CN109060686A - A kind of detection device and detection method of quartz glass hydroxy radical content EDS maps - Google Patents

A kind of detection device and detection method of quartz glass hydroxy radical content EDS maps Download PDF

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CN109060686A
CN109060686A CN201810946297.9A CN201810946297A CN109060686A CN 109060686 A CN109060686 A CN 109060686A CN 201810946297 A CN201810946297 A CN 201810946297A CN 109060686 A CN109060686 A CN 109060686A
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quartz glass
detected
light
sample
hydroxyl content
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CN109060686B (en
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王蕾
向在奎
王慧
邵竹锋
符博
王佳佳
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China Building Materials Academy CBMA
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China Building Materials Academy CBMA
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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Abstract

The present invention relates to the detection devices and detection method of hydroxy radical content EDS maps in a kind of quartz glass.Detection device includes, spectrophotometer, sample support frame, mobile device, hood and computer, the spectrophotometric is in respect of optical path export element, the mobile device is for driving the sample support frame or the optical path export element to move, the hood is used to provide detection space for sample, and the computer is connect with the spectrophotometer and mobile device.Detection device provided by the invention can detect automatically the EDS maps of hydroxy radical content in quartz glass to be measured, simplify detecting step, meanwhile, quartz glass to be measured can directly be detected, without preparing thin sample, improve the accuracy of testing result.

Description

Detection equipment and detection method for distribution of hydroxyl content surface of quartz glass
Technical Field
The invention relates to the field of glass detection, in particular to a device and a method for detecting the distribution of hydroxyl content surface of quartz glass.
Background
The quartz glass has high purity, low heat conductivity, excellent thermal vibration resistance, very high deformation temperature and softening temperature, wide optical transmission capacity and other comprehensive performance, and is used widely in electric light source, infrared optics, laser engineering, space engineering and other fields.
The quartz glass is composed of single SiO4]The glass of the composition, OH, is a main impurity component of the silica glass and is an important factor affecting the performance of the silica glass. The hydroxyl content is high, which seriously affects the service life of the electric light source, so that the hydroxyl content is controlled to be reduced; the method is applied to the field of infrared optics, and the hydroxyl generates strong absorption at a position of 2.73 mu m, so that the spectral transmittance of an infrared band is influenced, and the content of the hydroxyl is controlled to be reduced; the OH plays a role in buffering in the quartz glass structure, so that the glass is not easy to damage when being irradiated by laser or cosmic rays, the capacity of resisting the irradiation damage of the laser and the cosmic rays is improved, and the hydroxyl content is controlled to be improved, so that the detection and the control of the hydroxyl content in the quartz glass are very important.
The optical uniformity of silica glass is an important index for measuring the optical quality of silica glass, and it indicates the degree of uniformity of refractive index inside an isotropic medium. When quartz glass is used in laser engineering, poor optical uniformity will result in energy loss during laser transmission; when the quartz glass is applied to an optical lens, the poor optical uniformity causes wavefront distortion, and the imaging resolution is reduced. The refractive index of the quartz glass is reduced by hydroxyl groups, and the refractive index is graded by the gradient of the distribution of the hydroxyl groups, so that the optical uniformity of the quartz glass is influenced.
The optical uniformity can be detected by a laser interferometer. Besides hydroxyl, other metal elements and chlorine in the quartz glass can also influence the refractive index, so that the influence of each component of the quartz glass on the uniformity cannot be specifically analyzed only by using an interferometer, and all influencing factors are mixed together, thereby being not beneficial to scientific research and production link control. In the prior art, the content of OH in quartz glass is detected by adopting a GB/T12442-90 mode of distributed sampling, and then the position and the content are respectively used as a horizontal coordinate and a vertical coordinate to draw so as to represent the distribution gradient of hydroxyl in the quartz glass.
However, in the above detection method, in order not to destroy the finished glass, a thin layer of glass on the upper surface or the lower surface of the finished glass before processing is usually taken, and then distributed sampling processing is performed to obtain the detection size required by the national standard. It can be seen that, by using the upper surface or the lower surface of the quartz glass to be detected as an object to be detected, the distribution of OH on the upper surface or the lower surface is obtained, and the distribution of OH in the quartz glass with a certain thickness is represented by the distribution. Therefore, the distribution of the OH content in the quartz glass obtained by the existing detection method is inaccurate, the reliability is low, and in order to obtain the distribution rule of OH in the quartz glass, a plurality of detection samples need to be processed, so that the workload and the complexity of the detection process are increased.
Disclosure of Invention
The invention mainly aims to provide a device and a method for detecting the distribution of hydroxyl content surface of quartz glass. According to the detection equipment and the detection method for the distribution of the hydroxyl content surface of the quartz glass, the thickness of the quartz glass sample to be detected is not limited, namely the detection object can be a whole piece of quartz glass, so that the accuracy of the detection result is improved, meanwhile, the whole piece of quartz glass can be automatically detected, a plurality of samples do not need to be processed, the detection process is simplified, and the detection efficiency is improved.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.
