Disclosure of Invention
The invention aims to provide a microchannel plate with high stability and high detection efficiency, which can be used for ultraviolet light and X-ray detection, wherein a functional film layer with high conversion efficiency is plated on the input surface and the inner wall of a channel of the microchannel plate to serve as a reflective cathode, so that high detection efficiency is obtained, and meanwhile, after the film layer is plated, an ultrathin compact waterproof protective film layer is prepared, so that the cathode film layer which is easily influenced by humid air is ensured to have good stability, and meanwhile, the detection efficiency and the electron multiplication function of MCP are not influenced.
According to a first aspect of the present invention, there is provided a high stability, high detection efficiency ultraviolet light and micro-channel plate for X-ray detection, comprising:
An array type electron multiplier formed by arranging millions of mutually parallel channel type electron multiplication units, wherein each electron multiplication unit forms a micro-channel structure;
Forming a reflective photocathode on the surface of the input surface and the inner wall of the channel of the electron multiplier unit, wherein the reflective photocathode is made of a material with high responsivity to ultraviolet light and X-rays, and
And a compact ultrathin waterproof protective layer with uniform thickness is prepared on the surface of the reflective photocathode.
Preferably, the reflective photocathode comprises a single film layer or a composite film layer which is prepared by at least one of cesium iodide, copper iodide, potassium bromide and potassium chloride.
Preferably, the ultrathin waterproof protective layer comprises a single film layer or a composite film layer which is prepared by at least one of silicon oxide, hafnium oxide, aluminum oxide, titanium oxide and silicon nitride.
Preferably, the coverage surface of the reflective photocathode is the whole input surface and the preset depth of the inner wall of the channel, the depth range is controlled to be 3D-20D, D is the aperture of each electron multiplication unit of the MCP, and the coating depth is more than or equal to 1/tan (theta), wherein theta is the chamfer angle of the electron multiplication unit.
Preferably, the covering surface of the ultrathin waterproof protective layer is the whole input surface and the whole inner wall of the channel.
Preferably, the thickness of the reflective photocathode is controlled to be 100-2000 nm, and the total thickness of the film layer of the ultrathin waterproof protective layer is controlled to be 0.5-20 nm.
According to a second aspect of the present invention, there is also provided a method for manufacturing a microchannel plate for high stability, high detection efficiency ultraviolet light and X-ray detection, comprising the steps of:
Preparing a film layer as a reflective photocathode on the surface of an input surface and the inner wall of a channel of an electron multiplication unit of an array type electron multiplier formed by arranging millions of channel type electron multiplication units which are parallel to each other by utilizing a material with a photoelectric conversion function, wherein the reflective photocathode is made of a material with high responsivity to ultraviolet light and X rays;
and preparing a compact ultrathin waterproof protective layer with uniform thickness on the surface of the reflective photocathode.
It should be understood that all combinations of the foregoing concepts, as well as additional concepts described in more detail below, may be considered a part of the inventive subject matter of the present disclosure as long as such concepts are not mutually inconsistent. In addition, all combinations of claimed subject matter are considered part of the disclosed inventive subject matter.
The foregoing and other aspects, embodiments, and features of the present teachings will be more fully understood from the following description, taken together with the accompanying drawings. Other additional aspects of the invention, such as features and/or advantages of the exemplary embodiments, will be apparent from the description which follows, or may be learned by practice of the embodiments according to the teachings of the invention.
Detailed Description
For a better understanding of the technical content of the present invention, specific examples are set forth below, along with the accompanying drawings.
Aspects of the invention are described in this disclosure with reference to the drawings, in which are shown a number of illustrative embodiments. The embodiments of the present disclosure are not necessarily intended to include all aspects of the invention. It should be understood that the various concepts and embodiments described above, as well as those described in more detail below, may be implemented in any of a number of ways, as the disclosed concepts and embodiments are not limited to any implementation. Additionally, some aspects of the disclosure may be used alone or in any suitable combination with other aspects of the disclosure.
The microchannel plate for high stability and high detection efficiency ultraviolet light and X-ray detection in combination with the embodiment shown in figures 1 and 2 comprises an array type electron multiplier, a reflective photocathode prepared on the input surface and the channel of the array type electron multiplier and an ultrathin waterproof protective layer prepared on the surface of the reflective photocathode.
The array type electron multiplier is formed by arranging millions of channel type electron multiplying units which are parallel to each other, and has an input surface and an output surface.
