CN103274372B - Cadmium tellude preparation method - Google Patents
Cadmium tellude preparation method Download PDFInfo
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- CN103274372B CN103274372B CN201310241279.8A CN201310241279A CN103274372B CN 103274372 B CN103274372 B CN 103274372B CN 201310241279 A CN201310241279 A CN 201310241279A CN 103274372 B CN103274372 B CN 103274372B
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Abstract
The invention provides a cadmium tellude preparation method, which comprises steps of primary synthesis and secondary synthesis. The primary synthesis comprises the steps: putting tellurium and cadmium which are arranged in a staggered and up-and-down manner into a first graphite boat in a layered manner, putting the first graphite boat in a first quartz tube, and then placing the first quartz tube in a first synthesis furnace; filling first protective gas to discharge air in the first quartz tube; conducting three-section temperature increment, filling the first protective gas into the first section, and filling a first reducing gas into the second and the third section; filling the first reducing gas after the completion of synthesis reaction, and cooling down to an room temperature; and obtaining a first synthetic product. The secondary synthesis comprises the steps: putting the first synthetic product into a second graphite boat after being crushed, placing the second graphite boat into a second quartz tube, and placing the quartz tube into a second synthesis furnace; filling a second protective gas to discharge air in the second quartz tube; conducting two-section temperature increment, filling the second protective gas into the first section, and filling a second reducing gas into the second section; and after the completion of synthesis reaction, stopping heating, filling the second reducing gas, cooling down to the room temperature, so as to obtain a second synthetic product. Due to adoption of the method provided by the invention, the raw materials can be prevented from oxidation and being in contact with poisonous substances.
Description
Technical field
The present invention relates to a kind of preparation method of synthetic materials, relate in particular to a kind of preparation method of cadmium telluride.
Background technology
The preparation method of cadmium telluride is synthetic after being mostly to adopt cadmium powder and tellurium powder to mix at present, wherein on November 20th, 2002 Granted publication Chinese patent CN1380246A a kind of preparation method of cadmium antimonide powder is disclosed, the method adopts cadmium powder and tellurium powder synthetic in the crucible of vacuum condition, synthetic after through grinding anneal; On February 20th, 2008, the Chinese patent CN101125679A of Granted publication disclosed a kind of preparation method of high-purity cadmium telluride, method is that 5N tellurium and 5N cadmium are mixed according to the proportioning of mol ratio 1:1, pellet is pulverized or ground to form to compound, present method can increase the probability of cadmium powder oxidation in mixing or grinding to form the process of pellet, also increased the probability that operator contacts cadmium powder, therefore human body is had to certain injury, if adopt cadmium powder to synthesize cadmium telluride simultaneously, wherein cadmium powder is oxidizable, and the cost compare of production cadmium powder is high; On June 16th, 2010, the Chinese patent CN101734630A of Granted publication disclosed a kind of preparation method of high-purity cadmium telluride, the method is that 5N cadmium material and 5N tellurium material are placed in the airtight silica tube after utter misery is processed, by cadmium material with tellurium material is divided into respectively N-1 part according to 1:1.1～1.15 and N part is alternately positioned in silica tube, and at first and last what place is tellurium material, after deoxidation, adopt the method for High Temperature High Pressure to synthesize, because the condition of the method is High Temperature High Pressure, therefore there is certain danger in building-up process, output is smaller, and industrialization cost compare is high.
Summary of the invention
In view of the problem that background technology exists, the object of the present invention is to provide a kind of preparation method of cadmium telluride, it can avoid raw material oxidized and avoid contacting objectionable impurities.
The object of the present invention is to provide a kind of preparation method of cadmium telluride, it can under normal pressure, carry out single sintering and secondary is synthetic.
The object of the present invention is to provide a kind of preparation method of cadmium telluride, the production cost that it can be lower.
To achieve these goals, the invention provides a kind of preparation method of cadmium telluride, it comprises single sintering step and secondary synthesis step.
