USH532H - Method of chemically polishing fused quartz - Google Patents
Method of chemically polishing fused quartz Download PDFInfo
- Publication number
- USH532H USH532H US06/920,626 US92062686A USH532H US H532 H USH532 H US H532H US 92062686 A US92062686 A US 92062686A US H532 H USH532 H US H532H
- Authority
- US
- United States
- Prior art keywords
- fused quartz
- high pressure
- etchant
- fused
- quartz
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000005350 fused silica glass Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims description 21
- 238000005498 polishing Methods 0.000 title claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract 2
- 238000001816 cooling Methods 0.000 claims abstract 2
- 238000009987 spinning Methods 0.000 claims abstract 2
- 238000005530 etching Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 230000035939 shock Effects 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 230000003746 surface roughness Effects 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 239000013078 crystal Substances 0.000 description 7
- 239000010453 quartz Substances 0.000 description 7
- 239000011521 glass Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- 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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
- C03C15/02—Surface treatment of glass, not in the form of fibres or filaments, by etching for making a smooth surface
Definitions
- This invention relates in general to a method of chemically polishing fused quartz and in particular, to such a method wherein the chemically polished fused quartz will be suitable for use in electrical components having low electric loss, high temperature stability, high heat shock resistance and low thermal expansion.
- Ser. No. 781,166 there is disclosed and claimed a method of chemically polishing quartz crystal blanks involving treating the quartz crystal blanks with an etching solution at high pressure in a high pressure vessel.
- the Ser. No. 781,166 method although desirable for treating a quartz crystal blank having piezoelectric properties and thus suitable for use in a crystal oscillator does not teach or suggest that the method could be usable for treating any other type of material such as for example, a fused quartz or glass type material that does not have piezoelectric properties.
- fused quartz or glass is not piezoelectric. It cannot be used in quartz crystal oscillators. It is not cut from a crystal and is not doubly rotated. Fused quartz has a random internal orientation.
- Fused quartz has potential for use in electrical components having low electric loss, high temperature stability and high heat shock resistance and low thermal expansion. In such application, it would be desirable to improve device fabrication by removing surface damage such as microcracks from the surface or the fused quartz and polishing the surface of the fused quartz.
- the general object of this invention is to provide a method of chemically polishing fused quartz.
- a more specific object of the invention is to provide such a method that enables one to remove surface damage such as microcracks from the surface of the fused quartz so that a good surface finish is obtained for device fabrication.
- the surface of a sample of fused quartz is first lapped about 3 microns, the piece of fused quartz that has been lapped then thoroughly cleaned, and then treated with an etchant having an HF concentration of 4.50 to 4.66 moles per liter obtained by blending a 40 percent NH ⁇ F solution with a 49 percent HF solution, at high pressures in a high pressure vessel while agitating to circulate the etchant solution, the vessel then cooled, the fused quartz removed and then thoroughly rinsed with water and then, spun dry.
- an etchant having an HF concentration of 4.50 to 4.66 moles per liter obtained by blending a 40 percent NH ⁇ F solution with a 49 percent HF solution, at high pressures in a high pressure vessel while agitating to circulate the etchant solution, the vessel then cooled, the fused quartz removed and then thoroughly rinsed with water and then, spun dry.
- the method of the invention requires that the fused quartz sample be thoroughly cleaned prior to pressure polishing.
- the high pressure vessel used in the invention must be inert to corrosive chemicals used to etch fused quartz.
- a vessel can conveniently be a teflon lined high pressure autoclave that has built in magnetic stirring.
- the stirring and agitation circulates the etchant and maintains a uniform temperature throughout the etching solution.
- the temperature can range from about 70 degrees C. to about 100 degrees C. with a temperature of 75 degrees C.preferred.
- the gas pressure can be supplied by nitrogen or an inert gas.
- the pressure can be from about 350 psi to about 1,050 psi.
