阅读说明：本技术 一种零部件表面污染物组分的非破坏性检测方法 (Nondestructive detection method for pollutant components on surface of part ) 是由 李文阁 贺贤汉 侯晓晨 张正伟 蒋立峰 于 2020-12-25 设计创作，主要内容包括：本发明涉及检测技术领域。一种零部件表面污染物组分的非破坏性检测方法,包括如下步骤：步骤一,双面导电胶带固定；将扫描电子显微镜的样品台上铺设双面导电胶带；步骤二,样品台取样；撕除双面导电胶带上的保护条,将待测的零部件表面区域粘附在样品台上的双面导电胶上；步骤三,样品台密封保存；将样品台取下并放入洁净的样品台管中并固定,将样品台管密封；步骤四,对异物区域进行EDX图谱采集；从样品台管中取下样品台并放入扫描电子显微镜的样品舱中,利用扫描电子显微镜观察双面导电胶上粘附的异物,并用能谱仪对异物区域进行EDX图谱采集；步骤五：对EDX谱图进行元素定性和半定量分析,得到零部件表面物质的元素组成。(The invention relates to the technical field of detection. A non-destructive detection method for pollutant components on the surface of a part comprises the following steps: fixing a double-sided conductive adhesive tape; laying a double-sided conductive adhesive tape on a sample table of a scanning electron microscope; step two, sampling by a sample stage; tearing off the protective strip on the double-sided conductive adhesive tape, and adhering the surface area of the part to be tested on the double-sided conductive adhesive on the sample table; step three, the sample stage is sealed and stored; taking down the sample stage, placing the sample stage into a clean sample stage tube, fixing the sample stage tube, and sealing the sample stage tube; step four, carrying out EDX map collection on the foreign body area; taking the sample platform from the sample platform pipe and placing the sample platform into a sample cabin of a scanning electron microscope, observing foreign matters adhered to the double-sided conductive adhesive by using the scanning electron microscope, and carrying out EDX (electronic discharge X) spectrum acquisition on a foreign matter area by using an energy spectrometer; step five: and carrying out element qualitative and semi-quantitative analysis on the EDX spectrogram to obtain the element composition of the surface substance of the part.)

1. A method for non-destructive testing of contaminant components on the surface of a component, comprising the steps of:

fixing a double-sided conductive adhesive tape;

laying a double-sided conductive adhesive tape on a sample table of a scanning electron microscope;

step two, sampling by a sample stage;

tearing off the protective strip on the double-sided conductive adhesive tape, and adhering the surface area of the part to be tested on the double-sided conductive adhesive on the sample table;

step three, the sample stage is sealed and stored;

taking down the sample stage, placing the sample stage into a clean sample stage tube, fixing the sample stage tube, and sealing the sample stage tube;

step four, carrying out EDX map collection on the foreign body area;

taking the sample platform from the sample platform pipe and placing the sample platform into a sample cabin of a scanning electron microscope, observing foreign matters adhered to the double-sided conductive adhesive by using the scanning electron microscope, and carrying out EDX (electronic discharge X) spectrum acquisition on a foreign matter area by using an energy spectrometer arranged on the scanning electron microscope;

step five: and carrying out element qualitative and semi-quantitative analysis on the EDX spectrogram to obtain the element composition of the surface substance of the part.

2. The method of claim 1, wherein the method comprises the steps of: in the fifth step, the atomic number of the element is 5 to 92.

3. The method of claim 1, wherein the method comprises the steps of: and in the second step, taking down the sample table after the sample table and the surface area of the part to be detected are adhered for two minutes.

4. The method of claim 1, wherein the method comprises the steps of: the sample platform is an internal thread sample platform, and the internal thread sample platform threaded connection has a threaded rod.

5. The method of claim 1, wherein the method comprises the steps of: the sample table is a nail-shaped sample table;

the nail-shaped sample table comprises a table body and an upright post, and the table body is fixedly connected with the upright post.

6. The method of claim 1, wherein the method comprises the steps of: the double-sided conductive adhesive tape is a double-sided carbon conductive adhesive tape, and the substrate of the adhesive tape is an insulating non-woven fabric or an aluminum foil.

7. The method of claim 1, wherein the method comprises the steps of: and step five, the acquisition time of the EDX spectrogram is not less than 30 seconds.

