CN104667562A - Organic material bi-directional vacuum sublimation purification equipment and continuous or non-continuous purifying method - Google Patents
Organic material bi-directional vacuum sublimation purification equipment and continuous or non-continuous purifying method Download PDFInfo
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- CN104667562A CN104667562A CN201510046229.3A CN201510046229A CN104667562A CN 104667562 A CN104667562 A CN 104667562A CN 201510046229 A CN201510046229 A CN 201510046229A CN 104667562 A CN104667562 A CN 104667562A
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Abstract
The invention relates to the technical field of organic material purification equipment and in particular relates to organic material bi-directional vacuum sublimation purification equipment and a continuous or non-continuous purifying method, belonging to the field of the physical vapor deposition technology. The organic material bi-directional vacuum sublimation purification equipment comprises a vacuum cavity, a vacuumizing device and a cooling device, wherein a valve and a quartz tube assembly with openings at two ends are arranged in the vacuum cavity, and the quartz tube assembly can be used for sublimation purification when comprising a collecting section and a heating section, which are connected in series, and can be used for continuous sublimation purification when comprising a coarse sublimation groove, a transitional groove and a deep sublimation groove, which are sequentially connected. The organic material bi-directional vacuum sublimation purification equipment has simple structure, can be operated easily, has high efficiency, and can improve the purity of organic materials while effectively saving the time. The continuous or non-continuous purifying method can remarkably increase the purification purity.
Description
Technical field
The present invention relates to the equipment for purifying technical field of organic material, particularly relate to a kind of organic material bidirectional vacuum sublimation purification equipment and continuous or discontinuous method of purification, belong to technical field of physical vapor deposition.
Background technology
In recent years, the development of mobile interchange and FPD industry, Organic Light Emitting Diode, by its numerous advantage, has welcome the development as emerging rapidly in large numbersBamboo shoots after a spring rain, and receives increasing concern.It is of many uses that its main advantage has due to organic material, especially on a lot of photoelectric devices, embody good performance, but this and the purity of organic material are inseparable relations, in organic material, impurity directly can cause electric charge accumulation, forms local current excessive, thus reduces efficiency and the life-span of opto-electronic device, therefore the purity of organic material is higher, and performance is also better.But domestic organic material purity is always lower, cannot meet the demand of present stage industry.
Vacuum equipment for purifying for present domestic application mainly adopts the mode of unidirectional distillation, mainly according to the process of gradient increased temperature, by the process that impurity and target product are separated gradually, be characterised in that, organic compound in sublimation pipe spreads according to the direction of vacuum pneumatic, along with the gradient of temperature reduces, the purification of realize target material.But the method is in the process of heating, when low-temperature region, impurity can be attached on leading portion tube wall in the process of distillation, thus cause impurity can not effectively be separated with target product, thus target product of can not effectively purifying, simultaneously, the density of organic material is smaller, and frequent single sampling amount effectively can not reach the maximum deposition of apophorometer, makes the effectiveness that can not make full use of apophorometer.If obtain efficient high-purity target compound to need repeatedly to purify, so we devise a kind of method of two-way sublimation purification, the effective method solving impurity and can not effectively be separated.
Summary of the invention
For solving the deficiencies in the prior art, the invention provides a kind of bidirectional vacuum sublimation purification equipment of organic material.
Object of the present invention is achieved through the following technical solutions.
A kind of bidirectional vacuum sublimation purification equipment of organic material, comprise: vacuum cavity, vacuum extractor and cooling device, be respectively arranged with the first valve and the second valve at the two ends of described vacuum cavity, in described vacuum cavity, be provided with the quartz ampoule assembly of both ends open;
Described vacuum extractor is connected described cooling device, described first valve of described cooling device series connection, and an openend of described quartz ampoule assembly is near described first valve;
Described vacuum extractor is connected described cooling device, and described second valve of described cooling device series connection, another openend of described quartz ampoule assembly is near described second valve.
Preferably, described quartz ampoule assembly comprises collection section and the bringing-up section of series connection, and described collection section is positioned at the side near described first valve, and described bringing-up section is positioned at the side near described second valve.
Preferably, the bidirectional vacuum sublimation purification equipment of described organic material also comprises the heater heated described bringing-up section.
