CN114689634A - Method for measuring polymer sub-layer X photoelectron spectrum by cluster plasma etching - Google Patents
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Abstract
The invention discloses a method for measuring an X photoelectron spectrum of a polymer sub-layer by cluster plasma etching, which mainly utilizes argon ion clusters to bombard the surface of a polymer, peels off dozens of nanometer deep atoms on the surface, then adopts X rays to irradiate the surface of the polymer after being peeled off, generates an X ray photoelectron spectrum and accurately analyzes the element chemical combination state and content of a new interface after being peeled off. The invention combines the cluster plasma etching technology with the X-ray photoelectron spectrum, detects the X-ray photoelectron spectrum at different depth positions of the interface layers of different polymer films of the semiconductor, obtains the element combination state and content, is favorable for exploring the relation between the properties of the polymer semiconductor film and the performances of the photoelectric device, and has wide application prospect in the field of film analysis.
Description
Technical Field
The invention belongs to the field of X-ray photoelectron spectroscopy tests, and particularly relates to a method for measuring an X-ray photoelectron spectroscopy of a polymer sublayer by cluster plasma etching.
Background
Organic thin film transistors are active devices that regulate the conductivity of organic semiconductor thin films by electric fields. Compared with inorganic transistors, organic thin film transistors have the characteristics of light weight, low price, good flexibility and various material types, and have wide application prospects in the aspects of low-cost intelligent tags, electronic paper, sensors and the like.
The core part of the organic field effect transistor is an organic semiconductor material which plays a role in carrier transportation and is the most important component part of the field effect transistor, and the organic semiconductor material can be divided into a small molecular semiconductor material and a high molecular polymer semiconductor material according to molecular weight, wherein the small molecular semiconductor material has a simple structure, is easy to purify and crystallize, and can be subjected to dry deposition in a vacuum coating mode. Compared with small molecular materials, the high molecular polymer semiconductor material is usually in an unfixed state, has poor crystallinity, has better flexibility and tensile property and has wide application prospect.
In the analysis and research of semiconductor polymer films, surface analysis is mostly performed by using an X-ray photoelectron spectroscopy method, but the currently adopted surface analysis method cannot detect the X-ray photoelectron spectroscopy at different depth positions of the interface layers of different polymer films of a semiconductor, so that improvement is needed.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. To this end, it is an object of the present invention to provide a method for measuring the X photoelectron spectrum of a polymer sublayer using cluster plasma etching.
The technical scheme of the invention is as follows: a method for measuring X photoelectron spectrum of a polymer sub-layer by cluster plasma etching is characterized by comprising the following steps:
s1: placing the semiconductor polymer film in a pre-vacuumizing chamber of an X-ray photoelectron spectrometer for vacuumizing;
s2: when the vacuum degree of the pre-vacuum chamber reaches 10-9Feeding the semiconducting polymer film into an analysis chamber in mbar;
s3: the chamber to be analyzed is evacuated to 10-10Mbar, double-clicking software "Advantage", opening a program interface, clicking "Source" to select "X-Ray Gun", selecting X-Ray Gun type as "Mono Anode (XR 6)" monochromatized aluminum target, and selecting a spot size of 500 μm;
s4: clicking 'Miscelllaneous' under a 'Mono 500 μm' program module, adding a sub-program 'Charge compression', selecting 'Flood Gun' to add a double-beam argon ion neutralizing Gun, and 'Mode' to select 'Charge Com Standard' Standard magnetic lens Mode;
s5: adding a point to be tested under a program module of 'Charge Compensation', clicking 'point', selecting 'point' in type, moving a sample, positioning a view field at the center of the sample, adjusting 'Z axis', focusing an optimal view field, clicking 'Read' at 'Position' when a crystal grain in the view field is most clear visually, automatically reading a record by a view field coordinate X, Y, Z, selecting 'Enable Auto Height' at 'Position', automatically seeking Height of equipment in the vicinity of a selected 'Z' value in the subsequent process, and determining a final 'Z' value according to the highest intensity value;
s6: establishing a subprogram under a point module, clicking the Profile, selecting the Depth Profile, and setting parameters in the Profile: "Delay after Etch(s)" in "Etching" is set to xx seconds, meaning that the test starts after xx seconds of stability after each Etching, "Move to Etch position" in "Etching"; "Rotation" selects "None";
