WO2023165148A1

WO2023165148A1 - High throughput xps equipment, detection method, and application

Info

Publication number: WO2023165148A1
Application number: PCT/CN2022/128961
Authority: WO
Inventors: 董红; 罗锋; 冯泽
Original assignee: 南开大学
Priority date: 2022-03-04
Filing date: 2022-11-01
Publication date: 2023-09-07
Also published as: CN114594121B; CN114594121A

Abstract

High throughput XPS equipment, a detection method, and an application. A sample (3) is irradiated by using a high beam current x-ray source (1), an annular energy analyzer (7) collects photoelectrons excited from the sample (3), test data is converted into an XPS spectrogram by means of a data system (10), and a detection result is obtained on the basis of XPS spectrum analysis. Also, the circular frustrum-shaped high beam current x-ray source (1) is provided, a circular frustrum-shaped anode target (21) side face grazing angle light emergent direction has a strongest distribution, x-rays (2) are brought to a single point via a monochromator (24), the brightness of the high beam current x-ray source (1) is greatly improved, and the number of photoelectrons emitted in the sample (3) can also be increased. In addition, the annular energy analyzer (7) greatly increases electron collection efficiency without a detection angle being altered. The high throughput XPS equipment can be used in industrial production lines such as for integrated circuits, and is used during production for rapidly detecting surface information such as a valence band, an energy band, and a surface component of a material.

Description

A high-throughput XPS device, detection method and application

technical field

The invention belongs to the technical field of XPS equipment, and in particular relates to a high-throughput XPS equipment, a detection method and an application.

Background technique

Currently, in the modern semiconductor industrial process, a large number of measurements are required. Under advanced manufacturing processes, optical technology cannot meet the requirements. X-ray photoelectron spectroscopy (XPS) is used to non-destructively characterize the film composition, valence state, thickness, energy band and other information.

The basic principle of XPS technology detection is that monochromatic X-rays irradiate the sample to generate photoelectrons, which pass through the energy analyzer, then reach the electron detector, and finally convert them into XPS spectra through the data processing system. Since the electron current is detected by the electron spectrometer and it is very weak, the electron multiplier is often used to increase the number of electrons and measure the number of electrons. Among them, in order to improve the data acquisition ability and reduce the acquisition time, modern energy spectrometers mostly use multi-channel electronic detectors.

However, the current use of XPS technology for sample detection is inefficient. The main reason is that the XPS technology takes too long to detect a single point. In the detection process of the traditional XPS system, limited by the brightness of X-rays, the number of outgoing photoelectrons is small, and then the XPS spectrum with poor signal-to-noise ratio is obtained. Therefore, multiple scans are required to improve the accuracy of XPS spectra. This greatly improves the detection time of samples. Therefore, the current XPS detection on the production line adopts the random inspection mode.

Increasing the number of photoelectrons collected per unit time is the core of improving the detection efficiency, which is related to the brightness of the X-ray source and the efficiency of the energy analyzer.

Problems and defectives existing in the prior art:

The anode of conventional X-ray light sources is planar and cannot be focused, resulting in divergent light intensity distribution;

Conventional XPS energy analyzers use a single point with a small solid angle to collect photoelectrons for detection, but the ability to collect photoelectrons is weak and the detection efficiency is low.

The difficulty of solving the above problems and defects is:

(1) How to focus X-rays.

(2) How to increase the electron collection solid angle as much as possible while ensuring that the electron incident direction on the analyzer is at the same angle as the sample surface.

The significance of solving the above problems and defects is:

Significantly increase the efficiency of photoelectron detection, and XPS is widely used in the detection and measurement of wafers and other workpieces in production lines such as the semiconductor industry.

Contents of the invention

Aiming at the problems existing in the prior art, the present invention provides a high-throughput XPS device, detection method and application.

The present invention is achieved in this way, a high-throughput XPS detection method, the high-throughput XPS detection method includes: X-rays are emitted from the side of the truncated anode, the strongest distribution is the grazing emission angle, and converged at one point/through a single The colorimeter concentrates X-rays at one point and irradiates the sample; the photoelectron beam excited from the sample is collected by a ring energy analyzer, which ensures that the angle of the outgoing photoelectron is the same as that of the energy analyzer.

