CN117950106A - Detection and transmission integrated scintillation single crystal optical fiber and preparation method and application thereof - Google Patents

Detection and transmission integrated scintillation single crystal optical fiber and preparation method and application thereof Download PDF

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Publication number
CN117950106A
CN117950106A CN202410031343.8A CN202410031343A CN117950106A CN 117950106 A CN117950106 A CN 117950106A CN 202410031343 A CN202410031343 A CN 202410031343A CN 117950106 A CN117950106 A CN 117950106A
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optical fiber
single crystal
crystal optical
detection
transmission
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陈俊锋
王皙彬
武安华
李翔
张振
寇华敏
苏良碧
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention provides a detection and transmission integrated scintillation single crystal optical fiber and a preparation method and application thereof. Meanwhile, the preparation method and the application of the detection and transmission integrated scintillation single crystal optical fiber provided by the invention have the characteristics of good practicality, high universality and good market application prospect.

Description

Detection and transmission integrated scintillation single crystal optical fiber and preparation method and application thereof
Technical Field
The invention relates to the technical field of radiation detection materials, and further relates to a detection transmission integrated scintillation single crystal optical fiber, a preparation method and application thereof.
Background
Radiation detection based on the scintillation effect is a very important technology in the fields of high-energy physics, nuclear security, environmental monitoring, radiology, etc., where accurate measurement of radiation dose is required to protect human and environmental safety.
With the wide application of radiation protection, radiation therapy and nuclear medicine, rapid, accurate, high sensitivity and strong radiation-resistant radiation detection are extremely critical requirements. Fiber optic probes are of great interest for their flexibility, high accuracy, low dose response, and shorter response times. However, the existing glass and organic scintillation fiber probes have serious irradiation damage problems in a high-dose environment, and the actual application of the glass and organic scintillation fiber probes in a strong irradiation environment is seriously affected.
In recent years, with the rapid development of optical technology and material science, a scintillation single crystal optical fiber with an inorganic matrix has received a great deal of attention because of the advantages of excellent high sensitivity, high time and spatial resolution, irradiation resistance and the like. The use of the scintillation single crystal optical fiber can simplify the structure of the detection device, improve the integration level and the stability of the detection device, and provide a new solution for radiation detection. However, many doped (such as rare earth ions) luminescence has a problem of self absorption, so that the light attenuation length of the scintillation single crystal fiber is short, and serious transmission loss is caused after the scintillation single crystal fiber is used, so that the application of the scintillation single crystal fiber in the radiation detection field is greatly limited. Therefore, people have to adopt a composite structure design with a scintillation single crystal optical fiber as a sensitive unit and a glass or plastic optical fiber as a transmission unit, the design faces various problems, such as larger optical coupling loss between the transmission unit and the scintillation single crystal optical fiber, complex coupling structure and high cost, and the glass or plastic optical fiber as the transmission unit has weak irradiation resistance and light attenuation phenomenon caused by irradiation damage under a strong irradiation environment, thereby seriously affecting the service characteristics and service life of the whole detection system, and the application of the design is also greatly limited.
Therefore, how to provide a scintillation single crystal optical fiber which is suitable for a strong irradiation environment, has small optical coupling loss and good service performance is a problem to be solved urgently by those skilled in the art.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a detection and transmission integrated scintillation single crystal optical fiber, a preparation method and application thereof, wherein one end of a detection unit D is connected with one end of a transmission unit T to form a coupling-free detection and transmission integrated scintillation single crystal optical fiber, the detection unit D is the scintillation single crystal optical fiber, the transmission unit T is the single crystal optical fiber capable of transmitting scintillation light of the detection unit D, the coupling-free integrated structure can effectively solve the problem of light loss caused by coupling between the scintillation single crystal optical fiber and the transmission optical fiber, the detection precision, the sensitivity and the transmission efficiency are improved, the inorganic scintillation single crystal optical fiber is adopted to replace the traditional glass or plastic transmission optical fiber, the irradiation resistance is remarkably improved, and the whole service performance and the service life of the optical fiber are improved.
In order to achieve the above object, the present invention provides the following technical solutions:
The detection and transmission integrated scintillation single crystal optical fiber comprises a detection unit D and a transmission unit T, wherein one end of the detection unit D is connected with one end of the transmission unit T to form a coupling-free integrated structure; the detection unit D is a scintillation single crystal optical fiber which comprises luminescent ions and a matrix; the transmission unit T is a single crystal optical fiber that is transparent to the scintillation light of the detection unit D.
In some embodiments, the matrix of the scintillation single crystal fiber is any one of LuAG、YAG、LuYAG、LuGdAG、GYGG、GYAG、TbAG、GAGG、GGG、BGO、PbWO4、LuAP、YAP、LuYAP、LuScAP、YScAP、LuGAP、Lu2O3、Y2O3、Sc2O3、Gd2O3、Ga2O3、(LuxY1-x)2O3、(LuxSc1-x)2O3、(YxSc1-x)2O3、LYSO、LSO、LGSO、CaF2 and SrF 2.
In some embodiments, the luminescent ion is one or more of Ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb, bi, ti, cr, mn, fe, co, ni, cu and Zn.
