CN114136516A - Method for testing intrinsic stress of quartz glass - Google Patents
Method for testing intrinsic stress of quartz glass Download PDFInfo
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- CN114136516A CN114136516A CN202111372186.XA CN202111372186A CN114136516A CN 114136516 A CN114136516 A CN 114136516A CN 202111372186 A CN202111372186 A CN 202111372186A CN 114136516 A CN114136516 A CN 114136516A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000012360 testing method Methods 0.000 title claims abstract description 49
- 230000035882 stress Effects 0.000 claims abstract description 96
- 238000000137 annealing Methods 0.000 claims abstract description 32
- 230000008646 thermal stress Effects 0.000 claims abstract description 29
- 238000005498 polishing Methods 0.000 claims abstract description 17
- 230000007797 corrosion Effects 0.000 claims abstract description 11
- 238000005260 corrosion Methods 0.000 claims abstract description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 18
- 238000010583 slow cooling Methods 0.000 claims description 11
- 238000010998 test method Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 3
- 238000009662 stress testing Methods 0.000 claims description 2
- 230000002950 deficient Effects 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 230000003746 surface roughness Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 235000012149 noodles Nutrition 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000005304 optical glass Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 101001053395 Arabidopsis thaliana Acid beta-fructofuranosidase 4, vacuolar Proteins 0.000 description 1
- 229910003641 H2SiO3 Inorganic materials 0.000 description 1
- 229910004014 SiF4 Inorganic materials 0.000 description 1
- 229910004074 SiF6 Inorganic materials 0.000 description 1
- 229910020439 SiO2+4HF Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
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-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/24—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
- B24B7/20—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
- B24B7/22—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
- B24B7/24—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain for grinding or polishing glass
- B24B7/242—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain for grinding or polishing glass for plate glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses a method for testing intrinsic stress of quartz glass, which comprises the following steps: providing a quartz glass sample, and carrying out surface fine grinding and polishing on the quartz glass; carrying out surface corrosion on the quartz glass subjected to surface finish grinding and polishing to remove mechanical stress; the quartz glass subjected to surface corrosion and mechanical stress removal is subjected to annealing process to eliminate thermal stress; the intrinsic stress test was performed on the quartz glass, the thermal stress of which was removed by the annealing process, by using a birefringence stress meter. According to the invention, the surface of the quartz glass is finely ground and polished, then the surface is corroded to remove mechanical stress, and the annealing process is adopted to eliminate thermal stress, so that the test operation is simple, the interference of the mechanical stress and the thermal stress can be effectively eliminated, the intrinsic stress of the quartz glass can be accurately measured, the quartz glass blank with excellent performance can be screened out, the quartz glass blank with poor performance can be eliminated, the quality is improved in the early stage of engineering application, the defective rate of subsequent part processing is reduced, and the cost is saved.
Description
Technical Field
The invention relates to the technical field of material testing, in particular to a method for testing intrinsic stress of quartz glass.
Background
The composition of the quartz glass stress includes mechanical stress, thermal stress and intrinsic stress. The mechanical stress is mainly surface stress caused by applying mechanical processing method on quartz glass, and the stress can be eliminated or reduced by a certain chemical corrosion method. The thermal stress is mainly due to the stress of the quartz glass caused by the temperature gradient, which can be eliminated or reduced by the heat treatment process. However, intrinsic stress is a self-stress characteristic of quartz glass and cannot be changed and removed.
At present, the stress test method of quartz glass mainly uses a stress meter to test, and then the stress magnitude and distribution of quartz glass are evaluated through the test result. Obviously, although the method can test the stress of the obtained quartz glass, the mechanical stress and the thermal stress cannot be eliminated, and the intrinsic stress of the quartz glass cannot be obtained.
The method for testing the intrinsic stress of the quartz glass, which is simple in testing operation, can effectively eliminate the interference of mechanical stress and thermal stress and accurately measure the intrinsic stress of the quartz glass, is one of the technical problems to be solved by the technical staff in the field.
