A kind of preparation method of cuprous telluride
Technical field
The present invention relates to materials synthesis field more particularly to a kind of preparation methods of cuprous telluride.
Background technology
Cuprous telluride (Cu2Te it is) a kind of black-and-blue octahedral crystal, relative density 7.27, about 900 DEG C of fusing point.Its is molten
In bromine water, but not soluble in water, hydrochloric acid and sulfuric acid.This semi-conducting material because with unique ionic conductivity and pyroelectricity, from
And it is widely used in area of solar cell.Therefore, the preparation process for developing cuprous telluride is for cuprous telluride in following hair
Exhibition plays the role of critically important.
Disclosed cuprous telluride is protected in crucible coated with sodium chloride and potassium chloride by cathode copper and pure tellurium in the prior art
Sheath fusing is made.Due to needing to use sodium chloride and potassium chloride in preparation method as protective layer, thus, final tellurium obtained
Change it is cuprous in be inevitably mixed with content more sodium and potassium, and then influence the purity of cuprous telluride product so that telluride is sub-
Copper it is second-rate.Meanwhile this method needs could be completed at high temperature under high pressure, need using complicated and expensive equipment,
It is complicated for operation to the more demanding of equipment, it is with high costs.
Invention content
In view of this, the technical problem to be solved in the present invention is to provide a kind of preparation method of cuprous telluride, by this
Cuprous telluride quality prepared by method is more excellent, and purity is higher.
The present invention provides a kind of preparation methods of cuprous telluride, include the following steps:
Elemental copper and simple substance tellurium are mixed, reaction is heated under conditions of vacuum, obtains cuprous telluride.
Preferably, the elemental copper and the molar ratio of the simple substance tellurium are 2:1.
Preferably, the vacuum degree of the vacuum is 1 × 10-3Pa~1 × 10-2Pa。
Preferably, the heating reaction carries out in the quartz ampoule for being coated with carbon film.
Preferably, the mode of heating of the heating reaction is three-stage gradient-heated.
Preferably, the three-stage gradient-heated is:
A 400 DEG C~550 DEG C) are heated to, keeps the temperature 1h~2h;
B 850 DEG C~950 DEG C) are heated to, keeps the temperature 1h~3h;
C 1100 DEG C~1180 DEG C) are heated to, keeps the temperature 2h~4h.
Preferably,
Step A) in, the heating rate of the heating is 5 DEG C/min~10 DEG C/min;
Step B) in, the heating rate of the heating is 3 DEG C/min~6 DEG C/min;
Step C) in, the heating rate of the heating is 3 DEG C/min~6 DEG C/min.
Preferably, 1100 DEG C~1180 DEG C obtained material mixings are heated to described, time of the mixing for 2h~
4h。
Preferably, the mode of the mixing is swung left and right for vertical 60 degree.
Preferably, after the heating reaction, cooling is further included.
The present invention provides a kind of preparation methods of cuprous telluride, include the following steps:Elemental copper and simple substance tellurium are mixed,
Reaction is heated under conditions of vacuum, obtains cuprous telluride.The raw material components that preparation method disclosed by the invention is used are less,
After being added to elemental copper and simple substance tellurium, without additionally adding other raw materials again, without high pressure, it is possible to cuprous telluride is made, and
Cuprous telluride quality obtained is more excellent, and purity is higher.Meanwhile preparation method is simple and practicable, is set without complicated and expensive
Standby, manufacturing cost is relatively low.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's all other embodiments obtained without making creative work, belong to this hair
The range of bright protection.
The present invention provides a kind of preparation methods of cuprous telluride, include the following steps:
Elemental copper and simple substance tellurium are mixed, reaction is heated under conditions of vacuum, obtains cuprous telluride.
The present invention has no the source of the elemental copper and simple substance tellurium special limitation, can be general commercially available.The present invention
Special limitation is had no to the purity of the elemental copper and simple substance tellurium, is purity well known to those skilled in the art.This hair
The simple substance tellurium that the elemental copper and purity that purity is 5N bright preferably is 5N.The elemental copper can be blocky or granular, the list
Matter tellurium can be blocky, granular or powdery.The elemental copper and the molar ratio of the simple substance tellurium are preferably 2:1.
After elemental copper and simple substance tellurium are mixed, reaction is heated under conditions of vacuum.The present invention is preferably by elemental copper and list
After the mixing of matter tellurium, under conditions of vacuum, reaction is heated in closed environment.
Heating reaction disclosed by the invention need not be carried out in high pressure, thus, without complicated and expensive equipment, prepare
Cost is relatively low, meanwhile, method is simple and practicable.The vacuum degree of the vacuum is preferably 1 × 10-3Pa~1 × 10-2Pa;In the present invention
Some embodiments in, the vacuum degree of the vacuum is 1 × 10-3Pa、2×10-3Pa、5×10-3Pa or 1 × 10-2Pa。
The heating reaction carries out preferably in the quartz ampoule for being coated with film.The present invention has no the film special limitation,
As long as being not involved in reaction in the heating reaction, the present invention is preferably one kind in carbon film, boron nitride film or platinum film, is examined
Consider economical and practical, more preferably carbon film.The present invention has no special limitation to the heating equipment of the heating reaction, using this
Heating equipment known to field technology personnel, the present invention are preferably heating furnace.