Single sintering step comprises: 5N cadmium grain and 5N tellurium grain are placed in the first graphite boat from top to bottom according to the relatively low cadmium grain of fusing point from the lowest layer and the relatively high tellurium grain of fusing point for staggered minute, and wherein the lowest layer is cadmium grain; Charged the first graphite boat is positioned in the first silica tube; The first silica tube that is placed with the first graphite boat is positioned in the first synthetic furnace; Pass into the air in emptying the first silica tube of the first protective gas; After air in the first silica tube is emptying by the first protective gas, the first synthetic furnace adopts three sections of heating modes, and first paragraph passes into the first protective gas, and second segment and the 3rd section pass into the first reducing gas; After building-up reactions, the first synthetic furnace stops heating and being cooled to room temperature, continues to pass into the first reducing gas in temperature-fall period; And from the first silica tube, take out the first graphite boat, then take out single sintering thing in the first graphite boat.
Secondary synthesis step comprises: the cadmium telluride crystal grain that single sintering thing is crushed to specified dimension; The good cadmium telluride crystal grain of fragmentation is encased in the second graphite boat; The second graphite boat that broken good cadmium telluride crystal grain is housed is positioned in the second silica tube; The second silica tube that is placed with the second graphite boat is positioned in the second synthetic furnace; Pass into the air in emptying the second silica tube of the second protective gas; After air in the second silica tube is emptying by the second protective gas, the second synthetic furnace adopts two sections of heating modes, and first paragraph passes into the second protective gas, and second segment passes into the second reducing gas; After building-up reactions, the second synthetic furnace stops heating and being cooled to room temperature, continues to pass into the second reducing gas in temperature-fall period; And from the second silica tube, take out the second graphite boat, then take out secondary synthetics in the second graphite boat.
Wherein:
In described single sintering step, three sections of heating modes are: the temperature rise rate of first paragraph is 2～15 ℃/min, from room temperature, are warming up to 150～250 ℃, and insulation 1.5～5h passes into the first protective gas in first paragraph; The temperature rise rate of second segment is 2～15 ℃/min, continues to be warming up to 350～500 ℃, and insulation 10～90min passes into the first reducing gas in second segment; And the temperature rise rate of the 3rd section is 5～20 ℃/min, continue to be warming up to 850～1000 ℃, insulation 0.5～3h passes into the first reducing gas in the 3rd section;
In described secondary synthesis step, two sections of heating modes are: the temperature rise rate of first paragraph is 8～25 ℃/min, from room temperature, rise to 350～450 ℃, and insulation 10～60min passes into the second protective gas in first paragraph; And the temperature rise rate of second segment is 2～10 ℃/min, continue to be warming up to 850～1000 ℃, insulation 2～20h passes into the second reducing gas in second segment.
Beneficial effect of the present invention is as follows:
The preparation method of the cadmium telluride that the present invention adopts does not contact objectionable impurities in preparation process, has reduced the injury of cadmium grain to human body, and has reduced the oxidized probability of cadmium grain;
The method is reacted under normal pressure, and safety performance is high; Adopt in process of production cadmium grain and tellurium grain cheaply, reduced the production cost of raw material;
The cadmium telluride of preparation can access the macrocrystal that approaches chemical theory proportioning, and stable performance can meet the demand of the various granularities of client.
Embodiment
Describe preparation method and the embodiment of the cadmium telluride according to the present invention below in detail.
First preparation method according to cadmium telluride of the present invention is described.
According to the preparation method of cadmium telluride of the present invention, comprise single sintering step and secondary synthesis step.
Wherein, single sintering step comprises: 5N cadmium grain and 5N tellurium grain are placed in the first graphite boat from top to bottom according to the relatively low cadmium grain of fusing point from the lowest layer and the relatively high tellurium grain of fusing point for staggered minute, and wherein the lowest layer is cadmium grain; Charged the first graphite boat is positioned in the first silica tube; The first silica tube that is placed with the first graphite boat is positioned in the first synthetic furnace; Pass into the air in emptying the first silica tube of the first protective gas; After air in the first silica tube is emptying by the first protective gas, the first synthetic furnace adopts three sections of heating modes, and first paragraph passes into the first protective gas, and second segment and the 3rd section pass into the first reducing gas; After building-up reactions, the first synthetic furnace stops heating and being cooled to room temperature, continues to pass into the first reducing gas in temperature-fall period; And from the first silica tube, take out the first graphite boat, then take out single sintering thing in the first graphite boat.
