CN105268370A - Fluidization device and fluidization technology - Google Patents
Fluidization device and fluidization technology Download PDFInfo
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- CN105268370A CN105268370A CN201510852425.XA CN201510852425A CN105268370A CN 105268370 A CN105268370 A CN 105268370A CN 201510852425 A CN201510852425 A CN 201510852425A CN 105268370 A CN105268370 A CN 105268370A
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- trimethyl indium
- chuck
- casing
- fluidizer
- condensation
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Abstract
The invention provides a fluidization device which comprises a melting device and a crystallization device of which the inlet is connected with the outlet of the melting device, wherein the crystallization device is a box body with a clamping sleeve on the side wall; an inlet is formed in the upper part of the box body; a material receiving device is arranged at the lower part of the box body; a condensing substance is arranged in the clamping sleeve of the box body; and a multihole condensing air pipe is arranged in the box body. According to the fluidization device provided by the invention, after being melted, trimethyl indium is discharged from the outlet of the melting device and enters the box body from the inlet of the crystallization device; under the dual condensation action of the box body and the condensing air pipe, the melted trimethyl indium condensing effect is extremely good; meanwhile, condensing air sweeps the dropping trimethyl indium through holes in the condensing air pipe, so that trimethyl indium particles received by the receiving device are large in size, uniform and high in flowability.
Description
Technical field
The present invention relates to technical field of semiconductors, especially relate to a kind of fluidizer and fluid technology.
Background technology
Trimethyl indium, as the primary raw material of LED industry, is widely used in MOCVD, molecular beam epitaxy field.Trimethyl indium character is active, and meeting water blast, meet air spontaneous combustion, is white crystalline solid.And it is in the application process of MOCVD, need grain diameter evenly, good fluidity because large particle can increase material gas-contact area in use, in use procedure, flow can be more stable, and use amount is more thorough.Cannot produce as requested in prior art and formulate the trimethyl indium of size, so one bottle of 350g fills that trimethyl indium utilization rate is the highest can only accomplish 85% ~ 90% in utilization rate, remaining 10% ~ 15% cannot use.
In prior art to the control of trimethyl indium granularity mostly for control on a production line, be specially in rectifying is produced, the trimethyl indium producing granular size uneven directly enters condenser condenses, and by controlling condensing reflux ratio thus making condensation rate slow, directly can affect the progress of production line, and this kind of condensing mode crystallization effect is final also bad, thus cause utilization rate low.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of fluidizer, and the trimethyl indium particle of fluidizer fluidisation provided by the invention is large, good fluidity and utilization rate is high.
The invention provides a kind of fluidizer, comprising: the crystallization apparatus that thawing apparatus is connected with the outlet of described thawing apparatus with entrance;
Described crystallization apparatus is the casing that sidewall is provided with chuck, and described casing top is provided with entrance, and bottom is provided with material receiver;
Condensed material is provided with in the chuck of casing;
Porous condensation tracheae is provided with in casing.
Preferably, described condensation tracheae enters in casing through the chuck of casing.
Preferably, the hole on described condensation tracheae is uniformly distributed.
Preferably, the aperture on described condensation tracheae becomes large gradually by entrance to the Way out of condensation tracheae.
Preferably, the tank inlet of described crystallization apparatus is provided with Dropping feeder.
Preferably, described thawing apparatus sidewall is provided with chuck, is provided with heatable substance in described chuck.
The invention provides a kind of technique adopting fluidizer fluidisation trimethyl indium described in technique scheme, comprising:
Trimethyl indium is inserted thawing apparatus heating and melting, the chuck in crystallization apparatus and condensing gas pipework condensation, obtain the trimethyl indium of fluidisation on the reception device;
In described condensation tracheae, gas flow rate is 10 ~ 30L/min.
Preferably, the tank inlet of described crystallization apparatus is provided with Dropping feeder, and described rate of addition is 10 ~ 60d/min.
Preferably, the described thawing time is 2 ~ 3h.
Preferably, described heating-up temperature is 90 ~ 110 DEG C.
