CN112285067A - Method for preparing high-uniformity sample film - Google Patents
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Abstract
A method for preparing a sample film with high uniformity comprises preparing a sample solution with high uniformity and preparing the sample film with high uniformity. The invention sets the volumetric flask into a plurality of areas, monitors the areas one by one, and generally judges the uniformity through the related data of the transmissivity. The invention adopts a mode of photographing the spin-coated sample film and extracting the gray value to judge the uniformity of the film.
Description
Technical Field
The invention relates to the field of sample preparation, in particular to the field of sample film preparation, and more particularly relates to the field of preparation of high-uniformity films.
Background
The sample film preparation has wide application in sample qualitative and quantitative detection, and some elements and devices with the film. In the qualitative and quantitative detection of a sample, the uniformity of the sample has a very important influence on the detection accuracy. In the fabrication of some precision instruments, the uniformity of the thin film also plays a critical role in the performance of the instrument or device. Therefore, how to ensure the uniformity of the sample film has important significance.
The preparation of the film sample usually includes a drop diffusion method, and finally forms a film, and the prerequisite for the uniformity of the film sample obtained by the drop diffusion method is whether the sample in the mixed solution or suspension is completely diffused or not, and is also a key factor influencing the uniformity of the film sample. Meanwhile, since the uniformity of the thin film formed by the dropping diffusion method is not particularly good, another preparation method of the sample thin film, i.e., a spin coating method, is employed. The Shanghai silicon research of the Chinese academy of sciences discloses a spin-coating sample preparation method for total reflection X-ray fluorescence analysis, in which a mixed solution is dropped on a sample carrier to perform spin-coating, and then the sample is subjected to ray fluorescence detection, but how to ensure the uniformity of the spin-coating is not described.
The prior art mentions that the higher the rotation speed, the more uniform the sample film, but the experiment proves that there is no strict such relationship. The smaller the rotation speed, the less the sample droplet is likely to bloom, and the thicker the middle and the thinner the periphery may be, while the larger the rotation speed, the more the opposite is, the droplet is likely to be thrown around, causing the thinner the middle and the thicker the periphery, and even more, the risk of the sample being thrown away. Therefore, the solution or suspension under the same condition needs to be monitored in real time, the rotating speed conforming to the condition is found, and a theoretical basis is provided for large-scale production.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing a high-uniformity sample film, which starts from the homogenization of a raw material solution or a suspension, strictly controls the uniformity of the film coating process and ensures the preparation of the high-uniformity sample film.
The invention specifically realizes a method for detecting and improving the uniformity of solution or suspension, which is characterized by comprising the following steps
S1, adding a sample into a cylindrical volumetric flask, and then fixing the volume with water;
s2, evenly dividing the volumetric flask into n areas along the longitudinal direction;
s3, homogenizing the mixed solution to form a solution or a suspension;
s4, transversely irradiating each area by using laser with the same light intensity, and detecting the transmissivity of each area, namely T1, T2, … and Tn;
s5, calculating the average value of the transmissivity of each area;
s6, calculating the standard deviation of the transmissivity of the n areas
S7, comparing sigma with a first threshold, if sigma is larger than the first threshold, determining that the solution or the suspension is not uniform, and repeating the steps S3-S7; if the sigma is not larger than the second threshold value, the solution or the suspension is qualified, and the subsequent operation can be carried out.
According to the method of the embodiment of the invention, in the step S8, if σ is not greater than the first threshold, the step S8 is executed; s8 is that d is calculatedi,j＝|Ti-Ti+j1, |, where i ═ 1,2, …, n-1; j is 1,2, …, n-1, and i + j is less than or equal to n; if d is presenti,jIf the value is larger than the second threshold value, the solution or the suspension is determined to be not uniform, and the steps S3-S8 are required to be repeated; if d isi,jIf the value is not greater than the second threshold value, the solution or the suspension is qualified, and the subsequent operation can be carried out.
