CN114908332A - Method for accurately measuring thinnest contribution thickness of low secondary electron emission coefficient material - Google Patents
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- CN114908332A CN114908332A CN202210473415.5A CN202210473415A CN114908332A CN 114908332 A CN114908332 A CN 114908332A CN 202210473415 A CN202210473415 A CN 202210473415A CN 114908332 A CN114908332 A CN 114908332A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
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- G01B21/08—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness for measuring thickness
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method for accurately measuring the thinnest contribution thickness of a material with a low secondary electron emission coefficient, which belongs to the field of material characterization and comprises the following steps: s1, firstly, selecting a substrate material and exceeding the thinnest contribution thickness thereof; s2, firstly, putting the substrate material into a reaction chamber in atomic layer deposition equipment for deposition to prepare a sample; s3, placing the sample into a secondary electronic test system for measurement; s4, obtaining a corresponding relation between the cycle number and the secondary electron emission yield, and determining the least cycle number; s5, growing the target material with the least cycle number on the silicon substrate, and measuring the thickness of the film; according to the invention, a material with a high secondary electron emission coefficient relative to a target material is selected as a substrate, the cycle number is controlled by an atomic layer deposition method so as to obtain the minimum cycle number of the thinnest contribution thickness of the material with the low secondary electron emission coefficient, and the thickness of the thin film is repeatedly measured on the silicon substrate, so that the accurate thinnest contribution thickness of the material with the low secondary electron emission coefficient is obtained.
Description
Technical Field
The invention belongs to the field of material characterization, and relates to a method for accurately measuring the thinnest contribution thickness of a material with a low secondary electron emission coefficient.
Background
The generation of secondary electrons is based on the incident electron energy, the angle of incidence and the Secondary Electron Emission (SEE) coefficient of the material. The Secondary Electron Emission (SEE) coefficient of a material is defined as the ratio of emitted secondary electrons to primary electrons incident on a surface. The physical process is that primary electrons enter the material to a certain incident depth to collide to generate inner secondary electrons, part of the inner secondary electrons collide in the material to be dissipated, part of the inner secondary electrons collide with the material on the surface layer in a relay manner to generate inner secondary electrons, the relay is kept, and finally the inner secondary electrons escape from the surface to generate emitted secondary electrons. When the material is too thin, the measured secondary electrons cannot represent the secondary electron emission coefficient of the material; when the material is too thick, internal secondary electrons generated in the deep part cannot escape from the surface of the material and cannot contribute to secondary electrons emitted by the material, so that the material has the thinnest contribution thickness. The thinnest contribution thicknesses of SEE coefficients generated by different materials are different, and the thinnest contribution thicknesses of different materials are required to be accurately measured in order to meet the scientific research requirements of devices such as spacecraft microwave components, electron multipliers and the like. In the past, films are grown by means of magnetron sputtering and the like and then roughly tested, because the incident depth of primary electrons is between a few nanometers and dozens of nanometers, the thickness of an angstrom-scale film can be accurately controlled by the atomic layer deposition technology through cycle times, and the atomic layer deposition technology becomes one of the key technologies in the aspect of researching the thinnest contribution thickness in recent years. Films of different cycle numbers are typically grown on a silicon substrate and placed into a secondary electron test system for testing as shown in figure 2.
The current testing difficulties are as follows: the material with high SEE coefficient is greatly different from the SEE coefficient of the silicon substrate, even the material easy to deliquesce is easy to obtain the minimum cycle number so as to obtain the thinnest contribution thickness of the material, but the material with low SEE coefficient is slightly different from the SEE coefficient of the silicon substrate, the difference of the secondary electron yield of the material with different cycle numbers is not large, and some materials easy to deliquesce are more difficult to distinguish in the measuring process, and the minimum cycle number cannot be obtained as shown in fig. 3.
Disclosure of Invention
The invention provides a method for accurately measuring the thinnest contribution thickness of a material with a low secondary electron emission coefficient aiming at the problems.
The technical scheme of the invention is as follows: a method for accurately measuring the thinnest contribution thickness of a low secondary electron emission coefficient material, the method comprising the steps of:
s1, firstly, selecting a material with a secondary electron emission coefficient higher than that of the target material as a substrate and exceeding the thinnest contribution thickness;
s2, putting the substrate into a reaction chamber of atomic layer deposition equipment, and depositing target materials with different cycle times to obtain a sample;
s3, placing the sample into a secondary electronic test system for measurement;
s4, obtaining a corresponding relation between the cycle number and the secondary electron emission yield, and determining the least cycle number;
and S5, finally growing the target material with the minimum cycle number on the silicon substrate, and carrying out film thickness measurement.
