CN105717137A - Silica-glass micro-defect detecting method - Google Patents
Silica-glass micro-defect detecting method Download PDFInfo
- Publication number
- CN105717137A CN105717137A CN201610055734.9A CN201610055734A CN105717137A CN 105717137 A CN105717137 A CN 105717137A CN 201610055734 A CN201610055734 A CN 201610055734A CN 105717137 A CN105717137 A CN 105717137A
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- Prior art keywords
- quartz glass
- detection method
- silica
- samples
- acid solution
- Prior art date
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Classifications
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- 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
Abstract
The invention discloses a silica-glass micro-defect detecting method. The method includes the following steps that two light transmitting faces of a silica-glass sample are accurately polished; the polished silica-glass sample is corroded with an acid solution; after being corroded for 0.5-2 hours, the silica-glass sample is taken out and cleaned with deionized water, and the silica-glass sample is observed and detected with a microscope; according to the steps, the silica-glass sample is repeatedly corroded and observed till defects in the silica-glass sample are observed, or till defects are still not observed when the residual thickness of the silica-glass sample is 20-30 microns. By means of the silica-glass micro-defect detecting method, the micro-defects in silica glass can be detected.
Description
Technical field
The present invention relates to glass defect detection technical field, particularly relate to a kind of quartz glass microdefect detection side
Method.
Background technology
Quartz glass has superior physicochemical property, is described as " king of glass " by field of new expert, is state
Irreplaceable basic raw material in family's strategic industry and mainstay industry development, is widely used in light and leads to
The high-new skills such as news, microelectronics, photoelectron, Aero-Space, nuclear technology, laser, precision optics and electric light source
Art field.Owing to quartz glass preparation process cannot avoid the generation of the defects such as bubble, particularly microbubble (little
In 0.01mm) generation, and the defects such as bubble to the optical homogeneity of quartz glass, spectral characteristic, anti-swash
The performances such as light injury threshold and the stability of quartz glass product, reliability etc. all can cause extreme influence,
The especially quartz pendulous reed of quartz flexible accelerometer, the thickness of quartz pendulous reed is typically smaller than 1mm, if system
There is the defects such as microbubble in the quartz glass substrate of standby quartz pendulous reed, quartz pendulous reed flexible beam can be had a strong impact on
Stability, the performance such as concordance and intensity, and then affect high accuracy and the high reliability of accelerometer.
Detection method currently for defects such as Bubbles in Glass has multiple: is usually taken and is irradiated by area source
Glass, the method for front visual inspection, this detection method relies primarily on the micro-judgment of people, visual chi
Very little the most limited, it is often more important that the defect such as bubble for different layered distribution is difficult to check, therefore this detection
Method reliability is low, detection bubble size is relatively big, the most only does some rough detection and judgements.Existing skill
Also having a kind of side that light source is arranged on glass to be checked in art, source light is from the positive shadow-mark of glass sides to be checked
Angle carries out transmission and enters glass to be checked, then uses the method for visual inspection or use the linear probe of computer to sweep
Retouch transmission and enter the source light in glass to be checked, whether be blocked according to the light being transmitted in glass to be checked or
Change the key elements such as transmission direction, detect in glass to be checked, whether to there is the defects such as foreign body, bubble, nickel sulfide,
The bubble size of this method detection is the most relatively large, and this detection method is only applicable to simple glass.And it is right
For the accurate device quartz glasss such as quartz flexible accelerometer quartz pendulous reed, main employing optics is put
Big principle, as utilized optical microscope, optical loupes etc. to detect, utilizes light transmission or reflection to arrive
Quartz specimen surface, amplifies microdefect profiles such as microbubbles, detects its size and quantity, but due to stone
The erratic behavior of the microdefect such as microbubble distribution in English glass, the depth and position are inconsistent, missing inspection often occur
Phenomenon, it is often more important that the defect such as 0.01mm and following microbubble thereof cannot be detected, make quartz glass former
The quality of material can not get effectively controlling, and enters the production of the goods manufacturing procedures such as follow-up quartz pendulous reed, causes
Production cost is wasted, and even makes the quality of items such as quartz pendulous reed can not get effectively and controls.
Summary of the invention
In view of this, the embodiment of the present invention provides a kind of quartz glass microdefect detection method, and main purpose is
There is provided a kind of and detect the method for microdefect in quartz glass.
