CN114959872A - Preparation method of p-terphenyl organic scintillation monocrystal - Google Patents

Preparation method of p-terphenyl organic scintillation monocrystal Download PDF

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CN114959872A
CN114959872A CN202210479060.0A CN202210479060A CN114959872A CN 114959872 A CN114959872 A CN 114959872A CN 202210479060 A CN202210479060 A CN 202210479060A CN 114959872 A CN114959872 A CN 114959872A
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crucible
crystal
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马捷
许文斌
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Beijing University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/02—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method without using solvents
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/006—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/54—Organic compounds
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/2055—Analysing diffraction patterns
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/20—Measuring radiation intensity with scintillation detectors
    • G01T1/202—Measuring radiation intensity with scintillation detectors the detector being a crystal

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Abstract

A preparation method of a p-terphenyl organic scintillation monocrystal belongs to the field of organic scintillation crystals. The synthesis method comprises weighing a certain amount of p-terphenyl powder with purity of 99%, placing into a single-layer ampoule, and rapidly vacuumizing to 10% ‑4 Pa. After the vacuum degree meets the growth requirement, the ampoule is sealed by welding by using an oxyacetylene flame method, and the lower part of the ampoule is wrapped by wet cloth soaked in cold water before sealing. Packaging, setting the temperature of the high-temperature region not more than 220 ℃ and the lowest temperature of the low-temperature region to 180 ℃, adjusting the temperature gradient of the growth furnace to 4-6 ℃/cm, placing the ampoule at the high-temperature region of the growth furnace, after the raw materials are completely melted, performing crystal growth at the falling speed of 0.5mm/h, wherein the content of impurities in the crystal is lowThe crystal has good quality, stable performance and good fluorescence performance.