Further, the material with higher secondary electron emission coefficient than the target material in step 1 is used as the substrate and exceeds the thinnest contribution thickness, for example, when the target material is Cu, ZnO, B 2 O 3 Al exceeding 8nm when the secondary electron emission coefficient is about 2 2 O 3 The secondary electron emission coefficient is about 4, the MgO secondary electron emission coefficient exceeding 20nm is about 8, in this case, MgO exceeding 20nm and Al exceeding 8nm 2 O 3 Can be used as the substrate when the target material is Al 2 O 3 In this case, MgO having a size exceeding 20nm can be selected as the substrate.
MgO of more than 20nm described in step S1 by Mg (Cp) 2 Reacting with steam to form Mg (Cp) 2 Heating to 50-60 ℃, controlling the temperature of the reaction chamber to be 200 ℃, and growing a MgO atomic layer by the atomic layer deposition technology according to the circulation ventilation time and sequence of Mg (Cp) 2 /N 2 /H 2 O/N 2 Circulating the process for more than 180 times, wherein the process is 150ms/4s/150ms/4 s;
al exceeding 8nm in step S1 2 O 3 Is prepared through the reaction between trimethyl aluminum TMA and water vapor at 200 deg.c to form one Al layer by atomic layer deposition 2 O 3 Cycle ventilation time and sequence of atomic layers: TMA/N 2 /H 2 O/N 2 Cycling the process for more than 50 times, wherein the process is 150ms/4s/150ms/4 s;
further, the minimum number of cycles described in step S4 is obtained by obtaining a map of the number of cycles and the secondary electron emission yield, and the difference between the secondary electron emission yields of adjacent cycles is first within 0.3, and the smallest of the two adjacent cycles is determined as the minimum number of cycles.
Further, the film thickness measurement described in step S5 may be performed by an ellipsometer, a film thickness meter, or the like to measure the thickness of the nano-scale thin film.
The invention has the following advantages and positive effects:
1. the invention successfully solves the problem of accurately measuring the thinnest contribution thickness of the material with the low secondary electron emission coefficient by selecting the material with the high secondary electron emission coefficient as the substrate as shown in figure 4.
2. By adopting the test method, MgO material is selected as a substrate, and the deliquescent B with low secondary electron emission coefficient is successfully measured 2 O 3 See fig. 5 for the thinnest contributing thickness.
3. In the past, a large number of samples need to be prepared for measurement and averaging, and the number of the samples to be measured is reduced to a few samples through the test method, so that the growth cycle number of the thinnest contribution thickness of the material with the low secondary electron emission coefficient can be smoothly found.
Drawings
FIG. 1 is a schematic diagram of a method for testing a low secondary electron emission coefficient material.
FIG. 2 shows Al growth on a silicon substrate with different cycle times 2 O 3 The secondary electron emission coefficient varies with the incident electron energy.
FIG. 3 shows B for different cycle number of growth on a silicon substrate 2 O 3 The secondary electron emission coefficient varies with the incident electron energy.
FIG. 4 shows the growth of 315 cycles of MgO on a silicon substrate followed by the regrowth of B for different cycles 2 O 3 The secondary electron emission coefficient of the sample varies with the incident electron energy.
FIG. 5 shows the growth of 315 cycles of MgO on a silicon substrate followed by a different number of cyclesB of (A) 2 O 3 . B of secondary electron emission coefficient with different cycle times under the same incident electron energy 2 O 3 A change in (c).
FIG. 6 shows the growth of 315 cycles of MgO on a silicon substrate followed by the regrowth of Al for different cycles 2 O 3 . Al with secondary electron emission coefficient along with different cycle times under same incident electron energy 2 O 3 A change in (c).
Reference is made to the accompanying drawings in which: 1-a target material; 2-high SEE material, 3-silicon substrate.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific examples.
According to an embodiment of the present invention, a method for preparing a thin film with a high secondary electron emission coefficient is provided, which comprises the following steps:
s1, selecting ratio B 2 O 3 High SEE material 2 with high SEE coefficient, MgO as substrate.
S2, placing the MgO substrate into a reaction chamber in the atomic layer deposition equipment, and performing B with different cycle numbers 2 O 3 And (4) depositing to prepare a sample.
S3, and then placing the sample into a secondary electron testing system for measurement.
And S4, continuously repeating S2 and S3 to obtain the corresponding relation between the cycle number and the secondary electron emission yield, and determining the minimum cycle number.
S5, finally growing the target material 1 on the silicon substrate 3 for the minimum number of cycles, and performing film thickness measurement.
Further, MgO described in step S1, by Mg (Cp) 2 Reacting with steam to form Mg (Cp) 2 Heating to 50-80 ℃, controlling the temperature of the reaction chamber to be 200 ℃, and growing a MgO atomic layer by the atomic layer deposition technology according to the circulation ventilation time and sequence of Mg (Cp) 2 /N 2 /H 2 O/N 2 The process is cycled for more than 180 times, 150ms/4s/150ms/4 s.
