CN1714061A - Apparatus and method for purifying an organic electroluminescent material - Google Patents
Apparatus and method for purifying an organic electroluminescent material Download PDFInfo
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- CN1714061A CN1714061A CN 02828095 CN02828095A CN1714061A CN 1714061 A CN1714061 A CN 1714061A CN 02828095 CN02828095 CN 02828095 CN 02828095 A CN02828095 A CN 02828095A CN 1714061 A CN1714061 A CN 1714061A
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- B01D7/00—Sublimation
Abstract
The apparatus for purifying an organic electroluminescent material includes one or more inner tubes for mounting material to be purified in their one ends, connection members for separating each of the inner tubes into a plurality of sections, a heat unit for heating the sections of respective inner tubes to more than sublimation temperature of the material to be purified, and a vacuum pump for vacuum-evacuating the sections of the inner tubes. Each of the connection members has a partition for partially closing space between two sections and a hole for making sublimate gas from the material to be purified pass therethrough, the hole being formed at a substantially central portion of the partition.
Description
Technical field
The present invention relates to be used to the to purify apparatus and method of electroluminescent organic material, the apparatus and method that more particularly, relate to the electroluminescent organic material that is used to purify, can reduce the treatment time and be applicable to batch process with high luminous and purification efficiency.
Background technology
Usually, the needs purification is used in the luminescent material in the organic electroluminescent device.The purpose of purifying is pure pigment composition and mixed luminescence material to be separated and pure composition is used for thin film deposition.The exploitation of luminescent material purification techniques has increased the luminous efficiency of purity and purification material, thereby uses this purification material to prolong the weather resistance of organic electroluminescent device.For producing electroluminescent organic material in batches, the purification efficiency that needs to reduce the treatment time and improve the electroluminescent organic material purification techniques.
Usually use the distillation method of purification electroluminescent organic material equipment of purifying.Distillation is meant from solid-state and is directly converted to gaseous state or is directly converted to solid-stately from gaseous state that and do not become fluid, this is in phase equilibrium figure, is lower than to take place under the condition of temperature and pressure of triple point.Even can when barometric point, when being lower than the low pressure of triple point, also be difficult to decompose by high temperature by the pyrolytic material.Therefore, the distillation device of energy controlled temperature gradient is used for the vacuum-sublimation method, and it is applied to heat on the mixing material has the impurity of different sublimation temperatures and do not decompose this material so that from then on separate.Because the vacuum-sublimation method is pure physical method, do not use any auxiliary reagent or chemical process, therefore, contamination reagent not.In addition, it is very useful to the organic materials that purification is used in the organic electroluminescent device to have a vacuum-sublimation method of high separableness.
Current, training (train) distillation method of purification is widely used in to purify and is used in luminescent material in the organic electroluminescent device.This method comprises material to be purified is placed in the end of open tube, by using vacuum pump, and the inside of vacuum-evacuate pipe and by using well heater to heat this pipe, so that on whole pipe, generate thermograde.At this moment because isolating material and impurity are had different sublimation temperatures, with the different interior location crystallizations of isolating pipe they.In some cases, for making the distillation gas stream effective, carrier gas to low temperature, does not have chemical reaction for the carrier gas of nitrogen or rare gas element demonstrates with the material that constitutes purifying plant from high-temperature stream in the scope of the vacuum tightness that influences pipe indistinctively.
Fig. 1 represents to be used to carry out the synoptic diagram of traditional sublimation purification device of above-mentioned training distillation method of purification.
As shown in Figure 1, the material of purifying is placed in the container (cell) 4, and on an end of interior pipe 1, arranges container 4.The various piece of pipe in transom 3 interconnection, and outer tube 2 covers interior pipe 1.Periphery along an end of outer tube 2 is installed well heater 5, and wherein the one end is corresponding to the end of the interior pipe 1 of placing container 4.Arrange that at the other end of interior pipe 1 vacuum pump 6 is so that its internal portion of vacuum-evacuate.
The perspective illustration of the container of material box 4 of will purify is preserved in the explanation of Fig. 2 example therein.
