CN105548329A - Method for measuring separation coefficient during process of silicon isotope separation (chemical exchange method) and apparatus thereof - Google Patents
Method for measuring separation coefficient during process of silicon isotope separation (chemical exchange method) and apparatus thereof Download PDFInfo
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Abstract
The invention discloses a method for measuring the separation coefficient during the process of silicon isotope separation (chemical exchange method) and an apparatus thereof. According to the method, an alcohol complexing agent is adopted, SiF4 gas and silicon tetrafluoride alcohol complex carry out silicon isotope chemical exchange reactions, and silicon isotope separation coefficients under different pressures at different temperatures are measured. The apparatus comprises a nitrogen gas steel cylinder (1), a reaction gas SiF4 steel cylinder (2), a SiF4 buffer tank (3), a molecular sieve column (4), a chemical exchange reactor (5), a freezing/heating device (6) with stirring and temperature adjusting functions, a liquid phase sampling bottle (7), a gas phase sampling bottle (8), a buffer tank (9), and a vacuum pump (10). The apparatus has a reasonable structure, and the method and apparatus can be used to measure the separation coefficients of isotope exchange of a silicon tetrafluoride- silicon tetrafluoride complex system under different pressures at different temperatures.
Description
Technical field
The invention belongs in hyundai electronics and semi-conductor industry, the purification of isotopic pure silicon materials and production field, in particular to a kind of assay method and the device that adopts thereof of chemical exchange method divided silicon isotope process factor, under it is applicable to different pressures and temperature conditions, relate to the measurement that the silicon tetrafluoride-silicon tetrafluoride chemistry of complex exchanges separation coefficient, basic data can be provided for the design of the tripping device of chemical exchange method divided silicon isotope and industrially scalable rank.
Background technology
In hyundai electronics and semi-conductor industry, silicon materials obtain a wide range of applications, and the semiconductor components and devices more than 90% is all made up of silicon.Natural silicon contains three kinds of stable isotopes
28si,
29si,
30si, its content is respectively 92.23%, and 4.67%, 3.10%.In recent years, the silicon materials of isotopic pure start with its excellent characteristic the concern being subject to scientists.
Along with the development of modern information industry and electronic computer industry, the volume of semi-conductor chip becomes less, integration degree is higher.But semi-conductor chip volume is less, circuit integrated level is higher, and current density will increase gradually, and unit volume internal heat generation amount increases, such will make components and parts operationally temperature raise, chip temperature is too high will cause performance of semiconductor element device and life-span to be declined to a great extent.Use isotopic pure
28si(99.85%) semiconductor devices made, the comparable natural silicon of the thermal conductivity under room temperature increases by 10% ~ 60%, and what increase at some specific temperature is more.Isotopic pure
28the diode reverse breakdown voltage that Si makes can improve more than 80% than the natural silicon diode of same process.Enrichment
29si is a kind of potential material for storing and operate quantum computerized information.Contain
30the silicon ingot of Si is the new material realizing neutron transmutation doping (NDT), and NDT is a kind of technology adopting the way of neutron irradiation to adulterate to material, and its maximum advantage is exactly that the impurities concentration distribution of mixing is very even.
At present, the method realizing silicon isotope separation mainly contains cryogenic rectification method, gas centrifugation, laser method, chemical exchange method etc.Wherein, chemical exchange method, owing to having the advantages such as separation coefficient is high, treatment capacity is large, has become the method being hopeful most to realize silicon isotope industrial separation.Exchange in the design of separation industries gasifying device in silicon tetrafluoride-silicon tetrafluoride chemistry of complex, need to calculate required equilibrium stage quantity by the separation coefficient under different condition and then determine tower height and amount of filler etc.
Silicon tetrafluoride and complex compound thereof have very strong toxicity and corrosivity, and owing to having a strong impact on containing the measurement of silicon for silicon isotope in category of glass instrument, therefore traditional glass quasi-instrument is no longer applicable, and the sealing for metal device proposes very high requirement.
