CN101891218A - Production method for high-purity boron tribromide - Google Patents
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- CN101891218A CN101891218A CN 201010199221 CN201010199221A CN101891218A CN 101891218 A CN101891218 A CN 101891218A CN 201010199221 CN201010199221 CN 201010199221 CN 201010199221 A CN201010199221 A CN 201010199221A CN 101891218 A CN101891218 A CN 101891218A
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Abstract
The invention discloses a production method for high-purity boron tribromide, which comprises the following steps of: placing industrial grade boron tribromide into a container, adding 1 to 2 percent of decoloration adsorbent, keeping with slightly stirring for 60 to 80 minutes, and filtering by using a microfilter of below 0.05 micron; distilling the obtained filtrate by using a sub-boiling distiller, and adjusting the heating pipe voltage-stabilized liquid level temperature to be 60 to 75 DEG C; feeding the obtained distillate into a plate rectification column for distillation reflux, controlling the reflux time to be 5 to 6 hours, removing a low-boiling-point substance, feeding a boron tribromide pure product obtained from 89 to 93-degree centigrade distillate to another rectification column for rectification again, and controlling the reflux time to be 5 to 6 hours; and feeding 89 to 92.5-degree centigrade distillate into a finished product groove, and after the product is detected to be qualified, filtering and packing under the purification environment of which the whole is no more than a thousand level and of which the part is no more than a hundred level to obtain a high-purity boron tribromide product of 99.99999 percent. The method has the advantages of simple process, convenient operation, easy quality control and low finished product cost.
Description
Technical field
The invention belongs to the material technology field, relate in particular to a kind of production method of microelectronics industry material.
Background technology
In recent years, along with being on the rise of problems such as energy shortage, environmental pollution, solar cell has obtained good development opportunity with its clean environment firendly, reproducible advantage, various countries formulate the encouragement policies of photovoltaic generation and huge photovoltaic engineering project one after another, for solar cell industry has been created the huge market space, it has been imported a rare high-speed developing period.The data demonstration, in nearly 10 years, 35 times of global solar battery industry scale enlarged proximal.
But the solar cell cost is high than water power, coal electricity, has seriously restricted the large-scale application of solar cell, and the low-cost solar battery is also being pursued by each macrocell producer, researches and develops variously can reduce the battery cost techniques.As: aspect crystal silicon cell, P type silion cell technology is arranged, N type silicon high-efficiency battery technology, laser grooving buries grid cell technology etc.; Aspect hull cell, the polycrystalline silicon thin film solar cell technology is arranged, CIGS battery technology, cadmium telluride battery technology etc.
Along with the development of N type silicon high performance solar batteries technology, it effectively reduces cell decay speed, extending battery life, and then advantage such as reduce cost receives much attention.Domestic each big sun power producer is all carrying out the experiment of this respect, and has obtained bigger progress.In Aerospace Engineering, it is the heavily doped of height field that boron tribromide also is used for to high performance solar batteries back of the body field, realizes the abundant accumulation to current carrier.A back of the body heavily doped use boron tribromide replenish/increases the weight of p type impurity concentration as doped source, and this kind battery has very high transformation efficiency.Boron tribromide is used as the P type doped source of this battery, and battery is had very strong antidamping ability, can reduce the production cost of solar cell greatly.Other uses boron tribromide as integrated circuit (IC) chip p type doped source, realizes base implant or blocking layer doping, the especially base implant of bipolar transistor.In the integrated circuit (IC) chip processing procedure, also use as the reverse blocking layer of active area doping agent.
The Wang Zhi of department of chemistry of Wuhan University clang, Xie Jine etc. have studied separate impurities technology in high-purity boron bromide, the method that propose to adopt cationic exchange village fat that Mn, Fe, Cr, Ni, Co, Pt, V0 etc. are adsorbed, but its impurity the highest reach 64ppb.Still can not satisfy the requirement of solar cell, unicircuit, discrete device and semiconductor material with high-purity boron tribromide.
Summary of the invention
A kind of technology that the objective of the invention is to overcome above-mentioned shortcoming and provide is simple, easy to operate, quality is convenient to control, the production method of high-purity boron tribromide of low finished product cost.
