CN106527043B - A kind of method that stamping technique prepares large area photon scintillation crystal - Google Patents
A kind of method that stamping technique prepares large area photon scintillation crystal Download PDFInfo
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- CN106527043B CN106527043B CN201611032018.5A CN201611032018A CN106527043B CN 106527043 B CN106527043 B CN 106527043B CN 201611032018 A CN201611032018 A CN 201611032018A CN 106527043 B CN106527043 B CN 106527043B
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- template
- large area
- scintillation crystal
- plastic scintillant
- stamping technique
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0002—Lithographic processes using patterning methods other than those involving the exposure to radiation, e.g. by stamping
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- General Physics & Mathematics (AREA)
- Luminescent Compositions (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The present invention relates to a kind of methods that stamping technique prepares large area photon scintillation crystal, choose impression block and required plastic scintillant, release treatment is carried out to template, hot nano impression is carried out to plastic scintillant using the template for carrying out release treatment, will coining treated that template is detached with plastic scintillant, so as to obtain the photon crystal structure with template graphics complementation, the wherein size of impression block is more than 400mm2, hot nano impression is carried out by the way of specific heating pressurization.Compared with prior art, the present invention can prepare the photonic crystal plastic scintillant of large area, and the photon crystal structure of enough depth can be obtained according to the temperature and pressure intensity parameter, can be to avoid the damage of template or sample in preparation process.
Description
Technical field
The invention belongs to field of nuclear radiation measurement, and the flicker of large area photon crystal is prepared more particularly, to a kind of stamping technique
The method of body.
Background technology
Plastic scintillant is important a member in scintillator family, in nuclear radiation measurement, particularly neutron measurement, neutron
Gamma, which is screened in measurement and the measurement of beta ray, has important application.The refractive index of plastic scintillant is usually 1.4-
It can meet with and be totally reflected at interface between 1.6, when passage of scintillation light enters air, so as to limit effective output of light.A kind of raising light
The method of output is to prepare photon crystal structure on plastic scintillant surface, utilizes total internal reflection light and the coupling of photon crystal structure
Cooperation is used, and generates effective extraction pattern, so as to increase light output, and then improve the sensitivity of detection system, detection efficient and
Signal-to-noise ratio.
It is big that the nanometer embossing that nineteen ninety-five Stephen Y professors Chou propose for people provides a kind of quick copy
The method of area photon crystal structure.However the process that traditional nanometer embossing prepares photonic crystal contains photoresist
Spin coating and pattern transfer process, the process is complex, more faces severe challenge for plastic scintillant, light most first
Chemical reaction can occur with plastic scintillant and destroy scintillator for photoresist, and the ion beam secondly used during pattern transfer is carved
The techniques such as erosion are easy to destroy plastic scintillant in itself, cause declining to a great extent for its luminescent properties, pattern transfer process is easily broken
Bad scintillator causes the tear or deformation of scintillator.
Publication No. discloses a kind of use nano-imprinting method for the patent application of 105425266 A of CN and prepares photon crystalline substance
The technology of body plastic scintillant in the art, the plastic scintillant by softening is directly imprinted using impression block, so as to obtain
Photonic crystal plastic scintillant is obtained, the benefit of this method, which is that of avoiding conventional photonic crystals preparation process, to be needed by photoresist
Spin coating and the process of pattern transfer reduce the risk of destruction scintillator during pattern transfer.However announced in the patent
Imprint temperature (90 DEG C) and pressure (50bar) parameter can be only applied to area less than 400mm2The Plastic scintillation of (20mm × 20mm)
It is prepared by the photonic crystal of body.When area increases, being such as unable to reach design using the photonic crystal depth of above-mentioned parameter acquisition will
It asks, can not realize enough light extraction efficiencies.
Invention content
The purpose of the present invention is exactly to overcome the problems, such as that large area plastic scintillant nano impression depth is insufficient and provides
A kind of method that stamping technique prepares large area photon scintillation crystal.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method that stamping technique prepares large area photon scintillation crystal, using following steps：
(1) it chooses size and is more than 400mm2Impression block and required plastic scintillant, mainly for the coining of large area
Template is handled, and the area of plastic scintillant is slightly larger than impression block area so that template can be completely covered by plastics sudden strain of a muscle
On bright body；
(2) release treatment is carried out to template；
(3) hot nano impression is carried out to plastic scintillant using the template for carrying out release treatment,；
(4) demould, will coining treated that template is detached with plastic scintillant, so as to obtain the light with template graphics complementation
Sub- crystal structure,
Hot nano impression is carried out in a manner that heating is pressurizeed in step (3),
The temperature used is imprinted according to formulaIt determines, wherein S is impression block
Area, unit is square millimeter, and T is temperature, and unit is degree Celsius,
Coining using pressure according toIt determines, wherein the area of impression block,
Unit is square millimeter, and P is pressure, and unit is bar.