Present invention also offers a kind of bidirectional vacuum sublimation purification method of organic material, comprise the steps:
1) organic material is placed in the bringing-up section of quartz ampoule assembly, closes the first valve and open the second valve, being evacuated to 10
-3~ 10
-4after Pa, heat organic material, temperature to control below the sublimation point of organic material 20 ~ 50 DEG C, and constant temperature 40 ~ 100 minutes, small-molecular-weight impurity is drawn in cooling device.
2) close the second valve, open the first valve, heat organic material, temperature controls more than the sublimation point of organic material between 0 ~ 80 DEG C, and constant temperature 60 ~ 200 minutes, organic material deposits in the collection section of quartz ampoule assembly.
Preferably, described quartz ampoule assembly comprises degree of depth distillation groove, the lead-over groove and the groove that slightly distils of connecting successively, and described degree of depth distillation slot is in the side near described first valve, and described thick distillation slot is in the side near described second valve.
Preferably, the bidirectional vacuum sublimation purification equipment of described organic material also comprises the loading slot be communicated with described lead-over groove, between described lead-over groove and described loading slot, be provided with the 5th valve.
Preferably, described quartz ampoule assembly also comprises the 3rd valve be arranged between described degree of depth distillation groove and described lead-over groove, and is arranged on the 4th valve between described lead-over groove and described thick distillation groove.
Preferably, the bidirectional vacuum sublimation purification equipment of described organic material also comprises the heater heated described quartz ampoule assembly.
Present invention also offers a kind of continuous bidirectional vacuum sublimation purification method of organic material, comprise the steps:
1) organic material to be placed in the lead-over groove of quartz ampoule assembly and to close the 5th valve, closing the first valve, the 3rd valve, the 4th valve, and open the second valve, be evacuated to 10
-3~ 10
-4after Pa, open the 4th valve, heat organic material, temperature to control below the sublimation point of organic material 20 ~ 50 DEG C, and constant temperature 40 ~ 100 minutes, small-molecular-weight impurity is drawn in cooling device.
2) the second valve is closed, open the first valve, the 3rd valve, organic material is heated, temperature to control more than the sublimation point of organic material between 0 ~ 80 DEG C, constant temperature 60 ~ 200 minutes, organic material carries out distillation deposition in quartz ampoule assembly, after having distilled, adds new sample and close the 5th valve by loading slot in lead-over groove.
3) step 1 is repeated) and step 2) n time, carry out continuous bidirectional vacuum sublimation purification, wherein, n >=1.
After completing continuous bidirectional vacuum distillation extraction, take out the organic material residues after having distilled.
Preferred, described cooling device is the cold well of liquid nitrogen.
The bidirectional vacuum sublimation purification device structure of organic material provided by the present invention is simple, be easy to operation, efficient, improve the purity of organic material in effective time saving situation, continuous print bidirectional vacuum sublimation purification can be carried out.
Accompanying drawing explanation
Fig. 1 is the overall structure schematic diagram of the bidirectional vacuum sublimation purification equipment of the organic material of the first embodiment provided by the present invention.
Fig. 2 is the overall structure schematic diagram of the bidirectional vacuum sublimation purification equipment of the organic material of the second embodiment provided by the present invention.
In accompanying drawing 1,2, the list of parts representated by each label is as follows:
1, vacuum cavity, 2, vacuum extractor, 3, quartz ampoule assembly, 31, collection section, 32, bringing-up section, 33, degree of depth distillation groove, 34, lead-over groove, 35, slightly to distil groove, 36, loading slot, 37, the 3rd valve, the 38, the 4th valve, the 39, the 5th valve, 4, the first valve, 5, the second valve, 6, cooling device, 7, heater.
Detailed description of the invention
Be described principle of the present invention and feature below in conjunction with accompanying drawing, illustrated embodiment, only for explaining the present invention, is not intended to limit scope of the present invention.
First embodiment
As shown in Figure 1, a kind of bidirectional vacuum sublimation purification equipment of organic material, comprising: the vacuum cavity 1 of the quartz material of the circular tube shaped of both ends open, vacuum extractor 2, cooling device 6 and heater 7.Cooling device 6 is the cold well of liquid nitrogen.Be respectively arranged with the first valve 4 and the second valve 5 at the two ends of described vacuum cavity 1, in described vacuum cavity 1, be provided with the quartz ampoule assembly 3 of both ends open.Described quartz ampoule assembly 3 comprises collection section 31 and the bringing-up section 32 of series connection.
