Feedstock gel and method of making glass-ceramic articles from the feedstock gel

Patent metadata

Field	Value
Publication number	US-10399886-B2
Application number	US-201715650490-A
Country	US
Kind code	B2
Filing date	Jul 14, 2017
Priority date	Jul 14, 2017
Publication date	Sep 3, 2019
Grant date	Sep 3, 2019

Abstract

A method of making a glass-ceramic article includes synthesizing a feedstock gel that includes a base oxide network comprising Na 2 O, CaO, and SiO 2 , in which a molar ratio of Na 2 O:CaO:SiO 2 in the gel is 1:2:3, and then converting the feedstock gel into a glass-ceramic article such as a container or a partially-formed container. The conversion of the feedstock gel into a glass-ceramic container may be performed at a temperature that does not exceed 900° C. and may include the steps of pressing the feedstock gel into a compressed solid green-body, sintering the green-body into a solid monolithic body of a glass-ceramic material, deforming the solid monolithic glass-ceramic body into a glass-ceramic preform, and cooling the preform. A glass-ceramic article having a glass-ceramic material that has a molar ratio of Na 2 O:CaO:SiO 2 that is 1:2:3 is also disclosed.

First claim

The invention claimed is:

1. A method of making a glass-ceramic article, the method comprising:
synthesizing a feedstock gel that includes a base oxide network comprising Na 2 O, CaO, and SiO 2 in which a molar ratio of Na 2 O:CaO:SiO 2 is 1:2:3;
pressing the feedstock gel into a compressed solid green-body;
sintering the compressed solid green-body of the feedstock gel at a temperature below 900° C. to produce a solid monolithic body of a glass-ceramic material having an amorphous residual glass phase and a crystalline phase distributed within the amorphous residual glass phase, the solid monolithic body of a glass-ceramic material having a density that is greater than a density of the feedstock gel;
deforming the solid monolithic body of a glass-ceramic material into a glass-ceramic preform having a container shape at a temperature of 600° C. or above; and
cooling the glass-ceramic preform into a hollow glass-ceramic article that retains the container shape.

2. The method set forth in claim 1 , wherein the step of synthesizing the feedstock gel comprises:
providing an aqueous solution that includes sodium silicate having a Na 2 O:SiO 2 molar ratio;
adding a soluble calcium salt to the aqueous solution to form a precipitate having a Na 2 O:CaO:SiO 2 molar ratio that corresponds to the molar ratio of Na 2 O:CaO:SiO 2 in the base oxide network of the feedstock gel; and
extracting liquid solvent from the precipitate to produce the feedstock gel.

3. The method set forth in claim 2 , wherein the calcium salt comprises at least one of calcium nitrate or calcium chloride.

4. The method set forth in claim 1 , wherein the step of synthesizing the feedstock gel comprises:
providing an aqueous solution that includes an acid catalyst;
adding a tetraalkoxysilane to the aqueous solution to form a polysiloxane through hydrolytic polycondensation of the tetraalkoxysilane;
adding a soluble sodium salt and a soluble calcium salt to the aqueous solution to introduce sodium and calcium, respectively, into the polysiloxane;
forming a precipitate that has a Na 2 O:CaO:SiO 2 molar ratio that corresponds to the molar ratio of Na 2 O:CaO:SiO 2 in the base oxide network of the feedstock gel; and
extracting liquid solvent from the precipitate to produce the feedstock gel.

5. The method set forth in claim 4 , wherein the tetraalkoxysilane is tetraethyl orthosilicate, tetramethyl orthosilicate, or a mixture thereof.

6. The method set forth in claim 4 , wherein the acid catalyst is nitric acid, acetic acid, or hydrochloric acid.

7. The method set forth in claim 4 , wherein the sodium salt comprises at least one of sodium hydroxide, sodium nitrate, or sodium chloride, and wherein the calcium salt comprises at least one of calcium nitrate or calcium chloride.

8. The method set forth in claim 1 , wherein the step of sintering the feedstock gel into the solid monolithic body of a glass-ceramic material is performed at a temperature of 600° C. to 900° C.

9. The method set forth in claim 1 , wherein the step of deforming the solid monolithic body of a glass-ceramic material into the glass-ceramic preform is performed at a temperature between 600° C. and 750° C.

