CN107675251B - A kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material - Google Patents
A kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material Download PDFInfo
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- CN107675251B CN107675251B CN201710900796.XA CN201710900796A CN107675251B CN 107675251 B CN107675251 B CN 107675251B CN 201710900796 A CN201710900796 A CN 201710900796A CN 107675251 B CN107675251 B CN 107675251B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
- C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
Abstract
A kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material, it is related to a kind of synthetic method of cadmium selenide polycrystalline material.The invention aims to solve existing cadmium selenide synthetic method there are reaction temperature height, time-consuming, and the problem that the cadmium selenide purity produced is low.Gas-phase synthesizing method: one, elemental selenium and simple substance cadmium are weighed；Two, vapor- phase synthesis: 1., reaction zone heating；2., condensing zone temperature control；3., elemental selenium gasification；4., simple substance cadmium gasification；5., vapor- phase synthesis, cadmium selenide polycrystalline deposits in solid form, and not sufficiently reactive gaseous elemental selenium flow to condensing zone with gaseous elemental cadmium and deposits, and is cooled to room temperature, and obtains cadmium selenide polycrystal powder.Advantage: reducing reaction temperature, shortens generated time.Improve cadmium selenide polycrystal powder purity, purity > 99%.Present invention is mainly used for the high-purity cadmium selenide polycrystalline of vapor- phase synthesis.
Description
Technical field
The present invention relates to a kind of synthetic methods of cadmium selenide polycrystalline material.
Background technique
Cadmium selenide is a kind of II-VI compound, is had biggish forbidden bandwidth (Eg=117eV).Selenizing Cd monocrystal is because excellent
In different, far infrared band optical property, it is non-thread to be commonly used for laser detector, various semiconductor light-emitting elements and mid and far infrared
Property optical device.High-purity cadmium selenide polycrystalline material synthesis is the basis of high-quality cadmium selenide crystal growth.Current cadmium selenide
Polycrystalline preparation method is that elemental selenium and simple substance cadmium are closed in vitreosil pipe, is warming up to 950-1000 DEG C using tube furnace,
Reaction 24-72 hours.The preparation method reaction temperature is high, the reaction time is long, reaction rate is difficult to control, and excessively high temperature makes
Reactant largely gasifies, and causes pressure is excessive to be easy to happen explosion.And the cadmium selenide fusing point generated is up to 1250 DEG C, in system
Inside existing in solid form, hampers the contact of reactant elemental selenium with simple substance cadmium, reaction is not enough, so that product
Purity, which receives, to be affected to some extent, and the polycrystalline material of acquisition is not used to crystal growth.
Summary of the invention
The invention aims to solve existing cadmium selenide synthetic method there are reaction temperature height, time-consuming, and produce
The low problem of cadmium selenide purity, and a kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material is provided.
A kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material, it is characterised in that it is completed by the following steps:
One, weigh: be (1~1.05) according to the molar ratio of Se and Cd: 1 weighs elemental selenium and simple substance cadmium；Two, gas phase is closed
At: it 1., to reaction zone vacuumizes, being evacuated to vacuum degree is (1~9) × 10-7Pa, then it is warming up to 550~600 DEG C；②,
Condensing zone is vacuumized, being evacuated to vacuum degree is (1~9) × 10-7Pa, and be 20~50 DEG C by temperature control；3., will
The weighed elemental selenium of step 1 is placed in elemental selenium gasification zone, then vacuumizes to elemental selenium gasification zone, is evacuated to vacuum
Degree is (1~9) × 10-7Pa, then 400~500 DEG C are warming up to, and gasify at being 400~500 DEG C in temperature to elemental selenium,
Obtain gaseous elemental selenium；4., the weighed simple substance cadmium of step 1 is placed in simple substance cadmium gasification zone, then simple substance cadmium gasification zone is carried out
It vacuumizes, being evacuated to vacuum degree is (1~9) × 10-7Pa, then 500~700 DEG C are warming up to, and be 500~700 DEG C in temperature
Under gasify to simple substance cadmium, obtain gaseous elemental cadmium；5., gaseous elemental selenium with gas flow be 0.04L/min~0.1L/
Min is sent into reaction zone, and gaseous elemental cadmium is sent into reaction zone with gas flow for 0.04L/min~0.1L/min, and guarantees gaseous state
Elemental selenium and gaseous elemental cadmium are sent into reaction zone simultaneously with same gas flow, gaseous elemental selenium at being 550~600 DEG C in temperature
Vapor- phase synthesis is carried out in reaction zone with gaseous elemental cadmium, reaction generates cadmium selenide polycrystalline and deposits in reaction zone in solid form,
Not sufficiently reactive gaseous elemental selenium and gaseous elemental cadmium flow to condensing zone by residual air check valve, when passing through residual air check valve
When the gas flow of not sufficiently reactive gaseous elemental selenium and gaseous elemental cadmium is 0L/min, by elemental selenium gasification zone, simple substance cadmium
Gasification zone and reaction zone are gradually cooling to room temperature, take out cadmium selenide polycrystal powder in reaction zone；And during vapor- phase synthesis, simple substance
Selenium gasification zone, simple substance cadmium gasification zone, reaction zone and condensing zone pressure < 0.5MPa；The purity > of the cadmium selenide polycrystal powder
99%.