The detection equipment for the distribution of the hydroxyl content surface of the quartz glass comprises a spectrophotometer, a sample support frame, a moving device, a light shield and a computer, wherein the spectrophotometer is provided with a light path leading-out element, the moving device is used for driving the sample support frame or the light path leading-out element to move, the light shield is used for providing a detection space for a sample, and the computer is connected with the spectrophotometer and the moving device.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, the optical path derivation element comprises a first optical path derivation element and a second optical path derivation element, light irradiated by a light source of the spectrophotometer is defined as first light, the first optical path derivation element changes the first light into second light, the second light passes through a sample to be detected, the second optical path derivation element changes the second light to obtain third light, and a detector of the spectrophotometer receives the third light to detect the third light.
Preferably, in the detection apparatus for detecting distribution of hydroxyl content of quartz glass, three-dimensional data of a sample to be detected is defined as length, height and thickness of the sample to be detected, a direction in which the length of the sample to be detected is located is defined as a horizontal direction, a direction in which the height of the sample to be detected is located is defined as a vertical direction, and the moving device drives the sample support frame to move in the horizontal direction and the vertical direction.
Preferably, the above-mentioned detection apparatus for detecting the distribution of hydroxyl content surface of quartz glass, wherein the moving device includes a control unit, configured to set and generate a motion path instruction; an execution unit to execute the motion path instruction.
Preferably, the detection device for detecting the hydroxyl content surface distribution of the quartz glass comprises an execution unit and a sample support frame, wherein the execution unit comprises a workbench for fixing the sample support frame.
Preferably, in the above apparatus for detecting distribution of hydroxyl content surface of quartz glass, the execution unit is a manipulator, or the execution unit includes a motor, a rolling screw, a workbench, and the like.
Preferably, in the detection apparatus for detecting distribution of hydroxyl content of quartz glass, the spectrophotometer and the sample support are both disposed in the light shield.
The purpose of the invention and the technical problem to be solved can be realized by adopting the following technical scheme.
The method for detecting the distribution of the hydroxyl content surface of the quartz glass comprises the steps of fixing the quartz glass to be detected on a sample support frame, setting a motion path in a control unit of a moving device, forming a motion path instruction, executing the motion path instruction by an execution unit of the moving device, driving the sample support frame to move along the motion path, driving the quartz glass to be detected to move by the sample support frame, completing the motion of the sample support frame and the motion of the quartz glass to be detected in a light shield, obtaining the base line spectral transmittance and the absorption peak spectral transmittance of the hydroxyl in the quartz glass to be detected at the positions of 1.38 mu m, 2.22 mu m or 2.73 mu m in the motion path, obtaining the extinction coefficients of the hydroxyl in the quartz glass at the positions of 1.38 mu m, 2.22 mu m or 2.73 mu m, calculating to obtain the hydroxyl content of different positions of the quartz glass to be detected, and counting to obtain the surface distribution of the hydroxyl content of the quartz glass to be detected.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, in the method for detecting distribution of hydroxyl content in silica glass, three-dimensional data of the silica glass to be detected is defined as length, height and thickness of a sample to be detected, a direction in which the length of the silica glass to be detected is located is defined as a horizontal direction, a direction in which the height of the silica glass to be detected is located is defined as a vertical direction, the motion path instruction includes a motion trajectory, a motion speed, a stop position and a stop time of the stop position, and the motion trajectory includes the horizontal direction and the vertical direction.
Preferably, in the method for detecting the distribution of the hydroxyl content of the quartz glass on the surface, the stop positions at least include a first stop position and a second stop position, coordinates of the first stop position and the second stop position are obtained, the hydroxyl content at the first stop position and the hydroxyl content at the second stop position are respectively calculated, and the distribution of the hydroxyl content of the quartz glass on the surface is obtained through statistics.
By means of the technical scheme, the detection equipment and the detection method for the distribution of the hydroxyl content surface of the quartz glass provided by the invention at least have the following advantages:
1. the invention provides the detection equipment for the distribution of the hydroxyl content surface in the quartz glass, which improves the accuracy of the detection result of the distribution of the hydroxyl content surface in the quartz glass and simplifies the detection steps.
According to the detection equipment provided by the invention, the light path leading-out element is arranged in the spectrophotometer and leads out light rays emitted by a light source of the spectrophotometer, so that a sample to be detected is detected outside a sample chamber, the detection equipment is not limited by the size of the sample chamber and can be used for detecting large-size quartz glass; meanwhile, the detection equipment provided by the invention comprises a moving device, wherein the moving device can be used for driving the sample support frame or the light path leading-out element to move, so that the automatic detection of the distribution of the hydroxyl content surface of the quartz glass is realized, the labor is saved, and the detection steps are simplified; meanwhile, the detection equipment provided by the invention can be used for detecting the quartz glass with a certain thickness without preparing a quartz glass sample, so that the detection steps are greatly saved, meanwhile, the detection result is the hydroxyl content under the thickness of the quartz glass to be detected, and the accuracy of the detection result is improved.
2. The invention also provides a method for detecting the surface distribution of the hydroxyl content of the quartz glass. By adopting the detection method, the hydroxyl content in the quartz glass to be detected can be automatically detected, the detection steps are simplified, and the accuracy of the detection result is improved.
