WO2013174251A1 - Method for preparing cadmium telluride - Google Patents
Method for preparing cadmium telluride Download PDFInfo
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- WO2013174251A1 WO2013174251A1 PCT/CN2013/075972 CN2013075972W WO2013174251A1 WO 2013174251 A1 WO2013174251 A1 WO 2013174251A1 CN 2013075972 W CN2013075972 W CN 2013075972W WO 2013174251 A1 WO2013174251 A1 WO 2013174251A1
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- graphite boat
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- inert gas
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Definitions
- the present invention relates to a method for preparing a synthetic material, and more particularly to a method for preparing cadmium telluride. Background technique
- One of the methods is to insert a hot rod into a mixed powder of cerium and cadmium and heat it to 500 ° C to form.
- the method adopts a hot rod heating method, the temperature is not uniform enough, and the reaction is insufficient. And the vacuum sealing technology is adopted, and the cost is high. Summary of the invention
- an object of the present invention is to provide a method for preparing cadmium telluride which is capable of uniform heating and sufficient synthesis of cadmium telluride.
- the present invention provides a process for producing cadmium telluride comprising a primary synthesis step and a secondary synthesis step.
- the one-step synthesis step comprises: mixing 5N tantalum powder and 5N cadmium powder in proportion to obtain a mixture; loading the mixture into the first graphite boat; placing the first graphite boat containing the mixture into the first quartz tube Place the first quartz tube on which the first graphite boat is placed into the first synthesis furnace; pass the first inert gas to evacuate the air in the first quartz tube; the air in the first quartz tube is evacuated by the first inert gas
- the first synthesis furnace adopts the first multi-stage heating and heat preservation method to synthesize the mixture in the first graphite boat in the first multi-stage heating and warming, the first stage is introduced into the first inert gas, and the latter stage is introduced into the first reduction.
- the first synthesis furnace stops adding Heat and sub-cooling to room temperature: in the stepwise cooling to room temperature, the first section is introduced into the first reducing gas, the latter section is introduced into the first inert gas; and the first graphite boat is taken out from the first quartz tube, and then from the first The composition was taken out once in the graphite boat.
- the secondary synthesis step includes: crushing the primary composition to the primary composite particles of a prescribed size; loading the primary composite particles into the second graphite boat; and placing the second graphite boat containing the primary composite particles to the second Inside the quartz tube; placing a second quartz tube in which the second graphite boat is placed into the second synthesis furnace; introducing a second inert gas to evacuate the air in the second quartz tube; and the air in the second quartz tube is being subjected to the second inert gas
- the second synthesis furnace adopts a second multi-stage heating and holding method to synthesize the first synthetic particles in the second graphite boat, and in the second multi-stage heating and holding, the front section is introduced with the second inert gas, and the latter stage
- the second reducing gas is introduced; after the synthesis reaction, the second synthesis furnace stops heating and is cooled down to room temperature in stages, and is cooled to room temperature in sections, the second reducing gas is introduced into the front stage, and the second inert gas is introduced in the latter stage.
- the preparation method of the cadmium telluride provided by the invention is synthesized by using a graphite boat, a quartz tube, and an inert gas and a reducing gas, which can make the cadmium telluride synthesis uniform and synthetically sufficient.
- the preparation method of the cadmium telluride provided by the invention adopts the graphite boat, the quartz tube, and the inert gas and the reducing gas to be synthesized twice, which can remove the oxygen element in the cadmium telluride, thereby improving the purity of the cadmium telluride. Obtain high quality and high purity cadmium telluride.
- the method for preparing cadmium telluride provided by the invention can reduce the manufacturing cost of cadmium telluride by using graphite boat and quartz tube. detailed description
- the method for producing cadmium telluride according to the present invention comprises a single synthesis step and a second synthesis step.
- one synthesis step comprises: mixing 5N tantalum powder and 5N cadmium powder in proportion to obtain a mixture; loading the mixture into the first graphite boat; placing the first graphite boat containing the mixture to the first Inside the quartz tube; placing the first quartz tube in which the first graphite boat is placed into the first synthesis furnace; introducing the first inert gas to evacuate the air in the first quartz tube; the air in the first quartz tube is the first inert gas
- the first synthesis furnace adopts the first multi-stage heating and holding method to synthesize the mixture in the first graphite boat, and in the first multi-stage heating and holding, the first section is introduced with the first inert gas, and the latter section is passed.
- the first synthesis furnace stops heating and is cooled to room temperature in multiple stages, and is cooled to room temperature in multiple stages, the first reducing gas is introduced into the front stage, and the first inert gas is introduced in the latter stage;
- the first graphite boat was taken out from a quartz tube, and the composition was taken out from the first graphite boat.
- the secondary synthesis step comprises: crushing the primary composition to the primary composite particles of a predetermined size; loading the primary composite particles into the second graphite boat; and placing the second graphite boat containing the primary composite particles into a second quartz tube placed in the second quartz tube; a second inert gas is introduced into the second quartz tube; the air in the second quartz tube is second; After the inert gas is emptied, the second synthesis furnace adopts a second multi-stage heating and holding method to synthesize the first synthetic particles in the second graphite boat.
- the front portion is introduced with the second inert gas,
- the second reducing gas is introduced into the section; and after the synthesis reaction, the second synthesis furnace stops heating and is cooled down to room temperature in sections, and is cooled to room temperature in sections, the second reducing gas is introduced into the front stage, and the second reducing gas is introduced in the front stage.
- Inert gas; from the first The second graphite boat was taken out from the two quartz tubes, and the secondary composition was taken out from the second graphite boat.
- the mixing ratio of the powder and the 5N cadmium powder may be a molar ratio of 1:1.
- the 5N tantalum powder and the 5N cadmium powder have a particle size of 0.5 to 5 mm.
- the first multi-stage heating and holding may be three-stage heating and holding: the first stage, at 2 to 10 ° C/min
- the heating rate is raised from room temperature to 150 ⁇ 300 °C, and the temperature is kept for 2 ⁇ 6h.
- the first inert gas is introduced into the first stage.
- the second stage is heated to the temperature rising rate of 2 ⁇ 10 °C/min.
- the first paragraph and the second paragraph can be defined as the front segment, and the third segment can be defined as the latter segment.
- the section in the one-step synthesis step, is cooled to room temperature to cool down to room temperature with two stages of natural cooling of the first synthesis furnace: 850 ⁇ 950 °C down to 200 ⁇ 80 °C, the first reducing gas is introduced in the first stage; the second stage is from 200 ⁇ 80 °C to room temperature, and the first inertia is introduced in the second stage. gas.
- the first paragraph can be defined as the front segment and the second segment is defined as the latter segment.
- the predetermined size for breaking the primary composition may be 0.5 to 5 mm.
- the second multi-stage heating and holding may be two-stage heating and warming: the first stage, at 5 to 20 ° C /
- the heating rate of min increases from room temperature to 380 ⁇ 450 °C, keeps warm for 10 ⁇ 60min, and enters the second in the first stage.
- the first paragraph can be defined as the front segment
- the second segment is defined as the latter segment.
- the stepwise cooling to room temperature is to cool down to room temperature with two stages of natural cooling of the second synthesis furnace: From 850 ⁇ 950°C to 200 ⁇ 80°C, the second reducing gas is introduced into the first section; the second section is from 200 ⁇ 80°C to room temperature, and the second section is passed to the second. Inert gas.
- the first paragraph can be defined as the front segment, and the second segment is defined as the latter segment.
- the first graphite boat in the primary synthesis step may be a high temperature water quenched graphite boat
- the second graphite boat in the secondary synthesis step may be high temperature water. Quenched graphite boat.
- the first inert gas in the primary synthesis step may be nitrogen
- the second inert gas in the secondary synthesis step may be nitrogen
- the first reducing gas in the primary synthesis step may be hydrogen
- the second The second reducing gas in the synthesis step may be hydrogen
- the first synthesis furnace in the primary synthesis step and the second synthesis furnace in the secondary synthesis step are synthetic furnaces which may be the same or different.
- the first synthesis furnace in the one-time synthesis step and the second synthesis furnace in the secondary synthesis step are the same synthesis furnace, it can be used for a small amount of prepared cadmium telluride.
- the first synthesis furnace in the one synthesis step and the second synthesis furnace in the secondary synthesis step are different synthesis furnaces, it can be used to prepare cadmium telluride on a large scale.
- the first graphite boat and the second graphite boat in the secondary synthesis step may be the same or different graphite boats.
- the second graphite boat is cleaned before use, Can be used for small amounts of prepared cadmium telluride.
- the first graphite boat in the one-time synthesis step and the second graphite boat in the secondary synthesis step are different graphite boats, it can be used to prepare cadmium telluride on a large scale.
- the first quartz tube in the primary synthesis step and the second quartz tube in the secondary synthesis step are the same or different quartz tubes.
- the first quartz tube in the one-step synthesis step and the second quartz tube in the second-synthesis step are the same quartz tube, in the second synthesis step, the second quartz tube is cleaned before use, Can be used for small amounts of prepared cadmium telluride.
- the first quartz tube in the one-step synthesis step and the second quartz tube in the secondary synthesis step are different quartz tubes, it can be used to prepare cadmium telluride on a large scale.
- the method may further include the steps of: after obtaining the secondary composition, performing fine crushing and sieving to obtain secondary compositions of different particle sizes.
- the particle size of 5N tantalum powder and 5N cadmium powder is 0.5 ⁇ 2mm, and uniformly mixed according to a molar ratio of 1:1 to obtain a mixture;
- the first synthesis furnace adopts a first multi-stage heating and holding method to synthesize the mixture in the first graphite boat, wherein the first plurality of stages are heated.
- the insulation method is three-stage heating and holding method, BP: the first section, the temperature rises from room temperature to 150 °C at a heating rate of 2 °C/min, and is kept at 150 °C for 6 hours, and the first section is passed.