Further, B in different numbers of cycles as described in step S2 2 O 3 Disclosure of the inventionPerBCl 3 Reacting with water vapor to generate a reaction product, wherein the temperature of a reaction chamber is 20-50 ℃, and a layer B grows by atomic layer deposition 2 O 3 Cyclic aeration time and sequence of atomic layers: BCl 3 /N 2 /H 2 O/N 2 Growing a layer of B (150 ms/4s/300ms/4 s) 2 O 3 And the sample one: cycle 1 time, sample two: cycle 2 times, sample three: cycle 3 times, sample four: cycle 4 times, sample five: cycle 5 times, sample six: cycle 6 times, sample six: circulating for 9 times;
further, B described in step S4 2 O 3 Minimum number of cycles of 5, B 2 O 3 The correspondence between the number of cycles and the secondary electron emission yield is shown in FIG. 5, and the difference between the number of cycles and the secondary electron emission yield between 5 and 9 is in the range of 0.3, so that 5 is considered as B 2 O 3 The minimum number of cycles.
Further, the film thickness measurement is performed as described in step S5, and the measurement is fitted by an ellipsometer.
According to another embodiment of the present invention, a method for preparing a thin film with high secondary electron emission coefficient is provided, comprising the steps of:
s1 selection ratio Al 2 O 3 High SEE material 2 with high SEE coefficient, MgO as substrate.
S2, putting the MgO substrate into a reaction chamber in the atomic layer deposition equipment, and carrying out Al with different cycle numbers 2 O 3 And (4) depositing to prepare a sample.
S3, and then placing the sample into a secondary electron testing system for measurement.
And S4, continuously repeating S2 and S3 to obtain the corresponding relation between the cycle number and the secondary electron emission yield, and determining the minimum cycle number.
S5, finally growing the target material 1 on the silicon substrate 3 for the minimum number of cycles, and performing film thickness measurement.
Further, MgO described in step S1, by Mg (Cp) 2 Reacting with steam to form Mg (Cp) 2 Heating to 50-80 ℃, controlling the temperature of the reaction chamber to be 200 ℃, and growing a first crystal by the atomic layer deposition technologyThe time and sequence of the venting of the MgO atomic layers Mg (Cp) 2 /N 2 /H 2 O/N 2 The process is cycled for more than 180 times, 150ms/4s/150ms/4 s.
Further, Al at different numbers of cycles as described in step S2 2 O 3 Is prepared through the reaction between TMA (trimethyl aluminum) and water vapor at 200 deg.C, and atomic layer deposition to grow a layer of Al 2 O 3 Cyclic aeration time and sequence of atomic layers: TMA/N 2 /H 2 O/N 2 Growing a layer of Al on the surface of the Al-Al alloy layer at 150ms/4s/150ms/4s 2 O 3 And the sample one: cycle 3 times, sample two: cycle 6 times, sample three: cycle 10, sample four: cycle 30 times, sample five: cycle 70 times, sample six: cycle 100 times, sample six: the cycle is 200 times.
Further, Al described in step S4 2 O 3 Minimum cycle number of 50, B 2 O 3 The correspondence between the number of cycles and the secondary electron emission yield is shown in FIG. 6, and the difference between the number of cycles and the secondary electron emission yield between 50 and 70 is in the range of 0.3, so that 50 is considered to be Al 2 O 3 The minimum number of cycles.
Further, the film thickness measurement is performed as described in step S5, and the measurement is fitted by an ellipsometer.
It should be noted that, in the present invention, the selection of a high-secondary-emission-coefficient material as the substrate, and particularly, the selection of MgO having a thickness of 20nm or more is very important for the implementation of the present invention, and is the key of the present invention.
The embodiments of the present invention are not intended to limit the present invention. Those skilled in the art can make numerous possible variations and modifications to the present invention, or modify equivalent embodiments, using the methods and techniques disclosed above, without departing from the scope of the present invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
Claims (7)
1. The method for accurately measuring the thinnest contribution thickness of the material with the low secondary electron emission coefficient is characterized by comprising the following steps of: the method comprises the following steps:
s1, firstly, selecting a material with a secondary electron emission coefficient higher than that of the target material as a substrate and exceeding the thinnest contribution thickness;
s2, putting the substrate into a reaction chamber of atomic layer deposition equipment, and depositing target materials with different cycle times to obtain a sample;
s3, placing the sample into a secondary electronic test system for measurement;
s4, obtaining a corresponding relation between the cycle number and the secondary electron emission yield, and determining the least cycle number;
and S5, finally growing the target material with the minimum cycle number on the silicon substrate, and carrying out film thickness measurement.