Description

Preparation method of p-terphenyl organic scintillation single crystal
Technical Field
The invention belongs to the technical field of organic scintillation crystal application, and particularly relates to optimization of a preparation process of a p-terphenyl organic scintillation single crystal.
Background
When high-energy particles or rays act on the scintillation crystal, electrons in the crystal are excited to a higher energy level, and when the electrons return to a low energy state, excess energy is released in a manner of emitting photons, and finally fluorescence is generated. The essence is the process by which the crystal converts the kinetic energy of high energy rays or particles into light energy. Scintillation crystals are classified into two categories, one being inorganic scintillation crystals and the other being organic scintillation crystals, according to their chemical composition. The inorganic scintillation crystal is mostly ion or atom crystal, and the constituent units are combined by covalent bond or ionic bond, so that the inorganic scintillation crystal is more convenient to be applied in reality, and the preparation process of the inorganic scintillation crystal reaches a relatively mature state from the initial mineral crystal to various artificial inorganic scintillation crystals at present. Most of the organic scintillating crystals are composed of large-chain organic molecules which are arranged and combined with each other by van der Waals force. Compared with inorganic scintillation crystals, organic scintillation crystals are difficult to prepare, and related preparation processes are not mature.
Para-terphenyl, also known as para-diphenylbenzene, is an aromatic compound consisting of three benzene rings, and is a white flaky crystal, and the crystal structure at room temperature belongs to a monoclinic system P2 1 A space group. Can be used as organic scintillator and is the light-emitting object of scintillation counter. Para-terphenyl organic scintillation crystals are one of the most common organic scintillation crystals. With the continuous progress of the technology, various organic materials with special functions are developed successively, and the process demand for preparing large-sized organic crystals in actual production is more urgent. The p-terphenyl scintillation crystal serving as a common organic scintillation crystal not only has good time sequence response capability, good scintillation efficiency, larger absorption coefficient and quantum yield, but also has the advantages of difficult surface deterioration, no moisture absorption and high radiation resistance. Has wide application prospect in the fields of radiation detection, microwave lasing, high-energy physics and the like.
At present, the growth research on the terphenyl single crystal is carried out at home and abroad, however, the general development level of the domestic terphenyl crystal is far behind abroad and still in the technical research and development stage, and the grown crystal has small size and unstable performance and can not meet the actual production requirement. Therefore, the invention aims to grow the p-terphenyl crystal with large size and high quality, and has important significance for the application of the crystal in practical production.
Disclosure of Invention
The invention aims to grow the high-quality large-size p-terphenyl single crystal which can be applied to actual industrial production, and the p-terphenyl single crystal has the advantages of low impurity content, good crystallization quality, stable performance, good fluorescence performance and contribution to the application of scintillation detection.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a p-terphenyl organic scintillation crystal comprises the following steps:
s1 designing a single-layer crucible; the shape of the single-layer crucible is designed into a cavity structure: the upper end is the tubbiness, and size location phi 12mm is 200mm, and the lower part is the funnel and the funnel neck is the taper point that the diameter gradually diminishes, and the pointed end seals, and the taper point half cone angle sets for 30 according to the equipment condition, and funnel neck axial total length are 3 ~ 5mm, and the top of tubbiness structure is equipped with the capillary intercommunication and is regarded as charge door and evacuation mouth. The specific structure is shown in fig. 1.
S2, filling raw materials; filling a prepared p-terphenyl raw material with the purity of 99 percent into a prepared crucible in a glove box, and paying attention to the fact that the tip part of the crucible is tightly filled to avoid gaps; after the charging is finished, the crucible is arranged on a molecular vacuum pump and is vacuumized to 10 DEG -4 Pa, and performing welding sealing;
s3 sealing the crucible; after the vacuum degree in the crucible meets the growth requirement, the crucible is sealed by welding, the funnel and the part of the funnel neck are wrapped by wet cloth soaked in cold water before the sealing by welding, and the crucible is sealed by welding by using an oxyacetylene flame method;
s4 designing growth process parameters; after the crucibles are packaged, a temperature field of the growth furnace is modulated, the gradient of the modulation temperature field is 4-6 ℃/cm, the temperature is gradually reduced from top to bottom, the temperature of a corresponding high-temperature area is not more than 220 ℃, the lowest temperature of a low-temperature area is set to be 180 ℃, a barrel-shaped position corresponding to the single-layer crucible is arranged at the position of the high-temperature area of the growth furnace, after raw materials are completely melted, the descending speed of the crucible is set to be 0.5mm/h, crystal growth is started from the high-temperature area to the low-temperature area from top to bottom, and finally, a p-terphenyl single crystal with the size of phi 12mm multiplied by 200mm is grown as shown in figure 2;
