CN114988710B - Method for obtaining horn-shaped MCP with large opening area ratio by acid solvent etching with organic oil solvent protection - Google Patents
Method for obtaining horn-shaped MCP with large opening area ratio by acid solvent etching with organic oil solvent protection Download PDFInfo
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- CN114988710B CN114988710B CN202210534196.7A CN202210534196A CN114988710B CN 114988710 B CN114988710 B CN 114988710B CN 202210534196 A CN202210534196 A CN 202210534196A CN 114988710 B CN114988710 B CN 114988710B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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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
- H01J43/06—Electrode arrangements
- H01J43/18—Electrode arrangements using essentially more than one dynode
- H01J43/24—Dynodes having potential gradient along their surfaces
- H01J43/246—Microchannel plates [MCP]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
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Abstract
The invention discloses a method for obtaining horn-shaped MCP with a large opening area ratio by etching with an acid solvent, wherein the method is protected by an organic oil solvent. After the corrosion process of the conventional microchannel plate, the hole-shaped channel array of the microchannel plate is completed, at the moment, an acid solution etching step protected by an organic oil solvent is added, an organic oil solvent with lower density is added to a certain amount of acid solution to obtain a layered mixed solution, the input face of the MCP is put into the mixed solution, the part outside the input face of the MCP is protected by the organic oil solvent, and the MCP input end channels at the mixed interface are subjected to non-directional flaring corrosion by the acid solution, so that a flared flaring structure can be obtained on the input face of the MCP. The horn mouth channel obtained by the method can effectively increase the number of electrons incident into the channel and improve the detection efficiency of the microchannel plate, thereby being beneficial to improving the gain of MCP.
Description
Technical Field
The invention relates to the technical field of microchannel plates, in particular to a horn mouth-shaped microchannel plate with a large opening area ratio obtained by adopting an acid solvent etching method protected by an organic oil solvent, which can be applied to the technical field of vacuum photoelectric detection such as an enhancer, a microchannel plate type photomultiplier and the like.
Background
The microchannel plate (Microchannel Plate, MCP) is a fine hollow glass fiber panel of a thin sheet-like honeycomb structure composed of a plurality of parallel channels having secondary electron multiplication capability, and can be used for detecting various particles such as electrons, neutrons, ions, high-energy particles, X-rays, and electromagnetic waves with high energy. The micro-channel plate has the advantages of small volume, light weight, high gain, high spatial resolution, low noise and the like, and can be widely applied to the fields of military, photoelectric instruments, high-energy particle detection, radiation detection and the like.
The basic structural parameters of the microchannel plate have important influences on the electrical performance indexes and the like, and the important structural parameters comprise length-diameter ratio, chamfer angle, opening area ratio and the like. The ratio of the open area is the ratio of the open area of the channel of the microchannel plate working area to the area of the entire working area. Photoelectrons incident on the surface of the MCP input surface will have a part of loss on the input surface, which is difficult to enter the channel and actually contributes to electron multiplication, so that the opening area ratio determines the detection efficiency of the microchannel plate, and thus the gain and noise factor of the microchannel plate will be affected to a certain extent. The Open Area Ratio (OAR) of the microchannel plate is calculated as:
where D is the channel aperture and D is the channel center-to-center distance. As can be seen from the formula, the aperture of the channel is properly enlarged, the space between the channels is reduced, and the opening area ratio of the channel can be increased. The thickness of the leather material pipe is reduced to increase the opening area ratio, but the requirement on the micro-channel plate channel array structure is high, and the problems of strength, channel wall breakage and the like are easily caused by the excessively thin leather material. The channel of the MCP input end is designed into a horn mouth shape by adopting a flaring technology, the influence on the micro-channel plate structure is avoided while the opening area ratio is improved, and the number of electrons incident into the channel can be effectively increased, so that the number of incident electrons capable of participating in multiplication is increased, and the gain of the MCP is improved. Therefore, it is a very significant research effort to improve the probing efficiency and gain of MCP using the flaring technique. However, the need for an excessively large opening area ratio can present significant difficulties in the process fabrication of microchannel plates. The open area ratio of the microchannel plate is typically 58% to 70%.
The main ways to enlarge the opening area ratio of the microchannel plate include ion physical etching and chemical solvent etching. The ion physical etching can realize the directional etching of the micro-channel plate, but large-scale specialized equipment is needed, the etching difficulty is high, the etching time is long, and the cost is high. The flaring by using chemical solvent to corrode MCP has the advantages of low cost, simple operation and high etching rate, but the process is difficult to control and mass production is difficult to carry out. If the microchannel plate is directly immersed in a solution with strong corrosion capability, the corrosion rate is difficult to control, and over-corrosion is easy to cause and a deep reaming structure is formed.
