Embodiment
Describe preparation method and the embodiment of the cadmium telluride according to the present invention below in detail.
Preparation method according to cadmium telluride of the present invention at first is described.
Comprise synthesis step and secondary synthesis step according to the preparation method of cadmium telluride of the present invention.
Wherein, one time synthesis step comprises: 5N cadmium grain is placed in first graphite boat according to interlocking from top to bottom to divide from the relative higher tellurium grain with fusing point of the relatively low cadmium grain of lowest layer fusing point with 5N tellurium grain, and wherein the lowest layer is the cadmium grain; Charged first graphite boat is positioned in first silica tube; First silica tube that is placed with first graphite boat is positioned in first synthetic furnace; Feed the air in the first protective gas emptying, first silica tube; Air in first silica tube is by after the first protective gas emptying, and first synthetic furnace adopts three sections heating modes, and first section feeds first protective gas, and second section and the 3rd section feeding first reducing gas; After the building-up reactions, first synthetic furnace stops heating and is cooled to room temperature, continues to feed first reducing gas in the temperature-fall period; And from first silica tube, take out first graphite boat, in first graphite boat, take out a synthetics again.
Wherein, the secondary synthesis step comprises: the cadmium telluride crystal grain that synthetics is crushed to specified dimension; The cadmium telluride crystal grain that fragmentation is good is encased in second graphite boat; Second graphite boat that the good cadmium telluride crystal grain of fragmentation is housed is positioned in second silica tube; Second silica tube that is placed with second graphite boat is positioned in second synthetic furnace; Feed the air in the second protective gas emptying, second silica tube; Air in second silica tube is by after the second protective gas emptying, and second synthetic furnace adopts two sections heating modes, and first section feeds second protective gas, second section feeding second reducing gas; After the building-up reactions, second synthetic furnace stops heating and is cooled to room temperature, continues to feed second reducing gas in the temperature-fall period; And from second silica tube, take out second graphite boat, in second graphite boat, take out the secondary synthetics again.
In the preparation method according to cadmium telluride of the present invention, preferably, in synthesis step, 5N cadmium grain is of a size of 1~10mm, and 5N tellurium grain is of a size of 1~10mm.
In the preparation method according to cadmium telluride of the present invention, preferably, in synthesis step, the blending ratio of 5N tellurium powder and 5N cadmium powder is mol ratio 1:1.
In the preparation method according to cadmium telluride of the present invention, in a described synthesis step, three sections heating modes can be: first section temperature rise rate is 2~15 ℃/min, is warming up to 150~250 ℃ from room temperature, insulation 1.5~5h feeds first protective gas in first section; Second section temperature rise rate is 2~15 ℃/min, continues to be warming up to 350~500 ℃, and insulation 10~90min feeds first reducing gas in second section; And the 3rd section temperature rise rate is 5~20 ℃/min, continues to be warming up to 850~1000 ℃, and insulation 0.5~3h feeds first reducing gas in the 3rd section.
In the preparation method according to cadmium telluride of the present invention, preferably, in described secondary synthesis step, described specified dimension with a synthetics fragmentation is 1~10mm.
In the preparation method according to cadmium telluride of the present invention, in described secondary synthesis step, two sections heating modes can be: first section temperature rise rate is 8~25 ℃/min, rises to 350~450 ℃ from room temperature, insulation 10~60min feeds second protective gas in first section; And second section temperature rise rate is 2~10 ℃/min, continues to be warming up to 850~1000 ℃, and insulation 2~20h feeds second reducing gas in second section.
In the preparation method according to cadmium telluride of the present invention, first graphite boat in the described synthesis step is the process Water Quenching before charging; Second graphite boat in the described secondary synthesis step is the process Water Quenching before charging; In the described synthesis step with described secondary synthesis step in first protective gas and second protective gas can be identical or different, be preferably first protective gas and second protective gas is nitrogen; In the described synthesis step with described secondary synthesis step in first reducing gas and second reducing gas can just as or different, be preferably first reducing gas and second reducing gas is hydrogen.
In the preparation method according to cadmium telluride of the present invention, first synthetic furnace in the described synthesis step is same or different synthetic furnaces with second synthetic furnace in the described secondary synthesis step; First graphite boat in the described synthesis step is same or different graphite boats with second graphite boat in the described secondary synthesis step, and when first graphite boat in the described synthesis step and second graphite boat in the described secondary synthesis step are same graphite boat, in described secondary synthesis step, before second graphite boat uses, second graphite boat is carried out clean; Second silica tube in the described synthesis step is same or different silica tubes with second silica tube in described secondary synthesis step, and when second silica tube in the described synthesis step and second silica tube in described secondary synthesis step are same silica tube, in described secondary synthesis step, before using, second silica tube carries out clean.
