CN102115093B - Preparation method of high-purity enriched 11B boron trifluoride gas - Google Patents
Preparation method of high-purity enriched 11B boron trifluoride gas Download PDFInfo
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- CN102115093B CN102115093B CN2011100595757A CN201110059575A CN102115093B CN 102115093 B CN102115093 B CN 102115093B CN 2011100595757 A CN2011100595757 A CN 2011100595757A CN 201110059575 A CN201110059575 A CN 201110059575A CN 102115093 B CN102115093 B CN 102115093B
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Abstract
The invention relates to a high-purity enriched 11B boron trifluoride gas and a preparation method thereof. The preparation method comprises the step of enriching the 11B in a double-tower in-series high-efficiency rectifying tower by a chemical exchange method by using a mass of 11B boron trifluoride methyl ether generated during producing the enriched 11B and taking the part of a byproduct as a raw material. The abundance of the 11B is higher than 95% (at.), and the purity is higher than 99wt%. Therefore, the 11B boron trifluoride methyl ether coordination compound is directly reacted with the sodium fluoride to obtain the 11B sodium fluoborate, so that the technical process is simple, the product purity is high, and the yield of the 11B sodium fluoborate is greatly improved. The 11B sodium fluoborate is directly heated at 600-700DEG C to be thermally decomposed so as to obtain the 11B boron trifluoride gas. The abundance of the prepared boron trifluoride gas 11B is higher than 95% (at.), and the purity is higher than 99.99vol%.
Description
Technical field
The present invention relates to technical field of semiconductor, be specifically related to a kind of high-purity enrichment
11The preparation method of B boron triflouride gas.
Background technology
Natural boron contains two kinds of isotropic substances:
10B with
11B.
10The natural abundance of B is 19.6% (at.),
11The natural abundance of B is 80.4% (at.).
11B has through neutron and gamma-ray effect.Will
11The abundance of B rises to 95% (at.), and refabrication becomes high-purity boron triflouride gas, can be used for the making of high performance solar panels; When
11When the abundance of B reaches more than 99% (at.), use this
11The B boron triflouride gas is widely used in semiconductor manufacturing industry, is used for silicon ion cloth as boron dope agent and plants, and can produce high integrated, highdensity microchip, and makes that volume is littler, performance is better.
Usually, natural boron boron trifluoride preparation has four kinds of methods, and promptly (1) is at boric anhydride (B
2O
3) and fluorite (CaF
2) mixture in add the vitriol oil; (2) hydrogen fluoride and borax reaction; (3) the direct chemical combination of boron and fluorine; (4) mixture of boron oxide and carbon heats in fluorine flux.Use these methods will obtain high-purity boron trifluoride, complex process, yield is low.
Relevant technology has the preparation method of number of patent application CN86104416 boron trifluoride; Be to adopt Sodium tetrafluoroborate (or potassium fluoborate) thermolysis under 600～700 ° of C (or 800～900 ° of C) temperature of natural boron to prepare boron trifluoride, it is characterized in that under 450～600 ° of C (or 650～800 ° of C) temperature, removing in advance silicon tetrafluoride.This method operational path is long and loaded down with trivial details, and the yield of preparation Sodium tetrafluoroborate has only about 60%.
Summary of the invention
The objective of the invention is provides a kind of high-purity enrichment to the deficiency of prior art existence and the needs of scientific technological advance
11The preparation method of B boron triflouride gas.
High-purity enrichment of the present invention's preparation
11The B boron triflouride gas, purity is higher than 99vol%,
11The abundance of B is higher than 95% (at.).
