CN112986276A - Method for accurately detecting inclusions in zinc selenide material - Google Patents

Method for accurately detecting inclusions in zinc selenide material Download PDF

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Publication number
CN112986276A
CN112986276A CN202110305687.XA CN202110305687A CN112986276A CN 112986276 A CN112986276 A CN 112986276A CN 202110305687 A CN202110305687 A CN 202110305687A CN 112986276 A CN112986276 A CN 112986276A
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Prior art keywords
scattering particles
zinc selenide
selenide material
sample
accurately detecting
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CN202110305687.XA
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Chinese (zh)
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唐伟民
尹士平
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Anhui Guangzhi Technology Co Ltd
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Anhui Guangzhi Technology Co Ltd
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Priority to CN202110305687.XA priority Critical patent/CN112986276A/en
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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
    • G01N21/84Systems specially adapted for particular applications
    • G01N21/88Investigating the presence of flaws or contamination
    • G01N21/95Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
    • 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
    • G01N21/84Systems specially adapted for particular applications
    • G01N21/88Investigating the presence of flaws or contamination
    • G01N21/89Investigating the presence of flaws or contamination in moving material, e.g. running paper or textiles
    • G01N21/892Investigating the presence of flaws or contamination in moving material, e.g. running paper or textiles characterised by the flaw, defect or object feature examined
    • 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
    • G01N21/84Systems specially adapted for particular applications
    • G01N21/88Investigating the presence of flaws or contamination
    • G01N21/89Investigating the presence of flaws or contamination in moving material, e.g. running paper or textiles
    • G01N21/892Investigating the presence of flaws or contamination in moving material, e.g. running paper or textiles characterised by the flaw, defect or object feature examined
    • G01N2021/8925Inclusions

Abstract

The invention belongs to the field of infrared material testing, and particularly discloses a method for accurately detecting inclusions in a zinc selenide material. The method provided by the invention obviously improves the recognition capability of scattering particles in the zinc selenide material, reduces the testing time, improves the working efficiency, realizes the measurement of the number and the size of the scattering particles on each layer in the zinc selenide material, and simultaneously reduces the damage of the light of the lamp to the eyes of a human body during the test.

