CN106241752B - A kind of preparation method of cuprous telluride - Google Patents
A kind of preparation method of cuprous telluride Download PDFInfo
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- CN106241752B CN106241752B CN201610838896.XA CN201610838896A CN106241752B CN 106241752 B CN106241752 B CN 106241752B CN 201610838896 A CN201610838896 A CN 201610838896A CN 106241752 B CN106241752 B CN 106241752B
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- MZEWONGNQNXVKA-UHFFFAOYSA-N [Cu].[Cu].[Te] Chemical compound [Cu].[Cu].[Te] MZEWONGNQNXVKA-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 57
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 27
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052802 copper Inorganic materials 0.000 claims abstract description 24
- 239000010949 copper Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000010453 quartz Substances 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- VMQMZMRVKUZKQL-UHFFFAOYSA-N Cu+ Chemical compound [Cu+] VMQMZMRVKUZKQL-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- JGJLWPGRMCADHB-UHFFFAOYSA-N hypobromite Inorganic materials Br[O-] JGJLWPGRMCADHB-UHFFFAOYSA-N 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005616 pyroelectricity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
本发明提供了一种碲化亚铜的制备方法，包括以下步骤：将单质铜和单质碲混合，在真空的条件下加热反应，得到碲化亚铜。本发明公开的制备方法用到的原料组分较少，在添加了单质铜和单质碲后，无需再额外添加其他原料，无需高压，就可以制得碲化亚铜，且制得的碲化亚铜质量较优，纯度较高。同时，制备方法简单易行，无需采用复杂且昂贵的设备，制备成本较低。The invention provides a preparation method of cuprous telluride, comprising the following steps: mixing elemental copper and elemental tellurium, heating and reacting under vacuum conditions to obtain cuprous telluride. The preparation method disclosed in the present invention uses less raw material components. After adding elemental copper and elemental tellurium, cuprous telluride can be produced without adding other raw materials and without high pressure, and the prepared tellurium Cuprous copper has better quality and higher purity. At the same time, the preparation method is simple and easy, without the need to use complex and expensive equipment, and the preparation cost is low.
Description
技术领域technical field
本发明涉及材料合成领域，尤其涉及一种碲化亚铜的制备方法。The invention relates to the field of material synthesis, in particular to a method for preparing cuprous telluride.
背景技术Background technique
碲化亚铜(Cu2Te)是一种蓝黑色八面体晶体，相对密度为7.27，熔点约900℃。其溶于溴水，但不溶于水、盐酸和硫酸。这种半导体材料因具有独特的离子导电性和热电性，从而广泛应用于太阳能电池领域。因此，开发碲化亚铜的制备工艺对于碲化亚铜在未来的发展有着很重要的作用。Cuprous telluride (Cu 2 Te) is a blue-black octahedral crystal with a relative density of 7.27 and a melting point of about 900°C. It is soluble in bromine water, but insoluble in water, hydrochloric acid and sulfuric acid. This semiconductor material is widely used in the field of solar cells due to its unique ionic conductivity and pyroelectricity. Therefore, the development of the preparation process of cuprous telluride plays a very important role in the future development of cuprous telluride.
现有技术中公开的碲化亚铜是由电解铜和纯碲在坩埚内覆以氯化钠和氯化钾保护层熔化制得。由于制备方法中需要用到氯化钠和氯化钾作为保护层，因而，最终制得的碲化亚铜中不可避免地混有含量较多的钠和钾，进而影响碲化亚铜产品的纯度，使得碲化亚铜的质量较差。同时，这种方法需要在高温高压下才能完成，需要使用复杂且昂贵的设备，对设备的要求较高，操作复杂，成本高昂。The cuprous telluride disclosed in the prior art is produced by melting electrolytic copper and pure tellurium in a crucible covered with a protective layer of sodium chloride and potassium chloride. Because sodium chloride and potassium chloride need to be used as protective layer in the preparation method, therefore, in the cuprous telluride that finally makes, inevitably be mixed with more sodium and potassium of content, and then influence the quality of cuprous telluride product Purity, making cuprous telluride of poor quality. At the same time, this method needs to be completed under high temperature and high pressure, requires complex and expensive equipment, has high requirements for equipment, complicated operation, and high cost.
发明内容Contents of the invention
有鉴于此，本发明要解决的技术问题在于提供一种碲化亚铜的制备方法，由这种方法制备的碲化亚铜质量较优，纯度较高。In view of this, the technical problem to be solved by the present invention is to provide a method for preparing cuprous telluride. The cuprous telluride prepared by this method has better quality and higher purity.