Summary of the invention
The present invention is directed to the existing category of glass reactor for measuring separation factor and relate to the problem be no longer suitable in silicon isotope system, and the assay method that a kind of chemical exchange method divided silicon isotope process factor is provided and the device adopted thereof, be intended to for industrialization design provides basic data.Apparatus structure of the present invention is reasonable, can be used in the separation coefficient of silicon tetrafluoride-silicon tetrafluoride complex compound (as silicon tetrafluoride methanol complex, silicon tetrafluoride ethanol complex, the silicon tetrafluoride butanol Compound etc.) isotope exchange reaction under measurement different temperatures and pressure condition.
For solving the problems of the technologies described above, the present invention realizes like this.
The assay method of chemical exchange method divided silicon isotope process factor is adopt alcohols complexing agent, by SiF
4gas and silicon tetrafluoride alcohols complex compound carry out silicon isotope chemical exchange reaction, and measure the silicon isotope separation coefficient under different temperatures and pressure, concrete steps are as follows:
(1) processed is carried out to alcohols complexing agent, make its water cut lower than 50ppm; SiF
4gas purity is higher than 99.99%; Nitrogen gas purity is higher than 99.9999%.
(2) alcohols complexing agent is joined in chemical exchange reaction still; The environment temperature of Sustainable Control chemical exchange reaction still.
(3) in chemical exchange reaction still, SiF is injected
4gas, carries out the complex reaction of silicon tetrafluoride and alcohols complexing agent; In course of reaction, progressively add SiF
4gas, when chemical exchange reaction temperature in the kettle and pressure remain unchanged, complex reaction completes.
(4) SiF
4gas and silicon tetrafluoride alcohols complex compound carry out silicon isotope chemical exchange reaction.
(5) chemical exchange reaction being reached the liquid after balance imports in liquid phase sampling jar; Chemical exchange reaction is reached the gas after balance to import in gas phase sampling jar.
(6) sample is carried out ICP-Mass and detect analysis, calculate the separation coefficient of silicon isotope.
As a kind of preferred version, in step of the present invention (3), in chemical exchange reaction still, inject the SiF of 0.1MPa pressure
4gas.
The device that the assay method of above-mentioned chemical exchange method divided silicon isotope process factor adopts, comprises nitrogen cylinder, reaction gas SiF
4steel cylinder, SiF
4buffer tank, molecular sieve column, chemical exchange reaction still, band stir freezing well heater, liquid phase sampling jar, gas phase sampling jar, surge tank and the vacuum pump with temp regulating function; The transmit port of described nitrogen cylinder is through molecular sieve column and SiF
4buffer tank communicates; Described SiF
4the transmit port of steel cylinder communicates with buffer tank; Described SiF
4the transmit port of buffer tank, liquid phase sampling jar and gas phase sampling jar communicates with chemical exchange reaction still respectively; The transmit port of described surge tank respectively with chemical exchange reaction still and SiF
4buffer tank communicates; The working port of described vacuum pump communicates with surge tank; Described chemical exchange reaction still is placed in band stirring to be had within the freezing well heater working chamber of temp regulating function.
As a kind of preferred version, the present invention is provided with anticorrosion rotor in described chemical exchange reaction still.
Further, the present invention is provided with the second tensimeter on described chemical exchange reaction still; Described second pressure gage measuring range is-0.1MPa ~ 1.6MPa.
Further, the present invention is provided with thermometer in described chemical exchange reaction still; The range of described thermometer is-50 ~ 300 DEG C; At described SiF
4buffer tank is provided with the first tensimeter; Described first pressure gage measuring range is-0.1MPa ~ 1.6MPa.
Further, buffer tank admission valve of the present invention, buffer tank outlet valve, reactor gas inlet valve, reactor complexing agent admission valve, liquid phase sample valve and gas phase sample valve are needle valve.Pipeline connects all employing metal ferrules and is connected with welding manner, and measuring system leak rate is less than
1×10
-10Pa·m
3·s
-1。
Further, in molecular sieve column of the present invention, molecular sieve deicer is housed.
Further, SiF of the present invention
4buffer tank, chemical exchange reaction still, band stir freezing well heater, liquid phase sampling jar and the gas phase sampling jar with temp regulating function and all adopt 316L stainless steel material.
