CN104944468B - Preparation method for zinc arsenide - Google Patents
Preparation method for zinc arsenide Download PDFInfo
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- CN104944468B CN104944468B CN201410118048.2A CN201410118048A CN104944468B CN 104944468 B CN104944468 B CN 104944468B CN 201410118048 A CN201410118048 A CN 201410118048A CN 104944468 B CN104944468 B CN 104944468B
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Abstract
The invention provides a preparation method for zinc arsenide. The preparation method comprises the following steps: weighing high-purity arsenic particles and high-purity zinc ingots with corresponding weights according to the molar proportion of arsenic and zinc in zinc arsenide, uniformly paving the weighed high-purity arsenic particles in a crucible boat, then covering the high-purity zinc ingots on the high-purity arsenic particles, and then horizontally placing the crucible boat in a plain-end quartz tube; vacuumizing the plain-end quartz tube filled with the high-purity arsenic particles and the high-purity zinc ingots by a vacuum unit, and then carrying out high-temperature sealing for the plain-end quartz tube by virtue of oxyhydrogen flame; placing the sealed plain-end quartz tube in a horizontal synthesis furnace, heating and insulating for a period of time, and then stopping heating and naturally cooling the horizontal synthesis furnace; after the horizontal synthesis furnace is cooled to a normal temperature, taking out the horizontal synthesis furnace and knocking open the plain-end quartz tube to obtain a high-purity zinc arsenide crystal. The preparation method provided by the invention increases the reaction speed of the synthesis process, can well control the arsenic vapour pressure during the synthesis process, and enables the reaction to be complete and adequate.
Description
Technical field
The present invention relates to technical field of material, more particularly, to a kind of preparation method of two arsenicization three zinc.
Background technology
Two arsenicization three zinc is gray crystals, is commonly used for spectrum analyses reagent and the raw material preparing electronic building brick, is also a kind of
Novel semiconductor material.In Semiconductor industry, two arsenicization three zinc also can be used as by the side such as epitaxy, chemical vapor deposition
The raw material of semi-conducting material or the arsenic sources such as the GaAs of method preparation, indium arsenide, gallium arsenide-phosphide, indium arsenic phosphide, its purposes is increasingly
Extensively.
At present the method for preparation two arsenicization three zinc mainly adopts after vapor- phase synthesis or vacuum volatilization synthesis vacuum distilling again
Separating-purifying, haves such problems as that response speed is slow, equipment investment is big, synthesis small scale, technique are more numerous and diverse.And because arsenic is 613
DEG C start to distil, its vapour pressure is increased dramatically with the rising of temperature, there is the potential safety hazards such as booster, so much making at present
Preparation Method is all using synthesizing primary two arsenicization three zinc at a lower temperature, but the reaction under low temperature is insufficient, deposits in synthesis material
In the arsenic dissociating in a large number, zinc and two zinc arsenides.
Content of the invention
A kind of in view of problem present in background technology, it is an object of the invention to provide preparation side of two arsenicization three zinc
Method, its synthesising reacting speed enabling in preparation process improves, the arsenic vapour pressure that can control well in building-up process
And make reaction cmpletely, thus obtain high-purity two arsenicization three zinc.
To achieve these goals, the invention provides a kind of preparation method of two arsenicization three zinc, it includes step: (1)
Weigh the high purity arsenic granule of corresponding weight and high-purity zinc ingot metal by arsenic in two arsenicization three zinc with the mol ratio of zinc, by the height claiming
The uniform shakedown of pure arsenic granule is sprinkled upon in a crucible boat, covers on high purity arsenic granule by high-purity zinc ingot metal afterwards, then by crucible boat
Level is put in flat mouth quartz ampoule；(2) will be equipped with high purity arsenic granule using vacuum pump set and the flat mouth quartz ampoule of high-purity zinc ingot metal is taken out
Vacuum is to 10-2Below pa, then carries out elevated-temperature seal using oxyhydrogen flame to the flat mouth quartz mouth of pipe；(3) by the flat mouth after sealing
Quartz ampoule is put in horizontal synthetic furnace, with the heating rate of 8～15 DEG C/min be warming up to 470～550 DEG C and be incubated 90～
150min, is warming up to 780～850 DEG C with the heating rate of 5～7 DEG C/min afterwards and is incubated 60～120min, then with 6～
The heating rate of 8.5 DEG C/min is warming up to 1050～1150 DEG C and is incubated 15～60min, subsequently stops heating and make level to synthesize
Stove Temperature fall；(4) after room temperature is down to by horizontal synthetic furnace, take out and knock open flat mouth quartz ampoule, that is, obtain two high-purity arsenic
Three zinc crystalline solid.
