CN209690000U - For analyzing the preprocessing system of trace impurity in chlorosilane - Google Patents
For analyzing the preprocessing system of trace impurity in chlorosilane Download PDFInfo
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- CN209690000U CN209690000U CN201822083005.1U CN201822083005U CN209690000U CN 209690000 U CN209690000 U CN 209690000U CN 201822083005 U CN201822083005 U CN 201822083005U CN 209690000 U CN209690000 U CN 209690000U
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Abstract
Present embodiment discloses a kind of for analyzing the preprocessing system of trace impurity in chlorosilane, it include: counteracting tank, comprising: tank body and the lid being covered on tank body, tank body and lid are tightly connected, tank body offers the first opening, the second opening for holding chlorosilane sample to be processed on lid；First pipe, first pipe are tightly connected with the first opening, and the first end of first pipe passes through the first opening and is located in tank body, and first pipe is for being passed through carrier gas into counteracting tank；Second pipe, second pipe and the second opening are tightly connected, and the first end of second pipe passes through the second opening and is located in tank body, and second pipe has the carrier gas of chlorosilane for output loading；Heating device is provided with heating zone, and heating zone is for accommodating counteracting tank and heating to it.The preprocessing system avoids chlorosilane sample to be processed and is secondarily contaminated, and the chlorosilane being evaporated by the carrying of carrier gas, can reduce the time of evaporation chlorosilane, improves working efficiency.
Description
Technical field
The present embodiment belongs to technical field of polysilicon production, and in particular to a kind of for analyzing trace impurity in chlorosilane
Preprocessing system.
Background technique
Chlorosilane is a kind of intermediate product of improved Siemens production polysilicon, by containing to impurity element in chlorosilane
The detection and analysis of amount and the entire technological process of production is monitored, it is ensured that the continual and steady progress of whole flow process, to reach
Control to product quality.The analysis of impurity content belongs to trace analysis in trichlorosilane, and technical requirements are more harsh, together
When, it is highly susceptible to pollute in sampling and sample making course.Therefore, how to reduce or avoid pollution in sample handling processes,
Preferably being enriched with boron, phosphorus and metallic element becomes a problem of current research.
According to literature survey, the pre-treating method type of chlorosilane sample is more, generallys use Hydrolyze method and concentration at present
Method, Hydrolyze method take a long time in sample pretreatment process, and the corrosive gas such as hydrogen chloride can be also generated in hydrolytic process, and
The content of phosphorus in chlorosilane, boron element can not accurately be measured.Complexing agent is added in concentration method in sample solution and metal ion is raw
It is volatilized under open state at stable comple, but in sample handling processes using polytetrafluoroethylene (PTFE) pincers pot, sample pole
Vulnerable to pollution, and the method still have analysis take a long time, detection effect and the problems such as poor reproducibility.
Utility model content
The technical problem to be solved is that aiming at the above shortcomings existing in the prior art, provide one kind to be used for for the present embodiment
The preprocessing system for analyzing trace impurity in chlorosilane, avoids chlorosilane sample to be processed and is secondarily contaminated, and pass through
The chlorosilane that the carrying of carrier gas is evaporated can greatly reduce the time of evaporation chlorosilane.
Technical solution used by solution the present embodiment technical problem is to provide a kind of miscellaneous for analyzing trace in chlorosilane
The preprocessing system of matter, comprising:
Counteracting tank, comprising: tank body and the lid being covered on tank body, tank body and lid are tightly connected, and tank body is for holding
Chlorosilane sample to be processed offers the first opening, the second opening on lid；
First pipe, first pipe are tightly connected with the first opening, and the first end of first pipe passes through the first opening and position
In in tank body, first pipe is for being passed through carrier gas into counteracting tank；
Second pipe, second pipe and the second opening are tightly connected, and the first end of second pipe passes through the second opening and position
In in tank body, second pipe has the carrier gas of chlorosilane for output loading；
Heating device is provided with heating zone, and heating zone is for accommodating counteracting tank and heating to it.
Preferably, lid with the connection type of tank body be clamped, be threadedly coupled, any one in interference connection.