According to the method of the embodiment of the present invention, in step S1, a dispersant is further added.
According to the method of the embodiment of the present invention, in the step S3, the method of homogenizing the mixed solution includes one or both of stirring and ultrasonic processing.
The homogeneity of the solution or suspension is a prerequisite for the detection and preparation of the film of the sample, under which the film sample prepared has the same sample content as the solution or suspension, without any great deviations. The method of the invention provides a method for detecting the homogeneity of the solution or the suspension, and provides a treatment mode under the condition of insufficient homogeneity. For some more demanding products, more conditions are required to be able to use the second embodiment of the invention. After obtaining a solution or suspension meeting the requirements, the preparation of the sample film can be carried out.
A method for detecting and optimizing the uniformity of a sample film comprises the following steps:
(a) moving a certain amount of the solution or the suspension liquid under the condition of qualified judgment, and adding the certain amount of the solution or the suspension liquid onto the sample bearing plate;
(b) placing the sample bearing plate attached with the solution or the suspension on a spin coating instrument, starting the spin coating instrument, and uniformly coating the sample on the sample bearing plate at a rotating speed N1;
(c) starting an illuminating device arranged obliquely above the spin coating instrument to illuminate the sample film, starting a CCD scanning camera arranged right above the sample film, and scanning the sample film from left to right to obtain an integral image of the sample film;
(d) converting the whole image of the sample film into a gray image, and enhancing the gray contrast of the whole image by using a method combining smooth filtering and morphological transformation;
(e) searching a region matched with the target object in the gray image as an interested region by adopting a target matching positioning algorithm, dividing the interested region into m multiplied by m regions, and obtaining the gray value G of each regionk,lWherein k is 1,2, …, n; 1,2, …, n; calculating the average value of the integral gray;
(f) calculate gkl＝|Gk,l- |/× 100%, and the calculation result is compared with a third threshold value, if g is presentklIf the rotation speed is larger than the third threshold value, increasing the rotation speed by deltaN, and repeating the steps (a) - (f); if g isklIf the value is not greater than the third threshold value, the sample film is determined to be uniformly spin-coated, and the next operation can be carried out.
According to the method of the embodiment of the invention, the initial rotating speed N1 and the iterative compensation deltaN are determined by empirically estimated relation between the thickness of the sample film and the rotating speed.
According to the method provided by the embodiment of the invention, the thickness of the sample thin film is monitored while the uniformity of the sample thin film is optimized, and the relation between the thickness of the thin film and the rotating speed is established, wherein the thickness of the sample thin film is represented by an image gray value, namely the relation between the image gray value and the rotating speed is established; the relation between the thickness of the sample film and the image gray value is obtained by training a neural network algorithm in advance.
According to the method provided by the embodiment of the invention, the gray value of the image obtained after iteration is fitted with the corresponding rotating speed, so that the relation between the gray value of the image and the rotating speed is obtained.
The relation between the thickness of the sample film and the rotating speed can be obtained according to the relation between the thickness of the sample film and the image gray value and the relation between the image gray value and the rotating speed, and the relation can be used as the basis of the current parameters of the sample film and other thickness conditions. When the uniformity of the sample film is detected or optimized, the thickness of the sample is considered, and the adjustment is carried out within the range of the required thickness of the sample, which needs to be carried out according to the relation between the thickness of the film and the rotating speed.
According to the method provided by the embodiment of the invention, the subsequent operation comprises the preparation of a thin film coating or the detection of the sample content and other properties.
According to the method for detecting the uniformity of the thin film, the determining factor of the third threshold value comprises the thickness of the thin film, and the thickness of the thin film can be characterized as the average value of gray scales. In some component manufacturing processes, there are certain requirements for thickness, which require uniformity adjustment over a range of thicknesses.
