CN114486844B - Spectrum analysis method and system for zinc oxide - Google Patents
Spectrum analysis method and system for zinc oxide Download PDFInfo
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Abstract
The invention relates to the field of material spectral analysis, in particular to a spectral analysis method and a system for zinc oxide, which comprises the following steps: the method comprises the steps of acquiring Raman shifts of different positions on zinc oxide samples prepared under different electric field strengths and temperatures by using a Raman spectrum detector, acquiring the Raman spectrum of each sample, clustering peaks on the Raman spectra of all the samples to obtain all peak types, randomly sampling position sets from the samples, acquiring the spectral reference degree of the position sets according to the peak types and the Raman shifts of all the positions in the position sets, combining the position sets with the maximum spectral reference degree and preset number into one set, and reconstructing the Raman spectrum of each sample according to the Raman shifts of all the positions in the set. The method enables the finally obtained Raman spectrum to show the crystallization rule of the zinc oxide more prominently, does not introduce noise caused by too many impurities, and enables the crystallization rule of the zinc oxide analyzed according to the Raman spectrum to be more accurate and credible.
Description
Technical Field
The invention relates to the field of material spectral analysis, in particular to a spectral analysis method and system for zinc oxide.
Background
Zinc oxide has important value in the fields of semiconductors and the like, in order to analyze the property of zinc oxide, prepare pure zinc oxide in a large scale and excavate application scenes thereof, the crystallization process of zinc oxide under different conditions in the preparation process needs to be researched, the existing crystallization process for researching zinc oxide utilizes the Raman effect of a zinc oxide sample on light, and the Raman effect refers to the phenomenon that when light passes through a transparent medium, the frequency of the light scattered by molecules changes; at present, zinc hydroxide is generally used and subjected to heat treatment at a certain temperature and electric field intensity to obtain a zinc oxide crystal, then a Raman spectrum of a zinc oxide sample is obtained according to the Raman effect of the zinc oxide sample, the Raman spectrum of different samples prepared at different temperatures and electric field intensities is analyzed to obtain the crystallization process of the zinc oxide, and the crystallization rule is analyzed.
However, impurities in a prepared zinc oxide sample are often ignored in the existing method, for example, zinc nitrate and sodium hydroxide are often used when zinc hydroxide is prepared, so that the zinc hydroxide contains impurities such as nitrate, impurities appear in the zinc oxide sample, and the crystallization process of zinc oxide in the sample cannot be accurately reflected through a raman spectrum.
Disclosure of Invention
In order to solve the above technical problems, the present invention aims to provide a method and a system for spectroscopic analysis of zinc oxide, wherein the technical scheme adopted is as follows:
the invention provides a spectral analysis method for zinc oxide, which comprises the following steps:
acquiring zinc oxide samples prepared under different electric field strengths and different temperatures, acquiring Raman shifts of different positions on each sample by using a Raman spectrum detector, constructing a Raman spectrum of each sample according to the Raman shifts of all the positions on each sample, and clustering peaks on the Raman spectra of all the samples to acquire all peak types;
randomly obtaining a position from each sample, wherein all the positions obtained from all the samples form a position set, obtaining the spectral reference degree of the position set according to the peak type and the Raman shifts of all the positions in the position set, obtaining the position set with the maximum spectral reference degree and the preset number, combining the position sets with the preset number into a set, reconstructing the Raman spectrum of each sample according to the Raman shifts of all the positions on each sample and in the combined set, and analyzing the zinc oxide.
Further, the step of obtaining the peak category includes:
all peaks in each Raman spectrum are obtained, all peaks with overlapping parts are grouped into one type in the Raman spectra of all samples, and each type in all the obtained types is a peak type.
Further, the step of obtaining all peaks in the raman spectrum comprises:
performing Fourier transform on the Raman spectrum to obtain the frequency and the intensity of all signals contained in the Raman spectrum, setting the intensity of the signals with the frequency less than a threshold value to be zero, then performing inverse Fourier transform on all the signals to obtain a first Raman spectrum, and regarding all peaks contained in the first Raman spectrum as all peaks on the Raman spectrum.
