CN105717137B - Method for detecting micro-defects of quartz glass - Google Patents
Method for detecting micro-defects of quartz glass Download PDFInfo
- Publication number
- CN105717137B CN105717137B CN201610055734.9A CN201610055734A CN105717137B CN 105717137 B CN105717137 B CN 105717137B CN 201610055734 A CN201610055734 A CN 201610055734A CN 105717137 B CN105717137 B CN 105717137B
- Authority
- CN
- China
- Prior art keywords
- quartz glass
- glass sample
- defects
- sample
- acid solution
- 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.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/95—Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
- G01N21/958—Inspecting transparent materials or objects, e.g. windscreens
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Materials By The Use Of Optical Means Adapted For Particular Applications (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a method for detecting micro-defects of quartz glass, which comprises the following steps: precisely polishing two light-passing surfaces of a quartz glass sample; corroding the polished quartz glass sample by using an acid solution; taking out the quartz glass sample after 0.5-2 hours of corrosion, cleaning the quartz glass sample by using deionized water, and observing and detecting the quartz glass sample by using a microscope; the etching and observation were repeated for the quartz glass sample in the above procedure until defects in the quartz glass sample were observed or until no defects were observed until 20 to 30 μm remained in the thickness of the quartz glass sample. The method of the invention can detect micro-defects in quartz glass.
Description
Technical Field
The invention relates to the technical field of glass defect detection, in particular to a method for detecting micro defects of quartz glass.
Background
Quartz glass has excellent physical and chemical properties, is known as 'king of glass' by experts in the field of new materials, is an irreplaceable basic raw material in the development of national strategic industry and pillar industry, and is widely applied to high and new technical fields such as optical communication, microelectronics, photoelectrons, aerospace, nuclear technology, laser, precise optics, electric light sources and the like. The quartz pendulous piece of the quartz flexible accelerometer is particularly, the thickness of the quartz pendulous piece is usually less than 1mm, if the quartz glass substrate for preparing the quartz pendulous piece has the defects of the micro bubbles and the like, the stability, the consistency, the strength and the like of the quartz pendulous piece flexible beam can be seriously influenced, and further the high precision and the high reliability of the accelerometer are influenced.
At present, there are various methods for detecting defects such as bubbles in glass: the detection method mainly depends on the experience judgment of people, the visual size is limited, and more importantly, defects such as bubbles distributed in different layers are difficult to detect, so the detection method has low reliability and large size of detected bubbles, and only some rough detection and judgment are usually carried out. In the prior art, a light source is arranged on the side surface of glass to be detected, light of the light source is transmitted into the glass to be detected from a positive perspective angle of the side surface of the glass to be detected, then a visual inspection method is adopted or a computer linear scanning head is adopted to scan the light of the light source transmitted into the glass to be detected, whether the defects such as foreign matters, bubbles, nickel sulfide and the like exist in the glass to be detected is detected according to the factors such as whether the light transmitted into the glass to be detected is blocked or the transmission direction is changed, the size of the bubbles detected by the method is relatively large, and the detection method is only suitable for common glass. For the quartz glass used for precise devices such as quartz pendulous reeds for quartz flexible accelerometers, the principle of optical amplification is mainly adopted, such as optical microscope, optical magnifier and the like are used for detection, light is transmitted or reflected to the surface of a quartz sample, the outline of micro-defects such as micro-bubbles and the like is amplified, and the size and the quantity of the micro-defects are detected, but the detection omission phenomenon often occurs due to the distribution irregularity, depth and position inconsistency of the micro-defects such as the micro-bubbles and the like in the quartz glass, more importantly, the defects such as the micro-bubbles with the size of 0.01mm or less cannot be detected, so that the quality of the raw material of the quartz glass cannot be effectively controlled, the quartz glass enters the production of the subsequent processing procedures of products such as the quartz pendulous reeds and the like, the production cost is.