本发明提供了一种碲化亚铜的制备方法，包括以下步骤：The invention provides a method for preparing cuprous telluride, comprising the following steps:
将单质铜和单质碲混合，在真空的条件下加热反应，得到碲化亚铜。Mix elemental copper and elemental tellurium, heat and react under vacuum conditions to obtain cuprous telluride.
优选的，所述单质铜和所述单质碲的摩尔比为2：1。Preferably, the molar ratio of the elemental copper to the elemental tellurium is 2:1.
优选的，所述真空的真空度为1×10-3Pa～1×10-2Pa。Preferably, the vacuum degree of the vacuum is 1×10 -3 Pa to 1×10 -2 Pa.
优选的，所述加热反应在镀有碳膜的石英管中进行。Preferably, the heating reaction is carried out in a quartz tube coated with carbon film.
优选的，所述加热反应的加热方式为三段式梯度加热。Preferably, the heating method of the heating reaction is a three-stage gradient heating.
优选的，所述三段式梯度加热为：Preferably, the three-stage gradient heating is:
A)加热至400℃～550℃，保温1h～2h；A) Heating to 400°C-550°C, keeping it warm for 1h-2h;
B)加热至850℃～950℃，保温1h～3h；B) Heating to 850°C-950°C, keeping it warm for 1h-3h;
C)加热至1100℃～1180℃，保温2h～4h。C) Heating to 1100°C-1180°C and keeping it warm for 2h-4h.
优选的，preferred,
步骤A)中，所述加热的升温速率为5℃/min～10℃/min；In step A), the heating rate is 5°C/min to 10°C/min;
步骤B)中，所述加热的升温速率为3℃/min～6℃/min；In step B), the heating rate is 3°C/min to 6°C/min;
步骤C)中，所述加热的升温速率为3℃/min～6℃/min。In step C), the heating rate is 3°C/min˜6°C/min.
优选的，将所述加热至1100℃～1180℃得到的物料混匀，所述混匀的时间为2h～4h。Preferably, the material obtained by heating to 1100° C. to 1180° C. is mixed evenly, and the mixing time is 2h to 4h.
优选的，所述混匀的方式为竖直60度左右摇摆。Preferably, the way of mixing is to shake vertically at about 60 degrees.
优选的，所述加热反应后，还包括冷却。Preferably, after the heating reaction, cooling is also included.
本发明提供了一种碲化亚铜的制备方法，包括以下步骤：将单质铜和单质碲混合，在真空的条件下加热反应，得到碲化亚铜。本发明公开的制备方法用到的原料组分较少，在添加了单质铜和单质碲后，无需再额外添加其他原料，无需高压，就可以制得碲化亚铜，且制得的碲化亚铜质量较优，纯度较高。同时，制备方法简单易行，无需采用复杂且昂贵的设备，制备成本较低。The invention provides a preparation method of cuprous telluride, comprising the following steps: mixing elemental copper and elemental tellurium, heating and reacting under vacuum conditions to obtain cuprous telluride. The preparation method disclosed in the present invention uses less raw material components. After adding elemental copper and elemental tellurium, cuprous telluride can be produced without adding other raw materials and without high pressure, and the prepared tellurium Cuprous copper has better quality and higher purity. At the same time, the preparation method is simple and easy, without the need to use complex and expensive equipment, and the preparation cost is low.
具体实施方式Detailed ways
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
本发明提供了一种碲化亚铜的制备方法，包括以下步骤：The invention provides a method for preparing cuprous telluride, comprising the following steps:
将单质铜和单质碲混合，在真空的条件下加热反应，得到碲化亚铜。Mix elemental copper and elemental tellurium, heat and react under vacuum conditions to obtain cuprous telluride.
本发明对所述单质铜和单质碲的来源并无特殊的限制，可以为一般市售。本发明对所述单质铜和单质碲的纯度并无特殊的限制，为本领域技术人员熟知的纯度即可。本发明优选为纯度为5N的单质铜和纯度为5N的单质碲。所述单质铜可以为块状或粒状，所述单质碲可以为块状、粒状或粉状。所述单质铜和所述单质碲的摩尔比优选为2：1。In the present invention, there is no special limitation on the source of the elemental copper and elemental tellurium, which can be generally commercially available. In the present invention, there is no special limitation on the purity of the elemental copper and elemental tellurium, and the purity well known to those skilled in the art will suffice. The present invention is preferably elemental copper with a purity of 5N and elemental tellurium with a purity of 5N. The elemental copper may be in block or granular form, and the elemental tellurium may be in block, granular or powder form. The molar ratio of the elemental copper to the elemental tellurium is preferably 2:1.