With reference to figure 2, example explanation container 4 is by the silica tube 20 with the equal opening in two ends and be assembled to a pair of stainless steel cap 21 of managing each end of 20 respectively and form, and each cap 21 has the hole 22 that forms on the middle body basically at it.
For using traditional sublimation purification device of structure as mentioned above, manage 1 internal portion in vacuum pump 6 vacuum-evacuate, and to a small amount of carrier gas wherein is provided, so that generate slight pressure gradient.In addition, in raising lentamente, well heater 5 during pipe 1 temperature, generates thermograde.In this case, temperature distribution is represented normal distribution curve.As long as its temperature is higher than in it sublimation temperature of the material of will purify, material wherein begins distillation.Then, discharge sublimer and, shift to vacuum pump 6 from managing 20 by hole 22 owing to pressure gradient.At this moment, its sublimation temperature is higher than the impurity of sublimation temperature of the material that will purify still in container 4.In the part of interior pipe 2, wherein temperature is lower than sublimation temperature, and sublimer changes over solid-state it and crystallization on the surface, inside of interior pipe 2 mutually.After in heat is applied to fully, managing on 1, manage 1 in the cooling lentamente.When its temperature equals room temperature, pipe 1 and collection and acquisition purification material 25, i.e. crystalline material on the surface, inside of interior pipe 1 in breaking.
Usually, the material require in organic electroluminescent device is have minute quantity impurity highly purified.Therefore, should carry out repeatedly purification process so that obtain high purity material.Because for collecting, scrape the purification material from the surface, inside of interior pipe 1, mass loss appears.In addition,, just need take outer tube 2 apart as long as repeat purification process, therefore since with oxygen or steam reaction, pollute or worsen will purification material.In addition, increased the treatment time of purifying.
Summary of the invention
Therefore, main purpose of the present invention provides the improved device of the electroluminescent organic material that is used to purify.
Another object of the present invention provides improving one's methods of the electroluminescent organic material that is used to purify.
According to an aspect of the present invention, provide a kind of device of the electroluminescent organic material that is used to purify, this device comprises: pipe in one or more, an end of pipe in being used for material to be purified packed into; Transom is used for pipe in each is divided into a plurality of sections; Heating unit is used to make the section of pipe in each to be heated to above the sublimation temperature of the material that will purify; Vacuum pump, these sections that are used for pipe in the vacuum-evacuate, wherein, each transom has and is used for the hole that part is closed two intersegmental spatial dividing plates and is used to make the distillation gas from the material that will purify from then on to pass through, and this hole is formed on the centre portions basically of dividing plate.
According to a further aspect in the invention, provide a kind of method of the electroluminescent organic material that is used to purify, the method comprising the steps of: the internal portion part of pipes in one or more is connected a plurality of sections; Material to be purified is provided to an end of pipe in each; By the other end of pipe in each, each interior pipe of vacuum-evacuate; And sequentially heat in each to adjacent segment from the section of preservation material to be purified and to manage, so that be higher than the sublimation temperature of material to be purified.
Description of drawings
From the description of following preferred embodiment in conjunction with the accompanying drawings, above-mentioned and other purposes of the present invention and feature will become apparent, wherein:
Fig. 1 is used to purify the synoptic diagram of conventional apparatus of electroluminescent organic material;
The decomposition diagram of Fig. 2 example explanation conventional container box;
Fig. 3 represents according to the first embodiment of the present invention, the schematic representation of apparatus of the electroluminescent organic material that is used to purify;
Fig. 4 A and 4B be according to the first embodiment of the present invention, and coupling between transom and interior pipe and the coupled view between improved transom and interior pipe are described respectively;
The figure of the temperature distribution in Fig. 5 A to 5D describes respectively in the inside of pipe;
Fig. 6 describes according to second preferred embodiment of the present invention, the schematic representation of apparatus of the electroluminescent organic material that is used to purify;
Fig. 7 A and 7B provide according to a second embodiment of the present invention, are used for illustrating respectively coupling between transom and interior pipe and the coupled view between improved transom and interior pipe;
Fig. 8 A and 8B are according to second preferred embodiment of the present invention, set forth the frontview and the side-view of carrier gas feed unit respectively;
Fig. 9 discusses the synoptic diagram of organic electroluminescent device;
Figure 10 represents to be used for relatively using respectively the figure of luminous efficiency of the organic electroluminescent device of the electroluminescent organic material of being purified by according to a first advantageous embodiment of the invention device and conventional apparatus;
Figure 11 represents to be used for relatively using respectively the figure of purification efficiency of the organic electroluminescent device of the electroluminescent organic material of being purified by according to a first advantageous embodiment of the invention device and conventional apparatus; And
Figure 12 is provided for using more respectively the figure in treatment time of the purification of the device of first and second preferred embodiments of the present invention and conventional apparatus.