Disclosure of Invention
In view of the above, embodiments of the present invention provide a method for detecting micro defects in quartz glass, and mainly provide a method for detecting micro defects in quartz glass.
In order to achieve the purpose, the invention mainly provides the following technical scheme:
on one hand, the embodiment of the invention provides a method for detecting the microdefect of quartz glass, which comprises the following steps:
precisely polishing two light-passing surfaces of a quartz glass sample;
corroding the polished quartz glass sample by using an acid solution;
taking out the quartz glass sample after 0.5-2 hours of corrosion, cleaning the quartz glass sample by using deionized water, and observing and detecting the quartz glass sample by using a microscope;
the etching and observation were repeated for the quartz glass sample in the above procedure until defects in the quartz glass sample were observed or until no defects were observed until 20 to 30 μm remained in the thickness of the quartz glass sample.
Preferably, the initial thickness of the quartz glass sample is 1 to 20 mm.
Preferably, the acid solution for etching is a mixed acid solution of hydrofluoric acid and acetic acid.
Preferably, the mixed acid solution consists of high-grade pure hydrofluoric acid (HF is more than or equal to 40%) and analytically pure acetic acid (more than or equal to 99.5%) according to a volume ratio of 1: 3-3: 1.
Preferably, the acid solution temperature is 25 ℃ to 100 ℃.
Preferably, the temperature of the acid solution is controlled by a water bath or an oil bath.
Preferably, the precision polishing step of the two light-passing surfaces of the quartz glass sample is as follows: grinding the two light-passing surfaces of the cut quartz glass sample on a double-sided grinding machine or a single-axis grinding machine by using carborundum with the granularity of W40, W20, W10 and W5 in sequence, and precisely polishing the two light-passing surfaces of the quartz glass on a double-sided polishing machine or a single-axis polishing machine by using cerium oxide polishing powder, wherein the surface smoothness is grade 5.
Preferably, the defect is at least one of a bubble and an impurity.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for detecting the micro-defects of the quartz glass, provided by the embodiment of the invention, the quartz glass sample is corroded by the acid solution and then subjected to defect observation, after the acid corrosion, the defects such as micro-bubbles in the quartz glass sample are corroded and amplified, and are completely exposed and shown under the observation of a microscope, so that the accurate detection of the defects such as the micro-bubbles in the quartz glass substrate is realized. The method can accurately detect the defects of microbubbles with the size less than 0.01mm and the like in the quartz glass, solves the problem that the microbubbles with the size less than 0.01mm cannot be detected in the prior art, provides an accurate detection method for material selection in the use process of the quartz glass, ensures the safety, reliability and the like of the quartz glass material in the high and new technology field, and has wide application prospect.
Drawings
FIG. 1 is a photomicrograph of a sample of quartz glass directly examined by conventional optical magnification;
FIG. 2 is a micrograph of the quartz glass sample of FIG. 1 examined by the method of the invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The method for detecting the micro-defects of the quartz glass comprises the following steps:
precisely polishing two light-passing surfaces of a quartz glass sample;
corroding the polished quartz glass sample by using an acid solution;
taking out the quartz glass sample after 0.5-2 hours of corrosion, cleaning the quartz glass sample by using deionized water, and observing and detecting the quartz glass sample by using a microscope;
the etching and observation were repeated for the quartz glass sample in the above procedure until defects in the quartz glass sample were observed or until no defects were observed until 20 to 30 μm remained in the thickness of the quartz glass sample.
According to the method for detecting the micro-defects of the quartz glass, provided by the embodiment of the invention, the quartz glass sample is corroded by using an acid solution, and then defect observation is carried out. Therefore, the defects such as micro-bubbles and the like in the quartz glass sample are amplified through acid corrosion and are completely exposed and displayed under the observation of a microscope, and the accurate detection of the defects such as the micro-bubbles and the like in the quartz glass substrate is realized. The method can accurately detect the defects of micro bubbles with the size less than 0.01mm and the like in the quartz glass.