preparing a single crystal sample of S5; and after the crystal growth is finished, the crucible is slowly cut off by using a diamond knife, so that the generation of crystal cracks is avoided, and then the crystal is taken out. Selecting a growing crystal single crystal area, and cutting off a tail polycrystalline part by using a diamond cutting machine; the cutting speed is then slowed down, a single-crystal wafer is cut in the single-crystal area as shown in fig. 3, and is subjected to subsequent characterization processing.
Compared with the prior art, the common growth of the p-terphenyl single crystal adopts a double-layer crucible, the growth is carried out by using a Bridgman-Stockbarge method, the structure of the crucible is complicated, the preparation is difficult, and the raw materials are filled between the double walls during the growth, so the waste of the raw materials also limits the size of the crystal growth. The invention has the advantages that the single-layer crucible is adopted, the crystal growth is carried out by adjusting the technological parameters of the Bridgman-Stockbarger method, the structure is simple, the limitation to the crystal size is small, and the practical production is more convenient. XRD diffraction and rocking curve results of the prepared p-terphenyl crystal show that the p-terphenyl crystal is a single crystal (shown in figure 4) with good quality, less defects and impurities (shown in figure 5), larger excitation range (shown in figure 6) and short fluorescence attenuation life (shown in figure 7), and is favorable for application in scintillation detection.
Drawings
FIG. 1 is a schematic structural diagram of a crucible used for growth, and the design of a capillary tube at the lower end of the crucible enables a crystal nucleus which grows rapidly in one direction to inhibit crystal nuclei growing in other directions from preferentially growing, and finally a certain single-orientation crystal nucleus is generated and grown into a crystal, wherein the diameter size is selected to be 12mm, so that cracking of the crystal caused by overlarge temperature gradient of a radial temperature field can be avoided.
FIG. 2 is a crystal diagram of p-terphenyl grown in example 3
FIG. 3 is a single crystal sample prepared in example 3; as can be seen from FIGS. 2 and 3, the whole crystal is complete and transparent, no obvious crack is generated, and the quality of the grown crystal is high.
FIG. 4 is a powder XRD diffraction pattern of the crystal prepared in example 3 and a rocking curve at the (002) crystal plane of the single crystal compared with the standard card JCPDS 39-1727, the position and relative intensity of the diffraction peak are substantially identical to the standard card, and no other hetero-phase peak appears. The result proves that the grown crystal is pure p-terphenyl phase, and the peak shape is symmetrical, no impurity peak appears and the full width at half maximum is 175 arcsec by testing the rocking curve of the (002) crystal face, which indicates that the crystal has good crystallization quality.
FIG. 5 is the fluorescence emission spectrum of example 3 corresponding to the excitation wavelength of 290nm on a terphenyl single crystal, and it can be seen that the highest emission peak appears at 370.8nm, and one emission peak appears at 388nm at the shoulder. Corresponding to the interaction between different excited states or between vicinal hydrogens, respectively. The peak position occurs less because defects and impurities in the crystal molecules capture excited electrons and emit fluorescence, so that a new emission peak appears in the fluorescence spectrum and the emission peak is widened, so that the peak position does not occur as a result of the decrease in defects and impurities in the crystal.
FIG. 6 is an excitation spectrum of a terphenyl crystal of example 3. During measurement, the range of the excitation wavelength is 210-330 nm, and the intensity change of the 370nm emission peak is collected correspondingly. From the figure we can see that when the wavelength of the excitation light is 276.4nm, the intensity reaches a maximum and then levels off, and the optimum excitation range of the crystal is larger.
FIG. 7 is a graph showing the fluorescence decay of the terphenyl crystals of example 3. The fluorescence decay life at 372nm is 2.16ns, so that the fluorescence decay life of the grown p-terphenyl single crystal is short, and the application in the aspect of scintillation detection is facilitated.
Fig. 8 is a photograph of the p-terphenyl crystals prepared in example 1. It was found that crystals grown at a crucible descending speed of 1.5mm/h exhibited severe cracking.
Fig. 9 is a photograph of a p-terphenyl crystal prepared in example 2. It was found that the phenomenon of crystal cracking, which occurs at a falling rate of 1mm/h, is relatively reduced.
Fig. 10 is a photograph of a p-terphenyl crystal prepared in example 3. It was found that the crystals grown at the 0.5mm/h descent rate did not cause cracks.
Detailed Description
The present invention will be further described with reference to the following embodiments, but the scope of the present invention is not limited to the following embodiments.
The single-layer crucible in the S1 has simple structure, small limitation on the crystal size and more convenient practical production. The design of the capillary at the lower end of the crystal nucleus generator ensures that the crystal nucleus which grows rapidly in a certain direction inhibits the crystal nucleus which grows in other directions from growing preferentially, finally, a certain single-orientation crystal nucleus is generated and grows into a crystal, the diameter size is selected to be 12mm, and the cracking of the crystal caused by overlarge temperature gradient of a radial temperature field can be avoided; s2, the crucible is vacuumized and sealed, so that the p-terphenyl raw material grows under the vacuum condition, and the p-terphenyl raw material can be prevented from being oxidized due to high temperature in the subsequent operation process; in the S3, the part below the long neck of the ampoule is wrapped by wet cloth soaked in cold water before welding and sealing, so that the generation of new impurities caused by oxidation of raw materials at high temperature in the welding and sealing process can be avoided; in S4, the melting point of the p-terphenyl crystals is 214 ℃, if the temperature of the p-terphenyl crystals is increased after the p-terphenyl crystals are melted, liquid p-terphenyl can continuously volatilize, the temperature is not too high for avoiding the large-amount volatilization of the p-terphenyl, the highest temperature is set to be 220 ℃, the lowest temperature is set to be 180 ℃, the temperature gradient is about 4-6 ℃/cm, the power of crystallization is ensured, the descending speed is selected to be 0.5mm/h, the growth efficiency of the crystals is ensured, and the crystals are prevented from cracking caused by stress due to the fact that the descending speed is too high.