Description

Method for accurately detecting inclusions in zinc selenide material
Technical Field
The invention belongs to the field of infrared material testing, and particularly relates to a method for accurately detecting inclusions in a zinc selenide material.
Background
The detection of the inclusion in the zinc selenide material is to measure scattering particles (such as inclusions, bubbles, large dislocation areas, fog filaments and the like) in the material, namely to test the number and the size of the scattering particles. At present, the method for detecting the inclusions in the zinc selenide material mainly adopts a method combining visual observation and magnifier measurement, and the method uses a strong light lamp to emit oblique light into the interior of the zinc selenide polishing sheet material in the environment illuminated by a fluorescent lamp, observes the interior of the material by naked eyes, measures the scattering particles in the material by the magnifier after finding the scattering particles in the material, and finally reads the measured value. The measurement method is simple, but it can only detect scattering particles which are formed inside the zinc selenide material due to foreign matters introduced by raw materials or equipment and have colors different from the intrinsic color of the material, such as black, red, white and other scattering particles which are very easy to find, but the measurement method is difficult to find the scattering particles which are formed in the chemical vapor deposition process due to incomplete reaction or other reasons and have colors closer to the color of the material (such as gray/gray scattering particles), and the magnifier cannot detect all layers inside the material, i.e. cannot focus on all layers inside the material, so that the detection of all layers of scattering particles inside the material cannot be realized; in addition, the high-light lamp applied by the testing method is mostly parallel light which is emitted in an oblique angle, when in detection, part of light can be reflected from the polished surface of the product and finally enters the eyes of a detector, which not only causes interference to the test, but also causes certain damage to vision after long-time testing.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for accurately detecting impurities in a zinc selenide material, which obviously improves the identification capability of scattering particles in the zinc selenide material, shortens the observation time, improves the working efficiency, realizes the measurement of the number and the size of the scattering particles on each layer of the zinc selenide material, and simultaneously reduces the damage of light to human eyes.
In order to realize the purpose of the invention, the specific technical scheme is as follows:
a method for accurately detecting inclusions in a zinc selenide material comprises the following steps:
the method comprises the following steps: wiping the surface of a zinc selenide material sample to be tested clean, and carrying out the test in a dark room without any visible light;
step two: placing a sample on a table top padded with a black film, using a light source to directly irradiate the side face of the sample in the growth direction of the crystal, finding out the position where scattering particles are densely distributed, and marking;
step three: transferring the sample to an object stage of a microscope, wherein the object stage is padded with a black film, finding scattering particles after the sample is in focus at the marked position by using the microscope, and measuring the size and the number of the scattering particles, wherein the size comprises the length value a and the width value b of the scattering particles;
step four: calculating the size of the scattering particles, wherein the specific formulas (1) and (2) are as follows:
a=k×n1(1)
b=k×n2(2)
wherein: a is the length of the scattering particles to be detected; b is the width of the scattering particles to be measured; k is a dividing ruler grid value; n is the number of graduated scales.
The invention reduces the interference and influence of other light rays on the test process in a darkroom without any light rays; in the second step, light is totally emitted from the side surface of the material (namely the crystal growth direction), and the scattering condition of the scattering particles in the crystal is observed from the front surface of the wafer by means of scattering caused by the total reflection action of impurity particles, bubbles and the like in the crystal on the light. In the third step, a black film is selected as a substrate for detection, so that scattering particles different from black inside the material can be more easily identified.
Further, in the first step, the upper and lower surfaces of the sample of zinc selenide material to be measured need to be polished on both sides.
Furthermore, in the second step, the light source is an LED cold light lamp or a halogen lamp, and the LED cold light lamp which can provide uniform illumination, has low power, high illumination and good color temperature and basically does not generate heat is selected. A halogen lamp that provides uniform illumination, has excellent shielding properties, and does not cause the specimen to heat may also be used.
Further, in the second step, the inside of the sample is observed by naked eyes, and the position where the scattering particles are densely distributed is found out.
Furthermore, in the third step, a measuring microscope with the magnification of 25-50 times is selected, so that accurate measurement of scattering particles on each layer inside the material after focusing is achieved, and the material can be graded according to the size and the number of the scattering particles in the material.
Further, in step three, the measuring the size of the scattering particles specifically includes: and moving the mechanical table, aligning the length and the width of the scattering particles with the graduated scale, reading the number of the scales, and recording the length value a and the width value b of the scattering particles until the scattering particles in a complete frame are measured.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method comprises the steps of firstly, using an LED cold light lamp or a halogen lamp to irradiate the inside of the material from the side in the environment without any light, enabling the material to be transparent by the light, enabling the light penetrating through the material to be very weak, reducing the damage of the light to human eyes, directly measuring the polished zinc selenide material by a tester with naked eyes, moving a sample to an objective table of a microscope after finding scattering particles in the material, accurately measuring the scattering particles in the material by the microscope, and finally reading a measured value. The method of the invention uses two special and relatively soft lights and the black film is used as the substrate, thereby improving the identification capability of scattering particles in the zinc selenide material, reducing the testing time and improving the working efficiency.
(2) The method creates better conditions for the identification and measurement of other scattering particles (except black spots, red spots and white spots), some scattering particles can be seen only under the illumination condition of an LED cold light lamp or a halogen lamp, and the detection of the scattering particles of each layer of material is realized by using a microscope.
(3) The technology of the invention is used for detecting the same amount of products, and the average detected amount of the scattering particles is several times or even tens of times of the amount of the scattering particles detected by the prior art.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is a view showing a structure of a microscope in example 2 of the present invention.
Detailed Description
The present invention will now be described in detail with reference to the drawings, which are given by way of illustration and explanation only and should not be construed to limit the scope of the present invention in any way. Furthermore, features from embodiments in this document and from different embodiments may be combined accordingly by a person skilled in the art from the description in this document.
Example 1
The embodiment discloses a method for accurately detecting inclusions in a zinc selenide material, which comprises the following steps:
the method comprises the following steps: randomly taking a 5PCS zinc selenide wafer with the size of D38 multiplied by H9mm, polishing the upper surface and the lower surface of a zinc selenide material sample to be tested to the surface quality of 60/40, wiping the surface of the sample clean by using dust-free cloth and alcohol, and carrying out the test in a dark room without any visible light;
step two: placing a sample on a table top padded with a black film, using an LED cold light lamp or a halogen lamp to directly irradiate the side face of the sample in the growth direction of the crystal, finding out the position where scattering particles are densely distributed, and marking a frame on the surface of the zinc selenide wafer by using an oil pen;
step three: transferring the sample to an object stage of a microscope, wherein the object stage is padded with a black film, finding scattering particles after the sample is in focus at the marked position by using the microscope, and measuring the size and the number of the scattering particles, wherein the size comprises the length value a and the width value b of the scattering particles;
step four: calculating the size of the scattering particles, wherein the specific formulas (1) and (2) are as follows:
a=k×n1(1)
b=k×n2(2)
wherein: a is the length of the scattering particles to be detected; b is the width of the scattering particles to be measured; k is a dividing ruler grid value; n is the number of graduated scales.
Comparative example 1
The comparative example is a method for most people to know the inclusion in the zinc selenide material, and comprises the following steps:
the method comprises the following steps: comparative example 1 the test was carried out in a daylight lamp environment with the other parameters being the same as in example 1;
step two: irradiating the material from the surface by using a common high-intensity lamp at an oblique angle, and observing the interior of the polished zinc selenide material by naked eyes under the condition of no black background to find out scattering particles in the material;
step three: measuring scattering particles in the material by using a magnifying glass, and measuring the size and the number of the scattering particles by using the magnifying glass, wherein the size comprises the length value a and the width value b of the scattering particles;
step four: the size of the scattering particles was calculated as in step four of the example.
The measurement data in example 1 and comparative example 1 are shown in the following table:
Figure 81173DEST_PATH_IMAGE001
it can be seen that the detection method of example 1 has significantly enhanced ability to test internal scattering particles of zinc selenide material, compared to comparative example 1 using the prior conventional art.
Example 2
This example provides a microscope to which the detection method described in example 1 is applied.
As shown in fig. 1, the microscope according to the present embodiment includes an eyepiece 1, a lens barrel 2, an objective lens 3, an objective lens changer 4, an LED cold light/halogen lamp 5, a stage 6 lined with a black thin film, a coarse focusing screw 7, a fine focusing screw 8, and a back of the lens 9.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (6)