As a preference of the above embodiment, the initial thickness of the quartz glass sample is 1 to 20 mm. In the embodiment, the thickness of the quartz glass sample can reflect the defect condition of the quartz glass as truly as possible, and the defect missing detection or the detection time too long due to the overlarge thickness can be avoided to the maximum extent.
In any of the above embodiments, the acid solution for etching is preferably a mixed acid solution of hydrofluoric acid and acetic acid. The mixed acid liquid can be used for amplifying the original defects in the quartz glass without interfering the observation result. The mixed acid solution is generally prepared by mixing superior pure hydrofluoric acid (HF is more than or equal to 40%) and analytically pure acetic acid (more than or equal to 99.5%). The volume ratio of the superior pure hydrofluoric acid (HF is more than or equal to 40%) to the analytically pure acetic acid (more than or equal to 99.5%) is 1: 3-3: 1. The mixed acid solution prepared according to the embodiment has a proper corrosion rate, fully amplifies the original defects and does not influence the observation result.
In any of the above embodiments, the acid solution temperature is preferably 25 to 100 ℃. By controlling the acid solution within the range, sufficient corrosion rate and corrosion effect can be ensured, and further guarantee is provided for the accuracy of the observation result. The temperature of the acid solution is controlled by a water bath or oil bath. The water bath or oil bath allows for better control of the temperature of the acid solution.
Preferably, in any of the above embodiments, the step of precisely polishing the two light-passing surfaces of the quartz glass sample comprises: grinding the two light-passing surfaces of the cut quartz glass sample on a double-sided grinding machine or a single-axis grinding machine by using carborundum with the granularity of W40, W20, W10 and W5 in sequence, and precisely polishing the two light-passing surfaces of the quartz glass on a double-sided polishing machine or a single-axis polishing machine by using cerium oxide polishing powder, wherein the surface smoothness is grade 5.
FIG. 1 is a photomicrograph of a sample of quartz glass directly examined by conventional optical magnification; FIG. 2 is a photomicrograph of the quartz glass specimen of FIG. 1 examined by the method of the invention (observed under optical magnification after etching). Wherein, the acid solution for corroding the quartz glass sample is prepared by mixing superior pure hydrofluoric acid (HF is more than or equal to 40 percent) and analytically pure acetic acid (more than or equal to 99.5 percent) according to the weight ratio of 9: 4, placing the mixed acid solution in a constant-temperature water bath, heating to 40 ℃, continuously keeping the temperature constant, and vertically placing the polished quartz glass sample in the mixed acid solution for corrosion; after 1 hour of corrosion, the quartz glass sample is cleaned by deionized water, and the condition of the surface of the quartz glass is detected by using an optical amplification method of a microscope. Fig. 2 is the result observed after 2 times of etching. As can be seen from FIG. 1, defects such as bubbles of any size were not detected in the silica glass substrate by the conventional optical amplification method. As can be seen from fig. 2, the detection method of the present invention detects that a large number of microbubbles exist in the quartz glass substrate, and the microbubbles are all exposed and revealed under the observation of a microscope after being corroded and amplified by the mixed acid solution, i.e., the method of the present invention realizes the accurate detection of the defects such as the microbubbles in the quartz glass substrate. The figure shows the defect as microbubbles. Of course, impurities which are not easily detected by conventional methods can also be detected by the method of the present invention. In the same principle as the bubble, when a quartz glass sample is etched, the etching direction and rate at the impurity are different, and therefore, the defect at the position is amplified, and