CN111198116A - Target detection method - Google Patents
Target detection method Download PDFInfo
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- CN111198116A CN111198116A CN201811382625.3A CN201811382625A CN111198116A CN 111198116 A CN111198116 A CN 111198116A CN 201811382625 A CN201811382625 A CN 201811382625A CN 111198116 A CN111198116 A CN 111198116A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
A target detection method comprises the following steps: providing a target material sample; providing a detection corrosive liquid and a reference corrosive liquid; dissolving the target sample in the detection corrosion solution, wherein the metal part in the metal target is completely dissolved, but the non-metal particles in the metal target are not dissolved in the detection corrosion solution; the method comprises the steps of accurately detecting the particle size, the quantity and the distribution of microparticles in liquid by adopting a liquid microparticle technology, enabling a reference corrosive liquid and a detection corrosive liquid to meet a microparticle technology detection condition by a dilution means, detecting the microparticle content of the reference corrosive liquid and the detection corrosive liquid, and accurately calculating the microparticle content of a provided target sample by taking the microparticle content in the reference corrosive liquid as a reference, so that a basis for judging the performance of the target sample can be provided.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a target detection method.
Background
After the preparation process of the sputtering target is completed, the performance of the target needs to be detected, because the purity of the target is an important basis for representing the quality of the target.
According to researches, when the target material is used, the alarm that the Particle (micro Particle) of the high-purity metal target material is too high occurs in the using process, the wafer defect is caused by the too high Particle in the target material, and the yield is reduced. The Particle in the target material is mainly caused by the fact that non-metal particles are contained in the metal target material. Therefore, the use performance of the target can be effectively judged by detecting the quantity and the particle size distribution of the non-metal particles in the material. The common scheme in the prior art is to melt a target material by using strong acid, filter the melted acid solution by using filter paper, and finally observe the residual on the filter paper. However, the method can only subjectively judge the amount of residues by naked eyes, cannot quantify the amount of residues, and cannot accurately judge the service performance of the target material.
Therefore, a method for detecting the amount of non-metallic particles in the target material more accurately is needed.
Disclosure of Invention
The invention solves the problem that the content of the non-metal microparticles in the metal target material cannot be accurately judged.
In order to solve the above problems, the present invention provides a target detection method, including: providing a target material sample; providing a detection corrosive liquid and a reference corrosive liquid; putting the target sample into the detection corrosive liquid for dissolving; diluting the detection corrosive liquid dissolved with the target sample and the reference corrosive liquid by the same times; detecting the parameters of the micro-particles in the detection corrosive liquid and the reference corrosive liquid by adopting a liquid micro-particle technology; and comparing the parameters of the micro-particles in the detected corrosive liquid with the parameters of the micro-particles in the reference corrosive liquid to obtain specific values of the parameters of the micro-particles in the target material sample.
Optionally, the microparticle parameter comprises a content of non-metallic microparticles.
Optionally, the target sample is a copper target, a copper alloy target, or an aluminum alloy target.
Optionally, the detection etching solution and the reference etching solution are nitric acid, sulfuric acid or hydrofluoric acid.
Optionally, the detection etching solution and the reference etching solution are mixed solutions composed of the nitric acid, the sulfuric acid or the hydrofluoric acid.
Optionally, before the target sample is placed in the detection corrosive liquid for dissolution, the method further includes: and pre-pickling the target material sample.
Optionally, the target material sample after pre-pickling is washed with deionized water and then weighed.
Optionally, the volumes of the detection corrosive liquid and the reference corrosive liquid are equal.
Optionally, the volumes of the detection corrosive liquid and the reference corrosive liquid are 20ml to 60 ml.
Optionally, the detection corrosive liquid and the reference corrosive liquid are diluted by 10-40 times.
Optionally, the detection corrosion solution and the reference corrosion solution are diluted by 10 times.
Compared with the prior art, the technical scheme of the invention has the following advantages:
dissolving the target material sample in the detection corrosive liquid, wherein the metal target material is completely dissolved, but the non-metal particles in the metal target material are not dissolved in the detection corrosive liquid; and diluting the reference corrosive liquid and the solution in the detection corrosive liquid by the same times, wherein the purpose of dilution is to ensure that the concentration of the solution can meet the accurate detection of a detection instrument in the liquid microparticle technology. The liquid microparticle technology can accurately detect the particle size, the quantity and the distribution of microparticles in liquid through various optical instrument combinations, so that the content of microparticles in a reference corrosive liquid and the content of microparticles in the detected corrosive liquid are respectively detected, and the content of microparticles in the reference corrosive liquid is subtracted from the content of microparticles in the detected corrosive liquid by taking the content of microparticles in the reference corrosive liquid as a reference through comparison, so that the content of microparticles in the provided target sample can be accurately calculated.