For reaching above-mentioned purpose, present invention generally provides following technical scheme:
On the one hand, a kind of quartz glass microdefect detection method is embodiments provided, including walking as follows
Rapid:
Quartz glass samples two is led to bright finish and carries out precise polished；
The most polished quartz glass samples acid solution is corroded；
Quartz glass samples is corroded taking-up in 0.5～2 hour and cleans up with deionized water, utilizes microscope to see
Examine detection quartz glass samples；
By above-mentioned steps, quartz glass samples is repeated corrosion and observation, until observing in quartz glass samples
Defect or to quartz glass samples thickness remain 20-30 μm do not observe defect yet.
As preferably, the original depth of described quartz glass samples is 1-20mm.
As preferably, described corrosion acid solution is the mixed acid solution of Fluohydric acid. and acetic acid.
As preferably, described mixed acid solution by the pure Fluohydric acid. of top grade (HF >=40%) and analytical pure acetic acid (>=
99.5%) the volume ratio composition of 1:3～3:1 is pressed.
As preferably, acid solution temperature is 25 DEG C～100 DEG C.
As preferably, the temperature of described acid solution is controlled by water-bath or oil bath.
As preferably, described quartz glass samples two leads to bright finish, and to carry out precise polished step as follows: by well cutting
Quartz glass samples, on twin grinder or single shaft grinder, successively use granularity be W40, W20,
The corundum of W10 and W5 grinds quartz glass samples two and leads to bright finish, then at Twp-sided polishing machine or single shaft buffing machine
On, use the precise polished quartz glass of cerium rouge two to lead to bright finish, surface smoothness is 5 grades.
As preferably, described defect is at least one in bubble and impurity.
Compared with prior art, the beneficial effects of the present invention is:
The quartz glass microdefect detection method that the embodiment of the present invention provides is rotten with acid solution by quartz glass samples
Then erosion carries out Observation of Defects, and after acid corrosion, present in quartz glass samples, the defect such as microbubble is rotten
Erosion is amplified, and all exposes under microscopic visualization and displays, it is achieved that microbubble in quartz glass substrate
Accurate detection etc. defect.The inventive method can accurately detect and be smaller in size than below 0.01mm in quartz glass
The defect such as microbubble, solve prior art and cannot detect the problem of the following microbubble of size 0.01mm,
The selection using process for quartz glass provides one detection method accurately, it is ensured that high-technology field
By the safety of silica glass material and reliability etc., have a extensive future.
Accompanying drawing explanation
Fig. 1 is that quartz glass samples is directly by the microphotograph of traditional optical amplifying method detection；
Fig. 2 is the microphotograph of quartz glass samples the inventive method detection of Fig. 1.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, but not as the limit to the present invention
Fixed.In the following description, what different " embodiments " or " embodiment " referred to is not necessarily same enforcement
Example.Additionally, special characteristic, structure or feature in one or more embodiment can be by any suitable form groups
Close.
Quartz glass microdefect detection method, comprises the steps:
Quartz glass samples two is led to bright finish and carries out precise polished；
The most polished quartz glass samples acid solution is corroded；
Quartz glass samples is corroded taking-up in 0.5～2 hour and cleans up with deionized water, utilizes microscope to see
Examine detection quartz glass samples；
By above-mentioned steps, quartz glass samples is repeated corrosion and observation, until observing in quartz glass samples
Defect or to quartz glass samples thickness remain 20-30 μm do not observe defect yet.
The quartz glass microdefect detection method of the embodiment of the present invention is first rotten with acid solution by quartz glass samples
Erosion, then carries out Observation of Defects.So present in quartz glass samples the defect such as microbubble through acid corrosion
Amplify, all expose under microscopic visualization and display, it is achieved that microbubble etc. in quartz glass substrate
The accurate detection of defect.The inventive method can accurately detect and be smaller in size than below 0.01mm's in quartz glass
The defects such as microbubble.
Preferred as above-described embodiment, the original depth of quartz glass samples is 1-20mm.In the present embodiment
The thickness of quartz glass samples can the defect situation of actual response quartz glass as far as possible, avoid to greatest extent
Defect missing inspection or owing to thickness is excessive, causes the detection time oversize.