Described vacuum extractor 2 is connected described cooling device 6, and described cooling device 6 is connected described first valve 4, and described collection section 31 is positioned at the side near described first valve 4.
Described vacuum extractor 2 is connected described cooling device 6, and described cooling device 6 is connected described second valve 5, and described bringing-up section 32 is positioned at the side near described second valve 5.
Heater 7 is arranged on the outside of vacuum cavity 1, for what heat bringing-up section 32.
The bidirectional vacuum sublimation purification method of organic material provided by the present invention is specific as follows:
1) organic material is placed in the bringing-up section 32 of quartz ampoule assembly 3, closes the first valve 4 and open the second valve 5, being evacuated to 10
-3~ 10
-4after Pa, heat organic material, temperature to control below the sublimation point of organic material 20 ~ 50 DEG C, and constant temperature 40 ~ 100 minutes, small-molecular-weight impurity is drawn in cooling device 6.
Under the condition reaching high vacuum, and lower than sublimation point temperature 20-60 DEG C, the first valve is in closed condition, second valve is in opening, impurity in organic material enters liquid nitrogen well by the second valve and to be condensed deposition, and after reaching certain hour, the impurity in compound is removed.
2) close the second valve 5, open the first valve 4, heat organic material, temperature controls more than the sublimation point of organic material between 0 ~ 80 DEG C, constant temperature 60 ~ 200 minutes, and organic material deposits in the collection section 31 of quartz ampoule assembly 3.
Close the second valve, open the first valve, temperature is elevated to the above 10-100 DEG C of compound subliming point, such compound will start distillation, and deposits in the collection section that temperature is lower, is namely the High Purity compound that we need.
In the present embodiment, because the two ends at vacuum cavity are provided with valve, make to define two two-way passages at the two ends of vacuum cavity.By controlling the duty of two valves and the heating-up temperature to organic material, make a wing passage for the removal of small-molecular-weight impurity, one wing passage is used for the collection of organic material, thus is separated in organic material by small-molecular-weight impurity cleverly, reaches the object that removal of impurities is purified.
Embodiment and effect example
The present embodiment adopts three (4-carbazole-9 bases-phenyl) amine (TCTA) for distillation sample, and before distillation, sample purity is 96.8%, and repeatedly distil respectively, concrete operations flow process is as follows:
1) organic material is placed in the bringing-up section of quartz ampoule, closes the second valve and open the first valve, being evacuated to 10
-3~ 10
-4after Pa, heat organic material, temperature to control below the sublimation point of organic material 20 DEG C, and constant temperature 60 minutes, small-molecular-weight impurity is drawn in cooling device.
2) close the first valve, open the second valve, continue to heat organic material, temperature controls more than the sublimation point of organic material between 40 DEG C, and constant temperature 120 minutes, organic material deposits in the collection section of quartz ampoule.
3) complete distillation, close heater, after temperature cool to room temperature, after vacuum breaker, collect the compound of deposition section, and the purity of testing product.
Adopt the present invention and traditional equipment for purifying to carry out Contrast on effect, its two kinds of devices to obtain the purity of product as shown in table 1 below:
| Conventional method | This patent method | |
| Do not distil sample | 96.8％ | 96.8％ |
| First time distillation | 98.6％ | 99.5％ |
| Second time distillation | 99.1％ | 99.7％ |
| Third time distillation | 99.4％ | 99.8％ |
For organic material sublimation purification, if it is higher to want to obtain the purity of compound, distillation difficulty is larger, and as can be seen from the above table, the two-way distillation that this patent uses, effectively achieves being separated of target compound and impurity, obtain higher purity.
Second embodiment
As shown in Figure 2, a kind of bidirectional vacuum sublimation purification equipment of organic material, comprising: the vacuum cavity 1 of the quartz material of the circular tube shaped of both ends open, vacuum extractor 2, cooling device 6 and heater 7.Be respectively arranged with the first valve 4 and the second valve 5 at the two ends of described vacuum cavity 1, in described vacuum cavity 1, be provided with the quartz ampoule assembly 3 of both ends open.Described quartz ampoule assembly 3 comprises degree of depth distillation groove 33, lead-over groove 34 and the thick distillation groove 35 of connecting successively.The 3rd valve 37 is provided with between described degree of depth distillation groove 33 and described lead-over groove 34.The 4th valve 38 is provided with between described lead-over groove 34 and described thick distillation groove 35.
