CN107665799A - A kind of preparation method of fluorescent screen for transmission electron microscope - Google Patents
A kind of preparation method of fluorescent screen for transmission electron microscope Download PDFInfo
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- CN107665799A CN107665799A CN201710133975.5A CN201710133975A CN107665799A CN 107665799 A CN107665799 A CN 107665799A CN 201710133975 A CN201710133975 A CN 201710133975A CN 107665799 A CN107665799 A CN 107665799A
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- fluorescent screen
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- phosphor powder
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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
- H01J9/20—Manufacture of screens on or from which an image or pattern is formed, picked up, converted or stored; Applying coatings to the vessel
- H01J9/22—Applying luminescent coatings
- H01J9/221—Applying luminescent coatings in continuous layers
- H01J9/223—Applying luminescent coatings in continuous layers by uniformly dispersing of liquid
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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
- H01J9/20—Manufacture of screens on or from which an image or pattern is formed, picked up, converted or stored; Applying coatings to the vessel
- H01J9/205—Applying optical coatings or shielding coatings to the vessel of flat panel displays, e.g. applying filter layers, electromagnetic interference shielding layers, anti-reflection coatings or anti-glare coatings
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- Manufacturing & Machinery (AREA)
- Cathode-Ray Tubes And Fluorescent Screens For Display (AREA)
Abstract
A kind of preparation method of fluorescent screen for transmission electron microscope of the invention, including fluorescent screen, it is characterised in that：The fluorescent screen includes substrate layer, phosphor powder layer, aluminum membranous layer；Bonded between substrate layer and phosphor powder layer by inorganic bond；Specific steps include：Prepare the KP1 aqueous solution；Prepare electrolyte；Weigh appropriate fluorescent material and form suspension；Soluble barium salt or the strontium salt aqueous solution are added, mixed liquor is clarified after standing 30 minutes, and most of fluorescent material has deposited to bottom；The overflow valve of dislodger is opened, forms 10~30um of thickness fluorescence coating；Substrate after evaporation of aluminum is put into Muffle furnace high-temperature roasting one hour at 500 DEG C, taken out after Temperature fall；The aluminium film planarization being now deposited is good and has good reflectivity, and the brightness of fluorescent screen greatly improves；Emphasis of the present invention solves the problems, such as the service life of fluorescent screen, while can improve brightness and the resolution ratio of fluorescent screen, and aqueous dispersion is used in manufacturing process, avoids Organic Pollution.
Description
Technical field
The present invention relates to the making of the making of fluorescent screen, more particularly to a kind of fluorescent screen for transmission electron microscope
Method.
Background technology
At present, transmission electron microscope (TEM) is using the electron beam emitted by electron gun, in vacuum passage
Condenser is passed through along mirror body optical axis, it is converged to by a branch of tapering, bright and uniform hot spot, irradiation by condenser
On sample in sample room；Carry the structural information of sample interior through the electron beam after sample, fine and close place is saturating in sample
The amount of electrons crossed is few, and the amount of electrons that sparse place passes through is more；After the convergence focusing and primary amplification of object lens, electron beam enters
The intermediate lens of subordinate and the 1st, the 2nd projection lens carry out comprehensive magnification imaging, and the electron image being finally exaggerated is incident upon sight
On the screen plate for examining interior；Electron image is converted into visible image so that user observes by fluorescent screen.
Traditional fluorescent screen is that fluorescent material and adhesive (generally collodion) solution are hybridly prepared into suspension, so
Fluorescent material is precipitated and is adhered on substrate by the precipitation method afterwards, then strengthens its electric conductivity in its surface plating a thin layer aluminium film.
The operating voltage of main flow transmission electron microscope (TEM) is between 120~400 kilovolts, because collodion is one
Kind organic matter, it is easy to decompose flavescence, blackening under the bombardment of high-power electron beam, has a strong impact on observing effect.Conventional fluorescent screen
To use collodion ethyl acetate solution in manufacturing process, the adhesion strength of fluorescent material and substrate is very low, use in TEM or
Fluorescent material easily occurs in maintenance process to come off, causes the reduction of fluorescent screen image quality, influences its service life.Therefore, originally
Invention emphasis solves the problems, such as the service life of fluorescent screen, while can improve brightness and the resolution ratio of fluorescent screen, and makes
Aqueous dispersion is used in journey, avoids Organic Pollution.
