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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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000010410 layer Substances 0.000 claims abstract description 98
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 239000011241 protective layer Substances 0.000 claims abstract description 15
- 239000010409 thin film Substances 0.000 claims abstract description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract 12
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000005273 aeration Methods 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000005355 lead glass Substances 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims 2
- 239000010408 film Substances 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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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
- 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
- C23C16/44—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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- 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
- 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
- C23C16/02—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
- 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
- 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
- H01J43/00—Secondary-emission tubes; Electron-multiplier tubes
- H01J43/04—Electron multipliers
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Abstract
本发明公开了一种高二次电子发射系数薄膜及其制备方法，属于器件材料领域，包括如下步骤：1)首先将已获得需要电导率的衬底层放入原子层沉积设备中的反应腔室；2)先生长Al2O3缓冲层，所述缓冲层的厚度大于或等于2nm，小于或等于2.5nm；3)然后生长MgO主体层，所述主体层厚度为6～15nm；4)最后生长Al2O3保护层，所述保护层的厚度小于或等于1.0nm，大于或等于0.3nm。电子放大器件增益与薄膜的二次发射系数的高低有密切的关系，薄膜厚度如果较薄二次发射系数偏低导致增益偏低，如果较厚虽然二次发射系数变高但电导层不能及时补充电子导致增益降低。本发明通过控制Al2O3缓冲层和保护层Al2O3的厚度，从而使薄膜厚度适中且长期维持较高的二次电子发射系数。
The invention discloses a high secondary electron emission coefficient thin film and a preparation method thereof, belonging to the field of device materials, comprising the following steps: 1) firstly placing a substrate layer with required electrical conductivity into a reaction chamber in an atomic layer deposition equipment; 2) First grow an Al 2 O 3 buffer layer, the thickness of the buffer layer is greater than or equal to 2 nm and less than or equal to 2.5 nm; 3) Then grow a MgO host layer, the thickness of the host layer is 6-15 nm; 4) Finally grow Al 2 O 3 protective layer, the thickness of the protective layer is less than or equal to 1.0 nm and greater than or equal to 0.3 nm. The gain of the electronic amplifier device is closely related to the secondary emission coefficient of the film. If the film thickness is thinner, the secondary emission coefficient will be low, resulting in a lower gain. The electrons cause the gain to decrease. The invention controls the thickness of the Al 2 O 3 buffer layer and the Al 2 O 3 protective layer, so that the film thickness is moderate and a high secondary electron emission coefficient is maintained 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)
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