In some embodiments, the diameter d of the detection transmission integrated scintillation single crystal fiber is 0.01-10mm.
In some embodiments, the length of the detection transmission integrated scintillation single crystal optical fiber is L between 0.1 and 100000mm; the length of the detection unit D is 0.5-30mm, and the length of the transmission unit T is greater than or equal to 0.1mm.
The invention also provides a preparation method of the detection and transmission integrated scintillation single crystal optical fiber, which comprises the following steps: s1, proportioning: preparing scintillation single crystal optical fiber powder doped with luminescent ions and single crystal optical fiber powder respectively; s2, optical fiber growth: the detection and transmission integrated scintillation single crystal optical fiber is prepared by adopting any one growth method of a laser heating base method, an optical floating zone method, a micro-drop-down method or a guided mode method.
In some embodiments, when the growth method is a laser heated susceptor method, the method comprises the steps of:
S21, pouring the scintillating single crystal optical fiber powder and the single crystal optical fiber powder into a sealed elastic die according to the design length, and pressing the scintillating single crystal optical fiber powder and the single crystal optical fiber powder into an integrated structure through a static pressure machine to obtain a rod-shaped raw material;
S22, calcining the rod-shaped raw material, and cutting the calcined rod-shaped raw material into a preset size to obtain a detection and transmission integrated scintillating ceramic source rod;
s23, placing the detection and transmission integrated scintillating ceramic source rod in a laser heating base furnace, fixing one end of the detection unit D on a blanking rod, and fixing seed crystals containing the monocrystal optical fiber matrixes on seed crystal rods;
S24, sealing the furnace chamber, vacuumizing, introducing nitrogen to adjust the air pressure, and heating by laser to enable one end of the transmission unit T to be melted into a hemispherical melting zone;
and S25, butting the seed crystal with the hemispherical melting zone, and after the butting is stable, carrying out stable growth at a preset pulling speed and a preset feeding speed to finally obtain the detection and transmission integrated scintillation single crystal optical fiber.
In some embodiments, when the growth method is a micro-drop down method or a guided mode method, the method comprises the steps of:
And sequentially adding the single crystal optical fiber powder and the scintillation single crystal optical fiber powder into a crucible or a special die at different stages, melting the powder at high temperature, and growing the melt of the single crystal optical fiber powder and the melt of the scintillation single crystal optical fiber powder through capillary holes on the crucible or the special die under the guidance of seed crystals to finally obtain the scintillation single crystal optical fiber with integrated detection and transmission.
In some embodiments, in the step S1, the preparation step of the scintillation single crystal optical fiber powder doped with luminescent ions includes: s11, respectively weighing the matrix of the scintillation single crystal optical fiber and the luminescent ions according to stoichiometric proportions, placing the matrix and the luminescent ions in a mortar, adding a mixing agent, and fully grinding to obtain first mixed powder; s12, pressing the first mixed powder into a first rod-shaped raw material; s13, calcining and grinding the first rod-shaped raw material to obtain the scintillating single crystal optical fiber powder; and/or the number of the groups of groups,
The preparation method of the single crystal optical fiber powder comprises the following steps: s14, placing the matrix of the single crystal optical fiber in a mortar, and grinding to obtain second mixed powder; s15, pressing the second mixed powder into a second bar-shaped raw material; s16, calcining and grinding the second rod-shaped raw material to obtain the single crystal optical fiber powder.
The invention also provides application of the detection and transmission integrated scintillation single crystal optical fiber, the detection and transmission integrated scintillation single crystal optical fiber or the detection and transmission integrated scintillation single crystal optical fiber manufactured by adopting the preparation method of the detection and transmission integrated scintillation single crystal optical fiber is coupled with a photosensitive element, and a reflection layer is adopted for wrapping and packaging, so that a radiation detection module is obtained, and the radiation detection module is applied to the field of strong irradiation resistance.
Compared with the prior art, the invention has the following beneficial effects:
The invention provides a detection and transmission integrated scintillation single crystal optical fiber and a matched preparation method and application thereof, wherein the detection and transmission integrated scintillation single crystal optical fiber comprises a detection unit D and a transmission unit T, wherein the detection unit D is a scintillation single crystal optical fiber, the transmission unit T is a single crystal optical fiber capable of transmitting scintillation light of the detection unit D, one end of the detection unit D and one end of the transmission unit T are connected to form a coupling-free integrated structure, the problem of light loss caused by directly coupling the scintillation single crystal optical fiber and the transmission optical fiber is effectively solved, the self-absorption problem in the scintillation light transmission process in the scintillation single crystal optical fiber is weakened, the scintillation light attenuation length of the scintillation single crystal optical fiber is prolonged, the amplitude of a finally detected light signal is increased, the detection precision is improved, and the high sensitivity and the transmission efficiency of signals in the detection and transmission stages are ensured; the irradiation resistance of the transmission optical fiber is obviously improved by adopting the inorganic scintillation single crystal optical fiber to replace the traditional glass or plastic transmission optical fiber, the service performance of the existing irradiation dose probe based on the scintillation single crystal optical fiber and the glass/plastic transmission optical fiber in a strong irradiation environment is improved, and the service life of the irradiation dose probe is prolonged. The preparation method and the application of the detection and transmission integrated scintillation single crystal optical fiber provided by the invention have the characteristics of good practicality, high universality and good market application prospect.