Further, the step of obtaining the spectral reference level of the position set comprises:
for each position in the position set, acquiring all peaks on the Raman spectrum of the sample corresponding to each position, further acquiring a peak where the Raman shift of each position is located, namely the peak of each position, taking the Raman shift corresponding to the peak of each position as the reference Raman shift of each position, performing weighted summation on absolute values of differences between the Raman shifts of all positions in the position set and the reference Raman shifts of all positions, and taking the reciprocal of the obtained result as the spectral reference degree of the position set.
Further, the step of obtaining the weight of each position in the weighted summation process includes:
combining the peak value and the width of each peak into a feature vector of each peak, acquiring all comparison peaks of the peaks at each position, acquiring the mean value of Euclidean distances between the feature vector of each peak at each position and the feature vectors of all comparison peaks, and taking the mean value as the weight of each position.
Further, the step of obtaining all the comparison peaks of the peak at each position comprises:
obtaining the wave crest category to which the wave crest at each position belongs, and obtaining the temperature and the electric field intensity of a sample corresponding to each wave crest in the wave crest categories during preparation;
in the peak category, if one peak corresponds to a temperature which is larger than the temperature corresponding to the peak at each position and has the smallest difference, the peak is taken as a comparison peak of the peak at each position; if one peak corresponds to a temperature smaller than the temperature corresponding to the peak at each position and has the smallest difference, the peak is taken as a comparison peak of the peak at each position; if the corresponding electric field intensity of one peak is larger than that of the peak at each position and the difference is minimum, the peak is taken as a comparison peak of the peak at each position; if the corresponding electric field intensity of one peak is smaller than the corresponding electric field intensity of the peak at each position and the difference is minimum, the peak is taken as a comparison peak of the peak at each position;
and then all the comparison wave crests of the wave crests at each position are obtained through comparison and judgment.
Further, the raman spectrum represents the raman intensity of the sample at different raman shifts.
The invention also provides a zinc oxide spectral analysis system which comprises a processor and a memory, wherein the processor is used for processing instructions stored in the memory so as to realize the steps of the zinc oxide spectral analysis method.
The invention has the following beneficial effects: according to the method, the Raman spectra of the zinc oxide sample under various temperatures and electric field intensities are obtained, the rough crystallization process of the zinc oxide sample under the interference of impurities is obtained, then the position set is obtained, and the Raman shifts of all the positions in the position set are closest to the rough crystallization process, so that the Raman spectrum is reconstructed according to the position set, and the Raman spectrum is prevented from introducing noise caused by too many impurities; in addition, by paying attention to the spectral characteristics of the Raman effect which changes greatly, the crystallization rule of the zinc oxide can be more highlighted by the Raman spectrum, and the crystallization rule of the zinc oxide analyzed by the Raman spectrum is more accurate and credible.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions and advantages of the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flowchart of a method for spectroscopic analysis of zinc oxide according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a peak in the filled spectrum according to an embodiment of the present invention.
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 a method and system for spectroscopy analysis of zinc oxide according to the present invention, and the specific implementation, structure, features and effects thereof with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "another embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The following describes a specific scheme of the spectroscopic analysis method for zinc oxide provided by the invention in detail with reference to the accompanying drawings.
Referring to fig. 1, a method for analyzing zinc oxide by spectrum according to the present invention is shown, which comprises the following steps:
and S001, preparing zinc oxide samples at different temperatures and electric field intensities, and obtaining the Raman spectrum of each zinc oxide sample.
Preparing zinc hydroxide by using zinc nitrate and sodium hydroxide, then respectively carrying out oil bath heat treatment on the zinc hydroxide at N temperatures, wherein each temperature corresponds to M electric field intensities, and each sample is respectively subjected to heat treatment for Q hours, so that K = M × N × Q zinc oxide samples are finally obtained. The temperature of N =6,N is respectively 100 ℃, 110 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃, and the voltage of M =3,M electric fields is respectively 0 kilovolt, 2 kilovolts and 4 kilovolts; q =6; each zinc oxide sample may contain chemical components such as zinc oxide, impurities, and the like;
pressing each zinc oxide sample into a sheet with a certain area by using a tablet press, and then acquiring the Raman shift of each position on each sample sheet by using a Raman spectrometer, wherein the Raman shift is reflected by the frequency change of light after the light penetrates through each position, and the value is only related to the chemical composition of each position; and obtaining the Raman intensity corresponding to each Raman shift through the Raman shifts of all the positions on each sample, and further obtaining the Raman spectrum of each sample, namely the Raman spectrum reacts on the Raman intensities under different Raman shifts. However, all raman spectra cannot accurately reflect the zinc oxide crystallization process in the sample due to impurities contained in the sample.