将单质铜和单质碲混合后，在真空的条件下加热反应。本发明优选将单质铜和单质碲混合后，在真空的条件下，在密闭环境中加热反应。After mixing elemental copper and elemental tellurium, the reaction is heated under vacuum conditions. In the present invention, it is preferred to mix the elemental copper and elemental tellurium, and then heat and react in a closed environment under vacuum conditions.
本发明公开的加热反应无需在高压进行，因而，无需采用复杂且昂贵的设备，制备成本较低，同时，方法简单易行。所述真空的真空度优选为1×10-3Pa～1×10-2Pa；在本发明的某些实施例中，所述真空的真空度为1×10-3Pa、2×10-3Pa、5×10-3Pa或1×10-2Pa。The heating reaction disclosed by the invention does not need to be carried out under high pressure, therefore, no complicated and expensive equipment is needed, the preparation cost is low, and the method is simple and easy. The vacuum degree of the vacuum is preferably 1×10 -3 Pa to 1×10 -2 Pa; in some embodiments of the present invention, the vacuum degree of the vacuum is 1×10 -3 Pa, 2×10 - 3 Pa, 5×10 -3 Pa or 1×10 -2 Pa.
所述加热反应优选在镀有膜的石英管中进行。本发明对所述膜并无特殊的限制，只要在所述加热反应中不参与反应即可，本发明优选为碳膜、氮化硼膜或铂膜中的一种，考虑到经济实惠，更优选为碳膜。本发明对所述加热反应的加热设备并无特殊的限制，采用本领域技术人员熟知的加热设备即可，本发明优选为加热炉。The heating reaction is preferably carried out in a membrane-coated quartz tube. The present invention has no special restrictions on the film, as long as it does not participate in the reaction in the heating reaction, the present invention is preferably a carbon film, a boron nitride film or a platinum film, and in consideration of economic benefits, more Carbon films are preferred. The present invention has no special limitation on the heating equipment for the heating reaction, and the heating equipment well-known to those skilled in the art can be used, and the present invention is preferably a heating furnace.
所述加热反应的加热方式优选为三段式梯度加热。优选的，所述三段式梯度加热具体为：The heating method of the heating reaction is preferably three-stage gradient heating. Preferably, the three-stage gradient heating is specifically:
A)加热至第一温度，保温1h～2h；A) heating to the first temperature and keeping it warm for 1h to 2h;
B)加热至第二温度，保温1h～3h；B) heating to the second temperature and keeping it warm for 1h to 3h;
C)加热至第三温度，保温2h～4h。C) Heating to the third temperature and keeping it warm for 2h-4h.
在步骤A)中，所述第一温度为400℃～550℃；在本发明的某些实施例中，所述第一温度为400℃、500℃或550℃。所述第一温度下的保温时间为1h～2h；在本发明的某些实施例中，所述保温时间为1h、1.5h或2h。所述加热的升温速率优选为5℃/min～10℃/min；在本发明的某些实施例中，所述加热的升温速率为5℃/min、8℃/min、9℃/min或10℃/min。In step A), the first temperature is 400°C-550°C; in some embodiments of the present invention, the first temperature is 400°C, 500°C or 550°C. The holding time at the first temperature is 1h-2h; in some embodiments of the present invention, the holding time is 1h, 1.5h or 2h. The temperature rise rate of the heating is preferably 5°C/min～10°C/min; in some embodiments of the present invention, the temperature rise rate of the heating is 5°C/min, 8°C/min, 9°C/min or 10°C/min.
在步骤B)中，所述第二温度为850℃～950℃；在本发明的某些实施例中，所述第二温度为850℃、900℃、920℃或950℃。所述第二温度下的保温时间为1h～3h；在本发明的某些实施例中，所述保温时间为1h或2h。所述加热的升温速率优选为3℃/min～6℃/min；在本发明的某些实施例中，所述加热的升温速率为3℃/min、4℃/min或5℃/min。In step B), the second temperature is 850°C-950°C; in some embodiments of the present invention, the second temperature is 850°C, 900°C, 920°C or 950°C. The holding time at the second temperature is 1h-3h; in some embodiments of the present invention, the holding time is 1h or 2h. The heating rate is preferably 3°C/min˜6°C/min; in some embodiments of the present invention, the heating rate is 3°C/min, 4°C/min or 5°C/min.