Described vacuum extractor 2 is connected described cooling device 6, and described cooling device 6 is connected described first valve 4, and described degree of depth distillation groove 33 is positioned at the side near described first valve 4.
Described vacuum extractor 2 is connected described cooling device 6, and described cooling device 6 is connected described second valve 5, and described thick distillation groove 35 is positioned at the side near described second valve 5.
Heater 7 is arranged on the outside of vacuum cavity 1, for heating with thick distillation groove 35 etc. the degree of depth distillation groove 33 of quartz ampoule assembly 3.
For realizing continuous print sublimation purification, the bidirectional vacuum sublimation purification equipment of described organic material also arranges the loading slot 36 be communicated with described lead-over groove 34.Loading slot 36 can be communicated to the outside of vacuum cavity 1, realizes continuous sample-adding fast and easily.The 5th valve 39 is provided with between lead-over groove 34 and described loading slot 36.
The concrete steps of the continuous bidirectional vacuum sublimation purification method of organic material provided by the present invention are as follows:
1) organic material to be placed in the lead-over groove 34 of quartz ampoule assembly 3 and to close the 5th valve 39, closing the first valve 4, the 3rd valve 37, the 4th valve 38, and open the second valve 5, be evacuated to 10
-3~ 10
-4after Pa, open the 4th valve 38, heat organic material, temperature to control below the sublimation point of organic material 20 ~ 50 DEG C, and constant temperature 40 ~ 100 minutes, small-molecular-weight impurity is drawn in cooling device 6.
Under the condition reaching high vacuum, and lower than sublimation point temperature 20-60 DEG C, first valve is in closed condition, second valve is in opening, impurity in organic material enters liquid nitrogen well by the second valve and to be condensed deposition, after reaching certain hour, the impurity in compound is by a large amount of removings.
After this step completes, a large amount of materials containing a small amount of impurity can be deposited on thick distillation groove 35.
2) the second valve 5 is closed, open the first valve 4, the 3rd valve 37, organic material is heated, temperature to control more than the sublimation point of organic material between 0 ~ 80 DEG C, constant temperature 60 ~ 200 minutes, organic material carries out distillation deposition at quartz ampoule assembly 3, after having distilled, adds new sample and close the 5th valve 39 by loading slot 36 in lead-over groove 34.
Close the second valve, open the first valve, the 3rd valve, temperature is elevated to the above 10-100 DEG C of compound subliming point, such compound will start distillation.In this process, be deposited on the material that the thick impurity content distilled in groove 35 is less, in sublimation process this time, a large amount of transfers in degree of depth distillation groove 33, thus further increases the purity of target compound.
3) step 1 is repeated) and step 2) repeatedly, carry out continuous bidirectional vacuum sublimation purification, the organic material of rear taking-up removal of impurities of having purified.
In step 1) and step 2 repetitive process in, the purity of organic material through repeatedly thick distillation groove 35 and degree of depth distillation groove 33 back and forth in, impurity is constantly removed, thus further increases the purity of target compound.
In the present embodiment, because the two ends at vacuum cavity are provided with valve, make to define two two-way passages at the two ends of vacuum cavity.By controlling the duty of four valves and the heating-up temperature to organic material, make a wing passage for the removal of small-molecular-weight impurity, a wing passage is used for the collection of organic material.Further, based on organic material in the distillation repeatedly, precipitation of thick distil groove 35 and degree of depth distillation groove 33, carry out of small-molecular-weight impurity in organic material maximum possible is separated, reaches the object that removal of impurities is purified.
Embodiment and effect example
The present embodiment adopts three (4-carbazole-9 bases-phenyl) amine (TCTA) for distillation sample, and before distillation, sample purity is 96.8%, and repeatedly distil respectively, concrete operations flow process is as follows:
1) organic material to be placed in the lead-over groove of quartz ampoule assembly and to close the 5th valve, closing the first valve, the 3rd valve, the 4th valve, and open the second valve, be evacuated to 10
-3~ 10
-4after Pa, open the 4th valve, heat organic material, temperature to control below the sublimation point of organic material 20 DEG C, constant temperature 60 minutes, and small-molecular-weight impurity is drawn in cooling device, and a large amount of sedimentation of organic material is in thick distillation groove.