Drawings
The above features, technical features, advantages and implementation of the present invention will be further described in the following description of preferred embodiments with reference to the accompanying drawings in a clear and easily understood manner.
FIG. 1 is a schematic diagram of the working principle of a scintillation single crystal optical fiber with integrated detection and transmission provided by the invention;
FIG. 2 is a sample physical diagram of the scintillation single crystal optical fiber integrated with detection and transmission provided by the invention;
FIG. 3 is a radiation emission spectrum of the scintillation single crystal fiber integrated with detection and transmission, provided by the embodiment 4 of the invention, collected by the T end face of a transmission unit under excitation of different positions of a Mini X-ray source (40 kV,80 μA);
FIG. 4 is a graph showing the Z-shaped element distribution of a transmission unit T of the scintillation single crystal fiber integrated with detection and transmission provided in the embodiment 4 of the invention under excitation of different positions of a Mini X-ray source (40 kV,80 μA);
FIG. 5 is a chart showing the multi-channel energy spectrum of the detection transmission integrated scintillation single crystal fiber provided by the embodiment 4 of the invention at different positions collected by the end face of the detection unit D under the excitation of gamma rays (59.5 KeV) of 241 Am source at equal intervals;
FIG. 6 is a graph showing the multi-channel energy spectrum of the detection and transmission integrated scintillation single crystal fiber according to the embodiment 4 of the present invention at different positions collected by the T end face of the transmission unit under the excitation of gamma rays (59.5 KeV) of 241 Am source at equal intervals;
Fig. 7 is a diagram showing correlation between the energy spectrum full-energy peak channel address and the excitation position collected by two end faces of the detection unit D and the transmission unit T under the equidistant radiation excitation of the gamma ray (59.5 KeV) of the 241 Am source of the scintillation single crystal optical fiber provided by the embodiment 4 of the present invention.
Detailed Description
The technical scheme of the present invention will be clearly and completely described in the following in connection with specific embodiments. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention.
Example 1
Fig. 1 shows a schematic diagram of the working principle of the detection and transmission integrated scintillation single crystal optical fiber provided by the invention, wherein the uniformly doped scintillation single crystal optical fiber in the prior art has the advantages of high irradiation resistance hardness and no coupling, but has high transmission loss, while the composite structure of the uniformly doped scintillation single crystal optical fiber transmission optical fiber has low irradiation resistance hardness and larger coupling light loss although having low transmission loss, and the detection and transmission integrated scintillation single crystal optical fiber provided by the invention has the advantages of no coupling structure, no coupling light loss, high irradiation resistance hardness and low transmission loss.
The detection and transmission integrated scintillation single crystal optical fiber comprises a detection unit D and a transmission unit T, wherein one end of the detection unit D is connected with one end of the transmission unit T to form a coupling-free integrated structure, and the detection unit D and the transmission unit T are not mutually influenced, as shown in fig. 2.
The detection unit D is a scintillation single crystal optical fiber, and the scintillation single crystal optical fiber comprises luminescent ions and a matrix; and the transmission unit T is a single crystal optical fiber that is transparent to the scintillation light of the detection unit D.
In some embodiments, the matrix of the scintillation single crystal fiber is any one of LuAG、YAG、LuYAG、Lu GdAG、GYGG、GYAG、TbAG、GAGG、GGG、BGO、PbWO4、LuAP、YAP、LuYAP、LuScAP、YScAP、LuGAP、Lu2O3、Y2O3、Sc2O3、Gd2O3、Ga2O3、(LuxY1-x)2O3、(LuxSc1-x)2O3、(YxSc1-x)2O3、LYSO、LSO、LGSO、CaF2 and SrF 2, but is not limited thereto.
The luminescent ion is one or more of Ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb, bi, ti, cr, mn, fe, co, ni, cu and Zn.
In some embodiments, the matrix of the single crystal optical fiber described above may be the same as or different from the matrix of the scintillation single crystal optical fiber, but requires scintillation light that is transmitted through the scintillation single crystal optical fiber.
It should be noted that the above listed elements of the matrix and luminescent ions of the scintillation single crystal fiber are merely for further explanation of the present invention, and should not be construed as limiting the scope of the detection and transmission integrated scintillation single crystal fiber material system of the present invention, and some insubstantial modifications and adjustments made by those skilled in the art based on the above description of the present invention are all within the scope of the present invention.
In some embodiments, the diameter d of the detection transmission integrated scintillation single crystal fiber is 0.01-10mm.
In some embodiments, the length of the detection transmission integrated scintillation single crystal fiber is L from 0.1mm to 100000mm. Wherein the length of the detection unit D is 0.5-30mm, and the length of the transmission unit T is greater than or equal to 0.1mm.
Example 2
On the basis of the embodiment 1, the invention also provides a preparation method of the detection and transmission integrated scintillation single crystal optical fiber, which comprises the following steps:
s1, proportioning: and respectively preparing scintillation single crystal optical fiber powder doped with luminescent ions and single crystal optical fiber powder.