- the second stage after the first stage, at a heating rate of 3 °C / min, continue to raise the temperature to 380 ° C, and incubated at 380 ° C for 60 min, the first inert gas is introduced in the second stage;
- the third stage after the second stage, the temperature is raised to 850 ° C at a heating rate of 2 ° C / min, and kept at 850 ° C for 2 h, and the first reducing gas is introduced into the third stage, the first reducing property
- the gas is hydrogen;
- the first synthesis furnace stops heating and is cooled in two stages with the first synthesis furnace to cool down to room temperature: the first stage, from 850 ° C to 200 ° C, in the first stage Passing the first reducing gas; the second stage, from 200 ° C to room temperature, in the first An inert gas into the first section.
- the second synthesis furnace adopts a second multi-stage heating and holding method to synthesize the primary composite particles in the second graphite boat, wherein the second plurality of segments
- the heating and warming method is a two-stage heating and holding method, namely: the first section, rising from room temperature to 380 °C at a heating rate of 5 °C/min, and holding at 380 °C for 60 min, in the first section a second inert gas; the second stage, after the first stage, the temperature is further increased to 850 ° C at a temperature increase rate of 2 ° C / min, and is kept at 850 ° C for 2.5 h, and a second reduction is introduced in the second stage.
- the second reducing gas is hydrogen.
- the second synthesis furnace is stopped and cooled to room temperature in two stages with natural cooling in the second synthesis furnace: the first stage, from 850 ° C to 120 ° C, in the first paragraph a second reducing gas; the second stage, from 120 ° C to room temperature, in the second section of the second inert gas.
- the first synthesis furnace and the second synthesis furnace are the same synthesis furnace, and the first graphite boat and the second graphite boat are the same graphite boat, the first quartz tube and the second The quartz tube is the same quartz tube, and in the secondary synthesis step, the second graphite boat and the second quartz tube are cleaned before use.
- the 5N tantalum powder and the 5N cadmium powder have a particle size of 2 to 3.5 mm, and are uniformly mixed at a molar ratio of 1:1 to obtain a mixture; (a2) loading the mixture into the first graphite boat, the first graphite boat being a high temperature water quenched graphite boat;
- the first synthesis furnace adopts a first multi-stage heating and holding method to synthesize the mixture in the first graphite boat, wherein the first plurality of stages are heated.
- the heat preservation method is three-stage heating and holding method, namely: the first stage, at a heating rate of 3 °C /min, from room temperature to 180 °C, and at 180 ° C for 2.5 h, in the first paragraph An inert gas;
- the temperature is raised to 400 °C at a heating rate of 3 °C /min, and kept at 400 °C for 20 minutes, and the first inert gas is introduced into the second stage;
- the temperature is raised to 890 °C at a heating rate of 5 °C /min, and kept at 890 °C for 1.5 h.
- the first reducing gas is required to pass through, the first reduction The gas is hydrogen.
- the first synthesis furnace is stopped and cooled to room temperature in two stages with natural cooling in the first synthesis furnace: the first stage, from 890 °C to 150 °C, the first stage is introduced into the first stage. Reducing gas; the second stage, from 150 ° C to room temperature, in the second stage, the first inert gas is passed through a nitrogen gas for protection.
- the second synthesis furnace adopts a second multi-stage heating and holding method to synthesize the primary composite particles in the second graphite boat, wherein the second plurality of segments
- the heating and heating method is a two-stage heating and holding method, namely: the first stage, at a heating rate of 10 ° C / min, from room temperature to 400 ° C, and kept at 400 ° C for 30 min, in the first paragraph a second inert gas; the second stage, after the first stage, the temperature is further increased to 890 ° C at a temperature increase rate of 7 ° C / min, and is kept at 890 ° C for 2 h, and the second reduction is introduced in the second stage.
- the gas, the second reducing gas is hydrogen.
- the first synthesis furnace and the second synthesis furnace are the same synthesis furnace, and the first graphite boat and the second graphite boat are the same graphite boat, the first quartz tube and the second The quartz tube is the same quartz tube, and in the secondary synthesis step, the second graphite boat and the second quartz tube are cleaned before use.
- the first synthesis furnace adopts a first multi-stage heating and holding method to synthesize the mixture in the first graphite boat, wherein the first plurality of stages are heated.
- the heat preservation method is a three-stage heating and holding method, that is, the first stage is heated at room temperature to 300 °C at a heating rate of 10 ° C /min, and is kept at 300 ° C for 2 h, and is first introduced in the first stage.
- the temperature is raised to 450 °C at a heating rate of 10 ° C /min, and the temperature is kept at 450 ° C for 10 minutes, and the first inert gas is introduced into the second stage;
- the temperature is raised to 950 °C at a heating rate of 10 °C/min, and the temperature is maintained at 950 °C for 0.5 h.
- a first reducing gas is introduced, and the first reducing gas is hydrogen.
- the first synthesis furnace stops heating and is cooled down to room temperature in two stages with natural cooling in the first synthesis furnace:
- the first stage from 950 ° C to 80 ° C, the first stage is passed first. Reducing gas; the second stage, from 80 ° C to room temperature, the first inert gas is introduced in the second stage.
- the second synthesis furnace adopts the second The section heating and holding method makes the synthesis of the first synthetic particles in the second graphite boat, wherein the second multi-stage heating and holding method is a two-stage heating and holding method, namely: the first section, at a heating rate of 20 ° C / min, The temperature is raised to 450 ° C at room temperature, and is kept at 450 ° C for 10 min, and a second inert gas is introduced into the first stage; the second stage is further heated to a temperature increase rate of 10 ° C / min after the first stage to At 950 ° C, and kept at 950 ° C for 1 h, a second reducing gas is introduced into the second stage, and the second reducing gas is hydrogen.
- the second multi-stage heating and holding method is a two-stage heating and holding method, namely: the first section, at a heating rate of 20 ° C / min, The temperature is raised to 450 ° C at room temperature, and is kept at 450 ° C for 10 min,
- the second synthesis furnace stops heating and is cooled in two stages with the second synthesis furnace to cool down to room temperature: the first stage, from 950 ° C to 80 ° C, in the first paragraph The second reducing gas; the second stage, from 80 ° C to room temperature, in the second section of the second inert gas.
- the first synthesis furnace and the second synthesis furnace are the same synthesis furnace, and the first graphite boat and the second graphite boat are the same graphite boat, the first stone
- the British tube and the second quartz tube are the same quartz tube, and in the secondary synthesis step, the second graphite boat and the second quartz tube are cleaned before use.
- the secondary composite (ie, cadmium telluride) product was inspected by inductively coupled plasma mass spectrometry (ICP-MS) (manufactured by PE, model: DRC-II).
- the test conditions for this device are: Temperature 18 °C -28 °C, relative humidity is 30-70%, cleanliness is 1000.
- Detection principle Inductively coupled plasma mass spectrometer detection method: After the element is subjected to plasma high-temperature ionization, it enters the mass analyzer in the form of positive charge. According to the difference of mass/charge ratio, it is received by the detector and generates a signal. The signal generated by the element to be tested and the reference material of the standard substance are worth the content of the element to be tested.
- Table 1 shows the test results of Examples 1-3.
- the cadmium telluride obtained by the present invention has a purity of 5N.
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Abstract
The present invention provides a method for preparing cadmium telluride, comprising primary synthesis and secondary synthesis. The primary synthesis comprises: mixing tellurium and cadmium and inputting the mixture into a first graphite boat that is put in a first quartz tube that is placed in a first synthesis furnace; inputting a first inert gas to evacuate air from the first quartz tube; performing first multi-section heating and heat preservation, inputting the first inert gas into a front section, and inputting a first reducing gas into a rear section; after the synthesis reaction, lowering the temperature into the room temperature section by section, inputting the first reducing gas in the front section and inputting the first inert gas into the rear section; obtaining a primary synthetic product. The secondary synthesis comprises: inputting the primary synthetic product into a second graphite boat that is put in a second quartz tube that is placed in a second synthesis furnace, and inputting a second inert gas to evacuate air from the second quartz tube; performing second multi-section heating and heat preservation, inputting the second inert gas into the front section, and inputting a second reducing gas into the rear section; after the synthesis reaction, stopping heating, lowering the temperature to the room temperature section by section, inputting the second reducing gas into the front section, and inputting the second inert gas into the rear section, so as to obtain a secondary synthetic product.
Description
碲化镉的制备方法 技术领域 Preparation method of cadmium telluride
本发明涉及一种合成材料的制备方法， 尤其涉及一种碲化镉的制备方 法。 背景技术 The present invention relates to a method for preparing a synthetic material, and more particularly to a method for preparing cadmium telluride. Background technique
当前碲化镉的制备存在有多种方法。 其中一种方法是将热棒插入碲和镉 的混合粉末中， 加热到 500°C而生成。 该方法采用热棒加热方式， 温度不够 均匀， 反应不够充分。 且采用了真空封管技术， 成本较高。 发明内容 There are various methods for preparing cadmium telluride. One of the methods is to insert a hot rod into a mixed powder of cerium and cadmium and heat it to 500 ° C to form. The method adopts a hot rod heating method, the temperature is not uniform enough, and the reaction is insufficient. And the vacuum sealing technology is adopted, and the cost is high. Summary of the invention
针对背景技术中存在的不足， 本发明的目的在于提供一种碲化镉的 制备方法， 其能使碲化镉合成加热均匀、 合成充分。 In view of the deficiencies in the prior art, an object of the present invention is to provide a method for preparing cadmium telluride which is capable of uniform heating and sufficient synthesis of cadmium telluride.
本发明的目的在于提供一种碲化镉的制备方法， 其能降低碲化镉的 制造成本。 It is an object of the present invention to provide a method for preparing cadmium telluride which can reduce the manufacturing cost of cadmium telluride.