Embodiment
Will be with reference to the accompanying drawings, describe the present invention in detail.
Fig. 3 schematically shows according to a first advantageous embodiment of the invention, the device of the electroluminescent organic material that is used to purify.
As can be seen from Figure 3, device according to a first advantageous embodiment of the invention comprises the interior pipe of being made by quartz 31, the outer tube 32 that covers interior pipe 31 and the first to fourth well heater 34a to 34d that installs along the circumference of outer tube 32.In pipe 31 have the container of material box 35 that is used to keep with purifying.Because the composition of container 35 omits its detailed description with identical with reference to the composition of figure 2 described containers.A plurality of for example four transoms 33 are divided into five sections of a plurality of for example first to the 5th section A-E with the internal portion of interior pipe 31, and each section of managing 31 in the interconnection.Each well heater 34a-34d corresponds respectively to each section A-D, therefore, can heat its correspondent section independently with a certain temperature.If its correspondent section of heating of well heater 34a-34d, the temperature of the section that is adjacent also increases.Because in the present invention, each well heater can heat each section continuously corresponding to each section.At least two sections heat-processed of this pipe also can be by carrying out with respect to the pipe traveling heater or by the sliding apparatus that moves pipe with respect to well heater.
Simultaneously, be installed in vacuum pump 37 its internal portions of energy vacuum-evacuate of an end of interior pipe 31.In addition, in the carrier gas feed unit 38 that is installed in its other end can be transported to nitrogen or rare gas element in the pipe 31.
Fig. 4 A describes according to a first advantageous embodiment of the invention, the coupling that transom 33 and interior pipe are 31.Manage in 31 in the part that each transom 33 inserts between two sections of interior pipe 31.Each transom 33 has and is used for part closes two intersegmental spatial dividing plates 42 and the hole 41 that forms on the centre portions basically of dividing plate 42.
Fig. 4 B describes the coupling of 31 of improved transom 33a and interior pipes.As can be seen from Figure 4B, the structure of improved transom 33a with in the similar of the transom 33 shown in Fig. 4 A.That is, each improves the hole 46 that transom 33a also has dividing plate 45 and forms on the centre portions of dividing plate 45, except that the net of arranging on hole 46 43.
Transom 33 and 33a and net 43 can be made by any material of selecting from quartz, stainless steel, aluminium, gold and silver, platinum, nickel, tetrafluoroethylene, urethane and glass or these mixtures of material.Hole 41 and 46 diameter are approximately greater than 3mm but less than 10mm.Each calibration of net 43 is from about 0.1mm * 0.1mm to about 5mm * 5mm.
Hereinafter, use description to method by the material that uses according to a first advantageous embodiment of the invention purifying plant to purify to purify.
The material with purifying that comprises impurity is placed in the container 35, and container 35 is placed among first section A of interior pipe 31.If heat this well heater 34a, the material of mainly purifying is shifted to second section B so that be higher than the sublimation temperature that is included in the pure material in the purification material.At this moment, as can be seen from Figure 5A, in first section A, the temperature of interior pipe 31 the highest and in next section B to D step-down.The material that to purify when distillation and when making it be phase-changed into gas is discharged distillation gas by the hole of container 35, and the carrier gas stream by being provided by carrier gas feed unit 38 is shifted to second section B then.In this case, gas shown in Fig. 4 A, or passes through net 43, shown in Fig. 4 B by the hole of the dividing plate 42 of transom 33. Dividing plate 42 and 45 hole 41 and 46 are used to prevent that impurity from shifting to another section.