S2, optical fiber growth: the detection and transmission integrated scintillation single crystal optical fiber is prepared by adopting any one growth method of a laser heating base method, an optical floating zone method, a micro-drop-down method or a guided mode method.
Specific:
in the step S1, the preparation steps of the scintillation single crystal optical fiber powder doped with luminescent ions comprise:
S10, taking high-purity powder of the scintillation single crystal optical fiber matrix and high-purity powder of luminescent ions as raw materials, respectively putting the two raw material powders into a baking oven for baking so as to remove water and CO 2 in the raw material powders, wherein the baking time is preferably 12 hours.
S11, respectively weighing matrix raw material powder and luminescent ion raw material powder of the scintillation single crystal optical fiber according to stoichiometric proportion, placing the matrix raw material powder and the luminescent ion raw material powder into a mortar, adding a mixing agent, and fully grinding to obtain first mixed powder.
The mixture is preferably absolute ethanol and the milling time is preferably 2 hours.
S12, pressing the first mixed powder into a first rod-shaped raw material.
Preferably, the first mixed powder is poured into rubber balls, 2000Mpa pressure is applied to the rubber balls in a cold isostatic press, and the rubber balls are pressed for 10min to obtain the first rod-shaped raw material.
And S13, calcining and grinding the first rod-shaped raw material to obtain the scintillating single crystal optical fiber powder.
Preferably, the first rod-shaped material described above is placed in a crucible, then in a muffle furnace, calcined at 1650 ℃ for 10 hours, and then cooled to room temperature. And (3) putting the calcined first rod-shaped raw material into a mortar for full grinding, so as to obtain the scintillation single crystal optical fiber powder doped with luminescent ions.
In step S1, the preparation step of the single crystal optical fiber powder comprises:
s14, taking the matrix of the single crystal optical fiber, placing the matrix in a mortar, and fully grinding to obtain second mixed powder.
S15, pressing the second mixed powder into a second rod-shaped raw material.
Preferably, the second mixed powder is poured into rubber balls, 2000 Mpa of pressure is applied to the rubber balls in a cold isostatic press, and the rubber balls are pressed for 10 minutes to obtain the second rod-shaped raw material.
S16, calcining and grinding the second rod-shaped raw material to obtain single crystal optical fiber powder.
Preferably, the second rod-shaped material described above is placed in a crucible, then in a muffle furnace, calcined at 1650 ℃ for 10 hours, and then cooled to room temperature. And (3) putting the calcined second rod-shaped raw material into a mortar for full grinding, and obtaining the monocrystalline optical fiber powder.
In some embodiments, when the growth method described in step S2 is a laser heating susceptor method, the method further comprises the steps of:
s20, placing the scintillating single crystal optical fiber powder obtained in the step S1 and the single crystal optical fiber powder into a baking oven for baking, and fully removing the mixture (absolute ethyl alcohol), wherein the baking time is preferably 3 hours.
S21, sequentially filling the scintillating single crystal optical fiber powder obtained in the step S1 and the single crystal optical fiber powder into a sealed elastic mold according to the design length, and pressing the scintillating single crystal optical fiber powder into an integrated structure through a hydrostatic press to obtain the rod-shaped raw material.
The rod-shaped raw material can be understood as that one end of the detecting unit D is fixedly connected with one end of the transmission unit T, so that a coupling-free integrated structure is formed.
The sealing elastic mold is rubber ball, the static press is preferably a cold isostatic press, the pressing pressure is 200Mpa, and the pressing time is 10min.
S22, calcining the obtained rod-shaped raw material, and cutting the calcined rod-shaped raw material into a preset size to obtain the detection and transmission integrated scintillating ceramic source rod.
Preferably, the rod-shaped raw materials are placed in a crucible, placed in a muffle furnace, calcined for 10 hours at the temperature of 1200 ℃, and cooled to room temperature along with the furnace after the calcination is finished, so that the scintillation ceramic source rod integrating detection and transmission can be obtained.
Further, the calcined rod-shaped raw material is cut into a detection and transmission integrated scintillating ceramic source rod with the bottom side length of 1.5mm multiplied by 1.5 mm.
S23, placing the obtained detection and transmission integrated scintillating ceramic source rod in a laser heating base furnace, and fixing the other end of the detection unit D on the blanking rod, fixing seed crystals containing monocrystalline fiber matrix materials on the seed crystal rod and the other end of the transmission unit T towards the seed crystals as one end of the detection unit D on the detection and transmission integrated scintillating ceramic source rod is fixedly connected with one end of the transmission unit T, and simultaneously adjusting the positions of the detection and transmission integrated scintillating ceramic source rod and the seed crystals to enable the detection and transmission integrated scintillating ceramic source rod and the position of the seed crystals to be in the same straight line with a laser gathering point.
When one end of the transmission unit T is fixed on the blanking rod and the other end of the detection unit D faces the seed crystal, the material of the seed crystal may be selected from materials including a matrix of scintillation single crystal optical fibers.
S24, sealing the furnace chamber, vacuumizing, introducing nitrogen to adjust the air pressure of the furnace chamber, and heating by laser to enable one end of the transmission unit T to be melted into a hemispherical melting zone.