The invention has the advantages that the present invention is respectively placed in two different warm areas from simple substance cadmium using elemental selenium in gas-phase synthesizing method
Gasify, stable gasification rate is obtained by adjusting thermal field, so that gaseous elemental selenium and gaseous elemental cadmium are in third warm area
The cadmium selenide polycrystalline of haptoreaction, vapor- phase synthesis is deposited in the form of solid, unreacted gaseous elemental selenium and gaseous elemental cadmium
Then continue flow forward to recycle to four-temperature region is cooling, whole system controls material gasification rate and unreacted by adjusting temperature
Gas condensing rate, guarantee elemental selenium gasification zone, simple substance cadmium gasification zone, reaction zone and condensing zone pressure < 0.5MPa, peace
Overall coefficient greatly improves.And the contact of gaseous elemental greatly reduces reaction temperature, and whole system temperature is no more than 800
DEG C, and the time-consuming of vapor- phase synthesis greatly reduces.The cadmium selenide polycrystalline of synthesis is deposited on third warm area, and unreacted simple substance flows to
Four-temperature region recycling, so the purity superelevation significantly of the cadmium selenide polycrystal powder obtained, the purity > of cadmium selenide polycrystal powder
99%.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of cadmium selenide polycrystalline apparatus for gas-phase synthesis described in specific embodiment party eight；1 indicates simple substance in figure
Selenium gasification installation, 2 indicate simple substance cadmium gasification installation, and 3 indicate gas phase haptoreaction device, and 4 indicate gas condensing unit, and 5 indicate
Remote controllers, 6 indicate elemental selenium control valve, and 7 indicate simple substance cadmium control valve, and 8 indicate residual air check valve, and 9 indicate elemental selenium gas
Flowmeter body, 10 indicate simple substance cadmium gas flowmeter, and 11 indicate residual air gas flowmeter.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material, it is
It completes according to the following steps:
One, weigh: be (1~1.05) according to the molar ratio of Se and Cd: 1 weighs elemental selenium and simple substance cadmium；Two, gas phase is closed
At: it 1., to reaction zone vacuumizes, being evacuated to vacuum degree is (1~9) × 10-7Pa, then it is warming up to 550~600 DEG C；②,
Condensing zone is vacuumized, being evacuated to vacuum degree is (1~9) × 10-7Pa, and be 20~50 DEG C by temperature control；3., will
The weighed elemental selenium of step 1 is placed in elemental selenium gasification zone, then vacuumizes to elemental selenium gasification zone, is evacuated to vacuum
Degree is (1~9) × 10-7Pa, then 400~500 DEG C are warming up to, and gasify at being 400~500 DEG C in temperature to elemental selenium,
Obtain gaseous elemental selenium；4., the weighed simple substance cadmium of step 1 is placed in simple substance cadmium gasification zone, then simple substance cadmium gasification zone is carried out
It vacuumizes, being evacuated to vacuum degree is (1~9) × 10-7Pa, then 500~700 DEG C are warming up to, and be 500~700 DEG C in temperature
Under gasify to simple substance cadmium, obtain gaseous elemental cadmium；5., gaseous elemental selenium with gas flow be 0.04L/min~0.1L/
Min is sent into reaction zone, and gaseous elemental cadmium is sent into reaction zone with gas flow for 0.04L/min~0.1L/min, and guarantees gaseous state
Elemental selenium and gaseous elemental cadmium are sent into reaction zone simultaneously with same gas flow, gaseous elemental selenium at being 550~600 DEG C in temperature
Vapor- phase synthesis is carried out in reaction zone with gaseous elemental cadmium, reaction generates cadmium selenide polycrystalline and deposits in reaction zone in solid form,
Not sufficiently reactive gaseous elemental selenium and gaseous elemental cadmium flow to condensing zone by residual air check valve, when passing through residual air check valve
When the gas flow of not sufficiently reactive gaseous elemental selenium and gaseous elemental cadmium is 0L/min, by elemental selenium gasification zone, simple substance cadmium
Gasification zone and reaction zone are gradually cooling to room temperature, take out cadmium selenide polycrystal powder in reaction zone；And during vapor- phase synthesis, simple substance
Selenium gasification zone, simple substance cadmium gasification zone, reaction zone and condensing zone pressure < 0.5MPa；The purity > of the cadmium selenide polycrystal powder
99%.
