CN112593206B - High-secondary-electron-emission-coefficient film and preparation method thereof - Google Patents
High-secondary-electron-emission-coefficient film and preparation method thereof Download PDFInfo
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- CN112593206B CN112593206B CN202011422992.9A CN202011422992A CN112593206B CN 112593206 B CN112593206 B CN 112593206B CN 202011422992 A CN202011422992 A CN 202011422992A CN 112593206 B CN112593206 B CN 112593206B
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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]
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- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
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Abstract
The invention discloses a high secondary electron emission coefficient film and a preparation method thereof, belonging to the field of device materials and comprising the following steps: 1) firstly, a substrate layer with required conductivity is obtained and is put into a reaction chamber in atomic layer deposition equipment; 2) first growing Al2O3A buffer layer having a thickness greater than or equal to 2nm and less than or equal to 2.5 nm; 3) then growing an MgO main body layer, wherein the thickness of the main body layer is 6-15 nm; 4) finally growing Al2O3A protective layer having a thickness of less than or equal to 1.0nm and greater than or equal to 0.3 nm. The gain of the electronic amplifier is closely related to the secondary emission coefficient of the film, if the film thickness is thinner, the secondary emission coefficient is lower, the gain is lower, and if the film thickness is thicker, although the secondary emission coefficient is higher, the electric conduction layer can not supplement electrons in time, the gain is reduced. The invention controls Al2O3Buffer layer and protective layer Al2O3Thereby making the film thickness moderate and maintaining a high secondary electron emission coefficient for a long time.
Description
Technical Field
The invention belongs to the field of device materials, and relates to a novel high-secondary-electron-emission-coefficient film.
Background
The atomic layer deposition technology is a technology that precursor gas and reaction gas enter a substrate alternately at a controllable speed, physical and chemical adsorption or surface saturation reaction is carried out on the surface of the substrate, and substances are deposited on the surface of the substrate layer by layer in the form of a monatomic film. Based on self-limiting reactions, atomic layer deposition techniques can produce continuous pinhole-free films with excellent step coverage and control of atomic-scale film thickness and composition.
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 gain of the electronic amplifier is closely related to the secondary emission coefficient of the film, if the film thickness is thinner, the secondary emission coefficient is lower, the gain is lower, and if the film thickness is thicker, although the secondary emission coefficient is higher, the electric conduction layer can not supplement electrons in time, the gain is reduced. Therefore, the film preparation thickness is suitable between 5nm and 15 nm.
The current technology has the following disadvantages:
the Secondary Electron Emission (SEE) coefficient delta of Al2O3 is about 4, which is lower than that of MgO, and the thickness of the prepared emission layer is between 5 and 9nm, as shown in FIG. 2.
The Secondary Electron Emission (SEE) coefficient δ of MgO was about 9, but MgO was easily deliquesced, and the secondary emission coefficient decreased after deliquescence for 1 month as shown in fig. 3.
MgO has a Secondary Electron Emission (SEE) coefficient of about 9, and if the thickness of the secondary electron emission coefficient emitting layer of 9 is at least 15nm or more, the emitting layer is too thick.
Disclosure of Invention
Aiming at the problems, the invention provides a novel high secondary electron emission coefficient film and a preparation method thereof.
The technical scheme of the invention is as follows: a preparation method of a film with high secondary electron emission coefficient comprises the following steps:
1. the substrate layer with the required conductivity is firstly put into a reaction chamber in the atomic layer deposition equipment.
2. Firstly growing Al with the thickness of 2 nm-2.5 nm2O3A buffer layer.
3. And then growing an MgO main body layer with the thickness of 6-15 nm.
4. Then growing Al with the thickness of 0.3 nm-1 nm2O3And a protective layer.
Further, the substrate layer which has obtained the required conductivity and is described in step 1 is deposited on the glass or metal as the substrate layer by using lead glass which is reduced by hydrogen to obtain the required conductivity as the substrate layer or growing a thin film with the required resistivity by using an atomic layer deposition technology or preparing a thin film with the required resistivity by using other technologies. The desired conductivity is 1M to 1 G.OMEGA..
Further, Al described in step 22O3The Al-based material is generated by reaction of TMA (trimethyl aluminum) and water vapor, the temperature of a reaction chamber is 180-250 ℃, and a layer of Al grows through atomic layer deposition2O3Time and sequence of aeration of the atomic layers: TMA/N2/H2O/N2Growing 20-25 layers of the material for 100-1000 ms/5-45 s/100-1000 ms/5-45 s.