Compared with prior art, the invention provides a kind of fluidizer, comprising: the crystallization apparatus that thawing apparatus is connected with the outlet of described thawing apparatus with entrance; Described crystallization apparatus is the casing that sidewall is provided with chuck, and described casing top is provided with entrance, and bottom is provided with material receiver; Condensed material is provided with in the chuck of casing; Porous condensation tracheae is provided with in casing.Fluidizer provided by the invention by by after trimethyl indium melting, is exported out by thawing apparatus, then enters casing by crystallization apparatus entrance, by the dual condensation of casing and condensation tracheae, makes for melting trimethyl indium condensation effect fabulous; And condensed gas purges the trimethyl indium of drippage by the hole on condensation tracheae, make the trimethyl indium particle that finally receives at receiving system large, evenly and good fluidity and utilization rate is high.
Accompanying drawing explanation
Fig. 1 is the fluidizer stereogram shown in the embodiment of the present invention;
Fig. 2 is the fluidizer side view shown in the embodiment of the present invention.
Detailed description of the invention
The invention provides a kind of fluidizer, comprising: the crystallization apparatus that thawing apparatus is connected with the outlet of described thawing apparatus with entrance;
Described crystallization apparatus is the casing that sidewall is provided with chuck, and described casing top is provided with entrance, and bottom is provided with material receiver;
Condensed material is provided with in the chuck of casing;
Porous condensation tracheae is provided with in casing.
Fluidizer provided by the invention comprises thawing apparatus.Described thawing apparatus is preferably clamping device, and more preferably the sidewall of thawing apparatus is provided with chuck, is provided with heatable substance in the chuck of described clamping device.
The present invention does not limit for the shape of described thawing apparatus and specification, can be cuboid or cylindrical.Described thawing apparatus preferably adopts 316L stainless steel to make.
The volume of the chuck of described thawing apparatus and the volume ratio of thawing apparatus are preferably 1:(8 ~ 10).
Conduction oil is preferably in the chuck of described thawing apparatus.It is made to melt by above-mentioned heat-conducting oil heating trimethyl indium.
In the present invention, described thawing apparatus sidewall is provided with heater import and heating means exit, and described heater import is arranged at bottom, and heating means exit is arranged at top.
The volume of described interpolation conduction oil is preferably more than 90% of whole jacket volume.
In the present invention, described thawing apparatus is preferably provided with dismountable top cover, produces front opening, closes during use.
In the present invention, the entrance of described crystallization apparatus is connected with the outlet of described thawing apparatus.Preferably, described thawing apparatus is arranged on described crystallization apparatus.
The invention provides crystallization apparatus is the casing that sidewall is provided with chuck, and described casing top is provided with entrance, and bottom is provided with material receiver; Condensed material is provided with in the chuck of casing; Porous condensation tracheae is provided with in casing.
In the present invention, described crystallization apparatus is the casing that sidewall is provided with chuck, and crystallization apparatus of the present invention preferably adopts 316L stainless steel to make.In the side of crystallization apparatus of the present invention, except arranging the one side of opening, all the other each faces are provided with chuck.
In the present invention, the ratio of the volume of the chuck of described crystallization apparatus and the volume of described crystallization apparatus is preferably 1:6 ~ 8.
Preferably be provided with liquid nitrogen in described chuck, the volume of described liquid nitrogen and the ratio of described jacket volume are preferably 1.5 ~ 2.5:3.Described chuck wall box is also provided with liquid nitrogen import.
Described chuck wall box is also provided with offgas outlet, for emission.
In the present invention, the tank inlet of described crystallization apparatus is provided with Dropping feeder, and described Dropping feeder preferably includes valve, can pass through Valve controlling rate of addition.Preferably, described Dropping feeder is arranged at casing top.
The quantity of described Dropping feeder is preferably 1 ~ 10, is more preferably 2 ~ 8.
Described Dropping feeder is preferably provided with insulation material outward, and described insulation material preferably adopts inner glass cotton, middle PTFE wall and outside watertight composition.
In the present invention, porous condensation tracheae is provided with in described casing, described condensation tracheae is preferably arranged along wall box, more preferably be parallel to bottom half along wall box to arrange, the magnitude setting of the present invention to described condensation tracheae does not limit, and can arrange a circle, two circles or multi-turn arrange along wall box.
In the present invention, described casing both sides are provided with condensing gas tube inlet and outlet, and described condensing gas tube inlet is preferably disposed on body side bottom.Be more preferably concrete bottom 40 ~ 80mm, most preferably be distance bottom 50 ~ 70mm.