By the temperature of control heater 34a and the flow rate of carrier gas, can control the crystallization position of the distillation gas on the internal surface of second section B.Be preferably in crystallization and purification material on the centre portions of second section B.
After finishing first purification process, only the impurity from main purification material is retained among first section A.On the other hand, purer material is present among second section B.Then, well heater 34b heats its correspondent section, i.e. second section B.At this moment, thermograde is shown in Fig. 5 B.The gas that distils in second section B flows into the 3rd section C by the hole 41 of transom 33 or by the net 43 for preparing on the hole of transom 33.As the result of aforesaid second stage purification process, from the impurity of purer material still in second section B and purer material in the 3rd section C.
In a like fashion, operate the 3rd well heater and the 4th well heater, and in the 3rd section C and the 4th section D, with material to be purified purifying more and more.Therefore, the purest material is retained among the 5th section E.
Purifying plant according to a first advantageous embodiment of the invention is applied to be used to purify oxine (8-hydroxyquinolinato) aluminium (Alq
3) experiment, oxine aluminium is the luminescent material that is used to make organic electroluminescent device, wherein, Alq
3The producer guarantee the Alq comprised
3Purity greater than 95%.
Alq with 20g
3Put into container 35, and in first section A, settle container 35.Then, by managing 31 in vacuum pump 37 vacuum-evacuate, make per minute 50cm then
3Nitrogen flow into wherein.When room temperature, make the temperature of primary heater 34a be elevated to 340 ℃ and reach three hours, its enough high so that distillation electroluminescent organic material, and the temperature that is raise was kept six hours.At this moment, because the high temperature of primary heater 34a, the temperature of second section B reaches about 220 ℃.When the temperature of primary heater 34a reaches 340 ℃, make the temperature of secondary heater 34b be elevated to 340 ℃ after five hours from 220 ℃.Reach 340 ℃ the moment from the temperature of secondary heater 34b, naturally cooling primary heater 34a.Make the temperature maintenance of secondary heater 34b reach six hours at 340 ℃.After five hours, the 3rd well heater 34c begins heating.Said process can be applied to third and fourth well heater 34c and the 34d equally.In addition, in another case, by moving single well heater with respect to pipe in single, or with respect to single well heater move single in pipe, also can heat at least two sections.
For method of the present invention and traditional method are compared, can differently carry out experiment.In other words, after the operation of finishing secondary heater 34b, collect the lip-deep crystalline purification in the inside material of the 3rd section C shown in Figure 3.In another experiment, after the operation of finishing the 4th well heater 34d, collect the still material in the 5th section E.When finishing heating at last, pipe 31 reaches three hours in the naturally cooling, till its temperature reaches room temperature.Then, discharge the vacuum state of interior pipe 31 and the Alq that collects purification
3After finishing purification process, finding has a small amount of chocolate impurity in the internal portion of container 35 and on the internal surface of second to the 4th section B to D of interior pipe 31.
In first preferred embodiment of the present invention shown in Fig. 3,4A and the 4B, the quantity of material if increase is packed in this container, the heat transfer that enters the material in the container becomes difficult, therefore, has increased the purification processes time, thereby worsens purification efficiency.In addition, under the situation of needs purification lot of materials, carrier gas may be transported in the interior pipe unevenly.
For addressing the above problem, according to second preferred embodiment of the present invention, the device of the electroluminescent organic material that is used to purify have a large amount of in pipe and a plurality of transom.
Total cross-sectional area of pipe approximates the cross-sectional area of interior pipe according to a first advantageous embodiment of the invention in according to a second, preferred embodiment of the present invention.
Fig. 6 describes according to second preferred embodiment of the present invention, the schematic representation of apparatus of the electroluminescent organic material that is used to purify.The explanation of Fig. 7 A and 7B example is used in transom 53 and the 53a in according to a second embodiment of the present invention the purifying plant.Fig. 8 A and 8B schematically show the carrier gas feed unit that is used in the purifying plant.