Further, the high-throughput XPS detection method specifically includes: step 1, the filament is grounded and heated, the electrons are accelerated by the target at high pressure to generate high-energy electrons, and the high-energy electrons bombard the surface of the target to generate X-rays;

Step 2: X-rays emerge from the surface of the anode target, and the X-rays emitted from the side of the truncated anode at a grazing angle have the strongest distribution, and the strongest distributed rays will converge at one point/converge the X-rays at one point through the monochromator; the test process starts with the sample height adjustment so that the surfaces intersect at this point;

Step 3, using a ring energy analyzer to collect photoelectrons excited from the sample, the minimum step size can be set to 0.05eV;

Step 4, using the data analysis system to visualize the collected data and transform it into an XPS spectrum, and obtain the detection result based on the XPS spectrum.

Further, before the high-throughput XPS equipment detects samples, the system work function is calibrated;

Use the molecular pump (combinable ion pump) unit to keep the cavity at ultra-high vacuum, put the sample to be tested into the fast sampling chamber, and when the vacuum reaches 10 ^-7 mbar, send the sample into the test chamber through the transmission device ; Detect the position of the sample through the observation window and camera, and adjust the height of the sample through the sample stage system.

Further, when the high-energy electrons bombard the anode target in the second step to generate X-rays, an accelerating voltage is applied between the filament and the metal anode target, the filament is grounded, and the anode target is connected to a positive voltage. What needs to be done: the inside of the circular truncated anode target is provided with a cooling water circulation channel to conduct away the heat generated by the anode target.

Further, the detection results obtained based on the XPS spectrum in the step 4 include: distinguishing the material composition and valence state; detecting the thickness of the film and the change of the work function; analyzing the interface dipole; determining the difference between each point in the sample sex.

A high-throughput XPS device of the present invention includes: the frustum-shaped anode side grazing emits high-intensity X-rays, converges at one point/converges X-rays at one point through a monochromator, and irradiates the sample;

Ring energy analyzer, including ring input lens, ring analyzer, ring electron multiplier tube, pulse preamplifier, receiver;

Further, the annular input lens is used to collect photoelectrons excited from the sample and focus them on the entrance of the analyzer, while adjusting the kinetic energy of the photoelectrons to match the pass energy of the annular analyzer;

Further, the annular electron multiplier tube is located at the outlet of the annular analyzer to amplify the photoelectron current;

Further, the electronic pulse is detected by the pulse preamplifier and converted into an optical signal;

Further, the built-in high-speed comparison circuit in the pulse preamplifier is used to filter out system noise;

Further, the signal is transmitted to the receiving end through an optical fiber;

Further, mu metal is arranged between the annular input lens and the annular analyzer to prevent the magnetic field from penetrating into the analyzer;

Further, the circular energy analyzer mode can select constant analyzer energy mode (CAE) and constant reduction ratio mode (CRR).

Further, the receiving end will output digital pulse or analog signal, convert the test data into XPS spectrum through the data system, compare the corresponding data between different sample points, analyze the composition, peak position and difference between samples, based on the XPS Spectrum to get detection results.

Further, the high-throughput XPS equipment also includes: fast sampling chamber, transmission device, real-time monitoring device, vacuum system and sample stage system;

The fast sample injection chamber is used to shorten the sample injection and sampling time in the XPS test process;

The transport device is used for transporting samples;

The vacuum system is used to evacuate the test chamber and the fast sampling chamber;

The sample stage system ensures that the samples are at the same test height to ensure constant brightness of the high-beam X-ray source;

Further, the high-beam X-ray adopts a frustum-focused X-ray source, or adopts a fine array structure X-ray source;

The high-beam X-ray source adopts a conical focused X-ray source, including:

Filament, truncated anode target, monochromator and shielding system;

Filament, which can adopt a spiral structure;

The frustum-shaped anode target is used to adjust the position of the X-ray focus point by adjusting the shape of the frustum of the cone and the corresponding cone vertex angle; the frustum-shaped anode target is connected to a positive voltage; it is equipped with a water cooling system for setting outside the frustum-shaped anode target Or the internal cooling water circulation channel uses Cu as a heat-conducting material to conduct away the heat generated by the target in a circulating manner;

Monochromator: used to monochromatize the divergent X-rays while focusing the X-rays on one point;

Shielding system, consisting of a shielding cover and a filter window, is used to block the electrons generated by the filament.