3. The invention further provides a method for detecting the hydroxyl content of a single site of the quartz glass.
In the prior art, the transmittance of hydroxyl groups in quartz glass at 2.73 μm is only used for calculation. The method for measuring the hydroxyl content of the specific site of the quartz glass provided by the invention adopts the transmittance of hydroxyl in the quartz glass at the positions of 1.38 mu m, 2.22 mu m and/or 2.73 mu m to calculate, and overcomes the prejudice in the prior art.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 shows a device for detecting the hydroxyl content distribution of quartz glass according to an embodiment of the present invention,
1, a spectrophotometer, 2, a sample support frame, 3, a lens hood, 4, a computer and 5, wherein the sample is detected;
FIG. 2 is a graph showing the spectral transmittance of the silica glass in the wavelength range of 1000nm to 3200nm in example 1 of the present invention;
FIG. 3 is a graph showing the spectral transmittance of the synthetic quartz glass 1 in example 2 of the present invention in the wavelength range of 1000nm to 3200 nm;
FIG. 4 is a graph showing the spectral transmittance of the synthetic quartz glass 2 in example 3 of the present invention in the wavelength range of 1000nm to 3200 nm;
FIG. 5 is a graph showing the spectral transmittance of the synthetic quartz glass 3 in example 4 of the present invention in the wavelength range of 1000nm to 3200 nm.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to the specific embodiments, structures, features and effects of the detection apparatus and the detection method for detecting the distribution of hydroxyl content of quartz glass according to the present invention with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to different embodiments that are 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 invention provides a device for detecting the distribution of hydroxyl content surface of quartz glass.
The detection equipment for the distribution of the hydroxyl content surface of the quartz glass, disclosed by the invention, comprises a spectrophotometer 1, a sample support frame 2, a moving device, a light shield 3 and a computer 4, wherein the spectrophotometer is provided with a light path leading-out element, the moving device is used for driving the sample support frame or the light path leading-out element to move, the light shield is used for providing a detection space for a sample, and the computer is connected with the spectrophotometer and the moving device.
It should be noted that the type of the detection sample 5 of the detection apparatus provided by the present invention is not particularly limited as long as the apparatus provided by the present invention can be used for detecting the sample, and the sample to be detected can be quartz glass, for example, fused quartz glass, fumed quartz glass, synthetic quartz glass, plasma synthetic quartz glass, or the like.
The detection equipment provided by the invention is provided with a spectrophotometer, and the type, model and other parameters of the spectrophotometer are not particularly limited, and the spectrophotometer can be a visible-near infrared spectrophotometer. The sample support frame is used for supporting a sample to be measured, and the relative position between the sample support frame and the supported sample to be measured is not particularly limited, for example, the sample support frame may be used for fixing the lower bottom surface of the sample to be measured, or the sample support frame may be used for fixing the upper bottom surface of the sample to be measured. The moving device is used for driving the sample support frame or the light path leading-out element to move, and the moving device mainly comprises a motor, a rolling screw rod, a workbench and the like. The mobile device can be used for driving the sample support frame to move, for example, the sample support frame is used for fixing the lower bottom surface of the sample to be detected, at this time, the surface contacting with the lower bottom surface of the sample to be detected is defined as the upper bottom surface of the sample support frame, the surface opposite to the upper bottom surface is the lower bottom surface of the sample support frame, and the mobile device can be installed on the lower bottom surface of the sample support frame; for another example, the sample support is used to fix the upper bottom surface of the sample to be measured, in this case, the surface contacting with the upper bottom surface of the sample to be measured is defined as the lower bottom surface of the sample support, and the surface opposite to the lower bottom surface is defined as the upper bottom surface of the sample support, and the moving device may be mounted on the upper bottom surface of the sample support, in this case, the moving device may be a manipulator.
In the invention, the sample support frame is positioned outside a sample chamber of the spectrophotometer, and the light path leading-out element leads light irradiated by a light source of the spectrophotometer out of the sample chamber, so that the light can pass through a sample to be measured. The lens hood is used for providing the detection space for the sample, and specifically, provides dark detection space for the sample that awaits measuring. Preferably, the spectrophotometer, the sample support frame and the sample to be detected are all located in a light shield, and the light shield needs to provide enough dark space for the movement of the sample to be detected. The material of the light shield of the present invention is not particularly limited, and may be, for example, a hard plastic.
In the present invention, the "computer is connected to the spectrophotometer and the mobile device", it is understood that the computer is connected to the spectrophotometer and used for setting parameters of the spectrophotometer and simultaneously counting and analyzing detection results of the spectrophotometer, and the computer is connected to the mobile device and used for setting and generating a motion path instruction of the mobile device and controlling a motion path of the mobile device.
Preferably, the light path derivation element includes a first light path derivation element and a second light path derivation element, and the light irradiated by the light source of the spectrophotometer is defined as first light, the first light path derivation element changes the first light into second light, the second light passes through the sample to be detected, the second light path derivation element changes the second light to obtain third light, and a detector of the spectrophotometer receives the third light to detect the third light.
