirconia materials. [004] As noted above, the new substantially single-phase polycrystalline materials may comprise (or consist of, or consist essentially of) a solid solution of yttria-zirconia, wherein zirconium periodically substitutes for yttrium on the yttria cubic lattice. To facilitate the substantially single-phase solid solution, the new single-phase polycrystalline materials generally include from 0.01 to 20 mol. % zirconia and at least 80 mol. % yttria. The new single-phase polycrystalline materials also generally include from 40 to 7000 ppm by weight of aluminum. The new substantially single-phase polycrystalline materials may realize a high density, such as a density of at least 95% of theoretical density. The new substantially single-phase polycrystalline materials may realize a fine grain structure (e.g., an average grain size of not greater than 7 micrometers). The new substantially single-phase polycrystalline materials may realize a uniform grain structure (e.g., less than 10% of the grains are more than twice the average grain size). The new substantially single-phase polycrystalline materials may be resistant to erosion by halogen plasmas. The new substantially single-phase polycrystalline materials may be in the form of a monolithic (bulk) material, such as in the form of a shaped component. The shaped component may be suited for use, for instance, as a semiconductor component, including semiconductor components suited for use in a plasma processing chamber. Additional details are provided below. i. Substantially Single-Phase Material Compositions and Microstructures [005] As noted above, the new substantially single-phase polycrystalline materials may comprise (and may consist of, or consist essentially of) (i) a yttria-zirconia solid solution phase and (ii) from 40 to 7000 ppm of aluminum, which aluminum may also be present within the solid solution phase and/or may be present in another phase (e.g., the YAM phase (Y4AI2O9)). [006] As used herein, “substantially single-phase polycrystalline materials” means polycrystalline materials having at least 95 wt. % of a solid solution of yttria-zirconia (or REO- zirconia, if other REOs are used) as determined using x-ray diffraction (XRD). In other words, up to 5 wt. % of phases other than the yttria-zirconia solid solution phase may be present. These other phases may include, for instance, the YA