Further, the filament is placed on the outside of the truncated anode target; the shielding system is located on the outermost side of the high beam current X-ray source;

The filament, the truncated anode target, the monochromator and the shielding system are placed coaxially;

The filament is annular or helical;

The target material of the truncated conical anode target is one of Al, Mg, Ti, Cr, Fe, Cu, Ag, Mo, Au and Pt;

The shielding system includes: the filter window is located in front of the X-ray source, and the aluminum foil material can be used to prevent the electrons generated by the filament from interfering with the XPS spectral line signal, and at the same time to avoid the heating of the sample caused by the X-ray source, and to block the radiation generated by the filament. Impurities to avoid target contamination;

The shielding case is grounded;

There are multiple observation windows; cameras are arranged outside the multiple observation windows for collecting the position of the sample and other information in real time.

In combination with all the above-mentioned technical solutions, the advantages and positive effects of the present invention are:

The present invention provides a fast-scanning XPS device equipped with a circular platform focused high-beam X-ray source and an annular energy analyzer; it greatly improves the number of photoelectrons emitted in the sample and the number of photoelectrons collected by the energy analyzer, and greatly reduces single-point detection time.

Conventional XPS energy analyzers use a fixed single-point small solid angle to collect photoelectrons for detection, and the collection efficiency of photoelectrons is low. The energy analyzer of the present invention adopts a ring structure, which can be collected to the greatest extent under the condition that the angle between the outgoing photoelectron and the sample surface remains unchanged, which improves the detection efficiency of the XPS device, that is, a relatively high-resolution XPS can be obtained by scanning in a short time The spectrum accelerates the acquisition of chemical information on the sample surface/interface; improves the detection rate and reduces the detection cost.

The frustum-focused high-beam current X-ray source of the present invention: the X-rays emitted from the side of the frustum-shaped anode have the strongest distribution and converge at one point/converge the X-rays at one point through the monochromator, which greatly improves the brightness of the X-ray source . In turn, the number of emitted photoelectrons in the sample can be increased. Furthermore, it is also possible to further increase the power of the X-ray source by making a fine array structure on the anode target of the frustum-focused X-ray source, such as inserting a metal array on the diamond film wall through micro-nano processing technology.

The frustum-shaped structure adopted by the high-beam current X-ray source of the present invention is provided with a cooling water circulation channel outside or inside; the low energy density of the electron beam can generate high-brightness X-rays, which improves the service life of the anode and reduces maintenance costs.

Description of drawings

Fig. 1 is a schematic structural diagram of a fast-scanning XPS device equipped with a circular table-focused high-flux X-ray generator and a ring energy analyzer provided by an embodiment of the present invention.

Fig. 2 is a schematic structural diagram of a non-monochromatic frustoconical focusing type high-beam current X-ray source provided by an embodiment of the present invention.

Fig. 3 is a schematic structural diagram of a monochromatic frustoconical focusing type high-beam current X-ray source provided by an embodiment of the present invention.

Fig. 4 is a flow chart of the high-throughput XPS detection method provided by the embodiment of the present invention.

In the figure: 1. High beam current X-ray source; 2. X-ray; 3. Sample; 4. Sample stage system; 5. Ring input lens; 6. Photoelectron beam; 7. Ring energy analyzer; 8. Flange ;9. Wiring and water cooling; 10. Data system; 11. Observation window; 12. Camera; 13. Transmission device; 14. Ion pump; 15. Molecular pump and mechanical pump unit; 16. Vacuum gauge; 17. Rapid sampling chamber; 18. air breaking valve; 19. heating mantle; 20. filament; 21. round platform anode target; 22. shielding cover; 23. filter window; 24. monochromator.

Detailed ways

In order to make the object, technical solution and advantages of the present invention more clear, the present invention will be further described in detail below in conjunction with the examples. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.

Aiming at the problems existing in the prior art, the present invention provides a high-throughput XPS device. The present invention will be described in detail below with reference to the accompanying drawings.

The present invention innovatively adopts a circular energy analyzer, while the conventional XPS energy analyzer adopts a fixed small solid angle to collect photoelectrons for detection—the sampling range is small, and the photoelectron collection efficiency is low. Through the ring design, the solid angle of the collected photoelectrons is greatly increased under the condition that the angle between the outgoing photoelectrons and the sample surface remains unchanged, thereby improving the test efficiency.