Preferably, the liquid level h of the first end of first pipe chlorosilane sample to be processed in tank body1, low
In the liquid level h of the first end of second pipe chlorosilane sample to be processed in tank body2。
Preferably, the preprocessing system for being used to analyze trace impurity in chlorosilane, further includes:
Carrier gas feeding mechanism, connect with first pipe, and carrier gas feeding mechanism is used to supply by first pipe into counteracting tank
Answer carrier gas.
Preferably, the first valve is provided in first pipe, the first valve is Mini-adjustable valve.
Preferably, the preprocessing system for being used to analyze trace impurity in chlorosilane, further includes:
Container is absorbed, is connect with the second end of second pipe, container is absorbed for holding and absorbs the chlorosilane in carrier gas
Absorbing liquid.
Gas in second pipe is flowed into the absorbing liquid absorbed in container.
Preferably, heating device is no hot-water heating system.
Preferably, heating device is that graphite clears up instrument.
Preferably, the material of counteracting tank is one of PFA, PTFE.
The copolymer that PTFE is polytetrafluoroethylene (PTFE), PFA is perfluoro propyl perfluoroalkyl vinyl ether and polytetrafluoroethylene (PTFE).
Preferably, the material that at least first pipe protrudes into the intracorporal tube body of tank is one of PFA, PTFE；At least
The material that two pipelines protrude into the intracorporal tube body of tank is one of PFA, PTFE.
The preprocessing system for being used to analyze trace impurity in chlorosilane in the utility model, avoids chlorine silicon to be processed
Alkane sample is secondarily contaminated, and the chlorosilane being evaporated by the carrying of carrier gas, can greatly reduce evaporation chlorosilane
Time improves working efficiency, and the utility model is easy to operate, reproducibility is preferable, it can be achieved that trace impurity is fast in chlorosilane
Speed processing is conducive to the subsequent accurate, quantitative analysis read fastly.
Detailed description of the invention
Fig. 1 is in the present embodiment 2 for analyzing the structural schematic diagram of the preprocessing system of trace impurity in chlorosilane；
Fig. 2 is in the present embodiment 2 for analyzing the top view of the preprocessing system of trace impurity in chlorosilane.
In figure: 1- counteracting tank；2- first pipe；3- second pipe；4- heating device；The heating zone 5-；6- first pipe
First end；The first end of 7- second pipe；8- carrier gas feeding mechanism；The first valve of 9-；10- threeway；11- absorbs container；12-
The second end of two pipelines；13- tank body；14- lid.
Specific embodiment
To make those skilled in the art more fully understand the technical solution of the present embodiment, with reference to the accompanying drawing and it is embodied
Mode is described in further detail the present embodiment.
The embodiment of this patent is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, and is only used for explaining this patent, and cannot be understood as a limitation of this patent.
In the description of this patent, it is to be understood that the orientation or positional relationship of instruction is side based on the figure
Position or positional relationship are merely for convenience of description this patent and simplify description, rather than the device or member of indication or suggestion meaning
Part must have a particular orientation, be constructed and operated in a specific orientation, therefore should not be understood as the limitation to this patent.
Embodiment 1
The present embodiment provides a kind of for analyzing the preprocessing system of trace impurity in chlorosilane, comprising:
Counteracting tank, comprising: tank body and the lid being covered on tank body, tank body and lid are tightly connected, and tank body is for holding
Chlorosilane sample to be processed offers the first opening, the second opening on lid；
First pipe, first pipe are tightly connected with the first opening, and the first end of first pipe passes through the first opening and position
In in tank body, first pipe is for being passed through carrier gas into counteracting tank；
Second pipe, second pipe and the second opening are tightly connected, and the first end of second pipe passes through the second opening and position
In in tank body, second pipe has the carrier gas of chlorosilane for output loading；
Heating device is provided with heating zone, and heating zone is for accommodating counteracting tank and heating to it.
The preprocessing system for being used to analyze trace impurity in chlorosilane in the present embodiment, avoids chlorosilane to be processed
Sample is secondarily contaminated, and the chlorosilane being evaporated by carryings of carrier gas, can greatly reduce evaporate chlorosilane when
Between, working efficiency is improved, the utility model is easy to operate, reproducibility is preferable, it can be achieved that trace impurity is quick in chlorosilane
Processing is conducive to the subsequent accurate, quantitative analysis read fastly.