Present embodiment is respectively placed in two different warm areas from simple substance cadmium using elemental selenium in gas-phase synthesizing method and carries out gas
Change, stable gasification rate is obtained by adjusting thermal field, so that gaseous elemental selenium contacts instead with gaseous elemental cadmium in third warm area
It answers, the cadmium selenide polycrystalline of vapor- phase synthesis is deposited in the form of solid, and unreacted gaseous elemental selenium and gaseous elemental cadmium then continue
Flow forward is recycled to four-temperature region is cooling, and whole system controls material gasification rate and unreacted gas by adjusting temperature
Condensing rate, guarantee elemental selenium gasification zone, simple substance cadmium gasification zone, reaction zone and condensing zone pressure < 0.5MPa, safety coefficient
It greatly improves.And the contact of gaseous elemental greatly reduces reaction temperature, and whole system temperature is no more than 800 DEG C, and gas
The time-consuming being combined to greatly reduces.The cadmium selenide polycrystalline of synthesis is deposited on third warm area, and unreacted simple substance flows to the 4th temperature
Area's recycling, so the cadmium selenide polycrystal powder superelevation significantly obtained, the purity > 99% of cadmium selenide polycrystal powder.
Specific embodiment 2: the difference of present embodiment and specific embodiment one is: list described in step 1
Matter selenium is 6N selenium, and simple substance cadmium described in step 1 is 7N cadmium.Other are same as the specific embodiment one.
Specific embodiment 3: present embodiment and the difference of one of specific embodiment one or two are: step 2 is 3.
In with heating rate be 100 DEG C/h by the temperature of elemental selenium gasification zone from room temperature to 400~500 DEG C.Other and specific reality
It is identical to apply mode one or two.
Specific embodiment 4: the difference of present embodiment and one of specific embodiment one to three is: step 2 is 4.
In with heating rate be 100 DEG C/h by the temperature of simple substance cadmium gasification zone from room temperature to 500~700 DEG C.Other and specific reality
It is identical to apply mode one to three.
Specific embodiment 5: the difference of present embodiment and one of specific embodiment one to four is: step 2 is 4.
In with heating rate be 200 DEG C/h by the temperature of simple substance cadmium gasification zone from room temperature to 550~600 DEG C.Other and specific reality
It is identical to apply mode one to four.
Specific embodiment 6: the difference of present embodiment and one of specific embodiment one to five is: step 2 is 5.
In with rate of temperature fall be 20 DEG C/h~50 DEG C/h elemental selenium gasification zone, simple substance cadmium gasification zone and reaction zone are gradually cooling to room
Temperature.Other are identical as specific embodiment one to five.
Specific embodiment 7: the difference of present embodiment and one of specific embodiment one to six is: step 2 is 5.
During middle vapor- phase synthesis, pressure < 0.3MPa in elemental selenium gasification zone, the pressure < 0.3MPa in simple substance cadmium gasification zone.Its
He is identical as specific embodiment one to six.
Specific embodiment 8: the difference of present embodiment and one of specific embodiment one to seven is in conjunction with Fig. 1:
The vapor- phase synthesis of elemental selenium and simple substance cadmium, the cadmium selenide polycrystalline are carried out in step 2 using cadmium selenide polycrystalline apparatus for gas-phase synthesis
Apparatus for gas-phase synthesis is by elemental selenium gasification installation 1, simple substance cadmium gasification installation 2, gas phase haptoreaction device 3, gas condensing unit 4
It is formed with remote controllers 5, elemental selenium gasification installation 1 and the setting of simple substance cadmium gasification installation 2 are same in gas phase haptoreaction device 3
Side, gas condensing unit 4 are arranged relative to elemental selenium gasification installation 1 and simple substance cadmium gasification installation 2 in gas phase haptoreaction device 3
Opposite side, elemental selenium gasification installation 1 is connected to gas phase haptoreaction device 3, and elemental selenium control valve 6 is arranged on connecting pipe
With elemental selenium gas flowmeter 9；Simple substance cadmium gasification installation 2 is connected to gas phase haptoreaction device 3, and is arranged on connecting pipe
Simple substance cadmium control valve 7 and simple substance cadmium gas flowmeter 10；Gas condensing unit 4 is connected to gas phase haptoreaction device 3, and even
It threads a pipe upper setting residual air check valve 8 and residual air gas flowmeter 11, passes through remote controllers 5 and elemental selenium gasification is monitored and controlled
Device 1, simple substance cadmium gasification installation 2, gas phase haptoreaction device 3 and gas condensing unit 4 temperature and pressure, by remotely controlling
Device 5 processed controls elemental selenium control valve 6, simple substance cadmium control valve 7 and residual air check valve 8 and switchs, and monitors simple substance by remote controllers 5