在步骤C)中，所述第三温度为1100℃～1180℃；在本发明的某些实施例中，所述第三温度为1120℃、1130℃、1150℃或1180℃。所述第三温度下的保温时间为2h～4h；在本发明的某些实施例中，所述保温时间为2.5h或3h。所述加热的升温速率优选为3℃/min～6℃/min；在本发明的某些实施例中，所述加热的升温速率为3℃/min、4℃/min或5℃/min。In step C), the third temperature is 1100°C-1180°C; in some embodiments of the present invention, the third temperature is 1120°C, 1130°C, 1150°C or 1180°C. The holding time at the third temperature is 2h-4h; in some embodiments of the present invention, the holding time is 2.5h or 3h. The heating rate is preferably 3°C/min˜6°C/min; in some embodiments of the present invention, the heating rate is 3°C/min, 4°C/min or 5°C/min.
所述加热至第三温度时，将得到的物料混匀，所述混匀的时间与所述第三温度下的保温时间相同，本发明优选为2h～4h，更优选为2.5h～3h。所述混匀的方式优选为竖直60度左右摇摆。When heating to the third temperature, the obtained materials are mixed evenly, and the mixing time is the same as the holding time at the third temperature, preferably 2h-4h in the present invention, more preferably 2.5h-3h. The way of mixing is preferably to shake vertically at about 60 degrees.
上述加热反应完成后，优选还包括冷却，得到碲化亚铜。优选的，所述冷却具体为：加热反应得到的产物随加热反应的设备一起冷却。本发明对所述冷却的方式并无特殊的限制，采用本领域技术人员熟知的冷却方式即可，本发明优选为自然冷却。所述冷却的温度优选为35℃以下，更优选为25～35℃。After the above heating reaction is completed, preferably cooling is also included to obtain cuprous telluride. Preferably, the cooling specifically includes: the product obtained from the heating reaction is cooled together with the equipment for the heating reaction. The present invention has no special limitation on the cooling method, and any cooling method known to those skilled in the art can be used. Natural cooling is preferred in the present invention. The cooling temperature is preferably below 35°C, more preferably 25-35°C.
所述冷却后，优选还包括出料，从而得到碲化亚铜。After the cooling, it is preferred to also include discharging, so as to obtain cuprous telluride.
本发明提供了一种碲化亚铜的制备方法，包括以下步骤：将单质铜和单质碲混合，在真空的条件下加热反应，得到碲化亚铜。本发明公开的制备方法用到的原料组分较少，在添加了单质铜和单质碲后，无需再额外添加其他原料，无需高压，就可以制得碲化亚铜，且制得的碲化亚铜质量较优，纯度较高。同时，制备方法简单易行，无需采用复杂且昂贵的设备，制备成本较低。The invention provides a preparation method of cuprous telluride, comprising the following steps: mixing elemental copper and elemental tellurium, heating and reacting under vacuum conditions to obtain cuprous telluride. The preparation method disclosed in the present invention uses less raw material components. After adding elemental copper and elemental tellurium, cuprous telluride can be produced without adding other raw materials and without high pressure, and the prepared tellurium Cuprous copper has better quality and higher purity. At the same time, the preparation method is simple and easy, without the need to use complex and expensive equipment, and the preparation cost is low.
为了进一步说明本发明，以下结合实施例对本发明提供的一种碲化亚铜的制备方法进行详细描述，但不能将其理解为对本发明保护范围的限定。In order to further illustrate the present invention, a method for preparing cuprous telluride provided by the present invention will be described in detail below in conjunction with examples, but it should not be construed as limiting the protection scope of the present invention.
实施例1Example 1
将5N的铜粒和5N的碲块按摩尔比2：1配料1kg，装入镀有碳膜的石英管中，将石英管抽真空，直至真空度为1×10-3Pa后，封管。将封口后的石英管置于加热炉内，以5℃/min的速率升温至500℃，保温1h；再以3℃/min的速率升温至920℃，保温2h；然后以3℃/min的速率升温至1120℃，保温3h。当温度升至1120℃时，采用竖直60度左右摇摆的方式将石英管中的物料混匀，所述混匀的时间为3h。之后，将炉腔的温度自然冷却至25～35℃后，出料，得到碲化亚铜。Mix 1kg of 5N copper particles and 5N tellurium blocks at a molar ratio of 2:1, put them into a quartz tube coated with carbon film, vacuumize the quartz tube until the vacuum degree is 1×10 -3 Pa, and then seal the tube . Place the sealed quartz tube in a heating furnace, raise the temperature to 500°C at a rate of 5°C/min, and keep it for 1 hour; then raise the temperature to 920°C at a rate of 3°C/min, and hold it for 2 hours; Raise the temperature to 1120°C and keep it warm for 3h. When the temperature rises to 1120° C., the materials in the quartz tube are mixed evenly by swinging about 60 degrees vertically, and the mixing time is 3 hours. Afterwards, after the temperature of the furnace cavity is naturally cooled to 25-35° C., the material is discharged to obtain cuprous telluride.