The number and kind of the optical path leading-out elements are not particularly limited. Preferably, the first light path derivation component at least includes a first light path derivation component and a second light path derivation component, the first light path derivation component changes the first light, the second light path derivation component continuously changes the first light, that is, the first light continuously changes twice to obtain a second light which can be vertically incident into the sample to be measured, the second light path derivation component at least includes a third light path derivation component and a fourth light path derivation component, the third light path derivation component changes the second light which passes through the sample to be measured, the fourth light path derivation component continuously changes the second light, that is, the second light which passes through the sample to be measured continuously changes twice to obtain a third light which can be vertically received by the detector of the spectrophotometer. Preferably, the first light path derivation component and the second light path derivation component are located on two sides of the sample to be measured respectively, the first light path derivation component is located on one side of a light source of the spectrophotometer, and the second light path derivation component is located on one side of a detector of the spectrophotometer.
The three-dimensional data of the sample to be detected is respectively defined as the length, the height and the thickness of the sample to be detected, and the detection equipment provided by the invention can directly detect the sample to be detected without preparing the sample to be detected into a thin sample with a specific size and thickness. For example, in the prior art, a thin sample with a length of 20mm, a height of 20mm and a thickness of 0.5mm needs to be prepared for detection, but the device of the present invention is not particularly limited to the three-dimensional data of the sample to be detected, and for example, the length may be 450mm, the height may be 450mm and the thickness may be 50 mm.
The invention further provides a method for detecting the distribution of the hydroxyl content surface of the quartz glass, which comprises the steps of fixing the quartz glass to be detected on a sample support frame, setting a motion path of a mobile device in a control unit of the mobile device, forming a motion path instruction, executing the motion path instruction by an execution unit of the mobile device, driving the sample support frame to move along the motion path, driving the quartz glass to be detected to move along the motion path by the sample support frame, and finishing the motion of the sample support frame and the motion of the quartz glass to be detected in a light shield.
According to the detection method provided by the invention, the quartz glass to be detected can automatically move along the set movement path so as to complete the hydroxyl content at different detection positions in the movement path, and the surface distribution of the hydroxyl content of the quartz glass is obtained. Preferably, the motion path instruction includes parameters such as a motion track, a motion speed, a stop position, and a stop time of the stop position. The movement locus is not limited, and can be specifically set according to the position of the quartz glass to be detected, preferably, the movement locus comprises a horizontal direction and a vertical direction, and further preferably, the movement locus is a continuous locus formed by a plurality of horizontal directions and a plurality of vertical directions. The staying positions can be set according to the detection sites of the quartz glass to be detected, and the staying positions can be multiple for obtaining the surface distribution of the hydroxyl content; the retention time is the retention time at a specific retention position, and the length of the retention time can be set according to the time required by the spectrophotometer to complete the detection of the transmittance of a single site.
For example, when the hydroxyl content at three positions of the quartz glass to be detected needs to be detected, the detection method can include:
fixing the quartz glass to be detected on a sample support frame;
acquiring coordinates of the three sites in the quartz glass;
setting a motion path in a control unit of the mobile device according to the three points, and forming a motion path instruction;
the moving device drives the quartz glass to be detected to move along the motion track;
obtaining the base line spectral transmittance and the absorption peak spectral transmittance of hydroxyl groups in the quartz glass to be detected at positions of 1.38 mu m, 2.22 mu m or 2.73 mu m in the moving path;
obtaining extinction coefficients of hydroxyl groups in the quartz glass at three positions at 1.38 micrometers, 2.22 micrometers or 2.73 micrometers respectively;
calculating to obtain the hydroxyl content of the quartz glass to be measured at three positions,
and obtaining the surface distribution of the hydroxyl content of the quartz glass to be detected according to the coordinates of the three sites in the quartz glass and the hydroxyl content.
The invention further provides a method for detecting the content of the hydroxyl at each site.
The invention provides a nondestructive testing method for hydroxyl content in quartz glass, which comprises the following steps:
obtaining the extinction coefficient epsilon of hydroxyl groups in the quartz glass at 1.38 mu m, 2.22 mu m and/or 2.73 mu m1.38μm、ε2.22μmAnd/or epsilon2.73μm
The method and the apparatus for detecting the extinction coefficient are not particularly limited, for example, the method for detecting the extinction coefficient may be a method described in "extinction coefficient of hydroxyl group in quartz glass", luzonun et al, electronic device 1999 vol22(4), the apparatus for detecting the extinction coefficient may be a visible light-near infrared spectrophotometer, and the measurement range may be 1.0 μm to 3.2 μm. The kind of the quartz glass to be measured is not particularly limited in the present invention, and may be, for example, fused quartz glass, gas-smelted quartz glass, synthetic quartz glass, plasma synthetic quartz glass, or the like.
Note that "obtaining the extinction coefficient ε of hydroxyl groups at 1.38. mu.m, 2.22. mu.m, and/or 2.73. mu.m in the silica glass1.38μm、ε2.22μmAnd/or epsilon2.73μmThe "middle" quartz glass "is the same as or the same production batch as the" quartz glass to be measured ", and the" quartz glass "can show complete absorption peaks at 1.38 μm, 2.22 μm and 2.73 μm. The "quartz glass" herein may be a quartz glass having a specific thickness, for example, the thickness of an artificial quartz glass (i.e., a synthetic quartz glass) may be 0.4 to 0.7mm, the thickness of a fumed quartz glass may be 0.8 to 3.0mm, the thickness of an electrofused quartz glass may be 1.6 to 10.0mm, and the like.