8. The method of claim 1, wherein the method comprises the steps of: the foreign matter adhered to the double-sided conductive adhesive tape is a substance adhered from the surface of the part when the double-sided conductive adhesive tape is in contact with the surface of the part, is usually granular or film-shaped, and can be clearly distinguished from the double-sided conductive adhesive in a scanning electron microscope photo.

9. The method of claim 1, wherein the method comprises the steps of: in the fourth step, the method for observing the foreign matters adhered on the conductive adhesive by using the scanning electron microscope is to set the accelerating voltage of the scanning electron microscope at 15KV and adjust the magnification at 1000-1500 times;

moving the sample table in the shape of the Chinese character 'ji' to search for foreign matters;

the shiny particles in the visual field were found and identified as foreign bodies.

10. The method of claim 1, wherein the method comprises the steps of: the method is suitable for detecting surface pollutants of the alumina ceramic ring component or the cavity component with the yttria coating.

Technical Field

The invention relates to the technical field of detection, in particular to a method for detecting pollutant components.

Background

In the precision manufacturing process of semiconductor and display panel, the parts of key manufacturing equipment (such as photoetching equipment, etching equipment and film deposition equipment) are polluted by particles in the long-term use process or chemically react with process materials (such as special gas) to form a surface pollution layer, and the surface pollution layer needs to be cleaned and regenerated for reuse. The detection of the pollutant substance components on the surface of the part can help develop a more targeted cleaning and regeneration process, effectively remove the surface pollutants and reduce the loss of the part. Moreover, the analysis of the pollutant components on the surface of the part can provide important support data for the failure analysis of the part, and is beneficial to searching failure reasons.

The size of the parts of the semiconductor manufacturing equipment is often large and the shape is different, and general chemical component analysis instruments (such as a scanning electron microscope, an X-ray fluorescence spectrometer and an atomic emission direct-reading spectrometer) cannot directly observe and analyze the contaminated area of the parts due to the size of the sample chamber, and often need to perform destructive processing such as cutting on the samples. The handheld X-ray fluorescence spectrometer can analyze components of substances on the surface of a part, but cannot detect light elements such as B, C, N, O and F, and has limitation on the detection range of pollutant components.

The invention patent with application number '201610042487.9' discloses a method for rapidly detecting contaminants on the surface of an object. The method prepares a surface enhanced Raman substrate consisting of gold, silver or copper nanoparticles and a flexible polymer, attaches the substrate to the surface of a measured object, and then detects the object by using a handheld Raman spectrometer. Although this method can perform nondestructive surface contamination testing on parts, the contaminants detected by this method often need to be sufficiently responsive to raman spectroscopy. Since the raman spectrum is a molecular spectrum, this method cannot detect metal contaminants having no molecular structure.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a nondestructive detection method for pollutant components on the surface of a part, which aims to solve at least one technical problem.

In order to achieve the above object, the present invention provides a method for non-destructive detection of contaminant components on a surface of a component, comprising the steps of:

fixing a double-sided conductive adhesive tape;

laying a double-sided conductive adhesive tape on a sample table of a scanning electron microscope;

step two, sampling by a sample stage;

tearing off the protective strip on the double-sided conductive adhesive tape, and adhering the surface area of the part to be tested on the double-sided conductive adhesive on the sample table;

step three, the sample stage is sealed and stored;

taking down the sample stage, placing the sample stage into a clean sample stage tube, fixing the sample stage tube, and sealing the sample stage tube;

step four, carrying out EDX map collection on the foreign body area;

taking the sample platform from the sample platform pipe and placing the sample platform into a sample cabin of a scanning electron microscope, observing foreign matters adhered to the double-sided conductive adhesive by using the scanning electron microscope, and carrying out EDX (electronic discharge X) spectrum acquisition on a foreign matter area by using an energy spectrometer arranged on the scanning electron microscope;

step five: and carrying out element qualitative and semi-quantitative analysis on the EDX spectrogram to obtain the element composition of the surface substance of the part.

Further preferably, in step five, the atomic number of the element is 5 to 92.

Further preferably, in the second step, after the sample stage is attached to the surface area of the component to be tested for two minutes, the sample stage is removed.

Further preferably, the sample stage is an internally threaded sample stage, and the internally threaded sample stage is in threaded connection with a threaded rod.