Wherein, secondary synthesis step comprises: the cadmium telluride crystal grain that single sintering thing is crushed to specified dimension; The good cadmium telluride crystal grain of fragmentation is encased in the second graphite boat; The second graphite boat that broken good cadmium telluride crystal grain is housed is positioned in the second silica tube; The second silica tube that is placed with the second graphite boat is positioned in the second synthetic furnace; Pass into the air in emptying the second silica tube of the second protective gas; After air in the second silica tube is emptying by the second protective gas, the second synthetic furnace adopts two sections of heating modes, and first paragraph passes into the second protective gas, and second segment passes into the second reducing gas; After building-up reactions, the second synthetic furnace stops heating and being cooled to room temperature, continues to pass into the second reducing gas in temperature-fall period; And from the second silica tube, take out the second graphite boat, then take out secondary synthetics in the second graphite boat.
According in the preparation method of cadmium telluride of the present invention, preferably, in single sintering step, 5N cadmium grain is of a size of 1～10mm, and 5N tellurium grain is of a size of 1～10mm.
According in the preparation method of cadmium telluride of the present invention, preferably, in single sintering step, the blending ratio of 5N tellurium powder and 5N cadmium powder is mol ratio 1:1.
According in the preparation method of cadmium telluride of the present invention, in described single sintering step, three sections of heating modes can be: the temperature rise rate of first paragraph is 2～15 ℃/min, from room temperature, are warming up to 150～250 ℃, insulation 1.5～5h passes into the first protective gas in first paragraph; The temperature rise rate of second segment is 2～15 ℃/min, continues to be warming up to 350～500 ℃, and insulation 10～90min passes into the first reducing gas in second segment; And the temperature rise rate of the 3rd section is 5～20 ℃/min, continue to be warming up to 850～1000 ℃, insulation 0.5～3h passes into the first reducing gas in the 3rd section.
According in the preparation method of cadmium telluride of the present invention, preferably, in described secondary synthesis step, the described specified dimension by the fragmentation of single sintering thing is 1～10mm.
According in the preparation method of cadmium telluride of the present invention, in described secondary synthesis step, two sections of heating modes can be: the temperature rise rate of first paragraph is 8～25 ℃/min, from room temperature, rise to 350～450 ℃, insulation 10～60min passes into the second protective gas in first paragraph; And the temperature rise rate of second segment is 2～10 ℃/min, continue to be warming up to 850～1000 ℃, insulation 2～20h passes into the second reducing gas in second segment.
According in the preparation method of cadmium telluride of the present invention, the first graphite boat in described single sintering step before charging through Water Quenching; The second graphite boat in described secondary synthesis step is process Water Quenching before charging; In described single sintering step with described secondary synthesis step in the first protective gas and the second protective gas can be identical or different, be preferably the first protective gas and the second protective gas is nitrogen; In described single sintering step from the first reducing gas in described secondary synthesis step and the second reducing gas can just as or different, be preferably the first reducing gas and the second reducing gas is hydrogen.
According in the preparation method of cadmium telluride of the present invention, the second synthetic furnace in the first synthetic furnace in described single sintering step and described secondary synthesis step is same or different synthetic furnace; The second graphite boat in the first graphite boat in described single sintering step and described secondary synthesis step is same or different graphite boat, and when the second graphite boat in the first graphite boat in described single sintering step and described secondary synthesis step is same graphite boat, in described secondary synthesis step, before the second graphite boat is used, the second graphite boat is carried out to clean; The second silica tube in described single sintering step and the second silica tube in described secondary synthesis step are same or different silica tubes, and when the second silica tube in described single sintering step and the second silica tube in described secondary synthesis step are same silica tube, in described secondary synthesis step, before using, the second silica tube carries out clean.
According in the preparation method of cadmium telluride of the present invention, also comprise step: after obtaining secondary synthetics, carry out fragmentation screening, to obtain varigrained secondary synthetics.
Secondly explanation is according to the preparation method's of cadmium telluride of the present invention embodiment.
