CN107675251A - 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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- CN107675251A CN107675251A CN201710900796.XA CN201710900796A CN107675251A CN 107675251 A CN107675251 A CN 107675251A CN 201710900796 A CN201710900796 A CN 201710900796A CN 107675251 A CN107675251 A CN 107675251A
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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
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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 to have the problem of reaction temperature is high, and time-consuming, and the cadmium selenide purity produced is low.Gas-phase synthesizing method：First, elemental selenium and simple substance cadmium are weighed；2nd, 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 deposited, and is cooled to room temperature, obtains cadmium selenide polycrystal powder.Advantage：Reaction temperature is reduced, 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 method of cadmium selenide polycrystalline material.
Background technology
Cadmium selenide is a kind of II-VI compound, has larger energy gap (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 optics.High-purity cadmium selenide polycrystalline material synthesis is the basis of high-quality cadmium selenide crystal growth.Current cadmium selenide
More crystal preparation methods, it is that elemental selenium and simple substance cadmium are closed in vitreosil pipe, 950-1000 DEG C is warming up to using tube furnace,
React 24-72 hours.The preparation method reaction temperature is high, the reaction time is long, reaction rate is difficult to control, and too high temperature causes
Reactant largely gasifies, and causes pressure is excessive easily to explode.And the cadmium selenide fusing point of generation is up to 1250 DEG C, in system
Inside existing in solid form, hamper contact of the reactant elemental selenium with simple substance cadmium, reaction is not abundant enough, so that product
Purity receives is not used to crystal growth by certain influence, the polycrystalline material of acquisition.
The content of the invention
The invention aims to solve existing cadmium selenide synthetic method to have reaction temperature height, time-consuming, and produce
The problem of cadmium selenide purity is low, 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 according to the following steps：
First, weigh：Mol ratio according to Se and Cd is (1~1.05):1 weighs elemental selenium and simple substance cadmium；2nd, gas phase is closed
Into：1., reaction zone is vacuumized, it is (1~9) × 10 to be evacuated to vacuum-7Pa, then it is warming up to 550~600 DEG C；②、
Condensing zone is vacuumized, it is (1~9) × 10 to be evacuated to vacuum-7Pa, and be 20~50 DEG C by temperature control；3., will
The elemental selenium that step 1 weighs is placed in elemental selenium gasification zone, and then elemental selenium gasification zone is vacuumized, is evacuated to vacuum
Spend for (1~9) × 10-7Pa, then 400~500 DEG C are warming up to, and elemental selenium is gasified at being 400~500 DEG C in temperature,
Obtain gaseous elemental selenium；4., the simple substance cadmium that step 1 weighs is placed in simple substance cadmium gasification zone, then simple substance cadmium gasification zone is carried out
Vacuumize, it is (1~9) × 10 to be evacuated to vacuum-7Pa, then 500~700 DEG C are warming up to, and be 500~700 DEG C in temperature
Under simple substance cadmium is gasified, obtain gaseous elemental cadmium；5., gaseous elemental selenium is using gas flow as 0.04L/min~0.1L/
Min is sent into reaction zone, and gaseous elemental cadmium is sent into reaction zone by 0.04L/min~0.1L/min of gas flow, and ensures gaseous state
Elemental selenium is sent into reaction zone with same gas flow simultaneously with gaseous elemental cadmium, 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 generation cadmium selenide polycrystalline deposits in reaction zone in solid form,
Not sufficiently reactive gaseous elemental selenium flow to condensing zone with gaseous elemental cadmium 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, and cadmium selenide polycrystal powder is taken out in reaction zone；And during vapor- phase synthesis, simple substance
Selenium gasification zone, simple substance cadmium gasification zone, the pressure ＜ 0.5MPa of reaction zone and condensing zone；The purity ＞ of the cadmium selenide polycrystal powder
99%.
Advantage of the present invention：The present invention uses elemental selenium in gas-phase synthesizing method to be respectively placed in two different warm areas from simple substance cadmium
Gasified, obtain stable gasification rate by adjusting thermal field so that gaseous elemental selenium is with gaseous elemental cadmium in three-temperature-zone
Haptoreaction, the cadmium selenide polycrystalline of vapor- phase synthesis are deposited in the form of solid-state, unreacted gaseous elemental selenium and gaseous elemental cadmium
Then continue flow forward to four-temperature region and cool down recovery, whole system is by adjusting temperature control material gasification speed and unreacted
Gas condensing rate, ensure the pressure ＜ 0.5MPa of elemental selenium gasification zone, simple substance cadmium gasification zone, reaction zone and condensing zone, peace
Overall coefficient greatly improves.And the contact of gaseous elemental greatly reduces reaction temperature, 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 three-temperature-zone, and unreacted simple substance flows to
Four-temperature region is reclaimed, so the purity superelevation significantly of the cadmium selenide polycrystal powder obtained, the purity ＞ of cadmium selenide polycrystal powder
99%.