Apparatus structure of the present invention is reasonable, easy to operate, good seal.Reliability is high, can be used in the separation coefficient that the silicon tetrafluoride-silicon tetrafluoride complex system isotope under measurement different temperatures, different pressures condition exchanges.In the present invention, the gas phase of exchange equilibrium and liquid phase are through sample analysis, and calculate exchange separation coefficient according to the definition of separation factor and quantitative analysis results.The present invention can be used for measuring the silicon isotope separation coefficient of the separation system that other complexing agent and silicon tetrafluoride form, and ensure that real result is reliable.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the invention will be further described.Protection scope of the present invention is not only confined to the statement of following content.
Fig. 1 is one-piece construction schematic diagram of the present invention.
In figure: 1, nitrogen cylinder; 2, reaction gas SiF
4steel cylinder; 3, SiF
4buffer tank; 4, molecular sieve column; 5, chemical exchange reaction still; 6, band stirs the freezing well heater with temp regulating function; 7, liquid phase sampling jar; 8, gas phase sampling jar; 9, surge tank; 10, vacuum pump; 11, anticorrosion rotor; 12, the first tensimeter; 13, the second tensimeter; 14, thermometer; V1, nitrogen reduction valve; V2, SiF
4gas pressure reducer; V3, the first needle valve; V4, buffer tank admission valve; V5, buffer tank outlet valve; V6, reactor gas inlet valve; V7, reactor complexing agent admission valve; V8, liquid phase sample valve; V9, gas phase sample valve; V10, surge tank admission valve; V11, surge tank outlet valve.
Embodiment
Shown in Figure 1, the assay method of chemical exchange method divided silicon isotope process factor is adopt alcohols complexing agent, by SiF
4gas and silicon tetrafluoride alcohols complex compound carry out silicon isotope chemical exchange reaction, and measure the silicon isotope separation coefficient under different temperatures and pressure, concrete steps are as follows.
(1) processed is carried out to alcohols complexing agent, make its water cut lower than 50ppm; SiF
4gas purity is higher than 99.99%; Nitrogen gas purity is higher than 99.9999%.
(2) alcohols complexing agent is joined in chemical exchange reaction still; The environment temperature of Sustainable Control chemical exchange reaction still.
(3) in chemical exchange reaction still, SiF is injected
4gas, carries out the complex reaction of silicon tetrafluoride and alcohols complexing agent; In course of reaction, progressively add SiF
4gas, when chemical exchange reaction temperature in the kettle and pressure remain unchanged, complex reaction completes.
(4) SiF
4gas and silicon tetrafluoride alcohols complex compound carry out the reaction of silicon isotope chemical exchange reaction.
(5) chemical exchange reaction being reached the liquid after balance imports in liquid phase sampling jar; Chemical exchange reaction is reached the gas after balance to import in gas phase sampling jar.
(6) sample is carried out ICP-Mass and detect analysis, calculate the separation coefficient of silicon isotope.
In step of the present invention (3), in chemical exchange reaction still, inject the SiF of 0.1MPa pressure
4gas.
The device that the assay method of above-mentioned chemical exchange method divided silicon isotope process factor adopts, comprises nitrogen cylinder 1, reaction gas SiF
4steel cylinder 2, SiF
4buffer tank 3, molecular sieve column 4, chemical exchange reaction still 5, band stir freezing well heater 6, liquid phase sampling jar 7, gas phase sampling jar 8, surge tank 9 and the vacuum pump 10 with temp regulating function; The transmit port of described nitrogen cylinder 1 is through molecular sieve column 4 and SiF
4buffer tank 3 communicates; Described SiF
4the transmit port of steel cylinder 2 communicates with buffer tank 3; Described SiF
4the transmit port of buffer tank 3, liquid phase sampling jar 7 and gas phase sampling jar 8 communicates with chemical exchange reaction still 5 respectively; The transmit port of described surge tank 9 respectively with chemical exchange reaction still 5 and SiF
4buffer tank 3 communicates; The working port of described vacuum pump 10 communicates with surge tank 9; Described chemical exchange reaction still 5 is placed in band stirring to be had within freezing well heater 6 working chamber of temp regulating function.