In the preparation method according to cadmium telluride of the present invention, also comprise step: after obtaining the secondary synthetics, carry out fragmentation and 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 a: synthesis step
To be of a size of 1mm5N cadmium grain and be of a size of 1mm5N tellurium grain and be divided into 5 parts and 5 parts respectively according to mol ratio 1:1;
5N cadmium grain and 5N tellurium grain are placed in first graphite boat in order, placement places the lowest layer for first part of relatively low cadmium grain of fusing point in proper order, the higher relatively tellurium grain of fusing point is positioned on first part of cadmium grain for first part, place second part of cadmium grain, second part of tellurium grain, the 3rd part of cadmium grain, the 4th part of tellurium grain then, the rest may be inferred, staggered layer-by-layer distribution; First graphite boat carried out Water Quenching before charging;
Charged first graphite boat is positioned in first silica tube, first graphite boat is positioned over as far as possible the middle part of first silica tube;
First silica tube that is placed with first graphite boat is positioned in first synthetic furnace;
Feed first protective gas with the air emptying in first silica tube, wherein first protective gas is nitrogen;
After treating that the interior air of first silica tube is drained, adopt three sections heating modes to carry out hyperthermic treatment: first section temperature rise rate is 2 ℃/min, is warming up to 150 ℃ from room temperature, insulation 5h, and this process feeds the first protective gas nitrogen and protects; Second section temperature rise rate is 2 ℃/min, continues to be warming up to 500 ℃, insulation 90min, and this process feeds the first reducing gas hydrogen; The 3rd section temperature rise rate is 20 ℃/min, continues to be warming up to 1000 ℃, and insulation 3h stops heating;
After the building-up reactions, first synthetic furnace stops heating and naturally cools to room temperature, and this process continues to feed the first reducing gas hydrogen;
From first synthetic furnace, take out first silica tube, from first silica tube, take out first graphite boat again, in first graphite boat, take out a synthetics then.
B: secondary synthesis step
A synthetics is crushed to the cadmium telluride crystal grain that particle diameter is 1mm;
The cadmium telluride crystal grain that fragmentation is good is packed in second graphite boat, and second graphite boat carries out Water Quenching before charging;
Second graphite boat is positioned in second silica tube;
Second silica tube that second graphite boat is housed is positioned in second synthetic furnace;
Adopt second protective gas with the air emptying in second silica tube, wherein second protective gas is nitrogen;
After treating that the interior air of second silica tube is drained, adopt two sections heating modes to carry out hyperthermic treatment: 8 ℃/min of first section temperature rise rate, be warming up to 350 ℃ from normal temperature, insulation 10min, this process feeds the second protective gas nitrogen; Second section temperature rise rate is 2 ℃/min, continues to be warming up to 850 ℃, insulation 20h, and this process feeds the second reducing gas hydrogen;
After the building-up reactions, second synthetic furnace stops heating and naturally cools to room temperature, and this process continues to feed the second reducing gas hydrogen, obtains secondary synthetics cadmium telluride;
The broken and screening of secondary synthetics cadmium telluride process with obtaining obtains varigrained 5N secondary synthetics at last.
In the synthesis step and secondary synthesis step in embodiment 1, first synthetic furnace and second synthetic furnace are same synthetic furnace, first graphite boat and second graphite boat are same graphite boat, first silica tube and second silica tube are same silica tube, and in the secondary synthesis step, before second graphite boat and the use of second silica tube, carry out clean.
Embodiment 2
A a: synthesis step
To be of a size of 10mm5N cadmium grain and be of a size of 10mm5N tellurium grain and be divided into 12 parts and 12 parts respectively according to mol ratio 1:1;
5N cadmium grain and 5N tellurium grain are placed in first graphite boat in order, placement places the lowest layer for first part of relatively low cadmium grain of fusing point in proper order, the higher relatively tellurium grain of fusing point is positioned on first part of cadmium grain for first part, place second part of cadmium grain, second part of tellurium grain, the 3rd part of cadmium grain, the 4th part of tellurium grain then, the rest may be inferred, staggered layer-by-layer distribution; First graphite boat carried out Water Quenching before charging;
Charged first graphite boat is positioned in first silica tube, first graphite boat is positioned over as far as possible the middle part of first silica tube;
First silica tube that is placed with first graphite boat is positioned in first synthetic furnace;
Feed first protective gas with the air emptying in first silica tube, wherein first protective gas is nitrogen;
After treating that the interior air of first silica tube is drained, adopt three sections heating modes to carry out hyperthermic treatment: first section temperature rise rate is 10 ℃/min, is warming up to 230 ℃ from room temperature, insulation 3h, and this process feeds the first protective gas nitrogen and protects; Second section temperature rise rate is 15 ℃/min, continues to be warming up to 420 ℃, insulation 60min, and this process feeds the first reducing gas hydrogen; The 3rd section temperature rise rate is 17 ℃/min, continues to be warming up to 930 ℃, and insulation 0.5h stops heating;
After the building-up reactions, first synthetic furnace stops heating and naturally cools to room temperature, and this process continues to feed the first reducing gas hydrogen;
From first synthetic furnace, take out first silica tube, from first silica tube, take out first graphite boat again, in first graphite boat, take out a synthetics then.