Brief description of the drawings
Fig. 1 is the structural representation of cadmium selenide polycrystalline apparatus for gas-phase synthesis described in specific embodiment party eight；1 represents simple substance in figure
Selenium gasification installation, 2 represent simple substance cadmium gasification installation, and 3 represent gas phase haptoreaction device, and 4 represent gas condensing unit, and 5 represent
Remote controllers, 6 represent elemental selenium control valve, and 7 represent simple substance cadmium control valve, and 8 represent residual air check valve, and 9 represent elemental selenium gas
Flowmeter body, 10 represent simple substance cadmium gas flowmeter, and 11 represent residual air gas flowmeter.
Embodiment
Embodiment one：Present embodiment is a kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material, and it is
Complete according to the following steps：
First, weigh：Mol ratio according to Se and Cd is (1~1.05):1 weighs elemental selenium and simple substance cadmium；2nd, gas phase is closed
Into：1., reaction zone is vacuumized, it is (1~9) × 10 to be evacuated to vacuum-7Pa, then it is warming up to 550~600 DEG C；②、
Condensing zone is vacuumized, it is (1~9) × 10 to be evacuated to vacuum-7Pa, and be 20~50 DEG C by temperature control；3., will
The elemental selenium that step 1 weighs is placed in elemental selenium gasification zone, and then elemental selenium gasification zone is vacuumized, is evacuated to vacuum
Spend for (1~9) × 10-7Pa, then 400~500 DEG C are warming up to, and elemental selenium is gasified at being 400~500 DEG C in temperature,
Obtain gaseous elemental selenium；4., the simple substance cadmium that step 1 weighs is placed in simple substance cadmium gasification zone, then simple substance cadmium gasification zone is carried out
Vacuumize, it is (1~9) × 10 to be evacuated to vacuum-7Pa, then 500~700 DEG C are warming up to, and be 500~700 DEG C in temperature
Under simple substance cadmium is gasified, obtain gaseous elemental cadmium；5., gaseous elemental selenium is using gas flow as 0.04L/min~0.1L/
Min is sent into reaction zone, and gaseous elemental cadmium is sent into reaction zone by 0.04L/min~0.1L/min of gas flow, and ensures gaseous state
Elemental selenium is sent into reaction zone with same gas flow simultaneously with gaseous elemental cadmium, 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 generation cadmium selenide polycrystalline deposits in reaction zone in solid form,
Not sufficiently reactive gaseous elemental selenium flow to condensing zone with gaseous elemental cadmium 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, and cadmium selenide polycrystal powder is taken out in reaction zone；And during vapor- phase synthesis, simple substance
Selenium gasification zone, simple substance cadmium gasification zone, the pressure ＜ 0.5MPa of reaction zone and condensing zone；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 enters promoting the circulation of qi
Change, obtain stable gasification rate by adjusting thermal field so that gaseous elemental selenium contacts instead with gaseous elemental cadmium in three-temperature-zone
Should, the cadmium selenide polycrystalline of vapor- phase synthesis is deposited in the form of solid-state, and unreacted gaseous elemental selenium and gaseous elemental cadmium then continue
Flow forward is cooled down to four-temperature region and reclaimed, and whole system is by adjusting temperature control material gasification speed and unreacted gas
Condensing rate, ensure the pressure ＜ 0.5MPa of elemental selenium gasification zone, simple substance cadmium gasification zone, reaction zone and condensing zone, safety coefficient
Greatly improve.And the contact of gaseous elemental greatly reduces reaction temperature, whole system temperature is no more than 800 DEG C, and gas
What is be combined to time-consuming greatly reduces.The cadmium selenide polycrystalline of synthesis is deposited on three-temperature-zone, and unreacted simple substance flows to the 4th temperature
Area reclaims, so the cadmium selenide polycrystal powder superelevation significantly obtained, the purity ＞ 99% of cadmium selenide polycrystal powder.