According to a first formula, calculating to obtain the hydroxyl content in the quartz glass to be measured,
wherein, the first formula is as follows,
in the formula,
c is the hydroxyl content of the quartz glass to be detected,
epsilon is an extinction coefficient epsilon of hydroxyl groups in the quartz glass at 1.38 mu m, 2.22 mu m and 2.73 mu m1.38μm、 ε2.22μm、ε2.73μm
d is the thickness of the quartz glass to be measured,
m is the molar mass of the hydroxyl groups,
ρ is the density of the quartz glass,
T0the base line spectral transmittance T of hydroxyl groups in the quartz glass to be measured at 1.38 mu m, 2.22 mu m and 2.73 mu m0,1.38μm、T0,2.22μm、T0,2.73μm
T is the absorption peak spectral transmittance T of hydroxyl groups at 1.38 mu m, 2.22 mu m and 2.73 mu m in the quartz glass to be measured1.38μm、T2.22μm、T2.73μm
In the invention, the thickness d of the first formula is the thickness of the quartz glass to be measured, so that the actual thickness of the quartz glass to be measured can be adopted for calculation without processing the thickness of the quartz glass to be measured. Preferably, the thickness d of the quartz glass to be measured can be measured by a measuring tool with high precision, such as a micrometer, to further improve the accuracy of the measurement result.
It should be further noted that, according to the integrality of the absorption peaks at 2.73 μm, 2.22 μm and 1.38 μm in the spectral transmittance curve chart of the quartz glass to be measured, which peak position of 2.73 μm, 2.22 μm and 1.38 μm is selected for calculation can be determined. Namely, the base line spectral transmittance and the absorption peak spectral transmittance of the complete absorption peak positions in 2.73 micrometers, 2.22 micrometers and 1.38 micrometers are selected and substituted into the extinction coefficient of the peak position, and the hydroxyl group content of the quartz glass to be measured is calculated. When the absorption peak average ratios of the peak positions of 2.73 μm, 2.22 μm and 1.38 μm are complete, the conventional peak position (for example, at 2.73 μm) can be selected for calculation.
M in the first formula is the molar mass of hydroxyl groups, namely 17 g/mol; rho is the density of the quartz glass and can adopt a conventional value of 2.2g/cm3The first formula can be further expressed as:
further, the extinction coefficient epsilon of hydroxyl groups in the obtained quartz glass at 1.38 μm, 2.22 μm and/or 2.73 μm is obtained1.38μm、ε2.22μmAnd/or epsilon2.73μm"middle, epsilon1.38μmThe method for obtaining the image comprises the following steps,
obtaining the extinction coefficient epsilon of hydroxyl in the quartz glass at the position of 2.73 mu m2.73μm
According to a second formula, the extinction coefficient epsilon of the hydroxyl groups in the quartz glass at the position of 1.38 mu m is calculated1.38μm
Wherein the second formula is as follows,
the extinction coefficient epsilon of the hydroxyl groups in the quartz glass at the position of 1.38 mu m can be calculated according to the second formula provided by the invention1.38μm
Extinction coefficient epsilon of hydroxyl in quartz glass at 2.73 mu m2.73μmThe value is 77.5 L.mol-1·cm-1In China, 80.1 L.mol is generally adopted-1·cm-1In the present invention, 80.1 L.mol can be used-1·cm-1Go forward and go forwardThe extinction coefficient epsilon of hydroxyl in the quartz glass at the position of 1.38 mu m is carried out by combining the base line spectral transmittance and the absorption peak spectral transmittance at the positions of 2.73 mu m and 1.38 mu m in the spectral transmittance curve chart of the quartz glass in one step1.38μmAnd (4) calculating.
Further, the extinction coefficient epsilon of hydroxyl groups in the obtained quartz glass at 1.38 μm, 2.22 μm and/or 2.73 μm is obtained1.38μm、ε2.22μmAnd/or epsilon2.73μm"middle, epsilon2.22μmThe method for obtaining the image comprises the following steps,
obtaining the extinction coefficient epsilon of hydroxyl in the quartz glass at the position of 2.73 mu m2.73μm
According to a third formula, calculating to obtain the extinction coefficient epsilon of the hydroxyl groups in the quartz glass at the position of 2.22 mu m2.22μm
Wherein the third formula is as follows,
similarly, the extinction coefficient ε of hydroxyl groups at 2.73 μm in quartz glass can be used in the present invention2.73μmThe value 80.1L. mol-1·cm-1Further, the extinction coefficient ε of hydroxyl groups at 2.22 μm in silica glass was performed by further combining the base line spectral transmittance and the absorption peak spectral transmittance at 2.73 μm and 2.22 μm in the spectral transmittance graph of silica glass2.22μmAnd (4) calculating.