Example 1 (comparative example)
S1 designing a single-layer crucible; the shape of the single-layer crucible is designed to be that the upper end is positioned with the size phi of 12mm multiplied by 200mm, the lower part is in a funnel shape, the half cone angle is set to be 30 degrees according to the equipment condition, and the total length is 3-5 mm; the specific structure is shown in fig. 1.
S2 filling raw materials; the prepared crucible was filled with a pre-prepared p-terphenyl material having a purity of 99% in a glove box, taking care that the tip portion of the crucible was filled tightly to avoid voids. After the charging is finished, the crucible is arranged on a molecular vacuum pump and is vacuumized to 10 DEG -4 Pa, and performing welding seal.
S3, sealing the crucible by welding; after the vacuum degree in the crucible meets the growth requirement, the crucible is sealed by welding, and the part below the long neck of the ampoule is wrapped by wet cloth soaked in cold water before sealing by welding. The crucible was sealed using an oxyacetylene flame method.
S4 designing growth process parameters; after the crucible is packaged, the temperature field of the growth furnace is adjusted, and the temperature gradient is adjusted to 4-6 ℃. The temperature of the high-temperature area is 220 ℃, the lowest temperature of the low-temperature area is set to be 180 ℃, the ampoule is placed at the position of the high-temperature area of the growth furnace, after the raw materials are completely melted, the descending speed of the crucible is set to be 1.5mm/h, crystal growth is started, and finally, the p-terphenyl single crystal with the size of phi 12mm multiplied by 200mm is grown, as shown in figure 8, and cracks exist.
Example 2 (comparative example)
S1 designing a single-layer crucible; the shape of the single-layer crucible is designed into a capillary tube with the upper end dimension positioning phi 12mm multiplied by 200mm, the lower part presenting a funnel-shaped half cone angle set to be 30 degrees according to the equipment condition, and the total (3-5) mm of the funnel and the funnel neck. The specific structure is shown in fig. 1.
S2 filling raw materials; the prepared crucible was filled with a pre-prepared p-terphenyl material having a purity of 99% in a glove box, taking care that the tip portion of the crucible was filled tightly to avoid voids. After the charging is finished, the crucible is arranged on a molecular vacuum pump and is vacuumized to 10 DEG -4 Pa, and performing welding seal.
S3 sealing the crucible; after the vacuum degree in the crucible meets the growth requirement, the crucible is sealed by welding, and the part below the long neck of the ampoule is wrapped by wet cloth soaked in cold water before sealing by welding. The crucible was sealed using an oxyacetylene flame method.
S4 designing growth process parameters; after the crucible is packaged, the temperature field of the growth furnace is adjusted, and the temperature gradient is adjusted to 4-6 ℃. The temperature of the high-temperature area is 220 ℃, the lowest temperature of the low-temperature area is set to be 180 ℃, the ampoule is placed at the position of the high-temperature area of the growth furnace, after the raw materials are completely melted, the descending speed of the crucible is set to be 1mm/h, crystal growth is started, and finally, the p-terphenyl single crystal with the size of phi 12mm multiplied by 200mm is grown, as shown in figure 9, and cracks exist.
Example 3
S1 designing a single-layer crucible; the shape of the single-layer crucible is designed to be that the upper end is positioned with the size phi of 12mm multiplied by 200mm, the lower part is in a funnel shape half cone angle which is set to be 30 degrees according to the equipment condition, the total length (3-5) mm of the funnel and the funnel neck is shown in figure 1.
S2 filling raw materials; the prepared crucible was filled with a pre-prepared p-terphenyl material having a purity of 99% in a glove box, taking care that the tip portion of the crucible was filled tightly to avoid voids. In thatAfter the charging, the crucible is arranged on a molecular vacuum pump and is vacuumized to 10 DEG -4 Pa, and performing welding seal.
S3 sealing the crucible; after the vacuum degree in the crucible meets the growth requirement, the crucible is sealed by welding, and the part below the long neck of the ampoule is wrapped by wet cloth soaked in cold water before sealing by welding. The crucible was sealed using an oxyacetylene flame method.
S4 designing growth process parameters; after the crucible is packaged, the temperature field of the growth furnace is adjusted, and the temperature gradient is adjusted to 4-6 ℃. The temperature of the high-temperature area is 220 ℃, the lowest temperature of the low-temperature area is set to be 180 ℃, the ampoule is placed at the position of the high-temperature area of the growth furnace, after all raw materials are melted, the descending speed of the crucible is set to be 0.5mm/h, crystal growth is started, and finally, the p-terphenyl single crystal with the size of phi 12mm multiplied by 200mm is grown as shown in a figure 10 and is complete and has no cracks.