Embodiment two：The difference of present embodiment and embodiment one is：List described in step 1
Matter selenium is 6N selenium, and the simple substance cadmium described in step 1 is 7N cadmiums.Other are identical with embodiment one.
Embodiment three：The difference of present embodiment and one of embodiment one or two is：Step 2 is 3.
In using heating rate as 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.
Embodiment four：The difference of present embodiment and one of embodiment one to three is：Step 2 is 4.
In using heating rate as 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.
Embodiment five：The difference of present embodiment and one of embodiment one to four is：Step 2 is 4.
In using heating rate as 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.
Embodiment six：The difference of present embodiment and one of embodiment one to five is：Step 2 is 5.
In using rate of temperature fall as 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 with embodiment one to five.
Embodiment seven：The difference of present embodiment and one of embodiment one to six is：Step 2 is 5.
During middle vapor- phase synthesis, the pressure ＜ 0.3MPa in elemental selenium gasification zone, the pressure ＜ 0.3MPa in simple substance cadmium gasification zone.Its
He is identical with embodiment one to six.
Embodiment eight：With reference to Fig. 1, the difference of present embodiment and one of embodiment one to seven is：
Elemental selenium and the vapor- phase synthesis of simple substance cadmium, the cadmium selenide polycrystalline are carried out using cadmium selenide polycrystalline apparatus for gas-phase synthesis in step 2
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
Formed with remote controllers 5, it is same that elemental selenium gasification installation 1 and simple substance cadmium gasification installation 2 are arranged on gas phase haptoreaction device 3
Side, gas condensing unit 4 are arranged on gas phase haptoreaction device 3 relative to elemental selenium gasification installation 1 and simple substance cadmium gasification installation 2
Offside, elemental selenium gasification installation 1 connected with gas phase haptoreaction device 3, and elemental selenium control valve 6 is set on connecting pipe
With elemental selenium gas flowmeter 9；Simple substance cadmium gasification installation 2 connects with gas phase haptoreaction device 3, and is set on connecting pipe
Simple substance cadmium control valve 7 and simple substance cadmium gas flowmeter 10；Gas condensing unit 4 connects with gas phase haptoreaction device 3, and even
Thread a pipe upper setting residual air check valve 8 and residual air gas flowmeter 11, pass through remote controllers 5 elemental selenium is monitored and controlled and gasify
Device 1, simple substance cadmium gasification installation 2, the temperature and pressure of gas phase haptoreaction device 3 and gas condensing unit 4, by remotely controlling
Device 5 processed controls elemental selenium control valve 6, simple substance cadmium control valve 7 and residual air check valve 8 to switch, and simple substance is monitored 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 stage pumps, is first vacuumized, vacuumized using mechanical pump
It is 1Pa~10Pa to vacuum, then is vacuumized using adsorption pump, it is (1~5) × 10 to be evacuated to vacuum-4Pa, finally use
Ionic pump vacuumizes, and it is (1~9) × 10 to be evacuated to vacuum-7Pa, then using heating rate as 200 DEG C/h it is warming up to 550~
600℃；
B, gas condensing unit 4 is vacuumized using three stage pumps, first vacuumized using mechanical pump, is evacuated to true
Reciprocal of duty cycle is 1Pa~10Pa, then is vacuumized using adsorption pump, and it is (1~5) × 10 to be evacuated to vacuum-4Pa, finally using ion
Pumping vacuum, it is (1~9) × 10 to be evacuated to vacuum-7Pa, and be 20~50 DEG C by the temperature control of gas condensing unit 4；
C, the elemental selenium for weighing step 1 is placed in elemental selenium gasification installation 1, then using three stage pumps to list
Matter selenium gasification installation 1 is vacuumized, and is first vacuumized using mechanical pump, and it is 1Pa~10Pa to be evacuated to vacuum, then using suction
Attached pumping vacuum, it is (1~5) × 10 to be evacuated to vacuum-4Pa, finally vacuumized using ionic pump, be evacuated to vacuum
For (1~9) × 10-7Pa, elemental selenium control valve 6 is opened, then heated up by 100 DEG C/h of heating rate, pass through remote control