Further preferably, the sample stage is a nail-shaped sample stage;

the nail-shaped sample table comprises a table body and an upright post, and the table body is fixedly connected with the upright post.

Further preferably, the double-sided conductive adhesive tape is a double-sided carbon conductive adhesive tape, and the substrate of the adhesive tape is an insulating non-woven fabric or an aluminum foil.

Further preferably, in the fifth step, the acquisition time of the EDX spectrogram is not less than 30 seconds.

Further preferably, the foreign matter adhered to the double-sided conductive adhesive tape is a substance which is adhered to and removed from the surface of the component when the double-sided conductive adhesive tape is in contact with the surface of the component, is usually in a granular shape or a film shape, and can be clearly distinguished from the double-sided conductive adhesive in a scanning electron microscope picture.

Further preferably, in the fourth step, the method for observing the foreign matters adhered on the conductive adhesive by using the scanning electron microscope is to set the accelerating voltage of the scanning electron microscope at 15KV and adjust the magnification at 1000-;

moving the sample table in the shape of the Chinese character 'ji' to search for foreign matters;

the shiny particles in the visual field were found and identified as foreign bodies.

Further preferably, the method is suitable for the detection of surface contamination of an alumina ceramic ring component or a chamber component with an yttria coating.

Drawings

FIG. 1 is a flow chart of the present invention;

FIG. 2 is a schematic structural diagram of a sample stage according to the present invention;

FIG. 3 is a schematic view of a sample stage according to the present invention;

FIG. 4 is an SEM photograph of the foreign matter of embodiment 1.

FIG. 5 is an EDX spectrum of the foreign substance of example 1.

FIG. 6 is an SEM photograph of the foreign matter of embodiment 2.

FIG. 7 is an EDX spectrum of the foreign substance of example 2.

Detailed Description

The invention is further described below with reference to the accompanying drawings.

Referring to fig. 1, a method for non-destructive detection of contaminant components on a surface of a component includes the steps of:

fixing a double-sided conductive adhesive tape;

laying a double-sided conductive adhesive tape on a sample table of a scanning electron microscope;

step two, sampling by a sample stage;

tearing off the protective strip on the double-sided conductive adhesive tape, and adhering the surface area of the part to be tested on the double-sided conductive adhesive on the sample table;

step three, the sample stage is sealed and stored;

taking down the sample stage, placing the sample stage into a clean sample stage tube, fixing the sample stage tube, and sealing the sample stage tube;

step four, carrying out EDX map collection on the foreign body area;

taking the sample platform from the sample platform pipe and placing the sample platform into a sample cabin of a scanning electron microscope, observing foreign matters adhered to the double-sided conductive adhesive by using the scanning electron microscope, and carrying out EDX (electronic discharge X) spectrum acquisition on a foreign matter area by using an energy spectrometer arranged on the scanning electron microscope;

step five: and carrying out element qualitative and semi-quantitative analysis on the EDX spectrogram to obtain the element composition of the surface substance of the part.

Referring to fig. 3, the sample stage 2 is an internal thread sample stage, and the internal thread sample stage is in threaded connection with a threaded rod.

Referring to fig. 2, the sample stage 2 is a nail-shaped sample stage; the nail-shaped sample table comprises a table body and an upright post, and the table body is fixedly connected with the upright post.

Detailed description of the preferred embodiment 1

The method is suitable for surface pollution analysis of the alumina ceramic ring component.

A nondestructive detection method for pollutant components on the surface of a part specifically comprises the following steps:

the method comprises the following steps: paving a double-sided conductive adhesive tape on a sample table of a scanning electron microscope; the bottom of the sample table is provided with internal threads;

the diameter of the sample table is 30mm, and the height of the sample table is 6 mm.

The conductive adhesive is a double-sided conductive carbon adhesive tape with the width of 8mm, and the adhesive tape substrate is a high-purity aluminum foil.

Step two: and connecting the threaded rod with the internal thread plane sample table, removing the protective strip on the conductive adhesive tape, and adhering the front surface of the sample table adhered with the conductive adhesive tape to the surface area of the ceramic ring component to be detected by holding the threaded rod with hands.

Step three: and after the sample table and the surface of the alumina ceramic ring are adhered for one minute, taking down the sample table, quickly putting into a clean sample table tube and fixing by utilizing threads.