为了实现本发明的目的， 本发明提供一种碲化镉的制备方法， 包括 一次合成步骤以及二次合成步骤。 In order to achieve the object of the present invention, the present invention provides a process for producing cadmium telluride comprising a primary synthesis step and a secondary synthesis step.
一次合成步骤包括： 将 5N 碲粉和 5N 镉粉按比例混合， 以获得混 料； 将混料装入到第一石墨舟内； 将装有混料的第一石墨舟放置到第一 石英管内； 将放置有第一石墨舟的第一石英管放置到第一合成炉内； 通 入第一惰性气体排空第一石英管内的空气； 在第一石英管内的空气被第 一惰性气体排空之后， 第一合成炉采用第一多段升温保温方式使得第一 石墨舟内的混料进行合成反应在第一多段升温保温中， 前段通入第一惰 性气体， 而后段通入第一还原气体； 合成反应之后， 第一合成炉停止加
热并分段降温至室温： 在分段降温至室温中， 前段通入第一还原气体， 后段通入第一惰性气体； 以及从第一石英管中取出第一石墨舟， 再从第 一石墨舟内取出一次合成物。 The one-step synthesis step comprises: mixing 5N tantalum powder and 5N cadmium powder in proportion to obtain a mixture; loading the mixture into the first graphite boat; placing the first graphite boat containing the mixture into the first quartz tube Place the first quartz tube on which the first graphite boat is placed into the first synthesis furnace; pass the first inert gas to evacuate the air in the first quartz tube; the air in the first quartz tube is evacuated by the first inert gas After that, the first synthesis furnace adopts the first multi-stage heating and heat preservation method to synthesize the mixture in the first graphite boat in the first multi-stage heating and warming, the first stage is introduced into the first inert gas, and the latter stage is introduced into the first reduction. Gas; after the synthesis reaction, the first synthesis furnace stops adding Heat and sub-cooling to room temperature: in the stepwise cooling to room temperature, the first section is introduced into the first reducing gas, the latter section is introduced into the first inert gas; and the first graphite boat is taken out from the first quartz tube, and then from the first The composition was taken out once in the graphite boat.
二次合成步骤包括： 将一次合成物破碎至规定尺寸的一次合成物颗 粒； 将一次合成物颗粒装入到第二石墨舟内； 将装有一次合成物颗粒的 第二石墨舟放置到第二石英管内； 将放置有第二石墨舟的第二石英管放 置到第二合成炉内； 通入第二惰性气体排空第二石英管内的空气； 在第 二石英管内的空气被第二惰性气体排空之后， 第二合成炉采用第二多段 升温保温方式使得第二石墨舟内的一次合成物颗粒合成反应， 且在第二 多段升温保温中， 前段通入第二惰性气体， 后段通入第二还原性气体； 合成反应之后， 第二合成炉停止加热并分段降温至室温， 在分段降温至 室温中， 前段通入第二还原性气体， 后段通入第二惰性气体； 以及从第 二石英管中取出第二石墨舟， 再从第二石墨舟内取出二次合成物。 The secondary synthesis step includes: crushing the primary composition to the primary composite particles of a prescribed size; loading the primary composite particles into the second graphite boat; and placing the second graphite boat containing the primary composite particles to the second Inside the quartz tube; placing a second quartz tube in which the second graphite boat is placed into the second synthesis furnace; introducing a second inert gas to evacuate the air in the second quartz tube; and the air in the second quartz tube is being subjected to the second inert gas After the emptying, the second synthesis furnace adopts a second multi-stage heating and holding method to synthesize the first synthetic particles in the second graphite boat, and in the second multi-stage heating and holding, the front section is introduced with the second inert gas, and the latter stage The second reducing gas is introduced; after the synthesis reaction, the second synthesis furnace stops heating and is cooled down to room temperature in stages, and is cooled to room temperature in sections, the second reducing gas is introduced into the front stage, and the second inert gas is introduced in the latter stage. And removing the second graphite boat from the second quartz tube and removing the secondary composition from the second graphite boat.
本发明的有益效果如下。 The beneficial effects of the present invention are as follows.
本发明提供的碲化镉的制备方法， 由于采用了石墨舟、 石英管、 以 及惰性气体和还原气体两次合成， 其能使碲化镉合成加热均匀、 合成充 分。 The preparation method of the cadmium telluride provided by the invention is synthesized by using a graphite boat, a quartz tube, and an inert gas and a reducing gas, which can make the cadmium telluride synthesis uniform and synthetically sufficient.
本发明提供的碲化镉的制备方法， 由于采用了石墨舟、 石英管、 以 及惰性气体和还原气体两次合成， 其能除去碲化镉中的氧元素， 从而提 高了碲化镉的纯度， 获得优质高纯的碲化镉。 The preparation method of the cadmium telluride provided by the invention adopts the graphite boat, the quartz tube, and the inert gas and the reducing gas to be synthesized twice, which can remove the oxygen element in the cadmium telluride, thereby improving the purity of the cadmium telluride. Obtain high quality and high purity cadmium telluride.
本发明提供的碲化镉的制备方法， 由于采用了石墨舟和石英管， 可 以降低碲化镉的制造成本。
具体实施方式 The method for preparing cadmium telluride provided by the invention can reduce the manufacturing cost of cadmium telluride by using graphite boat and quartz tube. detailed description
首先说明根据本发明的碲化镉的制备方法。 First, a method of preparing cadmium telluride according to the present invention will be described.
根据本发明的碲化镉的制备方法包括一次合成步骤和二次合成步 骤。 The method for producing cadmium telluride according to the present invention comprises a single synthesis step and a second synthesis step.
其中， 一次合成步骤包括： 将 5N 碲粉和 5N 镉粉按比例混合， 以 获得混料； 将混料装入到第一石墨舟内； 将装有混料的第一石墨舟放置 到第一石英管内； 将放置有第一石墨舟的第一石英管放置到第一合成炉 内； 通入第一惰性气体排空第一石英管内的空气； 在第一石英管内的空 气被第一惰性气体排空之后， 第一合成炉采用第一多段升温保温方式使 得第一石墨舟内的混料进行合成反应， 且在第一多段升温保温中， 前段 通入第一惰性气体， 而后段通入第一还原气体； 以及合成反应之后， 第 一合成炉停止加热并以多段降温至室温， 在多段降温至室温中， 前段通 入第一还原气体， 后段通入第一惰性气体； 从第一石英管中取出第一石 墨舟， 再从第一石墨舟内取出一次合成物。 Wherein, one synthesis step comprises: mixing 5N tantalum powder and 5N cadmium powder in proportion to obtain a mixture; loading the mixture into the first graphite boat; placing the first graphite boat containing the mixture to the first Inside the quartz tube; placing the first quartz tube in which the first graphite boat is placed into the first synthesis furnace; introducing the first inert gas to evacuate the air in the first quartz tube; the air in the first quartz tube is the first inert gas After the emptying, the first synthesis furnace adopts the first multi-stage heating and holding method to synthesize the mixture in the first graphite boat, and in the first multi-stage heating and holding, the first section is introduced with the first inert gas, and the latter section is passed. After the first reducing gas; and after the synthesis reaction, the first synthesis furnace stops heating and is cooled to room temperature in multiple stages, and is cooled to room temperature in multiple stages, the first reducing gas is introduced into the front stage, and the first inert gas is introduced in the latter stage; The first graphite boat was taken out from a quartz tube, and the composition was taken out from the first graphite boat.
其中， 二次合成步骤包括： 将一次合成物破碎至规定尺寸的一次合 成物颗粒； 将一次合成物颗粒装入到第二石墨舟内； 将装有一次合成物 颗粒的第二石墨舟放置到第二石英管内； 将放置有第二石墨舟的第二石 英管放置到第二合成炉内； 通入第二惰性气体排空第二石英管内的空气; 在第二石英管内的空气被第二惰性气体排空之后， 第二合成炉采用第二 多段升温保温方式使得第二石墨舟内的一次合成物颗粒合成反应， 在第 二多段升温保温中， 前段通入第二惰性气体， 后段通入第二还原性气体; 以及合成反应之后， 第二合成炉停止加热并分段降温至室温， 在分段降 温至室温中， 前段通入第二还原性气体， 后段通入第二惰性气体； 从第
二石英管中取出第二石墨舟， 再从第二石墨舟内取出二次合成物。 Wherein, the secondary synthesis step comprises: crushing the primary composition to the primary composite particles of a predetermined size; loading the primary composite particles into the second graphite boat; and placing the second graphite boat containing the primary composite particles into a second quartz tube placed in the second quartz tube; a second inert gas is introduced into the second quartz tube; the air in the second quartz tube is second; After the inert gas is emptied, the second synthesis furnace adopts a second multi-stage heating and holding method to synthesize the first synthetic particles in the second graphite boat. In the second multi-stage heating and holding, the front portion is introduced with the second inert gas, The second reducing gas is introduced into the section; and after the synthesis reaction, the second synthesis furnace stops heating and is cooled down to room temperature in sections, and is cooled to room temperature in sections, the second reducing gas is introduced into the front stage, and the second reducing gas is introduced in the front stage. Inert gas; from the first The second graphite boat was taken out from the two quartz tubes, and the secondary composition was taken out from the second graphite boat.
在根据本发明所述的碲化镉的制备方法中， 在一次合成步骤中， 5N 碲 In the preparation method of cadmium telluride according to the present invention, 5N 碲 in one synthesis step
粉和 5N 镉粉的混合比例可为摩尔比 1 : 1。优选地， 5N 碲粉和 5N 镉 粉的颗粒尺寸为 0.5~5mm。 The mixing ratio of the powder and the 5N cadmium powder may be a molar ratio of 1:1. Preferably, the 5N tantalum powder and the 5N cadmium powder have a particle size of 0.5 to 5 mm.
