CN100998928A - Sublimation purification device of organic material - Google Patents
Sublimation purification device of organic material Download PDFInfo
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- CN100998928A CN100998928A CN 200610000696 CN200610000696A CN100998928A CN 100998928 A CN100998928 A CN 100998928A CN 200610000696 CN200610000696 CN 200610000696 CN 200610000696 A CN200610000696 A CN 200610000696A CN 100998928 A CN100998928 A CN 100998928A
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Abstract
A sublimation apparatus for purifying organic material is composed of a supporting frame with a top surface and a longitudinal slide track on said top surface, a vacuumizing unit, a heating furnace on said slide track, a purifying unit communicated with said vacuumizing unit and passing through said heating furnace, and a steel cylinder communicated with said purifying unit.
Description
Technical field
The invention belongs to technical field of semiconductor, relate to a kind of sublimation purification device of organic material.The present invention adopts thermograde sublimating technologe purified material, and this technology is for the purifying organic material, and especially the molecular beam deposition technique prepares the method that the employed powder sample of organic semiconductor device is the best.
Background technology
Organic compound is thought good insulator traditionally, is widely used as insulating materials technically.It is found that the electrical conductivity that can make polyacetylene film by mixing improved 12 magnitudes in 1977, become conductor by insulator, from then on opened up a new research field, promptly organic material is as the research of physical function (light, electricity, magnetic) material.Organic semiconducting materials as the information functional material of a new generation just with its photoelectric properties excellence, low production cost, processing technology is simple, selection range is broad, mechanical performance is soft, can and traditional silica-based process compatible remarkable advantages such as (being easy to integrated), attract worldwide sight, become the object that more and more research institutions competitively research and develop.
The organic semiconductor research work comprises the research of character such as the electricity, optics of high-molecular organic material, organic small molecule material and OMC material.Organic semiconducting materials has been widely used in photoelectricity and electricity research fields such as conduction, organic light emission, solar cell, field-effect transistor, electrochromism and electrochemical cell.Nowadays the organic semiconductor colorful display screen enters the practical stage.Highly purified organic material is the prerequisite that realizes the organic semiconductor device of function admirable.
The regularity that impurity meeting saboteur in the organic material piles up, these point defects reduce the mobility of charge carrier rate significantly.In addition, cause mutually combining between the unordered impurity of material, also affect the final character of material, device performance is descended.Harmful crystal defect also may be the big molecular impurity of introducing when coming from inappropriate purifying source material, or come from the fraction that source material decomposes in the heating sublimation process, and this fraction is that the condition by purifying and evaporation causes.
For preparing the organic semiconductor device of excellent performance, the purifying of organic source material is necessary.The invention provides a kind of sublimation purification device of organic material, adopt thermograde sublimating technologe purified material, this technology is for the purifying organic material, and especially the molecular beam deposition technique prepares the method that the employed powder sample of organic semiconductor device is the best.Because the molecular beam deposition technique prepares the employed organic source material of organic semiconductor device, great majority are at atmospheric pressure or be lower than under the atmospheric pressure and do not have liquid phase.
Summary of the invention
The object of the present invention is to provide a kind of sublimation purification device of organic material, this device can be removed the impurity in the organic material and the solvent of parcel, obtains highly purified organic material, for research and the good organic semiconductor device of processability lay the foundation.
The present invention is a kind of sublimation purification device that organic material is purified of being used for, and it is characterized in that purifying plant comprises:
One bracing frame, this bracing frame comprises a table top, and a slideway is vertically arranged on the table top;
One vacuum section, this vacuum section are positioned at a side of bracing frame table top;
One heating furnace, this heating furnace are positioned on the slideway of bracing frame table top top;
One purification part, this end of purifying part is connected with vacuum section, and this purification part is passed heating furnace;
One steel cylinder, this steel cylinder are positioned at an end of bracing frame, and are connected with the part of purifying by pipeline.
Wherein vacuum section comprises:
One adapter cavity;
A part pump, this molecular pump is connected with adapter cavity with pipeline;
One mechanical pump, this mechanical pump is connected with molecular pump with pipeline.
Wherein on this adapter cavity a vacuum meter is installed.
Wherein the temperature-control range of heating furnace is: room temperature ~ 600 ℃, temperature-controlled precision: ± 5 ℃.
The part of wherein purifying comprises: a quartz ampoule, and a quartz boat, this quartz boat are positioned at a side of quartz ampoule, a quartz socket tube, this quartz socket tube is positioned at the opposite side of quartz ampoule, at an end of quartz ampoule one valve is arranged.
Wherein the vacuum of quartz ampoule is that vacuum is 1 * 10 by mechanical pump and molecular pump control
-6Torr.