As an alternative embodiment, the array electron multiplier refers to an array electron multiplier formed by arranging millions of mutually parallel channel electron multiplying units, and is usually made from a raw material of cladding glass and core glass through the processes of wire drawing, multifilament drawing, screen arrangement, screen pressing, screen cutting, polishing, corrosion and hydrogen reduction, and is in a state of not plating any functional film layer.
Each electron multiplying unit constitutes a microchannel structure.
An example of a microchannel structure of an array type electron multiplier, i.e. an MCP background, is shown in connection with fig. 1, wherein reference numeral 10 denotes the inner walls of the channels, the region between the two inner walls of the channels constituting the microchannel. Reference numeral 20 denotes an input face of the array type electron multiplier.
As shown in fig. 1 and 2, a reflective photocathode 31 is prepared on the surface of the input surface 20 and the surface of the inner wall 10 of the channel of the electron multiplier unit, wherein the reflective photocathode is a film layer prepared from a material having a photoelectric conversion function.
Preferably, the reflective photocathode is made of a material with high responsiveness to ultraviolet light and X-rays, for example, a single film layer prepared from one of cesium iodide, copper iodide, potassium bromide and potassium chloride.
In further embodiments, the reflective photocathode 31 comprises a first composite film layer prepared from at least two of cesium iodide, copper iodide, potassium bromide, and potassium chloride.
In the foregoing embodiment, the total layer thickness of the reflective photocathode 31 is controlled to be 100-2000nm, whether it is a single film layer or a composite film layer.
The preparation process of the reflective photocathode can adopt physical vapor deposition methods for plating, such as thermal evaporation, electron beam evaporation, magnetron sputtering, ion plating process and the like.
In the embodiment of the invention, the reflective photocathode 31 covers the whole input surface and the predetermined depth of the inner wall of the channel, the covered depth is controlled to be 3D-20D, wherein D is the aperture of each electron multiplier unit of the MCP, and the coating depth is more than or equal to 1/tan (theta), wherein theta is the chamfer angle of the electron multiplier unit.
As shown in fig. 1 and 2, the surface of the reflective photocathode 31 is also provided with a dense ultra-thin waterproof protective layer 32 with uniform thickness. The ultra-thin waterproof layer 32 covers the entire surface of the input surface 20 and the entire inner wall 10 of the passage.
In further alternative embodiments, the ultra-thin waterproof layer 32 covers the entire input face 20 surface, the output face surface, and the entire channel inner wall 10.
In the examples shown in fig. 1 and 2, the preparation of the ultrathin waterproof protective layer can be performed by an atomic layer deposition technology, and the prepared film layer has high water vapor barrier capability and a certain secondary electron emission capability, and the types of materials include silicon oxide, hafnium oxide, aluminum oxide, titanium oxide, silicon nitride and the like.
In alternative embodiments, the ultra-thin waterproof protective layer 32 comprises a film layer made of one of silicon oxide, hafnium oxide, aluminum oxide, titanium oxide, silicon nitride, or a composite film layer made of at least two of silicon oxide, hafnium oxide, aluminum oxide, titanium oxide, silicon nitride.
The total thickness of the film layer of the ultra-thin waterproof protective layer 32 is controlled to be 0.5 nm-20 nm, whether it is a single film layer or a composite film layer.
The preparation method of the microchannel plate for ultraviolet light and X-ray detection with high stability and high detection efficiency disclosed by the invention comprises the following steps:
Preparing a film layer as a reflective photocathode on the surface of an input surface and the inner wall of a channel of an electron multiplication unit of an array type electron multiplier formed by arranging millions of channel type electron multiplication units which are parallel to each other by utilizing a material with a photoelectric conversion function, wherein the reflective photocathode is made of a material with high responsivity to ultraviolet light and X rays;
and preparing a compact ultrathin waterproof protective layer with uniform thickness on the surface of the reflective photocathode.
As an alternative embodiment, the reflective photocathode 31 may be plated by physical vapor deposition methods such as thermal evaporation, electron beam evaporation, magnetron sputtering, ion plating, etc., and may be a single film layer or a composite film layer prepared by using at least one of cesium iodide, copper iodide, potassium bromide, and potassium chloride. The parameters such as the aperture, the chamfer angle, the size and the like of the MCP substrate are not limited, the covered depth range is controlled to be 3D-20D, wherein D is the aperture of each electron multiplication unit of the MCP, the coating depth is more than or equal to 1/tan (theta), and theta is the chamfer angle of the electron multiplication unit.
The film material plating process parameters of the reflective photocathode 31 can be selected from the range of 100-2000 nm film thickness, 1-100 r/min tool rotation speed, 0.5-5 nm/s film plating speed, and pre-film plating baking at 50-200 ℃ for 10-60 min.