2. The method of accurately measuring the thinnest contributing thickness of a low secondary electron emission coefficient material of claim 1, wherein: the film thickness measurement was measured by an ellipsometer.
3. The method of accurately measuring the thinnest contributing thickness of a low secondary electron emission coefficient material of claim 1, wherein: the material with higher secondary electron emission coefficient than the target material is used as a substrate and exceeds the thinnest contribution thickness, namely when the target material is Cu, ZnO and B 2 O 3 Al exceeding 8nm when the secondary electron emission coefficient is about 2 2 O 3 The secondary electron emission coefficient is about 4, the MgO secondary electron emission coefficient exceeding 20nm is about 8, in this case, MgO exceeding 20nm and Al exceeding 5nm 2 O 3 Can be used as substrate when the target material is Al 2 O 3 In this case, MgO with a thickness exceeding 20nm can be selected as the substrate.
4. The method of accurately measuring the thinnest contributing thickness of a low secondary electron emission coefficient material of claim 1, wherein: the minimum cycle number is obtained from a map of the correspondence between the cycle number and the secondary electron emission yield, and the difference between the secondary electron emission yields of adjacent cycle numbers, which is the smallest of the two adjacent cycle numbers, is within 0.3 for the first time.
5. The method of accurately measuring the thinnest contributing thickness of a low secondary electron emission coefficient material of claim 1, wherein: the material having a higher secondary electron emission coefficient than the target material is used as the substrate.
6. A method for accurately measuring the thinnest contributing thickness of a low secondary electron emission coefficient material as recited in claim 3, wherein: MgO of 20nm by Mg (Cp) 2 Reacting with steam to form Mg (Cp) 2 Heating to 50-80 ℃, controlling the temperature of the reaction chamber to be 200 ℃, and growing a MgO atomic layer by the atomic layer deposition technology according to the circulation ventilation time and sequence of Mg (Cp) 2 /N 2 /H 2 O/N 2 The process is cycled for more than 180 times, 150ms/4s/150ms/4 s.
7. A method for accurately measuring the thinnest contributing thickness of a low secondary electron emission coefficient material as recited in claim 3, wherein: the Al exceeding 5nm 2 O 3 Is prepared through the reaction between trimethyl aluminum TMA and water vapor at 200 deg.c to form one Al layer by atomic layer deposition 2 O 3 Cycle ventilation time and sequence of atomic layers: TMA/N 2 /H 2 O/N 2 The process is cycled for more than 50 times (150 ms/4s/150ms/4 s).
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703880A (en) * | 2012-06-12 | 2012-10-03 | 浙江大学 | Method for preparing high-accuracy optical broadband anti-reflection multilayer film by utilizing atomic layer deposition |
| CN104152868A (en) * | 2014-07-28 | 2014-11-19 | 中国科学院西安光学精密机械研究所 | Method for preparing functional layer of microchannel plate by utilizing atomic layer deposition technology |
| CN108493083A (en) * | 2018-04-13 | 2018-09-04 | 中国建筑材料科学研究总院有限公司 | Ultralow temperature stablizes the microchannel plate and preparation method thereof of temperature resistance characteristic |
| CN112281141A (en) * | 2020-09-25 | 2021-01-29 | 西安空间无线电技术研究所 | Method for inhibiting secondary electron emission coefficient of medium surface based on controllable carbon nano coating |
| CN112593206A (en) * | 2020-12-08 | 2021-04-02 | 中国科学院高能物理研究所 | High-secondary-electron-emission-coefficient film and preparation method thereof |
| CN113684453A (en) * | 2021-06-23 | 2021-11-23 | 西安空间无线电技术研究所 | Film with low secondary electron emission coefficient and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703880A (en) * | 2012-06-12 | 2012-10-03 | 浙江大学 | Method for preparing high-accuracy optical broadband anti-reflection multilayer film by utilizing atomic layer deposition |
| CN104152868A (en) * | 2014-07-28 | 2014-11-19 | 中国科学院西安光学精密机械研究所 | Method for preparing functional layer of microchannel plate by utilizing atomic layer deposition technology |
| CN108493083A (en) * | 2018-04-13 | 2018-09-04 | 中国建筑材料科学研究总院有限公司 | Ultralow temperature stablizes the microchannel plate and preparation method thereof of temperature resistance characteristic |
| CN112281141A (en) * | 2020-09-25 | 2021-01-29 | 西安空间无线电技术研究所 | Method for inhibiting secondary electron emission coefficient of medium surface based on controllable carbon nano coating |
| CN112593206A (en) * | 2020-12-08 | 2021-04-02 | 中国科学院高能物理研究所 | High-secondary-electron-emission-coefficient film and preparation method thereof |
| CN113684453A (en) * | 2021-06-23 | 2021-11-23 | 西安空间无线电技术研究所 | Film with low secondary electron emission coefficient and preparation method thereof |
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