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, ensure that gaseous elemental selenium enters gas phase haptoreaction device by 0.04L/min~0.1L/min of gas flow
3；
D, the simple substance cadmium that step 1 weighs is placed in simple substance cadmium gasification installation 2, then using three stage pumps to simple substance cadmium
Gasification installation 2 is vacuumized, and is first vacuumized using mechanical pump, and it is 1Pa~10Pa to be evacuated to vacuum, then using adsorption pump
Vacuumize, it is (1~5) × 10 to be evacuated to vacuum-4Pa, finally vacuumized using ionic pump, be evacuated to vacuum as (1
~9) × 10-7Pa, simple substance cadmium control valve 7 is opened, then heated up by 100 DEG C/h of heating rate, examined by remote controllers 5
Simple substance cadmium gas flowmeter 9 is surveyed, when the gas flow of simple substance cadmium gas flowmeter 9 reaches 0.04L/min~0.1L/min, is stopped
Only heat up, ensure that gaseous elemental cadmium enters gas phase haptoreaction device 3 by 0.04L/min~0.1L/min of gas flow；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 liter
Warm speed is that 100 DEG C/h is heated up；
E, gaseous elemental selenium is sent into gas phase haptoreaction device 3, gaseous state by 0.04L/min~0.1L/min of gas flow
Simple substance cadmium is sent into gas phase haptoreaction device 3 by 0.04L/min~0.1L/min of gas flow, and ensure 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 generation cadmium selenide polycrystalline is in solid form in gas
The reaction unit 3 that is in contact is interior to be deposited, and not sufficiently reactive gaseous elemental selenium flow to gas with gaseous elemental cadmium 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, using rate of temperature fall as 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；During vapor- phase synthesis, the pressure ＜ in elemental selenium gasification installation 1
0.3MPa, the pressure ＜ 0.3MPa in simple substance cadmium gasification installation 2.
Other are identical with embodiment one to seven.
The gas phase transmission pipeline of present embodiment answers long enough, prevents it from connecting different warm areas and produces excessive heat and answer
Power, cause pipeline damaged；The purpose that one-way cock is set, ensure that two kinds of gases only react in gas phase haptoreaction region, prevent
Only a kind of gas excessively flows 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 utilization of materials is higher, but thing followed system pressure, and temperature can all raise.
Present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several embodiments
Contract sample can also realize the purpose of invention.
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, filled using cadmium selenide polycrystalline vapor- phase synthesis
Put and carry out elemental selenium and the vapor- phase synthesis of simple substance cadmium, 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 simple substance cadmium gasification installation 2 be arranged on the same side of gas phase haptoreaction device 3, gas condensing unit 4 gasifies relative to elemental selenium
Device 1 and simple substance cadmium gasification installation 2 are arranged on the offside of gas phase haptoreaction device 3, and elemental selenium gasification installation 1 contacts with gas phase
Reaction unit 3 is connected, and elemental selenium control valve 6 and elemental selenium gas flowmeter 9 are set on connecting pipe；Simple substance cadmium gasification dress
Put 2 to connect with gas phase haptoreaction device 3, and simple substance cadmium control valve 7 and simple substance cadmium gas flowmeter are set on connecting pipe
10；Gas condensing unit 4 is connected with gas phase haptoreaction device 3, and residual air check valve 8 and residual air gas are set on connecting pipe
Flowmeter body 11, elemental selenium gasification installation 1, simple substance cadmium gasification installation 2, gas phase is monitored and controlled by remote controllers 5 and contacts
The temperature and pressure of reaction unit 3 and gas condensing unit 4, elemental selenium control valve 6, simple substance cadmium are controlled by remote controllers 5
Control valve 7 and residual air check valve 8 are switched, and elemental selenium gas flowmeter 9, simple substance cadmium gas flow are monitored by remote controllers 5
Meter 10 and residual air gas flowmeter 11；It is specifically realized by the following steps：
First, weigh：Weigh 100.2g elemental seleniums and 140.7g simple substance cadmiums；