The invention relates to a method for preparing a high-uniformity sample film, which is used for preparing a uniform solution or a suspension by adopting the method for improving the uniformity of the solution or the suspension and preparing the high-uniformity sample film by adopting the method for optimizing the uniformity of the film.
Advantageous effects
In the invention, the pursuit of raw material homogenization and the pursuit of film homogenization are carried out to obtain a highly uniform sample film containing quantitative sample substances, and the highly uniform sample film is subsequently detected and applied.
In the prior art, a mixed solution or suspension obtained by dissolving a certain amount of sample has a certain concentration as a whole, but local regions may not be uniform, that is, the concentration of each region is not equal to the whole concentration, so that the uniformity in the preparation process of the solution or suspension needs to be monitored, and a specific means is adopted to obtain a solution or suspension meeting the requirements. The invention sets the volumetric flask into a plurality of areas, monitors the areas one by one, and performs general judgment on uniformity through related data of transmissivity, thus being simple, convenient and accurate.
Meanwhile, certain requirements are also made on the uniformity in the preparation process of the sample film. There is a certain requirement for the uniformity of the sample film in a certain area. The method adopts the mode of photographing the spin-coated sample film and extracting the gray value to judge the uniformity of the film, is simpler and easier than directly measuring the thickness of the film in each area, and ensures the accuracy.
Drawings
FIG. 1 shows a flow chart for performing solution or suspension homogeneity detection and optimization according to the present invention;
FIG. 2 is a schematic diagram illustrating transmittance measurements of different regions of a solution or suspension according to the present invention;
FIG. 3 shows a flow chart of the present invention for sample film uniformity detection and optimization.
Detailed Description
Example 1
The high uniformity of the sample film is ensured, and firstly, the uniformity of the raw material is ensured. The present invention provides a method for detecting and improving the homogeneity of a solution or suspension, which is now described in detail with reference to fig. 1 and 2.
The specific realization mode of the invention for the uniformity of the raw materials is a method for detecting and improving the uniformity of solution or suspension, which is characterized by comprising the following steps
S1, adding a sample into a cylindrical volumetric flask, and then fixing the volume with water;
s2, evenly dividing the volumetric flask into n areas along the longitudinal direction; the division of the zones is linked to the size of the volumetric flask, a preferred embodiment being the division of the volumetric flask into 5-10 sectors.
S3, homogenizing the mixed solution to form a solution or a suspension;
s4, transversely irradiating each area by using laser with the same light intensity, and detecting the transmissivity of each area, namely T1, T2, … and Tn; the monitoring of the transmissivity of each area can be simultaneously detected by adopting a linear array light source and a linear array detector, and the method has the advantages of high efficiency, no time delay and good accuracy.
S5, calculating the average value of the transmissivity of each area;
s6, calculating the standard deviation of the transmissivity of the n areas
S7, comparing sigma with a first threshold, if sigma is larger than the first threshold, determining that the solution or the suspension is not uniform, and repeating the steps S3-S7; if the sigma is not larger than the second threshold value, the solution or the suspension is qualified, and the subsequent operation can be carried out.
According to the method of the embodiment of the invention, in the step S8, if σ is not greater than the first threshold, the step S8 is executed; s8 is that d is calculatedi,j＝|Ti-Ti+j1, |, where i ═ 1,2, …, n-1; j is 1,2, …, n-1, and i + j is less than or equal to n; if d is presenti,jIf the value is larger than the second threshold value, the solution or the suspension is determined to be not uniform, and the steps S3-S8 are required to be repeated; if d isi,jIf the value is not greater than the second threshold value, the solution or the suspension is qualified, and the subsequent operation can be carried out.
According to the method of the embodiment of the present invention, in step S1, a dispersant is further added.
According to the method of the embodiment of the present invention, in the step S3, the method of homogenizing the mixed solution includes one or both of stirring and ultrasonic processing.