The battle array that impression block described in step (1) is formed for the cylindrical metal unit of structural cycle triangular in shape distribution
The distance between row, adjacent metal unit are 600nm, and a diameter of 300nm of metal unit, the height of metal unit is 300nm.
Plastic scintillant described in step (1), in complementary structure, is the battle array of poroid period of three-legged structure with impression block
The distance between row, adjacent holes are 600nm, bore dia 300nm, hole depth 270-300nm.Since the hole depth actually obtained often reaches
Less than the depth of template, therefore we provide a range met the requirements, and the core of this patent needs to obtain enough depths
Degree, here it is considered that 270-300nm belongs to the depth met the requirements.If do not use it is proposed that temperature and pressure if
The depth can not be obtained.
In addition, with the increase of sample area, in order to obtain the coining effect of enough depth, it is necessary to increase pressure.But such as
Fruit does not increase temperature while increasing pressure then may cause template to crack since the softening degree of plastic scintillant is inadequate, because
Temperature and pressure intensity parameter under the conditions of this acquisition different area is most important.
For the sample of some particular area, under conditions of depth of indentation is met, need using alap temperature,
To minimize destruction of the high temperature to the centre of luminescence in plastic scintillant, to keep its luminous efficiency to the maximum extent.It is high
Temperature can reduce luminous efficiency to a certain extent, and therefore, temperature and pressure, which need to meet specific relationship, can take into account various aspects,
Finally obtain preferable technique effect.
Plastic scintillant described in step (1) is the flicker using polyvinyl-toluene or polystyrene as host material
Body.
In step (2) by the way of vapor deposition, adhesive is deposited in template surface.
The material that release treatment uses in step (2) is perfluoro capryl trichlorosilane or crosses fluorine Kui base trichlorosilane.
Step (2) is using following steps：By template under nitrogen protection, it is passed through 20-30 points of the steam vapor deposition of adhesive
Then clock toasts 5-10 minutes at 120 DEG C, template surface forms one layer of fine and close molecule organic layer.
Temperature control is at 40-50 DEG C when step (4) demoulds.
Compared with prior art, the present invention can prepare the photonic crystal plastic scintillant of large area, according to institute of the present invention
The temperature and pressure intensity parameter of use can obtain the photon crystal structure of enough depth, in preparation process can to avoid template or
The damage of sample.
During using prior art preparation photonic crystal scintillator, when prepare area increase when pressure used and temperature be not enough to
Enough depth (parameter in such as 105425266 A of CN) are obtained, this is because being needed in the preparation using alap temperature
Degree is to reduce the loss of plastic scintillant luminous efficiency, however the viscosity of plastic scintillant that relatively low temperature obtains is higher,
Therefore it in order to obtain enough depth of indentation, needs under conditions of increasing pressure, suitably increases temperature (raising temperature if inappropriate
Degree may destroy template).In other words, in order to obtain the coining effect of enough depth, the pressure of used optimization and
Temperature is all the function of imprint area.
Description of the drawings
Fig. 1 is sample area and the relationship of the imprint temperature used.
Fig. 2 is sample area and the relationship of coining pressure used.
Fig. 3 is the atomic force microscope images of sample A and sample B in embodiment 1.
Fig. 4 is the luminescent spectrum of sample A and sample B under excitation of X-rays in embodiment 1.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Photonic crystal is prepared on model EJ212 plastic scintillants (matrix is polyvinyl-toluene) surface, it is selected
Formwork structure is the column periodic array of three-legged structure, and the period is 600nm, and pillar diameter is 300nm, and height is 300nm, template
It is a diameter of 101.6mm, area 8103mm2Circular shuttering, template material is silicon.
Preparation process is as follows：
Step 1：EJ212 plastic scintillants through and cuttings and polish the scintillator for obtaining surfacing, size is the length of side
For the square of 120mm, thickness 1mm, which is slightly larger than template size, prepares the identical sample of two panels, wherein one
Piece is prepared (sample A) according to the parameter that this patent provides, and another conduct is with reference to sample (sample B), using relatively low temperature and pressure
Prepared by power, as control, show the validity of parameter in this patent.Buy one piece of the template of above structure.
Step 2：Release treatment is carried out to template, template is put into, and it is pungent slowly to pour perfluor in the flask of nitrogen protection
Base trichlorosilane steam is deposited 20 minutes, then takes out template, toasts 5 minutes under the conditions of 120 DEG C in an oven, template surface
One layer of fine and close molecule organic layer is formed, so as to play adhesion between the scintillator that template is prevented in moulding process and is stamped
Effect.
