CN-122016753-A - On-line detection device for trace impurities in electronic-grade quartz crystal material

CN122016753ACN 122016753 ACN122016753 ACN 122016753ACN-122016753-A

Abstract

The application relates to the technical field of material detection, in particular to an online detection device for trace impurities in an electronic-grade quartz crystal material. Collecting material data of a plurality of target materials, then establishing a detection model, inputting a plurality of pretreatment data into the detection model, establishing a standard impurity spectrum database based on the pretreatment data of each target material through the detection model, calibrating by combining a dynamic correlation matching algorithm with a signal enhancement factor to detect the impurity content contained in the target materials, and finally inputting real-time data into the trained detection model to detect the impurity content contained in the real-time materials.

Inventors

LI JIANJUN
WANG JINHAI
ZHANG SONG

Assignees

江苏矽旺电子材料有限公司

Dates

Publication Date: 20260512
Application Date: 20260202

Claims (10)

1. An on-line detection device for trace impurities in an electronic grade quartz crystal material, which is characterized by comprising: The device comprises a conveying module, a laser positioning unit and a control unit, wherein the conveying module is used for conveying target materials and comprises a conveying track, a self-adaptive clamping mechanism and a laser positioning unit; the enrichment module is used for realizing rapid enrichment of trace impurities and microelements on the surface of the target material, and comprises a copper-based substrate and a silver nanowire heating unit; The multi-band stable laser is provided by the excitation module, and the characteristic spectral response of different trace impurities and microelements is adapted, wherein the excitation module comprises a laser light source group, a light path adjusting unit and a wavelength switching unit; The device comprises a collection module, a detection module and a control module, wherein the collection module is used for realizing high-efficiency enhancement and accurate collection of trace impurity Raman signals and comprises a resonant cavity assembly, a signal filtering unit and a high-sensitivity detector; The detection module is in communication connection with the acquisition module, and realizes real-time processing, qualitative and quantitative analysis and result output of detection data through the detection module, and the detection module comprises a data preprocessing unit, a characteristic spectrum matching unit, a quantitative calculation unit and a result output unit.
2. The on-line detection device for trace impurities in electronic grade quartz crystal materials according to claim 1, wherein the self-adaptive clamping mechanisms are arranged on two sides of the conveying track, the self-adaptive clamping mechanisms are used for fixing different types of target materials, and the positioning precision of the laser positioning unit is set to be +/-0.01 mm.
3. The device for on-line detection of trace impurities in electronic grade quartz crystal material according to claim 2, wherein the surface of the copper-based substrate is etched into a scale-like micro-nano structure, and the silver nanowire heating unit is integrated in the copper-based substrate.
4. The device for on-line detection of trace impurities in electronic grade quartz crystal material according to claim 3, wherein the laser light source group comprises a multiband laser generator, the optical path adjusting unit comprises a high-precision reflecting mirror and a lens group to realize collimation, focusing and calibration of laser beams, the focusing spot size is adjustable, and the switching response time of the wavelength switching unit is less than or equal to 1 second.
5. The device for on-line detection of trace impurities in electronic grade quartz crystal material according to claim 4, wherein the resonant cavity assembly is designed as a double-beam folded resonant cavity so as to enable laser to be reflected in the cavity for multiple times, and the detection wavelength range of the high-sensitivity detector is 200-4200cm < -1 > and the resolution is less than or equal to 5cm < -1 > @58550m.
6. An on-line detection method for trace impurities in an electronic grade quartz crystal material, which is applied to the on-line detection device for trace impurities in the electronic grade quartz crystal material as claimed in any one of claims 1 to 5, and is characterized by comprising the following steps: Collecting material data of a plurality of target materials, and preprocessing all the collected material data to obtain a plurality of preprocessed data; Creating a detection model; Inputting a plurality of preprocessing data into a detection model, respectively creating a standard impurity spectrum database based on the preprocessing data of each target material through the detection model, and calibrating by combining a dynamic correlation matching algorithm with a signal enhancement factor to detect the impurity content contained in the target material so as to obtain a trained detection model; and acquiring real-time data of the real-time material, and inputting the real-time data into the trained detection model to detect the impurity content contained in the real-time material.
7. The method for on-line detection of trace impurities in an electronic grade quartz crystal material according to claim 6, wherein the steps of collecting material data of a plurality of target materials, and preprocessing all collected material data to obtain a plurality of preprocessed data, comprise: Creating a material database; setting corresponding acquisition parameters for each target material, acquiring material data of a plurality of target materials based on the acquisition parameters, and putting all acquired material data into a material database, wherein the acquisition parameters comprise a clamping angle and clamping force; Randomly selecting material data of a target material from a material database; Judging whether repeated data exist in the material data of the target material; if the repeated data exist in the material data of the target material, deleting the repeated data; And returning the material data of randomly selecting one target material from the material database until all the target materials are selected to be completed, and obtaining a plurality of preprocessing data.
8. The method for on-line detection of trace impurities in an electronic grade quartz crystal material according to claim 7, wherein the steps of inputting a plurality of pieces of preprocessing data into a detection model, creating a standard impurity spectrum database based on the preprocessing data of each target material through the detection model, and calibrating by combining a dynamic correlation matching algorithm with a signal enhancement factor to detect the impurity content contained in the target material, and obtaining a trained detection model comprise: Dividing all the preprocessing information into a training set and a testing set according to random proportion; Inputting a training set into a detection model, respectively acquiring illumination data of each target material based on a multispectral excitation technology through the detection model, calculating the types of contained impurities through a dynamic correlation matching algorithm, and calculating the content of each type of impurities by combining a standard curve method and an internal standard method to obtain a trained detection model; and inputting the test set into the trained detection model, and verifying whether the trained detection is completed.
9. The method for online detection of trace impurities in an electronic grade quartz crystal material according to claim 8, wherein the training set is input into a detection model, illumination data of each target material are respectively collected based on a multispectral excitation technology through the detection model, then impurity types contained in the target material are calculated through a dynamic correlation matching algorithm, and the content of each impurity type is calculated by combining a standard curve method and an internal standard method, so that a trained detection model is obtained, and the method comprises the following steps: randomly selecting a target material from the training set; acquiring a characteristic spectrum signal obtained by multispectral excitation of the target material, and acquiring the impurity type contained in the target material through the characteristic spectrum signal; calculating the content of each impurity type through a signal enhancement factor; And randomly selecting one target material from the training set until all the target materials in the training set are selected, and obtaining the impurity type and content contained in each target material.
10. The method for on-line detection of trace impurities in an electronic grade quartz crystal material according to claim 9, wherein the steps of collecting real-time data of the real-time material and inputting the real-time data into a trained detection model to detect the impurity content contained in the real-time material comprise: Collecting real-time data of real-time materials; inputting real-time data into a trained detection model, and acquiring the impurity types contained in the real-time material and the impurity content of each type of impurity through the trained detection model; setting content threshold values for each type of impurities respectively; Sequentially judging whether the impurity content of each type of impurity in the real-time material is greater than or equal to a content threshold value; And if the impurity content of at least one type of impurity is greater than or equal to the content threshold value, sending out early warning.