Further, the step of calculating to obtain the hydroxyl group content in the to-be-detected quartz glass according to the first formula comprises the steps of obtaining a spectral transmittance curve of the to-be-detected quartz glass, and selecting T (absorption peak spectral transmittance) of absorption peak positions of 2.73 micrometers, 2.22 micrometers and 1.38 micrometers to be greater than or equal to 1%, wherein T is T0-a peak position where T (baseline spectral transmittance-absorption peak spectral transmittance) is greater than or equal to 1% as a calculated peak position, the baseline spectral transmittance, absorption peak spectral transmittance, sample thickness and extinction of the calculated peak position being taken asAnd substituting the coefficient into the first formula, and calculating to obtain the hydroxyl content in the quartz glass to be detected, thereby further improving the accuracy of the detection result. When the aforementioned three or two peak positions satisfy the condition, it is preferable to detect the peak position commonly used for the silica glass to be compared.
The invention further provides a definition rule of the thickness of the quartz glass to be measured.
Due to epsilon1.38μmAnd ε2.22μ m number-to-average ∈2.73μmMuch smaller, when the peak position of 2.22 μm is selected for calculation, the upper limit of the thickness detection of the quartz glass to be detected is that of the peak position of 2.73 μmAnd (4) doubling. When the peak position of 1.38 μm is selected for calculation, the upper limit of the thickness detection of the quartz glass to be detected is 2.73 μmAnd (4) doubling.
Example 1
This example provides an extinction coefficient ε of hydroxyl groups at 1.38 μm and 2.22 μm in quartz glass1.38μm、ε2.22μmThe method of (3).
In this example, the silica glass was a synthetic silica glass and had a thickness of 1 mm.
The spectral transmittance curve of the quartz glass in the wavelength range of 1000nm to 3200nm in this example is shown in FIG. 2. Base line spectral transmittances T at 2.73 μm, 2.22 μm, 1.38 μm positions in FIG. 20And absorption peak spectral transmittance T are shown in table 1.
TABLE 1T at the 2.73 μm, 2.22 μm, 1.38 μm positions in FIG. 20And T
In this example, the extinction coefficient ε of 2.73 μm hydroxyl groups in silica glass was selected2.73μmThe value 80.1L. mol-1·cm-1Calculating according to the second formula to obtain the extinction coefficient epsilon of the hydroxyl groups in the quartz glass at the position of 1.38 mu m1.38μmIs 0.45Lmol-1cm-1(ii) a According to the third formula, the extinction coefficient epsilon of the hydroxyl in the quartz glass at the position of 2.22 mu m is calculated2.22μmIs 1.61Lmol-1cm-1
Further, the extinction coefficient ε of hydroxyl groups at 1.38 μm in the quartz glass obtained by the above calculation1.38μ m0.45Lmol-1cm-1Or an extinction coefficient ε at 2.22 μm2.22μmIs 1.61Lmol-1cm-1Substituting the first formula into the first formula, and meanwhile, adding the molar mass M17 g/mol of hydroxyl; density of silica glass rho 2.2g/cm3Substituting said first formula, then:
when the peak position at 1.38 μm is selected for calculation, the first formula can be further expressed as:
when the peak position at 2.22 μm is selected for calculation, the first formula can be further expressed as:
definition of thickness of the quartz glass to be measured:
the extinction coefficient ε was calculated according to this example1.38μmAnd ε2.22μmWhen the peak position of 2.22 μm is selected for calculation, the upper limit of the thickness detection of the quartz glass to be detected is set to 2.73 μmDoubling; when the peak position of 1.38 μm is selected for calculation, the upper limit of the thickness detection of the quartz glass to be detected is 2.73 μmAnd (4) doubling.
Example 2
The embodiment provides a nondestructive testing method for hydroxyl content in synthetic quartz glass.
The thickness of the synthetic quartz glass 1 in this example was 5.25 mm.
The spectral transmittance curve of the synthetic quartz glass 1 of the present example in the wavelength range of 1000nm to 3200nm is shown in FIG. 3.
When the method for detecting the hydroxyl group content in the silica glass described in GB/T12442-90 of the prior art is used, since the thickness of the synthetic silica glass 1 in this example is 5.25mm, which exceeds the thickness of the artificial silica glass defined in this standard by 0.4-0.7mm, and as can be seen from FIG. 3, the spectral peak at 2.73 μm of the synthetic silica glass 1 in this example cannot be shown, and therefore, the method described in GB/T12442-90 cannot be used for detection.
Baseline spectral transmittance T at 2.22 μm, 1.38 μm position in FIG. 30And absorption peak spectral transmittance T are shown in table 2.
TABLE 2T at the 1.38 μm, 2.22 μm position in FIG. 30And T
The extinction coefficient ε obtained in example 12.22μmBaseline spectral transmittance T at 2.22 μm position0And absorption peak spectral transmittance T into the first public keyThe hydroxyl group content of the synthetic quartz glass 1 in this example was calculated to be 1377 ppm; the extinction coefficient ε obtained in example 11.38μmBase line spectral transmittance T at 1.38 μm position0And the absorption peak spectral transmittance T were substituted into the first formula to calculate, and the synthetic quartz glass 1 of the present example had a hydroxyl group content of 1370 ppm. It can be seen that the extinction coefficient ε provided in example 1 was used1.38μm、ε2.22μmThe difference from the content of hydroxyl groups in the synthetic quartz glass 1 calculated from the base line spectral transmittance and the absorption peak spectral transmittance in table 2 of this example was not large, and the deviation was 7 ppm.