The production method of a kind of high-purity boron tribromide of the present invention may further comprise the steps:
(1) gets the technical grade boron tribromide in container, add decolorizing adsorbent, under gentle agitation, keep filtering with millipore filter below 0.05 micron after 60-80 minute in the 1-2% ratio;
(2) gained filtrate is regulated heating tube voltage stable liquid surface temperature 60-75 ℃ of scope through the distillation of sub-boiling distillation device;
(3) gained distillation product import the column plate type rectifying tower and carry out distillation and reflux, and return time 5-6 hour, the removal low-boiling-point substance was got pure product of boron tribromide that 89-93 ℃ of fraction obtain and imported another rectifying tower and carry out rectifying once more, return time 5-6 hour;
(4) get 89-92.5 ℃ of fraction and send into pan tank, detect qualified back be not more than under the environment purification that thousand grades, part are not more than hundred grades in integral body filter, packing, obtain satisfactory 99.99999% high-purity boron tribromide product.
The production method of above-mentioned high-purity boron tribromide, wherein: decolorizing adsorbent is a granulated active carbon.
The production method of above-mentioned high-purity boron tribromide, wherein: the material of strainer and pipeline adopts high-purity polytetrafluoroethylmaterial material; Sub-boiling distillation device, container, rectifying tower and packaging vessel adopt pure quartz glass.
The production method of above-mentioned high-purity boron tribromide, wherein: the granulated active carbon granularity is 1-3mm.The present invention compared with prior art, has tangible beneficial effect, as can be known from the above technical solutions: adopting industrial boron tribromide is raw material, add active decolorizing adsorbent decolouring, remove heavy metal ion through sub-boiling distillation again, gained distillation product distill impurity such as removing low-boiling-point substance, complex compound by rectifying tower, make product purity reach 99.99999%.And in the whole process of production, product does not contact the external world, can guarantee quality product, environment is not impacted again, safety, reliable; Each step is continuous production, compares traditional intermittent distillation efficiency and improves greatly; The clean environment that is packaged in 100 grades carries out, and guarantees that product is not contaminated; The method that adopts rectifying to combine with sub-boiling distillation can make product mention a higher purity.Make product colourity less than 40 (APHA), the resultant metal content of impurities is lower than 100PPb, and the individual event metallic impurity are no more than 10PPb.Technology of the present invention is simple, easy to operate, quality is convenient to control, low finished product cost.Product can satisfy the quality requirements of manufacturing processedes such as solar cell, semiconductor material manufacturing and unicircuit, discrete device, and the finished product price is significantly less than the price of like product.
Embodiment
Embodiment 1:
A kind of production method of high-purity boron tribromide may further comprise the steps:
(1) get technical grade boron tribromide 26KG in the 15L quartz container, adding granularity in 1% ratio is the granulated active carbon of 1-3mm, keeps filtering with expanded microporous polytetra fluoroethylene-EPTEE strainer below 0.05 micron after 60 minutes under gentle agitation;
(2) gained filtrate is regulated heating tube voltage stable liquid surface temperature 66-70 ℃ of scope through the distillation of sub-boiling distillation device;
(3) gained distillation product import the column plate type rectifying tower and carry out distillation and reflux, return time 5 hours, and the removal low-boiling-point substance is got pure product of boron tribromide that 89-93 ℃ of fraction obtain and is imported another rectifying tower and carry out rectifying once more, return time 5 hours;
(4) get 89-92.5 ℃ of fraction and send into pan tank, detect qualified back be not more than under the environment purification that thousand grades, part are not more than hundred grades in integral body filter, packing, obtain satisfactory 99.99999% high-purity boron tribromide product.
Products obtained therefrom colourity 40 (APHA), product detects wherein Al, Sb, As, Ba, Cd, Ca, Cr, Co, Cu, Au, Fe, Pb, Li, Mg, Mn, Ni, K, Sr, Ti, Zn, Hg content with ICP-MS, and the result is as follows: Fe≤9ppb, Cu≤2ppb, Cr≤1ppb, Mn≤1ppb, Zn≤5ppb, Al≤5ppb, Au≤1ppb, As≤8ppb, Ba≤1ppb, Ca≤9ppb, Co≤2ppb, Pb≤2ppb, Mg≤8ppb, Ni≤2ppb, Li≤2ppb, Cd≤2ppb, K≤3ppb, Na≤6ppb, Sr≤1ppb, Ti≤2ppb, Hg≤4ppb.The resultant metal content of impurities is lower than 100PPb, and the individual event metallic impurity are no more than 10PPb.