Selenium gas flowmeter 9, simple substance cadmium gas flowmeter 10 and residual air gas flowmeter 11；
Detailed process is as follows:
A, gas phase haptoreaction device 3 is vacuumized using three stages pump, is first vacuumized, is vacuumized using mechanical pump
It is 1Pa~10Pa to vacuum degree, then is vacuumized using adsorption pump, being evacuated to vacuum degree is (1~5) × 10-4Pa is finally used
Ionic pump vacuumizes, and being evacuated to vacuum degree is (1~9) × 10-7Pa, then with heating rate be 200 DEG C/h be warming up to 550~
600℃；
B, gas condensing unit 4 is vacuumized using three stages pump, is first vacuumized using mechanical pump, is evacuated to true
Reciprocal of duty cycle is 1Pa~10Pa, then is vacuumized using adsorption pump, and being evacuated to vacuum degree is (1~5) × 10-4Pa finally uses ion
Pumping vacuum, being evacuated to vacuum degree is (1~9) × 10-7Pa, and be 20~50 DEG C by the control of the temperature of gas condensing unit 4；
C, the weighed elemental selenium of step 1 is placed in elemental selenium gasification installation 1, is then pumped using three stages to list
Matter selenium gasification installation 1 is vacuumized, and is first vacuumized using mechanical pump, and being evacuated to vacuum degree is 1Pa~10Pa, then using suction
Attached pumping vacuum, being evacuated to vacuum degree is (1~5) × 10-4Pa is finally vacuumized using ionic pump, and vacuum degree is evacuated to
For (1~9) × 10-7Pa is opened elemental selenium control valve 6, then is heated up with heating rate for 100 DEG C/h, by remotely controlling
Device 5 detects elemental selenium gas flowmeter 9, when the gas flow of elemental selenium gas flowmeter 9 reaches 0.04L/min~0.1L/min
When, stop heating, guarantees that gaseous elemental selenium enters gas phase haptoreaction device with gas flow for 0.04L/min~0.1L/min
3；
D, the weighed simple substance cadmium of step 1 is placed in simple substance cadmium gasification installation 2, is then pumped using three stages to simple substance cadmium
Gasification installation 2 is vacuumized, and is first vacuumized using mechanical pump, and being evacuated to vacuum degree is 1Pa~10Pa, then uses adsorption pump
It vacuumizes, being evacuated to vacuum degree is (1~5) × 10-4Pa is finally vacuumized using ionic pump, and being evacuated to vacuum degree is (1
~9) × 10-7Pa is opened simple substance cadmium control valve 7, then is heated up with heating rate for 100 DEG C/h, is examined by remote controllers 5
Simple substance cadmium gas flowmeter 9 is surveyed to stop when the gas flow of simple substance cadmium gas flowmeter 9 reaches 0.04L/min~0.1L/min
It only heats up, guarantees that gaseous elemental cadmium enters gas phase haptoreaction device 3 with gas flow for 0.04L/min~0.1L/min；And
Elemental selenium control valve 6 is opened simultaneously with simple substance cadmium control valve 7, and elemental selenium gasification installation 1 and simple substance cadmium gasification installation 2 are simultaneously to rise
Warm rate is that 100 DEG C/h heats up；
E, gaseous elemental selenium is sent into gas phase haptoreaction device 3, gaseous state with gas flow for 0.04L/min~0.1L/min
Simple substance cadmium with gas flow be 0.04L/min~0.1L/min be sent into gas phase haptoreaction device 3, and guarantee gaseous elemental selenium with
Gaseous elemental cadmium is sent into gas phase haptoreaction device 3 with same gas flow, gaseous elemental selenium at being 550~600 DEG C in temperature
Vapor- phase synthesis is carried out in gas phase haptoreaction device 3 with gaseous elemental cadmium, reaction generates cadmium selenide polycrystalline in solid form in gas
The interior deposition of the reaction unit 3 that is in contact, not sufficiently reactive gaseous elemental selenium and gaseous elemental cadmium flow to gas by residual air check valve 8
Body condensing unit 4, when the gas flow that residual air gas flowmeter 11 is shown is 0L/min, with rate of temperature fall for 20 DEG C/h~50
DEG C/elemental selenium gasification installation 1, the gentle reaction unit 3 that is in contact of simple substance cadmium gasification installation 2 be gradually cooling to room temperature by h, in gas phase
Cadmium selenide polycrystal powder is taken out in haptoreaction device 3；Pressure < during vapor- phase synthesis, in elemental selenium gasification installation 1
0.3MPa, the pressure < 0.3MPa in simple substance cadmium gasification installation 2.
Other are identical as specific embodiment one to seven.
The gas phase transmission pipeline of present embodiment answers long enough, prevents it from connecting different warm areas and generating excessive heat and answer
Power causes pipeline damaged；The purpose of one-way cock setting guarantees that two kinds of gases only react in gas phase haptoreaction region, prevents
Only a kind of gas is excessive and flow back to the gasification zone haptoreaction of another simple substance；One-way cock pressure, the bigger gas phase of pressure
Haptoreaction is more abundant, and material utilization is higher, but the following system pressure, temperature can all increase.
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific embodiments
The purpose of invention also may be implemented in contract sample.