Furthermore, the present invention innovatively provides a frustum-focused high-beam X-ray source. The X-rays are emitted from the side of the truncated anode and converged at one point/the X-rays are concentrated at one point by the monochromator, which greatly improves the brightness of the X-ray source, thereby increasing the number of photoelectrons emitted from the sample.

An embodiment of the present invention provides a high-throughput XPS detection method, including: using a high-beam current X-ray source to irradiate a sample;

The ring energy analyzer collects the photoelectron beam excited from the sample, converts the test data into an XPS spectrum through the data system, and obtains the detection result based on the XPS spectrum.

As shown in Figures 1 to 3, the high-throughput XPS device provided by the embodiment of the present invention includes: a high beam current X-ray source 1, an X-ray 2, a sample 3, a sample stage system 4, an annular input lens 5, and a photoelectron beam 6 , ring energy analyzer 7, flange plate 8, wiring and water cooling 9, data system 10, observation window 11, camera 12, transmission device 13, ion pump 14, molecular pump and mechanical pump group 15, vacuum gauge 16, rapid advance A sample chamber 17, a vent valve 18, a heating jacket 19, a filament 20, a circular truncated anode target 21, a shielding cover 22, a filter window 23, and a monochromator 24.

Among them, the high-beam current X-ray source 1 can adopt the frustum-focused X-ray source provided by the present invention, or other existing high-beam current X-ray sources, such as fine array structure X-ray sources, etc.;

Sample stage system 4, the temperature range of the heatable sample holder is 77-1000K; in-situ heating/cooling can be realized; the sample stage can be moved/rotated freely, and is used to adjust the position of the receiving sample 3 so that when different samples are tested, the high The brightness of the beam X-ray source is constant;

The ring energy analyzer 7 adopts a ring cavity; it is used to collect the photoelectrons generated by excitation to the greatest extent;

The data system 10 is used to convert test data into XPS spectra; at the same time, it is used to compare the corresponding data between different sample points, analyze the composition, peak position and other differences between samples, and quickly visualize the comparative analysis results;

Rapid sampling chamber 17, used to shorten the sampling and sampling time in the XPS testing process;

The transport device 13 is used to transport the sample;

The vacuum system is made up of a molecular pump and a mechanical pump group 15 and a vacuum gauge 16; the molecular pump and the mechanical pump group include: a mechanical pump, a molecular pump and an ion pump 14; the vacuum gauge 16 includes a resistance gauge and an ion gauge;

Heating mantle 19, the chamber heating mantle is used for baking the chamber when the XPS device restores the system after the chamber is opened, and removes water vapor in the chamber.

In a preferred embodiment, the high beam current X-ray source 1 includes:

Filament 20, frustum-shaped anode target 21 and shielding system, monochromator 24 are optional devices;

Filament 20, the filament can adopt a spiral structure;

The frustum-shaped anode target 21 is used to adjust the position of the X-ray focus point by adjusting the shape of the frustum of the cone and the corresponding cone vertex angle; there is a water cooling system in it, which is used to circulate the cooling water on the outside or inside of the frustum-shaped anode target 21. The heat generated by the target is conducted away by means of the target, and the inner wall of the target can be solid copper, silver, aluminum and other metals or alloys;

The shielding system is composed of a shielding cover 22 and a filter window 23; it is used to block the electrons generated by the filament and at the same time to isolate the heat of the X-ray source.

The filament 20 provided by the embodiment of the present invention is placed on the outside of the conical anode target 21; the shielding system is located on the outermost side of the high beam current X-ray source 1;

The filament 20, the truncated anode target 21 and the shielding system are placed coaxially.

The target material of the truncated conical anode target 21 provided in the embodiment of the present invention can be Al, Mg, Ti, Cr, Fe, Cu, Ag, Mo, Au, Pt.

The shielding system provided by the embodiment of the present invention includes:

The filter window 23 is located in front of the X-ray source 1, and can be made of aluminum foil to prevent the electrons generated by the filament from interfering with the XPS spectral line signal, and to avoid heating of the sample caused by the X-ray source, to block impurities generated by the filament, and to avoid target material pollution;

The shield case 22 is grounded.

The high-throughput XPS device provided by the embodiment of the present invention is provided with multiple observation windows 11; a camera 12 is provided outside the observation windows 11 for real-time collection of the position of the sample and other information.

The technical solution of the present invention will be further described below in conjunction with the working principle.