Between one end of the quartz ampoule in the part of wherein purifying and the table top of bracing frame a support is arranged, the side of this support is one L shaped, one side at support has two fixing holes, this fixing hole is oval, be screwed on table top, so that the vertical direction of the slideway of support on the table top has the 1cm amount of movement.
Between wherein said purification part and the steel cylinder valve is arranged.
Description of drawings
For further specifying content of the present invention and characteristics, below in conjunction with accompanying drawing and example the present invention is done a detailed description, wherein:
Fig. 1 is the structural representation of purifying plant of the present invention.
Fig. 2 is the quartz ampoule of purifying plant of the present invention and the vertical view of valve junction support.
The specific embodiment
See also Fig. 1 and Fig. 2, the present invention is a kind of to be used for sublimation purification device that organic material is purified, it is characterized in that purifying plant comprises:
One bracing frame 10, this bracing frame 10 comprises a table top 13, and a slideway 12 is vertically arranged on the table top 13;
One vacuum section 20, this vacuum section 20 is positioned at a side of bracing frame 10 table tops 13;
One adapter cavity 24 is equipped with a vacuum meter 23 on this adapter cavity 24;
A part pump 21, these molecular pump 21 usefulness pipelines are connected with adapter cavity 24;
One mechanical pump 22, these mechanical pump 22 usefulness pipelines are connected with molecular pump 21;
One heating furnace 30, this heating furnace 30 are positioned on the slideway 12 of bracing frame 10 table tops 13 tops; The temperature-control range of this heating furnace 30 is: room temperature-600 ℃, temperature-controlled precision: ± 5 ℃;
One purification part 40, an end of this purification part 40 is connected with vacuum section 20, and should purification part 40 pass heating furnace 30;
The part of wherein purifying 40 comprises: a quartz ampoule 44, one quartz boats 42, and this quartz boat 42 is positioned at a side of quartz ampoule 44, a quartz socket tube 43, this quartz socket tube 43 is positioned at the opposite side of quartz ampoule 44, at an end of quartz ampoule 44 valve 41 is arranged; The vacuum of this quartz ampoule 44 is that vacuum is 1 * 10 by mechanical pump 22 and molecular pump 21 controls
-6Torr; Between one end of the quartz ampoule 44 in this purification part 40 and the table top 13 of bracing frame 10 support 11 is arranged, the side of this support 11 is one L shaped, one side at support 11 has two fixing holes 111, this fixing hole 111 is oval, be fixed on the table top 13 with screw 112, so that the vertical direction of the slideway 12 of support 11 on the table top 13 has the 1cm amount of movement;
One steel cylinder 50, this steel cylinder 50 is positioned at an end of bracing frame 10, and is connected with purification part 40 by pipeline;
One valve 51 is arranged between described purification part 40 and the steel cylinder 50.
Please consult Figure 1 and Figure 2 again, be that content of the present invention is described in further detail, the present invention is a kind of sublimation purification device of organic material that organic material is purified of being used for, and this device is made up of bracing frame 10, vacuum section 20, heating furnace 30, purification part 40 and steel cylinder 50 5 parts.Bracing frame 10 comprises that a table top 13, one holes 14, are positioned at slideway 12, on the table top 13 and are positioned at support 11 on the table top 13.The adapter cavity 24 of vacuum section 20, heating furnace 30 and purification part 40 all are positioned on the table top 13, and the side above the table top 13 has a hole 14, molecular pump 21 usefulness pipelines by these hole 14 vacuum section 20 link to each other with adapter cavity 24, fix two parallel elongated iron rods above the table top 13, form slideway 12, place diverse location on the table top 13 as requested so that be positioned at heating furnace 30 on the slideway 12; Vacuum section 20 is positioned at the upper and lower of bracing frame 10 table tops 13, comprising: an adapter cavity 24, a part pump 21, one mechanical pumps 22, one vacuum meters 23.These molecular pump 21 usefulness pipelines are connected with adapter cavity 24, are positioned at the bottom of adapter cavity 24, and mechanical pump 22 usefulness pipelines are connected with molecular pump 21, and vacuum meter 23 is installed on the adapter cavity 24, is used to measure the vacuum of whole device; Heating furnace 30 is positioned on the slideway 12 of bracing frame 10 table tops 13 tops, and there are 4 pulleys (figure do not show) heating furnace 30 belows, can move freely in slideway 12 upper edge slideways 12 directions, and the temperature-control range of heating furnace 30 is: room temperature ~ 600 ℃, temperature-controlled precision: ± 5 ℃; One end of purification part 40 is connected with vacuum section 20, and should purification part 40 pass heating furnace 30, purification part 40 comprises: a quartz ampoule 44, one quartz boat 42, one quartz socket tube 43, quartz boat 42 are positioned at a side of quartz ampoule 44, and quartz socket tube 43 is positioned at the opposite side of quartz ampoule 44, end at quartz ampoule 44 has a valve 41, is used to control the gas flow that feeds purification part 40; Steel cylinder 50 is positioned at an end of bracing frame 10, and is connected with purification part 40 by pipeline, and steel cylinder is used nitrogen cylinder usually, and whole device continues logical nitrogen in experimentation; One support 11 is arranged between the table top 13 of quartz ampoule 44 and bracing frame 10, the side of this support 11 is one L shaped, one side at support 11 has two fixing holes 111, this fixing hole 111 is oval, support 11 usefulness screws 112 are fixed on the table top 13 by fixing hole 111, so that the vertical direction of the slideway 12 of support 11 on the table top 13 has the 1cm amount of movement.