The invention has the benefit that
The preparation method of two arsenicization three zinc of the present invention improves the response speed of building-up process, can control conjunction well
Arsenic vapour pressure during one-tenth, makes reaction cmpletely.
The equipment investment of the preparation method of two arsenicization three zinc of the present invention is low, and reaction condition is easily-controllable, simple, safety, product
Synthesis scale is changeable, and preparation cost is low.
Specific embodiment
Preparation method the following detailed description of two arsenicization three zinc according to the present invention and embodiment and detection process and
Testing result.
The preparation method of two arsenicization three zinc according to the present invention is described first, including step: (1) presses arsenic in two arsenicization three zinc
Weigh the high purity arsenic granule of corresponding weight and high-purity zinc ingot metal with the mol ratio of zinc, by uniform for the high purity arsenic claiming granule shakedown
It is sprinkled upon in a crucible boat, afterwards high-purity zinc ingot metal is covered on high purity arsenic granule, then crucible boat level is put into flat mouth quartz
In pipe；(2) will be equipped with high purity arsenic granule using vacuum pump set and the flat mouth quartz ampoule of high-purity zinc ingot metal is evacuated to 10-2Below pa,
Then using oxyhydrogen flame, elevated-temperature seal is carried out to the flat mouth quartz mouth of pipe；(3) the flat mouth quartz ampoule after sealing is put into level to close
Become stove in, be warming up to 470～550 DEG C with the heating rate of 8～15 DEG C/min and be incubated 90～150min, afterwards with 5～7 DEG C/
The heating rate of min is warming up to 780～850 DEG C and is incubated 60～120min, then with the heating rate liter of 6～8.5 DEG C/min
Temperature to 1050～1150 DEG C and is incubated 15～60min, subsequently stops heating and making horizontal synthetic furnace Temperature fall；(4) treat level
After room temperature is down to by synthetic furnace, take out and knock open flat mouth quartz ampoule, that is, obtain high-purity two arsenicization three zinc crystalline solid.
In the preparation method according to two arsenicization three zinc of the present invention, in step (1), zinc ingot metal covers in high purity arsenic
It is in order that the relatively low high-purity zinc ingot metal of fusing point melts completely in lower temperature and the high purity arsenic by bottom solid-state above granule
Grain all wraps so that the high purity arsenic granule of high-purity zinc ingot metal of melt and solid-state is fully contacted and reacts and (improves and synthesized
The response speed of journey, makes reaction cmpletely), greatly reduce the volatilization of arsenic such that it is able to control building-up process well simultaneously
In arsenic vapour pressure, improve the purity of obtained two arsenicization three zinc.
In the preparation method according to two arsenicization three zinc of the present invention, in step (1), cover in high purity arsenic granule
On the set-up procedure of high-purity zinc ingot metal be: another crucible boat that (a) will be equipped with high purity zinc is placed in bistrique quartz ampoule and to bistrique
It is filled with protective gas in quartz ampoule, then bistrique quartz ampoule level is put in horizontal heating furnace, afterwards level is heated stove heat
It is warming up to 455～550 DEG C and is incubated 30～60min, being then turned off horizontal heating furnace makes the high purity zinc in this crucible boat cold with stove
But form high-purity zinc ingot metal to room temperature；B () is opened bistrique quartz ampoule and is taken out one section of high-purity zinc ingot metal dilute hydrochloric acid immersion of cooling
Time, and vacuum drying after deionized water is rinsed well, weigh the weight of high-purity zinc ingot metal.
In the preparation method according to two arsenicization three zinc of the present invention, in step (a)., the purity of high purity zinc can be
5n and more than, the purity of high-purity zinc ingot metal can be 5～6n.
In the preparation method according to two arsenicization three zinc of the present invention, in step (a)., protective gas can be nitrogen
Or noble gases.
In the preparation method according to two arsenicization three zinc of the present invention, in step (a)., crucible boat can for 4n and with
On high purity graphite crucible boat or zirconium oxide crucible boat.
In the preparation method according to two arsenicization three zinc of the present invention, in step (b), the concentration of dilute hydrochloric acid can be
10%.
In the preparation method according to two arsenicization three zinc of the present invention, in step (b), high-purity zinc ingot metal is in dilute hydrochloric acid
The time of middle immersion can be 2～5min.
In the preparation method according to two arsenicization three zinc of the present invention, in step (1), crucible boat can for 4n and with
On high purity graphite crucible boat or zirconium oxide crucible boat.
In the preparation method according to two arsenicization three zinc of the present invention, in step (1), the purity of high purity arsenic granule
Can for 5n and more than.
