# US 2017/0283313 A1 · Fluoride glazes from fluorine ion treatment

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- Number: US 2017/0283313 A1
- Document ID: US20170283313A1
- Status: Published application
- Kind: A1
- Application number: 15/418,615
- Filed: 2017-01-27
- Published: 2017-10-05
- Earliest claimed: 2016-03-29
- Assignees: Applied Materials, Inc.
- Applicants: Applied Materials, Inc.
- Inventors: Chengtsin Lee; Jennifer Y. Sun
- Web page: https://patentgrep.com/patent/US20170283313A1

## CPC

- C03C 17/22: with other inorganic material (C03C17/34, C03C17/44 take precedence)
- C03C 4/18: for ion-sensitive glass
- C03C 8/06: containing halogen
- C03C 10/00: Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C 10/16: Halogen containing crystalline phase
- C03C 17/245: by deposition from the vapour phase
- C03C 21/007: {in gaseous phase}
- C03C 2204/00: Glasses, glazes or enamels with special properties
- C03C 2209/00: Compositions specially applicable for the manufacture of vitreous glazes
- C03C 2217/214: Al2O3
- C03C 2217/285: Fluorides
- C03C 2218/13: from melts
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS

## Abstract

An article comprises a body having a coating. The coating comprising a mixture of a first oxide and a second oxide. The coating includes a glaze on a surface of the coating, the glaze comprising a eutectic system having a super-lattice of a first fluoride and a second fluoride.

## Claims

### Claim 1

A method comprising:
forming an article or a coating comprising an initial mixture comprising a first oxide and a second oxide;
heating the article or coating to a treatment temperature of at least 910° C.;
exposing the article or coating to anhydrous hydrogen fluoride gas at the treatment temperature of at least 910° C., wherein exposure of the article or coating to the anhydrous hydrogen fluoride gas at the temperature of at least 910° C. causes:
replacement of oxygen molecules in the first oxide and the second oxide with fluorine molecules at a surface of the article or the coating;
transformation of the initial mixture comprising the first oxide and the second oxide into a final mixture comprising a first fluoride and a second fluoride at the surface of the article or the coating;
formation of a eutectic system from the final mixture, the eutectic system having a super-lattice of the first fluoride and the second fluoride at the surface of the article or the coating; and
formation of a glaze from the eutectic system at the surface of the article or the coating.

### Claim 2 (depends on 1)

The method of claim 1, wherein the glaze has a thickness of 0.5 to 200 microns.

### Claim 3 (depends on 1)

The method of claim 1, wherein the formation of the eutectic system from the final mixture comprises:
melting the first fluoride, wherein the first fluoride has a first melting temperature that is below the treatment temperature;
dissolving the second fluoride by the melted first fluoride, wherein the second fluoride has a second melting temperature that is above the treatment temperature; and
combining of the melted first fluoride and the dissolved second fluoride into the eutectic system, wherein the eutectic system has a third melting temperature that is below the first melting temperature.

### Claim 4 (depends on 1)

The method of claim 1, wherein the first oxide is ZrO2 and the second oxide is Y2O3.

### Claim 5 (depends on 1)

The method of claim 1, wherein the initial mixture comprises a ceramic compound comprising Y4Al2O9 and a solid-solution of Y2O3—ZrO2, and wherein the exposure of the article or the coating to the anhydrous hydrogen fluoride gas at the temperature of at least 910° C. further causes the Al to be removed from the ceramic compound at the surface of the article or the coating through formation and vaporization of AlF3.

### Claim 6 (depends on 5)

The method of claim 5, wherein the exposure of the article or coating to the anhydrous hydrogen fluoride gas at the temperature of at least 910° C. further causes vaporization of at least one of trace transition metals or aluminum from the surface of the article or the coating.

### Claim 7 (depends on 5)

The method of claim 5, wherein the first oxide and the second oxide are selected from a group consisting of Y2O3, Nd2O3, La2O3, Er2O3, Sc2O3, TiO2, ZrO2, HfO2, Al2O3 and SiO2.

### Claim 8 (depends on 5)

The method of claim 5, wherein the article comprises a sintered ceramic article.

### Claim 9 (depends on 5)

The method of claim 5, further comprising:
forming the coating on an object by performing one of dip coating, doctor blade coating, thermal spray coating, plasma spray coating, ion assisted deposition, or physical vapor deposition.

### Claim 10 (depends on 1)

The method of claim 1, wherein the 50-100% of a thickness of the coating is converted to the glaze.

### Claim 11 (depends on 1)

The method of claim 1, wherein the initial mixture comprises the first oxide, the second oxide and a third oxide, the final mixture comprises the first fluoride and the second fluoride and a third fluoride at the surface of the article or the coating, and the eutectic system has a super-lattice of the first fluoride, the second fluoride and the third fluoride at the surface of the article or the coating.

### Claim 12

An article comprising:
a body;
a coating on the body, the coating comprising a mixture of a first oxide of a first metal and a second oxide of a second metal; and
a glaze on a surface of the coating, the glaze comprising a eutectic system having a super-lattice of a first fluoride of the first metal and a second fluoride of the second metal.

### Claim 13 (depends on 10)

The article of claim 10, wherein the coating has a first thickness of approximately 1 to 200 microns and the glaze has a second thickness that is 50% to 100% of the first thickness.

### Claim 14 (depends on 10)

The article of claim 10, wherein:
the first metal and the second metal are selected from a group consisting of Nd, La, Er, Sc, Ti, Zr, Hf, Al, Si and Y;
the first oxide and the second oxide are selected from a group consisting of Nd2O3, La2O3, Er2O3, Sc2O3, TiO2, ZrO2, HfO2, Al2O3 and SiO2, and Y2O3; and
the first fluoride and the second fluoride are selected from a group consisting of NdF3, LaF3, ErF3, ScF3, TiF3, ZrF4, HfF4, AlF3, SiF4 and YF3.

### Claim 15 (depends on 10)

The article of claim 10, wherein the article comprises a sintered ceramic article.

### Claim 16

A method comprising:
heating an article or coating comprising an oxide to a treatment temperature of 350° C. to 1000° C.;
exposing the article or coating to anhydrous hydrogen fluoride gas at the treatment temperature, wherein exposure of the article or coating to the anhydrous hydrogen fluoride gas at the treatment temperature causes a reaction that replaces oxygen molecules in the oxide with fluorine molecules at a surface of the article or the coating to transform the oxide into a fluoride or into an oxy-fluoride; and
cooling the article or coating.

### Claim 17 (depends on 16)

The method of claim 16, wherein the oxide is Al2O3 and the fluoride is AlF4.

### Claim 18 (depends on 16)

The method of claim 16, wherein the oxide is Al2O3 and the oxy-fluoride is aluminum oxy-fluoride.

### Claim 19 (depends on 16)

The method of claim 16, wherein the oxide is selected from a group consisting of Y2O3, ZrO2, Nd2O3, La2O3, Er2O3, Sc2O3, TiO2, HfO2, and SiO2.

### Claim 20 (depends on 16)

The method of claim 16, wherein the reaction penetrates into the surface of the article or coating to a depth of about 0.5-40 microns.