Example 3
The embodiment provides a nondestructive testing method for hydroxyl content in synthetic quartz glass.
The thickness of the synthetic quartz glass 2 in this example was 11 mm.
The spectral transmittance curve of the synthetic quartz glass 2 of this example in the wavelength range of 1000nm to 3200nm is shown in FIG. 4. Baseline spectral transmittance T at 2.22 μm, 1.38 μm position in FIG. 40And absorption peak spectral transmittance T are shown in table 3.
TABLE 3T at the 1.38 μm, 2.22 μm position in FIG. 40And T
The extinction coefficient ε obtained in example 12.22μmBaseline spectral transmittance T at 2.22 μm position0Substituting the absorption peak spectral transmittance T into the first formula, and calculating to obtain 1469ppm of hydroxyl content of the synthetic quartz glass 2 in the embodiment; the extinction coefficient ε obtained in example 11.38μmBase line spectral transmittance T at 1.38 μm position0And substituting the absorption peak spectral transmittance T into the first formula, and calculating to obtainThe synthetic quartz glass 2 of this example had a hydroxyl group content of 1467 ppm. It can be seen that the extinction coefficient ε provided in example 1 was used1.38μm、ε2.22μmThe difference from the content of hydroxyl groups in the synthetic quartz glass 2 calculated from the base line spectral transmittance and the absorption peak spectral transmittance in table 3 of this example was not large, and the deviation was 2 ppm.
Example 4
The embodiment provides a nondestructive testing method for hydroxyl content in synthetic quartz glass.
The thickness of the synthetic quartz glass 3 in this example was 21 mm.
The spectral transmittance curve of the synthetic quartz glass 3 in the wavelength range of 1000nm to 3200nm in this example is shown in FIG. 5. Baseline spectral transmittance T at 2.22 μm, 1.38 μm position in FIG. 50And absorption peak spectral transmittance T are shown in table 4.
TABLE 4T at 1.38 μm, 2.22 μm position in FIG. 50And T
The extinction coefficient ε obtained in example 12.22μmBaseline spectral transmittance T at 2.22 μm position0Substituting the absorption peak spectral transmittance T into the first formula, and calculating to obtain 1464ppm of hydroxyl content of the synthetic quartz glass 3 in the embodiment; the extinction coefficient ε obtained in example 11.38μmBase line spectral transmittance T at 1.38 μm position0And the absorption peak spectral transmittance T were substituted into the first formula, and calculation was made to obtain 1467ppm of the hydroxyl group content of the synthetic quartz glass 3 in this example. It can be seen that the extinction coefficient ε provided in example 1 was used1.38μm、ε2.22μmAnd the calculated base line spectral transmittance and absorption peak spectral transmittance in Table 4 of this example to obtain hydroxyl group in synthetic quartz glass 3The content of radicals was not very different, with a deviation of 3 ppm.
The above examples 2 to 4 provided by the present invention can show that the nondestructive testing method for hydroxyl group content in quartz glass provided by the present invention is applicable to quartz glass with different thicknesses.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
It will be appreciated that the relevant features of the devices described above may be referred to one another. In addition, "first", "second", and the like in the above embodiments are for distinguishing the embodiments, and do not represent merits of the embodiments.
The foregoing is a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any simple modification, equivalent changes and modifications made to the foregoing embodiment according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.

Claims (10)

1. The utility model provides a check out test set that quartz glass hydroxyl content face distributes which characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
a spectrophotometer, a sample support frame, a mobile device, a lens hood and a computer,
wherein the spectrophotometer has an optical path deriving element,
the moving device is used for driving the sample support frame or the light path leading-out element to move,
the light shield is used for providing a detection space for the sample,
the computer is connected with the spectrophotometer and the mobile device.
2. The apparatus for detecting the distribution of hydroxyl content surface of quartz glass according to claim 1, wherein:
the optical path derivation member includes a first optical path derivation member and a second optical path derivation member,
the method comprises the steps of defining light irradiated by a light source of the spectrophotometer as first light, changing the first light into second light by a first light path leading-out element, enabling the second light to penetrate through a sample to be detected, changing the second light by a second light path leading-out element to obtain third light, receiving the third light by a detector of the spectrophotometer, and detecting the third light.
3. The apparatus for detecting the distribution of hydroxyl content surface of quartz glass according to claim 1, wherein:
respectively defining the three-dimensional data of the sample to be detected as the length, the height and the thickness of the sample to be detected, defining the direction of the length of the sample to be detected as the horizontal direction and the direction of the height of the sample to be detected as the vertical direction,
the moving device drives the sample support frame to move in the horizontal direction and the vertical direction.