Preferred as any of the above-described embodiment, corrosion acid solution is the mixed acid solution of Fluohydric acid. and acetic acid.
Use this mix acid liquor can amplify original defect in quartz glass, again without interference with observed result.Mixing
Acid solution is typically by the pure Fluohydric acid. of top grade (HF >=40%) and analytical pure acetic acid (>=99.5%) mixed preparing.
The pure Fluohydric acid. of top grade (HF >=40%) is 1:3～3:1 with the volume ratio of analytical pure acetic acid (>=99.5%).Press
The mixed acid solution prepared according to this embodiment has suitable corrosion rate, fully amplifies original defect, again
Do not interfere with observed result.
Preferred as any of the above-described embodiment, acid solution temperature is 25 DEG C～100 DEG C.Molten by controlling acid
Liquid is within the range, it is ensured that enough corrosion rates and corrosive effect, for observed result accurately further
Provide guarantee.The temperature of acid solution is controlled by water-bath or oil bath.Water-bath or oil bath can better control over
The temperature of acid solution.
Preferred as any of the above-described embodiment, quartz glass samples two is led to bright finish and is carried out precise polished step such as
Under: by the quartz glass samples of well cutting, on twin grinder or single shaft grinder, use granularity successively
Corundum grinding quartz glass samples two for W40, W20, W10 and W5 leads to bright finish, then at Twp-sided polishing machine
Or on single shaft buffing machine, use the precise polished quartz glass of cerium rouge two to lead to bright finish, surface smoothness
It it is 5 grades.
Fig. 1 is that quartz glass samples is directly by the microphotograph of traditional optical amplifying method detection；Fig. 2 is Fig. 1
Quartz glass samples the inventive method detection (after corrosion, carrying out optical amplifier observation again) microphotograph.
Wherein, the acid solution of etch quartz glass sample by the pure Fluohydric acid. of top grade (HF >=40%) and analytical pure acetic acid (>=
99.5%) pressing the volume ratio configuration of 9:4, mixed acid solution is positioned over water bath with thermostatic control and is heated to 40 DEG C and continues
This temperature of constant temperature, is disposed vertically polished quartz glass samples and corrodes in mixed acid solution；Often
Corrode 1 hour, after being cleaned up by quartz glass samples deionized water, utilize microscopical optical amplifier
Method detection Quartz glass surfaces situation.Fig. 2 is the result observed after corrosion 2 times.From fig. 1, it can be seen that adopt
The defects such as the bubble that there is not any size in quartz glass substrate are detected with traditional optical amplifying method.And from
Fig. 2 understands, and is detected by the detection method of the present invention and there are more microbubble in quartz glass substrate,
After these microbubbles are mixed acid solution corrosion amplification, all expose under microscopic visualization and display,
The accurate detection of the defects such as microbubble in quartz glass substrate is i.e. achieved by the inventive method.Accompanying drawing is shown
Defect be microbubble.Certainly, the impurity for being difficult to detect by conventional method can use this too
Bright method detects.Identical with the principle of bubble, when quartz glass samples is corroded, at impurity
The corrosion position at place and speed are different, therefore, can be amplified the defect at this, afterwards can be by aobvious
Micro mirror observes directly the defect after amplification.For quartz glass prepared by same batch, its microbubble
It is consistent Deng Key Performance Indicator, therefore by same batch quartz glass is randomly drawed 1-3 sheet by this
Bright method detects, and its testing result can represent the relevant parameter of microbubble in this batch quartz glass.
It addition, according to the principle that defect is carried out corrosion amplification of the inventive method, any suitable corrosion can be used
Solution, and it is not limited to the mixed acid solution of above-described embodiment.
The above, the only detailed description of the invention of the present invention, but protection scope of the present invention is not limited to
This, any those familiar with the art, in the technical scope that the invention discloses, can readily occur in
Change or replacement, all should contain within protection scope of the present invention.Therefore, protection scope of the present invention should
It is as the criterion with described scope of the claims.
Claims (8)
1. quartz glass microdefect detection method, it is characterised in that comprise the steps:
Quartz glass samples two is led to bright finish and carries out precise polished；
The most polished quartz glass samples acid solution is corroded；
Quartz glass samples is corroded taking-up in 0.5～2 hour and cleans up with deionized water, utilizes microscope to see
Examine detection quartz glass samples；
By above-mentioned steps, quartz glass samples is repeated corrosion and observation, until observing in quartz glass samples
Defect or to quartz glass samples thickness remain 20-30 μm do not observe defect yet.