Operation principle of the present invention is: the quartz boat 42 that the organic material of waiting to purify will be housed is placed on quartz ampoule 44 inside left near valve 41 about 20cm places; Heating furnace 30 moves on slideway 12, makes quartz boat 42 place the mid portion of heating furnace 30, and heating furnace 30 usefulness clips are fixed; Before the intensification, vacuumize, open mechanical pump 22 earlier, treat that vacuum is 1 * 10 with 20 pairs of whole devices of vacuum section
-2Behind the Torr, open molecular pump 21; In the process that vacuumizes, support 11 is adjusted the position automatically, avoids quartz ampoule 44 mouths of pipe to break because of stressed; Vacuum is 1 * 10
-6Behind the Torr, open valve 51, open valve 41 then, with the nitrogen wash purification part 40 in the steel cylinder 50, to remove the air in the quartz ampoule 44; By-pass valve control 41 makes nitrogen slowly feed from quartz ampoule 44 left ends, treats steady back (pressure is 0.2Mpa), starts heating furnace 30, and control furnace temperature gradient formula increases, up to the sublimation temperature that reaches material.After organic material is purified and is finished, earlier with heating furnace 30 coolings, after temperature is reduced to room temperature, closing valve 51, closing valve 41 is closed vacuum section 20 again, closes mechanical pump 22 earlier, and the closure molecule pump 21 then, and whole purification process finishes.Under the transporting of nitrogen, the organic material behind the purifying is collected in the quartz socket tube 43, and a large amount of volatile impurity are blown away and are drawn out of by nitrogen stream, and not volatile impurity is stayed the end of quartz ampoule; Shift out quartz socket tube 43 then, take out the organic material after purifying.During the purification organic material, control the throughput of nitrogen according to the characteristics of material.
Claims (8)
1, a kind of sublimation purification device that organic material is purified of being used for is characterized in that purifying plant comprises:
One bracing frame, this bracing frame comprises a table top, and a slideway is vertically arranged on the table top;
One vacuum section, this vacuum section are positioned at a side of bracing frame table top;
One heating furnace, this heating furnace are positioned on the slideway of bracing frame table top top;
One purification part, this end of purifying part is connected with vacuum section, and this purification part is passed heating furnace;
One steel cylinder, this steel cylinder are positioned at an end of bracing frame, and are connected with the part of purifying by pipeline.
2, the sublimation purification device that organic material is purified of being used for according to claim 1 is characterized in that wherein vacuum section comprises:
One adapter cavity;
A part pump, this molecular pump is connected with adapter cavity with pipeline;
One mechanical pump, this mechanical pump is connected with molecular pump with pipeline.
3, the sublimation purification device that organic material is purified of being used for according to claim 2 is characterized in that, wherein on this adapter cavity a vacuum meter is installed.
4, the sublimation purification device that organic material is purified of being used for according to claim 1 is characterized in that wherein the temperature-control range of heating furnace is: one 600 ℃ of room temperatures, temperature-controlled precision: ± 5 ℃.
5, the sublimation purification device that organic material is purified of being used for according to claim 1, it is characterized in that, the part of wherein purifying comprises: a quartz ampoule, one quartz boat, this quartz boat is positioned at a side of quartz ampoule, one quartz socket tube, this quartz socket tube is positioned at the opposite side of quartz ampoule, at an end of quartz ampoule one valve is arranged.
6, the sublimation purification device that organic material is purified of being used for according to claim 5 is characterized in that, wherein the vacuum of quartz ampoule is that vacuum is 1 * 10 by mechanical pump and molecular pump control
-5Torr.
7, the sublimation purification device that organic material is purified of being used for according to claim 1, it is characterized in that, between one end of the quartz ampoule in the part of wherein purifying and the table top of bracing frame a support is arranged, the side of this support is one L shaped, one side at support has two fixing holes, this fixing hole is oval, is screwed on table top, so that the vertical direction of the slideway of support on the table top has the 1cm amount of movement.