Embodiment 1
A: single sintering step
To be of a size of 1mm 5N cadmium grain and be of a size of 1mm 5N tellurium grain and be divided into respectively 5 parts and 5 parts according to mol ratio 1:1;
5N cadmium grain and 5N tellurium grain are placed in the first graphite boat in order, placement is sequentially placed in the lowest layer for first part of relatively low cadmium grain of fusing point, first part of the relatively high tellurium grain of fusing point is positioned on first part of cadmium grain, then place second part of cadmium grain, second part of tellurium grain, the 3rd part of cadmium grain, the 4th part of tellurium grain, the rest may be inferred, staggered layer-by-layer distribution; The first graphite boat carried out Water Quenching before charging;
Charged the first graphite boat is positioned in the first silica tube, the first graphite boat is positioned over as far as possible to the middle part of the first silica tube;
The first silica tube that is placed with the first graphite boat is positioned in the first synthetic furnace;
Pass into the first protective gas the air in the first silica tube is emptying, wherein the first protective gas is nitrogen;
After the air in the first silica tube is drained, adopt three sections of heating modes to carry out hyperthermic treatment: first paragraph temperature rise rate is 2 ℃/min, from room temperature, is warming up to 150 ℃, insulation 5h, this process passes into the first protective gas nitrogen and protects; Second segment temperature rise rate is 2 ℃/min, continues to be warming up to 500 ℃, insulation 90min, and this process passes into the first reducing gas hydrogen; The 3rd section of temperature rise rate is 20 ℃/min, continues to be warming up to 1000 ℃, and insulation 3h, stops heating;
After building-up reactions, the first synthetic furnace stops heating and naturally cooling to room temperature, and this process continues to pass into the first reducing gas hydrogen;
From the first synthetic furnace, take out the first silica tube, then from the first silica tube, take out the first graphite boat, then in the first graphite boat, take out single sintering thing.
B: secondary synthesis step
Single sintering thing is crushed to the cadmium telluride crystal grain that particle diameter is 1mm;
The good cadmium telluride crystal grain of fragmentation is packed in the second graphite boat, and the second graphite boat carries out Water Quenching before charging;
The second graphite boat is positioned in the second silica tube;
The second silica tube that the second graphite boat is housed is positioned in the second synthetic furnace;
Adopt the second protective gas that the air in the second silica tube is emptying, wherein the second protective gas is nitrogen;
After the air in the second silica tube is drained, adopt two sections of heating modes to carry out hyperthermic treatment: 8 ℃/min of first paragraph temperature rise rate, from normal temperature, be warming up to 350 ℃, insulation 10min, this process passes into the second protective gas nitrogen; Second segment temperature rise rate is 2 ℃/min, continues to be warming up to 850 ℃, insulation 20h, and this process passes into the second reducing gas hydrogen;
After building-up reactions, the second synthetic furnace stops heating and naturally cooling to room temperature, and this process continues to pass into the second reducing gas hydrogen, obtains secondary synthetics cadmium telluride;
The secondary synthetics cadmium telluride obtaining, through broken and screening, is finally obtained to bis-syntheticss of varigrained 5N.
In single sintering step and secondary synthesis step in embodiment 1, the first synthetic furnace and the second synthetic furnace are same synthetic furnace, the first graphite boat and the second graphite boat are same graphite boat, the first silica tube and the second silica tube are same silica tube, and in secondary synthesis step, before the second graphite boat and the use of the second silica tube, carry out clean.
Embodiment 2
A: single sintering step
To be of a size of 10mm 5N cadmium grain and be of a size of 10mm 5N tellurium grain and be divided into respectively 12 parts and 12 parts according to mol ratio 1:1;
5N cadmium grain and 5N tellurium grain are placed in the first graphite boat in order, placement is sequentially placed in the lowest layer for first part of relatively low cadmium grain of fusing point, first part of the relatively high tellurium grain of fusing point is positioned on first part of cadmium grain, then place second part of cadmium grain, second part of tellurium grain, the 3rd part of cadmium grain, the 4th part of tellurium grain, the rest may be inferred, staggered layer-by-layer distribution; The first graphite boat carried out Water Quenching before charging;
Charged the first graphite boat is positioned in the first silica tube, the first graphite boat is positioned over as far as possible to the middle part of the first silica tube;
The first silica tube that is placed with the first graphite boat is positioned in the first synthetic furnace;
Pass into the first protective gas the air in the first silica tube is emptying, wherein the first protective gas is nitrogen;
After the air in the first silica tube is drained, adopt three sections of heating modes to carry out hyperthermic treatment: first paragraph temperature rise rate is 10 ℃/min, from room temperature, is warming up to 230 ℃, insulation 3h, this process passes into the first protective gas nitrogen and protects; Second segment temperature rise rate is 15 ℃/min, continues to be warming up to 420 ℃, insulation 60min, and this process passes into the first reducing gas hydrogen; The 3rd section of temperature rise rate is 17 ℃/min, continues to be warming up to 930 ℃, and insulation 0.5h, stops heating;
After building-up reactions, the first synthetic furnace stops heating and naturally cooling to room temperature, and this process continues to pass into the first reducing gas hydrogen;
From the first synthetic furnace, take out the first silica tube, then from the first silica tube, take out the first graphite boat, then in the first graphite boat, take out single sintering thing.