s7: the "Ion Gun" Ar Ion Gun parameters are set under the "Depth Profile" module: "Ion Energy" is 4000 eV; selecting a Cluster plasma Mode by the Mode; "Cluster Size" selects "500"; selecting Manual from the Raster Size, inputting a parameter of 5mm, and selecting ten times of the X-Ray spot area according to the selection principle; selecting "Turn gun of fwhen finished";
s8: setting 'Etch Phases' under a 'Depth Profile' module, and setting the first layer etching time to be 30 s; clicking 'Insert' to Insert the second layer, and setting the etching time of the second layer to be 30 s; clicking 'Insert' to Insert a third layer, and setting the etching time of the third layer to be 20 s; clicking 'Insert' to Insert the fourth layer, and setting the etching time of the fourth layer to be 20 s; clicking 'Insert' to Insert a fifth layer, and setting the etching time of the fifth layer as 10 s; clicking 'Insert' to Insert the sixth layer, and setting the etching time of the sixth layer to be 10 s; clicking 'Insert' to Insert the seventh layer, and setting the etching time of the seventh layer to be 10 s; clicking 'Insert' to Insert the eighth layer, and setting the etching time of the eighth layer to be 20 s; clicking 'Insert' to Insert the ninth layer, and setting the etching time of the ninth layer to be 20 s; clicking 'Insert' to Insert the tenth layer, and setting the etching time of the tenth layer to be 30 s;
s9: setting 'Etch Position' under a 'Depth Profile' module, and clicking 'Read Position' in 'Native Coordinates' to Read a coordinate X, Y, Z value corresponding to each layer of etching points;
s10: selecting a Depth profile under a program tree 'experience', clicking 'Spectrum' to select 'Multi Spectrum' to add an element to be tested, and selecting a certain track electron of the element to be tested in 'Insert Multi Spectrum Into experience';
s11: selecting a program tree 'expert', clicking 'Source' to select 'Gun shutdown', and closing an 'electron Gun' and a 'neutralizing Gun' after the program etching and testing operation are set;
s12: and clicking the 'expert Run' program to Run after the program is set.
Preferably, "Etch Phases" is set under the "Depth Profile" module in step S8, and each layer of etching time is set to a different time according to the thickness of each layer of polymer.
Compared with the prior art, the invention has the following beneficial effects:
the method mainly utilizes argon ion clusters to bombard the surface of a polymer, peels off dozens of nanometer deep atoms on the surface, then adopts X rays to irradiate the peeled surface of the polymer, generates an X ray photoelectron spectrum, and accurately analyzes the element chemical combination state and content of a new interface after peeling. The invention combines the cluster plasma etching technology with the X-ray photoelectron spectrum, detects the X-ray photoelectron spectrum at different depth positions of the interface layers of different polymer films of the semiconductor, obtains the element combination state and content, is favorable for exploring the relationship between the properties of the polymer semiconductor film and the performance of the photoelectric device, and has wide application prospect in the field of film analysis.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts:
FIG. 1 is a schematic of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for measuring X-ray photoelectron spectroscopy of a polymer sublayer using cluster plasma etching according to an embodiment of the present invention will be described with reference to fig. 1 of the accompanying drawings, comprising the steps of:
s1: the semiconductor polymer film is placed in a pre-vacuumizing chamber of an X-ray photoelectron spectrometer for vacuumizing, and the X-ray photoelectron spectrometer is a surface analysis technology and is mainly used for representing surface elements and chemical states of materials. The basic principle is that X-rays interact with the surface of a sample, the photoelectric effect is utilized to excite the surface of the sample to emit photoelectrons, namely, X-ray photons with energy h are used to excite electrons on a state energy level, the energy of the emitted photoelectrons is analyzed by a photoelectron spectrometer to obtain data, and a graph of intensity to electron energy, namely an X-ray induced X-ray photoelectron spectrum, is drawn.
EB＝hv-Ek-W
Wherein hv is photon energy; ekIs the kinetic energy of the electron; w is the spectrometer work function.
EBIs the binding energy of an electron, a parameter that is used exclusively in the field of elemental and atomic energy levels to identify an electron.
In an X-ray photoelectron spectrometer, the X-ray source is an X-ray tube using Al or Mg as an anode. Their photon energies are 1486eV and 1254eV, respectively. Filters (or monochromators) are installed to reduce photon energy dispersion. The ion gun is used for sputtering to remove the surface contamination of the sample so as to obtain a clean surface, thereby improving the accuracy of the analysis; alternatively, the sample may be sputter stripped to analyze the composition of the sample at different depths. The sample frame in the sample chamber is provided with a transmission mechanism which can move in the directions of x, y and z which are mutually perpendicular and can rotate along a certain coordinate axis by a certain angle, so that the conditions of different parts of the sample can be observed, analyzed and researched conveniently.