High-purity enrichment of the present invention
11The preparation method of B boron triflouride gas, carry out as follows:
(1) enrichment
11B: will
11The boron trifluoride methyl ether title complex of B abundance>=90% (at.) adds in the double-column in series high-efficient spiral-screen column; For bearing under 0.05Mpa～negative 0.1Mpa condition, heat to 80～110 ° of C in vacuum tightness, carry out rectifying; Through rectifying in 72～384 hours, in first step column overhead phegma
11The B abundance reaches when being higher than 95% (at.), and material is taken out, and obtains purity and is higher than 99wt%
11B boron trifluoride methyl ether title complex;
(2) preparation
11B Sodium tetrafluoroborate: (1) is obtained
11B abundance>=95% (at.), purity are higher than 99wt%'s
11B boron trifluoride methyl ether title complex adds to be fluoridized in the still, is stirring the NaF aqueous solution that drips mass concentration 30%, purity 99wt% under the cooling conditions, and control reaction temperature is no more than 35 ° of C, to there not being CH
3OCH
3Bubble produces, and drips to finish, and continues then to stir 30 minutes; Reaction soln is heated to 100 ° of C, carries out evaporation concentration extremely
11B Sodium tetrafluoroborate solution is saturated; With this
11B Sodium tetrafluoroborate saturated solution is cooled to be lower than 10 ° of C, obtains
11The crystallization of B Sodium tetrafluoroborate;
11The crystallization of B Sodium tetrafluoroborate just obtains after washing and drying
11In the crystallization of B Sodium tetrafluoroborate
11The B abundance is higher than 99wt% greater than 95% (at.), purity;
(3) high-purity
11B boron triflouride gas preparation: (2) are obtained
11The B abundance is higher than 99wt%'s greater than 95% (at.), purity
11The crystallization of B Sodium tetrafluoroborate adds in the vacuum reactor, after vacuum tightness reaches below the 10Pa, keeps constant temperature after being warming up to 200 ° of C, continues to vacuumize 60 minutes, makes vacuum tightness reach 0.1～1pa, heat temperature raising to 600～700 ° C,
11The B Sodium tetrafluoroborate decomposites
11The B boron triflouride gas will
11The B boron triflouride gas imports in the stainless steel gas cylinder and collects.Obtain
11The B boron triflouride gas
11The B abundance is higher than 99vol% greater than 95% (at.), purity;
Separation and concentration of the present invention
11The employed double-column in series high-efficient spiral-screen column of B boron trifluoride methyl ether title complex, 11～16 meters of tower heights, tower internal diameter 100～200mm, inner-tower filling material are the structured packing of multilayer Stainless Steel Cloth, and be as shown in Figure 1.
Compared with prior art, characteristics of the present invention and beneficial effect thereof are:
1.
11B has through neutron and gamma-ray effect, will
11The abundance of B rises to 95% (at.), and refabrication becomes high-purity boron triflouride gas, can be used for the making of high performance solar panels; When
11When the abundance of B reaches more than 99% (at.), use this
11The B boron triflouride gas is widely used in semiconductor manufacturing industry, is used for silicon ion cloth as boron dope agent and plants, and can produce high integrated, highdensity microchip, and makes that volume is littler, performance is better;
2. the raw material that uses of the present invention is the production enrichment
10What produce in the B process is a large amount of
11B boron trifluoride methyl ether title complex (
11Boron abundance>=90% (at.)), its chemical formula is BF
3O (CH
3)
2, be a kind of pure boron cpd;
Target of the present invention is preparation
11The B boron trifluoride, must be at first with
11The B enrichment is higher than 95% (at.) to its abundance.Therefore, the first step of the present invention is to use the enrichment of double-column in series high-efficient spiral-screen column
11B;
3. the present invention adopts
11Direct and the Fluorinse prepared in reaction Sodium tetrafluoroborate of B boron trifluoride methyl ether title complex, technological process is simple, and product purity is high, and the yield of Sodium tetrafluoroborate reaches more than 95%.Common way is earlier title complex to be processed boric acid through steps such as defluorinate, esterifications, and boric acid and hydrofluoric acid reaction are processed fluoroboric acid, again fluoroboric acid and yellow soda ash reaction is processed Sodium tetrafluoroborate, its objective is the removal of impurity.Operational path is long and loaded down with trivial details, and the yield of Sodium tetrafluoroborate has only about 60%;
4. the present invention is high-purity
11B boron triflouride gas preparation has more simplification, and just one with pure
11The process of B Sodium tetrafluoroborate crystallization thermal degradation.Not existing report is such, need under 450～600 ° of C (or 650～800 ° of C) temperature, remove silicon tetrafluoride in advance;
5. the present invention's preparation is high-purity
11The B boron triflouride gas,
11The abundance of B is for being higher than the making that 95% (at.) can be used for high performance solar panels; When
11When the abundance of B reaches more than 99% (at.), use this
11The semi-conductor chip that the B boron triflouride gas is produced have volume little, highly accurately, the characteristics of highly integrated, high-density, stable performance.This be the boron trifluoride made of natural boron can not than.