In the preparation method according to two arsenicization three zinc of the present invention, in step (1), the granule of high purity arsenic granule
Degree can be 0.5～5mm.
In the preparation method according to two arsenicization three zinc of the present invention, in step (2), vacuum can for 1.0 ×
10-3～9 × 10-3pa.
Secondly the embodiment of the preparation method according to two arsenicization three zinc of the present invention for the explanation.
Embodiment 1
(1) by long 30cm, it is placed in bistrique quartz ampoule and to bistrique quartz equipped with the high purity graphite crucible boat of 5n high purity zinc
Logical nitrogen protection in pipe, then bistrique quartz ampoule level is put in horizontal heating furnace, horizontal heating furnace is warming up to 455 DEG C afterwards,
Constant temperature 60min, after high purity zinc all melts, the horizontal heating furnace of closing makes the high purity zinc furnace cooling in high purity graphite crucible boat
Form high-purity zinc ingot metal to room temperature；
(2) open bistrique quartz ampoule and take out high-purity zinc ingot metal, soak, with dilute hydrochloric acid, the oxide-film that 2min processes surface, then spend
Ionized water is rinsed well and vacuum drying, and the weight of the high-purity zinc ingot metal after must processing is called 453.6g；
(3) calculated according to arsenic and zinc mol ratio 2:3 and weigh corresponding weight 5n is high-purity, granularity is the arsenic of 0.5mm
Grain 346.6g, the high purity arsenic weighing granule is equably laid in high purity graphite crucible boat bottom, afterwards will be straight for high-purity zinc ingot metal
Connect covering above high purity arsenic granule, then put into high purity graphite crucible boat level in flat mouth quartz ampoule；
(4) will be equipped with high purity arsenic granule using vacuum pump set and the flat mouth quartz ampoule of high-purity zinc ingot metal is evacuated to 7.3 × 10- 3Pa, then carries out elevated-temperature seal using oxyhydrogen flame to the flat mouth quartz mouth of pipe；
(5) the flat mouth quartz ampoule after tube sealing is put into constant temperature section length in the horizontal synthetic furnace of 80cm, by program control
Intensification heating process processed, is rapidly heated to 470 DEG C with the speed of 8 DEG C/min, constant temperature 150min, then with the speed of 7 DEG C/min
It is warming up to 850 DEG C, constant temperature 60min, subsequently it is warming up to 1100 DEG C with the speed of 7.5 DEG C/min, constant temperature 30min, closes afterwards and adds
Heat, makes horizontal synthetic furnace Temperature fall；
(6) after room temperature is down to by horizontal synthetic furnace, take out and knock open flat mouth quartz ampoule, that is, obtain in high purity graphite crucible boat
Reaction completely, uniformly, no layering, the no high-quality of dephasign, high-purity 5n bis- arsenicization three zinc 796.5g, product yield is 99.5%.
Embodiment 2
(1) by long 45cm, it is placed in bistrique quartz ampoule and to bistrique stone equipped with the high-purity zirconia crucible boat of 6n high purity zinc
Logical argon protection in English pipe, then bistrique quartz ampoule level is put in horizontal heating furnace, horizontal heating furnace is warming up to 500 afterwards
DEG C, constant temperature 40min, after high purity zinc all melts, the horizontal heating furnace of closing makes high purity zinc cool down in high-purity zirconia crucible boat
Form high-purity zinc ingot metal to room temperature；
(2) open bistrique quartz ampoule and take out high-purity zinc ingot metal, soak, with dilute hydrochloric acid, the oxide-film that 3min processes surface, use afterwards
The clean simultaneously vacuum drying of deionized water rinsing, the weight weighing the high-purity zinc ingot metal after process is 921.1g；
(3) calculated according to arsenic and zinc mol ratio 2:3 and weigh corresponding weight 6n is high-purity, granularity is the arsenic granule of 5mm
703.7g, the high purity arsenic weighing granule is equably laid in high-purity zirconia crucible boat bottom, high-purity zinc ingot metal is directly covered
Cover above high purity arsenic granule, then put into high-purity zirconia crucible boat level in flat mouth quartz ampoule；
(4) will be equipped with high purity arsenic granule using vacuum pump set and the flat mouth quartz ampoule of high-purity zinc ingot metal is evacuated to 8.6 × 10- 3Pa, carries out elevated-temperature seal using oxyhydrogen flame to the flat mouth quartz mouth of pipe；
(5) the flat mouth quartz ampoule after tube sealing is put into constant temperature section length in the horizontal synthetic furnace of 95cm, by program control
Intensification heating process processed, is rapidly heated to 500 DEG C with the speed of 12 DEG C/min, constant temperature 90min, then with the speed of 5 DEG C/min
It is warming up to 780 DEG C, constant temperature 120min, subsequently it is warming up to 1150 DEG C with the speed of 8.5 DEG C/min, constant temperature 15min, closes afterwards and adds
Heat, makes horizontal synthetic furnace Temperature fall；
(6) after room temperature is down to by horizontal synthetic furnace, take out and knock open flat mouth quartz ampoule, that is, obtain high-purity zirconia crucible boat
Interior reaction completely, uniformly, no layering, the no high-quality of dephasign, high-purity 6n bis- arsenicization three zinc 1607.3g, product yield is
98.9%.