The electron energy analyzer is a key component of the X-ray photoelectron spectrometer and is used for measuring the electron energy distribution and the relative intensities of electrons with different energies, and the electron energy analyzer and the electron multiplier system are completely controlled by a microcomputer.
S2: when the vacuum degree of the pre-vacuum chamber reaches 10-9Feeding the semiconducting polymer film into an analysis chamber in mbar;
s3: the chamber to be analyzed is evacuated to 10-10Mbar, double-clicking software "Advantage", opening a program interface, clicking "Source" to select "X-Ray Gun", selecting X-Ray Gun type as "Mono Anode (XR 6)" monochromatized aluminum target, and selecting a spot size of 500 μm;
s4: clicking 'Miscelllaneous' under a 'Mono 500 μm' program module, adding a sub-program 'Charge compression', selecting 'Flood Gun' to add a double-beam argon ion neutralizing Gun, and 'Mode' to select 'Charge Com Standard' Standard magnetic lens Mode;
s5: adding a point to be tested under a program module of 'Charge Compensation', clicking 'point', selecting 'point' in type, moving a sample, positioning a view field at the center of the sample, adjusting 'Z axis', focusing an optimal view field, clicking 'Read' at 'Position' when a crystal grain in the view field is most clear visually, automatically reading a record by a view field coordinate X, Y, Z, selecting 'Enable Auto Height' at 'Position', automatically seeking Height of equipment in the vicinity of a selected 'Z' value in the subsequent process, and determining a final 'Z' value according to the highest intensity value;
s6: establishing a subprogram under a point module, clicking the Profile, selecting the Depth Profile, and setting parameters in the Profile: "Delay after Etch(s)" in "Etching" is set to xx seconds, meaning that the test starts after xx seconds of stability after each Etching, "Move to Etch position" in "Etching"; "Rotation" selects "None";
s7: the "Ion Gun" Ar Ion Gun parameters are set under the "Depth Profile" module: "Ion Energy" is 4000 eV; selecting a Cluster plasma Mode by the Mode; "Cluster Size" selects "500"; selecting Manual from the 'Raster Size', inputting a parameter of 5mm, and selecting ten times of the X-Ray spot area according to the selection principle; selecting "Turn gun of fwhen finished";
s8: setting 'Etch Phases' under a 'Depth Profile' module, and setting the first layer etching time to be 30 s; clicking 'Insert' to Insert the second layer, and setting the etching time of the second layer to be 30 s; clicking 'Insert' to Insert a third layer, and setting the etching time of the third layer to be 20 s; clicking 'Insert' to Insert the fourth layer, and setting the etching time of the fourth layer to be 20 s; clicking 'Insert' to Insert a fifth layer, and setting the etching time of the fifth layer as 10 s; clicking 'Insert' to Insert the sixth layer, and setting the etching time of the sixth layer to be 10 s; clicking 'Insert' to Insert the seventh layer, and setting the etching time of the seventh layer to be 10 s; clicking 'Insert' to Insert the eighth layer, and setting the etching time of the eighth layer to be 20 s; clicking 'Insert' to Insert the ninth layer, and setting the etching time of the ninth layer to be 20 s; click "Insert" to Insert the tenth layer, set the tenth layer etch time to 30 s.
In the step, the 'Depth profiles' module sets 'Etch Phases', the etching time of each layer is set to be different according to the thickness of each layer of polymer, the etching time near the interface between different polymer layers is set to be shorter, the combination state and the content of elements near the interface can be accurately tested, and the change rule of the combination state and the content of the elements near the interface is analyzed.
S9: setting 'Etch Position' under the 'Depth Profile' module, and clicking 'Read Position' in 'Native Coordinates' to Read a coordinate X, Y, Z value corresponding to each layer of etching points;
s10: selecting a Depth profile under a program tree 'experience', clicking 'Spectrum' to select 'Multi Spectrum' to add an element to be tested, and selecting a certain track electron of the element to be tested in 'Insert Multi Spectrum Into experience';
s11: selecting a program tree 'expert', clicking 'Source' to select 'Gun shutdown', and closing an 'electron Gun' and a 'neutralizing Gun' after the program etching and testing operation are set;
s12: and clicking the 'Experimental Run' program to Run after the program is set.