Description of drawings
Fig. 1 double-column in series high-efficient spiral-screen column structural representation, wherein 11 is a Tata still, and 12 is a Tata body, and 13 is a tower condensing surface, and 14 is the vacuum system interface, 15 do
11B product holding tank, 16 do
11The B outlet for product, 21 is No. two Tata stills, and 22 is No. two Tata bodies, and 23 is No. two tower condensing surfaces, and 24 do
11The B raw material drips jar, and 25 do
10The outlet of B enriched substance; Fig. 2 is embodiment's 3
11B boron trifluoride mass spectrum.
Embodiment
Below in conjunction with embodiment the present invention is elaborated, but protection scope of the present invention is not limited only to following embodiment;
The performance measurement method of products obtained therefrom is following among the embodiment:
(1) boron triflouride gas is checked via chemical industrial gas quality supervision and test center; Nitrogen+argon+oxygen total content<1.0 * 10
-6The bright institute in Dalian detected gas purity reaches 99.99vol%;
(2)
11The B abundance adopts icp ms to measure; Enrichment through 4 batches of China Atomic Energy Science Research Institute's detections
11The B Sodium tetrafluoroborate, all batches
11The abundance of B, consistent with the abundance of raw material title complex, the boron triflouride gas of preparation, as shown in Figure 2, Semiconductor Co., Ltd of the triumphant WorldCom check through Shanghai,
11The B abundance does not change.
Embodiment 1
Preparation
11(at.) is high-purity for B abundance 95%
11The B boron triflouride gas, raw materials used is the production enrichment
10Produce in the B process
11B boron trifluoride methyl ether title complex (
11B abundance>=90% (at.)), adopts chemical exchange method enrichment in the double-column in series high-efficient spiral-screen column
11B.Make
11The abundance of B reaches 95% (at.), thus
11B title complex and Sodium Fluoride direct reaction are processed
11The B Sodium tetrafluoroborate, again by
11The thermolysis of B Sodium tetrafluoroborate goes out
11The B boron triflouride gas.Prepared
11The B boron triflouride gas is through measuring
11The abundance of B is 95.5% (at.), purity 99.99vol%;
The present invention's preparation
11(at.) is high-purity for B abundance 95%
11The B boron triflouride gas, preparing method's step is following:
(1) enrichment
11The B abundance reaches 95% (at.): separation and concentration
11The B isotropic substance carries out in the double-column in series high-efficient spiral-screen column, and 10 meters of tower heights, tower internal diameter 100 mm, inner-tower filling material are the structured packing of multilayer Stainless Steel Cloth, and vacuum tightness is negative 0.05Mpa, 80 ° of C of tower still temperature; Will
11The boron trifluoride methyl ether title complex of B abundance>=90% (at.) adds in the double-column in series high-efficient spiral-screen column; Heat temperature raising under condition of negative pressure; To 80 ° of C; Three of boron is fluoridized the methyl ether title complex and is become gaseous state and rise to cat head, and after condenser condenses, being in a liquid state passes back in the tower, and the liquid of backflow and the gas of rising carry out the physical chemistry exchange.With constantly carrying out of gas-liquid exchange in the system,
11B enrichment in first step column overhead phegma,
10B enrichment in the Tata still of the second stage.After the gas-liquid exchange reaches equilibrium state in the system, in tower, drip
11B boron trifluoride methyl ether title complex raw material, extraction is rich from the Tata still of the second stage
10The material of B.Through rectifying in 72 hours, in the first step column overhead phegma
11The B abundance reaches 95 % (at.), and material is taken out, and obtains
11The B abundance is that 95 % (at.), purity are higher than 99wt%'s
11B boron trifluoride methyl ether title complex;
(2) preparation
11B Sodium tetrafluoroborate: (1) is obtained
11B abundance 95 % (at.), purity are higher than 99% boron trifluoride methyl ether title complex and add and fluoridize in the still, are stirring the cooling conditions slow NaF aqueous solution of dropping mass concentration 30wt%, purity 99wt% down, and control reaction temperature is no more than 35 ° of C.To there not being CH
3OCH
3Bubble produces, and drips to finish.After dripping end, continue to stir 30 minutes.Reaction soln is heated to 100 ° of C, carries out evaporation concentration extremely
11B Sodium tetrafluoroborate solution is saturated.With this
11B Sodium tetrafluoroborate saturated solution is cooled to be lower than 10 ° of C, obtains
11The crystallization of B Sodium tetrafluoroborate.