Disclosure of Invention
The invention aims to provide an acid etching technology which is low in cost, simple to operate, controllable in process and capable of finely adjusting the length-diameter ratio of a channel and the flatness of an input surface so as to obtain a bell mouth-shaped MCP with a large opening area ratio.
The technical solution for achieving the purpose of the invention is a method for obtaining a bell mouth-shaped MCP with a large opening area by adopting an acid etching technology protected by an organic oil solvent, comprising the following steps:
the method for obtaining the horn-shaped MCP with the large opening area ratio by using the acid solvent etching and adopting the organic oil solvent protection is characterized in that after the MCP is corroded with core glass and before hydrogen reduction, the MCP input surface is placed in a mixed solution of an acid solution with the organic oil solvent on the upper layer and a certain concentration on the lower layer, the surface of the MCP input end facing the interface of the organic oil solvent and the acid solution is subjected to acid etching for a period of time, and the input surface of the MCP channel array is subjected to etching treatment, so that the horn-shaped MCP with the large opening area ratio is obtained.
The input face of the MCP channel array is etched, so that the opening is in a horn mouth shape, and the channel wall of the input face is round. The MCP is made of lead silicate glass, an organic oil solvent is used for protecting the MCP, the surface of the input end of the MCP is subjected to non-directional etching by utilizing the acid solution, a horn mouth shape is formed, and the opening area ratio of the MCP is enlarged.
Wherein the density relationship among the acid solvent, the MCP and the organic oil solvent is ρ 1 >ρ 2 >ρ 3 Wherein the acid solution has a density ρ 1 MCP has a density ρ 2 The density of the organic oil solvent is ρ 3 。
Wherein the temperature of the acid solution used is 21+/-1 ℃ and the mass fraction is 0.1-10%.
Preferably, the mass fraction of the hydrofluoric acid solution is selected to be 0.1% -5%.
Wherein, the etching time is controlled within the range of 30 s-200 s.
Wherein hydrofluoric acid is selected as the acid solution, and the use content is 5-20 mL; the organic oil solvent is one of edible oil and liquid paraffin oil, wherein the density of the edible oil is 0.92g/cm 3 ～0.93g/cm 3 The density of the liquid paraffin oil was 0.83g/cm 3 ～0.89g/cm 3 . The using amount of the organic oil solvent is 50mL.
Compared with the prior art, the invention firstly proposes to chemically corrode the MCP input end under the protection of the organic oil solvent, overcomes the defect of difficult control of the process when the chemical corrosion is directly carried out, protects most of the MCP substrate by the organic oil solvent, is favorable for controlling the corrosion process, can finely adjust the length-diameter ratio of the MCP channel and the planeness of the input surface, and has simple and controllable operation and low cost.
Compared with the method that the other surface of the microchannel plate is not required to be corroded, the method has the advantages that the organic oil solvent can completely protect the output surface of the microchannel plate and the structures in the channel from corrosion, the oil solvent can be completely removed conveniently and rapidly through the organic solvents such as acetone, diethyl ether and the like, and the microchannel plate is not easy to be polluted.
Drawings
FIG. 1 is a schematic diagram of an MCP before and after organic solvent protection and etching of flares with acid solvents.
Detailed Description
The invention aims to provide a method for obtaining a horn-shaped MCP with a large opening area ratio by acid solvent etching under the protection of an organic oil solvent. After the MCP is corroded with the core material glass and before hydrogen reduction, placing the MCP input surface downwards in a mixed solution of an acid solution with an upper layer of an organic oil solvent and a lower layer of a certain concentration, and performing acid etching on the surface of the MCP input end facing to the interface of the organic oil solvent and the acid solution for a period of time to realize etching treatment on the input surface of the MCP channel array. The organic solvent protects the outer portion of the MCP input during the etching process, thereby enabling a flared structure to be obtained on the MCP input surface, thereby significantly expanding the opening area ratio of the MCP input surface.
The input face of the MCP channel array is etched, so that the opening is in a horn mouth shape, and the channel wall of the input face is round.
In an alternative embodiment, the MCP is made of lead silicate glass, an organic oil solvent is used for protecting the MCP, the surface of the input end of the MCP is subjected to non-directional etching by using the acid solution, a horn mouth shape is formed, and the opening area ratio of the MCP is enlarged.