Therefore, aiming at the problems in the prior art, the designer of the scheme actively researches and improves by virtue of years of experience in the industry, and then the invention provides a method for testing the intrinsic stress of the quartz glass.
Disclosure of Invention
The invention aims to provide a method for testing intrinsic stress of quartz glass, aiming at the defects that in the prior art, although the stress of the quartz glass can be obtained through the traditional quartz glass stress test, the mechanical stress and the thermal stress cannot be eliminated, the intrinsic stress of the quartz glass cannot be obtained and the like.
In order to achieve the object of the present invention, the present invention provides a method for testing intrinsic stress of quartz glass, comprising:
step S1 is executed: providing a quartz glass sample, and carrying out surface fine grinding and polishing on the quartz glass;
step S2 is executed: carrying out surface corrosion on the quartz glass subjected to surface finish grinding and polishing to remove mechanical stress;
step S3 is executed: the quartz glass subjected to surface corrosion and mechanical stress removal is subjected to annealing process to eliminate thermal stress;
step S4 is executed: the intrinsic stress test was performed on the quartz glass, the thermal stress of which was removed by the annealing process, by using a birefringence stress meter.
Optionally, the provided quartz glass sample is divided equally, and the steps S1 to S4 are performed on the equally divided quartz glass sample, and then the stress test result of the equally divided quartz glass is compared with the stress test result of the original sample to verify the feasibility of the test method.
Optionally, the quartz glass after surface finish polishing is subjected to surface etching to remove mechanical stress by using hydrofluoric acid solution.
Optionally, the hydrofluoric acid solution contains 10% to 35% by mass of hydrofluoric acid.
Optionally, an annealing process is used to relieve the thermal stress of the quartz glass.
Optionally, the annealing process further includes:
step S31 is executed: heating the quartz glass from room temperature to a first temperature TnThe temperature rise time is T1The first temperature TnLess than the annealing point temperature of the quartz glass material and greater than the strain point temperature of the quartz glass material;
step S32 is executed: at a first temperature TnThen, the quartz glass is subjected to heat preservation for a time period T2-T1；
Step S33 is executed: subjecting the quartz glass to heat preservation from a first temperature TnSlowly cooling to a second temperature TmSaid second temperature TmLess than the strain point temperature of the quartz glass material and has a slow cooling time T3-T2；
Step S34 is executed: for slow cooling to the second temperature TmThe quartz glass is quickly cooled to room temperature, and the quick cooling time is T4-T3。
Optionally, the temperature and time parameters of the annealing process are set according to the material characteristics of the quartz glass.
Optionally, the first temperature TnThe temperature rise rate was 5 ℃/min at 1050 ℃.
Optionally, the quartz glass is subjected to heat preservation for a time period T2-T1＝10h。
Optionally, the second temperature TmThe slow cooling rate is 1 ℃/min at 750 ℃.
In conclusion, the method for testing the intrinsic stress of the quartz glass has the advantages that the surface of the quartz glass is finely ground and polished, then the surface is corroded to remove the mechanical stress, and the annealing process is adopted to eliminate the thermal stress, so that the testing operation is simple, the interference of the mechanical stress and the thermal stress can be effectively eliminated, the intrinsic stress of the quartz glass can be accurately tested, the quartz glass blank with excellent performance can be screened out, the quartz glass blank with poor performance can be eliminated, the early stage of engineering application is good, the defective rate of subsequent part processing is reduced, and the cost is saved.
Drawings
FIG. 1 is a flow chart showing the method of intrinsic stress testing of quartz glass according to the present invention;
FIG. 2 is a temperature profile of an annealing process for relieving thermal stress of quartz glass according to the present invention.
Detailed Description
The invention will be described in detail with reference to the following embodiments and drawings for illustrating the technical content, structural features, and achieved objects and effects of the invention.