The mode of heating of the heating reaction is preferably three-stage gradient-heated.Preferably, the three-stage gradient-heated
Specially:
A the first temperature) is heated to, keeps the temperature 1h~2h;
B second temperature) is heated to, keeps the temperature 1h~3h;
C third temperature) is heated to, keeps the temperature 2h~4h.
In step A) in, first temperature is 400 DEG C~550 DEG C;In certain embodiments of the present invention, described first
Temperature is 400 DEG C, 500 DEG C or 550 DEG C.Soaking time at a temperature of described first is 1h~2h;In certain implementations of the present invention
In example, the soaking time is 1h, 1.5h or 2h.The heating rate of the heating is preferably 5 DEG C/min~10 DEG C/min;At this
In some embodiments of invention, the heating rate of the heating is 5 DEG C/min, 8 DEG C/min, 9 DEG C/min or 10 DEG C/min.
In step B) in, the second temperature is 850 DEG C~950 DEG C;In certain embodiments of the present invention, described second
Temperature is 850 DEG C, 900 DEG C, 920 DEG C or 950 DEG C.Soaking time under the second temperature is 1h~3h;In certain of the present invention
In a little embodiments, the soaking time is 1h or 2h.The heating rate of the heating is preferably 3 DEG C/min~6 DEG C/min;At this
In some embodiments of invention, the heating rate of the heating is 3 DEG C/min, 4 DEG C/min or 5 DEG C/min.
In step C) in, the third temperature is 1100 DEG C~1180 DEG C;In certain embodiments of the present invention, described
Three temperature are 1120 DEG C, 1130 DEG C, 1150 DEG C or 1180 DEG C.Soaking time at a temperature of the third is 2h~4h;In this hair
In bright some embodiments, the soaking time is 2.5h or 3h.The heating rate of the heating be preferably 3 DEG C/min~6 DEG C/
min;In certain embodiments of the present invention, the heating rate of the heating for 3 DEG C/min, 4 DEG C/min or 5 DEG C/min.
The material mixing that when being heated to third temperature, will be obtained, the time of the mixing at a temperature of the third
Soaking time it is identical, the present invention be preferably 2h~4h, more preferably 2.5h~3h.The mode of the mixing is preferably vertical 60
Degree is swung left and right.
After the completion of above-mentioned heating reaction, cooling is preferably further included, obtains cuprous telluride.Preferably, described cool down is specially:
Product obtained by the reaction is heated to cool down with the equipment of heating reaction.The present invention has no the mode of the cooling special limit
System, using the type of cooling well known to those skilled in the art, the present invention is preferably natural cooling.The temperature of the cooling is excellent
35 DEG C are selected as hereinafter, more preferably 25~35 DEG C.
After the cooling, discharging is preferably further included, so as to obtain cuprous telluride.
The present invention provides a kind of preparation methods of cuprous telluride, include the following steps:Elemental copper and simple substance tellurium are mixed,
Reaction is heated under conditions of vacuum, obtains cuprous telluride.The raw material components that preparation method disclosed by the invention is used are less,
After being added to elemental copper and simple substance tellurium, without additionally adding other raw materials again, without high pressure, it is possible to cuprous telluride is made, and
Cuprous telluride quality obtained is more excellent, and purity is higher.Meanwhile preparation method is simple and practicable, is set without complicated and expensive
Standby, manufacturing cost is relatively low.
In order to further illustrate the present invention, with reference to embodiments to a kind of preparation side of cuprous telluride provided by the invention
Method is described in detail, but cannot be understood as limiting the scope of the present invention.
Embodiment 1
By the tellurium block of the copper particle of 5N and 5N in molar ratio 2:1 dispensing 1kg, is fitted into the quartz ampoule for being coated with carbon film, will be quartzy
Pipe vacuumizes, until vacuum degree is 1 × 10-3After Pa, tube sealing.Quartz ampoule after sealing is placed in heating furnace, with 5 DEG C/min's
Rate is warming up to 500 DEG C, keeps the temperature 1h;920 DEG C are warming up to the rate of 3 DEG C/min again, keeps the temperature 2h;Then with the speed of 3 DEG C/min
Rate is warming up to 1120 DEG C, keeps the temperature 3h.It, will be in quartz ampoule using vertical 60 degree of wiggly modes when temperature rises to 1120 DEG C
Material mixing, time of the mixing is 3h.Later, after the temperature of furnace chamber being naturally cooled to 25~35 DEG C, discharging obtains
Cuprous telluride.