The present invention is provided with anticorrosion rotor 11 in described chemical exchange reaction still 5.
The present invention is provided with the second tensimeter 13 on described chemical exchange reaction still 5; Described second tensimeter 13 range is-0.1MPa ~ 1.6MPa.
The present invention is provided with thermometer 14 in described chemical exchange reaction still 5; The range of described thermometer 14 is-50 ~ 300 DEG C; At described SiF
4buffer tank 3 is provided with the first tensimeter 12; Described first tensimeter 12 range is-0.1MPa ~ 1.6MPa.
Buffer tank admission valve V4 of the present invention, buffer tank outlet valve V5, reactor gas inlet valve V6, reactor complexing agent admission valve V7, liquid phase sample valve V8 and gas phase sample valve V9 are needle valve.Pipeline connects all employing metal ferrules and is connected with welding manner, and measuring system leak rate is less than 1 × 10
-10pam
3s
-1.
In molecular sieve column 4 of the present invention, molecular sieve deicer is housed.
SiF of the present invention
4buffer tank 3, chemical exchange reaction still 5, band stir freezing well heater 6, liquid phase sampling jar 7 and the gas phase sampling jar 8 with temp regulating function and all adopt 316L stainless steel material.
The concrete assay method of the present invention is as follows.
The first step, installs.Each several part is connected by cutting ferrule or welding manner, installation.
Second step, leak test.Make each needle valve be in open-circuit condition respectively, open vacuum pump simultaneously, until meet vacuum pressure requirement.
3rd step, exhaust.Make nitrogen reduction valve V1 and SiF respectively
4gas pressure reducer V2 is in closed condition, the first needle valve V3, buffer tank admission valve V4, buffer tank outlet valve V5, reactor gas inlet valve V6, reactor complexing agent admission valve V7, liquid phase sample valve V8, gas phase sample valve V9, surge tank admission valve V10, surge tank outlet valve V11 is made to be in open mode, open vacuum pump, until the close-0.1MPa of pressure gauge reading also no longer changes simultaneously; Close surge tank outlet valve V11, close vacuum pump, open nitrogen reduction valve V1, making to be full of drying nitrogen in whole device and each pipeline, is 0.1MPa to pressure gauge reading, closes nitrogen reduction valve V1; Repeat above-mentioned two step 3 ~ 5 times, guarantee the complete emptying of air in system.Be operating as the last time and vacuumize, after end of operation, close buffer tank outlet valve V11, reactor gas inlet valve V6, reactor complexing agent admission valve V7, liquid phase sample valve V8 and gas phase sample valve V9.
4th step, adds complexing agent.Complexing agent storage tank is connected with pipeline, opens reactor complexing agent admission valve V7, by complexing agent suction chemical exchange reaction still.Chemical exchange reaction still 5 is put into band and stir the freezing well heater 6 with temp regulating function, temperature is regulated the assigned temperature be set in needed for reaction, in heating or cooling procedure, open magnetic agitation.
5th step, intake process.Surge tank admission valve V10, nitrogen reduction valve V1, the first needle-valve V3, buffer tank outlet valve V11 are closed, opens SiF
4gas pressure reducer V2 and buffer tank admission valve V10, injects reaction gas in buffer tank, when the first tensimeter 12 reading reaches required pressure, closes SiF
4gas pressure reducer V2 and buffer tank admission valve V4.Open buffer tank outlet valve V5, the SiF in buffer tank
4gas enters chemical exchange reaction still, when the second tensimeter 13 reading reaches reaction pressure, closes buffer tank outlet valve V5.
6th step, chemical exchange reaction.Under the temperature and pressure of specifying, balance until silicon tetrafluoride and its complex compound exchange reaction arrive.If when the second tensimeter 13 reading is lower than reaction pressure in course of reaction, opens buffer tank outlet valve V5, close during reaction pressure to be achieved.
7th step, liquid sampling.Slowly open liquid phase sample valve, the liquid after chemical exchange reaction reaches balance enters in liquid phase sampling jar, and in bottle to be sampled, amount of liquid reaches aequum, closes liquid phase sample valve V8.