Step 3：Hot nano impression is carried out to plastic scintillant using the template for carrying out release treatment, by template and waits to press
Print plastic scintillant substrate is put into the vacuum chamber of marking press, fixes plastic scintillant to be imprinted.
For sample A, it is heated slowly to
After sample thermal balance, template is slowly covered in sample center, slowly apply pressure until
The process lasts about 20 minutes, and plastic sample surface softening back template suppresses the figure with template graphics complementation
Shape.For sample B, 90 DEG C are heated slowly to, after sample thermal balance, template is slowly covered in sample center, is slowly applied
For pressure until 50bar, which lasts about 20 minutes, and plastic sample surface softening back template suppresses and template graphics complementation
Figure.
Step 4：Temperature is slowly reduced, can be demoulded when 40 DEG C, be treated that sample temperature drops to room temperature, that is, obtain surface
Plastic scintillant with photon crystal structure.
The relationship of above-mentioned temperature and pressure is to have carried out a series of experiments, under the conditions of obtaining different area plastic scintillant
Temperature and pressure intensity parameter, form the area that is shown respectively in Fig. 1 and Fig. 2 and temperature and the relationship of area and pressure.Wherein,
Rectangle stain is experimental data point, and black solid line is matched curve, meets the formula of above-mentioned temperature and pressure.
The atomic force microscope that surface topography is carried out to sample A and sample B characterizes, and observes its periodic structure and hole depth, such as
Shown in Fig. 3.The surface topography of sample A is shown in wherein A1, and the depth made along the trend of white line in A1 figures is shown in A2
Number of degrees value, mean depth are about 285nm, meet design requirement；The surface topography of contrast sample B is shown in B1, and B2 is shown
Be the depth value made along the trend of white line in B1 figures, mean depth is about 110nm, and depth of indentation is unsatisfactory for designing
It is required that.
In order to show influence of the photonic crystal for light extraction efficiency of two kinds of different depths, we test X ray and swash
Give the luminous intensity of sample.As shown in Figure 4, the results showed that sample A enhances 3.2 times, and contrast sample B only enhances 1.76
Times.
Embodiment 2
A kind of method that stamping technique prepares large area photon scintillation crystal, using following steps：
(1) it chooses size and is more than 400mm2Impression block and required polyvinyl-toluene for host material plastics dodge
Bright body, the array that impression block is formed for the cylindrical metal unit of structural cycle triangular in shape distribution, between adjacent metal unit
Distance for 600nm, a diameter of 300nm of metal unit, the height of metal unit is 300nm, plastic scintillant and making ide
Plate is in complementary structure, is the poroid periodic array of three-legged structure, and the distance between adjacent holes are 600nm, bore dia 300nm, hole
Deep 270nm, area are slightly larger than impression block.
(2) release treatment is carried out to template, it is pungent in template surface vapor deposition adhesive perfluor by the way of vapor deposition
Base trichlorosilane, by template under nitrogen protection, the steam for being passed through adhesive are deposited 20 minutes, are then toasted at 120 DEG C
10 minutes, template surface formed one layer of fine and close molecule organic layer；
(3) hot nano impression is carried out to plastic scintillant using the template for carrying out release treatment,
Hot nano impression is carried out in a manner that heating is pressurizeed in step (3),
The temperature used is imprinted according to formulaIt determines, wherein S is making ide
The area of plate, unit are square millimeters, and T is temperature, and unit is degree Celsius,
Coining using pressure according toIt determines, wherein S is the face of impression block
Product, unit is square millimeter, and P is pressure, and unit is bar.
(4) demoulded controlled at 40 DEG C, will coining treated that template is detached with plastic scintillant, so as to obtain
With the photon crystal structure of template graphics complementation.
Embodiment 3
A kind of method that stamping technique prepares large area photon scintillation crystal, using following steps：
(1) it chooses size and is more than 400mm2Impression block and required polystyrene be host material Plastic scintillation
Body, the array that impression block is formed for the cylindrical metal unit of structural cycle triangular in shape distribution, between adjacent metal unit
Distance is 600nm, and a diameter of 300nm of metal unit, the height of metal unit is 300nm, plastic scintillant and impression block
It is the distance between the poroid periodic array of three-legged structure, adjacent holes for 600nm, bore dia 300nm, hole depth in complementary structure
270nm, area are slightly larger than impression block.
(2) release treatment is carried out to template, by the way of vapor deposition, fluorine Kui is crossed in template surface vapor deposition adhesive
Base trichlorosilane, by template under nitrogen protection, the steam for being passed through adhesive are deposited 30 minutes, then toast 5 at 120 DEG C
Minute, template surface forms one layer of fine and close molecule organic layer；
(3) hot nano impression is carried out to plastic scintillant using the template for carrying out release treatment,
Hot nano impression is carried out in a manner that heating is pressurizeed in step (3),
The temperature used is imprinted according to formulaIt determines, wherein S is making ide
The area of plate, unit are square millimeters, and T is temperature, and unit is degree Celsius,
Coining using pressure according toIt determines, wherein S is the face of impression block
Product, unit is square millimeter, and P is pressure, and unit is bar.