Embodiment 2
By the tellurium block of the copper particle of 5N and 5N in molar ratio 2:1 dispensing 1.5kg, is fitted into the quartz ampoule for being coated with carbon film, by stone
English pipe vacuumizes, until vacuum degree is 5 × 10-3After Pa, tube sealing.Quartz ampoule after sealing is placed in heating furnace, with 8 DEG C/min
Rate be warming up to 500 DEG C, keep the temperature 1h;900 DEG C are warming up to the rate of 4 DEG C/min again, keeps the temperature 1h;Then with 3 DEG C/min's
Rate is warming up to 1150 DEG C, keeps the temperature 3h.When temperature rises to 1150 DEG C, using vertical 60 degree of wiggly modes by quartz ampoule
In material mixing, time of the mixing is 3h.Later, after the temperature of furnace chamber being naturally cooled to 25~35 DEG C, discharging obtains
To cuprous telluride.
Embodiment 3
By the tellurium block of the copper particle of 5N and 5N in molar ratio 2:1 dispensing 2kg, is fitted into the quartz ampoule for being coated with carbon film, will be quartzy
Pipe vacuumizes, until vacuum degree is 2 × 10-3After Pa, tube sealing.Quartz ampoule after sealing is placed in heating furnace, with 10 DEG C/min
Rate be warming up to 500 DEG C, keep the temperature 1h;920 DEG C are warming up to the rate of 3 DEG C/min again, keeps the temperature 1h;Then with 4 DEG C/min's
Rate is warming up to 1130 DEG C, keeps the temperature 3h.When temperature rises to 1130 DEG C, using vertical 60 degree of wiggly modes by quartz ampoule
In material mixing, time of the mixing is 3h.Later, after the temperature of furnace chamber being naturally cooled to 25~35 DEG C, discharging obtains
To cuprous telluride.
Embodiment 4
By the tellurium block of the copper particle of 5N and 5N in molar ratio 2:1 dispensing 2kg, is fitted into the quartz ampoule for being coated with boron nitride film, will
Quartz ampoule vacuumizes, until vacuum degree is 1 × 10-3After Pa, tube sealing.Quartz ampoule after sealing is placed in heating furnace, with 5 DEG C/
The rate of min is warming up to 550 DEG C, keeps the temperature 1.5h;850 DEG C are warming up to the rate of 3 DEG C/min again, keeps the temperature 2h;Then with 5 DEG C/
The rate of min is warming up to 1180 DEG C, keeps the temperature 3h.It, will using vertical 60 degree wiggly modes when temperature rises to 1180 DEG C
Material mixing in quartz ampoule, the time of the mixing is 3h.Later, after the temperature of furnace chamber being naturally cooled to 25~35 DEG C,
Discharging, obtains cuprous telluride.
Embodiment 5
By the tellurium block of the copper particle of 5N and 5N in molar ratio 2:1 dispensing 1.5kg, is fitted into the quartz ampoule for being coated with platinum film, by stone
English pipe vacuumizes, until vacuum degree is 1 × 10-2After Pa, tube sealing.Quartz ampoule after sealing is placed in heating furnace, with 9 DEG C/min
Rate be warming up to 400 DEG C, keep the temperature 2h;950 DEG C are warming up to the rate of 5 DEG C/min again, keeps the temperature 1h;Then with 5 DEG C/min's
Rate is warming up to 1180 DEG C, keeps the temperature 2.5h.It, will be quartzy using vertical 60 degree of wiggly modes when temperature rises to 1180 DEG C
Material mixing in pipe, the time of the mixing is 2.5h.Later, after the temperature of furnace chamber being naturally cooled to 25~35 DEG C, go out
Material, obtains cuprous telluride.
Embodiment 6
The purity of cuprous telluride that Examples 1 to 5 obtains is detected:
Using icp ms (ICP-MS, manufacturer be PE companies, model DRC-II) carry out
Detection, the condition of the detection of the equipment are:Temperature is 18 DEG C~28 DEG C, and relative humidity is 30%~70%, cleanliness factor 1000
Grade.Icp ms detection mode:Element to be measured is after plasma high-temperature ionizes, in the form of positive charge
Into mass analyzer, according to mass/charge than difference, received by detector, generate signal.The signal that element to be measured generates
The elemental signals ratio obtains constituent content to be measured with standard substance.Testing result is shown in Table 1.
The impurity and its content (unit that the cuprous telluride that 1 Examples 1 to 5 of table obtains contains:ppm)
As it can be seen from table 1 dopant species and content contained in cuprous telluride prepared by Examples 1 to 5 are less, it is pure
Degree is higher, in more than 5N.
The explanation of above example is only intended to facilitate the understanding of the method and its core concept of the invention.To these embodiments
A variety of modifications will be apparent for 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 the most wide model consistent with the principles and novel features disclosed herein
It encloses.