Purifying plant according to a second, preferred embodiment of the present invention comprise by quartz make a plurality ofly for example manage 51 in 7, cover in the outer tube 52 of pipe 51 and the first to fourth well heater 54a to 54b that settles along the periphery of outer tube 52.Because pipe 51 has identical 26S Proteasome Structure and Function in each, its description will be managed in one.
Simultaneously, the vacuum pump 56 that is installed in an end of outer tube 52 can manage 51 in the vacuum-evacuate.In addition, in the carrier gas feed unit 57 that is installed in the other end of outer tube 52 can be transported to nitrogen or rare gas element in the pipe 51.
Fig. 7 A and 7B are provided for illustrating respectively the coupling of 51 of transom 53 and interior pipes and improve transom 53a and the coupled view of 51 of interior pipes according to a second embodiment of the present invention.
Fig. 7 A once is connected in seven with transom 53 among the 7B and manages 51, therefore, can carry out seven purification process simultaneously.
With reference to figure 7A, example explanation is with the transom 53 of several sections of the internal portion compositions of quartz inner pipe 51.Transom 53 has seven dividing plate 47a, is used for seven hole 46a that part is closed two intersegmental spaces and formed at the centre portions basically of dividing plate 47a.Each transom 53 is connected two sections of settling on its left and right sides, in addition, and pipe 51 in forming.
Structure and the transom 53 shown in Fig. 7 A of transom 53a shown in Fig. 7 B are similar.That is, the hole 46b that transom 53a also has a plurality of dividing plate 47b and forms in the office of central part basically of dividing plate 47b is except that the net 48 of each 46b place, hole preparation.
Carrier gas feed unit 57 shown in Fig. 8 A and the 8B has and is used to hold the space 81 of carrier gas and is used for during a plurality of purification process, makes a plurality of holes 82 of the even mobile of carrier gas.Carrier gas feed unit 57 can be made by use any material of selecting from quartz, stainless steel, aluminium, gold and silver, platinum, nickel, tetrafluoroethylene, urethane, glass or these mixtures of material.The diameter in each hole 82 is in from about 0.1mm to the scope of about 5mm.
Be used for by the method for the material that uses above-mentioned purifying plant according to a second, preferred embodiment of the present invention to purify to purify identical with the device of first preferred embodiment of the application of the invention.Difference is in second preferred embodiment of the present invention, carries out a plurality of purification process simultaneously by pipe 51 in a plurality of.
Although the explanation of foregoing description example has the interior pipe 51 of circular cross section, the cross section of interior pipe 51 can be a rectangle.For example, have the mode of the interior pipe of rectangular cross section with preparation, can carry out purification process, and the material that distributes equably and will purify at the bottom surface portions of interior pipe, wherein the cross-sectional area of pipe approximates total cross-sectional area of pipe in the above-mentioned circle in the rectangle.
Purifying plant according to a second, preferred embodiment of the present invention is applied to be used to purify oxine aluminium (Alq
3) experiment, Alq
3Be the luminescent material that is used to make organic electroluminescent device, wherein Alq
3Manufacturers guarantee the Alq that comprised
3Purity greater than 95%.
The Alq of 3g will be kept
3Seven containers 55 be placed among first section A of pipe 51 in each.Each interior pipe 51 of vacuum pump 56 vacuum-evacuate, then, carrier gas feed unit 57 per minutes are with 50cm
3Nitrogen be transported to wherein.Primary heater 54a at room temperature is heated, and makes its three hours to rise to 340 ℃, and makes enough height keep reaching four hours with the temperature of this rising of the above-mentioned electroluminescent organic material that distils.At this moment, because the high temperature of primary heater 54a, the temperature of second section B reaches 220 ℃.When the temperature of primary heater 54a reaches 340 ℃, make the temperature of secondary heater 54b rise to 340 ℃ after three hours from 220 ℃.Reach 340 ℃ the moment from the temperature of secondary heater 54b, primary heater 54a begins naturally cooling.The temperature maintenance of secondary heater 54b reaches four hours at 340 ℃, and after three hours, the 3rd well heater 54c begins heating.These processes can similarly be applied to third and fourth well heater 54c and the 54d.Also can carry out at least two sections heat-processed of pipe by being used for moving the sliding apparatus of pipe with respect to the pipe traveling heater or with respect to well heater.