在根据本发明所述的碲化镉的制备方法中， 在所述一次合成步骤中， 所述第一多段升温保温可为三段升温保温： 第一段， 以 2~10 °C/min 的升 温速率， 从室温升温至 150~300°C， 保温 2~6h， 在第一段中通入第一惰 性气体； 第二段， 以 2~10 °C/min 的升温速率， 继续升温至 380~450 °C， 保温 10~60min， 在第二段中通入第一惰性气体； 以及第三段， 以 2~10 °C /min 的升温速率， 继续升温至 850~950°C， 保温 0.5~2h， 在第三段中 通入第一还原气体。 其中， 第一段和第二段可定义为前段， 而第三段可 定义为后段。 In the method for preparing cadmium telluride according to the present invention, in the first synthesis step, the first multi-stage heating and holding may be three-stage heating and holding: the first stage, at 2 to 10 ° C/min The heating rate is raised from room temperature to 150~300 °C, and the temperature is kept for 2~6h. The first inert gas is introduced into the first stage. The second stage is heated to the temperature rising rate of 2~10 °C/min. 380~450 °C, keep warm for 10~60min, pass the first inert gas in the second stage; and the third stage, continue to raise the temperature to 850~950°C at the heating rate of 2~10 °C /min, keep warm 0.5~2h, the first reducing gas is introduced into the third stage. Among them, the first paragraph and the second paragraph can be defined as the front segment, and the third segment can be defined as the latter segment.
在根据本发明所述的碲化镉的制备方法中， 在所述一次合成步骤中， 所述分段降温至室温为随第一合成炉自然冷却的两段降温至室温： 第一 段， 从 850~950 °C降至 200~80°C， 在第一段中通入第一还原性气体； 第 二段， 从 200~80°C降至室温， 在第二段中通入第一惰性气体。 其中第一 段可定义为前段， 而第二段定义为后段。 In the method for preparing cadmium telluride according to the present invention, in the one-step synthesis step, the section is cooled to room temperature to cool down to room temperature with two stages of natural cooling of the first synthesis furnace: 850~950 °C down to 200~80 °C, the first reducing gas is introduced in the first stage; the second stage is from 200~80 °C to room temperature, and the first inertia is introduced in the second stage. gas. The first paragraph can be defined as the front segment and the second segment is defined as the latter segment.
在根据本发明所述的碲化镉的制备方法中， 在所述二次合成步骤中， 所述将一次合成物破碎的规定尺寸可为 0.5~5mm。 In the method for producing cadmium telluride according to the present invention, in the secondary synthesis step, the predetermined size for breaking the primary composition may be 0.5 to 5 mm.
在根据本发明所述的碲化镉的制备方法中， 在所述二次合成步骤中， 所述第二多段升温保温可为两段升温保温： 第一段， 以 5~20 °C/min 的升 温速率， 从室温升至 380~450 °C， 保温 10~60min， 在第一段中通入第二
惰性气体；以及第二段，以 2~10°C/min 的升温速率，继续升温至 850~950 °C， 保温 l~2.5h， 在第二段中通入第二还原性气体。 其中， 第一段可定 义为前段， 而第二段定义为后段。 In the method for preparing cadmium telluride according to the present invention, in the second synthesis step, the second multi-stage heating and holding may be two-stage heating and warming: the first stage, at 5 to 20 ° C / The heating rate of min increases from room temperature to 380~450 °C, keeps warm for 10~60min, and enters the second in the first stage. The inert gas; and the second stage, at a temperature increase rate of 2 to 10 ° C / min, continue to raise the temperature to 850 ~ 950 ° C, heat l ~ 2.5h, in the second stage into the second reducing gas. Among them, the first paragraph can be defined as the front segment, and the second segment is defined as the latter segment.
在根据本发明所述的碲化镉的制备方法中， 在所述二次合成步骤中， 所述分段降温至室温为随第二合成炉自然冷却的两段降温至室温： 第一 段， 从 850~950°C降至 200~80°C， 在第一段中通入第二还原性气体； 第 二段， 从 200~80°C降至室温， 在第二段中通入第二惰性气体。 其中， 第 一段可定义为前段， 而第二段定义为后段。 In the method for preparing cadmium telluride according to the present invention, in the secondary synthesis step, the stepwise cooling to room temperature is to cool down to room temperature with two stages of natural cooling of the second synthesis furnace: From 850~950°C to 200~80°C, the second reducing gas is introduced into the first section; the second section is from 200~80°C to room temperature, and the second section is passed to the second. Inert gas. Among them, the first paragraph can be defined as the front segment, and the second segment is defined as the latter segment.
在根据本发明所述的碲化镉的制备方法中， 所述一次合成步骤中的 第一石墨舟可为高温水淬石墨舟， 所述二次合成步骤中的第二石墨舟可 为高温水淬石墨舟。 In the method for preparing cadmium telluride according to the present invention, the first graphite boat in the primary synthesis step may be a high temperature water quenched graphite boat, and the second graphite boat in the secondary synthesis step may be high temperature water. Quenched graphite boat.
在根据本发明所述的碲化镉的制备方法中， 所述一次合成步骤中的 第一惰性气体可为氮气， 所述二次合成步骤中的第二惰性气体可为氮气。 In the method for producing cadmium telluride according to the present invention, the first inert gas in the primary synthesis step may be nitrogen, and the second inert gas in the secondary synthesis step may be nitrogen.
在根据本发明所述的碲化镉的制备方法中， 在根据本发明所述的碲 化镉的制备方法中， 所述一次合成步骤中的第一还原性气体可为氢气， 所述二次合成步骤中的第二还原性气体可为氢气。 In the method for producing cadmium telluride according to the present invention, in the method for producing cadmium telluride according to the present invention, the first reducing gas in the primary synthesis step may be hydrogen, the second The second reducing gas in the synthesis step may be hydrogen.
在根据本发明所述的碲化镉的制备方法中， 所述一次合成步骤中的 第一合成炉和所述二次合成步骤中的第二合成炉为可同一或不同的合成 炉。 当所述一次合成步骤中的第一合成炉和所述二次合成步骤中的第二 合成炉为同一合成炉时， 可用于少量制备的碲化镉。 当所述一次合成步 骤中的第一合成炉和所述二次合成步骤中的第二合成炉为不同的合成炉 时， 可用于大规模地制备碲化镉。 In the method for producing cadmium telluride according to the present invention, the first synthesis furnace in the primary synthesis step and the second synthesis furnace in the secondary synthesis step are synthetic furnaces which may be the same or different. When the first synthesis furnace in the one-time synthesis step and the second synthesis furnace in the secondary synthesis step are the same synthesis furnace, it can be used for a small amount of prepared cadmium telluride. When the first synthesis furnace in the one synthesis step and the second synthesis furnace in the secondary synthesis step are different synthesis furnaces, it can be used to prepare cadmium telluride on a large scale.
在根据本发明所述的碲化镉的制备方法中， 所述一次合成步骤中的
第一石墨舟和所述二次合成步骤中的第二石墨舟可为同一或不同的石墨 舟。 当所述一次合成步骤中的第一石墨舟和所述二次合成步骤中的第二 石墨舟为同一石墨舟时， 在所述二次合成步骤中在第二石墨舟使用前进 行清洁处理， 可用于少量制备的碲化镉。 当所述一次合成步骤中的第一 石墨舟和所述二次合成步骤中的第二石墨舟为不同的石墨舟时， 可用于 大规模地制备碲化镉。 In the method for producing cadmium telluride according to the present invention, in the one-time synthesis step The first graphite boat and the second graphite boat in the secondary synthesis step may be the same or different graphite boats. When the first graphite boat in the one-time synthesis step and the second graphite boat in the second synthesis step are the same graphite boat, in the second synthesis step, the second graphite boat is cleaned before use, Can be used for small amounts of prepared cadmium telluride. When the first graphite boat in the one-time synthesis step and the second graphite boat in the secondary synthesis step are different graphite boats, it can be used to prepare cadmium telluride on a large scale.
在根据本发明所述的碲化镉的制备方法中， 所述一次合成步骤中的 第一石英管和所述二次合成步骤中的第二石英管为同一或不同的石英 管。 当所述一次合成步骤中的第一石英管和所述二次合成步骤中的第二 石英管为同一石英管时， 在所述二次合成步骤中在第二石英管使用前进 行清洁处理， 可用于少量制备的碲化镉。 当所述一次合成步骤中的第一 石英管和所述二次合成步骤中的第二石英管为不同的石英管时， 可用于 大规模地制备碲化镉。 In the method for producing cadmium telluride according to the present invention, the first quartz tube in the primary synthesis step and the second quartz tube in the secondary synthesis step are the same or different quartz tubes. When the first quartz tube in the one-step synthesis step and the second quartz tube in the second-synthesis step are the same quartz tube, in the second synthesis step, the second quartz tube is cleaned before use, Can be used for small amounts of prepared cadmium telluride. When the first quartz tube in the one-step synthesis step and the second quartz tube in the secondary synthesis step are different quartz tubes, it can be used to prepare cadmium telluride on a large scale.
在根据本发明所述的碲化镉的制备方法中， 还可包括步骤： 在获得 二次合成物之后， 进行精细破碎及筛分， 以获得不同粒度的二次合成物。 In the method for producing cadmium telluride according to the present invention, the method may further include the steps of: after obtaining the secondary composition, performing fine crushing and sieving to obtain secondary compositions of different particle sizes.
其次说明根据本发明的碲化镉的制备方法的实施例。 Next, an embodiment of a method for producing cadmium telluride according to the present invention will be described.