11The crystallization of B Sodium tetrafluoroborate just obtains purified after washing and drying
11The B Sodium tetrafluoroborate,
11B abundance 95.5% (at.), purity is higher than 99wt%;
(3) high-purity
11B boron triflouride gas preparation: (2) are obtained
11B abundance 95% (at.), purity are higher than 99wt%'s
11The crystallization of B Sodium tetrafluoroborate adds in the vacuum reactor, and reactor drum is sealedly connected on the reactive system, with vacuum pump total system is vacuumized.Vacuum tightness is warming up to 200 ° of C after reaching below the 10Pa, and constant temperature continued to find time 60 minutes, and vacuum tightness reaches 0.1pa.Heat temperature raising to 600 ° C,
11The B Sodium tetrafluoroborate decomposites
11The B boron triflouride gas.Will
11The B boron triflouride gas imports in the stainless steel gas cylinder and collects.Obtain
11In the B boron triflouride gas
11The abundance of B detects through Semiconductor Co., Ltd of triumphant WorldCom of China Atomic Energy Science Research Institute and Shanghai,
11The abundance 95.5% (at.) of B; Purity is the detection of bright institute through Dalian, reaches 99.99vol%.
Embodiment 2
Preparation
11(at.) is high-purity for B abundance 97%
11The B boron triflouride gas, raw materials used is the production enrichment
10Produce in the B process
11B boron trifluoride methyl ether title complex (
11B abundance>=90% (at.)), adopts chemical exchange method enrichment in the double-column in series high-efficient spiral-screen column
11B.Make
11The abundance of B reaches 97% (at.), thus
11B title complex and Sodium Fluoride reaction are processed
11The B Sodium tetrafluoroborate, reheat
11The B Sodium tetrafluoroborate decomposites
11The B boron triflouride gas.Prepared
11The B boron triflouride gas
11The abundance of B is 97.3% (at.), purity 99.99vol%;
Preparing method's step is following:
(1) enrichment
11The B abundance reaches 97% (at.): separation and concentration
11The B isotropic substance carries out in the double-column in series high-efficient spiral-screen column, and 13 meters of tower heights, tower internal diameter 150mm, inner-tower filling material are the structured packing of multilayer Stainless Steel Cloth, and vacuum tightness is negative 0.08Mpa, 95 ° of C of tower still temperature.Will
11The boron trifluoride methyl ether title complex of B abundance>=90% (at.) adds in the double-column in series high-efficient spiral-screen column; Heat temperature raising under condition of negative pressure; To 95 ° of C; Boron trifluoride methyl ether title complex becomes gaseous state and rises to cat head, and after condenser condenses, being in a liquid state passes back in the tower, and the liquid of backflow and the gas of rising carry out the physical chemistry exchange.With constantly carrying out of gas-liquid exchange in the system,
11B enrichment in first step column overhead phegma,
10B enrichment in the Tata still of the second stage.After the gas-liquid exchange reaches equilibrium state in the system, in tower, drip
11B boron trifluoride methyl ether title complex raw material, extraction is rich from the Tata still of the second stage
10The material of B.Through rectifying in 168 hours, in the first step column overhead phegma
11The B abundance reaches 97% (at.), and material is taken out, and obtains
11The B abundance is that 97% (at.), purity are higher than 99wt%'s
11B boron trifluoride methyl ether title complex;
(2) preparation
11B Sodium tetrafluoroborate: (1) is obtained
11B abundance 97% (at.), purity are higher than the boron trifluoride methyl ether title complex adding of 99wt% fluoridizes in the still, is stirring the NaF aqueous solution that slowly drips mass concentration 30%, purity 99wt% under the cooling conditions, and control reaction temperature is no more than 35 ° of C.To there not being CH
3OCH
3Bubble produces, and drips to finish.After dripping end, continue to stir 30 minutes.Reaction soln is heated to 100 ° of C, carries out evaporation concentration extremely
11B Sodium tetrafluoroborate solution is saturated.With this
11B Sodium tetrafluoroborate saturated solution is cooled to be lower than 10 ° of C, obtains
11The crystallization of B Sodium tetrafluoroborate.