- the pressure polishing can take about 11/2 hours up to about 5 hours.
- the time of pressure polishing is determined from the rate of etching of the particular etchant and the desired depth of etching.
- Fused quartz is a glass and is not piezoelectric, as opposed to crystalline quartz which is piezoelectric and has application in quartz crystal oscillators.
- the fused quartz samples to be chemically polished are lapped about 3 microns and then thoroughly cleaned before processing.
- the lapped fused quartz is then mounted inside a teflon-lined high pressure autoclave.
- the autoclave is then filled with a hydrofluoric acid based etchant having an HF concentration of 4.50-4.66 moles per liter obtained by blending a 40 percent NH ⁇ F solution with a 49 percent HF solution.
- the autoclave is then sealed tight using a teflon gasket and steel clamps.
- thermocouple A teflon-clad thermocouple is immersed in the etching solution through the cover, vacuum sealed, to measure temperature.
- the chamber is then filled with nitrogen to a pressure of about 350 p.s.i.
- the magnetic stirring is then turned on to circulate the etchant.
- the autoclave which sits within a heating mantle, is heated to 75 degrees C.
- the fused quartz samples are then soaked at about 75 degrees C. for about 11/2]hours while maintaining the pressure at about 350 psi to about 1,050 psi.
- the autoclave is then shut off and allowed to cool to 65 degrees C. in 20 minutes.
- the pressure is then released, the cover removed from the autoclave and the samples removed.
- the fused quartz is then thoroughly rinsed with water and spun dry. Fused quartz processed in this manner has a polished surface with a surface roughness of better than 0.09 micron.
- Evaporation of etchant is a problem with the conventional method which causes the etch rate of the etchant to constantly change.
- the method of this invention eliminates evaporation of the etchant.
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- ing And Chemical Polishing (AREA)
Abstract
Fused Quartz is chemically polished by lapping the fused quartz surface tobout 3 microns, thoroughly cleaning the lapped fused quartz, treating the lapped fused quartz with an etchant at high pressure in a high pressure vessel while agitating to circulate the etchant and maintaining a uniform temperature throughout the etchant, cooling the vessel, removing the fused quartz, rinsing thoroughly with water and spinning dry.
Description
The invention described herein may be manufactured, used, and licensed by or for the Government for governmental purposes, without the payment to me of any royalty thereon.
This invention relates in general to a method of chemically polishing fused quartz and in particular, to such a method wherein the chemically polished fused quartz will be suitable for use in electrical components having low electric loss, high temperature stability, high heat shock resistance and low thermal expansion.
The invention is copending with U.S. patent application Ser. No. 781,166 filed Sept. 30, 1985 by Ronald J. Brandmayr for "Method of Chemically Polishing Quartz Crystal Blanks" and assigned to a common assignee.
In Ser. No. 781,166, there is disclosed and claimed a method of chemically polishing quartz crystal blanks involving treating the quartz crystal blanks with an etching solution at high pressure in a high pressure vessel. The Ser. No. 781,166 method, although desirable for treating a quartz crystal blank having piezoelectric properties and thus suitable for use in a crystal oscillator does not teach or suggest that the method could be usable for treating any other type of material such as for example, a fused quartz or glass type material that does not have piezoelectric properties.
In this connection, fused quartz or glass is not piezoelectric. It cannot be used in quartz crystal oscillators. It is not cut from a crystal and is not doubly rotated. Fused quartz has a random internal orientation.
Fused quartz has potential for use in electrical components having low electric loss, high temperature stability and high heat shock resistance and low thermal expansion. In such application, it would be desirable to improve device fabrication by removing surface damage such as microcracks from the surface or the fused quartz and polishing the surface of the fused quartz.
The general object of this invention is to provide a method of chemically polishing fused quartz. A more specific object of the invention is to provide such a method that enables one to remove surface damage such as microcracks from the surface of the fused quartz so that a good surface finish is obtained for device fabrication.