Further, MgO described in step 3 is prepared by Mg (Cp)2Reacting with steam to form Mg (Cp)2Heating to 50-80 ℃, controlling the temperature of the reaction chamber to be 180-250 ℃, and controlling the aeration time and sequence of growing a layer of MgO atomic layer by the atomic layer deposition technology, wherein the aeration time and sequence are Mg (Cp)2/N2/H2O/N2Growing 54-135 layers of the glass substrate for 100-1000 ms/5-45 s/100-1000 ms/5-45 s;
further, Al described in step 42O3The Al-based material is generated by reaction of TMA (trimethyl aluminum) and water vapor, the temperature of a reaction chamber is 180-250 ℃, and a layer of Al grows through atomic layer deposition2O3Time and sequence of aeration of the atomic layers: TMA/N2/H2O/N2Growing 3-10 layers of the glass substrate for 100-1000 ms/5-45 s/100-1000 ms/5-45 s;
the invention also provides a high secondary electron emission coefficient film prepared by the method, and the film comprises a three-layer structure: al (Al)2O3A buffer layer having a thickness greater than or equal to 2nm and less than or equal to 2.5 nm; a MgO main body layer, the thickness of the main body layer is 6-15 nm; al (Al)2O3A protective layer having a thickness of less than or equal to 1.0nm and greater than or equal to 0.3 nm.
The invention has the following advantages and positive effects:
(a) in the case of a higher secondary electron emission coefficient which can likewise be achieved, Al is first prepared2O3The buffer layer can achieve the purpose of reducing the thickness of MgO as shown in FIG. 4; not only the thickness requirement range of the film is 5 nm-15 nm, but also the high secondary electron emission coefficient which is possessed only when the thickness of MgO is more than 20nm is obtained.
(b) Preparation of Al on MgO2O3The protective layer can achieve the purpose of protecting MgO, which is not easily deliquesced, and can have a high secondary electron emission coefficient as shown in fig. 5.
(c) In the present invention, Al2O3The thickness of the buffer layer cannot be too small to be less than 20 layers, and if it is too small, it does not contribute to the improvement of the MgO secondary electron emission coefficient, as shown in FIG. 4. The invention provides at least 20 buffer layers.
(d) In the present invention, Al2O3The thickness of the protective layer is set not to be too thick and not to be larger than 10 layers (1nm), otherwise, the MgO secondary electron emission coefficient is affected as shown in FIG. 5, and if it is larger than 1nm, Al is mainly expressed2O3Secondary electron emission coefficient, no longer plays a role of protecting MgO but represents Al2O3The performance of (c).
Drawings
FIG. 1 is a schematic representation of a novel high secondary electron emission coefficient film;
FIG. 2 shows Al of different thicknesses2O3The secondary electron emission coefficient varies with the incident electron energy;
FIG. 3 is a graph showing the variation of the secondary electron emission coefficient with the incident electron energy before and after the deliquescence of MgO of different thicknesses;
FIG. 4 shows different Al2O3The secondary electron emission coefficient of the same 9nm MgO grown under the thickness of the buffer layer varies with the incident electron energy, and no Al2O3Comparison of 35nmMgO in the buffer layer;
FIG. 5 shows the growth of Al of different thicknesses on 35nm MgO2O3The protective layer, the secondary electron emission coefficient before and after deliquescence changes with the incident electron energy.
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:
1) the substrate layer with the required conductivity is first placed in an atomic layer deposition device.
2) First growing Al with a thickness of 2nm2O3An atomic layer.
3) An atomic layer of MgO was then grown to a thickness of 9 nm.
4) Then Al with the thickness of 0.6nm is grown2O3An atomic layer.
Further, the substrate layer which is described in the step 1) and has obtained the required conductivity is deposited on the glass or the metal as the substrate layer by using lead glass which is reduced by hydrogen and has obtained the required conductivity as the substrate layer or growing a film with the required resistivity by using an atomic layer deposition technology and depositing the film with the required resistivity on the glass or the metal as the substrate layer or preparing the film with the required resistivity by using other technologies and depositing the film on the glass or the metal as the substrate layer. The desired conductivity is 1M to 1 G.OMEGA..
Further, Al described in step 22O3The Al-based material is generated by reaction of TMA (trimethyl aluminum) and water vapor, the temperature of a reaction chamber is 180-250 ℃, and a layer of Al grows through atomic layer deposition2O3Time and sequence of aeration of the atomic layers: TMA/N2/H2O/N2Growing a layer of Al in 150ms/15s/300ms/15s2O3Growing 20 layers to obtain Al with the thickness of 2nm2O3；
Further, MgO described in step 3 is prepared by Mg (Gp)2Reacting with steam to form Mg (Cp)2Heating to 50-80 ℃, controlling the temperature of the reaction chamber to be 180-250 ℃, and controlling the aeration time and sequence of growing a layer of MgO atomic layer by the atomic layer deposition technology, wherein the aeration time and sequence are Mg (Cp)2/N2/H2O/N2Growing a layer of MgO at 450ms/15s/300ms/15s, and growing 81 layers to obtain MgO with the thickness of 9 nm;
further, Al described in step 42O3By TMA (trimethylaluminum)) Reacting with water vapor to generate the Al, wherein the temperature of a reaction chamber is 180-250 ℃, and a layer of Al grows through atomic layer deposition2O3Time and sequence of aeration of the atomic layers: TMA/N2/H2O/N2Growing a layer of Al in 150ms/15s/300ms/15s2O36 layers are grown to obtain Al with the thickness of 0.6nm2O3；
According to another 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:
1. the substrate layer with the required conductivity is firstly put into a reaction chamber in the atomic layer deposition equipment.