Referring to FIG. 1, FIG. 1 is a flow chart illustrating a method for testing intrinsic stress of quartz glass according to the present invention. The method for testing the intrinsic stress of the quartz glass comprises the following steps:
step S1 is executed: providing a quartz glass sample, and carrying out surface fine grinding and polishing on the quartz glass;
step S2 is executed: carrying out surface corrosion on the quartz glass subjected to surface finish grinding and polishing to remove mechanical stress;
step S3 is executed: the quartz glass subjected to surface corrosion and mechanical stress removal is subjected to annealing process to eliminate thermal stress;
step S4 is executed: the intrinsic stress test was performed on the quartz glass, the thermal stress of which was removed by the annealing process, by using a birefringence stress meter.
In order to further verify the feasibility of the test method of the intrinsic stress of the quartz glass, the provided quartz glass sample is uniformly divided, and the step S1-step S4 are executed on the uniformly divided quartz glass sample; and then comparing the stress test result of the equaled quartz glass with the stress test result of the original sample to verify the feasibility of the test method.
Referring to fig. 2 in conjunction with fig. 1, fig. 2 is a temperature diagram of an annealing process for removing thermal stress of quartz glass by using an annealing process according to the present invention.
In step S2 of the present invention, the surface of the quartz glass that has been subjected to surface finish grinding and polishing is subjected to surface etching to remove mechanical stress using a hydrofluoric acid solution.
More specifically, the hydrofluoric acid solution contains 10-35% of hydrofluoric acid by mass. Step S3 is to remove thermal stress of the quartz glass by an annealing process, the annealing process further comprising:
step S31 is executed: heating the quartz glass from room temperature to a first temperature TnThe temperature rise time is T1The first temperature TnLess than the annealing point temperature of the quartz glass material and greater than the strain point temperature of the quartz glass material;
step S32 is executed: at a first temperature TnThen, the quartz glass is subjected to heat preservation for a time period T2-T1；
Step S33 is executed: subjecting the quartz glass to heat preservation from a first temperature TnSlowly cooling to a second temperature TmSaid second temperature TmLess than the strain point temperature of the quartz glass material and has a slow cooling time T3-T2；
Step S34 is executed: for slow cooling to the second temperature TmThe quartz glass is quickly cooled to room temperature, and the quick cooling time is T4-T3。
As a person skilled in the art will readily understand, the temperature and time parameters of the annealing process are set according to the material characteristics of the quartz glass to effectively eliminate thermal stress. Wherein the holding temperature (first temperature T) in the annealing processn) And holding time (T)2-T1) Is the key to eliminate the thermal stress; slow cooling is the key to avoid the generation of new thermal stresses.
In order to more intuitively disclose the technical scheme of the invention and to highlight the beneficial effects of the invention, the method for testing the intrinsic stress of the quartz glass and the working principle thereof are now described with reference to the specific embodiments. In the specific embodiment, the temperature, time, temperature rise value of the annealing process, and the quartz glass material is quartz 7979 material, etc. are only examples, and should not be construed as limiting the technical solution of the present invention.
In the invention, a stress birefringence test method is selected as a stress test method, and a birefringence stress meter is selected as test equipment. When the silica glass is subjected to a stress, whether this stress is an external force or an internal force, the isotropic characteristic of the optical glass is changed, and the change is not generally uniformly changed. Because of different anisotropies, when a light beam passes through, the light beam can generate a stress birefringence phenomenon, the propagation speeds of two light paths after birefringence are different, the refractive index and the refraction angle are also different, and the material anisotropy caused by stress can cause the two light beams to generate optical path difference through quartz glass. The stress birefringence test method is to evaluate the stress according to the optical path difference.
In a specific embodiment, the method for testing intrinsic stress of quartz glass comprises the following steps:
step S1 is executed: providing a quartz glass sample, and carrying out surface fine grinding and polishing on the quartz glass;
easily know, when quartz glass's surface roughness is relatively poor, the light beam shines quartz glass's surface and can take place serious diffuse reflection effect, enters birefringence test light path formation stray light that disturbs the test through multiple diffuse reflection, and quartz glass's surface roughness is worse, and stray light's interference is stronger. The surface roughness of the optical glass can be improved by grinding and polishing the surface of the quartz glass, the interference of stray light on stress test is reduced, and the accuracy of the stress test is improved. In the present invention, the process parameters of the quartz glass surface treatment are shown in table 1.