Embodiment 2:
A kind of production method of high-purity boron tribromide may further comprise the steps:
(1) get technical grade boron tribromide 26KG in the 15L quartz container, adding granularity in 2% ratio is the granulated active carbon of 1-3mm, keeps filtering with expanded microporous polytetra fluoroethylene-EPTEE strainer below 0.05 micron after 80 minutes under gentle agitation;
(2) gained filtrate is regulated heating tube voltage stable liquid surface temperature 60-65 ℃ of scope through special sub-boiling distillation device distillation;
(3) gained distillation product import the column plate type rectifying tower and carry out distillation and reflux, return time 6 hours, and the removal low-boiling-point substance is got pure product of boron tribromide that 89-93 ℃ of fraction obtain and is imported another rectifying tower and carry out rectifying once more, return time 6 hours;
(4) get 89-92.5 ℃ of fraction and send into pan tank, detect qualified back be not more than under the environment purification that thousand grades, part are not more than hundred grades in integral body filter, packing, obtain satisfactory 99.99999% high-purity boron tribromide product.
Products obtained therefrom colourity 36 (APHA), product detects wherein Al, Sb, As, Ba, Cd, Ca, Cr, Co, Cu, Au, Fe, Pb, Li, Mg, Mn, Ni, K, Sr, Ti, Zn content with ICP-MS, and the result is as follows: Fe≤6ppb, Cu≤2ppb, Cr≤1ppb, Mn≤1ppb, Zn≤5ppb, Al≤5ppb, Au≤1ppb, As≤7ppb, Ba≤1ppb, Ca≤8ppb, Co≤2ppb, Pb≤1ppb, Mg≤8ppb, Ni≤2ppb, Li≤2ppb, Cd≤2ppb, K≤3ppb, Na≤6ppb, Sr≤1ppb, Ti≤2ppb, Hg≤2ppb.The resultant metal content of impurities is lower than 100PPb, and the individual event metallic impurity are no more than 10PPb.
Embodiment 3:
A kind of production method of high-purity boron tribromide may further comprise the steps:
(1) get technical grade boron tribromide 26KG in the 15L quartz container, adding granularity in 1.5% ratio is the granulated active carbon of 1-3mm, keeps filtering with expanded microporous polytetra fluoroethylene-EPTEE strainer below 0.05 micron after 70 minutes under gentle agitation;
(2) gained filtrate is regulated heating tube voltage stable liquid surface temperature 70-75 ℃ of scope through special sub-boiling distillation device distillation;
(3) gained distillation product import the column plate type rectifying tower and carry out distillation and reflux, return time 6 hours, and the removal low-boiling-point substance is got pure product of boron tribromide that 89-93 ℃ of fraction obtain and is imported another rectifying tower and carry out rectifying once more, return time 6 hours;
(4) get 89-92.5 ℃ of fraction and send into pan tank, detect qualified back be not more than under the environment purification that thousand grades, part are not more than hundred grades in integral body filter, packing, obtain satisfactory 99.99999% high-purity boron tribromide product.
Products obtained therefrom colourity 37 (APHA), product detects wherein Al, Sb, As, Ba, Cd, Ca, Cr, Co, Cu, Au, Fe, Pb, Li, Mg, Mn, Ni, K, Sr, Ti, Zn content with ICP-MS, and the result is as follows: Fe≤7ppb, Cu≤2ppb, Cr≤1ppb, Mn≤1ppb, Zn≤5ppb, Al≤5ppb, Au≤1ppb, As≤9ppb, Ba≤1ppb, Ca≤8ppb, Co≤2ppb, Pb≤2ppb, Mg≤8ppb, Ni≤2ppb, Li≤2ppb, Cd≤3ppb, K≤3ppb, Na≤6ppb, Sr≤1ppb, Ti≤2ppb, Hg≤3ppb.The resultant metal content of impurities is lower than 100PPb, and the individual event metallic impurity are no more than 10PPb.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.