It has now been found that the aforementioned objects can be attained by applying the general teaching of Ser. No. 781,166 to the processing of fused quartz. That is, the method of the invention enables one to remove surface damage such as microcracks from the surface of the fused quartz.
More particularly, according to this invention, the surface of a sample of fused quartz is first lapped about 3 microns, the piece of fused quartz that has been lapped then thoroughly cleaned, and then treated with an etchant having an HF concentration of 4.50 to 4.66 moles per liter obtained by blending a 40 percent NHμF solution with a 49 percent HF solution, at high pressures in a high pressure vessel while agitating to circulate the etchant solution, the vessel then cooled, the fused quartz removed and then thoroughly rinsed with water and then, spun dry.
The method of the invention requires that the fused quartz sample be thoroughly cleaned prior to pressure polishing.
The high pressure vessel used in the invention must be inert to corrosive chemicals used to etch fused quartz. Such a vessel can conveniently be a teflon lined high pressure autoclave that has built in magnetic stirring. The stirring and agitation circulates the etchant and maintains a uniform temperature throughout the etching solution. The temperature can range from about 70 degrees C. to about 100 degrees C. with a temperature of 75 degrees C.preferred.
The gas pressure can be supplied by nitrogen or an inert gas. The pressure can be from about 350 psi to about 1,050 psi.
The pressure polishing can take about 11/2 hours up to about 5 hours. The time of pressure polishing is determined from the rate of etching of the particular etchant and the desired depth of etching.
Fused quartz is a glass and is not piezoelectric, as opposed to crystalline quartz which is piezoelectric and has application in quartz crystal oscillators. The fused quartz samples to be chemically polished are lapped about 3 microns and then thoroughly cleaned before processing. The lapped fused quartz is then mounted inside a teflon-lined high pressure autoclave. The autoclave is then filled with a hydrofluoric acid based etchant having an HF concentration of 4.50-4.66 moles per liter obtained by blending a 40 percent NHμF solution with a 49 percent HF solution. The autoclave is then sealed tight using a teflon gasket and steel clamps. A teflon-clad thermocouple is immersed in the etching solution through the cover, vacuum sealed, to measure temperature. The chamber is then filled with nitrogen to a pressure of about 350 p.s.i. The magnetic stirring is then turned on to circulate the etchant. The autoclave, which sits within a heating mantle, is heated to 75 degrees C. The fused quartz samples are then soaked at about 75 degrees C. for about 11/2]hours while maintaining the pressure at about 350 psi to about 1,050 psi. The autoclave is then shut off and allowed to cool to 65 degrees C. in 20 minutes. The pressure is then released, the cover removed from the autoclave and the samples removed. The fused quartz is then thoroughly rinsed with water and spun dry. Fused quartz processed in this manner has a polished surface with a surface roughness of better than 0.09 micron.
Evaporation of etchant is a problem with the conventional method which causes the etch rate of the etchant to constantly change. The method of this invention eliminates evaporation of the etchant.
I wish it to be understood that I do not desire to be limited to the exact details as described, for obvious modifications will occur to a person skilled in the art.
Claims (8)
1. Method of chemically polishing a fused quartz surface so that the fused quartz will be suitable for use in electrical components having low electric loss, high temperature stability, high heat shock resistance and low thermal expansion, said method including the steps of:
(a) lapping the fused quartze surface about 3 microns,
(B) thoroughly cleaning the piece of fused quartz that has been lapped,
(C) treating the fused quartz with an etchant having an HF concentration of 4.50 to 4.66 moles per liter obtained by blending a 40 percent NHμF solution with a 49 percent HF solution at high pressure from about 350 psi to about 1,050 psi in a high pressure vessel while agitating to circulate the etchant and maintaining uniform temperature througout the etching solution just long enough to polish the surface of the fused quartz,
(D) cooling the vessel,
(E) removing the fused quartz the then thoroughly rinsing the fused quartz with water, and
(f) spinning dry.