B: secondary synthesis step
A synthetics is crushed to the cadmium telluride crystal grain that particle diameter is 10mm;
The cadmium telluride crystal grain that fragmentation is good is packed in second graphite boat, and second graphite boat carries out Water Quenching before charging;
Second graphite boat is positioned in second silica tube;
Second silica tube that second graphite boat is housed is positioned in second synthetic furnace;
Adopt second protective gas with the air emptying in second silica tube, wherein second protective gas is nitrogen;
After treating that the interior air of second silica tube is drained, adopt two sections heating modes to carry out hyperthermic treatment: 15 ℃/min of first section temperature rise rate, be warming up to 450 ℃ from normal temperature, insulation 60min, this process feeds the second protective gas nitrogen; Second section temperature rise rate is 8 ℃/min, continues to be warming up to 940 ℃, insulation 10h, and this process feeds the second reducing gas hydrogen;
After the building-up reactions, second synthetic furnace stops heating and naturally cools to room temperature, and this process continues to feed the second reducing gas hydrogen, obtains secondary synthetics cadmium telluride;
The broken and screening of secondary synthetics cadmium telluride process with obtaining obtains varigrained 5N secondary synthetics at last.
In the synthesis step and secondary synthesis step in embodiment 2, first synthetic furnace and second synthetic furnace are same synthetic furnace, first graphite boat and second graphite boat are same graphite boat, first silica tube and second silica tube are same silica tube, and in the secondary synthesis step, before second graphite boat and the use of second silica tube, carry out clean.
Embodiment 3
A a: synthesis step
To be of a size of 5mm5N cadmium grain and be of a size of 7mm5N tellurium grain and be divided into 8 parts and 8 parts respectively according to mol ratio 1:1;
5N cadmium grain and 5N tellurium grain are placed in first graphite boat in order, placement places the lowest layer for first part of relatively low cadmium grain of fusing point in proper order, the higher relatively tellurium grain of fusing point is positioned on first part of cadmium grain for first part, place second part of cadmium grain, second part of tellurium grain, the 3rd part of cadmium grain, the 4th part of tellurium grain then, the rest may be inferred, staggered layer-by-layer distribution; First graphite boat carried out Water Quenching before charging;
Charged first graphite boat is positioned in first silica tube, first graphite boat is positioned over as far as possible the middle part of first silica tube;
First silica tube that is placed with first graphite boat is positioned in first synthetic furnace;
Feed first protective gas with the air emptying in first silica tube, wherein first protective gas is nitrogen;
After treating that the interior air of first silica tube is drained, adopt three sections heating modes to carry out hyperthermic treatment: first section temperature rise rate is 15 ℃/min, is warming up to 250 ℃ from room temperature, insulation 1.5h, and this process feeds the first protective gas nitrogen and protects; Second section temperature rise rate is 10 ℃/min, continues to be warming up to 350 ℃, insulation 10min, and this process feeds the first reducing gas hydrogen; The 3rd section temperature rise rate is 5 ℃/min, continues to be warming up to 850 ℃, and insulation 1.5h stops heating;
After the building-up reactions, first synthetic furnace stops heating and naturally cools to room temperature, and this process continues to feed the first reducing gas hydrogen;
From first synthetic furnace, take out first silica tube, from first silica tube, take out first graphite boat again, in first graphite boat, take out a synthetics then.
B: secondary synthesis step
A synthetics is crushed to the cadmium telluride crystal grain that particle diameter is 7mm;
The cadmium telluride crystal grain that fragmentation is good is packed in second graphite boat, and second graphite boat carries out Water Quenching before charging;
Second graphite boat is positioned in second silica tube;
Second silica tube that second graphite boat is housed is positioned in second synthetic furnace;
Adopt second protective gas with the air emptying in second silica tube, wherein second protective gas is nitrogen;
After treating that the interior air of second silica tube is drained, adopt two sections heating modes to carry out hyperthermic treatment: 25 ℃/min of first section temperature rise rate, be warming up to 380 ℃ from normal temperature, insulation 40min, this process feeds the second protective gas nitrogen; Second section temperature rise rate is 10 ℃/min, continues to be warming up to 1000 ℃, insulation 2h, and this process need feeds the second reducing gas hydrogen;
After the building-up reactions, second synthetic furnace stops heating and naturally cools to room temperature, and this process continues to feed the second reducing gas hydrogen, obtains secondary synthetics cadmium telluride;
The broken and screening of secondary synthetics cadmium telluride process with obtaining obtains varigrained 5N secondary synthetics at last.
In the synthesis step and secondary synthesis step in embodiment 3, first synthetic furnace and second synthetic furnace are same synthetic furnace, first graphite boat and second graphite boat are same graphite boat, first silica tube and second silica tube are same silica tube, and in the secondary synthesis step, before second graphite boat and the use of second silica tube, carry out clean.
Provide test result at last.
Secondary synthetics (being cadmium telluride) product adopts icp ms (ICP-MS) to detect that (manufacturer is PE company, model is: DRC-II), the testing conditions of this equipment is: temperature is 18 ℃-28 ℃, and relative humidity is 30-70%, and cleanliness factor is 1000 grades.Detect principle: the icp ms detection mode: after the element process plasma high-temperature to be measured ionization, enter mass analyzer with the positive charge form, the difference according to the mass 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
From table as can be seen, as seen from Table 1, the cadmium telluride that the present invention obtains reaches 5N purity.