实施例 1 Example 1
A: 一次合成步骤 A: One synthesis step
(al) 将 5N 碲粉和 5N 镉粉颗粒尺寸为 0.5~2mm， 按摩尔比 1 : 1 均 匀混合， 以获得混料； (al) The particle size of 5N tantalum powder and 5N cadmium powder is 0.5~2mm, and uniformly mixed according to a molar ratio of 1:1 to obtain a mixture;
(a2) 将混料装入到第一石墨舟内， 第一石墨舟为高温水淬石墨舟； (a2) loading the mixture into the first graphite boat, the first graphite boat being a high temperature water quenched graphite boat;
(a3) 将装有混料的第一石墨舟放置到第一石英管内； (a3) placing the first graphite boat containing the mixture into the first quartz tube;
(a4) 将放置有第一石墨舟的第一石英管放置到第一合成炉内；
(a5) 通入第一惰性气体排空第一石英管内的空气， 第一惰性气体为 (a4) placing the first quartz tube on which the first graphite boat is placed into the first synthesis furnace; (a5) introducing a first inert gas to evacuate air in the first quartz tube, the first inert gas is
(a6) 在第一石英管内的空气被第一惰性气体排空之后， 第一合成炉 采用第一多段升温保温方式使得第一石墨舟内的混料进行合成反应， 其 中第一多段升温保温方式为三段升温保温方式， BP : 第一段， 以 2°C/min 的升温速率， 从室温升温至 150°C， 并在 150°C保温 6h， 在第一段中通入 第一惰性气体； 第二段， 在第一段之后以 3 °C/min 的升温速率， 继续升 温至 380°C， 并在 380°C保温 60min， 在第二段中通入第一惰性气体； 第 三段， 在第二段之后以 2 °C/min 的升温速率， 继续升温至 850°C， 并在 850°C保温 2h，在第三段中通入第一还原性气体，第一还原性气体为氢气； (a7)合成反应之后，第一合成炉停止加热并分两段随第一合成炉自然 冷却降温至室温： 第一段， 从 850°C降至 200°C， 在第一段通入第一还原 性气体； 第二段， 从 200 °C降至室温， 在第二段通入第一惰性气体。(a6) After the air in the first quartz tube is emptied by the first inert gas, the first synthesis furnace adopts a first multi-stage heating and holding method to synthesize the mixture in the first graphite boat, wherein the first plurality of stages are heated. The insulation method is three-stage heating and holding method, BP: the first section, the temperature rises from room temperature to 150 °C at a heating rate of 2 °C/min, and is kept at 150 °C for 6 hours, and the first section is passed. Inert gas; the second stage, after the first stage, at a heating rate of 3 °C / min, continue to raise the temperature to 380 ° C, and incubated at 380 ° C for 60 min, the first inert gas is introduced in the second stage; In the third stage, after the second stage, the temperature is raised to 850 ° C at a heating rate of 2 ° C / min, and kept at 850 ° C for 2 h, and the first reducing gas is introduced into the third stage, the first reducing property The gas is hydrogen; (a7) After the synthesis reaction, the first synthesis furnace stops heating and is cooled in two stages with the first synthesis furnace to cool down to room temperature: the first stage, from 850 ° C to 200 ° C, in the first stage Passing the first reducing gas; the second stage, from 200 ° C to room temperature, in the first An inert gas into the first section.
ι8)从第一石英管中取出第一石墨舟，再从第一石墨舟内取出一次合 成物。 I 8) The first graphite boat was taken out from the first quartz tube, and the resultant was taken out from the first graphite boat.
Β. 二次合成步骤 Β. Secondary synthesis step
(bl) 将一次合成物破碎至 0.5mm 的一次合成物颗粒； (bl) crushing the primary composition to 0.5 mm of primary composite particles;
(b2) 将一次合成物颗粒装入到第二石墨舟内， 第二石墨舟为高温水 淬石墨舟； (b2) loading the primary composite particles into the second graphite boat, the second graphite boat being a high temperature water quenched graphite boat;
(b3) 将装有一次合成物颗粒的第二石墨舟放置到第二石英管内； (b3) placing a second graphite boat containing the primary composite particles into the second quartz tube;
(b4) 将放置有第二石墨舟的第二石英管放置到第二合成炉内； (b4) placing a second quartz tube in which the second graphite boat is placed into the second synthesis furnace;
(b5) 通入第二惰性气体排空第二石英管内的空气， 第二惰性气体为
(b6) 在第二石英管内的空气被第二惰性气体排空之后， 第二合成炉 采用第二多段升温保温方式使得第二石墨舟内的一次合成物颗粒合成反 应， 其中第二多段升温保温方式为两段升温保温方式， 即： 第一段， 以 5 °C/min 的升温速率， 从室温升至 380°C， 并在 380°C保温 60min， 在第一 段中通入第二惰性气体； 第二段， 在第一段之后以 2°C/min 的升温速率， 继续升温至 850°C， 并在 850°C保温 2.5h， 在第二段中通入第二还原性气 体， 第二还原性气体为氢气。 (b5) introducing a second inert gas to evacuate air in the second quartz tube, the second inert gas is (b6) After the air in the second quartz tube is emptied by the second inert gas, the second synthesis furnace adopts a second multi-stage heating and holding method to synthesize the primary composite particles in the second graphite boat, wherein the second plurality of segments The heating and warming method is a two-stage heating and holding method, namely: the first section, rising from room temperature to 380 °C at a heating rate of 5 °C/min, and holding at 380 °C for 60 min, in the first section a second inert gas; the second stage, after the first stage, the temperature is further increased to 850 ° C at a temperature increase rate of 2 ° C / min, and is kept at 850 ° C for 2.5 h, and a second reduction is introduced in the second stage. The second reducing gas is hydrogen.
(b7) 合成反应之后， 第二合成炉停止加热并分两段随第二合成炉自 然冷却降温至室温： 第一段， 从 850°C降至 120°C， 在第一段中通入第二 还原性气体；第二段，从 120°C降至室温，在第二段中通入第二惰性气体。 (b7) After the synthesis reaction, the second synthesis furnace is stopped and cooled to room temperature in two stages with natural cooling in the second synthesis furnace: the first stage, from 850 ° C to 120 ° C, in the first paragraph a second reducing gas; the second stage, from 120 ° C to room temperature, in the second section of the second inert gas.
(b8) 从第二石英管中取出第二石墨舟， 再从第二石墨舟内取出二次 合成物。 (b8) The second graphite boat was taken out from the second quartz tube, and the secondary composition was taken out from the second graphite boat.
在实施例 1 的一次合成步骤和二次合成步骤中， 第一合成炉和第二 合成炉为同一合成炉， 第一石墨舟和第二石墨舟为同一石墨舟， 第一石 英管和第二石英管为同一石英管， 且在二次合成步骤中， 在第二石墨舟 和第二石英管使用前进行清洁处理。 In the first synthesis step and the second synthesis step of Embodiment 1, the first synthesis furnace and the second synthesis furnace are the same synthesis furnace, and the first graphite boat and the second graphite boat are the same graphite boat, the first quartz tube and the second The quartz tube is the same quartz tube, and in the secondary synthesis step, the second graphite boat and the second quartz tube are cleaned before use.
C. 精细破碎及筛分 C. Fine crushing and screening
在获得二次合成物之后， 进行精细破碎及筛分， 以获得不同粒度的 二次合成物。 After the secondary composition is obtained, fine crushing and sieving are carried out to obtain secondary compositions of different particle sizes.
实施例 2 Example 2
A: 一次合成步骤 A: One synthesis step
(al) 将 5N 碲粉和 5N 镉粉颗粒尺寸为 2~3.5mm， 按摩尔比 1 : 1 均 匀混合， 以获得混料；
(a2) 将混料装入到第一石墨舟内， 第一石墨舟为高温水淬石墨舟；(al) The 5N tantalum powder and the 5N cadmium powder have a particle size of 2 to 3.5 mm, and are uniformly mixed at a molar ratio of 1:1 to obtain a mixture; (a2) loading the mixture into the first graphite boat, the first graphite boat being a high temperature water quenched graphite boat;
(a3) 将装有混料的第一石墨舟放置到第一石英管内； (a3) placing the first graphite boat containing the mixture into the first quartz tube;
(a4) 将放置有第一石墨舟的第一石英管放置到第一合成炉内； (a4) placing the first quartz tube on which the first graphite boat is placed into the first synthesis furnace;
(a5) 通入第一惰性气体排空第一石英管内的空气， 第一惰性气体为 (a5) introducing a first inert gas to evacuate air in the first quartz tube, the first inert gas is
(a6) 在第一石英管内的空气被第一惰性气体排空之后， 第一合成炉 采用第一多段升温保温方式使得第一石墨舟内的混料进行合成反应， 其 中第一多段升温保温方式为三段升温保温方式， 即： 第一段， 以 3 °C /min 的升温速率， 从室温升温至 180 °C， 并在 180°C保温 2.5h， 在第一段中通 入第一惰性气体； (a6) After the air in the first quartz tube is emptied by the first inert gas, the first synthesis furnace adopts a first multi-stage heating and holding method to synthesize the mixture in the first graphite boat, wherein the first plurality of stages are heated. The heat preservation method is three-stage heating and holding method, namely: the first stage, at a heating rate of 3 °C /min, from room temperature to 180 °C, and at 180 ° C for 2.5 h, in the first paragraph An inert gas;
第二段， 在第一段之后以 3 °C /min 的升温速率， 继续升温至 400 °C， 并在 400°C保温 20min， 在第二段中通入第一惰性气体； 第三段， 在第二 段之后以 5 °C /min 的升温速率，继续升温至 890 °C，并在 890 °C保温 1.5h， 在第三段该过程中需要通入第一还原性气体， 第一还原性气体为氢气。 In the second stage, after the first stage, the temperature is raised to 400 °C at a heating rate of 3 °C /min, and kept at 400 °C for 20 minutes, and the first inert gas is introduced into the second stage; After the second stage, the temperature is raised to 890 °C at a heating rate of 5 °C /min, and kept at 890 °C for 1.5 h. In the third stage, the first reducing gas is required to pass through, the first reduction The gas is hydrogen.