And S002, classifying peaks on all Raman spectrums according to the Raman spectrums of all samples.
Firstly, acquiring a peak of each Raman spectrum, wherein the specific method comprises the following steps: and performing Fourier transform on each Raman spectrum to obtain signals of all frequencies contained in each Raman spectrum and signal intensity, setting the intensity of the signal of which the frequency is less than a threshold value to be 0, then performing inverse Fourier transform on all the signals, and obtaining a result called a first Raman spectrum, wherein all peaks in the first Raman spectrum are used as peaks of each Raman spectrum. The purpose is to remove interference of low frequency signals in the raman spectrum.
Each peak represents a Raman spectrum segment and also represents Raman intensities corresponding to different Raman shifts in a Raman shift value interval, and the reaction is the corresponding characteristic of a certain chemical component in the sample to the Raman effect of the light wave; different chemical compositions have different peaks, and the crystallization process of the zinc oxide can be analyzed through the change of the peaks on all samples, such as the temperature, the electric field intensity and the time for starting crystallization or finishing crystallization of the zinc oxide can be obtained, but the analysis result is inaccurate due to the interference of impurities, and the analysis result cannot be reproduced.
In order to solve the secondary problem, firstly, the peaks of the Raman spectra of all zinc oxide samples are classified, and the specific method comprises the following steps: for all peaks on all raman spectra, clustering peaks with overlapping parts into a class, and each class in all obtained classes is called a peak class;
according to the actual shape, each peak in any one peak category can be known to come from the Raman spectra of different samples, and because the peaks on the Raman spectra cannot be overlapped, the peaks on the same Raman spectrum cannot be classified into the same peak category; when the number of peaks in a peak category is not equal to the number K of samples, which indicates that there is a sample and the raman spectrum thereof has no peak in a segment corresponding to other peaks, a virtual peak is assigned to such sample and is assigned to the peak category, and the virtual peak is obtained by: obtaining the mean value of Raman displacement at the peak value of all wave crests in the wave crest type; and acquiring Raman displacement value intervals of all the wave crests in the wave crest category, combining all the Raman displacement value intervals into one interval, wherein a virtual wave crest exists in the interval, the peak value of the wave crest is close to 0 but not equal to 0, the peak value is set to be 0.001, and the Raman displacement at the peak value is the mean value. By the operation, the number of the peaks in each peak category is equal to the number K of the samples, so that the accuracy of subsequent analysis is facilitated.
All peaks in the same category represent the corresponding features of the raman effect of the same chemical composition in the sample at different temperatures and electric field strengths, and the peak positions and widths in the same category should be the same if there is no impurity interference, only the peaks may be different.
And step S003, randomly obtaining a position set from all samples, and obtaining the spectral reference degree of the position set.
When the sample contains impurities, although the positions and widths of peaks in the same peak category may not be the same any more, the approximate change rule of the zinc oxide crystallization process can still be approximately reflected; in addition, the invention considers that the interference of impurities in the sample only appears at a small part of positions on the sample, or the impurities only interfere the Raman effect of the small part of positions on the sample, and the invention needs to eliminate the interference of the positions by the following method:
randomly selecting a position from each sample, forming a position set by the positions selected from all the samples, wherein the position set comprises K positions, and obtaining a set formed by all peaks on the Raman spectrum of the sample corresponding to the kth position in the position set, wherein the peak is a peak in the Raman spectrum of the sample corresponding to the kth position in the position set
The kth positionHas a Raman shift of
In a
In (C) acquisition
Wave crest
Taking the corresponding Raman shift at the peak value of the peak as the reference Raman shift of each position
The reference Raman shifts of all positions reflect the approximate change rule of the zinc oxide crystallization process.