2nd, gas phase haptoreaction device 3 is vacuumized using three stage pumps, it is 2.5Pa to be evacuated to vacuum, then
Vacuumized using adsorption pump, be evacuated to vacuum as 2 × 10-4Pa, finally vacuumized using ionic pump, be evacuated to vacuum
For 5.6 × 10-7Pa, then it is warming up to 600 DEG C by 200 DEG C/h of heating rate；
3rd, gas condensing unit 4 is vacuumized using three stage pumps, it is 2.5Pa to be evacuated to vacuum, then is used
Adsorption pump vacuumizes, and is evacuated to vacuum as 2 × 10-4Pa, finally vacuumized using ionic pump, being evacuated to vacuum is
4.7×10-7Pa, and be 50 DEG C by the temperature control of gas condensing unit 4；
4th, 100.2g elemental seleniums are placed in elemental selenium gasification installation 1, then using three stage pumps to elemental selenium gas
Makeup is put 1 and vacuumized, and is first vacuumized using mechanical pump, and it is 2.5Pa to be evacuated to vacuum, then true using absorption pumping
Sky, vacuum is evacuated to as 2 × 10-4Pa, finally vacuumized using ionic pump, be evacuated to vacuum as 2.5 × 10-7Pa,
Elemental selenium control valve 6 is opened, then is heated up by 100 DEG C/h of heating rate, elemental selenium gas is detected by remote controllers 5
Flowmeter 9, when the gas flow of elemental selenium gas flowmeter 9 reaches 0.08L/min, stop heating, ensure gaseous elemental selenium
Enter gas phase haptoreaction device 3 by 0.08L/min of gas flow；The temperature of elemental selenium gasification installation 1 is 455 DEG C；
5th, 140.7g simple substance cadmiums are placed in simple substance cadmium gasification installation 2, then simple substance cadmium, which is gasified, using three stage pumps is filled
Put 2 to be vacuumized, first vacuumized using mechanical pump, it is 3Pa to be evacuated to vacuum, then is vacuumized using adsorption pump, is taken out true
Sky to vacuum is 2.8 × 10-4Pa, finally vacuumized using ionic pump, be evacuated to vacuum as 2.5 × 10-7Pa, open
Simple substance cadmium control valve 7, then heated up by 100 DEG C/h of heating rate, detect simple substance cadmium gas flow by remote controllers 5
Meter 9, when the gas flow of simple substance cadmium gas flowmeter 9 reaches 0.08L/min, stop heating, ensure 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
Heated up for 100 DEG C/h；
6th, gaseous elemental selenium is sent into gas phase haptoreaction device 3 using gas flow as 0.08L/min, 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 generation cadmium selenide polycrystalline is in solid form in gas phase haptoreaction
Deposited in device 3, not sufficiently reactive gaseous elemental selenium flow to gas condensing unit with gaseous elemental cadmium by residual air check valve 8
4,11h is reacted, the gas flow that now residual air gas flowmeter 11 is shown is 0L/min, is 30 DEG C/h by simple substance using 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, is filled in gas phase haptoreaction
Cadmium selenide polycrystal powder is taken out in putting 3；During vapor- phase synthesis, pressure in elemental selenium gasification installation 1 for 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 is 100Pa~1000Pa.
Elemental selenium described in the present embodiment step 1 is 6N selenium, and the simple substance cadmium described in step 1 is 7N cadmiums.
The present embodiment elemental selenium gasification installation 1, simple substance cadmium gasification installation 2, gas phase haptoreaction device 3 and gas condensation dress
Put 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.Examined through ICP
The purity of cadmium selenide polycrystal powder made from analysis of checking the mark is 99.9999%, and Se and Cd mol ratios are in cadmium selenide polycrystal powder
1.007:1。
Embodiment 2：A kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material, filled using cadmium selenide polycrystalline vapor- phase synthesis
Put and carry out elemental selenium and the vapor- phase synthesis of simple substance cadmium, 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 simple substance cadmium gasification installation 2 be arranged on the same side of gas phase haptoreaction device 3, gas condensing unit 4 gasifies relative to elemental selenium
Device 1 and simple substance cadmium gasification installation 2 are arranged on the offside of gas phase haptoreaction device 3, and elemental selenium gasification installation 1 contacts with gas phase