Preferably, the vacuum is pumped to below 1.0E -1, and after the pressure of the furnace chamber is adjusted to 1.008Mpa by introducing nitrogen, the laser heating can be started.
Further, the laser frequency and time are adjusted until one end of the transfer unit T is melted into a hemispherical molten zone.
S25, butting seed crystals with the hemispherical melting zone, and after the butting is stable, carrying out stable growth at a preset pulling speed and a preset feeding speed to finally obtain the detection and transmission integrated scintillation single crystal optical fiber.
Preferably, the preset pull-up speed is 20mm/h and the preset feed speed is 6.98mm/h.
S26, setting preset time for reducing power, and taking out the detection and transmission integrated scintillation single crystal optical fiber after the temperature of the detection and transmission integrated scintillation single crystal optical fiber and the temperature in the cavity of the laser heating base furnace are reduced to the room temperature.
Preferably, the preset time for power reduction is 1h.
It should be noted that, the optical floating zone method is similar to the growth process of the laser heating pedestal method described above, and the difference is that the optical floating zone method generally uses an ellipsoidal mirror to focus a halogen lamp or a xenon lamp light source onto a growth rod to realize growth, while the laser heating pedestal method uses laser as a heating light source to perform growth, and both single crystal fiber powder and scintillation single crystal fiber powder need to be made into a detection transmission integrated scintillation ceramic source rod with specific length and specific diameter, and the fusion zone is butt jointed by using a seed crystal and lifted and fed to form an optical fiber.
In some embodiments, when the growth method in step S2 is a micro-pulldown method or a guided mode method, the single crystal optical fiber powder in step S1 and the scintillating single crystal optical fiber powder in step S1 are directly used without manufacturing a scintillating ceramic source rod integrating detection and transmission, specifically:
when the micro-downdraw method is adopted, the following steps are adopted: and adding monocrystalline optical fiber powder and scintillating monocrystalline optical fiber powder into the crucible in sequence at different stages, melting the monocrystalline optical fiber powder and the scintillating monocrystalline optical fiber powder at high temperature, enabling the melt of the monocrystalline optical fiber powder and the melt of the scintillating monocrystalline optical fiber powder to flow out through capillary holes at the bottom of the crucible under the action of gravity, enabling seed crystals to contact the melt flowing out from the bottom of the crucible, continuously pulling downwards, and controlling the pull-down speed and the heating power to realize the growth of the optical fiber, so as to finally obtain the scintillation monocrystalline optical fiber integrating detection and transmission.
For example, the scintillation single crystal optical fiber powder is added into the crucible, the scintillation single crystal optical fiber powder melt after high temperature melting flows out through the capillary holes at the bottom of the crucible, the scintillation single crystal optical fiber starts to grow into the scintillation single crystal optical fiber under the guidance of the seed crystal, when the design length is reached, the single crystal optical fiber powder is added, after high temperature melting, the scintillation single crystal optical fiber powder flows out from the capillary holes at the bottom of the crucible and is connected with the tail part of the scintillation single crystal optical fiber, and after the scintillation single crystal optical fiber continues to grow to the design size, the coupling-free detection and transmission integrated scintillation single crystal optical fiber is obtained.
When the guided mode method is adopted, the following steps are: the method is characterized in that the single crystal optical fiber powder and the scintillating single crystal optical fiber powder are sequentially added into a special mould at different stages, the special mould adopted by the guided mode method is provided with an inner cavity for containing melt, the special mould is similar to a crucible, the inner cavity is provided with a capillary slit, the melt can rise to the top outlet of the capillary slit by utilizing capillary action, at the moment, seed crystals are contacted with the melt and pulled upwards, and the growth of the optical fiber is realized by controlling the pull-up speed and heating power.
For example, adding monocrystalline fiber powder into the inner cavity of the special die, guiding the melt of the monocrystalline fiber powder after high-temperature melting to flow to the top of the capillary slit under the action of the capillary, starting growth under the traction of seed crystals, adding scintillating monocrystalline fiber powder into the inner cavity of the special die when the design length is reached, flowing out of the top of the capillary slit after high-temperature melting, connecting with the tail of the monocrystalline fiber powder, and continuing to grow to the design size, thereby obtaining the coupling-free detection and transmission integrated scintillating monocrystalline fiber.
It should be noted that, in the above two methods, the addition sequence of the single crystal optical fiber powder and the scintillation single crystal optical fiber powder may be determined according to the actual preparation condition, and the present invention is not limited to the addition sequence of the two powders.
In some embodiments, the method further comprises the step of machining the detection-transmission integrated scintillation single crystal optical fiber produced in step S2, including: s3, cutting, grinding and polishing the detection and transmission integrated scintillation single crystal optical fiber to obtain the detection and transmission integrated scintillation single crystal optical fiber meeting the use specification.
Preferably, the processing length of the scintillation single crystal optical fiber integrated with detection and transmission is 0.1-10000 mm.
Example 3
On the basis of the embodiment 1 and the embodiment 2, the invention also provides an application of the detection transmission integrated scintillation single crystal optical fiber, the detection transmission integrated scintillation single crystal optical fiber is coupled with the photosensitive element, and the reflection layer is adopted for wrapping and packaging, so that a radiation detection module is obtained, and the applicable fields of the radiation detection module comprise: high energy physics, nuclear safety, environmental monitoring, radiation therapy and other strong radiation resistant fields.