(a7) 合成反应之后， 第一合成炉停止加热并分两段随第一合成炉自 然冷却降温至室温： 第一段， 从 890 °C降至 150°C， 在第一阶段通入第一 还原性气体； 第二段， 从 150°C降至室温， 在第二段通入第一惰性气体通 入氮气进行保护。 (a7) After the synthesis reaction, the first synthesis furnace is stopped and cooled to room temperature in two stages with natural cooling in the first synthesis furnace: the first stage, from 890 °C to 150 °C, the first stage is introduced into the first stage. Reducing gas; the second stage, from 150 ° C to room temperature, in the second stage, the first inert gas is passed through a nitrogen gas for protection.
(a8) 从第一石英管中取出第一石墨舟， 再从第一石墨舟内取出一次 合成物。 (a8) The first graphite boat was taken out from the first quartz tube, and the composite was taken out from the first graphite boat.
B. 二次合成步骤 B. Secondary synthesis step
(bl) 将一次合成物破碎至 0.7mm 的一次合成物颗粒； (bl) crushing the primary composition to a primary composite particle of 0.7 mm;
(b2) 将一次合成物颗粒装入到第二石墨舟内， 第二石墨舟为高温水
淬石墨舟； (b2) loading the primary composite particles into the second graphite boat, the second graphite boat being high temperature water Quenched graphite boat;
(b3) 将装有一次合成物颗粒的第二石墨舟放置到第二石英管内； (b3) placing a second graphite boat containing the primary composite particles into the second quartz tube;
(b4) 将放置有第二石墨舟的第二石英管放置到第二合成炉内；(b4) placing a second quartz tube in which the second graphite boat is placed into the second synthesis furnace;
(b5) 通入第二惰性气体排空第二石英管内的空气， 第二惰性气体为 (b5) introducing a second inert gas to evacuate air in the second quartz tube, the second inert gas is
(b6) 在第二石英管内的空气被第二惰性气体排空之后， 第二合成炉 采用第二多段升温保温方式使得第二石墨舟内的一次合成物颗粒合成反 应， 其中第二多段升温保温方式为两段升温保温方式， 即： 第一段， 以 10°C/min 的升温速率， 从室温升至 400°C， 并在 400°C保温 30min， 在第 一段中通入第二惰性气体； 第二段， 在第一段之后以 7°C/min 的升温速 率， 继续升温至 890°C， 并在 890°C保温 2h， 在第二段中通入第二还原性 气体， 第二还原性气体为氢气。 (b6) After the air in the second quartz tube is emptied by the second inert gas, the second synthesis furnace adopts a second multi-stage heating and holding method to synthesize the primary composite particles in the second graphite boat, wherein the second plurality of segments The heating and heating method is a two-stage heating and holding method, namely: the first stage, at a heating rate of 10 ° C / min, from room temperature to 400 ° C, and kept at 400 ° C for 30 min, in the first paragraph a second inert gas; the second stage, after the first stage, the temperature is further increased to 890 ° C at a temperature increase rate of 7 ° C / min, and is kept at 890 ° C for 2 h, and the second reduction is introduced in the second stage. The gas, the second reducing gas is hydrogen.
(b7) 合成反应之后， 第二合成炉停止加热并分两段随第二合成炉自 然冷却降温至室温： 第一段， 从 890°C降至 200°C， 在第一段中通入第二 还原性气体；第二段，从 200 °C降至室温，在第二段中通入第二惰性气体。 (b7) After the synthesis reaction, the second synthesis furnace is stopped and cooled down to room temperature in two stages with natural cooling in the second synthesis furnace: The first stage, from 890 ° C to 200 ° C, in the first paragraph The second reducing gas; the second stage, from 200 ° C to room temperature, a second inert gas is introduced into the second stage.
(b8) 从第二石英管中取出第二石墨舟， 再从第二石墨舟内取出二次 合成物。 (b8) The second graphite boat was taken out from the second quartz tube, and the secondary composition was taken out from the second graphite boat.
在实施例 2 的一次合成步骤和二次合成步骤中， 第一合成炉和第二 合成炉为同一合成炉， 第一石墨舟和第二石墨舟为同一石墨舟， 第一石 英管和第二石英管为同一石英管， 且在二次合成步骤中， 在第二石墨舟 和第二石英管使用前进行清洁处理。 In the first synthesis step and the second synthesis step of Embodiment 2, the first synthesis furnace and the second synthesis furnace are the same synthesis furnace, and the first graphite boat and the second graphite boat are the same graphite boat, the first quartz tube and the second The quartz tube is the same quartz tube, and in the secondary synthesis step, the second graphite boat and the second quartz tube are cleaned before use.
C. 精细破碎及筛分 C. Fine crushing and screening
在获得二次合成物之后， 进行精细破碎及筛分， 以获得不同粒度的
二次合成物。 After obtaining the secondary composition, finely crushing and sieving to obtain different particle sizes Secondary composition.
实施例 3 Example 3
A: 一次合成步骤 A: One synthesis step
(al) 将 5N 碲粉和 5N 镉粉，颗粒尺寸为 3.5~5mm，按摩尔比 1 : 1 均 匀混合， 以获得混料； (al) 5N tantalum powder and 5N cadmium powder, the particle size is 3.5~5mm, and the molar ratio is 1:1 uniformly mixed to obtain the mixture;
(a2) 将混料装入到第一石墨舟内， 第一石墨舟为高温水淬石墨舟； (a3) 将装有混料的第一石墨舟放置到第一石英管内； (a2) loading the mixture into the first graphite boat, the first graphite boat being a high temperature water quenched graphite boat; (a3) placing the first graphite boat containing the mixture into the first quartz tube;
(a4) 将放置有第一石墨舟的第一石英管放置到第一合成炉内； (a5) 通入第一惰性气体排空第一石英管内的空气， 第一惰性气体为 氮气； (a4) placing a first quartz tube in which the first graphite boat is placed into the first synthesis furnace; (a5) introducing a first inert gas to evacuate air in the first quartz tube, the first inert gas being nitrogen;
(a6) 在第一石英管内的空气被第一惰性气体排空之后， 第一合成炉 采用第一多段升温保温方式使得第一石墨舟内的混料进行合成反应， 其 中第一多段升温保温方式为三段升温保温方式， 即：第一段， 以 10°C /min 的升温速率， 从室温升温至 300 °C， 并在 300°C保温 2h， 在第一段中通入 第一惰性气体； (a6) After the air in the first quartz tube is emptied by the first inert gas, the first synthesis furnace adopts a first multi-stage heating and holding method to synthesize the mixture in the first graphite boat, wherein the first plurality of stages are heated. The heat preservation method is a three-stage heating and holding method, that is, the first stage is heated at room temperature to 300 °C at a heating rate of 10 ° C /min, and is kept at 300 ° C for 2 h, and is first introduced in the first stage. Inert gas
第二段，在第一段之后以 10°C /min 的升温速率，继续升温至 450 °C， 并在 450°C保温 lOmin, 在第二段中通入第一惰性气体； 第三段， 在第二 段之后以 10 °C/min 的升温速率，继续升温至 950 °C，并在 950 °C保温 0.5h， 在第三段中通入第一还原性气体， 第一还原性气体为氢气。 In the second stage, after the first stage, the temperature is raised to 450 °C at a heating rate of 10 ° C /min, and the temperature is kept at 450 ° C for 10 minutes, and the first inert gas is introduced into the second stage; After the second stage, the temperature is raised to 950 °C at a heating rate of 10 °C/min, and the temperature is maintained at 950 °C for 0.5 h. In the third stage, a first reducing gas is introduced, and the first reducing gas is hydrogen.
(a7) 合成反应之后， 第一合成炉停止加热并分两段随第一合成炉自 然冷却降温至室温： 第一段， 从 950°C降至 80 °C， 在第一段通入第一还 原性气体； 第二段， 从 80°C降至室温， 在第二段通入第一惰性气体。 (a7) After the synthesis reaction, the first synthesis furnace stops heating and is cooled down to room temperature in two stages with natural cooling in the first synthesis furnace: The first stage, from 950 ° C to 80 ° C, the first stage is passed first. Reducing gas; the second stage, from 80 ° C to room temperature, the first inert gas is introduced in the second stage.
(a8) 从第一石英管中取出第一石墨舟， 再从第一石墨舟内取出一次
合成物。 (a8) Take out the first graphite boat from the first quartz tube and take it out from the first graphite boat. Composition.
B. 二次合成步骤 B. Secondary synthesis step
(bl) 将一次合成物破碎至 5mm 的一次合成物颗粒； (bl) crushing the primary composition to 5 mm of primary composite particles;
(b2) 将一次合成物颗粒装入到第二石墨舟内， 第二石墨舟为高温水 淬石墨舟； (b2) loading the primary composite particles into the second graphite boat, the second graphite boat being a high temperature water quenched graphite boat;
(b3) 将装有一次合成物颗粒的第二石墨舟放置到第二石英管内； (b3) placing a second graphite boat containing the primary composite particles into the second quartz tube;
(b4) 将放置有第二石墨舟的第二石英管放置到第二合成炉内；(b4) placing a second quartz tube in which the second graphite boat is placed into the second synthesis furnace;
(b5) 通入第二惰性气体排空第二石英管内的空气， 第二惰性气体为 (b6) 在第二石英管内的空气被第二惰性气体排空之后， 第二合成炉 采用第二多段升温保温方式使得第二石墨舟内的一次合成物颗粒合成反 应， 其中第二多段升温保温方式为两段升温保温方式， 即： 第一段， 以 20°C/min 的升温速率， 从室温升至 450°C， 并在 450°C保温 lOmin, 在第 一段中通入第二惰性气体； 第二段， 在第一段之后以 10°C/min 的升温速 率， 继续升温至 950°C， 并在 950°C保温 lh， 在第二段中通入第二还原性 气体， 第二还原性气体为氢气。 (b5) introducing a second inert gas to evacuate air in the second quartz tube, and the second inert gas is (b6) after the air in the second quartz tube is emptied by the second inert gas, the second synthesis furnace adopts the second The section heating and holding method makes the synthesis of the first synthetic particles in the second graphite boat, wherein the second multi-stage heating and holding method is a two-stage heating and holding method, namely: the first section, at a heating rate of 20 ° C / min, The temperature is raised to 450 ° C at room temperature, and is kept at 450 ° C for 10 min, and a second inert gas is introduced into the first stage; the second stage is further heated to a temperature increase rate of 10 ° C / min after the first stage to At 950 ° C, and kept at 950 ° C for 1 h, a second reducing gas is introduced into the second stage, and the second reducing gas is hydrogen.