2) the second valve is closed, open the first valve, the 3rd valve, organic material is heated, temperature to control more than the sublimation point of organic material between 40 DEG C, constant temperature 120 minutes, organic material deposits in the degree of depth distillation groove of quartz ampoule assembly, after having precipitated, adds new sample and close the 5th valve by loading slot in lead-over groove;
3) add new organic material, repeat step 3 time.
4) complete distillation, close heater, after temperature cool to room temperature, after vacuum breaker, collect the compound of deposition section, and the purity of testing product.
Adopt the present invention and traditional equipment for purifying to carry out Contrast on effect, its two kinds of devices to obtain the purity of product as shown in table 2 below:
| Conventional method | This patent method | |
| Do not distil sample | 96.8％ | 96.8％ |
| Distillation purity | 98.6％ | 99.2％ |
| Distillation amount | 200g | 600g |
For organic material sublimation purification, if it is higher to want to obtain the purity of compound, distillation difficulty is larger, and as can be seen from the above table, the continuous two-way distillation that this patent provides, effectively achieves being separated of target compound and impurity, obtain higher purity.Relative to common discontinuous vacuum sublimation, the distillation amount of target chemical combination is improved further.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. the bidirectional vacuum sublimation purification equipment of an organic material, it is characterized in that, comprise: vacuum cavity (1), vacuum extractor (2) and cooling device (6), be respectively arranged with the first valve (4) and the second valve (5) at the two ends of described vacuum cavity (1), in described vacuum cavity (1), be provided with the quartz ampoule assembly (3) of both ends open;
Described vacuum extractor (2) is connected described cooling device (6), described cooling device (6) is connected described first valve (4), and an openend of described quartz ampoule assembly (3) is near described first valve (4);
Described vacuum extractor (2) is connected described cooling device (6), described cooling device (6) is connected described second valve (5), and another openend of described quartz ampoule assembly (3) is near described second valve (5).
2. the bidirectional vacuum sublimation purification equipment of organic material according to claim 1, it is characterized in that: described quartz ampoule assembly (3) comprises collection section (31) and the bringing-up section (32) of series connection, described collection section (31) is positioned at the side near described first valve (4), and described bringing-up section (32) is positioned at the side near described second valve (5).
3. the bidirectional vacuum sublimation purification equipment of organic material according to claim 2, is characterized in that: the bidirectional vacuum sublimation purification equipment of described organic material also comprises the heater (7) heated described bringing-up section (32).
4. the bidirectional vacuum sublimation purification equipment of organic material according to claim 1, it is characterized in that: described quartz ampoule assembly (3) comprises degree of depth distillation groove (33), lead-over groove (34) and the groove (35) that slightly distils of connecting successively, described degree of depth distillation groove (33) is positioned at the side near described first valve (4), and described thick distillation groove (35) is positioned at the side near described second valve (5).
5. the bidirectional vacuum sublimation purification equipment of organic material according to claim 4, it is characterized in that: the bidirectional vacuum sublimation purification equipment of described organic material also comprises the loading slot (36) be communicated with described lead-over groove (34), between described lead-over groove (34) and described loading slot (36), be provided with the 5th valve (39).
6. the bidirectional vacuum sublimation purification equipment of the organic material according to claim 4 or 5, it is characterized in that: described quartz ampoule assembly (3) also comprises the 3rd valve (37) be arranged between described degree of depth distillation groove (33) and described lead-over groove (34), and is arranged on the 4th valve (38) between described lead-over groove (34) and described thick distillation groove (35).
7. the bidirectional vacuum sublimation purification equipment of the organic material according to claim 4 or 5, is characterized in that: the bidirectional vacuum sublimation purification equipment of described organic material also comprises the heater (7) heated described quartz ampoule assembly (3).
8. a bidirectional vacuum sublimation purification method for organic material, is characterized in that, comprise the steps:
1) organic material is placed in the bringing-up section (32) of quartz ampoule assembly (3), closes the first valve (4) and open the second valve (5), being evacuated to 10
-3~ 10
-4after Pa, heat organic material, temperature to control below the sublimation point of organic material 20 ~ 50 DEG C, constant temperature 40 ~ 100 minutes, and small-molecular-weight impurity is drawn in cooling device (6);
2) the second valve (5) is closed, open the first valve (4), organic material is heated, temperature to control more than the sublimation point of organic material between 0 ~ 80 DEG C, constant temperature 60 ~ 200 minutes, organic material deposits in the collection section (31) of quartz ampoule assembly (3).