Quartz glass microdefect detection method the most according to claim 1, it is characterised in that described stone
The original depth of English glass sample is 1-20mm.
Quartz glass microdefect detection method the most according to claim 1, it is characterised in that described corruption
Erosion acid solution is the mixed acid solution of Fluohydric acid. and acetic acid.
Quartz glass microdefect detection method the most according to claim 3, it is characterised in that described mixed
Close acid solution to be made up of by the volume ratio of 1:3～3:1 with analytical pure acetic acid the pure Fluohydric acid. of top grade.
Quartz glass microdefect detection method the most according to claim 1, it is characterised in that acid solution
Temperature is 25 DEG C～100 DEG C.
Quartz glass microdefect detection method the most according to claim 1, it is characterised in that described acid
The temperature of solution is controlled by water-bath or oil bath.
Quartz glass microdefect detection method the most according to claim 1, it is characterised in that described stone
English glass sample two leads to bright finish, and to carry out precise polished step as follows: by the quartz glass samples of well cutting, double
On surface grinding or single shaft grinder, the corundum using granularity to be W40, W20, W10 and W5 successively grinds
Quartz glass samples two leads to bright finish, then on Twp-sided polishing machine or single shaft buffing machine, uses cerium rouge
Precise polished quartz glass two leads to bright finish, and surface smoothness is 5 grades.
Quartz glass microdefect detection method the most according to claim 1, it is characterised in that described scarce
Fall into as at least one in bubble and impurity.
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| CN201610055734.9A CN105717137B (en) | 2016-01-27 | 2016-01-27 | Method for detecting micro-defects of quartz glass |
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| CN201610055734.9A CN105717137B (en) | 2016-01-27 | 2016-01-27 | Method for detecting micro-defects of quartz glass |
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Cited By (11)
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|---|---|---|---|---|
| CN106546469A (en) * | 2016-10-31 | 2017-03-29 | 东旭科技集团有限公司 | A kind of preparation method of the electron microscopic sample of plate glass |
| CN106959206A (en) * | 2017-03-21 | 2017-07-18 | 中国人民解放军国防科学技术大学 | Fused quartz element zero probability damage threshold Forecasting Methodology based on photo-thermal weak absorbing |
| CN107063112A (en) * | 2017-03-30 | 2017-08-18 | 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 measuring method |
| CN109191440A (en) * | 2018-08-24 | 2019-01-11 | 上海应用技术大学 | Glass blister detection and method of counting |
| CN111257347A (en) * | 2018-11-30 | 2020-06-09 | 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 |
| CN115372090A (en) * | 2022-07-29 | 2022-11-22 | 中国船舶重工集团公司第七0七研究所 | Method for manufacturing and detecting quartz glass subsurface damage depth sample |
| CN117589109A (en) * | 2024-01-19 | 2024-02-23 | 上海强华实业股份有限公司 | Quality detection and control method for quartz center tray manufacturing process |
| CN117705827A (en) * | 2024-02-06 | 2024-03-15 | 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 |
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| CN106546469A (en) * | 2016-10-31 | 2017-03-29 | 东旭科技集团有限公司 | A kind of preparation method of the electron microscopic sample of plate glass |
| 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 |
| CN106959206A (en) * | 2017-03-21 | 2017-07-18 | 中国人民解放军国防科学技术大学 | Fused quartz element zero probability damage threshold Forecasting Methodology based on photo-thermal weak absorbing |
| 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 |
| CN107063112A (en) * | 2017-03-30 | 2017-08-18 | 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 measuring method |
| 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 |
| CN111257347A (en) * | 2018-11-30 | 2020-06-09 | 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 |
| CN115372090A (en) * | 2022-07-29 | 2022-11-22 | 中国船舶重工集团公司第七0七研究所 | Method for manufacturing and detecting quartz glass subsurface damage depth sample |
| CN117589109A (en) * | 2024-01-19 | 2024-02-23 | 上海强华实业股份有限公司 | Quality detection and control method for quartz center tray manufacturing process |
| 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 |
| CN117705827A (en) * | 2024-02-06 | 2024-03-15 | 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 |
| 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 |
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