8th step, gas sample.Slowly open gas phase sample valve V9, the gas after chemical exchange reaction reaches balance enters in gas phase sampling jar, and in bottle to be sampled, pressure reaches specified pressure, closes gas phase sample valve V9.
9th step, sample analysis, calculates separation coefficient.
Embodiment 1.
The present embodiment makes complexing agent with methyl alcohol, by SiF
4gas and silicon tetrafluoride methanol complex carry out silicon isotope chemical exchange reaction, measure the silicon isotope separation coefficient under different temperatures and pressure.
Detailed process is as follows.
1, need to carry out processed to methyl alcohol before experiment, make its water cut lower than 50ppm.The SiF4 gas purity adopted is higher than 99.99%, and nitrogen gas purity is higher than 99.9999%.
2, repeat to vacuumize to whole device and inflated with nitrogen 3 times, finally vacuumize.
3,100ml methyl alcohol is joined in chemical exchange reaction still; Band stirs to have in the freezing well heater of temp regulating function and passes into distilled water, keeps 2 DEG C, the revolution of stirring rotator is set in 50r/min.
4, in chemical exchange reaction device, the SiF of 0.1MPa pressure is injected by reactor gas inlet valve
4gas, off-response still gas inlet valve.Under the temperature and pressure set, carry out the complex reaction of silicon tetrafluoride and methyl alcohol, in course of reaction, progressively can add SiF
4gas, when question response temperature in the kettle and pressure all remain unchanged, complex reaction completes.
5, keep the reaction of temperature of reaction 2 DEG C, reaction pressure 0.1MPa, rotor revolution number 50r/min to impose a condition, carry out by SiF
4gas and silicon tetrafluoride methanol complex carry out the reaction of silicon isotope chemical exchange reaction.After reaction 1h, stop reaction.
6. slowly open liquid phase sample valve, the liquid after chemical exchange reaction reaches balance enters in liquid phase sampling jar.Slowly open gas phase sample valve, the gas after chemical exchange reaction reaches balance enters in gas phase sampling jar.Sample is carried out ICP-Mass and detect analysis.Calculate the separation coefficient of silicon isotope.
Test other temperature and pressure only reaction conditions to be adjusted.
Through reality test, device energy Measurement accuracy SiF of the present invention
4gas and silicon tetrafluoride methanol complex carry out in the reaction of silicon isotope chemical exchange reaction, and measure the silicon isotope separation coefficient under different temperatures and pressure, measurement result accurately and reliably.
Embodiment 2.
The present embodiment makes complexing agent with ethanol, by SiF
4gas and silicon tetrafluoride ethanol complex carry out the reaction of silicon isotope chemical exchange reaction, measure the silicon isotope separation coefficient under different temperatures and pressure.
Detailed process is as follows.
Need dewatering of ethanol process before experiment, make its water cut lower than 50ppm.Amount of alcohol added 100ml.Add distilled water and ice cube in freezing heating stirrer, keep 0 DEG C.
Reaction conditions keeps temperature 0 DEG C, reaction pressure 0.1MPa, rotor revolution number 50r/min.
All the other operation stepss are identical with embodiment 1.
Through reality test, device energy Measurement accuracy SiF of the present invention
4gas and silicon tetrafluoride ethanol complex carry out in the reaction of silicon isotope chemical exchange reaction, and measure the silicon isotope separation coefficient under different temperatures and pressure, measurement result accurately and reliably.
From above-mentioned example 1,2, measurement mechanism structure is simple, easy to operate, good seal and reliability high, also can be used for measuring the silicon isotope separation coefficient of the separation system that other complexing agent and silicon tetrafluoride form, and ensure that real result is reliable.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. the assay method of chemical exchange method divided silicon isotope process factor, is characterized in that, adopts alcohols complexing agent, by SiF
4gas and silicon tetrafluoride alcohols complex compound carry out silicon isotope chemical exchange reaction, and measure the silicon isotope separation coefficient under different temperatures and pressure, concrete steps are as follows:
(1) processed is carried out to alcohols complexing agent, make its water cut lower than 50ppm; SiF
4gas purity is higher than 99.99%; Nitrogen gas purity is higher than 99.9999%;
(2) alcohols complexing agent is joined in chemical exchange reaction still; The environment temperature of Sustainable Control chemical exchange reaction still;
(3) in chemical exchange reaction still, SiF is injected
4gas, carries out the complex reaction of silicon tetrafluoride and alcohols complexing agent; In course of reaction, progressively add SiF
4gas, when chemical exchange reaction temperature in the kettle and pressure remain unchanged, complex reaction completes;
(4) SiF
4gas and silicon tetrafluoride alcohols complex compound carry out silicon isotope chemical exchange reaction;
(5) chemical exchange reaction being reached the liquid after balance imports in liquid phase sampling jar; Chemical exchange reaction being reached the gas after balance imports in gas phase sampling jar;
(6) sample is carried out ICP-Mass and detect analysis, calculate the separation coefficient of silicon isotope.