Patent of invention content
A kind of preparation method of fluorescent screen for transmission electron microscope, including fluorescent screen, the fluorescent screen include base
Flaggy, phosphor powder layer, aluminum membranous layer；Bonded between substrate layer and phosphor powder layer by inorganic bond；
Specific steps include：A) compound concentration is 1.5~3% KP1 (modulus m=2.5~3.5) aqueous solution；
Compound concentration is 0.02~0.05% electrolyte (soluble barium salt or strontium salt) aqueous solution.
B) appropriate fluorescent material is weighed according to the fluorescent material thickness that be deposited on fluorescent screen；According to fluorescent material weight (gram)
Mixed with the ratio between KP1 aqueous solution volume (milliliter) for 1: 120~1: 300, use magnetic stirrer 30 minutes, shape
Into suspension.
C) substrate is put into dislodger, adds soluble barium salt or the strontium salt aqueous solution, the suspension being stirred is direct
It is filled into 400 mesh screens in dislodger and carries out natural subsidence.Mixed liquor is clarified after standing 30 minutes, and most of fluorescent material sinks
Product has arrived bottom.The overflow valve of dislodger is opened, clear liquid is slowly flowed only, substrate is taken out and is put into thermostatic drying chamber at 120 DEG C
Under allow phosphor powder layer fully to dry, form thickness 10~30um fluorescence coating.
D) phosphor powder layer for seeming smooth on substrate is amplified it can be found that being scraggly, if being directly deposited one
Layer aluminium film, aluminium atom will penetrate into powder gap and form black aluminium.Therefore to be applied on phosphor powder layer before evaporation of aluminum one layer it is organic
Film, phosphor powder layer surface is set to become relative smooth, then AM aluminum metallization is conductive in vacuum evaporation instrument of the vacuum less than 10-3Pa
Layer.
E) substrate after evaporation of aluminum is put into Muffle furnace high-temperature roasting one hour at 500 DEG C, taken out after Temperature fall.This
When the aluminium film planarization that is deposited it is good and there is good reflectivity, the brightness of fluorescent screen greatly improves.
Further, KP1 (K2O.mSiO2, m are referred to as modulus) conduct is used in described fluorescent screen preparation method
Adhesive；Soluble barium salt or strontium salt are as precipitating reagent.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
1) powder natural sedimentation is used, makes fluorescent material and adhesive secure bond on substrate；
2) inorganic binder is used, the binding agent is not reacted with fluorescent material and water white transparency, does not interfere with the hair of fluorescent material
Light characteristic.
3) fluorescent screen binding agent will not decompose under beam bombardment, service life length；Add and be coated with manufacturing process
Machine membrane process, aluminium film flatness is high after evaporation of aluminum high-temperature roasting and has good reflection, and brightness greatly improves.
Brief description of the drawings
Fig. 1 is for being spread outside micelle in the preparation method of the fluorescent screen of Digital Imaging System for transmission electron microscope
Counter ions (such as potassium ion K+) schematic diagram.
Fig. 2 passes through intermolecular for the preparation method composition of the fluorescent screen for Digital Imaging System for transmission electron microscope
Dehydration forms oxygen bridge schematic diagram.
Fig. 3 is for phosphor powder layer structure in the preparation method of the fluorescent screen of Digital Imaging System for transmission electron microscope
Schematic diagram.
Embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and tool
Body embodiment is described in detail.
The present invention is used as adhesive using KP1 (K2O.mSiO2, m are referred to as modulus)；Soluble barium salt or strontium salt are made
For precipitating reagent.KP1 is strong base-weak acid salt, and intense hydrolysis can occur in water：
As shown in figure 1, hydrolyzing the general name that generated hydrated SiO 2 is various component silicate, can be written as
nSiO2.mH2O.Assemble when hydrated SiO 2 and just form " glue core " to a certain extent, because its surface has adsorption capacity, from
And the anion (HSiO3-, SiO32- or OH-) in adsorbent solution, turn into negatively charged " micelle ", spread outside micelle
Counter ions (such as potassium ion K+), are collectively referred to as " micelle ".
Many this micelles in KP1 solution as shown in Figure 2,3 just be present, form colloidal solution.Add fluorescence
After powder, this micelle is just adsorbed on the surface of powder, makes powder is stable to be suspended in colloidal solution.
Adding precipitating reagent (i.e. soluble barium salt or strontium salt) neutralizes the negative electrical charge in micelle, thus between generation molecule
Decomposition of hydrate, i.e. two potassium silicate micelles surrender two hydrones come, make to form oxygen bridge between potassium silicate molecule, this oxygen
Bridge is absorbed by substrate and fluorescent material, and the silicic acid of cohesion is formed by orthosilicate, firm between fluorescent material and substrate and fluorescent material
Solid bonding get up.