Embodiment 2
As shown in Figure 1, 2, the present embodiment provides a kind of for analyzing the preprocessing system of trace impurity in chlorosilane, wraps
It includes:
Counteracting tank 1, comprising: tank body 13 and the lid 14 being covered on tank body 13, tank body 13 and lid 14 are tightly connected, tank
Body 13 offers the first opening, the second opening for holding chlorosilane sample to be processed on lid 14；
First pipe 2, first pipe 2 and the first opening are tightly connected, and the first end 6 of first pipe 2 passes through the first opening
And be located in tank body 13, first pipe 2 is for being passed through carrier gas into counteracting tank 1；
Second pipe 3, second pipe 3 and the second opening are tightly connected, the first end 7 of second pipe pass through the second opening and
In tank body 13, second pipe 3 has the carrier gas of chlorosilane for output loading；
Heating device 4 is provided with heating zone 5, and heating zone 5 is for accommodating counteracting tank 1 and heating to it.
It should be noted that the lid 14 in the present embodiment is to be threadedly coupled with the connection type of tank body 13.
Specifically, the first end 6 of first pipe is located at the liquid of chlorosilane sample to be processed in tank body 13 in the present embodiment
Above face, the first end 7 of second pipe is located at the ullage of chlorosilane sample to be processed in tank body 13.Pass through first pipe
2 are passed through carrier gas into tank body 13, take the carrier gas for carrying chlorosilane steam out of tank body 13 by second pipe 3.
It should be noted that the first end 6 of first pipe chlorosilane sample to be processed in tank body 13 in the present embodiment
The liquid level h of product1, the liquid level of the chlorosilane sample to be processed in tank body 13 lower than the first end 7 of second pipe
h2, the carrier gas convenient for being passed into tank body 13 takes the chlorosilane evaporated out of.
It should be noted that for analyzing the preprocessing system of trace impurity in chlorosilane in the present embodiment, further includes:
Carrier gas feeding mechanism 8 is connect with first pipe 2, and carrier gas feeding mechanism 8 is used to pass through first pipe 2 to counteracting tank 1
Interior supply carrier gas.Specifically, the carrier gas in carrier gas feeding mechanism 8 in the present embodiment is argon gas.
It should be noted that being provided with the first valve 9 in the present embodiment in first pipe 2, the first valve 9 is trace regulation
Valve.The flow of carrier gas is controlled by the first valve 9, realizes that stabilization constantly provides argon gas.
Specifically, the preprocessing system that trace impurity in chlorosilane is analyzed in the present embodiment includes: two counteracting tanks 1, point
Two first pipes 2 not connecting with two counteracting tanks 1 are connected by threeway 10, and the carrier gas in carrier gas feeding mechanism 8 passes through three
Logical 10 separately flow into two counteracting tanks 1.Two first pipes 2 share tube body between threeway 10 and carrier gas feeding mechanism 8
Part, the carrier gas come out from two counteracting tanks 1 are absorbed in container 11 by being flowed into the second pipe 3 respectively connecting respectively.
It should be noted that for analyzing the preprocessing system of trace impurity in chlorosilane in the present embodiment, further includes:
Container 11 is absorbed, is connect with the second end 12 of second pipe, container 11 is absorbed and is used to hold the chlorine absorbed in carrier gas
The absorbing liquid of silane.Gas in second pipe 3 is flowed into the absorbing liquid absorbed in container 11.Specifically, in the present embodiment
Absorption container 11 be absorb bucket, absorbing liquid is water.The mixed gas volatilized is handled by absorbing container 11, is reduced outer
The content of the gas to cause damages in row's mixed gas to human body and environment.
Preferably, heating device 4 is no hot-water heating system.
It should be noted that heating device 4 is that graphite clears up instrument in the present embodiment, the heating zone 5 that graphite clears up instrument is recessed
Slot structure, for accommodating counteracting tank 1.Specifically, the contact area of graphite resolution instrument and counteracting tank 1 in the present embodiment is big, it can
Shorten heating and be evaporated the time, improves working efficiency.
Specifically, the material of the counteracting tank 1 in the present embodiment is PFA.The impurity of counteracting tank 1 is precipitated few.