Step S2 is executed: carrying out surface corrosion on the quartz glass subjected to surface finish grinding and polishing to remove mechanical stress;
more specifically, in order to eliminate the influence of machining stress, a hydrofluoric acid solution with the mass percent content of 10% -35% is adopted to corrode the surface of the quartz glass, and a machining damage layer is removed. Chemical reaction equation of SiO2+4HF＝SiF4+2H2O，4SiF4+2HF+3H2O＝3H2SiF6+H2SiO3. The hydrofluoric acid solution can uniformly corrode the surface of the quartz glass, and the surface roughness of the quartz glass is not obviously changed.
TABLE 1 Quartz glass surface treatment
| Serial number | Abrasive/polishing powder | Processed noodles | Amount of removal | Surface requirements |
| 1 | W10 carborundum | 1 side | 0.05mm | Even sand surface |
| 2 | W10 carborundum | 2 noodles | 0.05mm | Even sand surface |
| 3 | 200# polishing powder | 1 side | 0.01mm | Superficial defect B ═ VI |
| 4 | 200# polishing powder | 2 noodles | 0.01mm | Superficial defect B ═ VI |
Step S3 is executed: the quartz glass subjected to surface corrosion and mechanical stress removal is subjected to annealing process to eliminate thermal stress; the annealing process further comprises:
step S31 is executed: heating the quartz glass from room temperature to a first temperature T at a speed of 5 ℃/minn1050 deg.C, heating time is T1The first temperature TnLess than the annealing point temperature of the quartz glass material and greater than the strain point temperature of the quartz glass material;
step S32 is executed: at a first temperature TnKeeping the temperature of the quartz glass at 1050 ℃, wherein the keeping temperature duration is T2-T1＝10h；
Step S33 is executed: subjecting the quartz glass to heat preservation from a first temperature TnSlowly cooling to a second temperature T at 1050 deg.C/minm750 ℃, the second temperature TmLess than the strain point temperature of the quartz glass material and has a slow cooling time ofT3-T2；
Step S34 is executed: for slow cooling to the second temperature TmThe quartz glass is quickly cooled to room temperature, and the quick cooling time is T4-T3。
Step S4 is executed: the intrinsic stress test was performed on the quartz glass, the thermal stress of which was removed by the annealing process, by using a birefringence stress meter.
In order to further verify the feasibility of the test method of the intrinsic stress of the quartz glass, the provided quartz glass sample is uniformly divided, and the step S1-step S4 are executed on the uniformly divided quartz glass sample; and then comparing the stress test result of the equaled quartz glass with the stress test result of the original sample to verify the feasibility of the test method.
In conclusion, the method for testing the intrinsic stress of the quartz glass has the advantages that the surface of the quartz glass is finely ground and polished, then the surface is corroded to remove the mechanical stress, and the annealing process is adopted to eliminate the thermal stress, so that the testing operation is simple, the interference of the mechanical stress and the thermal stress can be effectively eliminated, the intrinsic stress of the quartz glass can be accurately tested, the quartz glass blank with excellent performance can be screened out, the quartz glass blank with poor performance can be eliminated, the early stage of engineering application is good, the defective rate of subsequent part processing is reduced, and the cost is saved.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (10)
1. A method for testing intrinsic stress of quartz glass is characterized by comprising the following steps:
step S1 is executed: providing a quartz glass sample, and carrying out surface fine grinding and polishing on the quartz glass;
step S2 is executed: carrying out surface corrosion on the quartz glass subjected to surface finish grinding and polishing to remove mechanical stress;
step S3 is executed: the quartz glass subjected to surface corrosion and mechanical stress removal is subjected to annealing process to eliminate thermal stress;
step S4 is executed: the intrinsic stress test was performed on the quartz glass, the thermal stress of which was removed by the annealing process, by using a birefringence stress meter.