1) subsider, magnetic stirring apparatus, 400 mesh screens and Muffle furnace are by means of in implementation process of the present invention.
2) subsider is a cuboid plastic channel, and bottom is equipped with overflow valve, there is one block of plate-like substrate microscope carrier in cell body.
Magnetic stirring apparatus, 400 mesh screens and Muffle furnace are commercially available finished product.
3) binding agent used in the present invention is KP1.
4) example 1：Make the TEM fluorescent screens of 30 μm of fluorescent layer thickness
A) compound concentration is 2.5% KP1 (modulus m=3.0) aqueous solution；Compound concentration is 0.04% acetic acid
The barium aqueous solution.
B) appropriate 3.5 grams of fluorescent material is weighed；770 milliliters of the KP1 aqueous solution is measured, mixes, uses magnetic stirring apparatus
Stirring 30 minutes, form suspension.
C) substrate is put into dislodger, adds soluble barium salt or the strontium salt aqueous solution, the suspension being stirred is direct
It is filled into 400 mesh screens in dislodger and carries out natural subsidence.Mixed liquor is clarified after standing 30 minutes, and most of fluorescent material sinks
Product has arrived bottom.The overflow valve of dislodger is opened, clear liquid is slowly flowed only, substrate is taken out and is put into thermostatic drying chamber at 120 DEG C
Under allow phosphor powder layer fully dry, formed 30 μm of thickness fluorescence coating.
D) phosphor powder layer for seeming smooth on substrate is amplified it can be found that being scraggly, if being directly deposited one
Layer aluminium film, aluminium atom will penetrate into powder gap and form black aluminium.Therefore to be applied on phosphor powder layer before evaporation of aluminum one layer it is organic
Film, phosphor powder layer surface is set to become relative smooth, then AM aluminum metallization is conductive in vacuum evaporation instrument of the vacuum less than 10-3Pa
Layer.
E) substrate after evaporation of aluminum is put into Muffle furnace high-temperature roasting one hour at 500 DEG C, taken out after Temperature fall.This
When the aluminium film planarization that is deposited it is good and there is good reflectivity, the brightness of fluorescent screen greatly improves.
5) example 2：Make the TEM fluorescent screens of 10 μm of fluorescent layer thickness
A) compound concentration is 2.5% KP1 (modulus m=2.6) aqueous solution；Compound concentration is 0.03% acetic acid
The barium aqueous solution.
B) appropriate 1.5 grams of fluorescent material is weighed；According to fluorescent material weight (gram) and KP1 aqueous solution volume (milliliter) it
Than for 1: 200 mixing, using magnetic stirrer 30 minutes, forming suspension.
C) substrate is put into dislodger, adds soluble barium salt or the strontium salt aqueous solution, the suspension being stirred is direct
It is filled into 400 mesh screens in dislodger and carries out natural subsidence.Mixed liquor is clarified after standing 30 minutes, and most of fluorescent material sinks
Product has arrived bottom.The overflow valve of dislodger is opened, clear liquid is slowly flowed only, substrate is taken out and is put into thermostatic drying chamber at 120 DEG C
Under allow phosphor powder layer fully dry, formed 10 μm of thickness fluorescence coating.
D) phosphor powder layer for seeming smooth on substrate is amplified it can be found that being scraggly, if being directly deposited one
Layer aluminium film, aluminium atom will penetrate into powder gap and form black aluminium.Therefore to be applied on phosphor powder layer before evaporation of aluminum one layer it is organic
Film, phosphor powder layer surface is set to become relative smooth, then AM aluminum metallization is conductive in vacuum evaporation instrument of the vacuum less than 10-3Pa
Layer.
E) substrate after evaporation of aluminum is put into Muffle furnace high-temperature roasting one hour at 500 DEG C, taken out after Temperature fall.This
When the aluminium film planarization that is deposited it is good and there is good reflectivity, the brightness of fluorescent screen greatly improves.
Embodiment described above only expresses a kind of preparation method of the fluorescent screen for transmission electron microscope, and it is retouched
State more specific and in detail, but therefore can not be interpreted as the limitation to the scope of the claims of the present invention.It should be pointed out that pair
For one of ordinary skill in the art, without departing from the inventive concept of the premise, some deformations can also be made and changed
Enter, these belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should using appended claims as
It is accurate.