Reaction unit 3 is connected, and elemental selenium control valve 6 and elemental selenium gas flowmeter 9 are set on connecting pipe；Simple substance cadmium gasification dress
Put 2 to connect with gas phase haptoreaction device 3, and simple substance cadmium control valve 7 and simple substance cadmium gas flowmeter are set on connecting pipe
10；Gas condensing unit 4 is connected with gas phase haptoreaction device 3, and residual air check valve 8 and residual air gas are set on connecting pipe
Flowmeter body 11, elemental selenium gasification installation 1, simple substance cadmium gasification installation 2, gas phase is monitored and controlled by remote controllers 5 and contacts
The temperature and pressure of reaction unit 3 and gas condensing unit 4, elemental selenium control valve 6, simple substance cadmium are controlled by remote controllers 5
Control valve 7 and residual air check valve 8 are switched, and elemental selenium gas flowmeter 9, simple substance cadmium gas flow are monitored by remote controllers 5
Meter 10 and residual air gas flowmeter 11；It is specifically realized by the following steps：
First, weigh：Weigh 40.0g elemental seleniums and 55.2g simple substance cadmiums；
2nd, gas phase haptoreaction device 3 is vacuumized using three stage pumps, first vacuumized using mechanical pump, taken out true
Sky to vacuum is 1.5Pa, then is vacuumized using adsorption pump, is evacuated to vacuum as 2.5 × 10-4Pa, finally using ion
Pumping vacuum, vacuum is evacuated to as 8.1 × 10-7Pa, then it is warming up to 550 DEG C by 200 DEG C/h of heating rate；
3rd, gas condensing unit 4 is vacuumized using three stage pumps, is first vacuumized, be evacuated to using mechanical pump
Vacuum is 1.5Pa, then vacuumized using adsorption pump, is evacuated to vacuum as 2.5 × 10-4Pa, finally using ion pumping
Vacuum, vacuum is evacuated to as 7.9 × 10-7Pa, and be 30 DEG C by the temperature control of gas condensing unit 4；
4th, 40.0g elemental seleniums are placed in elemental selenium gasification installation 1, then using three stage pumps to elemental selenium gas
Makeup is put 1 and vacuumized, and is first vacuumized using mechanical pump, and it is 1.5Pa to be evacuated to vacuum, then true using absorption pumping
Sky, vacuum is evacuated to as 2.5 × 10-4Pa, finally vacuumized using ionic pump, be evacuated to vacuum as 1.3 × 10- 7Pa, elemental selenium control valve 6 is opened, then heated up by 100 DEG C/h of heating rate, elemental selenium is detected by remote controllers 5
Gas flowmeter 9, when the gas flow of elemental selenium gas flowmeter 9 reaches 0.04L/min, stop heating, ensure gaseous state list
Matter selenium enters gas phase haptoreaction device 3 by 0.04L/min of gas flow；The temperature of elemental selenium gasification installation 1 is 415 DEG C；
5th, 55.2g simple substance cadmiums are placed in simple substance cadmium gasification installation 2, then simple substance cadmium, which is gasified, using three stage pumps is filled
Put 2 to be vacuumized, first vacuumized using mechanical pump, it is 3.5Pa to be evacuated to vacuum, then is vacuumized using adsorption pump, is taken out
Vacuum to vacuum is 3 × 10-4Pa, finally vacuumized using ionic pump, be evacuated to vacuum as 1.3 × 10-7Pa, open
Simple substance cadmium control valve 7, then heated up by 100 DEG C/h of heating rate, detect simple substance cadmium gas flow by remote controllers 5
Meter 9, when the gas flow of simple substance cadmium gas flowmeter 9 reaches 0.04L/min, stop heating, ensure 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
Heated up for 100 DEG C/h；
6th, gaseous elemental selenium is sent into gas phase haptoreaction device 3 using gas flow as 0.04L/min, 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 generation cadmium selenide polycrystalline is in solid form in gas phase haptoreaction
Deposited in device 3, not sufficiently reactive gaseous elemental selenium flow to gas condensing unit with gaseous elemental cadmium by residual air check valve 8
4,5h is reacted, the gas flow that now residual air gas flowmeter 11 is shown is 0L/min, is 30 DEG C/h by simple substance using 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, is filled in gas phase haptoreaction
Cadmium selenide polycrystal powder is taken out in putting 3；During vapor- phase synthesis, pressure in elemental selenium gasification installation 1 for 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 is 100Pa~2000Pa.
Elemental selenium described in the present embodiment step 1 is 6N selenium, and the simple substance cadmium described in step 1 is 7N cadmiums.