The homogeneity of the solution or suspension is a prerequisite for the detection and preparation of the film of the sample, under which the film sample prepared has the same sample content as the solution or suspension, without any great deviations. The method of the invention provides a method for detecting the homogeneity of the solution or the suspension, and provides a treatment mode under the condition of insufficient homogeneity. For some more demanding products, more conditions are required to be able to use the second embodiment of the invention. After obtaining a solution or suspension meeting the requirements, the preparation of the sample film can be carried out.
Example 2
Control of the preparation of the sample film is also important in the case of obtaining a satisfactory solution or suspension. The method for detecting and optimizing the uniformity of a sample film according to the present invention will now be described with reference to fig. 3, which comprises the following steps:
(a) moving a certain amount of the solution or the suspension liquid under the condition of qualified judgment, and adding the certain amount of the solution or the suspension liquid onto the sample bearing plate;
(b) placing the sample bearing plate attached with the solution or the suspension on a spin coating instrument, starting the spin coating instrument, and uniformly coating the sample on the sample bearing plate at a rotating speed N1; the initial rotating speed N1 is estimated from the thickness of the sample film, and the thickness of the obtained sample film can be ensured to meet the requirement.
(c) Starting an illuminating device arranged obliquely above the spin coating instrument to illuminate the sample film, starting a CCD scanning camera arranged right above the sample film, and scanning the sample film from left to right to obtain an integral image of the sample film;
(d) converting the whole image of the sample film into a gray image, and enhancing the gray contrast of the whole image by using a method combining smooth filtering and morphological transformation;
(e) searching a region matched with the target object in the gray image as an interested region by adopting a target matching positioning algorithm, dividing the interested region into m multiplied by m regions, and obtaining the gray value G of each regionk,lWherein k is 1,2, …, n; 1,2, …, n; calculating the average value of the integral gray; the m × m regions may be selected to be 3 × 3, 4 × 4, or more according to the size of the region of interest.
(f) Calculate gkl＝|Gk,l- |/× 100%, and the calculation result is compared with a third threshold value, if g is presentklIf the rotation speed is larger than the third threshold value, increasing the rotation speed by deltaN, and repeating the steps (a) - (f); if g isklIf the value is not greater than the third threshold value, the sample film is determined to be uniformly spin-coated, and the next operation can be carried out.
According to the method of the embodiment of the invention, the initial rotating speed N1 and the iterative compensation deltaN are determined by empirically estimated relation between the thickness of the sample film and the rotating speed.
According to the method provided by the embodiment of the invention, the uniformity of the sample thin film is optimized, meanwhile, the thickness of the sample thin film is monitored, and the relation between the thickness of the thin film and the rotating speed is established, wherein the thickness of the sample thin film is represented by an image gray value, namely the relation between the image gray value and the rotating speed is established; the relation between the thickness of the sample film and the image gray value is obtained by training in advance through a neural network algorithm.
According to the method provided by the embodiment of the invention, the gray value of the image obtained after iteration is fitted with the corresponding rotating speed, so that the relation between the gray value of the image and the rotating speed is obtained.
The relation between the thickness of the sample film and the rotating speed can be obtained according to the relation between the thickness of the sample film and the image gray value and the relation between the image gray value and the rotating speed, and the relation can be used as the basis of the current parameters of the sample film and other thickness conditions. When the uniformity of the sample film is detected or optimized, the thickness of the sample is considered, and the adjustment is carried out within the range of the required thickness of the sample, which needs to be carried out according to the relation between the thickness of the film and the rotating speed.
According to the method of the embodiment of the invention, the subsequent operation comprises preparing a coating or detecting the property of the film.
According to the method for detecting the uniformity of the thin film, the determining factor of the third threshold value comprises the thickness of the thin film, and the thickness of the thin film can be characterized as the average value of gray scales. In some component manufacturing processes, there are certain requirements for thickness, which require uniformity adjustment over a range of thicknesses.