As an alternative embodiment, the ultra-thin waterproof protective layer 32 includes a single film layer or a composite film layer prepared by at least one of silicon oxide, hafnium oxide, aluminum oxide, titanium oxide, and silicon nitride.
As an alternative embodiment, the ultrathin waterproof protective layer 32 is prepared by adopting an atomic layer deposition technology, and the prepared film layer has high water vapor blocking capability and certain secondary electron emission capability. The prepared ultrathin waterproof protective layer uniformly covers the input surface of the MCP and the whole surface of the inner wall of the penetrating channel, the thickness range of the film layer is 0.5-20 nm, and the deposition temperature range of the film layer is 150-300 ℃.
In the following we take examples 1,2 and microchannel plates plated with reflective photocathodes only as examples, the same MCP assemblies were assembled for detection testing of 2KeV X-rays.
Example 1:
Step 1, plating a photoelectric conversion reflective cathode film layer by adopting a physical vapor deposition method:
1) Preparing MCP with aperture of 12 μm, diameter of 50mm and chamfer angle of 12 degree after plating NiCr electrode;
2) Preparing cesium iodide coating material;
3) Placing the MCP into a special clamp capable of correcting the bevel angle, and placing the clamp on a coater fixture with the coating angle adjusted so that the coating depth is 10D;
4) Proper coating parameters are set, namely the thickness of the coating layer is 1000nm, the rotating speed of the tool is 5r/min, the coating speed is 1nm/s, the baking before coating is carried out, namely the temperature is 150 ℃ and the time is 30min, and the coating process is automatically operated, so that the coating process is completed.
Step 2, preparing a protective film layer by adopting an atomic layer deposition technology
1) Preparing a precursor SiH 2(NEt2)2+O3 for depositing silicon oxide;
2) The MCP plated with the reflective photocathode film layer is directly transferred to the ALD equipment through a sample transfer channel connected with the vacuum equipment, and the MCP is suspended in the ALD equipment;
3) And (3) carrying out deposition of a film layer, wherein the deposition temperature is 280 ℃, and the deposition thickness of the film layer is 1nm.
4) After the deposition of the protective film layer was completed, air was discharged to obtain MCP sample 1.
And 3, packaging the MCP sample 1 into an MCP assembly, and performing detection efficiency and moisture resistance tests.
Example 2:
Step 1, plating a photoelectric conversion reflective cathode film layer by adopting a physical vapor deposition method, wherein the method is the same as that in the embodiment 1.
Step 2, preparing a protective film layer by adopting an atomic layer deposition technology
1) Preparing a precursor SiH 2(NEt2)2+O3 for depositing silicon oxide;
2) The MCP plated with the reflective photocathode film layer is directly transferred to the ALD equipment through a sample transfer channel connected with the vacuum equipment, and the MCP is suspended in the ALD equipment;
3) Depositing a film layer, wherein the deposition temperature is 280 ℃, and the deposition thickness of the film layer is 20nm;
4) After the deposition of the protective film layer was completed, air was released to obtain MCP sample 2.
And 3, packaging the MCP sample 2 into an MCP assembly, and performing detection efficiency and moisture resistance tests.
By comparing the test results of example 1, example 2 and the unplated ultra-thin waterproof protective film layer as follows
* The moist air condition is that the temperature is 22-25 ℃ and the relative humidity is 60 percent.
* SEM pictures of the morphology change of the crystal grains are shown in figure 3.
According to the detection result of the embodiment, the thickness of the ultrathin waterproof protective film layer is thicker, so that the detection efficiency of X-rays is more and more obviously influenced, the thicker the ultrathin waterproof protective film layer is, the more stable the storage in the air is, and the more stable the detection efficiency is along with the extension of the storage time, therefore, in the embodiment of the invention, the thickness of the ultrathin waterproof protective film layer is selected to be 0.5-20nm, the detection efficiency of X-rays and ultraviolet is basically not influenced, the cathode film layer which is easily influenced by humid air is ensured to have good stability, the ultrathin waterproof protective film layer can be widely applied to an open structure detector and related equipment, the change of multiple times of vacuum and atmospheric environment is not obvious, and the application range of materials such as halides which are easily influenced by humid air as MCP input surface reflective photocathodes is greatly expanded.
While the invention has been described with reference to preferred embodiments, it is not intended to be limiting. Those skilled in the art will appreciate that various modifications and adaptations can be made without departing from the spirit and scope of the present invention. Accordingly, the scope of the invention is defined by the appended claims.