The copolymer that PTFE is polytetrafluoroethylene (PTFE), PFA is perfluoro propyl perfluoroalkyl vinyl ether and polytetrafluoroethylene (PTFE).
Preferably, the material that at least first pipe 2 protrudes into the tube body in tank body 13 is one of PFA, PTFE；Extremely
The material that few second pipe 3 protrudes into the tube body in tank body 13 is one of PFA, PTFE.Specifically, first in the present embodiment
The material of pipeline 2 is PTFE；The material of second pipe 3 is PTFE.First pipe 2, the impurity precipitation of second pipe 3 are few.
Specifically, carrying out chlorine using the above-mentioned preprocessing system for analyzing trace impurity in chlorosilane in the present embodiment
The pre-treating method of trace impurity in silane, comprising the following steps:
(1) chlorosilane to be processed of 10ml is added into the tank body 13 of counteracting tank 1, covers lid 14, is placed on heating dress
The heating zone 5 for setting 4 carries out being heated to 45 DEG C by heating zone 5, and carrier gas argon is supplied into counteracting tank 1 by carrier gas feeding mechanism 8
Gas adjusts carrier gas flux by the first valve 9, and carrier gas is flowed into the chlorosilane taken away in counteracting tank 1 and evaporated in counteracting tank 1
Gas flows out counteracting tank 1, then is flowed into the absorbing liquid absorbed in container 11, until the chlorosilane to be processed in counteracting tank 1
Evaporation is complete.
(2) after the chlorosilane evaporation completely to be processed in counteracting tank 1, lid 14 is opened, is added into tank body 13
2% mannitol solution of 0.1ml and the HF (GR) of 2ml, the heating temperature of adjustment heating device 4 are 130 DEG C, until in tank body 13
Silica dissolve and be evaporated, silica source is added in the product of the partial hydrolysis of chlorosilane into counteracting tank 1
0.5ml nitric acid (GR), sufficiently dissolves, and solution constant volume is to be measured.
Comparative experiments provides a kind of pre-treating method of trace impurity in chlorosilane, the difference with the method in the present embodiment
Are as follows:
(1) chlorosilane to be processed that 10ml is held using crucible, is heated on heating device 4, and heating device 4 adds
Hot temperature is 45 DEG C, until the chlorosilane evaporation to be processed in crucible is complete.
(2) after the chlorosilane evaporation completely to be processed in crucible, 2% mannitol solution of 0.1ml is added into crucible
With the HF (GR) of 2ml, the heating temperature for adjusting heating device 4 is 130 DEG C, until the silica in crucible is dissolved and is evaporated,
0.5ml nitric acid (GR) is added into crucible in the product of the partial hydrolysis of chlorosilane in silica source, sufficiently dissolves, molten
Liquid constant volume is to be measured.
Chlorosilane to be processed in above-mentioned method of contrast is listed in following table 1 is evaporated time used, this reality
It applies chlorosilane to be processed in the method in example and is evaporated the time used, by following table it is found that being used to divide using in the present embodiment
The preprocessing system for analysing trace impurity in chlorosilane carries out the pre-treating method of trace impurity in chlorosilane, is evaporated chlorosilane institute
Time is shorter.
Table 1
Trace in chlorosilane is carried out using the preprocessing system for analyzing trace impurity in chlorosilane in the present embodiment
After the pre-treating method processing chlorosilane of impurity, obtained solution is detected by ICP-OES, is finally obtained in chlorosilane
Boron, phosphorus impurities such as the following table 2:
Table 2
By the test result in table 2 it is found that using in the present embodiment for analyzing the preceding of trace impurity in chlorosilane
The detected value of reason system, the chlorosilane sample measured is close, and relative standard deviation is small, and recovery of standard addition is high.
The preprocessing system for being used to analyze trace impurity in chlorosilane in the present embodiment, avoids chlorosilane to be processed
Sample is secondarily contaminated, and the chlorosilane being evaporated by carryings of carrier gas, can greatly reduce evaporate chlorosilane when
Between, working efficiency is improved, the utility model is easy to operate, reproducibility is preferable, it can be achieved that trace impurity is quick in chlorosilane
Processing is conducive to the subsequent accurate, quantitative analysis read fastly.
Embodiment 3
The present embodiment provides a kind of for analyzing the preprocessing system of trace impurity in chlorosilane, is with embodiment 2
The difference of system are as follows:
The connection type of lid and tank body is clamping.