2. The method for testing intrinsic stress of silica glass according to claim 1, wherein the provided silica glass sample is first equally divided, and the steps S1 to S4 are performed on the equally divided silica glass sample, and then the stress test result of the equally divided silica glass is compared with the stress test result of the original sample to verify the feasibility of the test method.
3. The method for testing the intrinsic stress of the quartz glass according to claim 1, wherein the quartz glass surface-polished by the surface finish polishing is subjected to surface etching to remove the mechanical stress by using a hydrofluoric acid solution.
4. The method for testing the intrinsic stress of the quartz glass according to claim 3, wherein the hydrofluoric acid solution contains 10 to 35 mass% of hydrofluoric acid.
5. The method for testing intrinsic stress of quartz glass according to claim 1, wherein the thermal stress of the quartz glass is removed by an annealing process.
6. The method for intrinsic stress testing of quartz glass according to claim 5, wherein the annealing process further comprises:
step S31 is executed: heating the quartz glass from room temperature to a first temperature TnThe temperature rise time is T1The first temperature TnLess than the annealing point temperature of the quartz glass material and greater than the strain point temperature of the quartz glass material;
step S32 is executed: at a first temperature TnLower, toThe quartz glass is subjected to heat preservation, and the heat preservation time length is T2-T1；
Step S33 is executed: subjecting the quartz glass to heat preservation from a first temperature TnSlowly cooling to a second temperature TmSaid second temperature TmLess than the strain point temperature of the quartz glass material and has a slow cooling time T3-T2；
Step S34 is executed: for slow cooling to the second temperature TmThe quartz glass is quickly cooled to room temperature, and the quick cooling time is T4-T3。
7. The method for testing the intrinsic stress of the quartz glass according to claim 6, wherein the temperature and time parameters of the annealing process are set according to the material properties of the quartz glass.
8. The method for testing the intrinsic stress of quartz glass according to claim 6, wherein the first temperature T is set tonThe temperature rise rate was 5 ℃/min at 1050 ℃.
9. The method for testing the intrinsic stress of the quartz glass according to claim 6, wherein the quartz glass is kept warm for a time T2-T1＝10h。
10. The method for testing the intrinsic stress of quartz glass according to claim 6, wherein the second temperature T is set tomThe slow cooling rate is 1 ℃/min at 750 ℃.
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| CN202111372186.XA CN114136516A (en) | 2021-11-18 | 2021-11-18 | Method for testing intrinsic stress of quartz glass |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201598229U (en) * | 2009-11-24 | 2010-10-06 | 北京金格兰石英玻璃有限公司 | High-efficient annealing equipment for quartz glass products |
| CN101913759A (en) * | 2010-08-26 | 2010-12-15 | 湖州东科电子石英有限公司 | Process for relieving stress of quartz glass |
| CN105717137A (en) * | 2016-01-27 | 2016-06-29 | 中国建筑材料科学研究总院 | Silica-glass micro-defect detecting method |
| CN113125242A (en) * | 2021-05-11 | 2021-07-16 | 郜梓宇 | Stress detector for quartz glass product and detection method |
-
2021
- 2021-11-18 CN CN202111372186.XA patent/CN114136516A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201598229U (en) * | 2009-11-24 | 2010-10-06 | 北京金格兰石英玻璃有限公司 | High-efficient annealing equipment for quartz glass products |
| CN101913759A (en) * | 2010-08-26 | 2010-12-15 | 湖州东科电子石英有限公司 | Process for relieving stress of quartz glass |
| CN105717137A (en) * | 2016-01-27 | 2016-06-29 | 中国建筑材料科学研究总院 | Silica-glass micro-defect detecting method |
| CN113125242A (en) * | 2021-05-11 | 2021-07-16 | 郜梓宇 | Stress detector for quartz glass product and detection method |
Non-Patent Citations (1)
| Title |
|---|
| 孔敏等: "高性能石英玻璃精密退火工艺研究", 《武汉理工大学学报》, vol. 32, no. 22, pages 17 - 1 * |
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