According to the detection method of the film uniformity, sample films with different thicknesses are obtained through a series of rotating speeds, the sample films are obtained through detection of methods in the prior art such as ultrasound, then the image average gray values of the sample films with different thicknesses are obtained through steps T3-T4, and the relation between the image average gray values and the sample film thicknesses is obtained through a partial least square method.
Example 3
According to the method of the embodiment of the invention, the subsequent operation comprises detecting the raw material to be detected. The content of the substance to be detected is detected by the prepared film, so that the operation is simple and easy, but if an accurate result is obtained, the raw materials for preparing the film are uniform, and the sample film is uniform.
Dissolving known amount (10g) of lysozyme protein into buffer solution, then adding the lysozyme protein into a 100ml volumetric flask, adding a small amount of dispersing agent, and fixing the volume with water to obtain standard suspension with the sample content of 10%; when the standard deviation sigma of the transmittance of the final solution is not more than 0.05 or d is not more than 0.04 while monitoring and mixing by the method of example 1, the lysozyme protein suspension is satisfactory, and the film preparation can be carried out.
The lysozyme protein film was prepared and monitored for uniformity using the method of example 2. The lysozyme protein film has a thickness ranging from 30 mu m to 50 mu m, the response of the film to the spectrum is good, and the content of lysozyme protein can be obtained more accurately by adopting a total reflection X-ray fluorescence spectrometry to carry out film detection. As determined by the way of example 2, when 3000r/min is adopted, a relatively uniform sample film can be obtained, the thickness of the sample can reach 34 μm, and gkl is less than the third threshold value by 3%, which meets the requirement. And finally, placing the sample plate carrying the sample film into a total reflection X-ray fluorescence spectrometer for detection to obtain the detection content.
The content of the standard lysozyme suspension with the content of 1%, 2%, 5% and 20% is respectively detected by the same method, and finally, the sample plate bearing the sample film is placed into a total reflection X-ray fluorescence spectrometer for detection, and the results are as follows:
therefore, the method can accurately detect the content of the object to be detected, the error rates of the method are all below 3%, and the accuracy rate of the method gradually increases along with the increase of the content of the object to be detected. Compared with the common detection method, the method has high accuracy.
Example 4
According to the method of the embodiment of the invention, the subsequent operation comprises preparing a coating film on the surface of the device. The energy of the device is also closely related to the uniformity of the thin film. How to ensure the uniformity of the coated film becomes a problem in the art.
In the field of micro-nano manufacturing, a polypropylene film is used as a sacrificial layer, and the uniformity of the polypropylene film directly influences the performance of a device in the manufacturing process of a polypropylene film capacitor. Preparing a polypropylene mixed solution according to requirements, homogenizing the polypropylene mixed solution by adopting a magnetic stirring or ultrasonic mode, monitoring the homogenization degree of the polypropylene mixed solution according to the mode of the embodiment 1, moving the polypropylene mixed solution to a sample to be processed, such as a silicon wafer or a metal foil, then placing the polypropylene mixed solution on a spin coater for thin film processing after the requirement is met, establishing the relation between the gray value and the rotating speed and the relation between the thin film thickness and the gray value while monitoring the thin film uniformity, determining the appropriate thin film thickness, and continuously selecting or continuously adjusting the thin film uniformity within the specified thin film thickness range to obtain a functional device with the optimal performance.
The established relationship between the gray value and the rotating speed and the relationship between the film thickness and the gray value can provide basis for other devices adopting the polypropylene film to prepare, such as the preparation of polypropylene film capacitors with different specifications, the different specifications require different thicknesses of the polypropylene films, the corresponding rotating speed range can be obtained through the two relational expressions, the uniformity is optimized in the rotating speed range, and the requirements of large-scale production can be met.
The above embodiments are merely illustrative of the present invention, and the details in the examples are not to be construed as limiting the scope of the invention.