4. The apparatus for detecting the distribution of hydroxyl content surface of quartz glass according to claim 1, wherein:
the mobile device comprises a mobile terminal and a mobile terminal,
the control unit is used for setting and generating a motion path instruction;
an execution unit to execute the motion path instruction.
5. The apparatus for detecting the distribution of hydroxyl content surface of quartz glass according to claim 4, wherein:
the execution unit comprises a workbench used for fixing the sample support frame.
6. The apparatus for detecting the distribution of hydroxyl content surface of quartz glass according to claim 4, wherein:
the execution unit comprises a manipulator;
or,
the execution unit comprises a motor, a rolling screw rod and a workbench.
7. The apparatus for detecting the distribution of hydroxyl content surface of quartz glass according to claim 1, wherein:
the spectrophotometer and the sample support frame are both arranged in the light shield.
8. A method for detecting the distribution of hydroxyl content surface of quartz glass is characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
fixing the quartz glass to be measured on a sample support frame,
setting a motion path in a control unit of the mobile device, forming a motion path instruction,
the execution unit of the mobile device executes the motion path instruction to drive the sample support frame to move along the motion path, the sample support frame drives the quartz glass to be detected to move, the movement of the sample support frame and the movement of the quartz glass to be detected are completed in the light shield,
obtaining the base line spectral transmittance and the absorption peak spectral transmittance of hydroxyl groups in the quartz glass to be detected at the positions of 1.38 mu m, 2.22 mu m or 2.73 mu m in the moving path,
obtaining the extinction coefficient of the hydroxyl in the quartz glass at the position of 1.38 μm, 2.22 μm or 2.73 μm,
calculating to obtain the hydroxyl content of different positions of the quartz glass to be detected,
and counting to obtain the surface distribution of the hydroxyl content of the quartz glass to be detected.
9. The method for detecting the distribution of the hydroxyl content surface of the quartz glass according to claim 8, wherein:
respectively defining the three-dimensional data of the quartz glass to be detected as the length, the height and the thickness of a sample to be detected, defining the direction of the length of the quartz glass to be detected as the horizontal direction, and the direction of the height of the quartz glass to be detected as the vertical direction,
the motion path instruction comprises a motion track, a motion speed, a stop position and stop time of the stop position, and the motion track comprises a horizontal direction and a vertical direction.
10. The method for detecting the distribution of the hydroxyl content surface of the quartz glass according to claim 9, wherein:
the stopping positions at least comprise a first stopping position and a second stopping position, the coordinates of the first stopping position and the second stopping position are obtained,
calculating the hydroxyl content at the first and second dwell positions separately,
and (5) counting to obtain the surface distribution of the hydroxyl content of the quartz glass.
CN201810946297.9A 2018-08-17 2018-08-17 Detection equipment and detection method for distribution of hydroxyl content surface of quartz glass Active CN109060686B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114034669A (en) * 2021-12-13 2022-02-11 中国建筑材料科学研究总院有限公司 Method for detecting spectral transmittance of quartz glass
CN116930115A (en) * 2023-09-15 2023-10-24 久智光电子材料科技有限公司 Quartz glass hydroxyl detection method and detection device

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101046442A (en) * 2007-01-09 2007-10-03 陈士斌 Infrared spectrum analysis process for measuring hydroxy radical content in natural quartz
CN201993309U (en) * 2011-01-04 2011-09-28 无锡安特电子有限公司 Device for on-line testing scale numbers of auto-dimming soldering face mask
CN102478505A (en) * 2010-11-30 2012-05-30 新奥科技发展有限公司 Device for determining optical parameters of fluid
CN103472019A (en) * 2013-09-30 2013-12-25 重庆大学 Spectrographic method for fast detecting pesticide residues
CN203405407U (en) * 2013-08-22 2014-01-22 泰通(泰州)工业有限公司 Reflectivity test cabinet externally connected with ultraviolet visible light spectrophotometer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101046442A (en) * 2007-01-09 2007-10-03 陈士斌 Infrared spectrum analysis process for measuring hydroxy radical content in natural quartz
CN102478505A (en) * 2010-11-30 2012-05-30 新奥科技发展有限公司 Device for determining optical parameters of fluid
CN201993309U (en) * 2011-01-04 2011-09-28 无锡安特电子有限公司 Device for on-line testing scale numbers of auto-dimming soldering face mask
CN203405407U (en) * 2013-08-22 2014-01-22 泰通(泰州)工业有限公司 Reflectivity test cabinet externally connected with ultraviolet visible light spectrophotometer
CN103472019A (en) * 2013-09-30 2013-12-25 重庆大学 Spectrographic method for fast detecting pesticide residues

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
安捷伦科技: "药物分析应用中的分子光谱产品", 《HTTPS://WWW.DOCIN.COM/P-1701293268.HTML》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114034669A (en) * 2021-12-13 2022-02-11 中国建筑材料科学研究总院有限公司 Method for detecting spectral transmittance of quartz glass
CN116930115A (en) * 2023-09-15 2023-10-24 久智光电子材料科技有限公司 Quartz glass hydroxyl detection method and detection device
CN116930115B (en) * 2023-09-15 2023-12-12 久智光电子材料科技有限公司 Quartz glass hydroxyl detection method and detection device

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