Step four: the sample stage tube is taken into a clean room laboratory of 100000 grades or more. And taking out the sample table from the sample table tube, and mounting the sample table on the adaptive sample table base. And putting the sample platform and the base into a sample cabin of the scanning electron microscope. The electron acceleration voltage of the scanning electron microscope was set to 15kV, and the detection signal was a backscattered electron signal. Adjusting the magnification to 1500 times, moving the sample stage in the shape of Chinese character Ji, observing the foreign matters adhered on the conductive adhesive, and carrying out EDX atlas collection on the foreign matter region by using an energy spectrometer arranged on a scanning electron microscope. The EDX spectrogram acquisition time is 40 seconds.

Step five: and carrying out element qualitative and semi-quantitative analysis on the EDX spectrogram to obtain the element composition of the surface substance of the part.

Fig. 4 is an SEM photograph of the foreign material particles of embodiment 1, and fig. 5 is an EDX spectrum of the foreign material particles of embodiment 1.

The EDX spectrum of the foreign particles of specific example 1 (region 1 in fig. 4) was qualitatively analyzed, and the result showed that the foreign particles were mainly composed of C, O, Al, Fe, Ni and Cr. Among them, the C element is greatly interfered by the signal of the conductive tape component, and Al may be derived from the component on the alumina ceramic substrate.

Semi-quantitative analysis was performed on the spectrum shown in fig. 5, and the atomic percentages of the O, Al, Fe, Ni, and Cr elements were 21.9%, 6.6%, 41.6%, 5.3%, and 9.3%, respectively. From the results of atomic percentages, it can be concluded that the main components of the foreign matter are Fe, Ni, and Cr metals, and that they contain small amounts of oxides of Fe, Ni, and Cr.

Specific example 2

Surface contamination analysis of chamber components having yttria coatings.

A method for non-destructive testing of contaminant components on the surface of a component, comprising the steps of:

the method comprises the following steps: paving a double-sided conductive adhesive tape on a sample table of a scanning electron microscope; the bottom of the sample table is provided with internal threads;

the diameter of the sample table is 15mm, and the height of the sample table is 6 mm. The conductive adhesive is a double-sided conductive carbon adhesive tape with the width of 8mm, and the adhesive tape substrate is a high-purity aluminum foil.

Step two: and connecting the threaded rod with the internal thread plane sample table, removing the protective strip on the conductive adhesive tape, and adhering the front surface of the sample table adhered with the conductive adhesive tape to the surface area of the cavity component to be detected.

Step three: and after the surface adhesion time of the sample table and the cavity component reaches two minutes, taking down the sample table, quickly putting into a clean sample table tube, and fixing by using threads.

Step four: the sample stage tube is taken into a clean room laboratory of 100000 grades or more. And taking out the sample table from the sample table tube, and mounting the sample table on the adaptive sample table base. And putting the sample platform and the base into a sample cabin of a scanning electron microscope, and observing the foreign matters adhered to the conductive adhesive by using the scanning electron microscope. The accelerating voltage of the scanning electron microscope is set to be 15KV, and the magnification is adjusted to be 1000 times. The sample stage is moved in the shape of the Chinese character 'ji' to search for foreign matters. The shiny particles in the visual field were found and confirmed as foreign matter, as shown in fig. 6. The region of the foreign matter (region 1 in fig. 6) was subjected to EDX spectrum acquisition by an energy spectrometer mounted on a scanning electron microscope, and the spectrum was analyzed. The EDX spectrogram has the acquisition time of 60 seconds.

Step five: and carrying out element qualitative and semi-quantitative analysis on the EDX spectrogram to obtain the element composition of the surface substance of the part.

The EDX spectrogram in FIG. 7 is subjected to qualitative and semi-quantitative element analysis, signal interference of the C component of the conductive adhesive is eliminated, and the substance on the upper surface of the coating of the cavity part mainly comprises O, F, Al and Y. And performing semi-quantitative analysis on the content of each element in the spectrogram to obtain O, F, Al and Y element with the atomic percentage content of 18.1%, 7.0%, 2.7% and 6.5% respectively. Considering that the coating layer is Y₂O₃Thus, it can be concluded that the principal component of the contaminant is YF formed by the reaction of the surface component of the coating with the F-containing semiconductor etching process gas₃And has a low content ofAmount of Al₂O₃Or AlF₃。

The foregoing is only a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.