Claims (9)
1. The method for detecting and improving the uniformity of the solution or the suspension is characterized by comprising the following steps
S1, adding a sample into a cylindrical volumetric flask, and then fixing the volume with water;
s2, dividing the volumetric flask into n areas from top to bottom;
s3, homogenizing the mixed solution to form a solution or a suspension;
s4, transversely irradiating each area by using laser with the same light intensity, and detecting the transmissivity of each area, namely T1, T2, … and Tn;
s5, calculating the average value of the transmissivity of each area
S6, calculating the standard deviation of the transmissivity of the n areas
S7, comparing sigma with a first threshold, if sigma is larger than the first threshold, determining that the solution or the suspension is not uniform, and repeating the steps S3-S7; if the sigma is not larger than the second threshold value, the solution or the suspension is qualified, and the subsequent operation can be carried out.
2. A method according to claim 1, wherein in step S8, if σ is not greater than the first threshold, performing step S8; s8 is that d is calculatedi,j＝|Ti-Ti+j1, |, where i ═ 1,2, …, n-1; j is 1,2, …, n-1, and i + j is less than or equal to n; if d is presenti,jIf the value is larger than the second threshold value, the solution or the suspension is determined to be not uniform, and the steps S3-S8 are required to be repeated; if d isi,jIf the value is not greater than the second threshold value, the solution or the suspension is qualified, and the subsequent operation can be carried out.
3. The method of claim 1 or 2, further comprising adding a dispersant in step S1.
4. The method according to claim 1 or 2, wherein in the step S3, the method for homogenizing the mixed solution includes one or both of stirring and ultrasound.
5. A method for detecting and optimizing the uniformity of a sample film comprises the following steps:
(a) transferring a certain amount of the solution or suspension qualified in the determination of claim 1 or 2, and adding the solution or suspension onto the sample carrier plate;
(b) placing the sample bearing plate attached with the solution or the suspension on a spin coating instrument, starting the spin coating instrument, and uniformly coating the sample on the sample bearing plate at a rotating speed N1;
(c) starting an illuminating device arranged obliquely above the spin coating instrument to illuminate the sample film, starting a CCD scanning camera arranged right above the sample film, and scanning the sample film from left to right to obtain an integral image of the sample film;
(d) converting the whole image of the sample film into a gray image, and enhancing the gray contrast of the whole image by using a method combining smooth filtering and morphological transformation;
(e) searching a region matched with the target object in the gray image as an interested region by adopting a target matching positioning algorithm, dividing the interested region into m multiplied by m regions, and obtaining the gray value G of each regionk,lWherein k is 1,2, …, n; 1,2, …, n; calculating the average value of the integral gray;
(f) calculate gkl＝|Gk,l- |/× 100%, and the calculation result is compared with a third threshold value, if g is presentklIf the rotating speed is larger than the third threshold value, increasing the rotating speed by deltaN, and repeating the steps (a) - (f); if g isklIf the value is not greater than the third threshold value, the sample film is determined to be uniformly spin-coated, and the next operation can be carried out.
6. The method of claim 5, wherein the initial rotation rate N1 and the iterative compensation δ N are determined from empirically estimated relationships between the thickness of the sample film and the rotation rate.
7. The method according to claim 5, wherein the thickness of the sample film is monitored while the uniformity of the sample film is optimized, and a relationship between the thickness of the sample film and the rotation speed is established, wherein the thickness of the sample film is characterized by an image gray value, i.e. the relationship between the image gray value and the rotation speed is established; the relation between the thickness of the sample film and the image gray value is obtained by training a neural network algorithm in advance.
8. The method of claim 7, fitting the image gray scale values obtained after the iteration for a plurality of times to the corresponding rotation speeds to obtain the relationship between the image gray scale values and the rotation speeds.
9. The method of claim 5, wherein the subsequent operation comprises preparing a coating or detecting a property of the film.
A method of preparing a highly uniform sample film by preparing a homogeneous solution or suspension by the method of any one of claims 1 to 4 and preparing a highly uniform film by the method of any one of claims 5 to 9.
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