1. A method for accurately detecting inclusions in a zinc selenide material is characterized by comprising the following steps:
the method comprises the following steps: wiping the surface of a zinc selenide material sample to be tested and polished on both sides, and carrying out the test in a dark room without any visible light;
step two: placing a sample on a table top padded with a black film, using a light source to directly irradiate the side face of the sample in the growth direction of the crystal, finding out the position where scattering particles are densely distributed, and making a mark;
step three: transferring the sample to an object stage of a microscope, wherein the object stage is padded with a black film, finding scattering particles after the sample is in focus at the marked position by using the microscope, and measuring the size and the number of the scattering particles, wherein the size comprises the length value a and the width value b of the scattering particles;
step four: calculating the size of the scattering particles, wherein the specific formulas (1) and (2) are as follows:
a=k×n1 (1)
b=k×n2 (2)
wherein: a is the length of the scattering particles to be detected; b is the width of the scattering particles to be measured; k is a dividing ruler grid value; n is the number of graduated scales.
2. The method for accurately detecting the inclusions in the zinc selenide material according to claim 1, wherein in the first step, the upper surface and the lower surface of a sample of the zinc selenide material to be detected are subjected to double-sided polishing treatment.
3. The method for accurately detecting inclusions in a zinc selenide material according to claim 1, wherein in the second step, the light source is an LED cold light lamp or a halogen lamp.
4. The method for accurately detecting the inclusions in the zinc selenide material according to claim 1, wherein in the second step, the interior of the sample is observed by naked eyes to find out the position where the scattering particles are densely distributed.
5. The method for accurately detecting the inclusions in the zinc selenide material according to claim 1, wherein in the third step, a measuring microscope with a magnification of 25-50 times is selected.
6. The method for accurately detecting inclusions in a zinc selenide material according to claim 1, wherein in the third step, the step of measuring the size of scattering particles specifically comprises: and moving the mechanical table, aligning the length and the width of the scattering particles with the graduated scale, reading the number of the scales, and recording the length value a and the width value b of the scattering particles until the scattering particles in a complete frame are measured.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001073410A1 (en) * 2000-03-29 2001-10-04 Corning Incorporated Detecting inclusions in transparent sheets
US20030076492A1 (en) * 2001-10-23 2003-04-24 Stora Enso North America And Spectracode, Inc. Identification of material inclusions in pulp and paper using Raman spectroscopy
US20050259247A1 (en) * 2004-05-21 2005-11-24 Cyr David G Apparatus and process for detecting inclusions
CN103063576A (en) * 2012-12-14 2013-04-24 天津钢铁集团有限公司 Method for quantitatively analyzing inclusions in steel under laser microscope

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001073410A1 (en) * 2000-03-29 2001-10-04 Corning Incorporated Detecting inclusions in transparent sheets
US20030076492A1 (en) * 2001-10-23 2003-04-24 Stora Enso North America And Spectracode, Inc. Identification of material inclusions in pulp and paper using Raman spectroscopy
US20050259247A1 (en) * 2004-05-21 2005-11-24 Cyr David G Apparatus and process for detecting inclusions
CN103063576A (en) * 2012-12-14 2013-04-24 天津钢铁集团有限公司 Method for quantitatively analyzing inclusions in steel under laser microscope

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
上海钢铁研究所: "钢中常见非金属夹杂物的生成及金相鉴定", 《江苏机械》, no. 04, pages 12 - 31 *
钱月平: "膨胀合金4J43组织和性能的初步研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, no. 03, pages 022 - 32 *

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