10. The method set forth in claim 9 , wherein the step of deforming the solid monolithic body of a glass-ceramic material into the glass-ceramic preform comprises hot-pressing the monolithic body of a glass-ceramic material in a mold cavity.

11. The method set forth in claim 1 , wherein the glass-ceramic article is a container that comprises a hollow main body that defines an opening and an internal containment space accessible through the opening.

12. The method set forth in claim 1 , wherein the glass-ceramic article is a glass-ceramic parison, and further comprising:
blowing the glass-ceramic parison to expand the parison into a glass-ceramic container comprised of a hollow main body that has a bottom wall, an upstanding side wall extending from a periphery of the bottom wall, and a neck portion extending from the side wall opposite the bottom wall and defining an opening to an internal containment space defined by the hollow main body.

13. A method of making a glass-ceramic article, the method comprising:
synthesizing a feedstock gel from a liquid precursor medium that includes a reactive silicon-containing precursor compound, the feedstock gel including a base oxide network comprising Na 2 O, CaO, and SiO 2 in which a molar ratio of Na 2 O:CaO:SiO 2 is 1:2:3;
pressing the feedstock gel into a compressed solid green-body;
sintering the compressed solid green-body of the feedstock gel at a temperature below 900° C. to produce a solid monolithic body of a glass-ceramic material having an amorphous residual glass phase and a crystalline phase distributed within the amorphous residual glass phase;
deforming the solid monolithic body of a glass-ceramic material into a glass-ceramic preform having a container shape at a temperature of 600° C. or above; and
cooling the glass-ceramic preform into a glass-ceramic container comprised of a hollow main body that has a bottom wall, an upstanding side wall extending from a periphery of the bottom wall, and a neck portion extending from the side wall opposite the bottom wall and defining an opening to an internal containment space defined by the hollow main body.

14. The method set forth in claim 13 , wherein the liquid precursor medium is selected from an aqueous silicate solution that includes sodium silicate or an acidic aqueous solution that includes an alkoxysilane.

15. The method set forth in claim 13 , wherein deforming the solid monolithic body of a glass-ceramic material comprises hot-pressing the solid monolithic body of a glass-ceramic material in a mold cavity at a temperature between 600° C. to 750° C. to form the glass-ceramic preform having a container shape.

16. A method of making a glass-ceramic article, the method comprising:
synthesizing a feedstock gel that includes a base oxide network comprising Na 2 O, CaO, and SiO 2 in which a molar ratio of Na 2 O:CaO:SiO 2 is 1:2:3, wherein synthesizing the feedstock gel comprises;
providing a liquid precursor medium that includes a reactive silicon-containing precursor compound selected from sodium silicate or a polysiloxane;
adding at least one soluble salt to the liquid precursor medium selected from a soluble sodium salt, a soluble calcium salt, or both a soluble sodium salt and a soluble calcium salt, wherein adding the at least one soluble salt causes a precipitate to form that includes Na 2 O, CaO, and SiO 2 in which a molar ratio of Na 2 O:CaO:SiO 2 in the precipitate is 1:2:3; and
extracting liquid solvent from the precipitate to produce the feedstock gel;

pressing the feedstock gel into a compressed solid green-body;
sintering the compressed solid green-body of the feedstock gel at a temperature below 900° C. to produce a solid monolithic body of a glass-ceramic material having an amorphous residual glass phase and a crystalline phase distributed within the amorphous residual glass phase;
deforming the solid monolithic body of a glass-ceramic material into a glass-ceramic preform having a container shape at a temperature of 600° C. or above; and
cooling the glass-ceramic preform into a glass-ceramic article in the form of a container or a parison.

17. The method set forth in claim 16 , wherein deforming the solid monolithic body of a glass-ceramic material comprises hot-pressing the solid monolithic body of a glass-ceramic material in a mold cavity at a temperature between 600° C. and 750° C. to form the

Assignees

• Owens Brockway Glass Container

Inventors

• Cooper Scott P

Classifications

• C03C3/087

  containing calcium oxide, e.g. common sheet or container glass · CPC title

• C03C1/006

  to produce glass through wet route · CPC title

• C04B2235/656

  characterised by specific heating conditions during heat treatment · CPC title

• C03B19/063

  by hot-pressing powders · CPC title

• C04B35/62204

  using waste materials or refuse (clay-wares containing waste materials C04B33/132) · CPC title