The present embodiment elemental selenium gasification installation 1, simple substance cadmium gasification installation 2, gas phase haptoreaction device 3 and gas condensation dress
Put 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.Examined through ICP
The purity of cadmium selenide polycrystal powder made from analysis of checking the mark is 99.9999%, and Se and Cd mol ratios are in cadmium selenide polycrystal powder
1.005:1。
Claims (8)
1. a kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material, it is characterised in that it is completed according to the following steps：
First, weigh：Mol ratio according to Se and Cd is (1~1.05):1 weighs elemental selenium and simple substance cadmium；2nd, vapor- phase synthesis：①、
Reaction zone is vacuumized, it is (1~9) × 10 to be evacuated to vacuum-7Pa, then it is warming up to 550~600 DEG C；2., to condensation
Area is vacuumized, and it is (1~9) × 10 to be evacuated to vacuum-7Pa, and be 20~50 DEG C by temperature control；3., by step 1
The elemental selenium weighed is placed in elemental selenium gasification zone, and then elemental selenium gasification zone is vacuumized, and is evacuated to vacuum as (1
~9) × 10-7Pa, then 400~500 DEG C are warming up to, and elemental selenium is gasified at being 400~500 DEG C in temperature, obtain gas
State elemental selenium；4., the simple substance cadmium that step 1 weighs is placed in simple substance cadmium gasification zone, then simple substance cadmium gasification zone take out true
Sky, it is (1~9) × 10 to be evacuated to vacuum-7Pa, then 500~700 DEG C are warming up to, and it is right in the case where temperature is 500~700 DEG C
Simple substance cadmium is gasified, and obtains gaseous elemental cadmium；5., gaseous elemental selenium gives by 0.04L/min~0.1L/min of gas flow
Enter reaction zone, gaseous elemental cadmium is sent into reaction zone by 0.04L/min~0.1L/min of gas flow, and ensures gaseous elemental selenium
Reaction zone is sent into same gas flow simultaneously with gaseous elemental cadmium, gaseous elemental selenium and gaseous state at being 550~600 DEG C in temperature
Simple substance cadmium carries out vapor- phase synthesis in reaction zone, and reaction generation cadmium selenide polycrystalline deposits in reaction zone in solid form, not fully
The gaseous elemental selenium of reaction flow to condensing zone with gaseous elemental cadmium by residual air check valve, when passing through the inabundant of residual air check valve
When the gaseous elemental selenium of reaction and the gas flow of gaseous elemental cadmium are 0L/min, by elemental selenium gasification zone, simple substance cadmium gasification zone
Room temperature is gradually cooling to reaction zone, cadmium selenide polycrystal powder is taken out in reaction zone；And during vapor- phase synthesis, elemental selenium gasification
Area, simple substance cadmium gasification zone, the pressure ＜ 0.5MPa of reaction zone and condensing zone；The purity ＞ 99% of the cadmium selenide polycrystal powder.
A kind of 2. 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 the simple substance cadmium described in step 1 is 7N cadmiums.
A kind of 3. gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material according to claim 1, it is characterised in that step
Two 3. in using heating rate as 100 DEG C/h by the temperature of elemental selenium gasification zone from room temperature to 400~500 DEG C.
A kind of 4. gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material according to claim 1, it is characterised in that step
Two 4. in using heating rate as 100 DEG C/h by the temperature of simple substance cadmium gasification zone from room temperature to 500~700 DEG C.
A kind of 5. gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material according to claim 1, it is characterised in that step
Two 4. in using heating rate as 200 DEG C/h by the temperature of simple substance cadmium gasification zone from room temperature to 550~600 DEG C.
A kind of 6. gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material according to claim 1, it is characterised in that step
Two 5. in elemental selenium gasification zone, simple substance cadmium gasification zone and reaction zone are gradually cooling to using rate of temperature fall as 20 DEG C/h~50 DEG C/h
Room temperature.
A kind of 7. gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material according to claim 1, it is characterised in that step
Two 5. during middle vapor- phase synthesis, the pressure ＜ 0.3MPa in elemental selenium gasification zone, the pressure ＜ in simple substance cadmium gasification zone
0.3MPa。
A kind of 8. gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material according to claim 1, it is characterised in that step
Elemental selenium and the vapor- phase synthesis of simple substance cadmium, the cadmium selenide polycrystalline gas phase are carried out using cadmium selenide polycrystalline apparatus for gas-phase synthesis in two
Synthesizer is by elemental selenium gasification installation (1), simple substance cadmium gasification installation (2), gas phase haptoreaction device (3), gas condensation dress
(4) and remote controllers (5) composition are put, it is anti-that elemental selenium gasification installation (1) and simple substance cadmium gasification installation (2) are arranged on gas phase contact