Preferably, the photosensitive element includes, but is not limited to, a photodiode, a photomultiplier tube, a silicon photomultiplier tube, and the like.
More preferably, the detection transmission integrated scintillation single crystal optical fiber and the photosensitive element are coupled in the following manner: the photosensitive element is coupled to the end of the transmission unit T not connected to the detection unit D.
In order to better understand and apply the scheme and effectively demonstrate the corresponding benefits, the detection and transmission integrated scintillation single crystal optical fiber, the preparation method and the application thereof are further described below with reference to specific embodiments.
Example 4
On the basis of the embodiment, the embodiment provides a LuAG-Ce (0.1 at%) -LuAG detection transmission integrated scintillation single crystal optical fiber.
Wherein the matrix of the detection unit D is LuAG, the luminescent ion is Ce, and the atomic percentage of Ce is 0.1at%.
The matrix of the transfer unit T is LuAG.
The preparation method comprises the following steps:
S1, proportioning: the scintillation single crystal optical fiber powder Ce 0.003Lu2.997Al5O12 doped with luminescent ions and the single crystal optical fiber powder Lu 3Al5O12 are respectively prepared. The method specifically comprises the following steps:
S10, taking high-purity powder of a scintillation single crystal optical fiber matrix LuAG and high-purity powder of luminescent ions Ce as raw materials, and respectively putting the two raw material powders into an oven to bake for 12 hours to remove water and CO 2.
S11, respectively weighing matrix LuAG raw material powder and luminescent ion Ce raw material powder of the scintillation single crystal optical fiber according to stoichiometric proportion, placing the raw material powder into a mortar, adding absolute ethyl alcohol, and fully grinding to obtain first mixed powder.
S12, filling the first mixed powder into rubber balls, and applying 2000Mpa pressure in a cold isostatic press for 10min to obtain a first bar-shaped raw material.
S13, placing the first rod-shaped raw material into a crucible, then placing into a muffle furnace, calcining at 1650 ℃ for 10 hours, and then cooling to room temperature. And (3) putting the calcined first rod-shaped raw material into a mortar for full grinding, so as to obtain the scintillation single crystal optical fiber powder Ce 0.003Lu2.997Al5O12 doped with luminescent ions.
S14, taking the matrix LuAG of the single crystal optical fiber, placing the matrix LuAG in a mortar, and fully grinding to obtain second mixed powder.
S15, filling the second mixed powder into rubber balls, and applying 2000Mpa pressure in a cold isostatic press for 10min to obtain a second bar-shaped raw material.
S16, placing the second rod-shaped raw material into a crucible, then placing into a muffle furnace, calcining at 1650 ℃ for 10 hours, and then cooling to room temperature. And (3) putting the calcined second rod-shaped raw material into a mortar for full grinding, and obtaining the monocrystal optical fiber powder Lu 3Al5O12.
S2, optical fiber growth: the growth method of the laser heating base method is adopted to prepare the scintillation single crystal optical fiber with integrated detection and transmission. The method specifically comprises the following steps:
S20, placing the scintillation single crystal optical fiber powder Ce 0.003Lu2.997Al5O12 and the single crystal optical fiber powder Lu 3Al5O12 obtained in the step S1 into an oven to be dried for 3 hours, and fully removing the absolute ethyl alcohol.
S21, pouring the dried scintillation single crystal optical fiber powder Ce 0.003Lu2.997Al5O12 and the single crystal optical fiber powder Lu 3Al5O12 into rubber balls according to the design length, and pressing for 10min by applying 200Mpa pressure in a cold isostatic press to obtain the rod-shaped raw material.
The rod-shaped raw material can be understood as that one end of the detecting unit D is fixedly connected with one end of the transmission unit T, so that a coupling-free integrated structure is formed.
S22, placing the rod-shaped raw materials into a crucible, placing the crucible into a muffle furnace, calcining for 10 hours at the temperature of 1200 ℃, and cooling to room temperature along with the furnace after calcining, so that the detection and transmission integrated scintillation ceramic source rod can be obtained.
Further, the calcined rod-shaped raw material is cut into a detection and transmission integrated scintillating ceramic source rod with the bottom side length of 1.5mm multiplied by 1.5 mm.
S23, placing the obtained detection and transmission integrated scintillating ceramic source rod in a laser heating base furnace, and fixing the other end of the detection unit D (Ce 0.003Lu2.997Al5O12) on a blanking rod and fixing a seed crystal containing a single crystal optical fiber matrix on the seed crystal rod as one end of the detection unit D (Ce 0.003Lu2.997Al5O12) on the detection and transmission integrated scintillating ceramic source rod is fixedly connected with one end of the transmission unit T (Lu 3Al5O12), wherein the other end of the transmission unit T (Lu 3Al5O12) faces the seed crystal, and simultaneously adjusting the positions of the detection and transmission integrated scintillating ceramic source rod and the seed crystal so that the detection and transmission integrated scintillating ceramic source rod and the position of the seed crystal are positioned on the same straight line with a laser gathering point.