Claims (1)

1. A preparation method of a p-terphenyl organic scintillation crystal is characterized by comprising the following steps:
s1 designing a single-layer crucible; the shape of the single-layer crucible is designed into a cavity structure: the upper end is barrel-shaped, the size is positioned to be phi 12mm multiplied by 200mm, the lower part is a funnel, the funnel neck is a cone-shaped tip with the diameter gradually reduced, the tip is closed, the half cone angle of the cone-shaped tip is set to be 30 degrees according to the equipment condition, the axial total length of the funnel and the funnel neck is 3-5 mm, and the top of the barrel-shaped structure is provided with a capillary tube which is communicated with a feeding port and a vacuum pumping port;
s2, filling raw materials; filling a prepared p-terphenyl raw material with the purity of 99 percent into a prepared crucible in a glove box, and paying attention to the fact that the tip part of the crucible is tightly filled to avoid gaps; after the charging is finished, the crucible is arranged on a molecular vacuum pump and is vacuumized to 10 DEG -4 Pa, and performing welding sealing;
s3 sealing the crucible; after the vacuum degree in the crucible meets the growth requirement, the crucible is sealed by welding, the funnel and the part of the funnel neck are wrapped by wet cloth soaked in cold water before sealing by welding, and the crucible is sealed by welding by using an oxyacetylene flame method;
s4 designing growth process parameters; after the crucibles are packaged, modulating a temperature field of the growth furnace, wherein the gradient of the modulation temperature field is 4-6 ℃/cm, the temperature is gradually reduced from top to bottom, the temperature of a corresponding high-temperature area is not more than 220 ℃, the lowest temperature of a low-temperature area is set to be 180 ℃, a barrel-shaped position corresponding to the single-layer crucible is arranged at the position of the high-temperature area of the growth furnace, after raw materials are completely melted, the descending speed of the crucible is set to be 0.5mm/h, crystal growth is started from the high-temperature area to the low-temperature area from top to bottom, and finally, a p-terphenyl single crystal with the size of phi 12mm multiplied by 200mm is grown;
preparing a single crystal sample of S5; and after the crystal growth is finished, the crucible is slowly cut off by using a diamond knife, so that the generation of crystal cracks is avoided, and then the crystal is taken out. Selecting a growing crystal single crystal area, and cutting off a tail polycrystalline part by using a diamond cutting machine; then, the cutting speed is slowed down, and the single crystal wafer is cut in the single crystal area.
CN202210479060.0A 2022-05-05 2022-05-05 Preparation method of p-terphenyl organic scintillation monocrystal Pending CN114959872A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104072327A (en) * 2013-03-26 2014-10-01 江苏中能化学有限公司 A preparing method of para-terphenyl
CN209024672U (en) * 2018-04-17 2019-06-25 湖北理工学院 A kind of double-deck ampoule of Fuse Type sealing
CN209024671U (en) * 2018-04-17 2019-06-25 湖北理工学院 A kind of filling auxiliary seal bilayer ampoule

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104072327A (en) * 2013-03-26 2014-10-01 江苏中能化学有限公司 A preparing method of para-terphenyl
CN209024672U (en) * 2018-04-17 2019-06-25 湖北理工学院 A kind of double-deck ampoule of Fuse Type sealing
CN209024671U (en) * 2018-04-17 2019-06-25 湖北理工学院 A kind of filling auxiliary seal bilayer ampoule

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
冯玉祥: "对三联苯晶体生长的数值模拟与实验研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, vol. 2019, no. 03, pages 014 - 346 *
许文斌 等: "对三联苯有机晶体的生长及性能", 《人工晶体学报》, vol. 50, no. 10, pages 1979 - 1983 *

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Application publication date: 20220830