Wherein, the pore diameter range of the MCP substrate before etching is 5 mu m-40 mu m, and the density of the MCP substrate before etching is 0.95g/cm 3 ～1.05g/cm 3 。
As an alternative embodiment, the density relationship of the acid solvent, the MCP and the organic oil solvent is ρ 1 >ρ 2 >ρ 3 Wherein the acid solution has a density ρ 1 MCP has a density ρ 2 The density of the organic oil solvent is ρ 3 。
As a preferred example, the acid solution used in the method of the present invention is hydrofluoric acid having a density of 1.15g/cm 3 ～1.17g/cm 3 The temperature of the acid solution is 21+/-1 ℃; the acid solution is used in an amount of 5 mL-20 mL.
The mass fraction of the hydrofluoric acid solution used is 0.1% -10%, and preferably, the mass fraction range of the hydrofluoric acid solution is selected to be 0.1% -5%.
Thus, it can be confirmed that the etching time is controlled to be in the range of 30s to 200s. Preferably, the time of the hydrofluoric acid etching is 50 s-180 s.
As an alternative embodiment, the organic solvent is selected from one of edible oil and liquid paraffin oil, wherein the density of the edible oil is 0.92g/cm 3 ～0.93g/cm 3 The density of the liquid paraffin oil is 0.83g/cm 3 ～0.89g/cm 3 . The amount of organic solvent used was 50mL.
As an optional operation step, the method of obtaining a bell mouth-shaped MCP having a large opening area using the organic oil solvent protected acid etching technique of the present invention includes the steps of:
firstly, taking a plastic beaker, firstly adding a certain amount of HF solution with the mass fraction of 0.1% -10%, wherein the acid temperature is 21+/-1 ℃, then adding 50mL of edible oil or liquid paraffin oil into the plastic beaker, and standing for ten minutes to enable an acid-oil interface to be stable;
secondly, clamping a piece of micro-channel plate by using polytetrafluoroethylene tweezers, lightly placing the input surface in the mixed liquid prepared in the first step, corroding the input surface of the micro-channel plate at the interface of the mixed liquid by using hydrofluoric acid, and taking out the micro-channel plate by using the polytetrafluoroethylene tweezers after 30-200 seconds of corrosion;
sequentially and alternately ultrasonically cleaning the micro-channel plate for a plurality of times by using acetone, absolute ethyl alcohol and deionized water, wherein the ultrasonic cleaning time is 30s-3min each time;
and thirdly, ultrasonically cleaning the micro-channel plate by using absolute ethyl alcohol for 2-10min, and then placing the micro-channel plate in a clean oven at 120-250 ℃ and drying to obtain the horn-shaped micro-channel plate.
The present invention will be described in further detail with reference to the following examples, which are microchannel plates having a channel diameter of 6. Mu.m, a channel pitch of 7.2. Mu.m, a plate thickness of 0.29mm and an aspect ratio of 48.
Example 1
Firstly, taking a plastic beaker, adding 10mL of HF solution with the mass fraction of 5% into the plastic beaker, measuring 50mL of edible oil into the plastic beaker, and standing for ten minutes to enable the acid-oil interface to be stable, wherein the acid temperature is 21+/-1 ℃.
And secondly, clamping a piece of microchannel plate by using polytetrafluoroethylene tweezers, and lightly placing the microchannel plate with the input surface downwards in the mixed liquid prepared in the first step so as to enable the microchannel plate to float at the interface of the mixed liquid. And (3) corroding the input surface of the microchannel plate at the interface of the mixed solution by using hydrofluoric acid, and taking out the microchannel plate clamp by using polytetrafluoroethylene tweezers after corroding for 50 s. And sequentially and alternately ultrasonically cleaning the microchannel plate for 3 times by using acetone, absolute ethyl alcohol and deionized water, wherein the ultrasonic cleaning time is 3min each time.
And thirdly, ultrasonically cleaning the micro-channel plate by using absolute ethyl alcohol for 5min, and then placing the micro-channel plate in a clean oven at 180 ℃ for 30min to obtain the horn-shaped micro-channel plate.
Example 2
Firstly, taking a plastic beaker, adding 10mL of HF solution with the mass fraction of 0.1% into the plastic beaker, measuring 100mL of edible oil into the plastic beaker at the acid temperature of 21+/-1 ℃, and standing for ten minutes to enable the acid-oil interface to be stable.
And secondly, clamping a piece of microchannel plate by using polytetrafluoroethylene tweezers, and lightly placing the microchannel plate with the input surface downwards in the mixed liquid prepared in the first step so as to enable the microchannel plate to float at the interface of the mixed liquid. And (3) corroding the input surface of the microchannel plate at the interface of the mixed solution by using hydrofluoric acid, and taking out the microchannel plate by using polytetrafluoroethylene tweezers after corroding for 180 seconds. And sequentially and alternately ultrasonically cleaning the microchannel plate for 3 times by using acetone, absolute ethyl alcohol and deionized water, wherein the ultrasonic cleaning time is 3min each time.