When the system is restored after the XPS cavity is opened, the test chamber is pumped to an ultra-high vacuum atmosphere by means of the molecular pump and mechanical pump group 15 and the ion pump 14, combined with the heating sleeve 19 and baking. During baking, the vacuum of the chamber should not exceed 10 ^-5 mbar. The vacuum of the test chamber is read by a vacuum gauge 16 . A vent valve 18 is also installed on the chamber;

The sample to be tested is put into the rapid sampling chamber 17, and when the vacuum is drawn to 10 ⁻⁷ mbar or below, the sample is sent into the testing chamber through the transmission device 13 . During this period, the position of the sample can be observed through the observation window 11 and the camera 12 . The position of the sample is adjusted through the sample stage system 4 to ensure that the brightness of the high beam current X-ray source 1 is constant when different samples are tested.

Before testing the samples, the work function of the system is calibrated by Ni or Au spectral lines. Taking the frustoconical focusing type high-beam current X-ray source provided by the present invention as an example, the filament 20 is grounded and heated, and the electrons are accelerated through the target to form high-energy electrons, and the high-energy electrons bombard the anode target to generate X-rays 2. The anode target is a conical truncated target. That is, on the basis of the accumulation of grazing emission angles, the X-rays can be collected at the apex of the cone extended by the frustum of the cone (non-monochromatization)/further concentrated by the monochromator 24 at one point (ie, the position where the sample is placed during the test). The photoelectron beam 6 excited from the sample is collected by the annular input lens 5 at the front end of the annular energy analyzer 7 .

The wiring and water cooling 9 are connected to the heating jacket 19 through the flange 8; the wiring and water cooling 9 are connected to the data system 10 through wiring;

The test data is converted into an XPS spectrogram by the data system 10, and a detection result is obtained based on the XPS spectrogram.

The technical solution of the present invention will be further described below in conjunction with the high-throughput XPS detection method.

As shown in Figure 4, the high-throughput XPS detection method provided by the embodiment of the present invention includes:

S101, the filament is grounded and heated, the electrons are accelerated by the target at high voltage to produce high-energy electrons, and the high-energy electrons bombard the surface of the target to generate X-rays;

S102, X-rays emerge from the surface of the anode target, and the X-rays emitted from the side of the truncated anode at a grazing angle have the strongest distribution, so the strongest distributed rays will converge at one point/converge the X-rays at one point through the monochromator. The test process first adjusts the height of the sample so that the surface intersects at this point;

S103, using a ring energy analyzer to collect photoelectrons excited from the sample;

S104, converting the test data into an XPS spectrum through the data system, and obtaining a detection result based on the XPS spectrum.

In a preferred embodiment, the system work function is calibrated before the high-throughput XPS device detects the sample;

The high-throughput XPS chamber is kept in an ultra-high vacuum by a molecular pump and a mechanical pump group (an ion pump can be added), and the vacuum degree of the test chamber is tested by a vacuum gauge; When the vacuum reaches 10 ^-7 mbar, the sample is sent into the test chamber through the transmission device; the position of the sample is detected through the observation window and the camera, and the position of the sample is adjusted through the sample stage system.

In a preferred embodiment, when the high-energy electrons bombard the anode target in the step S102 to generate X-rays, an accelerating voltage is applied between the filament and the metal anode target, the filament is grounded, and the anode target is connected to a positive voltage. The accelerating voltage value is set to be 10 times the energy of the characteristic X-ray source. What needs to be done: the inside of the circular truncated anode target is provided with a cooling water circulation channel; at the same time, the shielding system is used to block the electrons generated by the filament.

In a preferred embodiment, the detection results obtained based on the XPS spectrum in step S104 include: distinguishing material components and valence states; detecting changes in film thickness and work function; analyzing interface dipoles; difference between points.

The technical solutions of the present invention will be further described below in conjunction with specific embodiments.

Example 1:

A fast-scanning high-throughput XPS device, including a high-beam current X-ray source, a ring energy analyzer, a data system, a fast sampling chamber, a transmission device, a real-time detection device, a vacuum system, a sample stage system and a reserved flange interface .

The ring-shaped electron energy analyzer has a high collection rate of photoelectrons generated by excitation, greatly improves the signal strength of photoelectrons, and avoids time waste caused by repeated scanning (reducing the signal-to-noise ratio).