In this experiment, after the operation of finishing the 4th well heater 54d, collect and remain in the 5th section material among the E.When finishing heating, pipe 51 naturally cooling reach three hours till its temperature reaches room temperature in making.Then, discharge the vacuum state of interior pipe 51 and the Alq that collects purification
3After finishing purification process, finding has a small amount of chocolate impurity on the internal surface of second to the 4th section B to D and in the internal portion of container 55.
For with traditional sublimation purification device with compare according to the sublimation purification device of first and second preferred embodiments of the present invention, use conventional apparatus to carry out following experiment.
In traditional sublimation purification device shown in Figure 1, the Alq of the 20g that container 4 maintenances will be purified
3, an end of pipe 1 in being placed in then, wherein it should hold the end corresponding to the outer tube that well heater 5 is installed.In addition, the condition that is used in the device of the present invention is applied to conventional apparatus equally.That is, by vacuum pump 6 vacuum-evacuate containers 4 and to delivery of carrier gas wherein.At room temperature heat this well heater 5 and reach three hours, reach till 340 ℃, and the temperature that keeps being improved reaches six hours up to its temperature.To next three hours, make container 4 coolings till its temperature reaches room temperature.Discharge the vacuum state of container 4 subsequently and collect the Alq that purifies
3At this moment, in container 4, find also not have the chocolate impurity of purification.Behind cleaning and drying receptacle box 4 and interior pipe 1, once more with the Alq that purifies
3Put into container 4, and carry out identical purification process four times.In each purification process, the Alq that verification is collected
3Amount and treatment time thereof.
Fig. 9 provides the synoptic diagram of the organic electroluminescent device that uses the electroluminescent organic material of purifying by first preferred embodiment of the present invention.
With reference to figure 9, hole transmission layer 63, the purification electroluminescent organic material (Alq for example of transparent electrode layer 62, for example triphenyldiamine (TPD) of ITO for example is installed sequentially on the surface of glass substrate 61
3) luminous/electron transfer layer 64 and metal electrode layer 65.Apply voltage at transparent electrode layer 62 and 65 on metal electron layer.
Figure 10 represents to be used for relatively using respectively the figure of luminous efficiency of the organic electroluminescent device of the electroluminescent organic material of purifying by conventional apparatus and device according to a first advantageous embodiment of the invention.
The luminous efficiency by the organic electroluminescent device of the material of purifying with reference to figure 1 described conventional apparatus is used in data point 71 expressions.In this case, it is frequent more to carry out purification process, and it is high more that luminous efficiency becomes.The luminous efficiency of the organic electroluminescent device of the material of being purified by device is according to a first advantageous embodiment of the invention used in data point 73 expressions.At this moment, the material of only operating the first and second well heater 34a and 34b and being collected in the 3rd section purification among the C.Simultaneously, operating each well heater 34a to 34d and be collected under the situation of the 5th section purification material among the E, data point 74 is described the luminous efficiency of the organic electroluminescent device that uses the material of being purified by device according to a first advantageous embodiment of the invention.As can be seen from Figure 10, the material of being purified by device according to a first advantageous embodiment of the invention provides higher luminous efficiency.
Figure 11 represents to be used for to use more respectively the figure of the purification efficiency of the organic electroluminescent device of being purified by according to a first advantageous embodiment of the invention device and conventional apparatus.
The quantity of material of data point 91 expressions by using conventional apparatus shown in Figure 1 to collect.The quantity of material that data point 92 and 93 expressions are collected in the 3rd and the 5th section C of device of the present invention shown in Figure 3 and E respectively.Can clearly be seen that from Figure 11, under the situation of the 20g material that input will be purified, carry out four purification process, thereby collect 17.2g (input 86%) with traditional method.Yet, if use according to a first advantageous embodiment of the invention apparatus and method, collect about 18.6g (input 93%), it provides the purification efficiency higher than traditional method.The manufacturers that considers the electroluminescent organic material of will purify guarantees 95% purity, with new method of purification, can collect the full dose of the material of almost purifying.