2. First growing Al with a thickness of 2.5nm2O3A buffer layer.
3. Then a MgO body layer with a thickness of 15nm is grown.
4. Then Al with the thickness of 0.3nm is grown2O3And a protective layer.
Further, Al described in step 22O3The Al-based material is generated by reaction of TMA (trimethyl aluminum) and water vapor, the temperature of a reaction chamber is 180-250 ℃, and a layer of Al grows through atomic layer deposition2O3Time and sequence of aeration of the atomic layers: TMA/N2/H2O/N2Growing a layer of Al in 150ms/15s/300ms/15s2O3Growing 25 layers to obtain Al with the thickness of 2.5nm2O3；
Further, MgO described in step 3 is prepared by Mg (Cp)2Reacting with steam to form Mg (Cp)2Heating to 50-80 ℃, controlling the temperature of the reaction chamber to be 180-250 ℃, and controlling the aeration time and sequence of growing a layer of MgO atomic layer by the atomic layer deposition technology, wherein the aeration time and sequence are Mg (Cp)2/N2/H2O/N2Growing a layer of MgO in 450ms/15s/300ms/15s, and growing 135 layers to obtain MgO with the thickness of 15 nm;
further, Al described in step 42O3The Al-based material is generated by reaction of TMA (trimethyl aluminum) and water vapor, the temperature of a reaction chamber is 180-250 ℃, and a layer of Al grows through atomic layer deposition2O3Time and sequence of aeration of the atomic layers: TMA/N2/H2O/N2Growing a layer of Al in 150ms/15s/300ms/15s2O3Growing 3 layers to obtain Al with thickness of 0.3nm2O3；
FIG. 5 shows the growth of Al of different thicknesses on 35nm MgO2O3The protective layer, the secondary electron emission coefficient before and after deliquescence changes with the incident electron energy.
The thickness ranges of the buffer layer and the protective layer in the present invention are very important for the implementation of the present invention, and are the key points 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 (3)
1. A preparation method of a film with high secondary electron emission coefficient is characterized by comprising the following steps:
1) firstly, a substrate layer with required conductivity is obtained and is put into a reaction chamber in atomic layer deposition equipment;
2) first growing Al2O3A buffer layer having a thickness greater than or equal to 2nm and less than or equal to 2.5 nm;
3) then growing an MgO main body layer, wherein the thickness of the main body layer is 6-15 nm;
4) finally growing Al2O3A protective layer having a thickness of less than or equal to 1.0nm and greater than or equal to 0.3 nm;
the Al is2O3The buffer layer is generated by the reaction of trimethyl aluminum TMA and water vapor, the temperature of the reaction chamber is 180-250 ℃, and a layer of Al grows through atomic layer deposition2O3Time and sequence of aeration of the atomic layers: TMA/N2/H2O/N2Growing 20-25 layers of the glass substrate for 100-1000 ms/5-45 s/100-1000 ms/5-45 s;
the MgO body layer is formed by Mg (Cp)2Reacting with steam to form Mg (Cp)2Heating to 50-80 ℃, controlling the temperature of the reaction chamber to be 180-250 ℃, and controlling the aeration time and sequence of growing a layer of MgO atomic layer by the atomic layer deposition technology, wherein the aeration time and sequence are Mg (Cp)2/N2/H2O/N2Growing 54-135 layers of the glass substrate for 100-1000 ms/5-45 s/100-1000 ms/5-45 s;
the Al is2O3The protective layer is generated by the reaction of trimethylaluminum TMA and water vapor, the temperature of a reaction chamber is 180-250 ℃, and a layer of Al grows through atomic layer deposition2O3Time and sequence of aeration of the atomic layers: TMA/N2/H2O/N2Growing 3-10 layers of the material in 100-1000 ms/5-45 s/100-1000 ms/5-45 s.
2. The method for preparing a thin film with a high secondary electron emission coefficient as claimed in claim 1, wherein the substrate layer with the required conductivity is prepared by using lead glass with the required conductivity obtained by hydrogen reduction as the substrate layer, or by growing a thin film with the required resistivity by atomic layer deposition technology and depositing the thin film on glass or metal as the substrate layer; the required resistance is 1M-1G omega.
3. A high secondary electron emission coefficient thin film prepared by the method of any one of claims 1 to 2, wherein said thin film comprises a three-layer structure: al (Al)2O3A buffer layer having a thickness greater than or equal to 2nm and less than or equal to 2.5 nm; a MgO main body layer, the thickness of the main body layer is 6-15 nm; al (Al)2O3A protective layer having a thickness of less than or equal to 1.0nm and greater than or equal to 0.3 nm.
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