2. the assay method of chemical exchange method divided silicon isotope process factor according to claim 1, is characterized in that: in described step (3), injects the SiF of 0.1MPa pressure in chemical exchange reaction still
4gas.
3. the device that adopts of the assay method of chemical exchange method divided silicon isotope process factor as claimed in claim 1 or 2, is characterized in that, comprise nitrogen cylinder (1), reaction gas SiF
4steel cylinder (2), SiF
4buffer tank (3), molecular sieve column (4), chemical exchange reaction still (5), band stir freezing well heater (6), liquid phase sampling jar (7), gas phase sampling jar (8), surge tank (9) and the vacuum pump (10) with temp regulating function; The transmit port of described nitrogen cylinder (1) is through molecular sieve column (4) and SiF
4buffer tank (3) communicates; Described SiF
4the transmit port of steel cylinder (2) communicates with buffer tank (3); Described SiF
4the transmit port of buffer tank (3), liquid phase sampling jar (7) and gas phase sampling jar (8) communicates with chemical exchange reaction still (5) respectively; The transmit port of described surge tank (9) respectively with chemical exchange reaction still (5) and SiF
4buffer tank (3) communicates; The working port of described vacuum pump (10) communicates with surge tank (9); Described chemical exchange reaction still (5) is placed in band stirring to be had within freezing well heater (6) working chamber of temp regulating function.
4. the device that adopts of the assay method of chemical exchange method divided silicon isotope process factor according to claim 3, is characterized in that: in described chemical exchange reaction still (5), be provided with anticorrosion rotor (11).
5. the device that adopts of the assay method of chemical exchange method divided silicon isotope process factor according to claim 4, is characterized in that: on described chemical exchange reaction still (5), be provided with the second tensimeter (13); Described second tensimeter (13) range is-0.1MPa ~ 1.6MPa.
6. the device that adopts of the assay method of chemical exchange method divided silicon isotope process factor according to claim 5, is characterized in that: in described chemical exchange reaction still (5), be provided with thermometer (14); The range of described thermometer (14) is-50 ~ 300 DEG C; At described SiF
4buffer tank (3) is provided with the first tensimeter (12); Described first tensimeter (12) range is-0.1MPa ~ 1.6MPa.
7. the device that adopts of the assay method of chemical exchange method divided silicon isotope process factor according to claim 6, is characterized in that: described buffer tank admission valve (V4), buffer tank outlet valve (V5), reactor gas inlet valve (V6), reactor complexing agent admission valve (V7), liquid phase sample valve (V8) and gas phase sample valve (V9) are needle valve.
8. the device that adopts of the assay method of chemical exchange method divided silicon isotope process factor according to claim 7, is characterized in that: described molecular sieve column is equipped with molecular sieve deicer in (4).
9. the device that adopts of the assay method of chemical exchange method divided silicon isotope process factor according to claim 8, is characterized in that: described SiF
4buffer tank (3), chemical exchange reaction still (5), band stir freezing well heater (6), liquid phase sampling jar (7) and the gas phase sampling jar (8) with temp regulating function and all adopt 316L stainless steel material.
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Cited By (1)
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| CN111341838A (en) * | 2020-03-09 | 2020-06-26 | 华东师范大学 | Application of silicon isotope Si-30 in semiconductor material or semiconductor device for resisting radiation of medium-high energy neutrons |
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Application publication date: 20160504 |