Then the spectral reference degree of the location set
Is composed of
Wherein
Weighting and summing absolute values of differences between the Raman shifts of all the positions and the reference Raman shifts of all the positions, wherein the smaller X is, the smaller the difference between the Raman shifts of all the positions and the reference Raman shifts of all the positions is, namely, the Raman shifts of all the positions are more consistent with the approximate change rule of the zinc oxide crystallization process, the Raman shift value of each position in the position set is taken as a reference, and the possibility of introducing noise and interference is lower; the larger X is, the larger difference between the Raman shift of all the positions and the reference Raman shift of all the positions is, namely the Raman shift of all the positions is less consistent with the approximate change rule of the zinc oxide crystallization process, and the larger X is, the larger difference is, the Raman shift of all the positions is, the more the Raman shift of all the positions is not consistent with the approximate change rule of the zinc oxide crystallization process, and the more the Raman shift of all the positions is, the more the reference Raman shift of all the positions is, the difference is, the indication that the Raman shift of the zinc oxide crystallization process isThe raman shift at each position in the set of positions is not worth referencing. Namely, it is
Is in inverse proportion to X.
Wherein
The weight is represented, and the calculation method comprises the following steps:
the peak at the kth position in the position set is
Obtaining
The temperature and electric field intensity of the sample corresponding to each peak in the belonging peak category during preparation; in that
In the category of the peaks, if a peak is present, the temperature ratio corresponding to it
The corresponding temperature is large and the difference is minimal, then the peak is taken as
The control peak of (3); if a peak, its corresponding temperature ratio
The corresponding temperature is small and the difference is minimal, then the peak is taken as
The control peak of (4); if a peak is present, the corresponding electric field intensity ratio
The corresponding electric field intensity is large and the difference is minimum, then the peak is regarded as
The control peak of (4); if a peak is present, the corresponding electric field intensity ratio
The corresponding electric field intensity is small and the difference is minimal, then the peak is taken as
The control peak of (4); and then obtained through comparison and judgment
All control peaks.
Firstly, the first step is to
And
the peak value of each peak in all the comparison peaks, the width of the peak are combined into a feature vector of the peak, and then each peak is obtained
The mean value of the Euclidean distances between the feature vector of (2) and the feature vectors of all the comparison peaks is used as the mean value
。
The greater the description
The greater the difference from all the control peaks, indicating that
The corresponding of a certain chemical component to the Raman effect of light waveThe characteristics are greatly changed, so that more attention is paid to
The size of (d); by introducing weights
The characteristic that the Raman spectrum which changes obviously is large in change is paid attention to as much as possible when the reference degree of the position set is calculated, because the fact that the Raman spectrum which changes obviously is large in change indicates that chemical components in a sample are changed obviously, the change has important reference significance for analyzing the zinc oxide crystallization process, disturbance caused by impurity interference when the reference degree of the position set is calculated is avoided, and the fact that the subsequent obtained Raman spectrum can highlight the crystallization rule of the zinc oxide is guaranteed.
And step S004, obtaining an accurate full spectrum according to the spectrum reference degree of the position set.
As described in step S003, the location sets are obtained by randomly sampling one location per sample, and by continuously sampling a large number of location sets are obtained, e.g., collecting
Position sets are collected, the spectral reference degree of each position set is calculated, and the spectral reference degree with the maximum degree is obtained
And combining the position sets into a set, reconstructing the Raman spectrum of each sample according to the Raman shifts of all the positions on each sample and in the combined set, wherein the obtained Raman spectrum of each sample can highlight the crystallization rule of the zinc oxide, and noise caused by too many impurities can not be introduced, so that the crystallization rule of the zinc oxide analyzed according to the Raman spectrum is more accurate and credible. Analysis from Raman spectraFor example, the earliest time of appearance of the peak is obtained according to all peaks corresponding to zinc oxide crystals on the obtained raman spectra of all samples, and the temperature and the electric field intensity for enabling the zinc oxide to crystallize fastest can be obtained.