The high-beam current X-ray source can be a frusto-conical focused high-beam X-ray source, and its structure is as follows: it includes a filament, a conical anode target and a shielding system. It is characterized in that: the fixed position of the truncated conical anode target includes a water cooling system, and the water cooling system adopts a circulation method; the filament is located outside the anode target; and the shielding system is located on the outermost side.

The filament, the truncated anode target, the monochromator and the shielding system are placed coaxially.

The filament can adopt a ring or helical structure.

The shielding system is further characterized in that: the shielding system is composed of a shielding case and a filter window. The filter window is located in front of the X-ray source and is usually made of aluminum foil; the shielding cover is grounded.

The filter window is further characterized in that: the filter window is used to prevent electrons generated by the filament from interfering with XPS spectral line signals; to avoid heating of the sample caused by the X-ray source; to avoid contamination of the target.

The high-beam current X-ray source can also use a fine array anode X-ray source, etc.;

The fast scanning XPS equipment is equipped with a fast sampling chamber, which is used to shorten the sampling (sampling) time in the XPS test process.

The rapid sample injection chamber can be pre-injected, and when the vacuum is pumped to 10 ^-7 mbar or below, it enters the test chamber through the transmission device;

The fast scanning XPS equipment is equipped with a transmission device, which can transmit samples before the fast sampling chamber and the test chamber, and the transmission device can be controlled by software (also manually operated by a joystick);

The sample platform system can be heated to control the temperature range of 77-1000K; it can realize in-situ temperature rise/cool; The brightness of the ray source is constant;

The vacuum system is composed of a molecular pump, a mechanical pump group and a vacuum meter, and the vacuum pump system is composed of a mechanical pump, a molecular pump and an ion pump.

The high-throughput XPS device is equipped with multiple observation windows and can be equipped with a camera to realize the regulation and real-time detection of the sample position;

The high-throughput XPS equipment is equipped with a vent valve, which is convenient for daily maintenance and repair of the equipment;

When the test chamber returns to the ultra-high vacuum atmosphere after opening the cavity, the chamber is often heated by baking or other means; this will slightly change the accuracy of detecting the kinetic energy of photoelectrons and the photon energy of emitted X-rays to a certain extent, often The impact of these factors on the test is often attributed to the system work function. Therefore, the work function of the system needs to be recalibrated after each cavity opening.

The data system carried by the XPS device can simply compare the corresponding data between different sample points, so as to easily analyze the differences in components, peak positions, etc. between samples;

Example 2:

A high-throughput XPS device suitable for rapid detection of device process defects in industrial production.

The fast-scanning XPS device is equipped with a high beam current X-ray source and a ring energy analyzer.

The high-beam X-ray source can use a conical focused high-beam X-ray source: the filament is grounded and heated, and the electrons are accelerated by the target at high pressure to generate high-energy electrons. It emits and converges at one point, which greatly improves the brightness of the X-ray source. Adjust the height of the sample at this point during the test.

The frustum-shaped anode target is equipped with a cooling deionized water circulation channel inside, which can generate high-brightness X-rays through the electron beam with a lower energy density, avoiding the problem of target melting caused by high temperature, so that it can work continuously , thereby improving the detection efficiency.

The shielding system is placed on the outermost side to prevent the electrons generated by the filament from interfering with the XPS line signal; to avoid heating of the sample caused by the X-ray source; to block impurities generated by the filament to avoid contamination of the target.

The annular energy analyzer is characterized in that it adopts an annular cavity design, which increases the number of incident photoelectrons and has a high photoelectron collection rate.

After the photoelectrons are selected by the ring electron energy analyzer, they are converted into XPS spectra by the data analysis system.

The method provided by the embodiment of the present invention is aimed at the functional requirements, and the method of data conversion processing is: distinguishing the material composition and valence state; detecting the thickness of the film and the change of the work function; analyzing the charging effect and the interface dipole; difference between the points.

The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Anyone familiar with the technical field within the technical scope disclosed in the present invention, whoever is within the spirit and principles of the present invention Any modifications, equivalent replacements and improvements made within shall fall within the protection scope of the present invention.