Described condensation tracheae more preferably enters in casing through the chuck of casing, and the present invention does not limit the described loop of condensation tracheae in chuck, can be preferably that one or more loop is arranged, also can arrange for helical form.
In the present invention, the endotracheal gas of described condensation is preferably nitrogen, and described condensation tracheae is arranged porose, the hole on condensation tracheae is uniformly distributed, and span is preferably 15 ~ 25mm; Preferred, the aperture on described condensation tracheae becomes large gradually by entrance to the Way out of condensation tracheae, and aperture, preferably with the 2 ~ 3mm started, increases by 0.4 ~ 0.6mm every 5 holes.
The perforate mode in the hole on described condensation tracheae is preferably oblique perforate, and oblique perforate is more conducive to condenser and blows to whole cavity, thus condensation effect is better.
The present invention adopts above-mentioned setting that the tolerance of condensation tracheae can be made to be uniformly distributed, and better carries out condensation.
Lower box of the present invention is provided with receiving system, and the present invention does not limit for the concrete shape of described receiving system and specification, can be take-up reel.
As long as after the trimethyl indium of the whereabouts of fused solution is subject to the lower chamber of low temperature, be subject to the purging of condenser, the solid-state trimethyl indium of final formation drops in receiving system.
Fluidizer provided by the invention by by after trimethyl indium melting, is exported out by thawing apparatus, then enters casing by crystallization apparatus entrance, by the dual condensation of casing and condensation tracheae, makes for melting trimethyl indium condensation effect fabulous; And condensed gas purges the trimethyl indium of drippage by the hole on condensation tracheae, make the trimethyl indium particle that finally receives at receiving system large, evenly and good fluidity.
As depicted in figs. 1 and 2, wherein, Fig. 1 is the fluidizer stereogram shown in the embodiment of the present invention to fluidizer structural representation described in one of them technical scheme of the present invention; Fig. 2 is the fluidizer side view shown in the embodiment of the present invention.
1 is heatable substance outlet, and 2 is thawing apparatus, and 3 is crystallization apparatus, and 4 is condensing gas import, and 5 is condensation tracheae circuit in chuck; 6 is condensed material import, and 7 is heatable substance entrance, and 8 is receiving system, and 9 is condensation tracheae, and 10 is Dropping feeder.
The invention provides a kind of technique adopting fluidizer fluidisation trimethyl indium described in technique scheme, comprising:
Trimethyl indium is inserted thawing apparatus heating and melting, the chuck in crystallization apparatus and condensing gas pipework condensation, obtain the trimethyl indium of fluidisation on the reception device;
In described condensation tracheae, gas flow rate is 10 ~ 30L/min.
First trimethyl indium is inserted thawing apparatus heating and melting by the present invention, and the temperature of described heating is preferably 90 ~ 110 DEG C, and the time of described heating and melting is preferably 2 ~ 3h.
The tank inlet of described crystallization apparatus is provided with Dropping feeder, and after thawing apparatus melts, dripped by Dropping feeder, described rate of addition is 10 ~ 60d/min, is more preferably 15 ~ 55d/min.
The rate of addition of above-mentioned Dropping feeder is slower, and particle is larger, can be controlled the granular size of the trimethyl indium needing to obtain by control rate.
The liquid trimethyl indium of melting is subject to the purging effect of condensation and condensation tracheal strips nitrogen in crystallization apparatus chuck, finally obtains the trimethyl indium of fluidisation on the reception device.
In the present invention, in described condensation tracheae, gas flow rate is 10 ~ 30L/min, is more preferably 15 ~ 25L/min.
Have above each device of the present invention clearly to describe and do not repeated them here.
When using device of the present invention to prepare fluidisation trimethyl indium, be preferably placed in glove box; Described glove box is preferably water oxygen value≤0.1ppm.
Device of the present invention preferably rinses through alkali cleaning, pickling, water, dries and put into the glove box being full of nitrogen more before use.
Be specially, through the alkali cleaning of 8% ~ 12%, through the pickling of 2% ~ 3%, and after totally dry through pure water rinsing the glove box put into again and be full of nitrogen.
The present invention does not limit for described alkali, alkali well known to those skilled in the art, can be NaOH, potassium hydroxide.
The present invention does not limit for described acid, acid well known to those skilled in the art, can be hydrochloric acid, nitric acid.