Using following verification experimental verifications effect of the present invention
Embodiment 1: a kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material is filled using cadmium selenide polycrystalline vapor- phase synthesis
The vapor- phase synthesis for carrying out elemental selenium and simple substance cadmium is set, the cadmium selenide polycrystalline apparatus for gas-phase synthesis is by elemental selenium gasification installation 1, list
Matter cadmium gasification installation 2, gas phase haptoreaction device 3, gas condensing unit 4 and remote controllers 5 form, elemental selenium gasification installation
1 and the setting of simple substance cadmium gasification installation 2 in 3 the same side of gas phase haptoreaction device, gas condensing unit 4 gasifies relative to elemental selenium
The opposite side of gas phase haptoreaction device 3 is arranged in device 1 and simple substance cadmium gasification installation 2, and elemental selenium gasification installation 1 is contacted with gas phase
Reaction unit 3 is connected to, and elemental selenium control valve 6 and elemental selenium gas flowmeter 9 are arranged on connecting pipe；Simple substance cadmium gasification dress
It sets 2 to be connected to gas phase haptoreaction device 3, and simple substance cadmium control valve 7 and simple substance cadmium gas flowmeter is set on connecting pipe
10；Gas condensing unit 4 is connected to gas phase haptoreaction device 3, and residual air check valve 8 and residual air gas are arranged on connecting pipe
Flowmeter body 11 is monitored and controlled elemental selenium gasification installation 1, simple substance cadmium gasification installation 2, gas phase by remote controllers 5 and contacts
The temperature and pressure of reaction unit 3 and gas condensing unit 4 controls elemental selenium control valve 6, simple substance cadmium by remote controllers 5
Control valve 7 and residual air check valve 8 switch, and monitor elemental selenium gas flowmeter 9, simple substance cadmium gas flow by remote controllers 5
Meter 10 and residual air gas flowmeter 11；It is specifically realized by the following steps:
One, it weighs: weighing 100.2g elemental selenium and 140.7g simple substance cadmium；
Two, gas phase haptoreaction device 3 is vacuumized using three stages pump, being evacuated to vacuum degree is 2.5Pa, then
It is vacuumized using adsorption pump, being evacuated to vacuum degree is 2 × 10-4Pa is finally vacuumized using ionic pump, and vacuum degree is evacuated to
It is 5.6 × 10-7Pa, then 600 DEG C are warming up to heating rate for 200 DEG C/h；
Three, gas condensing unit 4 is vacuumized using three stages pump, being evacuated to vacuum degree is 2.5Pa, then is used
Adsorption pump vacuumizes, and being evacuated to vacuum degree is 2 × 10-4Pa is finally vacuumized using ionic pump, is evacuated to vacuum degree and is
4.7×10-7Pa, and be 50 DEG C by the control of the temperature of gas condensing unit 4；
Four, 100.2g elemental selenium is placed in elemental selenium gasification installation 1, is then pumped using three stages to elemental selenium gas
Makeup is set 1 and is vacuumized, and is first vacuumized using mechanical pump, and being evacuated to vacuum degree is 2.5Pa, then true using absorption pumping
Sky, being evacuated to vacuum degree is 2 × 10-4Pa is finally vacuumized using ionic pump, and being evacuated to vacuum degree is 2.5 × 10-7Pa,
Elemental selenium control valve 6 is opened, then is heated up with heating rate for 100 DEG C/h, passes through remote controllers 5 and detects elemental selenium gas
Flowmeter 9 stops heating when the gas flow of elemental selenium gas flowmeter 9 reaches 0.08L/min, guarantees gaseous elemental selenium
It is that 0.08L/min enters gas phase haptoreaction device 3 with gas flow；The temperature of elemental selenium gasification installation 1 is 455 DEG C；
Five, 140.7g simple substance cadmium is placed in simple substance cadmium gasification installation 2, is then gasified using three stages pump to simple substance cadmium and is filled
It sets 2 to be vacuumized, first be vacuumized using mechanical pump, being evacuated to vacuum degree is 3Pa, then is vacuumized using adsorption pump, is taken out true
Sky to vacuum degree is 2.8 × 10-4Pa is finally vacuumized using ionic pump, and being evacuated to vacuum degree is 2.5 × 10-7Pa is opened
Simple substance cadmium control valve 7, then heated up with heating rate for 100 DEG C/h, pass through remote controllers 5 and detects simple substance cadmium gas flow
Meter 9 stops heating when the gas flow of simple substance cadmium gas flowmeter 9 reaches 0.08L/min, guarantees gaseous elemental cadmium with gas
Body flow is that 0.08L/min enters gas phase haptoreaction device 3；The temperature of simple substance cadmium gasification installation 2 is 620 DEG C；And elemental selenium
Control valve 6 is opened simultaneously with simple substance cadmium control valve 7, and elemental selenium gasification installation 1 and simple substance cadmium gasification installation 2 are simultaneously with heating rate
It heats up for 100 DEG C/h；
Six, gaseous elemental selenium with gas flow be 0.08L/min be sent into gas phase haptoreaction device 3, gaseous elemental cadmium with
Gas flow is that 0.08L/min is sent into gas phase haptoreaction device 3, gaseous elemental selenium and gaseous elemental at being 600 DEG C in temperature
Cadmium carries out vapor- phase synthesis in gas phase haptoreaction device 3, and reaction generates cadmium selenide polycrystalline in solid form in gas phase haptoreaction
Deposition, not sufficiently reactive gaseous elemental selenium and gaseous elemental cadmium flow to gas condensing unit by residual air check valve 8 in device 3
4,11h is reacted, the gas flow that residual air gas flowmeter 11 is shown at this time is 0L/min, is 30 DEG C/h by simple substance with rate of temperature fall
The gentle reaction unit 3 that is in contact of selenium gasification installation 1, simple substance cadmium gasification installation 2 is gradually cooling to room temperature, fills in gas phase haptoreaction
Set taking-up cadmium selenide polycrystal powder in 3；During vapor- phase synthesis, pressure in elemental selenium gasification installation 1 be 0.04MPa~
0.05MPa, pressure 0.04MPa~0.05MPa in simple substance cadmium gasification installation 2, the pressure in gas phase haptoreaction device 3 are
0.11MPa~0.15MPa, the pressure in gas condensing unit 4 are 100Pa~1000Pa.