2. Method according to claim 1 wherein the high pressure vessel is a teflon-lined high pressure autoclave.
3. Method according to claim 1 wherein the high pressure is provided by nitrogen gas.
4. Method according to claim 1 wherein the high pressure is provided by an inert gas.
5. Method according to claim 1 wherein the temperature is maintained at about 75 degrees C.
6. Method according to claim 1 wherein the etching time is from about 1.5 hours to as long as about 5 hours.
7. Method according to claim 2 wherein etchant is sealed in the chamber of the autoclave preventing evaportion of the etchane and maintaining a constant etch rate.
8. Method according to claim 1 wherein the fused quartz is chemically polished to a surface roughness of better than 0.09 micron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US06/920,626 USH532H (en) | 1986-10-20 | 1986-10-20 | Method of chemically polishing fused quartz |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US06/920,626 USH532H (en) | 1986-10-20 | 1986-10-20 | Method of chemically polishing fused quartz |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| USH532H true USH532H (en) | 1988-10-04 |
Family
ID=25444094
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US06/920,626 Abandoned USH532H (en) | 1986-10-20 | 1986-10-20 | Method of chemically polishing fused quartz |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | USH532H (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020078710A1 (en) * | 2000-12-27 | 2002-06-27 | Shin-Etsu Chemical Co., Ltd. | Silica glass substrates and their selection |
| US20040238487A1 (en) * | 2003-05-30 | 2004-12-02 | Kiehlbauch Mark W. | Methods of finishing quartz glass surfaces and components made by the methods |
| RU2680622C1 (en) * | 2017-12-18 | 2019-02-25 | Федеральное государственное бюджетное образовательное учреждение высшего образования - Российский химико-технологический университет имени Д.И. Менделеева (РХТУ им. Д.И. Менделеева) | Porous glass production method |
-
1986
- 1986-10-20 US US06/920,626 patent/USH532H/en not_active Abandoned
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020078710A1 (en) * | 2000-12-27 | 2002-06-27 | Shin-Etsu Chemical Co., Ltd. | Silica glass substrates and their selection |
| EP1219575A1 (en) * | 2000-12-27 | 2002-07-03 | Shin-Etsu Chemical Co., Ltd. | Silica glass substrates and their selection |
| US6928837B2 (en) | 2000-12-27 | 2005-08-16 | Shin-Etsu Chemical Co., Ltd. | Silica glass substrates and their selection |
| US20040238487A1 (en) * | 2003-05-30 | 2004-12-02 | Kiehlbauch Mark W. | Methods of finishing quartz glass surfaces and components made by the methods |
| US7250114B2 (en) * | 2003-05-30 | 2007-07-31 | Lam Research Corporation | Methods of finishing quartz glass surfaces and components made by the methods |
| US20080014754A1 (en) * | 2003-05-30 | 2008-01-17 | Lam Research Corporation | Methods of finishing quartz glass surfaces and components made by the methods |
| US7402258B2 (en) | 2003-05-30 | 2008-07-22 | Lam Research Corporation | Methods of removing metal contaminants from a component for a plasma processing apparatus |
| US8318035B2 (en) | 2003-05-30 | 2012-11-27 | Lam Research Corporation | Methods of finishing quartz glass surfaces and components made by the methods |
| RU2680622C1 (en) * | 2017-12-18 | 2019-02-25 | Федеральное государственное бюджетное образовательное учреждение высшего образования - Российский химико-технологический университет имени Д.И. Менделеева (РХТУ им. Д.И. Менделеева) | Porous glass production method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| STCF | Information on status: patent grant |
Free format text: PATENTED CASE |
|
| AS | Assignment |
Owner name: UNITED STATES OF AMERICA, THE, AS REPRESENTED BY T Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:BRANDMAYR, RONALD J.;REEL/FRAME:005036/0491 Effective date: 19861006 |