Embodiment 3
(1) by long 60cm, it is placed in bistrique quartz ampoule and to bistrique quartz equipped with the high purity graphite crucible boat of 5n high purity zinc
Logical nitrogen protection in pipe, then bistrique quartz ampoule level is put in horizontal heating furnace, horizontal heating furnace is heated to 550 afterwards
DEG C, constant temperature 30min, after high purity zinc all melts, the horizontal heating furnace of closing makes the high purity zinc in high purity graphite crucible boat cold with stove
But form high-purity zinc ingot metal to room temperature；
(2) open bistrique quartz ampoule and take out high-purity zinc ingot metal, soak, with dilute hydrochloric acid, the oxide-film that 5min processes surface, use afterwards
The clean simultaneously vacuum drying of deionized water rinsing, the weight weighing the high-purity zinc ingot metal after process is 1171.7g；
(3) calculated according to arsenic and zinc mol ratio 2:3 and weigh corresponding weight 5n is high-purity, granularity is the arsenic of 2.5mm
Grain 895.2g, the high purity arsenic weighing granule is equably laid in high purity graphite crucible boat bottom, high-purity zinc ingot metal is directly covered
Cover above high purity arsenic granule, then put into high purity graphite crucible boat in flat mouth quartz ampoule；
(4) will be equipped with high purity arsenic granule using vacuum pump set and the flat mouth quartz ampoule of high-purity zinc ingot metal is evacuated to 6.4 × 10- 3Pa, then carries out elevated-temperature seal using oxyhydrogen flame to the flat mouth quartz mouth of pipe；
(5) the flat mouth quartz ampoule after tube sealing is put into constant temperature section length in the horizontal synthetic furnace of 120cm, by program control
Intensification heating process processed, is rapidly heated to 550 DEG C with the speed of 15 DEG C/min, constant temperature 120min, then with the speed of 6 DEG C/min
It is warming up to 810 DEG C, constant temperature 90min, subsequently it is warming up to 1050 DEG C with the speed of 6 DEG C/min, constant temperature 60min, closes heating afterwards
And make horizontal synthetic furnace Temperature fall；
(6) after room temperature is down to by horizontal synthetic furnace, take out and knock open flat mouth quartz ampoule, that is, obtain in high purity graphite crucible boat
Reaction completely, uniformly, no layering, the no high-quality of dephasign, high-purity 5n bis- arsenicization three zinc 2050.8g, product yield is 99.2%.
Finally provide the detection process of two arsenicization three zinc and the testing result based on the synthesis of embodiment 1-3.
Using icp mses (icp-ms), product is detected that (manufacturer is pe company, model
For: drc-ii), the testing conditions of this equipment are: temperature is 18～28 DEG C, and relative humidity is 30～70%, and cleanliness factor is 1000
Level.The detection mode of icp mses (icp-ms) is: element to be measured through plasma high-temperature ionization after,
Mass analyzer is entered with positive charge form, according to the difference of mass/charge ratio, is received by detector, produce signal.By treating
Survey the signal of element generation and the ratio of the signal of this elemental standards material generation draws constituent content to be measured.
Table 1 gives the defects inspecting result of embodiment 1-3, as known from Table 1, the preparation side of two arsenicization three zinc of the present invention
Method significantly reduces the content of free arsenic, zinc and two zinc arsenides, and product purity reaches more than 5n.