Device (3) the same side is answered, gas condensing unit (4) is set relative to elemental selenium gasification installation (1) and simple substance cadmium gasification installation (2)
In the offside of gas phase haptoreaction device (3), elemental selenium gasification installation (1) connects with gas phase haptoreaction device (3), and even
Thread a pipe upper setting elemental selenium control valve (6) and elemental selenium gas flowmeter (9)；Simple substance cadmium gasification installation (2) contacts with gas phase
Reaction unit (3) is connected, and simple substance cadmium control valve (7) and simple substance cadmium gas flowmeter (10) are set on connecting pipe；Gas
Condensing unit (4) is connected with gas phase haptoreaction device (3), and residual air check valve (8) and residual air gas are set on connecting pipe
Flowmeter body (11), by remote controllers (5) be monitored and controlled elemental selenium gasification installation (1), simple substance cadmium gasification installation (2),
The temperature and pressure of gas phase haptoreaction device (3) and gas condensing unit (4), elemental selenium is controlled by remote controllers (5)
Control valve (6), simple substance cadmium control valve (7) and residual air check valve (8) switch, elemental selenium gas is monitored by remote controllers (5)
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 stage pumps, is first vacuumized, be evacuated to using mechanical pump
Vacuum is 1Pa~10Pa, then is vacuumized using adsorption pump, and it is (1~5) × 10 to be evacuated to vacuum-4Pa, finally use from
Sub- pumping vacuum, it is (1~9) × 10 to be evacuated to vacuum-7Pa, then it is warming up to 550~600 by 200 DEG C/h of heating rate
℃；
B, gas condensing unit (4) is vacuumized using three stage pumps, is first vacuumized using mechanical pump, be evacuated to vacuum
Spend for 1Pa~10Pa, then vacuumized using adsorption pump, it is (1~5) × 10 to be evacuated to vacuum-4Pa, finally using ionic pump
Vacuumize, it is (1~9) × 10 to be evacuated to vacuum-7Pa, and be 20~50 DEG C by the temperature control of gas condensing unit (4)；
C, the elemental selenium for weighing step 1 is placed in elemental selenium gasification installation (1), then using three stage pumps to simple substance
Selenium gasification installation (1) is vacuumized, and is first vacuumized using mechanical pump, and it is 1Pa~10Pa to be evacuated to vacuum, then using suction
Attached pumping vacuum, it is (1~5) × 10 to be evacuated to vacuum-4Pa, finally vacuumized using ionic pump, be evacuated to vacuum
For (1~9) × 10-7Pa, elemental selenium control valve (6) is opened, then heated up by 100 DEG C/h of heating rate, by remotely controlling
Device (5) processed detection elemental selenium gas flowmeter (9), when the gas flow of elemental selenium gas flowmeter (9) reach 0.04L/min~
During 0.1L/min, stop heating, ensure that gaseous elemental selenium contacts using gas flow as 0.04L/min~0.1L/min into gas phase
Reaction unit (3)；
D, the simple substance cadmium that step 1 weighs is placed in simple substance cadmium gasification installation (2), then using three stage pumps to simple substance cadmium gas
Makeup is put (2) and vacuumized, and is first vacuumized using mechanical pump, and it is 1Pa~10Pa to be evacuated to vacuum, then using adsorption pump
Vacuumize, it is (1~5) × 10 to be evacuated to vacuum-4Pa, finally vacuumized using ionic pump, be evacuated to vacuum as (1
~9) × 10-7Pa, simple substance cadmium control valve (7) is opened, then heated up by 100 DEG C/h of heating rate, pass through remote controllers
(5) detect simple substance cadmium gas flowmeter (9), when the gas flow of simple substance cadmium gas flowmeter (9) reach 0.04L/min~
During 0.1L/min, stop heating, ensure that gaseous elemental cadmium contacts using gas flow as 0.04L/min~0.1L/min into gas phase
Reaction unit (3)；And elemental selenium control valve (6) is opened with simple substance cadmium control valve (7) simultaneously, elemental selenium gasification installation (1) and list
Matter cadmium gasification installation (2) while heated up by 100 DEG C/h of heating rate；
E, gaseous elemental selenium is sent into gas phase haptoreaction device (3), gaseous state list by 0.04L/min~0.1L/min of gas flow
Matter cadmium using gas flow as 0.04L/min~0.1L/min be sent into gas phase haptoreaction device (3), and ensure 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
Selenium carries out vapor- phase synthesis with gaseous elemental cadmium in gas phase haptoreaction device (3), and reaction generation cadmium selenide polycrystalline is in solid form
Deposited in gas phase haptoreaction device (3), not sufficiently reactive gaseous elemental selenium passes through residual air check valve with gaseous elemental cadmium
(8) gas condensing unit (4) is flow to, when the gas flow of residual air gas flowmeter (11) display is 0L/min, with the speed that cools
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)
Room temperature is gradually cooling to, 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).
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| CN113416074A (en) * | 2021-08-10 | 2021-09-21 | 广东先导稀材股份有限公司 | Zinc telluride powder and preparation method of target thereof |
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