The material of counteracting tank is PTFE.
The material of first pipe in the present embodiment is PFA, and the material of second pipe is PFA.
Embodiment 4
The present embodiment provides a kind of for analyzing the preprocessing system of trace impurity in chlorosilane, is with embodiment 2
The difference of system are as follows:
The connection type of lid and tank body is interference connection.
The material that first pipe protrudes into the intracorporal tube body of tank is one of PFA；Second pipe protrudes into the intracorporal tube body of tank
Material be PFAE
It is understood that embodiment of above is merely to illustrate that the principle of the present embodiment and the exemplary reality that uses
Mode is applied, however the present embodiment is not limited thereto.For those skilled in the art, this implementation is not being departed from
In the case where the spirit and essence of example, various changes and modifications can be made therein, these variations and modifications are also considered as the present embodiment
Protection scope.
Claims (10)
1. a kind of for analyzing the preprocessing system of trace impurity in chlorosilane characterized by comprising
Counteracting tank, comprising: tank body and the lid being covered on tank body, tank body and lid are tightly connected, and tank body is for holding wait locate
The chlorosilane sample of reason offers the first opening, the second opening on lid；
First pipe, first pipe are tightly connected with the first opening, and the first end of first pipe passes through the first opening and is located at tank
In vivo, first pipe is for being passed through carrier gas into counteracting tank；
Second pipe, second pipe and the second opening are tightly connected, and the first end of second pipe passes through the second opening and is located at tank
In vivo, second pipe has the carrier gas of chlorosilane for output loading；
Heating device is provided with heating zone, and heating zone is for accommodating counteracting tank and heating to it.
2. according to claim 1 for analyzing the preprocessing system of trace impurity in chlorosilane, which is characterized in that lid
With the connection type of tank body be clamping, be threadedly coupled, interference connect in any one.
3. according to claim 1 for analyzing the preprocessing system of trace impurity in chlorosilane, which is characterized in that first
The liquid level h of the first end of pipeline chlorosilane sample to be processed in tank body1, lower than the first end distance of second pipe
The liquid level h of chlorosilane sample to be processed in tank body2。
4. it is according to any one of claims 1 to 3 for analyzing the preprocessing system of trace impurity in chlorosilane, it is special
Sign is, further includes:
Carrier gas feeding mechanism, connect with first pipe, and carrier gas feeding mechanism is used to supply load into counteracting tank by first pipe
Gas.
5. according to claim 4 for analyzing the preprocessing system of trace impurity in chlorosilane, which is characterized in that first
The first valve is provided on pipeline, the first valve is Mini-adjustable valve.
6. according to claim 1~3, for analyzing the preprocessing system of trace impurity in chlorosilane described in 5 any one,
It is characterized in that, further includes:
Container is absorbed, is connect with the second end of second pipe, container is absorbed and is used to hold the absorption for absorbing the chlorosilane in carrier gas
Liquid.
7. according to claim 1~3, for analyzing the preprocessing system of trace impurity in chlorosilane described in 5 any one,
It is characterized in that, heating device is no hot-water heating system.
8. according to claim 7 for analyzing the preprocessing system of trace impurity in chlorosilane, which is characterized in that heating
Device is that graphite clears up instrument.
9. according to claim 1~3, for analyzing the preprocessing system of trace impurity in chlorosilane described in 5 any one,
It is characterized in that, the material of counteracting tank is one of PFA, PTFE.
10. according to claim 1~3, for analyzing the preprocessing system of trace impurity in chlorosilane described in 5 any one,
It is characterized in that, it is one of PFA, PTFE that at least first pipe, which protrudes into the material of the intracorporal tube body of tank,；At least second pipe
The material for protruding into the intracorporal tube body of tank is one of PFA, PTFE.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111024483A (en) * | 2019-12-24 | 2020-04-17 | 亚洲硅业(青海)股份有限公司 | Chlorosilane pretreatment system and method for detecting impurity content in chlorosilane |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111024483A (en) * | 2019-12-24 | 2020-04-17 | 亚洲硅业(青海)股份有限公司 | Chlorosilane pretreatment system and method for detecting impurity content in chlorosilane |
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