9. a continuous bidirectional vacuum sublimation purification method for organic material, is characterized in that, comprise the steps:
1) organic material to be placed in the lead-over groove (34) of quartz ampoule assembly (3) and to close the 5th valve (39), close the first valve (4), the 3rd valve (37), the 4th valve (38), and open the second valve (5), be evacuated to 10
-3~ 10
-4after Pa, open the 4th valve (38), heat organic material, temperature to control below the sublimation point of organic material 20 ~ 50 DEG C, constant temperature 40 ~ 100 minutes, and small-molecular-weight impurity is drawn in cooling device (6);
2) the second valve (5) is closed, open the first valve (4), the 3rd valve (37), organic material is heated, temperature to control more than the sublimation point of organic material between 0 ~ 80 DEG C, constant temperature 60 ~ 200 minutes, organic material carries out distillation deposition at quartz ampoule assembly (3), after having distilled, in lead-over groove (34), add new sample by loading slot (36) and close the 5th valve (39);
3) step 1 is repeated) and step 2) n time, carry out continuous bidirectional vacuum sublimation purification, wherein, n >=1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108992962A (en) * | 2018-09-30 | 2018-12-14 | 深圳普瑞材料技术有限公司 | A kind of modularization sublimation purification system |
| CN109499090A (en) * | 2018-12-25 | 2019-03-22 | 威格气体纯化科技（苏州）股份有限公司 | A kind of apophorometer with control material processing environmental functional |
| CN111233710A (en) * | 2018-11-28 | 2020-06-05 | 弗萨姆材料美国有限责任公司 | Low halide lanthanide precursors for vapor deposition |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5596673A (en) * | 1994-11-18 | 1997-01-21 | Xerox Corporation | Evaporation crucible assembly |
| CN101738062A (en) * | 2008-11-14 | 2010-06-16 | 兰州科近真空冻干技术有限公司 | Vacuum freeze-drying device |
| CN102671411A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Device for recovering pyrogallic acids through electrostatic adsorption by using sublimation method |
| CN204601665U (en) * | 2015-01-29 | 2015-09-02 | 武汉尚赛光电科技有限公司 | Continuous or the discontinuous bidirectional vacuum sublimation purification equipment of organic material |
-
2015
- 2015-01-29 CN CN201510046229.3A patent/CN104667562B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5596673A (en) * | 1994-11-18 | 1997-01-21 | Xerox Corporation | Evaporation crucible assembly |
| CN101738062A (en) * | 2008-11-14 | 2010-06-16 | 兰州科近真空冻干技术有限公司 | Vacuum freeze-drying device |
| CN102671411A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Device for recovering pyrogallic acids through electrostatic adsorption by using sublimation method |
| CN204601665U (en) * | 2015-01-29 | 2015-09-02 | 武汉尚赛光电科技有限公司 | Continuous or the discontinuous bidirectional vacuum sublimation purification equipment of organic material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108992962A (en) * | 2018-09-30 | 2018-12-14 | 深圳普瑞材料技术有限公司 | A kind of modularization sublimation purification system |
| CN108992962B (en) * | 2018-09-30 | 2024-05-31 | 深圳普瑞材料技术有限公司 | Modularized sublimation purification system |
| CN111233710A (en) * | 2018-11-28 | 2020-06-05 | 弗萨姆材料美国有限责任公司 | Low halide lanthanide precursors for vapor deposition |
| US20210363162A1 (en) * | 2018-11-28 | 2021-11-25 | Versum Materials Us, Llc | Low Halide Lanthanum Precursors For Vapor Deposition |
| US11753420B2 (en) * | 2018-11-28 | 2023-09-12 | Versum Materials Us, Llc | Low halide lanthanum precursors for vapor deposition |
| CN109499090A (en) * | 2018-12-25 | 2019-03-22 | 威格气体纯化科技（苏州）股份有限公司 | A kind of apophorometer with control material processing environmental functional |
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| Publication number | Publication date |
|---|---|
| CN104667562B (en) | 2017-02-22 |
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