then the amplified defect can be directly observed through a microscope. For the quartz glass prepared in the same batch, key performance indexes such as microbubbles and the like are consistent, so that the detection result can represent related parameters of the microbubbles in the quartz glass of the batch by randomly extracting 1 to 3 quartz glass of the same batch and detecting the quartz glass by the method. In addition, according to the principle of the method of the present invention for etching and enlarging defects, any suitable etching solution may be used without being limited to the mixed acid solution of the above-described embodiment.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (3)
1. The method for detecting the micro-defects of the quartz glass is characterized by comprising the following steps of:
precisely polishing two light-passing surfaces of a quartz glass sample;
vertically placing the polished quartz glass sample in a mixed acid solution for corrosion;
taking out the quartz glass sample after 0.5-2 hours of corrosion, cleaning the quartz glass sample by using deionized water, and observing and detecting the quartz glass sample by using a microscope;
the etching and observation were repeated for the silica glass sample in accordance with the above procedure until defects in the silica glass sample were observed or no defects were observed until 20 to 30 μm of the thickness of the silica glass sample remained,
the mixed acid solution is composed of superior pure hydrofluoric acid and analytically pure acetic acid according to the volume ratio of 1: 3-3: 1, the temperature of the mixed acid solution is 25-100 ℃, and the temperature of the mixed acid solution is controlled by a water bath or an oil bath;
the defects are bubbles with the size smaller than 0.01 mm;
randomly selecting 1-3 quartz glass sheets in the same batch for detection, and then representing the related parameters of the microbubbles in the quartz glass in the batch.
2. The method for detecting the microdefects of the quartz glass according to claim 1, wherein the initial thickness of the quartz glass sample is 1-20 mm.
3. The method for detecting the micro-defects of the quartz glass according to claim 1, wherein the steps of precisely polishing the two light-passing surfaces of the quartz glass sample are as follows: grinding the two light-passing surfaces of the cut quartz glass sample on a double-sided grinding machine or a single-axis grinding machine by using carborundum with the granularity of W40, W20, W10 and W5 in sequence, and precisely polishing the two light-passing surfaces of the quartz glass on a double-sided polishing machine or a single-axis polishing machine by using cerium oxide polishing powder, wherein the surface smoothness is grade 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610055734.9A CN105717137B (en) | 2016-01-27 | 2016-01-27 | Method for detecting micro-defects of quartz glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610055734.9A CN105717137B (en) | 2016-01-27 | 2016-01-27 | Method for detecting micro-defects of quartz glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105717137A CN105717137A (en) | 2016-06-29 |
| CN105717137B true CN105717137B (en) | 2020-08-11 |
Family
ID=56154186
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610055734.9A Active CN105717137B (en) | 2016-01-27 | 2016-01-27 | Method for detecting micro-defects of quartz glass |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105717137B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106546469B (en) * | 2016-10-31 | 2019-03-12 | 东旭科技集团有限公司 | A kind of preparation method of the electron microscopic sample of plate glass |
| CN106959206B (en) * | 2017-03-21 | 2019-12-13 | 中国人民解放军国防科学技术大学 | Fused quartz element zero probability damage threshold prediction method based on photo-thermal weak absorption |
| CN107063112B (en) * | 2017-03-30 | 2019-01-01 | 中国航空工业集团公司西安飞行自动控制研究所 | A kind of glass orifice surface defect layer depth measurement method |
| CN109191440A (en) * | 2018-08-24 | 2019-01-11 | 上海应用技术大学 | Glass blister detection and method of counting |
| CN111257347B (en) * | 2018-11-30 | 2023-04-07 | 汕尾比亚迪实业有限公司 | Glass product detection method |