(b7) 合成反应之后， 第二合成炉停止加热并分两段随第二合成炉自 然冷却降温至室温： 第一段， 从 950°C降至 80°C， 在第一段中通入第二 还原性气体； 第二段， 从 80°C降至室温， 在第二段中通入第二惰性气体。 (b7) After the synthesis reaction, the second synthesis furnace stops heating and is cooled in two stages with the second synthesis furnace to cool down to room temperature: the first stage, from 950 ° C to 80 ° C, in the first paragraph The second reducing gas; the second stage, from 80 ° C to room temperature, in the second section of the second inert gas.
(b8) 从第二石英管中取出第二石墨舟， 再从第二石墨舟内取出二次 合成物。 (b8) The second graphite boat was taken out from the second quartz tube, and the secondary composition was taken out from the second graphite boat.
在实施例 3 的一次合成步骤和二次合成步骤中， 第一合成炉和第二 合成炉为同一合成炉， 第一石墨舟和第二石墨舟为同一石墨舟， 第一石
英管和第二石英管为同一石英管， 且在二次合成步骤中， 在第二石墨舟 和第二石英管使用前进行清洁处理。 In the first synthesis step and the second synthesis step of Embodiment 3, the first synthesis furnace and the second synthesis furnace are the same synthesis furnace, and the first graphite boat and the second graphite boat are the same graphite boat, the first stone The British tube and the second quartz tube are the same quartz tube, and in the secondary synthesis step, the second graphite boat and the second quartz tube are cleaned before use.
C. 精细破碎及筛分 C. Fine crushing and screening
在获得二次合成物之后， 进行精细破碎及筛分， 以获得不同粒度的 二次合成物。 After the secondary composition is obtained, fine crushing and sieving are carried out to obtain secondary compositions of different particle sizes.
最后给出测试结果。 Finally, the test results are given.
二次合成物（即碲化镉）产品采用电感耦合等离子体质谱仪（ICP-MS ) 进行检测 （生产厂家为 PE 公司， 型号为： DRC-II ) ， 该设备的检 测条件为： 温度为 18°C -28 °C， 相对湿度为 30-70%, 洁净度为 1000 级。 检测原理： 电感耦合等离子体质谱仪检测方式： 待测元素经过等离子体 高温电离后， 以正电荷形式进入质量分析器， 根据质量 /电荷比的差异， 被检测器接收， 产生信号。 待测元素产生的信号和标准物质该元素信号 比值得出待测元素含量。 The secondary composite (ie, cadmium telluride) product was inspected by inductively coupled plasma mass spectrometry (ICP-MS) (manufactured by PE, model: DRC-II). The test conditions for this device are: Temperature 18 °C -28 °C, relative humidity is 30-70%, cleanliness is 1000. Detection principle: Inductively coupled plasma mass spectrometer detection method: After the element is subjected to plasma high-temperature ionization, it enters the mass analyzer in the form of positive charge. According to the difference of mass/charge ratio, it is received by the detector and generates a signal. The signal generated by the element to be tested and the reference material of the standard substance are worth the content of the element to be tested.
表 1 给出了实施例 1-3 的测试结果 Table 1 shows the test results of Examples 1-3.
表 1 实施例 1-3 的二次合成物测试结果 （单位： ppm) Table 1 Test results of the secondary composition of Examples 1-3 (unit: ppm)
a里 实施例 1 实施例 2 实施例 3 杂质元素 a Example 1 Example 2 Example 3 Impurity elements
Ag 0.40 0.38 0.34 Ag 0.40 0.38 0.34
A1 0.50 0.48 0.46 A1 0.50 0.48 0.46
As 0.50 0.43 0.40 As 0.50 0.43 0.40
Bi 0.50 0.40 0.30 Bi 0.50 0.40 0.30
Ca 0.20 0.30 0.50
Cr 1.00 0.92 0.80Ca 0.20 0.30 0.50 Cr 1.00 0.92 0.80
Cu 0.50 0.40 0.60Cu 0.50 0.40 0.60
Fe 0.50 0.30 0.70Fe 0.50 0.30 0.70
Mg 0.50 0.30 0.20Mg 0.50 0.30 0.20
Mn 0.50 0.40 0.45Mn 0.50 0.40 0.45
Na 1.00 0.50 0.80Na 1.00 0.50 0.80
Ni 0.50 0.40 0.44Ni 0.50 0.40 0.44
Pb 0.50 0.42 0.80Pb 0.50 0.42 0.80
Se 1.00 0.80 1.20Se 1.00 0.80 1.20
Si 0.50 0.30 0.80Si 0.50 0.30 0.80
Sn 0.50 0.40 0.20Sn 0.50 0.40 0.20
Zn 0.50 0.20 0.10 合计 9.60 7.33 9.09 从表 1 看出， 本发明获得的碲化镉达到 5N 纯度。
Zn 0.50 0.20 0.10 Total 9.60 7.33 9.09 As seen from Table 1, the cadmium telluride obtained by the present invention has a purity of 5N.
Claims
1. 一种碲化镉的制备方法， 包括： A method for preparing cadmium telluride, comprising:
一次合成步骤， 包括： A synthesis step, including:
5 将 5N 碲粉和 5N 镉粉按比例混合， 以获得混料； 5 Mix 5N tantalum powder and 5N cadmium powder in proportion to obtain the mixture;
将混料装入到第一石墨舟内； Loading the mixture into the first graphite boat;
将装有混料的第一石墨舟放置到第一石英管内； Placing a first graphite boat containing the mixture into the first quartz tube;
将放置有第一石墨舟的第一石英管放置到第一合成炉内； Place the first quartz tube on which the first graphite boat is placed into the first synthesis furnace;
通入第一惰性气体排空第一石英管内的空气； Passing the first inert gas to evacuate the air in the first quartz tube;
在第一石英管内的空气被第一惰性气体排空之后， 第一合成炉采用 第一多段升温保温方式使得第一石墨舟内的混料进行合成反应在第一多 段升温保温中， 前段通入第一惰性气体， 而后段通入第一还原气体； 合成反应之后， 第一合成炉停止加热并分段降温至室温： 在分段降 温至室温中， 前段通入第一还原气体， 后段通入第一惰性气体； 以及 从第一石英管中取出第一石墨舟， 再从第一石墨舟内取出一次合成 物； 以及 After the air in the first quartz tube is emptied by the first inert gas, the first synthesis furnace adopts the first multi-stage heating and heat preservation method to synthesize the mixture in the first graphite boat in the first multi-stage heating and warming, the front stage The first inert gas is introduced, and the first reducing gas is introduced into the latter stage; after the synthesis reaction, the first synthesis furnace stops heating and is cooled down to room temperature in stages: in the stepwise cooling to room temperature, the first stage is introduced into the first reducing gas, and then a first inert gas is introduced into the segment; and the first graphite boat is taken out from the first quartz tube, and the composition is taken out from the first graphite boat;
二次合成步骤， 包括： The second synthesis step includes:
将一次合成物破碎至规定尺寸的一次合成物颗粒； Breaking the primary composition into primary synthetic particles of a specified size;
将一次合成物颗粒装入到第二石墨舟内； Loading the primary composite particles into the second graphite boat;
将装有一次合成物颗粒的第二石墨舟放置到第二石英管内； 将放置有第二石墨舟的第二石英管放置到第二合成炉内； Place a second graphite boat containing the primary composite particles into the second quartz tube; place the second quartz tube on which the second graphite boat is placed into the second synthesis furnace;
通入第二惰性气体排空第二石英管内的空气； Passing a second inert gas to evacuate air in the second quartz tube;
在第二石英管内的空气被第二惰性气体排空之后， 第二合成炉采用 第二多段升温保温方式使得第二石墨舟内的一次合成物颗粒合成反应， 且在第二多段升温保温中， 前段通入第二惰性气体， 后段通入第二还原 性气体； After the air in the second quartz tube is emptied by the second inert gas, the second synthesis furnace adopts a second multi-stage heating and heating method to synthesize the primary composite particles in the second graphite boat, and in the second multi-stage heating and heat preservation The second inert gas is introduced into the front section, and the second reducing gas is introduced into the rear section;
合成反应之后， 第二合成炉停止加热并分段降温至室温， 在分段降
温至室温中， 前段通入第二还原性气体， 后段通入第二惰性气体； 以及 After the synthesis reaction, the second synthesis furnace stops heating and is cooled down to room temperature in stages, in stages. Warming to room temperature, a second reducing gas is introduced into the front section, and a second inert gas is introduced in the latter stage;
从第二石英管中取出第二石墨舟， 再从第二石墨舟内取出二次合成 The second graphite boat is taken out from the second quartz tube, and the second graphite is taken out from the second graphite boat.