The present embodiment elemental selenium described in step 1 is 6N selenium, and simple substance cadmium described in step 1 is 7N cadmium.
The present embodiment elemental selenium gasification installation 1, simple substance cadmium gasification installation 2, gas phase haptoreaction device 3 and gas condensation dress
Set 4 usesQuartz ampoule be made, connecting pipe byQuartz ampoule be made.
The quality that the present embodiment takes out cadmium selenide polycrystal powder in gas phase haptoreaction device 3 is 238.1g.It is examined through ICP
Checking the mark and analysing the purity of cadmium selenide polycrystal powder obtained is 99.9999%, and Se and Cd molar ratio is in cadmium selenide polycrystal powder
1.007:1。
Embodiment 2: a kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material is filled using cadmium selenide polycrystalline vapor- phase synthesis
The vapor- phase synthesis for carrying out elemental selenium and simple substance cadmium is set, the cadmium selenide polycrystalline apparatus for gas-phase synthesis is by elemental selenium gasification installation 1, list
Matter cadmium gasification installation 2, gas phase haptoreaction device 3, gas condensing unit 4 and remote controllers 5 form, elemental selenium gasification installation
1 and the setting of simple substance cadmium gasification installation 2 in 3 the same side of gas phase haptoreaction device, gas condensing unit 4 gasifies relative to elemental selenium
The opposite side of gas phase haptoreaction device 3 is arranged in device 1 and simple substance cadmium gasification installation 2, and elemental selenium gasification installation 1 is contacted with gas phase
Reaction unit 3 is connected to, and elemental selenium control valve 6 and elemental selenium gas flowmeter 9 are arranged on connecting pipe；Simple substance cadmium gasification dress
It sets 2 to be connected to gas phase haptoreaction device 3, and simple substance cadmium control valve 7 and simple substance cadmium gas flowmeter is set on connecting pipe
10；Gas condensing unit 4 is connected to gas phase haptoreaction device 3, and residual air check valve 8 and residual air gas are arranged on connecting pipe
Flowmeter body 11 is monitored and controlled elemental selenium gasification installation 1, simple substance cadmium gasification installation 2, gas phase by remote controllers 5 and contacts
The temperature and pressure of reaction unit 3 and gas condensing unit 4 controls elemental selenium control valve 6, simple substance cadmium by remote controllers 5
Control valve 7 and residual air check valve 8 switch, and monitor elemental selenium gas flowmeter 9, simple substance cadmium gas flow by remote controllers 5
Meter 10 and residual air gas flowmeter 11；It is specifically realized by the following steps:
One, it weighs: weighing 40.0g elemental selenium and 55.2g simple substance cadmium；
Two, gas phase haptoreaction device 3 is vacuumized using three stages pump, is first vacuumized using mechanical pump, taken out true
Sky to vacuum degree is 1.5Pa, then vacuumizes using adsorption pump that being evacuated to vacuum degree is 2.5 × 10-4Pa finally uses ion
Pumping vacuum, being evacuated to vacuum degree is 8.1 × 10-7Pa, then 550 DEG C are warming up to heating rate for 200 DEG C/h；
Three, gas condensing unit 4 is vacuumized using three stages pump, is first vacuumized, is evacuated to using mechanical pump
Vacuum degree is 1.5Pa, then vacuumizes using adsorption pump that being evacuated to vacuum degree is 2.5 × 10-4Pa finally uses ion pumping
Vacuum, being evacuated to vacuum degree is 7.9 × 10-7Pa, and be 30 DEG C by the control of the temperature of gas condensing unit 4；
Four, 40.0g elemental selenium is placed in elemental selenium gasification installation 1, is then pumped using three stages to elemental selenium gas
Makeup is set 1 and is vacuumized, and is first vacuumized using mechanical pump, and being evacuated to vacuum degree is 1.5Pa, then true using absorption pumping
Sky, being evacuated to vacuum degree is 2.5 × 10-4Pa is finally vacuumized using ionic pump, and being evacuated to vacuum degree is 1.3 × 10- 7Pa is opened elemental selenium control valve 6, then is heated up with heating rate for 100 DEG C/h, is passed through remote controllers 5 and is detected elemental selenium
Gas flowmeter 9 stops heating when the gas flow of elemental selenium gas flowmeter 9 reaches 0.04L/min, guarantees gaseous state list
Matter selenium is that 0.04L/min enters gas phase haptoreaction device 3 with gas flow；The temperature of elemental selenium gasification installation 1 is 415 DEG C；
Five, 55.2g simple substance cadmium is placed in simple substance cadmium gasification installation 2, is then gasified using three stages pump to simple substance cadmium and is filled
It sets 2 to be vacuumized, first be vacuumized using mechanical pump, being evacuated to vacuum degree is 3.5Pa, then is vacuumized using adsorption pump, is taken out
Vacuum to vacuum degree is 3 × 10-4Pa is finally vacuumized using ionic pump, and being evacuated to vacuum degree is 1.3 × 10-7Pa is opened