Claims (4)
1. the production method of a high-purity boron tribromide may further comprise the steps:
(1) gets the technical grade boron tribromide in container, add decolorizing adsorbent, under gentle agitation, keep filtering with millipore filter below 0.05 micron after 60-80 minute in the 1-2% ratio;
(2) gained filtrate is regulated heating tube voltage stable liquid surface temperature 60-75 ℃ of scope through the distillation of sub-boiling distillation device;
(3) gained distillation product import the column plate type rectifying tower and carry out distillation and reflux, and return time 5-6 hour, the removal low-boiling-point substance was got pure product of boron tribromide that 89-93 ℃ of fraction obtain and imported another rectifying tower and carry out rectifying once more, return time 5-6 hour;
(4) get 89-92.5 ℃ of fraction and send into pan tank, detect qualified back be not more than under the environment purification that thousand grades, part are not more than hundred grades in integral body filter, packing, obtain satisfactory 99.99999% high-purity boron tribromide product.
2. the production method of high-purity boron tribromide as claimed in claim 1, wherein: decolorizing adsorbent is a granulated active carbon.
3. the production method of high-purity boron tribromide of stating as claimed in claim 1 or 2, wherein: the granulated active carbon granularity is 1-3mm.
4. as the production method of high-purity boron tribromide of stating as described in the claim 3, wherein: the material of strainer and pipeline adopts high-purity polytetrafluoroethylmaterial material; Sub-boiling distillation device, container, rectifying tower and packaging vessel adopt pure quartz glass.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950947A (en) * | 2014-05-20 | 2014-07-30 | 方治文 | Preparation method of high-purity boron trichloride-11 |
| CN103950949A (en) * | 2014-05-20 | 2014-07-30 | 方治文 | Preparation method of high-purity boron tribromide-11 |
| CN106829989A (en) * | 2017-02-15 | 2017-06-13 | 江西瑞合精细化工有限公司 | The production method and device of a kind of high-purity boron tribromide |
| CN108178185A (en) * | 2018-02-07 | 2018-06-19 | 贵阳精科技有限公司 | A kind of production method of ultra-high purity titanium tetrachloride |
| CN110668456A (en) * | 2019-11-19 | 2020-01-10 | 安徽艾佩科电子材料有限公司 | Purification method and device of high-purity boron tribromide |
| CN115124048A (en) * | 2022-06-13 | 2022-09-30 | 安徽泽升科技有限公司 | Production method of high-purity boron tribromide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2989375A (en) * | 1956-12-07 | 1961-06-20 | American Potash & Chem Corp | Production of boron tribromide |
| CN101214970A (en) * | 2008-01-17 | 2008-07-09 | 核工业理化工程研究院华核新技术开发公司 | Technique and deice for preparing high purity boron trifluoride gas |
-
2010
- 2010-06-12 CN CN2010101992218A patent/CN101891218B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2989375A (en) * | 1956-12-07 | 1961-06-20 | American Potash & Chem Corp | Production of boron tribromide |
| CN101214970A (en) * | 2008-01-17 | 2008-07-09 | 核工业理化工程研究院华核新技术开发公司 | Technique and deice for preparing high purity boron trifluoride gas |
Non-Patent Citations (1)
| Title |
|---|
| 《化学试剂》 19891231 王志铿等 高纯BBr3、POCl3基体中杂质的分离和测定 第132页三、分离方法至第133页六、试样分析 1-4 第11卷, 第3期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950947A (en) * | 2014-05-20 | 2014-07-30 | 方治文 | Preparation method of high-purity boron trichloride-11 |
| CN103950949A (en) * | 2014-05-20 | 2014-07-30 | 方治文 | Preparation method of high-purity boron tribromide-11 |
| CN103950949B (en) * | 2014-05-20 | 2015-09-09 | 方治文 | The preparation method of high-purity boron tribromide-11 |
| CN106829989A (en) * | 2017-02-15 | 2017-06-13 | 江西瑞合精细化工有限公司 | The production method and device of a kind of high-purity boron tribromide |
| CN106829989B (en) * | 2017-02-15 | 2021-04-06 | 江西瑞合特种材料有限公司 | Production method and device of high-purity boron tribromide |
| CN108178185A (en) * | 2018-02-07 | 2018-06-19 | 贵阳精科技有限公司 | A kind of production method of ultra-high purity titanium tetrachloride |
| CN110668456A (en) * | 2019-11-19 | 2020-01-10 | 安徽艾佩科电子材料有限公司 | Purification method and device of high-purity boron tribromide |
| CN115124048A (en) * | 2022-06-13 | 2022-09-30 | 安徽泽升科技有限公司 | Production method of high-purity boron tribromide |
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