In conclusion, the method mainly utilizes argon ion clusters to bombard the surface of the polymer, peels off dozens of nanometer deep atoms on the surface, and then adopts X rays to irradiate the peeled surface of the polymer, so as to generate an X-ray photoelectron spectrum and accurately analyze the element combination state and content of a new interface after peeling. The invention combines the cluster plasma etching technology with the X-ray photoelectron spectrum, detects the X-ray photoelectron spectrum at different depth positions of the interface layers of different polymer films of the semiconductor, obtains the element combination state and content, is favorable for exploring the relation between the properties of the polymer semiconductor film and the performances of the photoelectric device, and has wide application prospect in the field of film analysis.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (2)
1. A method for measuring an X photoelectron spectrum of a polymer sub-layer by cluster plasma etching is characterized by comprising the following steps:
s1: placing the semiconductor polymer film in a pre-vacuumizing chamber of an X-ray photoelectron spectrometer for vacuumizing;
s2: when the vacuum degree of the pre-vacuum chamber reaches 10-9Feeding the semiconducting polymer film into an analysis chamber in mbar;
s3: the chamber to be analyzed is evacuated to 10-10Mbar, double click software "Advantage, open the program interface, click "Source" to select "X-Ray Gun", select X-Ray Gun type as "Mono Antode (XR 6)" monochromatized aluminum target, spot size select 500 μm;
s4: clicking 'Miscelllaneous' under a 'Mono 500 μm' program module, adding a sub-program 'Charge compression', selecting 'Flood Gun' to add a double-beam argon ion neutralizing Gun, and 'Mode' to select 'Charge Com Standard' Standard magnetic lens Mode;
s5: adding a point to be tested under a program module of 'Charge Compensation', clicking 'point', selecting 'point' in type, moving a sample, positioning a view field at the center of the sample, adjusting 'Z axis', focusing an optimal view field, clicking 'Read' at 'Position' when a crystal grain in the view field is most clear visually, automatically reading a record by a view field coordinate X, Y, Z, selecting 'Enable Auto Height' at 'Position', automatically seeking Height of equipment in the vicinity of a selected 'Z' value in the subsequent process, and determining a final 'Z' value according to the highest intensity value;
s6: establishing a subprogram under a point module, clicking the Profile, selecting the Depth Profile, and setting parameters in the Profile: "Delay after Etch(s)" in "Etching" is set to xx seconds, meaning that the test starts after xx seconds of stability after each Etching, "Move to Etch position" in "Etching"; "Rotation" selects "None";
s7: the "Ion Gun" Ar Ion Gun parameters are set under the "Depth Profile" module: "Ion Energy" is 4000 eV; selecting a Cluster plasma Mode by the Mode; "Cluster Size" selects "500"; selecting Manual from the Raster Size, inputting a parameter of 5mm, and selecting ten times of the X-Ray spot area according to the selection principle; selecting "Turn gun of fwhen finished";
s8: setting 'Etch Phases' under a 'Depth Profile' module, and setting the first layer etching time to be 30 s; clicking 'Insert' to Insert the second layer, and setting the etching time of the second layer to be 30 s; clicking 'Insert' to Insert a third layer, and setting the etching time of the third layer to be 20 s; clicking 'Insert' to Insert the fourth layer, and setting the etching time of the fourth layer to be 20 s; clicking 'Insert' to Insert a fifth layer, and setting the etching time of the fifth layer as 10 s; clicking 'Insert' to Insert the sixth layer, and setting the etching time of the sixth layer to be 10 s; clicking 'Insert' to Insert the seventh layer, and setting the etching time of the seventh layer to be 10 s; clicking 'Insert' to Insert the eighth layer, and setting the etching time of the eighth layer to be 20 s; clicking 'Insert' to Insert the ninth layer, and setting the etching time of the ninth layer to be 20 s; clicking 'Insert' to Insert the tenth layer, and setting the etching time of the tenth layer to be 30 s;
s9: setting 'Etch Position' under the 'Depth Profile' module, and clicking 'Read Position' in 'Native Coordinates' to Read a coordinate X, Y, Z value corresponding to each layer of etching points;
s10: selecting a Depth profile under a program tree 'experience', clicking 'Spectrum' to select 'Multi Spectrum' to add an element to be tested, and selecting a certain track electron of the element to be tested in 'Insert Multi Spectrum Into experience';
s11: selecting a program tree 'expert', clicking 'Source' to select 'Gun shutdown', and closing an 'electron Gun' and a 'neutralizing Gun' after the program etching and testing operation are set;
s12: and clicking the 'expert Run' program to Run after the program is set.
2. The method of claim 1, wherein the etching time of each layer is set to different time according to the thickness of each layer of polymer by setting "Etch Phases" under a "Depth Profile" module in step S8.
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