(4) demoulded controlled at 50 DEG C, will coining treated that template is detached with plastic scintillant, so as to obtain
With the photon crystal structure of template graphics complementation.
Claims (8)
1. a kind of method that stamping technique prepares large area photon scintillation crystal, using following steps：
(1) impression block and required plastic scintillant are chosen；
(2) release treatment is carried out to template；
(3) hot nano impression is carried out to plastic scintillant using the template for carrying out release treatment；
(4) demould, will coining treated that template is detached with plastic scintillant, so as to obtain and the photon of template graphics complementation is brilliant
Body structure,
It is characterized in that,
The size of impression block described in step (1) is more than 400mm2,
Hot nano impression is carried out in a manner that heating is pressurizeed in step (3),
The temperature used is imprinted according to formulaIt determines, wherein S is the face of impression block
Product, unit are square millimeters, and T is temperature, and unit is degree Celsius,
Coining using pressure according toIt determines, wherein S is the area of impression block, single
Position is square millimeter, and P is pressure, and unit is bar.
2. the method that a kind of stamping technique according to claim 1 prepares large area photon scintillation crystal, feature exist
In the array that the impression block described in step (1) is formed for the cylindrical metal unit of structural cycle triangular in shape distribution is adjacent
The distance between metal unit is 600nm, and a diameter of 300nm of metal unit, the height of metal unit is 300nm.
3. the method that a kind of stamping technique according to claim 2 prepares large area photon scintillation crystal, feature exist
In plastic scintillant and impression block described in step (1) are in complementary structure, for the poroid periodic array of three-legged structure, phase
The distance between adjacent hole is 600nm, bore dia 300nm, hole depth 270-300nm.
4. the method that a kind of stamping technique according to claim 1 prepares large area photon scintillation crystal, feature exist
In, plastic scintillant described in step (1) be the scintillator using polyvinyl-toluene or polystyrene as host material.
5. the method that a kind of stamping technique according to claim 1 prepares large area photon scintillation crystal, feature exist
In in step (2) by the way of vapor deposition, in template surface vapor deposition adhesive.
6. the method that a kind of stamping technique according to claim 1 prepares large area photon scintillation crystal, feature exist
In the material that release treatment uses in step (2) is perfluoro capryl trichlorosilane or crosses fluorine Kui base trichlorosilane.
7. the method that a kind of stamping technique according to claim 1 prepares large area photon scintillation crystal, feature exist
In step (2) is using following steps：By template under nitrogen protection, it is passed through the steam vapor deposition of adhesive 20-30 minutes, so
It is toasted 5-10 minutes at 120 DEG C afterwards, template surface forms one layer of fine and close molecule organic layer.
8. the method that a kind of stamping technique according to claim 1 prepares large area photon scintillation crystal, feature exist
In temperature control is at 40-50 DEG C when step (4) demoulds.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108796604B (en) * | 2017-05-03 | 2019-11-12 | 中国科学院化学研究所 | A kind of colloidal photon crystal and preparation method thereof with curved-surface structure |
| CN109581469B (en) * | 2018-11-13 | 2023-06-13 | 中核四0四有限公司 | Processing method of large-area annular plastic scintillator |
| CN112716511A (en) * | 2020-12-21 | 2021-04-30 | 华中科技大学 | Novel scintillation crystal detector and design method and application thereof |
| CN112745416A (en) * | 2020-12-29 | 2021-05-04 | 苏州昊唐兴核高新材料有限公司 | Plastic scintillator sheet, preparation method and preparation device thereof |
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| CN105425266A (en) * | 2015-11-03 | 2016-03-23 | 同济大学 | Preparation method for photonic crystal plastic scintillator |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US9103921B2 (en) * | 2012-09-24 | 2015-08-11 | Savannah River Nuclear Solutions, Llc | Photonic crystal scintillators and methods of manufacture |
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| CN1799857A (en) * | 2005-12-31 | 2006-07-12 | 北京大学 | Nanometer imprinting method of biological stencil |
| KR20090108303A (en) * | 2008-04-11 | 2009-10-15 | 광주과학기술원 | Radiation detector containing photonic crystal crystal and method thereof |
| CN101665234A (en) * | 2008-09-03 | 2010-03-10 | 上海市纳米科技与产业发展促进中心 | Preparation technology for low-cost large-area nanoimprinting template with photonic crystal structure |
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