The present invention preferably adopts following assay method to measure the granular size of trimethyl indium, utilization rate and impurity content:
Granular size: use vernier caliper measurement after sieving.
Utilization rate: weighing method.
Dirt content test: 6N trimethyl indium standard.
In order to further illustrate the present invention, below in conjunction with embodiment, fluidizer provided by the invention and fluid technology are described in detail.
Embodiment 1
Fluidizer prepared by the overall 316L stainless steel that adopts.Be specially: thawing apparatus is cylindrical, external diameter is 400mm internal diameter is 360mm; Be conduction oil in chuck; Crystallization apparatus length is 450mm height for 600mm is wide is 400mm, and jacket thickness is 20mm; Be liquid nitrogen in chuck, condensation tracheal strips is nitrogen, condensing gas tube inlet distance bottom 60mm, and condensation tracheae is entered by both sides, casing is being entered along having walked a loop in chuck, in casing, being parallel to bottom along sidewall, son is arranged in " mouth ", and casing top arranges six Dropping feeders, and take-up reel is arranged at bottom, porose on condensation tracheae, span is 20mm, and aperture, with the 2mm started, increases 0.5mm every 5 holes.
Embodiment 2
Use the fluidizer that embodiment 1 prepares, open the top cover of upper cavity, put into trimethyl indium 500g qualified after testing, lock top cover, unlatching conduction oil circulates, and oil temperature is set as 100 DEG C, after trimethyl indium all melts (2 hours), lower chamber passes into liquid nitrogen, and amount of liquid nitrogen is 1/3 of chuck volume.After 10min, pass into nitrogen, control nitrogen flow rate is 10L/min.Open Dropping feeder valve, controlling the trimethyl indium speed of dripping is 10/min.Obtain the trimethyl indium 493g (after 10 object sieve, measuring diameter) that particle diameter is 2-3mm.After through sampling, analyze detect, impurity content meets 6N trimethyl indium standard.Fill one bottle of 350g trimethyl indium to use, use middle good fluidity.Compare using front and after using material to weigh, surplus 3g in steel cylinder, utilization rate can reach more than 99%.
Embodiment 3
Use the fluidizer that embodiment 1 prepares, open the top cover of upper cavity, put into trimethyl indium 500g qualified after testing, lock top cover, unlatching conduction oil circulates, and oil temperature is set as 90 DEG C, after trimethyl indium all melts (3 hours), lower chamber passes into liquid nitrogen, and amount of liquid nitrogen is 2/3 of chuck volume.After 10min, pass into nitrogen, control nitrogen flow rate is 15L/min.Open Dropping feeder valve, controlling the trimethyl indium speed of dripping is 30/min.Obtain the trimethyl indium 490g (after 18 object sieve, measuring diameter) that particle diameter is 1-1.5mm.After through sampling, analyze detect, impurity content meets 6N trimethyl indium standard.Fill one bottle of 350g trimethyl indium to use, use middle good fluidity.Compare using front and after using material to weigh, surplus 10g in steel cylinder, utilization rate can reach more than 97%.
Embodiment 4
Use the fluidizer that embodiment 1 prepares, open the top cover of upper cavity, put into trimethyl indium 500g qualified after testing, lock top cover, unlatching conduction oil circulates, and oil temperature is set as 110 DEG C, after trimethyl indium all melts (2 hours), lower chamber passes into liquid nitrogen, and amount of liquid nitrogen is 2/3 of chuck volume.After 10min, pass into nitrogen, control nitrogen flow rate is 20L/min.Open Dropping feeder valve, controlling the trimethyl indium speed of dripping is 50/min.Obtain the trimethyl indium 488g (after 35 object sieve, measuring diameter) that particle diameter is 0.5-0.7mm., after through sampling, analyze detect, impurity content meets 6N trimethyl indium standard.Fill one bottle of 350g trimethyl indium to use, use middle good fluidity.Compare using front and after using material to weigh, surplus 15g in steel cylinder, utilization rate can reach more than 95%.