In an alternative, before the target sample is put into the detection corrosive liquid for dissolution, the method further comprises the following steps: and pre-pickling the target material sample. Because the target sample to be subjected to sample preparation or detection is metal, generally copper metal, the metal target is very easily oxidized by air under a normal state, and an oxide film is formed on the surface of the metal target or impurities are generated on the surface of the metal target; after the target sample is pre-pickled, oxides or impurities on the surface of the target sample can be washed away, the pure target sample can be exposed, and data obtained by sample preparation or detection of the pure target sample is more real and reasonable.
In an alternative scheme, the target material sample after pre-pickling is washed by deionized water and then weighed. Impurities possibly remain on the surface of the target sample after the sample is pre-pickled, and deionized water is used for cleaning, so that the surface of the target sample is cleaner, and new impurity interference is not introduced into the deionized water. The target sample is cleaned and then weighed, so that the mass of the dissolved sample can be known, and the content of the microparticles in the target sample with the weight can be calculated conveniently and accurately.
Drawings
Fig. 1 is a flowchart of a target detection method according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a sampling process of the detection method according to an embodiment;
FIG. 3 is a schematic diagram illustrating an etching solution provided during a sample preparation process according to an embodiment of the detection method;
FIG. 4 is a schematic diagram illustrating pre-pickling performed during sample preparation by the detection method according to an embodiment;
FIG. 5 is a schematic diagram of a corresponding dissolved sample during sample preparation according to one embodiment of the detection method;
fig. 6 is a schematic diagram of a detection solution correspondingly prepared in a sample preparation process of the detection method according to an embodiment.
Detailed Description
As can be seen from the background art, in the prior art, the amount of the residue can be only roughly judged, and cannot be quantified, and the use performance of the target material cannot be accurately judged.
Analysis shows that in the prior art, after a target to be determined is dissolved by a corrosive liquid, a filter screen is used for filtering the melted liquid, and the amount of residues on the filter screen is judged by naked eyes, so that the method is only limited to roughly estimate the performance of the target.
In order to solve the problems, the invention provides a method for detecting a target, wherein a target sample is dissolved in the detection corrosive liquid, a metal part in the metal target is completely dissolved, but non-metal particles in the metal target are not dissolved in the detection corrosive liquid; the particle size, the quantity and the distribution of microparticles in liquid can be accurately detected through various optical instrument combinations by adopting a liquid microparticle technology, so that the reference corrosive liquid and the detection corrosive liquid meet the microparticle technology detection condition through a dilution means, the microparticle content of the reference corrosive liquid and the detection corrosive liquid is detected, the microparticle content in the reference corrosive liquid is used as a reference, and the microparticle content in the reference corrosive liquid is subtracted from the microparticle content in the detection corrosive liquid, so that the microparticle content in the provided target sample can be accurately calculated.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Referring to fig. 1, a flowchart of a target detection method according to an embodiment of the present invention is shown, and fig. 2 to 6 are schematic diagrams of steps corresponding to a sample preparation process of the detection method according to an embodiment of the present invention.
Step S1 is executed to provide a target sample.
In this embodiment, with continued reference to fig. 2, a copper target 100 is provided, wherein the copper target 100 is a target to be evaluated. Turning a proper amount of copper wires 101 on the surface of the copper target 100 by using a tool 200 to serve as a target sample to be detected, preferably turning 8g-15g of the copper wires 101, wherein the copper wires 101 are more convenient to dissolve in a later sample preparation process, the less the copper wires 101 are detected in the detection process, the more the liquid to be detected is prepared, and the more the copper wires 101 exceed 15g, the less the copper wires are detected, the dissolution is facilitated, and the sample preparation time is too long; the turned copper wire is not less than 8g, and multiple sample preparation liquids can be prepared as required to facilitate data comparison.
In other embodiments, the target sample may be other metal targets, such as copper alloy targets, aluminum alloy targets.
Step S2 is executed to provide an etching solution.
In this embodiment, a detection etching solution and a reference etching solution are provided. The detection corrosive liquid and the reference corrosive liquid are the same in solution and volume, so that the detection corrosive liquid and the reference corrosive liquid are beneficial to more conveniently comparing detection results in the later step. It should be noted that, the container containing the detection corrosive liquid and the reference corrosive liquid is cleaned by deionized water before containing the corrosive liquid, so that there is no impurity interference, and the precision of the final detection result is improved.