Description

On-line detection device for trace impurities in electronic-grade quartz crystal material Technical Field The invention relates to the technical field of material detection, in particular to an online detection device for trace impurities in an electronic-grade quartz crystal material. Background Electronic grade quartz crystal material (SiO 2 purity is more than or equal to 99.99%) is used as a core raw material in the tip fields of semiconductor silicon smelting, photovoltaic crucible, optical element and the like by virtue of high hardness, high temperature resistance, low thermal expansion coefficient, excellent light transmittance and electrical insulation. The performance stability and reliability of the material are highly dependent on the purity of the material, and the presence of trace (ppm level), especially trace (ppb/ppt level), impurities and microelements can significantly degrade the material performance, such as reducing carrier lifetime, increasing optical loss, affecting thermal stability, and further leading to downstream device failure. Therefore, trace detection and micro-element analysis are key links of electronic-grade quartz crystal material production and quality control. Currently, the mainstream technologies for detecting trace impurities and micro-elements in electronic grade quartz crystal materials include inductively coupled plasma mass spectrometry (ICP-MS), glow Discharge Mass Spectrometry (GDMS), raman spectrometry and the like. The traditional Raman spectroscopy is limited by the problems of low signal intensity, serious fluorescence interference and the like, has insufficient detection sensitivity on trace impurities and microelements, is difficult to meet the ppb level detection requirement, is easily influenced by the coffee ring effect, and causes uneven sample distribution and poor signal reproducibility. Disclosure of Invention The invention aims to solve the problems in the background technology and provides an online detection device for trace impurities in an electronic-grade quartz crystal material. The technical scheme of the invention is as follows: In one aspect, the application provides an on-line detection device for trace impurities in an electronic grade quartz crystal material, comprising: The device comprises a conveying module, a target material conveying module, a laser positioning unit and a control module, wherein the conveying module is used for conveying the target material, and the conveying module comprises a conveying track, a self-adaptive clamping mechanism and a laser positioning unit; the enrichment module is used for realizing rapid enrichment of trace impurities and microelements on the surface of the target material, and comprises a copper-based substrate and a silver nanowire heating unit; The multi-band stable laser is provided by the excitation module, and the characteristic spectral response of different trace impurities and microelements is adapted, wherein the excitation module comprises a laser light source group, a light path adjusting unit and a wavelength switching unit; The device comprises a collection module, a detection module and a control module, wherein the collection module is used for realizing high-efficiency enhancement and accurate collection of trace impurity Raman signals and comprises a resonant cavity assembly, a signal filtering unit and a high-sensitivity detector; The detection module is in communication connection with the acquisition module, and realizes real-time processing, qualitative and quantitative analysis and result output of detection data through the detection module, and the detection module comprises a data preprocessing unit, a characteristic spectrum matching unit, a quantitative calculation unit and a result output unit. Preferably, the self-adaptive clamping mechanisms are arranged on two sides of the conveying track, the fixing of different types of target materials is realized through the self-adaptive clamping mechanisms, and the positioning precision of the laser positioning unit is set to be +/-0.01 mm. Preferably, the surface of the copper-based substrate is etched to form a fish scale imitation micro-nano structure, and the silver nanowire heating unit is integrated in the copper-based substrate. Preferably, the laser light source group comprises a multiband laser generator, the light path adjusting unit comprises a high-precision reflecting mirror and a lens group so as to realize collimation, focusing and calibration of laser beams, the focusing spot size is adjustable, and the switching response time of the wavelength switching unit is less than or equal to 1 second. Preferably, the resonant cavity component is designed as a double-beam waist folding resonant cavity, so that laser light is reflected in the resonant cavity for multiple times, the detection wavelength range of the high-sensitivity detector is 200-4200cm < -1 >, and the resolution is less than or equal to 5cm < -1 >