Figure 12 is provided for using more respectively device and the conventional apparatus according to first and second preferred embodiments of the present invention, the figure in the treatment time of purification.
With reference to Figure 12, conventional apparatus needed about 14 hours so that carry out the primary purification process: the input time of material to be purified (1 hour), heat-up time (3 hours), heating are held time (6 hours), cooling time (3 hours), collection and scavenging period (1 hour) and re-enter the material that will purify.Therefore, this process is carried out four times in its cost 56 in a small amount.Yet, the iron device needs to carry out in 32 hours purification process according to a first advantageous embodiment of the invention: the material time (1 hour) that input will be purified, heat-up time (3 hours), heating hold time (24 hours, promptly 6 hours * 4 times), cooling time (3 hours) and collection and scavenging period (1 hour).Device according to a second, preferred embodiment of the present invention needs carry out in 24 hours purification process: the material time (1 hour) that input will be purified, heat-up time (3 hours), heating hold time (16 hours, promptly 4 hours * 4 times), cooling time (3 hours) and collection and scavenging period (1 hour).
Apparatus and method according to the electroluminescent organic material that is used to purify of the present invention provide than conventional apparatus and the higher luminous and purification efficiency of method.In addition, when the material of needs purification same amount, shorten the treatment time.In other words, when predefined process during, the more substantial material of purifying.Because the present invention carries out a plurality of processes at the fixed time, the material in the container can be distributed and conduct heat and become effective.Therefore, use the organic electroluminescent device of the electroluminescent organic material of purifying to help producing in batches and also providing high quality by apparatus and method of the present invention.
Although with reference to preferred embodiment, illustrate and described the present invention, it should be appreciated by those skilled in the art that and under the situation that does not deviate from the spirit and scope of the present invention that in the accessory claim book, limit, can make various changes and improvements.
Claims (20)
1. the device of the electroluminescent organic material that is used to purify, this device comprises:
Pipe in one or more, be used for material to be purified pack into described one or more in an end of pipes;
Transom is used for pipe in each is divided into a plurality of sections;
Heating unit is used to make these sections of pipe in each to be heated to above the sublimation temperature of material to be purified;
Vacuum pump, the section that is used for pipe in the vacuum-evacuate, wherein, each transom has and is used for partially enclosed two intersegmental spatial dividing plates and is used to make distillation gas from material to be purified from its hole of passing through, and this hole is formed on the centre portions basically of dividing plate.
2. purifying plant as claimed in claim 1 is characterized in that, material to be purified once is input to described one or more interior pipe, and further, carries out the purification process at least twice that distils continuously.
3. purifying plant as claimed in claim 1, it is characterized in that, described one or more in the section of pipe material that preservation is to be purified be used as the distillation section of the material to be purified that is used to distil, the section that is placed in the opposite end of distillation section is used as the collection section that is used to collect the purification material, and will distil section and the collection section between one or more sections be used as and distil section or the collection section.
4. purifying plant as claimed in claim 1 further comprises the carrier gas feed unit, be used for the carrier gas from an end of pipe in each is transported to the other end, the carrier gas feed unit be placed in described one or more in an end of pipes.
5. purifying plant as claimed in claim 1 is characterized in that, the hole of the dividing plate of described each transom has the net of the impurity that is used for refining distillation gas.
6. purifying plant as claimed in claim 4 is characterized in that, adjust the vacuum tightness of vacuum pump and the flow rate of the carrier gas supplied with by the carrier gas feed unit so that control the described crystallization position of the distillation gas on the internal surface of pipe in each.
7. purifying plant as claimed in claim 1 is characterized in that heating unit has a plurality of well heaters, and each well heater is corresponding to each section of pipe in each.
8. purifying plant as claimed in claim 1 is characterized in that, heating unit has and is used to heat the described well heater of each section of pipe in each, and can along described one or more in the section traveling heater of pipes.