S24, sealing the furnace chamber, vacuumizing to below 1.0E -1, introducing nitrogen to adjust the pressure of the furnace chamber to 1.008Mpa, and then heating by laser to enable one end of the transmission unit T (Lu 3Al5O12) to be melted into a hemispherical melting zone.
S25, butting seed crystals with the hemispherical melting zone, adjusting power, observing for 2min until the butting is stable, and then performing stable growth at a pulling speed of 20mm/h and a feeding speed of 6.98mm/h to obtain the scintillation single crystal optical fiber integrating detection and transmission.
S26, setting the power-reducing time to be 1h, and taking out the LuAG-Ce (0.1 at%) -LuAG detection and transmission integrated scintillation single crystal optical fiber after the temperature of the detection and transmission integrated scintillation single crystal optical fiber and the temperature in the cavity of the laser heating base furnace are reduced to the room temperature.
The light emission spectrum of radiation collected by the end face of the detection transmission unit T is shown in figure 4, and the distribution of Z-shaped elements of the transmission unit T is shown in figure 5 by adopting a Mini X-ray source (40 kV,80 mu A) and exciting the LuAG-Ce (0.1 at%) -LuAG detection transmission integrated scintillation single crystal optical fiber provided by the embodiment at different positions.
The gamma rays (59.5 KeV) of 241Am source are adopted to perform equidistant radiation excitation, the LuAG-Ce (0.1 at%) -LuAG detection and transmission integrated scintillation single crystal optical fiber provided by the embodiment is adopted, multi-channel energy spectrums at different positions collected by the end face of the detection unit D are shown in figure 5, multi-channel energy spectrums at different positions collected by the end face of the transmission unit T are shown in figure 6, and the correlation between the energy spectrum full-energy peak addresses collected by the end face of the detection unit D and the end face of the transmission unit T and the excitation position is shown in figure 7.
Example 5
The embodiment provides a scintillation single crystal optical fiber integrating detection and transmission of LuAG and Ce (0.5 at%).
Reference example 4 differs in that:
Wherein the matrix of the detection unit D is LuAG, the luminescent ion is Ce, and the atomic percentage of Ce is 0.5at%.
In the step S1, a scintillation single crystal optical fiber powder Ce 0.015Lu2.998Al5O12 doped with luminescent ions and a single crystal optical fiber powder Lu 3Al5O12 are prepared respectively.
The remaining preparation steps were the same as in example 5.
Example 6
The embodiment provides a LuAG: pr (0.3 at%) -LuAG detection transmission integrated scintillation single crystal fiber.
Reference example 4 differs in that:
Wherein the matrix of the detection unit D is LuAG, the luminescent ion is Pr, and the atomic percentage of Pr is 0.3at%.
In the step S1, scintillation single crystal optical fiber powder Pr 0.009Lu2.991Al5O12 doped with luminescent ions and single crystal optical fiber powder Lu 3Al5O12 are respectively prepared.
The remaining preparation steps were the same as in example 5.
Example 7
The embodiment provides a scintillation single crystal optical fiber integrating LuAG, yb (1 at%) -LuAG detection and transmission.
Reference example 4 differs in that:
Wherein the matrix of the detection unit D is LuAG, the luminescent ion is Yb, and the atomic percentage of Yb is 1at%.
In the step S1, scintillation single crystal optical fiber powder Yb 0.03Lu2.97Al5O12 doped with luminescent ions and single crystal optical fiber powder Lu 3Al5O12 are respectively prepared.
The remaining preparation steps were the same as in example 5.
Example 8
Based on the above embodiments, the present embodiment provides a specific application manner of the detection-transmission integrated scintillation single crystal optical fiber.
(1) The detection unit D in example 5 is LuAG: ce (0.5 at%), and the transmission unit T is a detection transmission integrated scintillation single crystal fiber of LuAG, wherein the diameters and lengths of the detection unit D and the transmission unit T are phi 1mm×50mm and phi 1mm×200mm respectively.
(2) Except for the end face (the end which is not connected with the detection unit D) of the transmission unit T, 1 layer of enhanced specular reflection sheet (ESR) with the thickness of 65 microns is adopted as a light reflection layer, and the rest part of the detection and transmission integrated scintillation single crystal optical fiber is uniformly wrapped so as to collect scintillation light emitted by the detection unit D as efficiently as possible.
(3) The end face of the unwrapped ESR was coupled with 1S 1226-18BK photodiode manufactured by Binsony corporation and packaged in an aluminum alloy housing to form a radiation detection module.
(4) The signal of the radiation detection module is connected to the signal acquisition system and placed in a strong X-ray field, so that the spatial distribution of the X-ray irradiation dose and the time-varying information can be obtained.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (10)

1. A detection and transmission integrated scintillation single crystal optical fiber is characterized in that,
The device comprises a detection unit D and a transmission unit T, wherein one end of the detection unit D is connected with one end of the transmission unit T to form a coupling-free integrated structure;
the detection unit D is a scintillation single crystal optical fiber which comprises luminescent ions and a matrix;
The transmission unit T is a single crystal optical fiber that is transparent to the scintillation light of the detection unit D.