Claims (2)
1. a kind of preparation method of fluorescent screen for transmission electron microscope, including fluorescent screen, it is characterised in that：The fluorescence
Screen includes substrate layer, phosphor powder layer, aluminum membranous layer；Bonded between substrate layer and phosphor powder layer by inorganic bond；
Specific steps include：A) compound concentration is 1.5~3% KP1 (modulus m=2.5~3.5) aqueous solution；Prepare dense
Spend electrolyte (soluble barium salt or strontium salt) aqueous solution for 0.02~0.05%.
B) appropriate fluorescent material is weighed according to the fluorescent material thickness that be deposited on fluorescent screen；According to fluorescent material weight (gram) and potassium water
The ratio between bath of glass liquor capacity (milliliter) is 1: 120~1：300 mixing, using magnetic stirrer 30 minutes, formed suspended
Liquid.
C) substrate is put into dislodger, adds soluble barium salt or the strontium salt aqueous solution, by the suspension being stirred directly with 400
Mesh screen, which is filled into dislodger, carries out natural subsidence.Mixed liquor is clarified after standing 30 minutes, and most of fluorescent material deposits to
Bottom.Open dislodger overflow valve, make clear liquid slowly flow only, taking-up substrate be put into thermostatic drying chamber allowed at 120 DEG C it is glimmering
Light bisque is fully dried, and forms 10~30um of thickness fluorescence coating.
D) phosphor powder layer for seeming smooth on substrate is amplified it can be found that being scraggly, if one layer of aluminium is directly deposited
Film, aluminium atom will penetrate into powder gap and form black aluminium.Therefore one layer of organic film is applied on phosphor powder layer before evaporation of aluminum, made glimmering
Light bisque surface becomes relative smooth, then the AM aluminum metallization conductive layer in vacuum evaporation instrument of the vacuum less than 10-3Pa.
E) substrate after evaporation of aluminum is put into Muffle furnace high-temperature roasting one hour at 500 DEG C, taken out after Temperature fall.Now it is deposited
Aluminium film planarization it is good and there is good reflectivity, the brightness of fluorescent screen greatly improves.
2. there is a kind of preparation method of fluorescent screen for transmission electron microscope described in asking 1 according to right, it is characterised in that：
Adhesive is used as using KP1 in described fluorescent screen preparation method (K2O.mSiO2, m are referred to as modulus)；Soluble barium salt
Or strontium salt is as precipitating reagent.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710133975.5A CN107665799A (en) | 2017-03-07 | 2017-03-07 | A kind of preparation method of fluorescent screen for transmission electron microscope |
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| CN201710133975.5A CN107665799A (en) | 2017-03-07 | 2017-03-07 | A kind of preparation method of fluorescent screen for transmission electron microscope |
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| CN107665799A true CN107665799A (en) | 2018-02-06 |
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| CN201710133975.5A Pending CN107665799A (en) | 2017-03-07 | 2017-03-07 | A kind of preparation method of fluorescent screen for transmission electron microscope |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020154032A (en) * | 2019-03-18 | 2020-09-24 | セイコーエプソン株式会社 | Wavelength conversion element, light source device, projector, and method for manufacturing wavelength conversion element |
| CN115156009A (en) * | 2022-06-13 | 2022-10-11 | 无锡机电高等职业技术学校 | Process for improving brightness of electron beam fluorescent screen |
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| CN101937821A (en) * | 2010-03-30 | 2011-01-05 | 中山大学 | Fluorescent screen of vacuum equipment and non-adhesive manufacturing method for fluorescent screen |
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2017
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Patent Citations (4)
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| CN101752161A (en) * | 2008-12-02 | 2010-06-23 | 北京有色金属研究总院 | Preparation method of fluorescent screen of transmission electron microscope |
| CN101937821A (en) * | 2010-03-30 | 2011-01-05 | 中山大学 | Fluorescent screen of vacuum equipment and non-adhesive manufacturing method for fluorescent screen |
| CN103805161A (en) * | 2013-12-13 | 2014-05-21 | 北京中科科仪股份有限公司 | Preparation method for scintillating medium of secondary electron detector |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020154032A (en) * | 2019-03-18 | 2020-09-24 | セイコーエプソン株式会社 | Wavelength conversion element, light source device, projector, and method for manufacturing wavelength conversion element |
| CN115156009A (en) * | 2022-06-13 | 2022-10-11 | 无锡机电高等职业技术学校 | Process for improving brightness of electron beam fluorescent screen |
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Application publication date: 20180206 |
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