B: secondary synthesis step
Single sintering thing is crushed to the cadmium telluride crystal grain that particle diameter is 10mm;
The good cadmium telluride crystal grain of fragmentation is packed in the second graphite boat, and the second graphite boat carries out Water Quenching before charging;
The second graphite boat is positioned in the second silica tube;
The second silica tube that the second graphite boat is housed is positioned in the second synthetic furnace;
Adopt the second protective gas that the air in the second silica tube is emptying, wherein the second protective gas is nitrogen;
After the air in the second silica tube is drained, adopt two sections of heating modes to carry out hyperthermic treatment: 15 ℃/min of first paragraph temperature rise rate, from normal temperature, be warming up to 450 ℃, insulation 60min, this process passes into the second protective gas nitrogen; Second segment temperature rise rate is 8 ℃/min, continues to be warming up to 940 ℃, insulation 10h, and this process passes into the second reducing gas hydrogen;
After building-up reactions, the second synthetic furnace stops heating and naturally cooling to room temperature, and this process continues to pass into the second reducing gas hydrogen, obtains secondary synthetics cadmium telluride;
The secondary synthetics cadmium telluride obtaining, through broken and screening, is finally obtained to bis-syntheticss of varigrained 5N.
In single sintering step and secondary synthesis step in embodiment 2, the first synthetic furnace and the second synthetic furnace are same synthetic furnace, the first graphite boat and the second graphite boat are same graphite boat, the first silica tube and the second silica tube are same silica tube, and in secondary synthesis step, before the second graphite boat and the use of the second silica tube, carry out clean.
Embodiment 3
A: single sintering step
To be of a size of 5mm 5N cadmium grain and be of a size of 7mm 5N tellurium grain and be divided into respectively 8 parts and 8 parts according to mol ratio 1:1;
5N cadmium grain and 5N tellurium grain are placed in the first graphite boat in order, placement is sequentially placed in the lowest layer for first part of relatively low cadmium grain of fusing point, first part of the relatively high tellurium grain of fusing point is positioned on first part of cadmium grain, then place second part of cadmium grain, second part of tellurium grain, the 3rd part of cadmium grain, the 4th part of tellurium grain, the rest may be inferred, staggered layer-by-layer distribution; The first graphite boat carried out Water Quenching before charging;
Charged the first graphite boat is positioned in the first silica tube, the first graphite boat is positioned over as far as possible to the middle part of the first silica tube;
The first silica tube that is placed with the first graphite boat is positioned in the first synthetic furnace;
Pass into the first protective gas the air in the first silica tube is emptying, wherein the first protective gas is nitrogen;
After the air in the first silica tube is drained, adopt three sections of heating modes to carry out hyperthermic treatment: first paragraph temperature rise rate is 15 ℃/min, from room temperature, is warming up to 250 ℃, insulation 1.5h, this process passes into the first protective gas nitrogen and protects; Second segment temperature rise rate is 10 ℃/min, continues to be warming up to 350 ℃, insulation 10min, and this process passes into the first reducing gas hydrogen; The 3rd section of temperature rise rate is 5 ℃/min, continues to be warming up to 850 ℃, and insulation 1.5h, stops heating;
After building-up reactions, the first synthetic furnace stops heating and naturally cooling to room temperature, and this process continues to pass into the first reducing gas hydrogen;
From the first synthetic furnace, take out the first silica tube, then from the first silica tube, take out the first graphite boat, then in the first graphite boat, take out single sintering thing.