8, the sublimation purification device that organic material is purified of being used for according to claim 1 is characterized in that, between wherein said purification part and the steel cylinder valve is arranged.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610000696 CN100998928A (en) | 2006-01-13 | 2006-01-13 | Sublimation purification device of organic material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610000696 CN100998928A (en) | 2006-01-13 | 2006-01-13 | Sublimation purification device of organic material |
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| CN100998928A true CN100998928A (en) | 2007-07-18 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101865611A (en) * | 2010-06-22 | 2010-10-20 | 沈阳慧宇真空技术有限公司 | Observation window structure for organic light emitting material sublimation purification device |
| CN102430260A (en) * | 2011-08-18 | 2012-05-02 | 友达光电股份有限公司 | Sleeve combination |
| CN102961890A (en) * | 2012-12-12 | 2013-03-13 | 中国科学院长春应用化学研究所 | Equipment and process for vacuum sublimation purification of small organic molecule material |
| CN104383712A (en) * | 2013-06-17 | 2015-03-04 | 罗门哈斯电子材料韩国有限公司 | Sublimation and purification apparatus |
| CN105561623A (en) * | 2014-10-31 | 2016-05-11 | 机光科技股份有限公司 | Purifying method for organic optoelectronic material |
| CN108854118A (en) * | 2018-08-02 | 2018-11-23 | 苏州大学 | A kind of low dose organic material method of purification and equipment for purifying |
| CN109030542A (en) * | 2017-06-09 | 2018-12-18 | 武汉尚赛光电科技有限公司 | A kind of organic material heat stability testing equipment |
| CN109646987A (en) * | 2019-01-10 | 2019-04-19 | 合肥欧莱迪光电技术有限公司 | A kind of continuous feeding and discharging high vacuum small organic molecule purification special equipment |
| CN111912220A (en) * | 2020-06-17 | 2020-11-10 | 周士海 | Zone-melting purification system, using method and zone-melting purification method |
| CN111939587A (en) * | 2020-06-10 | 2020-11-17 | 安徽贝意克智能科技有限公司 | Five-tube automatic protection small molecule purification equipment |
-
2006
- 2006-01-13 CN CN 200610000696 patent/CN100998928A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101865611B (en) * | 2010-06-22 | 2012-07-04 | 沈阳慧宇真空技术有限公司 | Observation window structure for organic light emitting material sublimation purification device |
| CN101865611A (en) * | 2010-06-22 | 2010-10-20 | 沈阳慧宇真空技术有限公司 | Observation window structure for organic light emitting material sublimation purification device |
| CN102430260A (en) * | 2011-08-18 | 2012-05-02 | 友达光电股份有限公司 | Sleeve combination |
| CN102430260B (en) * | 2011-08-18 | 2014-09-03 | 友达光电股份有限公司 | Sleeve combination |
| CN102961890A (en) * | 2012-12-12 | 2013-03-13 | 中国科学院长春应用化学研究所 | Equipment and process for vacuum sublimation purification of small organic molecule material |
| CN104383712A (en) * | 2013-06-17 | 2015-03-04 | 罗门哈斯电子材料韩国有限公司 | Sublimation and purification apparatus |
| CN105561623A (en) * | 2014-10-31 | 2016-05-11 | 机光科技股份有限公司 | Purifying method for organic optoelectronic material |
| CN105561623B (en) * | 2014-10-31 | 2018-07-31 | 机光科技股份有限公司 | Purification process for organic photoelectrical material |
| CN109030542B (en) * | 2017-06-09 | 2021-04-09 | 湖北尚赛光电材料有限公司 | Organic material thermal stability test equipment |
| CN109030542A (en) * | 2017-06-09 | 2018-12-18 | 武汉尚赛光电科技有限公司 | A kind of organic material heat stability testing equipment |
| CN108854118A (en) * | 2018-08-02 | 2018-11-23 | 苏州大学 | A kind of low dose organic material method of purification and equipment for purifying |
| CN109646987A (en) * | 2019-01-10 | 2019-04-19 | 合肥欧莱迪光电技术有限公司 | A kind of continuous feeding and discharging high vacuum small organic molecule purification special equipment |
| CN109646987B (en) * | 2019-01-10 | 2024-03-26 | 合肥百思智能装备有限公司 | Continuous feeding and discharging high-vacuum organic micromolecule purifying special equipment |
| CN111939587A (en) * | 2020-06-10 | 2020-11-17 | 安徽贝意克智能科技有限公司 | Five-tube automatic protection small molecule purification equipment |
| CN111939587B (en) * | 2020-06-10 | 2022-03-15 | 安徽贝意克智能科技有限公司 | Five-tube automatic protection small molecule purification equipment |
| CN111912220A (en) * | 2020-06-17 | 2020-11-10 | 周士海 | Zone-melting purification system, using method and zone-melting purification method |
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