2. The detection-transmission-integrated scintillation single-crystal optical fiber as recited in claim 1, wherein,
The matrix of the scintillation single crystal optical fiber is any one of LuAG、YAG、LuYAG、LuGdAG、GYGG、GYAG、TbAG、GAGG、GGG、BGO、PbWO4、LuAP、YAP、LuYAP、LuS cAP、YScAP、LuGAP、Lu2O3、Y2O3、Sc2O3、Gd2O3、Ga2O3、(LuxY1-x)2O3、(LuxSc1-x)2O3、(YxSc1-x)2O3、LYSO、LSO、LGSO、CaF2 and SrF 2.
3. The detection-transmission-integrated scintillation single-crystal optical fiber as recited in claim 1, wherein,
The luminescent ion is one or more of Ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb, bi, ti, cr, mn, fe, co, ni, cu and Zn.
4. The detection-transmission-integrated scintillation single-crystal optical fiber as recited in claim 1, wherein,
The diameter d of the detection transmission integrated scintillation single crystal optical fiber is 0.01-10mm.
5. The detection-transmission-integrated scintillation single-crystal optical fiber as recited in claim 1, wherein,
The length of the detection transmission integrated scintillation single crystal optical fiber is L0.1-100000 mm;
The length of the detection unit D is 0.5-30mm, and the length of the transmission unit T is greater than or equal to 0.1mm.
6. A method for producing a scintillation single crystal optical fiber with integrated detection and transmission as claimed in any one of claims 1 to 5, comprising the steps of:
S1, proportioning: preparing scintillation single crystal optical fiber powder doped with luminescent ions and single crystal optical fiber powder respectively;
S2, optical fiber growth: the detection and transmission integrated scintillation single crystal optical fiber is prepared by adopting any one growth method of a laser heating base method, an optical floating zone method, a micro-drop-down method or a guided mode method.
7. The method according to claim 6, wherein,
When the growth method is a laser heating susceptor method, the method comprises the following steps:
S21, pouring the scintillating single crystal optical fiber powder and the single crystal optical fiber powder into a sealed elastic die according to the design length, and pressing the scintillating single crystal optical fiber powder and the single crystal optical fiber powder into an integrated structure through a static pressure machine to obtain a rod-shaped raw material;
S22, calcining the rod-shaped raw material, and cutting the calcined rod-shaped raw material into a preset size to obtain a detection and transmission integrated scintillating ceramic source rod;
s23, placing the detection and transmission integrated scintillating ceramic source rod in a laser heating base furnace, fixing one end of the detection unit D on a blanking rod, and fixing seed crystals containing the monocrystal optical fiber matrixes on seed crystal rods;
S24, sealing the furnace chamber, vacuumizing, introducing nitrogen to adjust the air pressure, and heating by laser to enable one end of the transmission unit T to be melted into a hemispherical melting zone;
and S25, butting the seed crystal with the hemispherical melting zone, and after the butting is stable, carrying out stable growth at a preset pulling speed and a preset feeding speed to finally obtain the detection and transmission integrated scintillation single crystal optical fiber.
8. The method according to claim 6, wherein,
When the growth method is a micro-drop-down method or a guided mode method, the method comprises the following steps:
And sequentially adding the single crystal optical fiber powder and the scintillation single crystal optical fiber powder into a crucible or a special die at different stages, melting the powder at high temperature, and growing the melt of the single crystal optical fiber powder and the melt of the scintillation single crystal optical fiber powder through capillary holes on the crucible or the special die under the guidance of seed crystals to finally obtain the scintillation single crystal optical fiber with integrated detection and transmission.
9. The method according to claim 6, wherein,
In the step S1, the preparation steps of the scintillation single crystal optical fiber powder doped with luminescent ions include:
S11, respectively weighing the matrix of the scintillation single crystal optical fiber and the luminescent ions according to stoichiometric proportions, placing the matrix and the luminescent ions in a mortar, adding a mixing agent, and fully grinding to obtain first mixed powder;
s12, pressing the first mixed powder into a first rod-shaped raw material;
S13, calcining and grinding the first rod-shaped raw material to obtain the scintillating single crystal optical fiber powder; and/or the number of the groups of groups,
The preparation method of the single crystal optical fiber powder comprises the following steps:
s14, placing the matrix of the single crystal optical fiber in a mortar, and grinding to obtain second mixed powder;
s15, pressing the second mixed powder into a second bar-shaped raw material;
S16, calcining and grinding the second rod-shaped raw material to obtain the single crystal optical fiber powder.
10. An application of a detection and transmission integrated scintillation single crystal optical fiber is characterized in that,
Coupling the detection-transmission-integrated scintillation single-crystal optical fiber according to any one of claims 1 to 5 or the detection-transmission-integrated scintillation single-crystal optical fiber manufactured by the manufacturing method according to any one of claims 6 to 9 with a photosensitive element, and wrapping and packaging by adopting a reflecting layer to obtain a radiation detection module, wherein the radiation detection module is applied to the field of strong irradiation resistance.
CN202410031343.8A 2024-01-09 2024-01-09 Detection and transmission integrated scintillation single crystal optical fiber and preparation method and application thereof Pending CN117950106A (en)

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