Claims

A high-throughput XPS device, characterized in that the high-throughput XPS device includes: a high-beam X-ray source, the X-rays are emitted from the side of the truncated anode, and the X-rays are converged at one point by a monochromator to perform sample irradiation;

The ring energy analyzer is used to collect the photoelectron beam excited from the sample, convert the test data into an XPS spectrum through the data system, compare the corresponding data between different sample points, and analyze the composition, peak position and difference between samples, Obtain a detection result based on the XPS spectrogram;

The high-throughput XPS equipment also includes: a fast sampling chamber, a transmission device, a real-time monitoring device, a vacuum system and a sample platform system;

The fast sample injection chamber is used to shorten the sample injection and sampling time in the XPS test process;

The transport device is used for transporting samples;

The vacuum system is used to evacuate the test chamber and the fast sampling chamber;

The sample stage system is used to adjust the height of the receiving sample so that the brightness of the high-beam X-ray source is constant when different samples are tested;

The high-beam X-ray adopts a frustum-focused X-ray source;

The high-beam X-ray source adopts a frusto-conical focused X-ray source including:

Filament, truncated anode target, monochromator and shielding system;

The filament adopts a spiral structure;

The frustum-shaped anode target is used to adjust the position of the X-ray focus point by adjusting the shape of the frustum-shaped anode; way to conduct away the heat generated by the target, and the cooling water is deionized water;

Monochromator: used to monochromatize the divergent X-rays while focusing the X-rays on one point;

Shielding system, consisting of a shielding cover and a filter window, is used to prevent high temperature outgassing pollution of the filament.
The high-flux XPS device according to claim 1, wherein the filament is placed on the outside of the frusto-conical anode target; the shielding system is located on the outermost side of the high-beam X-ray source;

The filament, the truncated anode target, the monochromator and the shielding system are placed coaxially;

The target material of the truncated conical anode target is one of Al, Mg, Ti, Cr, Fe, Cu, Ag, Mo, Au and Pt;

The filter window is located in front of the X-ray source and is made of thin aluminum foil;

The shielding case is grounded;

There are multiple observation windows; cameras are arranged outside the multiple observation windows for real-time collection of position information of the sample.
A high-throughput XPS detection method based on the high-throughput XPS device described in any one of claims 1 to 2, characterized in that the high-throughput XPS detection method comprises: using a high-beam current X-ray source to irradiate the sample The ring energy analyzer collects the photoelectrons excited from the sample, and tests the electronic signal strengths of different kinetic energies within the set acquisition time to obtain XPS spectrograms, and obtains detection results based on the XPS spectrograms;

The high-throughput XPS detection method specifically includes:

Step 1, the filament is grounded and heated, and the electrons are accelerated by the high voltage of the anode target to bombard the surface of the target to generate X-rays;

Step 2: X-rays emerge from the surface of the anode target, and the X-rays emitted from the side of the frustum-shaped anode at a grazing angle have the strongest distribution, and the strongest distribution rays will converge the X-rays at one point through the monochromator; The surfaces intersect at this point;

Step 3, using a ring energy analyzer to collect photoelectrons excited from the sample, the minimum step size can be set to 0.05eV;

Step 4, convert the electron intensity and corresponding kinetic energy collected at different kinetic energies into an XPS spectrum, and use the relationship of binding energy=X-ray energy-electron kinetic energy-analyzer work function to convert the electronic signal intensity and binding energy The function image of , the function image is the XPS spectrum;

The high-throughput XPS equipment needs to go through the recovery operation and the calibration of the system work function before returning to use after the maintenance of the open cavity;

After calibrating the work function of the system, the high-throughput XPS chamber is kept at an ultra-high vacuum by a molecular pump and a mechanical pump group; the sample to be tested is placed in the rapid sampling chamber, and when the vacuum reaches 10 The sample is sent into the test chamber through the transmission device; the position of the sample is detected through the observation window and the camera, and the position of the sample is adjusted through the sample stage system;

In said step one, when high-energy electrons bombard the anode target to generate X-rays, an accelerating voltage is applied between the filament and the metal anode target, the filament is grounded, and the anode target is connected to a positive high voltage; moreover, a cooling water circulation channel is provided inside the circular frustum-shaped anode target, At the same time, the shielding system is used to block the electrons generated by the filament.
The high-throughput XPS detection method according to claim 3, wherein obtaining the detection result based on the XPS spectrum in the step 4 includes: analyzing the surface composition and valence state of the material; detecting the thickness of the film and the change of the work function ; Analyze the interface dipole; Determine the difference between each point in the sample.