And thirdly, ultrasonically cleaning the micro-channel plate by using absolute ethyl alcohol for 5min, and then placing the micro-channel plate in a clean oven at 180 ℃ for 30min to obtain the horn-shaped micro-channel plate.
Example 3
Firstly, taking a plastic beaker, adding 10mL of HF solution with the mass fraction of 10% into the plastic beaker, measuring 50mL of edible oil into the plastic beaker, and standing for ten minutes to enable the acid-oil interface to be stable, wherein the acid temperature is 21+/-1 ℃.
And secondly, clamping a piece of microchannel plate by using polytetrafluoroethylene tweezers, and lightly placing the microchannel plate with the input surface downwards in the mixed liquid prepared in the first step so as to enable the microchannel plate to float at the interface of the mixed liquid. And (3) corroding the input surface of the microchannel plate at the interface of the mixed solution by using hydrofluoric acid, and taking out the microchannel plate clamp by using polytetrafluoroethylene tweezers after corroding for 30 seconds. And sequentially and alternately ultrasonically cleaning the microchannel plate for 3 times by using acetone, absolute ethyl alcohol and deionized water, wherein the ultrasonic cleaning time is 3min each time.
And thirdly, ultrasonically cleaning the micro-channel plate by using absolute ethyl alcohol for 5min, and then placing the micro-channel plate in a clean oven at 180 ℃ for 30min to obtain the horn-shaped micro-channel plate.
Example 4
Firstly, taking a plastic beaker, adding 10mL of HF solution with the mass fraction of 2% into the plastic beaker, measuring 50mL of edible oil into the plastic beaker, and standing for ten minutes to enable the acid-oil interface to be stable, wherein the acid temperature is 21+/-1 ℃.
And secondly, clamping a piece of microchannel plate by using polytetrafluoroethylene tweezers, and lightly placing the microchannel plate with the input surface downwards in the mixed liquid prepared in the first step so as to enable the microchannel plate to float at the interface of the mixed liquid. And (3) corroding the input surface of the microchannel plate at the interface of the mixed solution by using hydrofluoric acid, and taking out the microchannel plate clamp by using polytetrafluoroethylene tweezers after corroding for 200 seconds. And sequentially and alternately ultrasonically cleaning the microchannel plate for 3 times by using acetone, absolute ethyl alcohol and deionized water, wherein the ultrasonic cleaning time is 3min each time.
And thirdly, ultrasonically cleaning the micro-channel plate by using absolute ethyl alcohol for 5min, and then placing the micro-channel plate in a clean oven at 180 ℃ for 30min to obtain the horn-shaped micro-channel plate.
Examples 1-4, the microchannel plates obtained by controlling the concentration of the HF solution, the time of reaction of the microchannel plates with the HF solution, were the final microchannel plates obtained according to the preparation method described above, and the ratio of the open area to the gain thereof are shown in table 1 below.
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Ratio of open area | 86.4％ | 84.3％ | 89.3％ | 90.1％ |
| Gain (800V) | 15435 | 15349 | 17859 | 18732 |
Through the test comparison, the horn-shaped MCP with a large opening area ratio, which is prepared by the method of the embodiment of the invention, has higher opening area ratio and gain, wherein the highest opening area ratio can reach 90%. The horn mouth channel obtained by the method can effectively increase the number of electrons incident into the channel and improve the detection efficiency of the microchannel plate, thereby being beneficial to improving the gain of MCP.
The foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (13)
1. A method for obtaining a horn-shaped MCP with a large opening area ratio by using acid solvent etching and adopting organic oil solvent protection is characterized in that after the MCP is corroded with core glass and before hydrogen reduction, the MCP input surface is placed in a mixed solution of an acid solution with an organic oil solvent on the upper layer and a certain concentration on the lower layer, acid etching is carried out on the MCP input end surface facing the interface of the organic oil solvent and the acid solution for a period of time, and etching treatment is carried out on the input surface of an MCP channel array to obtain the horn-shaped MCP with the large opening area ratio.
2. The method for obtaining a bell mouth-shaped MCP having a large opening area ratio by acid solvent etching using organic oil solvent protection according to claim 1, wherein the input face of the MCP channel array is subjected to etching treatment so that the opening shape assumes a bell mouth shape, and the input face channel wall is rounded.
