# US 11,299,417 B2 · Preparation of a quartz glass body in a melting crucible of refractory metal

> Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt

- Number: US 11,299,417 B2
- Document ID: US11299417B2
- Status: Granted
- Kind: B2
- Application number: 16/062,658
- Filed: 2016-12-16
- Published: 2019-03-07
- Granted: 2022-04-12
- Earliest claimed: 2015-12-18
- Assignees: Heraeus Quarzglas GmbH & Co. KG
- Applicants: Heraeus Quarzglas GmbH & Co. KG
- Inventors: Matthias Otter; Walter Lehmann; Michael Hünermann; Nils Christian Nielsen; Nigel Robert Whippey; Boris Gromann; Abdoul-Gafar Kpebane
- Web page: https://patentgrep.com/patent/US11299417B2

## CPC

- C03B 37/01211: {by inserting one or more rods or tubes into a tube}
- C03B 5/06: in pot furnaces {(C03B5/02 takes precedence)}
- C03B 17/04: Forming tubes or rods by drawing from stationary or rotating tools or from forming nozzles
- C03B 20/00: Processes specially adapted for the production of quartz or fused silica articles {, not otherwise provided for (C03B19/01, C03B19/066, C03B19/106, C03B19/12, C03B19/14, C03B37/00 take precedence)}
- C03C 3/06: with more than 90% silica by weight, e.g. quartz {(C03C3/045 takes precedence)}
- C03B 2201/04: Hydroxyl ion (OH)
- C03B 2201/07: Impurity concentration specified
- C03B 2201/23: doped with hydroxyl groups
- C03B 2207/42: Assembly details; Material or dimensions of burner; Manifolds or supports
- C03C 2201/02: Pure silica glass, e.g. pure fused quartz
- C03C 2203/10: Melting processes
- G01N 21/412: {Index profiling of optical fibres}
- Y02P 40/57: Improving the yield, e-g- reduction of reject rates
- C03B: MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- 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
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

The invention relates to a process for preparing a quartz glass body comprising the process steps i.) Providing a silicon dioxide granulate, ii.) Making a glass melt from the silicon dioxide granulate in a melting crucible, and iii.) Making a quartz glass body from at least a part of the glass melt, wherein the melting crucible is comprised in an oven and is made of at least one material comprising tungsten or molybdenum or a combination thereof. The invention further relates to a quartz glass body which can be obtained by this process. Further, the invention relates to a light guide, an illuminant and a formed body, each of which can be obtained by processing the quartz glass body further.

## Claims

### Claim 1

A process for preparing a quartz glass body comprising pyrogenic silicon dioxide, comprising:
providing a silicon dioxide granulate comprising:
providing a pyrogenic silicon dioxide powder; and
processing the silicon dioxide powder to give a silicon dioxide granulate,
wherein the silicon dioxide granulate has a larger particle diameter than the silicon dioxide powder;
making a glass melt from the silicon dioxide granulate in a melting crucible; and
making a quartz glass body from at least a part of the glass melt;
wherein the melting crucible is comprised in an oven,
wherein the melting crucible is made of at least one material comprising tungsten or molybdenum or a combination thereof, and
wherein the quartz glass body comprises:
an OH content of less than 500 ppm;
a chlorine content of less than 60 ppm;
a tungsten content of less than 1000 ppb;
a molybdenum content of less than 1000 ppb;
wherein the ppb and ppm are based on the total weight of the quartz glass body in each case.

### Claim 2 (depends on 1)

The process according to claim 1, wherein the oven has at least one gas inlet and one gas outlet, wherein a gas which is removed through the gas outlet has a dew point of less than 0° C. on exiting the oven through the gas outlet.

### Claim 3 (depends on 1)

The process according to claim 1, wherein the melting crucible does not have a coating selected from a material comprising rhenium, iridium, osmium or a combination thereof on the surface facing the glass melt.

### Claim 4 (depends on 1)

The process according to claim 1, wherein the quartz glass body comprises at least one of:
an aluminium content of less than 200 ppb;
an ODC content of less than 5·1015/cm3;
a metal content of metals which are different from aluminium of less than 1 ppm;
a viscosity (p=1013 hPa) in a range from log10 (η (1250° C.)/dPas)=11.4 to log10 (η (1250° C.)/dPas)=12.9, or log10 (η (1300° C.)/dPas)=11.1 to log10 (1300° C.)/dPas)=12.2, or log10 (η (1350° C.)/dPas)=10.5 to log10 (η (1350° C.)/dPas)=11.5;
a standard deviation of the OH content of not more than 10%, based on the OH content of the quartz glass body;
a standard deviation of the Cl content of not more than 10%, based on the Cl content of the quartz glass body;
a standard deviation of the Al content of not more than 10%, based on the Al content of the quartz glass body;
a refractive index homogeneity of less than 1*10−4; and
a cylindrical form,
wherein the ppb and ppm are based on the total weight of the quartz glass body in each case.

### Claim 5 (depends on 1)

The process according to claim 1, wherein the silicon dioxide powder comprises at least one of:
a BET surface area in a range from 20 to 60 m2/g;
a bulk density in a range from 0.01 to 0.3 g/cm3;
a carbon content of less than 50 ppm;
a chlorine content of less than 200 ppm;
an aluminium content of less than 200 ppb;
a total content of metals which are different from aluminium of less than 5 ppm;
at least 70 wt.-% of the powder particles have a primary particle size in a range from 10 to 100 nm;
a tamped density in a range from 0.001 to 0.3 g/cm3;
a residual moisture content of less than 5 wt.-%;
a particle size distribution D10 in a range from 1 to 7 μm;
a particle size distribution D50 in a range from 6 to 15 μm; and
a particle size distribution D90 in a range from 10 to 40 μm;
wherein the wt.-%, ppm and ppb are based on the total weight of the silicon dioxide powder in each case.

### Claim 6 (depends on 1)

The process according to claim 1, wherein the silicon dioxide powder is prepared from a compound selected from the group consisting of siloxanes, silicon alkoxides and silicon halides.

### Claim 7 (depends on 1)

The process according to claim 1, further comprising making a hollow body with at least one opening from the quartz glass body.

### Claim 8 (depends on 7)

A process for preparing a light guide, comprising:
providing
a hollow body with at least one opening obtained by a process according to claim 7;
introducing one or more core rods into the quartz glass body through the at least one opening to obtain a precursor; and
drawing the precursor from in the warm to obtain a light guide with one or more cores and a jacket.

### Claim 9 (depends on 7)

A process for preparing a light guide, comprising:
providing
a hollow body obtained by a process according to claim 7;
optionally fitting the hollow body with electrodes; and
filling the hollow body with a gas.

### Claim 10 (depends on 7)

A process for preparing a formed body comprising:
providing a quartz glass body according to claim 7; and
forming a formed body from the quartz glass body.