9. purifying plant as claimed in claim 1 is characterized in that, heating unit have be used to heat described one or more in the well heater of section of pipes, can be with respect to well heater, move described one or more in pipe.
10. purifying plant as claimed in claim 1 is characterized in that, described each transom connects the section of described one or more interior pipes simultaneously.
11. purifying plant as claimed in claim 4 is characterized in that, described carrier gas feed unit has and is used to make a plurality of holes of the even mobile of supply gas.
12. purifying plant as claimed in claim 4 is characterized in that, the carrier gas of being supplied with by the carrier gas feed unit is nitrogen or rare gas element.
13. purifying plant as claimed in claim 1 is characterized in that, transom is by making from any material of quartz, stainless steel, aluminium, gold and silver, platinum, nickel, tetrafluoroethylene, urethane and glass or the selection of these mixtures of material.
14. purifying plant as claimed in claim 5 is characterized in that, makes net by using from any material of quartz, stainless steel, aluminium, gold and silver, platinum, nickel, tetrafluoroethylene, urethane and glass or the selection of these mixtures of material.
15. the method for the electroluminescent organic material that is used to purify, the method comprising the steps of:
The internal portion part of pipes in one or more is connected a plurality of sections;
Material to be purified is provided to an end of pipe in each;
By the described the other end of pipe in each, the described pipe in each of vacuum-evacuate; And
Sequentially heat from the section of preservation material to be purified to adjacent segment and describedly to manage in each, to be higher than the sublimation temperature of material to be purified.
16. method as claimed in claim 15 is characterized in that, material to be purified once is input to described one or more interior pipe, and further, carries out the purification process at least twice that distils continuously.
17. method as claimed in claim 15, it is characterized in that, described one or more in the section of pipe material that preservation is to be purified be used as the distillation section of the material to be purified that is used to distil, the section that is placed in the opposite end of distillation section is used as the collection section that is used to collect the purification material, and will distil section and the collection section between one or more sections be used as and distil section or the collection section.
18. method as claimed in claim 15, further comprise with from described in each the carrier gas of an end of pipe be provided to the step of the other end.
19. method as claimed in claim 15 further comprises the step of the impurity that is used for refining distillation gas.
20. method as claimed in claim 18 further comprises the vacuum tightness that is used to control pipe in each and is provided to the flow rate of the described carrier gas of pipe in each so that be controlled at the described step of the crystallization position of the distillation gas on the internal surface of pipe in each.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR20010079725 | 2001-12-15 | ||
| KR2001/79725 | 2001-12-15 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1714061A true CN1714061A (en) | 2005-12-28 |
Family
ID=19717088
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02828095 Pending CN1714061A (en) | 2001-12-15 | 2002-12-13 | Apparatus and method for purifying an organic electroluminescent material |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP2005511864A (en) |
| KR (1) | KR100959824B1 (en) |
| CN (1) | CN1714061A (en) |
| AU (1) | AU2002358327A1 (en) |
| WO (1) | WO2003051796A1 (en) |
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Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2706936B2 (en) * | 1987-09-09 | 1998-01-28 | スタンレー電気株式会社 | Vacuum sublimation purification equipment |
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| JPH0724205A (en) * | 1993-07-05 | 1995-01-27 | Mitsubishi Cable Ind Ltd | Sublimating method |
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-
2002
- 2002-12-13 WO PCT/KR2002/002344 patent/WO2003051796A1/en active Application Filing
- 2002-12-13 KR KR1020020079681A patent/KR100959824B1/en not_active IP Right Cessation
- 2002-12-13 JP JP2003552688A patent/JP2005511864A/en active Pending
- 2002-12-13 CN CN 02828095 patent/CN1714061A/en active Pending
- 2002-12-13 AU AU2002358327A patent/AU2002358327A1/en not_active Abandoned
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Also Published As
| Publication number | Publication date |
|---|---|
| AU2002358327A1 (en) | 2003-06-30 |
| JP2005511864A (en) | 2005-04-28 |
| KR20030051311A (en) | 2003-06-25 |
| KR100959824B1 (en) | 2010-05-28 |
| WO2003051796A1 (en) | 2003-06-26 |
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