Simple substance cadmium control valve 7, then heated up with heating rate for 100 DEG C/h, pass through remote controllers 5 and detects simple substance cadmium gas flow
Meter 9 stops heating when the gas flow of simple substance cadmium gas flowmeter 9 reaches 0.04L/min, guarantees gaseous elemental cadmium with gas
Body flow is that 0.04L/min enters gas phase haptoreaction device 3；The temperature of simple substance cadmium gasification installation 2 is 534 DEG C；And elemental selenium
Control valve 6 is opened simultaneously with simple substance cadmium control valve 7, and elemental selenium gasification installation 1 and simple substance cadmium gasification installation 2 are simultaneously with heating rate
It heats up for 100 DEG C/h；
Six, gaseous elemental selenium with gas flow be 0.04L/min be sent into gas phase haptoreaction device 3, gaseous elemental cadmium with
Gas flow is that 0.04L/min is sent into gas phase haptoreaction device 3, gaseous elemental selenium and gaseous elemental at being 550 DEG C in temperature
Cadmium carries out vapor- phase synthesis in gas phase haptoreaction device 3, and reaction generates cadmium selenide polycrystalline in solid form in gas phase haptoreaction
Deposition, not sufficiently reactive gaseous elemental selenium and gaseous elemental cadmium flow to gas condensing unit by residual air check valve 8 in device 3
4,5h is reacted, the gas flow that residual air gas flowmeter 11 is shown at this time is 0L/min, is 30 DEG C/h by simple substance with rate of temperature fall
The gentle reaction unit 3 that is in contact of selenium gasification installation 1, simple substance cadmium gasification installation 2 is gradually cooling to room temperature, fills in gas phase haptoreaction
Set taking-up cadmium selenide polycrystal powder in 3；During vapor- phase synthesis, pressure in elemental selenium gasification installation 1 be 0.06MPa~
0.09MPa, pressure 0.07MPa~0.08MPa in simple substance cadmium gasification installation 2, the pressure in gas phase haptoreaction device 3 are
0.12MPa~0.15MPa, the pressure in gas condensing unit 4 are 100Pa~2000Pa.
The present embodiment elemental selenium described in step 1 is 6N selenium, and simple substance cadmium described in step 1 is 7N cadmium.
The present embodiment elemental selenium gasification installation 1, simple substance cadmium gasification installation 2, gas phase haptoreaction device 3 and gas condensation dress
Set 4 usesQuartz ampoule be made, connecting pipe byQuartz ampoule be made.
The quality that the present embodiment takes out cadmium selenide polycrystal powder in gas phase haptoreaction device 3 is 90.8g.It is examined through ICP
Checking the mark and analysing the purity of cadmium selenide polycrystal powder obtained is 99.9999%, and Se and Cd molar ratio is in cadmium selenide polycrystal powder
1.005:1。
Claims (2)
1. a kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material, it is characterised in that it is completed by the following steps:
One, weigh: be (1~1.05) according to the molar ratio of Se and Cd: 1 weighs elemental selenium and simple substance cadmium；
Two, the vapor- phase synthesis of elemental selenium and simple substance cadmium, the selenium vapor- phase synthesis: are carried out using cadmium selenide polycrystalline apparatus for gas-phase synthesis
Cadmium polycrystalline apparatus for gas-phase synthesis is by elemental selenium gasification installation (1), simple substance cadmium gasification installation (2), gas phase haptoreaction device
(3), gas condensing unit (4) and remote controllers (5) composition, elemental selenium gasification installation (1) and simple substance cadmium gasification installation (2) are set
It sets in gas phase haptoreaction device (3) the same side, gas condensing unit (4) is relative to elemental selenium gasification installation (1) and simple substance cadmium
Gasification installation (2) setting is filled in the opposite side of gas phase haptoreaction device (3), elemental selenium gasification installation (1) and gas phase haptoreaction
(3) connection is set, and elemental selenium control valve (6) and elemental selenium gas flowmeter (9) are set on connecting pipe；Simple substance cadmium gasification dress
It sets (2) to be connected to gas phase haptoreaction device (3), and simple substance cadmium control valve (7) and simple substance cadmium gas is set on connecting pipe
Flowmeter (10)；Gas condensing unit (4) is connected to gas phase haptoreaction device (3), and residual air list is arranged on connecting pipe
To valve (8) and residual air gas flowmeter (11), elemental selenium gasification installation (1), simple substance is monitored and controlled by remote controllers (5)
The temperature and pressure of cadmium gasification installation (2), gas phase haptoreaction device (3) and gas condensing unit (4), passes through remote controllers