It should be noted that: the precedence order of the above embodiments of the present invention is only for description, and does not represent the merits of the embodiments. And that specific embodiments have been described above. In addition, the processes depicted in the accompanying figures do not necessarily require the particular order shown, or sequential order, to achieve desirable results. In some embodiments, multitasking and parallel processing may also be possible or may be advantageous.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A method for spectroscopic analysis of zinc oxide, said method comprising the steps of:
acquiring zinc oxide samples prepared under different electric field strengths and different temperatures, acquiring Raman shifts of different positions on each sample by using a Raman spectrum detector, constructing a Raman spectrum of each sample according to the Raman shifts of all the positions on each sample, clustering peaks on the Raman spectra of all the samples to acquire all peak types, specifically:
performing Fourier transform on the Raman spectrum to obtain the frequency and the intensity of all signals contained in the Raman spectrum, setting the intensity of the signals with the frequency smaller than a threshold value to be zero, then performing inverse Fourier transform on all the signals to obtain a first Raman spectrum, regarding all peaks contained in the first Raman spectrum as all peaks on the Raman spectrum, clustering all the peaks with overlapped parts into one class on the Raman spectrum of all the samples, and obtaining each class in all the classes as a peak class;
randomly obtaining a position from each sample, wherein all the positions obtained from all the samples form a position set, and obtaining the spectral reference degree of the position set according to the peak category and the Raman shifts of all the positions in the position set, specifically:
for each position in the position set, acquiring all peaks on the Raman spectrum of the sample corresponding to each position, further acquiring a peak where the Raman shift of each position is located, namely the peak of each position, taking the Raman shift corresponding to the peak of each position as the reference Raman shift of each position, performing weighted summation on absolute values of differences between the Raman shifts of all positions in the position set and the reference Raman shifts of all positions, and taking the reciprocal of the obtained result as the spectral reference degree of the position set;
acquiring position sets with the maximum spectrum reference degree and the preset number, combining the position sets with the preset number into a set, reconstructing the Raman spectrum of each sample according to the Raman shifts of all the positions on each sample and in the combined set, and analyzing the zinc oxide.
2. The method for spectroscopic analysis of zinc oxide according to claim 1 wherein the step of obtaining the weight for each position in the weighted sum comprises:
combining the peak value and the width of each peak into a feature vector of each peak, acquiring all comparison peaks of the peaks at each position, acquiring the mean value of Euclidean distances between the feature vector of each peak at each position and the feature vectors of all comparison peaks, and taking the mean value as the weight of each position.
3. The method for spectroscopic analysis of zinc oxide according to claim 1 wherein said step of obtaining all control peaks for each peak position comprises:
obtaining the wave crest category to which the wave crest at each position belongs, and obtaining the temperature and the electric field intensity of a sample corresponding to each wave crest in the wave crest categories during preparation;
in the peak category, if one peak corresponds to a temperature larger than the temperature corresponding to the peak at each position and has the smallest difference, the peak is taken as a comparison peak of the peaks at each position; if one peak corresponds to a temperature smaller than the temperature corresponding to the peak at each position and has the smallest difference, the peak is taken as a comparison peak of the peak at each position; if the corresponding electric field intensity of one peak is larger than that of the peak at each position and the difference is minimum, the peak is taken as a comparison peak of the peak at each position; if the corresponding electric field intensity of one peak is smaller than that of the peak at each position and the difference is minimum, the peak is taken as a comparison peak of the peak at each position;
and then all the comparison wave crests of the wave crests at each position are obtained through comparison and judgment.
4. The method of claim 1, wherein the Raman spectrum is indicative of the Raman intensities of the sample at different Raman shifts.
5. A spectroscopic analysis system for zinc oxide comprising a processor and a memory, the processor being configured to process instructions stored in the memory to implement a spectroscopic analysis method for zinc oxide as set forth in any one of claims 1 to 4.
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| WO2010027098A1 (en) * | 2008-09-04 | 2010-03-11 | 国立大学法人 熊本大学 | Process for producing zinc oxide nanoparticles, and zinc oxide nanoparticles |
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| JP2015101493A (en) * | 2013-11-22 | 2015-06-04 | 宇部興産株式会社 | Conductive zinc oxide powder and method for producing the same |
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