The defects inspecting result (unit: ppm) of table 1 embodiment 1-3
Claims (10)
1. a kind of preparation method of two arsenicization three zinc is it is characterised in that include step:
(1) the high purity arsenic granule of corresponding weight and high-purity zinc ingot metal are weighed by arsenic in two arsenicization three zinc and the mol ratio of zinc, will
The uniform shakedown of high purity arsenic granule claiming is sprinkled upon in a crucible boat, covers on high purity arsenic granule by high-purity zinc ingot metal afterwards, then
Crucible boat level is put in flat mouth quartz ampoule；
(2) will be equipped with high purity arsenic granule using vacuum pump set and the flat mouth quartz ampoule of high-purity zinc ingot metal is evacuated to 10-2Below pa, so
Using oxyhydrogen flame, elevated-temperature seal is carried out to the flat mouth quartz mouth of pipe afterwards；
(3) the flat mouth quartz ampoule after sealing is put in horizontal synthetic furnace, be warming up to 470 with the heating rate of 8～15 DEG C/min
～550 DEG C and be incubated 90～150min, afterwards with the heating rate of 5～7 DEG C/min be warming up to 780～850 DEG C and be incubated 60～
120min, is then warming up to 1050～1150 DEG C with the heating rate of 6～8.5 DEG C/min and is incubated 15～60min, subsequently stops
Heat and make horizontal synthetic furnace Temperature fall；
(4) after room temperature is down to by horizontal synthetic furnace, take out and knock open flat mouth quartz ampoule, that is, obtain high-purity two arsenicization three zinc crystallization
Body.
2. the preparation method of two arsenicization three zinc according to claim 1 it is characterised in that in step (1), covers in height
The set-up procedure of the high-purity zinc ingot metal on pure arsenic granule is:
A another crucible boat that () will be equipped with high purity zinc is placed in bistrique quartz ampoule and is filled with protective gas into bistrique quartz ampoule,
Again bistrique quartz ampoule level is put in horizontal heating furnace, afterwards horizontal heating furnace is heated to 455～550 DEG C and is incubated
30～60min, is then turned off horizontal heating furnace and makes the high purity zinc in this crucible boat cool to room temperature with the furnace forming high-purity zinc ingot metal；
B () is opened bistrique quartz ampoule and is taken out the high-purity zinc ingot metal dilute hydrochloric acid of cooling and soak a period of time, and with deionization
Water rinses rear vacuum drying well, weighs the weight of high-purity zinc ingot metal.
3. the preparation method of two arsenicization three zinc according to claim 2 it is characterised in that in step (a)., high purity zinc
Purity be 5n and more than, the purity of high-purity zinc ingot metal is 5～6n.
4. the preparation method of two arsenicization three zinc according to claim 2 it is characterised in that in step (a)., protective gas
For nitrogen or noble gases.
5. it is characterised in that in step (a)., crucible boat is the preparation method of two arsenicization three zinc according to claim 2
4n and above high purity graphite crucible boat or zirconium oxide crucible boat.
6. the preparation method of two arsenicization three zinc according to claim 2 it is characterised in that in step (b), high-purity zinc ingot metal
The time soaked in dilute hydrochloric acid is 2～5min.
7. it is characterised in that in step (1), crucible boat is the preparation method of two arsenicization three zinc according to claim 1
4n and above high purity graphite crucible boat or zirconium oxide crucible boat.
8. the preparation method of two arsenicization three zinc according to claim 1 it is characterised in that in step (1), high purity arsenic
Grain purity be 5n and more than.
9. the preparation method of two arsenicization three zinc according to claim 1 it is characterised in that in step (1), high purity arsenic
The granularity of grain is 0.5～5mm.
10. the preparation method of two arsenicization three zinc according to claim 1 is it is characterised in that in step (2), vacuum
For 1.0 × 10-3～9 × 10-3pa.
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| CN201410118048.2A CN104944468B (en) | 2014-03-26 | 2014-03-26 | Preparation method for zinc arsenide |
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| CN106082326A (en) * | 2016-06-08 | 2016-11-09 | 云南锡业集团（控股）有限责任公司研究设计院 | A kind of equipment producing zinc arsenide |
| CN108101007B (en) * | 2018-02-28 | 2019-11-19 | 广东先导稀贵金属材料有限公司 | The method for preparing zinc telluridse |
| CN113233430B (en) * | 2021-04-16 | 2022-09-06 | 先导薄膜材料（广东）有限公司 | Preparation method of high-purity arsenic telluride |
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| US4240826A (en) * | 1979-09-13 | 1980-12-23 | Texasgulf Inc. | Process for the recovery of arsenic as a zinc arsenate and its _utilization in the purification of zinc plant electrolytes |
| CN101857270A (en) * | 2010-07-22 | 2010-10-13 | 武峰 | Method for synthesizing high-purity arsine |
| CN102786089B (en) * | 2012-07-18 | 2014-05-14 | 云南锡业集团有限责任公司研究设计院 | Production method of zinc arsenide |
| CN103130274B (en) * | 2013-03-06 | 2014-11-05 | 昆明理工大学 | Method for preparing zinc arsenide by vapor-phase synthesis |
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