(5) elemental selenium control valve (6), simple substance cadmium control valve (7) and residual air check valve (8) switch are controlled, is supervised by remote controllers (5)
Survey elemental selenium gas flowmeter (9), simple substance cadmium gas flowmeter (10) and residual air gas flowmeter (11)；
A, gas phase haptoreaction device (3) is vacuumized using three stages pump, is first vacuumized, is evacuated to using mechanical pump
Vacuum degree is 1Pa~10Pa, then is vacuumized using adsorption pump, and being evacuated to vacuum degree is (1~5) × 10-4Pa, finally using from
Sub- pumping vacuum, being evacuated to vacuum degree is (1~9) × 10-7Pa, then 550~600 are warming up to heating rate for 200 DEG C/h
℃；
B, gas condensing unit (4) is vacuumized using three stages pump, is first vacuumized using mechanical pump, is evacuated to vacuum
Degree is 1Pa~10Pa, then is vacuumized using adsorption pump, and being evacuated to vacuum degree is (1~5) × 10-4Pa finally uses ionic pump
It vacuumizes, being evacuated to vacuum degree is (1~9) × 10-7Pa, and be 20~50 DEG C by the control of the temperature of gas condensing unit (4)；
C, the weighed elemental selenium of step 1 is placed in elemental selenium gasification installation (1), is then pumped using three stages to elemental selenium gas
Makeup is set (1) and is vacuumized, and is first vacuumized using mechanical pump, and being evacuated to vacuum degree is 1Pa~10Pa, then uses adsorption pump
It vacuumizes, being evacuated to vacuum degree is (1~5) × 10-4Pa is finally vacuumized using ionic pump, and being evacuated to vacuum degree is (1
~9) × 10-7Pa is opened elemental selenium control valve (6), then is heated up with heating rate for 100 DEG C/h, and remote controllers are passed through
(5) detect elemental selenium gas flowmeter (9), when the gas flow of elemental selenium gas flowmeter (9) reach 0.04L/min~
When 0.1L/min, stop heating, guarantees that gaseous elemental selenium enters gas phase contact with gas flow for 0.04L/min~0.1L/min
Reaction unit (3)；
D, the weighed simple substance cadmium of step 1 is placed in simple substance cadmium gasification installation (2), is then pumped using three stages to simple substance cadmium gas
Makeup is set (2) and is vacuumized, and is first vacuumized using mechanical pump, and being evacuated to vacuum degree is 1Pa~10Pa, then uses adsorption pump
It vacuumizes, being evacuated to vacuum degree is (1~5) × 10-4Pa is finally vacuumized using ionic pump, and being evacuated to vacuum degree is (1
~9) × 10-7Pa is opened simple substance cadmium control valve (7), then is heated up with heating rate for 100 DEG C/h, and remote controllers are passed through
(5) detect simple substance cadmium gas flowmeter (9), when the gas flow of simple substance cadmium gas flowmeter (9) reach 0.04L/min~
When 0.1L/min, stop heating, guarantees that gaseous elemental cadmium enters gas phase contact with gas flow for 0.04L/min~0.1L/min
Reaction unit (3)；And elemental selenium control valve (6) is opened simultaneously with simple substance cadmium control valve (7), elemental selenium gasification installation (1) and list
Matter cadmium gasification installation (2) is simultaneously that 100 DEG C/h heats up with heating rate；
E, gaseous elemental selenium is sent into gas phase haptoreaction device (3) with gas flow for 0.04L/min~0.1L/min, gaseous state list
Matter cadmium with gas flow be 0.04L/min~0.1L/min be sent into gas phase haptoreaction device (3), and guarantee gaseous elemental selenium with
Gaseous elemental cadmium is sent into gas phase haptoreaction device (3) with same gas flow, gaseous elemental at being 550~600 DEG C in temperature
In gas phase haptoreaction device (3) progress vapor- phase synthesis, reaction generates cadmium selenide polycrystalline in solid form for selenium and gaseous elemental cadmium
The deposition in gas phase haptoreaction device (3), not sufficiently reactive gaseous elemental selenium and gaseous elemental cadmium pass through residual air check valve
(8) gas condensing unit (4) are flow to, when the gas flow of residual air gas flowmeter (11) display is 0L/min, with the speed that cools down
Rate is 20 DEG C/h~50 DEG C/h by elemental selenium gasification installation (1), the gentle reaction unit that is in contact (3) of simple substance cadmium gasification installation (2)
It is gradually cooling to room temperature, cadmium selenide polycrystal powder is taken out in gas phase haptoreaction device (3)；It is single during vapor- phase synthesis
Pressure < 0.3MPa in matter selenium gasification installation (1), the pressure < 0.3MPa in simple substance cadmium gasification installation (2), gas phase contact are anti-
Answer the pressure < 0.5MPa in device (3), the pressure < 0.5MPa in gas condensing unit (4)；
The purity > 99% of the cadmium selenide polycrystal powder.
2. a kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material according to claim 1, it is characterised in that step
Elemental selenium described in one is 6N selenium, and simple substance cadmium described in step 1 is 7N cadmium.
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