| CN112692650A (en) * | 2020-12-23 | 2021-04-23 | 华中光电技术研究所（中国船舶重工集团公司第七一七研究所） | Processing method of optical spherical surface |
| CN113237726A (en) * | 2021-05-18 | 2021-08-10 | 青岛泰睿思微电子有限公司 | Method for observing semiconductor device unsealing sample |
| CN114136516A (en) * | 2021-11-18 | 2022-03-04 | 华中光电技术研究所（中国船舶重工集团公司第七一七研究所） | Method for testing intrinsic stress of quartz glass |
| CN115372090B (en) * | 2022-07-29 | 2024-06-21 | 中国船舶重工集团公司第七0七研究所 | Manufacturing and detecting method for quartz glass subsurface damage depth sample |
| CN117589109B (en) * | 2024-01-19 | 2024-03-29 | 上海强华实业股份有限公司 | Quality detection and control method for quartz center tray manufacturing process |
| CN117705827B (en) * | 2024-02-06 | 2024-04-12 | 上海强华实业股份有限公司 | Method for optimizing quartz glass defect detection based on multivariable fine burning energy consumption |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003194736A (en) * | 2001-12-26 | 2003-07-09 | Univ Nihon | Detecting method for defect of glass |
| CN101558292B (en) * | 2006-12-14 | 2013-08-28 | 日本电气硝子株式会社 | Glass sheet defect detection device, glass sheet manufacturing method, glass sheet, glass sheet quality judging device, and glass sheet inspection method |
| CN100579723C (en) * | 2008-03-21 | 2010-01-13 | 中国科学院上海光学精密机械研究所 | Laser glass mechanical chemical polishing method |
| CN103698339B (en) * | 2013-12-29 | 2015-12-09 | 云南北方驰宏光电有限公司 | A kind of crystal dislocation corrosion detection method |
| CN104390983A (en) * | 2014-12-09 | 2015-03-04 | 南京中锗科技股份有限公司 | Corrosion detection method for COP defects in dislocation-free germanium single crystal |
| CN104900758B (en) * | 2015-05-25 | 2017-03-15 | 连云港市产品质量监督检验中心 | A kind of detection method of quasi-monocrystalline silicon microdefect |
-
2016
- 2016-01-27 CN CN201610055734.9A patent/CN105717137B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105717137A (en) | 2016-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105717137B (en) | Method for detecting micro-defects of quartz glass | |
| TWI749406B (en) | Glasses and glass ceramics including a metal oxide concentration gradient | |
| TWI679183B (en) | Strengthened glass with deep depth of compression | |
| JP6657173B2 (en) | Tempered glass with deep compression depth | |
| Esmaeilzare et al. | Investigation of subsurface damages and surface roughness in grinding process of Zerodur® glass–ceramic | |
| JP5751390B1 (en) | Chemically tempered glass | |
| KR101298236B1 (en) | Method for improving the specification of reinforcement by edge eching before reinforcing glass | |
| WO2016117476A1 (en) | Chemically strengthened glass and production method for same | |
| JP7056652B2 (en) | Chemically tempered glass | |
| CN107037059A (en) | A kind of detection method of optical material sub-surface crack depth | |
| Kang et al. | The deterioration characteristics and mechanism of polishing pads in chemical mechanical polishing of fused silica | |
| CN112020764B (en) | Method for evaluating semiconductor wafer and method for manufacturing semiconductor wafer | |
| CN111855782A (en) | Real-time measuring system for pH value of sapphire grinding fluid and preparation method thereof | |
| EP1968102B1 (en) | Method of evaluation of bonded wafer | |
| CN212364173U (en) | Real-time measuring system for pH value of sapphire grinding fluid | |
| Jones | Latent milling marks on glass | |
| CN117985940A (en) | Method for treating glass with defects | |
| Wang et al. | 3D topography of the micro cracks of subsurface damages by etching process | |
| CN115343301A (en) | Characterization method for subsurface damage depth of non-metallic material | |
| Goodman | Characterisation of Damage on the Fractured Edges of Float Glass | |
| Qin et al. | Subsurface Damage Detection and Quantitative Prediction of Thin-Walled Complex Curved-Surface Component | |
| Wang et al. | Measuring Subsurface Damage of the Ground Sample by Roughness along the Bevel | |
| Pramod et al. | Effect of Crystallographic Orientation on Ductile to Brittle Transition Using Nano-Scribing Method | |
| JP2011133397A (en) | Surface analysis pretreatment method of specific minute defect present in glass |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |