CN107858545B - Dissociate the minimizing technology of tellurium in a kind of high-melting-point telluride alloy - Google Patents
Dissociate the minimizing technology of tellurium in a kind of high-melting-point telluride alloy Download PDFInfo
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- CN107858545B CN107858545B CN201711273933.8A CN201711273933A CN107858545B CN 107858545 B CN107858545 B CN 107858545B CN 201711273933 A CN201711273933 A CN 201711273933A CN 107858545 B CN107858545 B CN 107858545B
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
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Abstract
The present invention provides a kind of minimizing technologies for the tellurium that dissociates in high-melting-point telluride alloy, by the heating of specific temperature twice and the heat preservation of certain time, well to separate free tellurium from high-melting-point telluride alloy under certain vacuum degree.Compared with prior art, minimizing technology of the invention is simple and easy, is not necessarily to waste a large amount of hydrogen in operation, is effectively saved resource, meanwhile, the mechanical performance of obtained high-melting-point telluride alloy is more excellent.In addition, the free tellurium separated can be collected by setting condensation and collection facility, it is effectively guaranteed the recycling of resource, reduces pollution.It is more than 95% that experiment, which shows to make using minimizing technology disclosed by the invention the removal rate of free tellurium in high-melting-point telluride alloy,.
Description
Technical field
The present invention relates to from the technical field more particularly to a kind of high-melting-point telluride alloy for removing free tellurium in material
The minimizing technology of free tellurium.
Background technique
Tellurium, chemical symbol Te are a kind of argenteous metals, and chemical property is similar with selenium and sulphur, is mainly used as alloy
Level semiconductor.Tellurium can generate telluride alloy with many element compounds, and purposes is very extensive, such as cadmium telluride alloy, zinc telluridse
Alloy etc. is largely used to solar energy film material, and telluride bismuth alloy is a kind of good thermoelectric material.These telluride alloys
It is general at present to be prepared using the method for high―temperature nuclei, during this, largely free tellurium is inevitably generated, significantly
Reduce the performance of material.
Currently, solution to the problems described above is mainly the process in logical hydrogen reducing deoxygenation while removing tellurium, but in this way
Need to waste a large amount of hydrogen, simultaneously as restoring deoxygenation and except the temperature of tellurium is different, thus, operation temperature is not easy to control,
Except tellurium effect is poor, the mechanical performance of telluride alloy is also highly susceptible to influence.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing the tellurium that dissociates in a kind of high-melting-point telluride alloy
Minimizing technology, this minimizing technology is more excellent except tellurium effect, and the mechanical performance of obtained high-melting-point telluride alloy is more excellent, meanwhile,
Operation is simple, is effectively saved resource.
The present invention provides a kind of minimizing technologies for the tellurium that dissociates in high-melting-point telluride alloy, comprising:
A high-melting-point telluride alloy) is heated to 300~600 DEG C, keeps the temperature 2~5h, the product after being heat-treated；
B the product after the heat treatment) is heated to 800~950 DEG C, 7~12h is kept the temperature, obtains after removing free tellurium
High-melting-point telluride alloy；
The step A) and step B) carried out under conditions of vacuum, the vacuum degree of the vacuum is less than 0.5Pa.
Preferably, before the heating by high-melting-point telluride alloy further include: carry out the high-melting-point telluride alloy
It is broken.
Preferably, the broken powder granularity is less than 70 mesh.
Preferably, step A) in, the heating rate of the heating is 2~10 DEG C/min.
Preferably, step B) in, the heating rate of the heating is 3~8 DEG C/min.
Preferably, step A) in, high-melting-point telluride alloy is heated to 500 DEG C, keeps the temperature 3h, the production after being heat-treated
Object.
Preferably, step B) in, the product after the heat treatment is heated to 900 DEG C, keeps the temperature 12h, it is free to obtain removal
High-melting-point telluride alloy after tellurium.
Preferably, step B) in, it further include cooling after the heat preservation.
Preferably, the temperature after the cooling is less than 30 DEG C.
The present invention provides a kind of minimizing technologies for the tellurium that dissociates in high-melting-point telluride alloy, comprising:
A high-melting-point telluride alloy) is heated to 300~600 DEG C, keeps the temperature 2~5h, the product after being heat-treated；
B the product after the heat treatment) is heated to 800~950 DEG C, 7~12h is kept the temperature, obtains after removing free tellurium
High-melting-point telluride alloy；
The step A) and step B) carried out under conditions of vacuum, the vacuum degree of the vacuum is less than 0.5Pa.
The present invention is under conditions of certain vacuum degree, by the heating of specific temperature twice and the heat preservation of certain time, very
Free tellurium is separated from high-melting-point telluride alloy well, meanwhile, the mechanicalness of obtained high-melting-point telluride alloy
It can be more excellent.Compared with prior art, minimizing technology of the invention is simple and easy, without wasting a large amount of hydrogen in operation, effectively
Resource is saved.In addition, the free tellurium separated can be collected by setting condensation and collection facility, effectively guarantee
The recycling of resource, reduces pollution.
The experimental results showed that can to dissociate in high-melting-point telluride alloy using minimizing technology disclosed by the invention
The removal rate of tellurium is more than 95%.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
The present invention provides a kind of minimizing technologies for the tellurium that dissociates in high-melting-point telluride alloy, comprising:
A high-melting-point telluride alloy) is heated to 300~600 DEG C, keeps the temperature 2~5h, the product after being heat-treated；
B the product after the heat treatment) is heated to 800~950 DEG C, 7~12h is kept the temperature, obtains after removing free tellurium
High-melting-point telluride alloy；
The step A) and step B) carried out under conditions of vacuum, the vacuum degree of the vacuum is less than 0.5Pa.
The present invention has no special limitation to the high-melting-point telluride alloy, can be the common high-melting-point tellurium in this field
Compound alloy.In certain embodiments of the present invention, the high-melting-point telluride alloy be telluride kirsite, cadmium telluride alloy or
Cuprous telluride alloy.The present invention has no special limitation to the source of the high-melting-point telluride alloy, and can make by oneself can also be with
It is general commercially available.In certain embodiments of the present invention, the source of the high-melting-point telluride alloy is general commercially available.
After obtaining high-melting-point telluride alloy, the high-melting-point telluride alloy is preferably crushed by the present invention.This hair
It is bright that special limitation is had no to the broken method and apparatus, using broken method well known to those skilled in the art and set
It is standby.In the present invention, the broken equipment is preferably tertiary crusher.The broken powder granularity is preferably smaller than
70 mesh.
Then, under conditions of vacuum, the high-melting-point telluride alloy is subjected to first time heat treatment.The first time
Heat treatment specifically: the high-melting-point telluride alloy is heated to 300~600 DEG C, keeps the temperature 2~5h, is obtained at heat for the first time
Product after reason.The vacuum degree of the vacuum is less than 0.5Pa.
The temperature of the heating is 300~600 DEG C.In certain embodiments of the present invention, the temperature of the heating is 600
DEG C, 500 DEG C or 350 DEG C.The time of the heat preservation is 2~5h.In certain embodiments of the present invention, the time of the heat preservation is
2h, 3h or 5h.Under certain vacuum condition, the first time of first time heating and certain time by specific temperature is kept the temperature,
It can effectively remove with the tellurium that dissociates existing for simple substance tellurium in high-melting-point telluride alloy, and to raising high-melting-point telluride alloy
Mechanical performance plays facilitation.
The heating rate of above-mentioned heating is preferably 2~10 DEG C/min.In certain embodiments of the present invention, the heating
Heating rate is 10 DEG C/min or 5 DEG C/min.The present invention is controlled and is heated in material by further controlling heating rate
The outer temperature difference has facilitation for removing the free tellurium in high-melting-point telluride alloy, meanwhile, high-melting-point tellurides will be closed
The influence of the mechanical performance of gold reduces as much as possible.
After product after being heat-treated, under conditions of vacuum, the product after first time heat treatment is carried out the
Secondary heat treatment.Second of the heat treatment specifically: the product after first time heat treatment is heated to 800~950 DEG C,
7~12h is kept the temperature, obtains removing the high-melting-point telluride alloy after free tellurium.The vacuum degree of the vacuum is less than 0.5Pa.
The temperature of the heating is 800~950 DEG C.In certain embodiments of the present invention, the temperature of the heating is 950
DEG C, 900 DEG C or 800 DEG C.The time of the heat preservation is 7~12h.In certain embodiments of the present invention, the time of the heat preservation
For 7h, 12h or 10h.Second of heating and second of guarantor of certain time under certain vacuum condition, by specific temperature
Temperature can be removed effectively with the tellurium that dissociates existing for other miscellaneous phases in high-melting-point telluride alloy, and to raising high-melting-point tellurides
The mechanical performance of alloy plays facilitation.
In the present invention, the heating rate of the heating is preferably 3~8 DEG C/min.In certain embodiments of the present invention,
The heating rate of the heating is 3 DEG C/min, 5 DEG C/min or 8 DEG C/min.The present invention, which passes through, further controls heating rate, into
And control and be heated the temperature difference of material inside and outside, there is facilitation for removing the free tellurium in high-melting-point telluride alloy, meanwhile,
The influence of mechanical performance to high-melting-point telluride alloy is reduced as much as possible.
After 7~12h of the heat preservation, it is also preferable to include coolings.The present invention has no special limitation to the method for the cooling,
Using the method for cooling well known to those skilled in the art, the present invention is preferably natural cooling.Temperature after the cooling
Preferably smaller than 30 DEG C.
The present invention has no special limitation to the equipment of first time heat treatment and second of the heat treatment, preferably exists
It is carried out in heating furnace.
The present invention has no special limitation to the source of above-mentioned used raw material components, can be general commercially available.
After high-melting-point telluride alloy after obtaining removing free tellurium, the present invention uses differential scanning calorimeter, according to GB/
T 22232-2008 " thermostabilization of chemical substance measures differential scanning calorimetry ", before and after measurement removes free tellurium, high-melting-point tellurium
The content of free tellurium in compound alloy.
The experimental results showed that can to dissociate in high-melting-point telluride alloy using minimizing technology disclosed by the invention
The removal rate of tellurium is more than 95%.
The present invention provides a kind of minimizing technologies for the tellurium that dissociates in high-melting-point telluride alloy, comprising:
A high-melting-point telluride alloy) is heated to 300~600 DEG C, keeps the temperature 2~5h, the product after being heat-treated；
B the product after the heat treatment) is heated to 800~950 DEG C, 7~12h is kept the temperature, obtains after removing free tellurium
High-melting-point telluride alloy；
The step A) and step B) carried out under conditions of vacuum, the vacuum degree of the vacuum is less than 0.5Pa.
The present invention is under conditions of certain vacuum degree, by the heating of specific temperature twice and the heat preservation of certain time, very
Free tellurium is separated from high-melting-point telluride alloy well, meanwhile, the mechanicalness of obtained high-melting-point telluride alloy
It can be more excellent.Compared with prior art, minimizing technology of the invention is simple and easy, without wasting a large amount of hydrogen in operation, effectively
Resource is saved.In addition, the free tellurium separated can be collected by setting condensation and collection facility, effectively guarantee
The recycling of resource, reduces pollution.
The experimental results showed that can to dissociate in high-melting-point telluride alloy using minimizing technology disclosed by the invention
The removal rate of tellurium is more than 95%.
In order to further illustrate the present invention, below with reference to embodiment to a kind of high-melting-point telluride alloy provided by the invention
In the dissociate minimizing technology of tellurium be described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Raw material used in following embodiment is commercially available.
Embodiment 1
By tertiary crusher, by zinc telluridse alloy breaks down at the powder less than 50 mesh.Take the telluride kirsite being crushed
Powder is put into quartz boat, is put into heating furnace, is vacuumized less than 0.5pa.Then 600 DEG C of heat preservations are warming up to 10 DEG C/min
2h.950 DEG C of heat preservation 7h are warming up to 3 DEG C/min again.Stop heating, when temperature is naturally cooled to less than 30 DEG C, comes out of the stove, closed
The telluride kirsite of lattice.
Embodiment 2
By tertiary crusher, cadmium telluride alloy is broken into the powder less than 50 mesh.Take the cadmium telluride alloy being crushed
Powder is put into quartz boat, is put into heating furnace, is vacuumized less than 0.5pa.Then 600 DEG C of heat preservations are warming up to 10 DEG C/min
2h.950 DEG C of heat preservation 7h are warming up to 3 DEG C/min again.Stop heating, when temperature is naturally cooled to less than 30 DEG C, comes out of the stove, closed
The cadmium telluride alloy of lattice.
Embodiment 3
By tertiary crusher, by cuprous telluride alloy breaks down at the powder less than 50 mesh.Take the cuprous telluride being crushed
Alloy powder is put into quartz boat, is put into heating furnace, is vacuumized less than 0.5pa.Then 600 DEG C of guarantors are warming up to 10 DEG C/min
Warm 2h.950 DEG C of heat preservation 7h are warming up to 3 DEG C/min again.Stop heating, when temperature is naturally cooled to less than 30 DEG C, comes out of the stove, obtain
Qualified cuprous telluride alloy.
Embodiment 4
The present invention uses differential scanning calorimeter, and according to GB/T 22232-2008, " thermostabilization of chemical substance measures differential
Scanning calorimetry ", measure the content of the free tellurium before and after removing free tellurium in Examples 1 to 3 in high-melting-point telluride alloy.Knot
Fruit is as shown in table 1.
The content and removal rate of the free tellurium in the high-melting-point telluride alloy of free tellurium front and back are removed in 1 Examples 1 to 3 of table
From table 1 it follows that high-melting-point telluride alloy middle reaches can be made using minimizing technology disclosed by the invention
Removal rate from tellurium is more than 95%.
Embodiment 5
Using using the impurity for removing free tellurium front and back high-melting-point telluride alloy in ICP-OE method detection Examples 1 to 3
Content.The results are shown in Table 2.
The impurity content of free tellurium front and back high-melting-point telluride alloy is removed in 2 Examples 1 to 3 of table
From Table 2, it can be seen that comparing the impurity content for removing free tellurium front and back high-melting-point telluride alloy, Ke Yifa
Existing, before and after removing free tellurium, the impurity content of high-melting-point telluride alloy is hardly affected.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.To these embodiments
A variety of modifications will be readily apparent to those skilled in the art, the general principles defined herein can be with
Without departing from the spirit or scope of the present invention, it realizes in other embodiments.Therefore, the present invention will not be limited
In the embodiments shown herein, and it is to fit to widest model consistent with the principles and novel features disclosed in this article
It encloses.
Claims (7)
1. a kind of minimizing technology for the tellurium that dissociates in high-melting-point telluride alloy, comprises the steps of:
A) high-melting-point telluride alloy is crushed, is heated to 300~600 DEG C, keeps the temperature 2~5h, the production after being heat-treated
Object；The high-melting-point telluride alloy is telluride kirsite, cadmium telluride alloy or cuprous telluride alloy；
B the product after the heat treatment) is heated to 800~950 DEG C, after keeping the temperature 7~12h, cooling is obtained after removing free tellurium
High-melting-point telluride alloy；
The step A) and step B) carried out under conditions of vacuum, the vacuum degree of the vacuum is less than 0.5Pa.
2. minimizing technology according to claim 1, which is characterized in that the broken powder granularity is less than 70 mesh.
3. minimizing technology according to claim 1, which is characterized in that step A) in, the heating rate of the heating is 2~
10℃/min。
4. minimizing technology according to claim 1, which is characterized in that step B) in, the heating rate of the heating is 3~
8℃/min。
5. minimizing technology described in any one according to claim 1~4, which is characterized in that step A) in, by high-melting-point telluride
Object alloy is heated to 500 DEG C, keeps the temperature 3h, the product after being heat-treated.
6. minimizing technology described in any one according to claim 1~4, which is characterized in that step B) in, by the heat treatment
Product afterwards is heated to 900 DEG C, keeps the temperature 12h, obtains removing the high-melting-point telluride alloy after free tellurium.
7. minimizing technology according to claim 1, which is characterized in that the temperature after the cooling is less than 30 DEG C.
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| CN110144458A (en) * | 2019-04-09 | 2019-08-20 | 紫金矿业集团股份有限公司 | A method of vacuum distillation cuprous telluride slag separating-purifying tellurium |
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| CN101125679A (en) * | 2007-08-31 | 2008-02-20 | 侯仁义 | Method for preparing highly pure cadmium telluride |
| CN102286741A (en) * | 2011-09-02 | 2011-12-21 | 南京大学 | Method for preparing cadmium telluride film |
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Application publication date: 20180330 Assignee: Pilot film materials Co.,Ltd. Assignor: Leading film materials (Guangdong) Co.,Ltd. Contract record no.: X2021440000141 Denomination of invention: A method for removing free tellurium from high melting point telluride alloy Granted publication date: 20190830 License type: Common License Record date: 20210730 |
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