11The crystallization of B Sodium tetrafluoroborate just obtains after washing and drying
11The B Sodium tetrafluoroborate,
11The B abundance is higher than 99wt% greater than 97% (at.), purity;
(3) high-purity
11B boron triflouride gas preparation: (2) are obtained
11B abundance 97% (at.), purity are higher than 99wt%'s
11The B Sodium tetrafluoroborate adds in the vacuum reactor, and reactor drum is sealedly connected on the reactive system, with vacuum pump total system is vacuumized.Vacuum tightness is warming up to 200 ° of C after reaching below the 10Pa, and constant temperature continued to find time 60 minutes, and vacuum tightness reaches 0.5pa.Heat temperature raising to 650 ° C,
11The B Sodium tetrafluoroborate decomposites
11The B boron triflouride gas.Will
11The B boron triflouride gas imports in the stainless steel gas cylinder and collects.Obtain
11The B boron triflouride gas
11The abundance of B detects through Semiconductor Co., Ltd of triumphant WorldCom of China Atomic Energy Science Research Institute and Shanghai, is 97.3% (at.); Purity is the detection of bright institute through Dalian, reaches 99.99vol%.
Embodiment 3
Preparation
11(at.) is high-purity for B abundance 99%
11The B boron triflouride gas, raw materials used is the production enrichment
10Produce in the B process
11B boron trifluoride methyl ether title complex (
11B abundance>=90% (at.)), adopts chemical exchange method enrichment in the double-column in series high-efficient spiral-screen column
11B.Make
11The abundance of B reaches 99% (at.), thus
11B title complex and Sodium Fluoride reaction are processed
11The B Sodium tetrafluoroborate, reheat
11The B Sodium tetrafluoroborate decomposites
11The B boron triflouride gas.Prepared
11In the B boron triflouride gas
11The abundance of B is 99.2% (at.), purity 99.99vol%;
Preparing method's step is following:
(1) enrichment
11The B abundance reaches 99% (at.), separation and concentration
11The B isotropic substance carries out in the double-column in series high-efficient spiral-screen column, and 16 meters of tower heights, tower internal diameter 200mm, inner-tower filling material are the structured packing of multilayer Stainless Steel Cloth, and vacuum tightness is negative 0.1Mpa, 110 ° of C of tower still temperature.Will
11The boron trifluoride methyl ether title complex of B abundance>=90% (at.) adds in the double-column in series high-efficient spiral-screen column; Under condition of negative pressure, heat to 110 ° of C; Boron trifluoride methyl ether title complex becomes gaseous state and rises to cat head; After condenser condenses, being in a liquid state passes back in the tower, and the liquid of backflow and the gas of rising carry out the physical chemistry exchange.With constantly carrying out of gas-liquid exchange in the system,
11B enrichment in first step column overhead phegma,
10B enrichment in the Tata still of the second stage.After the gas-liquid exchange reaches equilibrium state in the system, in tower, drip
11B boron trifluoride methyl ether title complex raw material, extraction is rich from the Tata still of the second stage
10The material of B.Through rectifying in 384 hours, in the first step column overhead phegma
11The B abundance reaches 99% (at.), and material is taken out, and obtains
11The B abundance reaches 99% (at.), purity is higher than 99wt%
11B boron trifluoride methyl ether title complex;
(2) preparation
11B Sodium tetrafluoroborate: (1) is obtained
11B abundance 99% (at.), purity are higher than the boron trifluoride methyl ether title complex adding of 99wt% fluoridizes in the still, is stirring the NaF aqueous solution that slowly drips mass concentration 30%, purity 99wt% under the cooling conditions, and control reaction temperature is no more than 35 ° of C.To there not being CH
3OCH
3Bubble produces, and drips to finish.After dripping end, continue to stir 30 minutes.Reaction soln is heated to 100 ° of C, carries out evaporation concentration extremely
11B Sodium tetrafluoroborate solution is saturated.With this
11B Sodium tetrafluoroborate saturated solution is cooled to be lower than 10 ° of C, obtains
11The crystallization of B Sodium tetrafluoroborate.
11The crystallization of B Sodium tetrafluoroborate just obtains after washing and drying
11The B Sodium tetrafluoroborate,
11The B abundance is that 99.2% (at.), purity are higher than 99wt%;
(3) high-purity
11B boron triflouride gas preparation: (2) are obtained
11B abundance 99% (at.), purity are higher than 99wt%'s
11The B Sodium tetrafluoroborate adds in the vacuum reactor, and reactor drum is sealedly connected on the reactive system, with vacuum pump total system is vacuumized.After below the 10Pa, be warming up to 200 ° of C, constant temperature continued to find time 60 minutes, and vacuum tightness reaches 1pa.Heat temperature raising to 700 ° C,
11The B Sodium tetrafluoroborate decomposites
11The B boron triflouride gas.Will
11The B boron triflouride gas imports in the stainless steel gas cylinder and collects.As shown in Figure 2, obtain
11The B boron triflouride gas
11The abundance of B detects through Semiconductor Co., Ltd of triumphant WorldCom of China Atomic Energy Science Research Institute and Shanghai, is 99.2% (at.); Purity is the detection of bright institute through Dalian, reaches 99.99vol%.
Claims (2)
1. high-purity enrichment
11The preparation method of B boron triflouride gas is characterized in that carrying out as follows:
(1) enrichment
11B: will
11The boron trifluoride methyl ether title complex of B abundance>=90% (at.) adds in the double-column in series high-efficient spiral-screen column; For bearing under 0.05MPa～negative 0.1MPa condition, heat to 80～110 ° of C in vacuum tightness, carry out rectifying; Through rectifying in 72～384 hours, in first step column overhead phegma
11The B abundance reaches when being higher than 95% (at.), and material is taken out, and obtains purity and is higher than 99wt%
11B boron trifluoride methyl ether title complex;
(2) preparation
11B Sodium tetrafluoroborate: step (1) is obtained
11B abundance>=95% (at.), purity are higher than 99wt%'s
11B boron trifluoride methyl ether title complex adds to be fluoridized in the still, is stirring the NaF aqueous solution that drips concentration 30wt%, purity 99wt% under the cooling conditions, and control reaction temperature is no more than 35 ° of C, to there not being CH
3OCH
3Bubble produces, and drips to finish, and continues then to stir 30 minutes; Reaction soln is heated to 100 ° of C, carries out evaporation concentration extremely
11B Sodium tetrafluoroborate solution is saturated; With this
11B Sodium tetrafluoroborate saturated solution is cooled to be lower than 10 ° of C, obtains
11The crystallization of B Sodium tetrafluoroborate;
11The crystallization of B Sodium tetrafluoroborate just obtains after washing and drying
11The crystallization of B Sodium tetrafluoroborate, its
11The B abundance is higher than 99wt% greater than 95% (at.), purity;
(3) high-purity
11B boron triflouride gas preparation: step (2) is obtained
11The B abundance is higher than 99wt%'s greater than 95% (at.), purity
11The crystallization of B Sodium tetrafluoroborate adds in the vacuum reactor, after vacuum tightness reaches below the 10Pa, keeps constant temperature after being warming up to 200 ° of C, continues to vacuumize 60 minutes, makes vacuum tightness reach 0.1～1Pa, heat temperature raising to 600～700 ° C,
11The B Sodium tetrafluoroborate decomposites
11The B boron triflouride gas will
11The B boron triflouride gas imports in the stainless steel gas cylinder and collects, and obtains
11The B boron triflouride gas
11The B abundance is higher than 99vol% greater than 95% (at.), purity.
2. high-purity enrichment according to claim 1
11The preparation method of B boron triflouride gas is characterized in that separation and concentration in the step (1)
11The employed double-column in series high-efficient spiral-screen column of B boron trifluoride methyl ether title complex, 11～16 meters of tower heights, tower internal diameter 100～200mm, inner-tower filling material are the structured packing of multilayer Stainless Steel Cloth.
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| KR102330961B1 (en) * | 2019-11-29 | 2021-11-25 | 주식회사 에프알디 | High purity boron trifluoride manufacturing apparatus |
| CN111282438B (en) * | 2020-04-01 | 2023-08-22 | 辽宁鸿昊化学工业股份有限公司 | High abundance 10 B isotope enrichment method |
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| CN86104416A (en) * | 1986-06-28 | 1987-11-11 | 化工部光明化工研究所 | The preparation method of boron trifluoride |
| CN1168349A (en) * | 1996-02-20 | 1997-12-24 | 日本石油化学株式会社 | Methed for separating and recovering boron trifluoride |
-
2011
- 2011-03-14 CN CN2011100595757A patent/CN102115093B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104416A (en) * | 1986-06-28 | 1987-11-11 | 化工部光明化工研究所 | The preparation method of boron trifluoride |
| CN1168349A (en) * | 1996-02-20 | 1997-12-24 | 日本石油化学株式会社 | Methed for separating and recovering boron trifluoride |
Non-Patent Citations (1)
| Title |
|---|
| Tony Masiello, et al..The analysis of combination and overtone states of 11BF3 from 1650 to 4600 cm-1.《Journal of Molecular Spectroscopy》.2007,第243卷第17页右栏第17行至第23行. * |
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