B: secondary synthesis step
Single sintering thing is crushed to the cadmium telluride crystal grain that particle diameter is 7mm;
The good cadmium telluride crystal grain of fragmentation is packed in the second graphite boat, and the second graphite boat carries out Water Quenching before charging;
The second graphite boat is positioned in the second silica tube;
The second silica tube that the second graphite boat is housed is positioned in the second synthetic furnace;
Adopt the second protective gas that the air in the second silica tube is emptying, wherein the second protective gas is nitrogen;
After the air in the second silica tube is drained, adopt two sections of heating modes to carry out hyperthermic treatment: 25 ℃/min of first paragraph temperature rise rate, from normal temperature, be warming up to 380 ℃, insulation 40min, this process passes into the second protective gas nitrogen; Second segment temperature rise rate is 10 ℃/min, continues to be warming up to 1000 ℃, insulation 2h, and this process need passes into the second reducing gas hydrogen;
After building-up reactions, the second synthetic furnace stops heating and naturally cooling to room temperature, and this process continues to pass into the second reducing gas hydrogen, obtains secondary synthetics cadmium telluride;
The secondary synthetics cadmium telluride obtaining, through broken and screening, is finally obtained to bis-syntheticss of varigrained 5N.
In single sintering step and secondary synthesis step in embodiment 3, the first synthetic furnace and the second synthetic furnace are same synthetic furnace, the first graphite boat and the second graphite boat are same graphite boat, the first silica tube and the second silica tube are same silica tube, and in secondary synthesis step, before the second graphite boat and the use of the second silica tube, carry out clean.
Finally provide test result.
Secondary synthetics (being cadmium telluride) product adopts icp ms (ICP-MS) to detect (WeiPE company of manufacturer, model is: DRC-II), the testing conditions of this equipment is: temperature is 18 ℃-28 ℃, relative humidity is 30-70%, and cleanliness factor is 1000 grades.Detect principle: icp ms detection mode: element to be measured, after plasma high-temperature ionization, enters mass analyzer with positive charge form, and the difference according to mass/charge ratio, is received by detector, produces signal.Signal and this element signal ratio of reference material that element to be measured produces draw constituent content to be measured.
Table 1 provides the test result of embodiment 1-3.
The secondary synthetics test result (PPm) of table 1 embodiment 1-3
As can be seen from the table, as seen from Table 1, the cadmium telluride that the present invention obtains reaches 5N purity.
Claims (8)
1. a preparation method for cadmium telluride, comprising:
Single sintering step, comprising:
5N cadmium grain and 5N tellurium grain are placed in the first graphite boat from top to bottom according to the relatively low cadmium grain of fusing point from the lowest layer and the relatively high tellurium grain of fusing point for staggered minute, and wherein the lowest layer is cadmium grain;
Charged the first graphite boat is positioned in the first silica tube;
The first silica tube that is placed with the first graphite boat is positioned in the first synthetic furnace;
Pass into the air in emptying the first silica tube of the first protective gas;
After air in the first silica tube is emptying by the first protective gas, the first synthetic furnace adopts three sections of heating modes, and first paragraph passes into the first protective gas, and second segment and the 3rd section pass into the first reducing gas;
After building-up reactions, the first synthetic furnace stops heating and being cooled to room temperature, continues to pass into the first reducing gas in temperature-fall period; And
From the first silica tube, take out the first graphite boat, then take out single sintering thing in the first graphite boat; And
Secondary synthesis step, comprising:
Single sintering thing is crushed to the cadmium telluride crystal grain of specified dimension;
The good cadmium telluride crystal grain of fragmentation is encased in the second graphite boat;
The second graphite boat that broken good cadmium telluride crystal grain is housed is positioned in the second silica tube;
The second silica tube that is placed with the second graphite boat is positioned in the second synthetic furnace;
Pass into the air in emptying the second silica tube of the second protective gas;
After air in the second silica tube is emptying by the second protective gas, the second synthetic furnace adopts two sections of heating modes, and first paragraph passes into the second protective gas, and second segment passes into the second reducing gas;
After building-up reactions, the second synthetic furnace stops heating and being cooled to room temperature, continues to pass into the second reducing gas in temperature-fall period; And
From the second silica tube, take out the second graphite boat, then take out secondary synthetics in the second graphite boat;
Wherein:
In described single sintering step, three sections of heating modes are: the temperature rise rate of first paragraph is 2～15 ℃/min, from room temperature, are warming up to 150～250 ℃, and insulation 1.5～5h passes into the first protective gas in first paragraph; The temperature rise rate of second segment is 2～15 ℃/min, continues to be warming up to 350～500 ℃, and insulation 10～90min passes into the first reducing gas in second segment; And the temperature rise rate of the 3rd section is 5～20 ℃/min, continue to be warming up to 850～1000 ℃, insulation 0.5～3h passes into the first reducing gas in the 3rd section;
In described secondary synthesis step, two sections of heating modes are: the temperature rise rate of first paragraph is 8～25 ℃/min, from room temperature, rise to 350～450 ℃, and insulation 10～60min passes into the second protective gas in first paragraph; And the temperature rise rate of second segment is 2～10 ℃/min, continue to be warming up to 850～1000 ℃, insulation 2～20h passes into the second reducing gas in second segment.