3. The method for obtaining a bell mouth-shaped MCP having a large opening area ratio by acid solvent etching using an organic oil solvent protection according to claim 1, characterized in that the pre-etching channel pore size ranges from 5 μm to 40 μm.
4. The method for obtaining a bell-mouthed MCP with a large opening area ratio by acid solvent etching with organic oil solvent protection as claimed in claim 1, wherein the acid solution, MCP and organic oil solvent have a density relationship ρ of 1 >ρ 2 >ρ 3 Wherein the acid solution has a density ρ 1 MCP has a density ρ 2 The density of the organic oil solvent is ρ 3 。
5. The method for obtaining a bell-mouthed MCP with a large opening area ratio by acid solvent etching with organic oil solvent protection as claimed in claim 1, wherein the density of MCP before etching is 0.95g/cm 3 ～1.05g/cm 3 。
6. The method for obtaining a bell mouth-shaped MCP with a large opening area ratio by acid solvent etching with organic oil solvent protection as claimed in claim 1, wherein the acid solution used is hydrofluoric acid with a density of 1.15g/cm 3 ～1.17g/cm 3 。
7. The method for obtaining a bell mouth-shaped MCP having a large opening area ratio by acid solvent etching using organic oil solvent protection according to claim 1, wherein the MCP is made of lead silicate glass material, the MCP is protected by the organic oil solvent, and the surface of the input end of the MCP is subjected to non-directional etching using the acid solution to form a bell mouth shape, thereby enlarging the opening area ratio of the MCP.
8. The method for obtaining a bell-mouth-shaped MCP having a large opening area ratio using acid solvent etching with organic oil solvent protection according to claim 1, characterized in that the temperature of the acid solution used is 21 ℃ ± 1 ℃.
9. The method for obtaining a bell mouth-shaped MCP having a large opening area ratio using acid solvent etching with organic oil solvent protection according to claim 1, wherein the mass fraction of the acid solution used is 0.1% to 10%.
10. The method for obtaining a bell-mouth-shaped MCP having a large opening area ratio by acid solvent etching using an organic oil solvent protection according to claim 1, characterized in that the etching time is 30s to 200s.
11. The method for obtaining a bell mouth-shaped MCP having a large opening area ratio by acid solvent etching using an organic oil solvent protection according to claim 1, wherein the acid solution is used in a content of 5mL to 20mL.
12. The method for obtaining a bell mouth-shaped MCP having a large opening area ratio using acid solvent etching with protection by an organic oil solvent according to any one of claims 1 to 11, wherein the organic oil solvent is one of an edible oil, a liquid paraffin oil, and a density of the edible oil is 0.92g/cm 3 ～0.93g/cm 3 The density of the liquid paraffin oil is 0.83g/cm 3 ～0.89g/cm 3 。
13. The method for obtaining a bell mouth-shaped MCP having a large opening area ratio using acid solvent etching with organic oil solvent protection according to claim 12, wherein the organic oil solvent is used in an amount of 50mL.
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| CN202210534196.7A CN114988710B (en) | 2022-05-17 | 2022-05-17 | Method for obtaining horn-shaped MCP with large opening area ratio by acid solvent etching with organic oil solvent protection |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837027A (en) * | 2006-04-21 | 2006-09-27 | 华东师范大学 | Method for making macroporous silicon micro-channel with high aspect ratio |
| CN102449746A (en) * | 2009-05-25 | 2012-05-09 | Az电子材料（日本）株式会社 | Liquid etchant and method for forming trench isolation structure using same |
| CN103646836A (en) * | 2013-12-06 | 2014-03-19 | 北方夜视技术股份有限公司 | Method of using solvent etching method to manufacture horn mouth micro channel plate |
| CN103787576A (en) * | 2014-01-13 | 2014-05-14 | 武汉市艾玻睿光电科技有限公司 | Preparation method and device for reaming holes on end of capillary glass tube |
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2022
- 2022-05-17 CN CN202210534196.7A patent/CN114988710B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837027A (en) * | 2006-04-21 | 2006-09-27 | 华东师范大学 | Method for making macroporous silicon micro-channel with high aspect ratio |
| CN102449746A (en) * | 2009-05-25 | 2012-05-09 | Az电子材料（日本）株式会社 | Liquid etchant and method for forming trench isolation structure using same |
| CN103646836A (en) * | 2013-12-06 | 2014-03-19 | 北方夜视技术股份有限公司 | Method of using solvent etching method to manufacture horn mouth micro channel plate |
| CN103787576A (en) * | 2014-01-13 | 2014-05-14 | 武汉市艾玻睿光电科技有限公司 | Preparation method and device for reaming holes on end of capillary glass tube |
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