Embodiment 5
Use the fluidizer that embodiment 1 prepares, open the top cover of upper cavity, put into trimethyl indium 500g qualified after testing, lock top cover, unlatching conduction oil circulates, and oil temperature is set as 110 DEG C, after trimethyl indium all melts (2 hours), lower chamber passes into liquid nitrogen, and amount of liquid nitrogen is 2/3 of chuck volume.After 10min, pass into nitrogen, control nitrogen flow rate is 30L/min.Open Dropping feeder valve, controlling the trimethyl indium speed of dripping is 60/min.Obtain the trimethyl indium 493g (after 50 object sieve, measuring diameter) that particle diameter is 0.3mm.After through sampling, analyze detect, impurity content meets 6N trimethyl indium standard.Fill one bottle of 350g trimethyl indium to use, use middle good fluidity.Compare using front and after using material to weigh, surplus 25g in steel cylinder, utilization rate can reach more than 92%.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a fluidizer, comprising: the crystallization apparatus that thawing apparatus is connected with the outlet of described thawing apparatus with entrance;
Described crystallization apparatus is the casing that sidewall is provided with chuck, and described casing top is provided with entrance, and bottom is provided with material receiver;
Condensed material is provided with in the chuck of casing;
Porous condensation tracheae is provided with in casing.
2. fluidizer according to claim 1, is characterized in that, described condensation tracheae enters in casing through the chuck of casing.
3. fluidizer according to claim 1, is characterized in that, the hole on described condensation tracheae is uniformly distributed.
4. fluidizer according to claim 3, is characterized in that, the aperture on described condensation tracheae becomes large gradually by entrance to the Way out of condensation tracheae.
5. fluidizer according to claim 1, is characterized in that, the tank inlet of described crystallization apparatus is provided with Dropping feeder.
6. fluidizer according to claim 1, is characterized in that, described thawing apparatus sidewall is provided with chuck, is provided with heatable substance in described chuck.
7. adopt a technique for fluidizer fluidisation trimethyl indium according to claim 1, comprising:
Trimethyl indium is inserted thawing apparatus heating and melting, the chuck in crystallization apparatus and condensing gas pipework condensation, obtain the trimethyl indium of fluidisation on the reception device;
In described condensation tracheae, gas flow rate is 10 ~ 30L/min.
8. fluid technology according to claim 7, is characterized in that, the tank inlet of described crystallization apparatus is provided with Dropping feeder, and described rate of addition is 10 ~ 60d/min.
9. fluid technology according to claim 7, is characterized in that, the described thawing time is 2 ~ 3h.
10. fluid technology according to claim 7, is characterized in that, described heating-up temperature is 90 ~ 110 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510852425.XA CN105268370A (en) | 2015-11-27 | 2015-11-27 | Fluidization device and fluidization technology |
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| CN201510852425.XA CN105268370A (en) | 2015-11-27 | 2015-11-27 | Fluidization device and fluidization technology |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2164312Y (en) * | 1993-07-05 | 1994-05-11 | 天津大学 | Caustic sode prill tower |
| US20060099270A1 (en) * | 2003-05-22 | 2006-05-11 | Applied Nanosystems B.V. | Production of small particles |
| GB2443531A (en) * | 2006-10-30 | 2008-05-07 | Sumitomo Chemical Co | Method of vaporizing solid organometallic compound |
| CN101279221A (en) * | 2007-12-28 | 2008-10-08 | 天津天士力制药股份有限公司 | Equipment for preparing dropping pill with air cooled by cold trap |
| CN202022876U (en) * | 2011-02-15 | 2011-11-02 | 江苏南大光电材料股份有限公司 | Trimethyl indium purifying device |
-
2015
- 2015-11-27 CN CN201510852425.XA patent/CN105268370A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2164312Y (en) * | 1993-07-05 | 1994-05-11 | 天津大学 | Caustic sode prill tower |
| US20060099270A1 (en) * | 2003-05-22 | 2006-05-11 | Applied Nanosystems B.V. | Production of small particles |
| GB2443531A (en) * | 2006-10-30 | 2008-05-07 | Sumitomo Chemical Co | Method of vaporizing solid organometallic compound |
| CN101279221A (en) * | 2007-12-28 | 2008-10-08 | 天津天士力制药股份有限公司 | Equipment for preparing dropping pill with air cooled by cold trap |
| CN202022876U (en) * | 2011-02-15 | 2011-11-02 | 江苏南大光电材料股份有限公司 | Trimethyl indium purifying device |
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Application publication date: 20160127 |