2. the preparation method of cadmium telluride according to claim 1, is characterized in that, in single sintering step, 5N cadmium grain is of a size of 1～10mm, and 5N tellurium grain is of a size of 1～10mm.
3. the preparation method of cadmium telluride according to claim 1, is characterized in that, in single sintering step, the blending ratio of 5N tellurium grain and 5N cadmium grain is mol ratio 1:1.
4. the preparation method of cadmium telluride according to claim 1, is characterized in that, in described secondary synthesis step, the described specified dimension by the fragmentation of single sintering thing is 1～10mm.
5. the preparation method of cadmium telluride according to claim 1, is characterized in that,
The first graphite boat in described single sintering step is process Water Quenching before charging;
The second graphite boat in described secondary synthesis step is process Water Quenching before charging;
In described single sintering step with described secondary synthesis step in the first protective gas and the second protective gas can be identical or different;
In described single sintering step from the first reducing gas in described secondary synthesis step and the second reducing gas can just as or different.
6. the preparation method of cadmium telluride according to claim 5, is characterized in that, the first protective gas and the second protective gas are nitrogen, and the first reducing gas and the second reducing gas are hydrogen.
7. the preparation method of cadmium telluride according to claim 1, is characterized in that,
The second synthetic furnace in the first synthetic furnace in described single sintering step and described secondary synthesis step is same or different synthetic furnace;
The second graphite boat in the first graphite boat in described single sintering step and described secondary synthesis step is same or different graphite boat, and when the second graphite boat in the first graphite boat in described single sintering step and described secondary synthesis step is same graphite boat, in described secondary synthesis step, before the second graphite boat is used, the second graphite boat is carried out to clean;
The second silica tube in described single sintering step and the second silica tube in described secondary synthesis step are same or different silica tubes, and when the second silica tube in described single sintering step and the second silica tube in described secondary synthesis step are same silica tube, in described secondary synthesis step, before using, the second silica tube carries out clean.
8. the preparation method of cadmium telluride according to claim 1, is characterized in that, also comprises step: after obtaining secondary synthetics, carry out fragmentation screening, to obtain varigrained secondary synthetics.
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| CN107522172A (en) * | 2017-07-31 | 2017-12-29 | 成都中建材光电材料有限公司 | A kind of preparation technology of cadmium antimonide powder |
| CN108069456B (en) * | 2017-12-28 | 2019-10-25 | 成都中建材光电材料有限公司 | A kind of preparation method of cadmium telluride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125679A (en) * | 2007-08-31 | 2008-02-20 | 侯仁义 | Method for preparing highly pure cadmium telluride |
| CN101734630A (en) * | 2009-12-30 | 2010-06-16 | 峨嵋半导体材料研究所 | Method for preparing high-purity cadmium telluride |
| CN102086031A (en) * | 2010-11-25 | 2011-06-08 | 广东先导稀有材料股份有限公司 | Liquid-phase synthesis method of cadmium telluride |
-
2013
- 2013-06-18 CN CN201310241279.8A patent/CN103274372B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125679A (en) * | 2007-08-31 | 2008-02-20 | 侯仁义 | Method for preparing highly pure cadmium telluride |
| CN101734630A (en) * | 2009-12-30 | 2010-06-16 | 峨嵋半导体材料研究所 | Method for preparing high-purity cadmium telluride |
| CN102086031A (en) * | 2010-11-25 | 2011-06-08 | 广东先导稀有材料股份有限公司 | Liquid-phase synthesis method of cadmium telluride |
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