2. 根据权利要求 1所述的碲化镉的制备方法， 其特征在于， 在一次 合成步骤中， 5N 碲粉和 5N 镉粉的混合比例为摩尔比 1 : 1。 The method for producing cadmium telluride according to claim 1, wherein in a single synthesis step, the mixing ratio of the 5N tantalum powder and the 5N cadmium powder is a molar ratio of 1:1.
3. 根据权利要求 1所述的碲化镉的制备方法， 其特征在于， 在所述 一次合成步骤中， 所述第一多段升温保温为三段升温保温： The method for preparing cadmium telluride according to claim 1, wherein in the one step of synthesizing, the first multi-stage heating and holding is a three-stage heating and holding:
第一段， 以 2〜10 °C /min 的升温速率， 从室温升温至 150〜300 °C， 保温 2〜6h， 在第一段中通入第一惰性气体； The first section, at a temperature rising rate of 2 to 10 ° C / min, is raised from room temperature to 150 to 300 ° C, kept for 2 to 6 hours, and the first inert gas is introduced into the first stage;
第二段， 以 2〜10 °C /min的升温速率， 继续升温至 380〜450 °C， 保 温 10〜60min， 在第二段中通入第一惰性气体； 以及 In the second stage, at a heating rate of 2 to 10 ° C /min, the temperature is further increased to 380 to 450 ° C, and the temperature is maintained for 10 to 60 minutes, and the first inert gas is introduced into the second stage;
第三段， 以 2〜10 °C /min的升温速率， 继续升温至 850〜950 °C， 保 温 0. 5〜2h， 在第三段中通入第一还原气体； In the third stage, at a heating rate of 2 to 10 ° C /min, the temperature is further increased to 850 to 950 ° C, and the temperature is maintained at 0.5 to 2 hours, and the first reducing gas is introduced into the third stage;
其中， 第一段和第二段为所述第一多段升温保温的前段， 而第三段 为所述第一多段升温保温的后段。 Wherein, the first segment and the second segment are the first segment of the first multi-stage heating and warming, and the third segment is the latter segment of the first plurality of segments of the temperature-increasing insulation.
4. 根据权利要求 3所述的碲化镉的制备方法， 其特征在于， 在所述 一次合成步骤中， 所述分段降温至室温为随第一合成炉自然冷却的两段 降温至室温： The method for preparing cadmium telluride according to claim 3, wherein in the one-step synthesis step, the stepwise cooling to room temperature is to cool down to room temperature with two stages of natural cooling of the first synthesis furnace:
第一段， 从 850〜950 °C降至 200〜80 °C， 在第一段中通入第一还原 性气体； The first section, from 850 to 950 ° C to 200 to 80 ° C, the first reducing gas is introduced into the first section;
第二段， 从 200〜80 °C降至室温， 在第二段中通入第一惰性气体； 其中第一段为所述分段降温至室温的前段， 而第二段所述分段降温
二次合成步骤中， 所述将一次合成物破碎的规定尺寸为 0. In the second stage, from 200 to 80 ° C to room temperature, a first inert gas is introduced into the second stage; wherein the first stage is the front section of the section cooled to room temperature, and the second section is cooled by the section In the secondary synthesis step, the predetermined size for breaking the primary composition is 0.
5〜5mm。 5~5mm.
6. 根据权利要求 1所述的碲化镉的制备方法， 其特征在于， 在所述 二次合成步骤中， 所述第二多段升温保温为两段升温保温： The method for preparing cadmium telluride according to claim 1, wherein in the second step of synthesizing, the second multi-stage heating and holding is a two-stage heating and holding:
第一段， 以 5〜20 °C /min的升温速率， 从室温升至 380〜450 °C， 保 温 10〜60min， 在第一段中通入第二惰性气体； 以及 In the first stage, the temperature rises from 5 to 20 ° C /min, from room temperature to 380 to 450 ° C, and the temperature is maintained for 10 to 60 minutes, and a second inert gas is introduced into the first stage;
第二段， 以 2〜10 °C /min的升温速率， 继续升温至 850〜950 °C， 保 温 l〜2. 5h， 在第二段中通入第二还原性气体； The second stage, at a temperature increase rate of 2 to 10 ° C / min, continue to raise the temperature to 850~950 ° C, and maintain the temperature of l~2. 5h, the second reducing gas is introduced into the second stage;
其中， 第一段为所述两段升温保温的前段， 而第二段为所述两段升 温保温的后段。 Wherein, the first section is the front section of the two sections of the temperature rise and heat insulation, and the second section is the latter section of the two sections of the temperature rise and insulation.
7. 根据权利要求 6所述的碲化镉的制备方法， 其特征在于， 在所述 二次合成步骤中， 所述分段降温至室温为随第二合成炉自然冷却的两段 降温至室温： The method for preparing cadmium telluride according to claim 6, wherein in the secondary synthesis step, the section is cooled to room temperature to cool down to room temperature with two stages of natural cooling of the second synthesis furnace. :
第一段， 从 850〜950 °C降至 200〜80 °C， 在第一段中通入第二还原 性气体； The first section, from 850 to 950 ° C to 200 to 80 ° C, the second reducing gas is introduced into the first section;
第二段， 从 200〜80 °C降至室温， 在第二段中通入第二惰性气体； 其中， 第一段为所述两段降温至室温定义的前段， 而第二段为所述 两段降温至室温定义的后段。 In the second stage, from 200 to 80 ° C to room temperature, a second inert gas is introduced into the second stage; wherein, the first stage is the front stage defined by the two stages of cooling to room temperature, and the second stage is The two sections are cooled to the back section defined by room temperature.
8. 根据权利要求 1 所述的碲化镉的制备方法， 其特征在于， 所述一次合成步骤中的第一石墨舟为高温水淬石墨舟， 所述二次合 成步骤中的第二石墨舟为高温水淬石墨舟； The method for preparing cadmium telluride according to claim 1, wherein the first graphite boat in the primary synthesis step is a high temperature water quenched graphite boat, and the second graphite boat in the secondary synthesis step Water quenching graphite boat for high temperature;
所述一次合成步骤中的第一惰性气体为氮气， 所述二次合成步骤中 的第二惰性气体为氮气； The first inert gas in the first synthesis step is nitrogen, and the second inert gas in the second synthesis step is nitrogen;
所述一次合成步骤中的第一还原性气体为氢气， 所述二次合成步骤 中的第二还原性气体为氢气。 The first reducing gas in the primary synthesis step is hydrogen, and the second reducing gas in the secondary synthesis step is hydrogen.
9. 根据权利要求 1所述的碲化镉的制备方法， 其特征在于， 所述一
次合成步骤中的第一合成炉和所述二次合成步骤中的第二合成炉为同一 或不同的合成炉； 9. The method for preparing cadmium telluride according to claim 1, wherein the one The first synthesis furnace in the subsynthesis step and the second synthesis furnace in the secondary synthesis step are the same or different synthesis furnaces;
所述一次合成步骤中的第一石墨舟和所述二次合成步骤中的第二石 墨舟为同一或不同的石墨舟， 且当所述一次合成步骤中的第一石墨舟和 所述二次合成步骤中的第二石墨舟为同一石墨舟时在所述二次合成步骤 中在第二石墨舟使用前对第二石墨舟进行清洁处理； The first graphite boat in the one-step synthesis step and the second graphite boat in the secondary synthesis step are the same or different graphite boats, and the first graphite boat and the second in the one-time synthesis step When the second graphite boat in the synthesizing step is the same graphite boat, the second graphite boat is cleaned before the second graphite boat is used in the second synthesizing step;
所述一次合成步骤中的第二石英管和在所述二次合成步骤中的第二 石英管为同一或不同的石英管， 且当所述一次合成步骤中的第二石英管 和在所述二次合成步骤中的第二石英管为同一石英管时在所述二次合成 步骤中在第二石英管使用前进行清洁处理。 The second quartz tube in the one-step synthesis step and the second quartz tube in the secondary synthesis step are the same or different quartz tubes, and when the second quartz tube in the one-time synthesis step is When the second quartz tube in the secondary synthesis step is the same quartz tube, the cleaning treatment is performed before the second quartz tube is used in the secondary synthesis step.
10. 根据权利要求 1 所述的碲化镉的制备方法， 其特征在于， 还包 括步骤： 在获得二次合成物之后， 进行精细破碎及筛分， 以获得不同粒 度的二次合成物。
10. The method of producing cadmium telluride according to claim 1, further comprising the step of: after obtaining the secondary composition, performing fine crushing and sieving to obtain secondary compositions of different particle sizes.
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| CN103754838B (en) * | 2014-02-08 | 2015-10-28 | 张家港绿能新材料科技有限公司 | A kind of method and apparatus preparing cadmium antimonide powder fast |
| CN103818886B (en) * | 2014-03-06 | 2015-11-18 | 张家港绿能新材料科技有限公司 | A kind of preparation method of cadmium telluride |
| CN106495108B (en) * | 2016-11-08 | 2018-07-06 | 广东先导稀材股份有限公司 | The preparation method of cadmium telluride |
| CN108017042B (en) * | 2017-12-25 | 2020-04-24 | 清远先导材料有限公司 | Preparation method of high-purity cadmium selenide |
| 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 |
| CN114524417B (en) * | 2022-03-07 | 2023-07-28 | 先导薄膜材料（广东）有限公司 | Preparation method of high-yield lead telluride |
| CN116022743A (en) * | 2022-12-12 | 2023-04-28 | 先导薄膜材料（广东）有限公司 | Antimony ditelluride and preparation method thereof |
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| CN1380246A (en) * | 2002-05-15 | 2002-11-20 | 西安交通大学 | Preparation method of cadmium antimonide powder |
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| CN1380246A (en) * | 2002-05-15 | 2002-11-20 | 西安交通大学 | Preparation method of cadmium antimonide powder |
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