In this embodiment, the detection etching solution and the reference etching solution are nitric acid solutions, and the concentrations of the nitric acid solutions are suitable for chemical reaction with the sample, that is, the concentrations of the nitric acid solutions are suitable for dissolving the copper wire 101. In this embodiment, the analytically pure concentrated nitric acid with the highest purity in GB/T626 is used, and analytically pure means that the concentrated nitric acid has a very high content of main components, a high purity, and very low interfering impurities, and is suitable for industrial analysis and chemical experiments. In other embodiments, the corrosive liquid is sulfuric acid, the concentration of which is suitable for dissolving the sample.
In other embodiments, the etching solution is a mixture of sulfuric acid and nitric acid, and the mixture is adapted to dissolve the sample. The detection etching solution and the reference etching solution may be any of nitric acid, sulfuric acid, and hydrofluoric acid, or may be a mixture of part or all of the nitric acid, sulfuric acid, and hydrofluoric acid, so as to dissolve the sample.
In this embodiment, with reference to fig. 3, the preparation process of the reference corrosion solution and the detection corrosion solution is as follows: providing the first container 10 and the second container 20 respectively, adding 30ml of the nitric acid solution into the first container 20 and the second container 20, and diluting the solutions by one time with deionized water respectively. In this case, the solution in the first container 10 is used as a reference etching solution, and the solution in the second container 20 is used as a detection etching solution.
In other embodiments, the reference etching solution and the liquid in the detection etching solution are diluted by one time for 20ml of the nitric acid solution. It should be noted that the amount of the nitric acid solution has no essential influence, and particularly, depending on the concentration and the degree of reaction with the target material, too much nitric acid solution is wasted, and too little nitric acid solution is insufficiently dissolved in the sample. Preferably, the nitric acid solution is added in an amount of 20m to 60ml for dilution, and the reference etching solution and the detection etching solution are more preferably prepared.
When other acids are used to prepare the detection etching solution and the reference etching solution, the dilution factor required for the other acids may be 1 or other factors.
Step S3 is performed to pre-acid wash the sample.
In this example, the target sample was pre-pickled. The pre-pickling is that the target sample to be subjected to sample preparation or detection is metal, generally copper metal, the metal target is very easily oxidized by air in a normal state, and an oxide film is formed on the surface of the metal target or impurities are on the surface of the metal target; after the target sample is pre-pickled, oxides or impurities on the surface of the target sample can be washed away, the pure target sample can be exposed, and data obtained by sample preparation or detection of the pure target sample is more real and reasonable.
In this embodiment, a pre-pickling solution is provided, and the pre-pickling solution is the same as the reference etching solution or the detection etching solution. Specifically, referring to fig. 4, a pre-pickling container 30 is provided, the nitric acid solution is added to the pre-pickling container 30 and diluted by one time with deionized water, and the target material sample, that is, the copper wire 101, is placed in the pre-pickling container 30 for pre-pickling. The pre-pickling solution is the same solution as the reference etching solution or the detection etching solution in order to avoid the introduction of different impurities.
In this example, the sample after the pre-pickling was washed with deionized water, dried by a blower, and then weighed. Impurities possibly remain on the surface of the target sample after the sample is pre-pickled, deionized water is used for cleaning, the surface of the target sample is cleaner, new impurity interference is not introduced into the deionized water, the target sample is weighed after being cleaned, the mass of the target sample can be known, and the content of the microparticles in the target sample with the weight can be calculated conveniently.
In other embodiments, the target sample after the pre-pickling is washed with high-purity distilled water, so that the surface of the target sample is free from interference of other impurities.
Step S4 is executed to prepare a sample.
In this embodiment, with reference to fig. 5, the target sample subjected to the step S13 is weighed for use, or a fixed gram of the target sample is taken out; and quantifying the target sample so as to accurately calculate the ratio of the insoluble particles in the target at a later stage. Weighing 4g of the copper wire 101 in the embodiment of the weighed target sample, and placing the weighed copper wire into the detection corrosion solution for reaction, so that no solid copper wire exists in the detection corrosion solution. In this case, referring to fig. 6, the solution in the reference etching solution and the solution in the detection etching solution are diluted by the same factor, and for convenience of description, the reference etching solution and the detection etching solution after dilution are referred to as a first sample preparation solution 11 and a second sample preparation solution 21, respectively.
In this embodiment, the dilution times of the reference corrosive solution and the detection corrosive solution are 10 to 30 times, so that the prepared first sample preparation solution 11 and the second sample preparation solution 21 meet the detection threshold of a later detection instrument.
In other embodiments, the target sample after the step S3 is directly weighed and recorded in grams for use. And weighing the target sample by proper gram, wherein the preferable range is 3g-6g, and no matter how many grams of the target sample is weighed for preparing the solution, the weighed target sample can be ensured to be completely reacted with the detection corrosion solution. And special attention is paid to the dilution factor so that the finally obtained sample preparation can meet the detection of the instrument.
It should be noted that any of the above manufacturing steps need to be performed in a clean room, so as to prevent the prepared sample preparation solution from being interfered by any impurities, and ensure accurate and effective results.
Step S5 is executed to perform detection.
In this embodiment, a liquid microparticle technology is provided, which combines various optical instruments to accurately detect the particle size, the number, and the distribution of microparticles in a liquid, so that the obtained first sample preparation liquid 11 and second sample preparation liquid 21 are respectively tested to respectively detect the content of microparticles in the first sample preparation liquid 11 and the second sample preparation liquid 21, and when the liquid microparticle detection technology is applied to microparticle detection of a target, the situation that the diameter of microparticles is very fine can also be detected, and according to the existing liquid microparticle technology, the diameter accuracy of detected insoluble microparticles can reach 0.5 um.
In this embodiment, the weighed content of the microparticles in the sample can be accurately calculated by taking the content of the microparticles in the first sample preparation liquid 11 as a reference, that is, the content of the microparticles in the reference etching liquid as a reference and subtracting the content of the microparticles in the reference etching liquid from the content of the microparticles in the second sample preparation liquid 21.
By the method provided by the invention, the microparticle content of the target can be further judged, so that the quality of the target can be more accurately judged, and the target can be more reasonably applied according to the quality of the target.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (11)
1. A method for detecting a target material, comprising:
providing a target material sample;
providing a detection corrosive liquid and a reference corrosive liquid;
putting the target sample into the detection corrosive liquid for dissolving;
diluting the detection corrosive liquid dissolved with the target sample and the reference corrosive liquid by the same times;
detecting the parameters of the micro-particles in the detection corrosive liquid and the reference corrosive liquid by adopting a liquid micro-particle technology;
and comparing the parameters of the micro-particles in the detected corrosive liquid with the parameters of the micro-particles in the reference corrosive liquid to obtain specific values of the parameters of the micro-particles in the target material sample.
2. The method for detecting a target according to claim 1, wherein the microparticle parameter comprises a content of non-metallic microparticles.
3. The method for detecting a target according to claim 1, wherein the target sample is a copper target, a copper alloy target, or an aluminum alloy target.
4. The method for detecting a target according to claim 1, wherein the detection etching solution and the reference etching solution are nitric acid, sulfuric acid, or hydrofluoric acid.
5. The method for detecting a target according to claim 4, wherein the detection etching solution and the reference etching solution are mixed solutions of the nitric acid, the sulfuric acid, or the hydrofluoric acid.
6. The method for detecting a target according to claim 1, wherein before the target sample is dissolved in the detection etchant, the method further comprises: and pre-pickling the target material sample.
7. The method for detecting a target according to claim 6, wherein the target sample after the pre-pickling is washed with deionized water and weighed.
8. The method for detecting a target according to claim 1, wherein the volumes of the detection etching liquid and the reference etching liquid are equal.
9. The method for detecting a target according to claim 8, wherein the volumes of the detection etching solution and the reference etching solution are 20ml to 60 ml.
10. The method for detecting a target according to claim 1, wherein the detection etching solution and the reference etching solution are diluted 10 to 40 times.
11. The method for detecting a target according to claim 10, wherein the detection etching solution and the reference etching solution are diluted by a factor of 10.
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Cited By (3)
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| CN111751254A (en) * | 2020-07-13 | 2020-10-09 | 宁波江丰电子材料股份有限公司 | Method for testing granularity of high-purity aluminum alloy sample |
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| CN113310903A (en) * | 2021-05-27 | 2021-08-27 | 新疆大全新能源股份有限公司 | Method for measuring content of micro silicon powder in polycrystalline silicon material |
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| CN113310903A (en) * | 2021-05-27 | 2021-08-27 | 新疆大全新能源股份有限公司 | Method for measuring content of micro silicon powder in polycrystalline silicon material |
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