实施例2Example 2
将5N的铜粒和5N的碲块按摩尔比2：1配料1.5kg，装入镀有碳膜的石英管中，将石英管抽真空，直至真空度为5×10-3Pa后，封管。将封口后的石英管置于加热炉内，以8℃/min的速率升温至500℃，保温1h；再以4℃/min的速率升温至900℃，保温1h；然后以3℃/min的速率升温至1150℃，保温3h。当温度升至1150℃时，采用竖直60度左右摇摆的方式将石英管中的物料混匀，所述混匀的时间为3h。之后，将炉腔的温度自然冷却至25～35℃后，出料，得到碲化亚铜。Mix 1.5kg of 5N copper grains and 5N tellurium blocks at a molar ratio of 2:1, put them into a quartz tube coated with carbon film, vacuumize the quartz tube until the vacuum degree is 5×10 -3 Pa, and then seal it. Tube. Place the sealed quartz tube in a heating furnace, raise the temperature to 500°C at a rate of 8°C/min, and keep it for 1h; then raise the temperature to 900°C at a rate of 4°C/min, and keep it for 1h; Raise the temperature to 1150°C and keep it warm for 3h. When the temperature rises to 1150° C., the materials in the quartz tube are mixed evenly by swinging about 60 degrees vertically, and the mixing time is 3 hours. Afterwards, after the temperature of the furnace cavity is naturally cooled to 25-35° C., the material is discharged to obtain cuprous telluride.
实施例3Example 3
将5N的铜粒和5N的碲块按摩尔比2：1配料2kg，装入镀有碳膜的石英管中，将石英管抽真空，直至真空度为2×10-3Pa后，封管。将封口后的石英管置于加热炉内，以10℃/min的速率升温至500℃，保温1h；再以3℃/min的速率升温至920℃，保温1h；然后以4℃/min的速率升温至1130℃，保温3h。当温度升至1130℃时，采用竖直60度左右摇摆的方式将石英管中的物料混匀，所述混匀的时间为3h。之后，将炉腔的温度自然冷却至25～35℃后，出料，得到碲化亚铜。Mix 2kg of 5N copper particles and 5N tellurium blocks at a molar ratio of 2:1, put them into a quartz tube coated with carbon film, vacuumize the quartz tube until the vacuum degree is 2×10 -3 Pa, and then seal the tube . Place the sealed quartz tube in a heating furnace, raise the temperature to 500°C at a rate of 10°C/min, and keep it for 1 hour; then raise the temperature to 920°C at a rate of 3°C/min, and hold it for 1 hour; The temperature was raised to 1130° C. and kept for 3 hours. When the temperature rose to 1130° C., the materials in the quartz tube were mixed evenly by swinging about 60 degrees vertically, and the mixing time was 3 hours. Afterwards, after the temperature of the furnace cavity is naturally cooled to 25-35° C., the material is discharged to obtain cuprous telluride.
实施例4Example 4
将5N的铜粒和5N的碲块按摩尔比2：1配料2kg，装入镀有氮化硼膜的石英管中，将石英管抽真空，直至真空度为1×10-3Pa后，封管。将封口后的石英管置于加热炉内，以5℃/min的速率升温至550℃，保温1.5h；再以3℃/min的速率升温至850℃，保温2h；然后以5℃/min的速率升温至1180℃，保温3h。当温度升至1180℃时，采用竖直60度左右摇摆的方式将石英管中的物料混匀，所述混匀的时间为3h。之后，将炉腔的温度自然冷却至25～35℃后，出料，得到碲化亚铜。Mix 2kg of 5N copper particles and 5N tellurium blocks at a molar ratio of 2:1, put them into a quartz tube coated with a boron nitride film, and evacuate the quartz tube until the vacuum degree is 1×10 -3 Pa. Seal tube. Place the sealed quartz tube in a heating furnace, raise the temperature to 550°C at a rate of 5°C/min, and keep it for 1.5h; then raise the temperature to 850°C at a rate of 3°C/min, and keep it for 2h; The temperature was raised to 1180°C at a certain rate, and the temperature was kept for 3 hours. When the temperature rises to 1180° C., the materials in the quartz tube are mixed evenly by swinging about 60 degrees vertically, and the mixing time is 3 hours. Afterwards, after the temperature of the furnace cavity is naturally cooled to 25-35° C., the material is discharged to obtain cuprous telluride.
实施例5Example 5
将5N的铜粒和5N的碲块按摩尔比2：1配料1.5kg，装入镀有铂膜的石英管中，将石英管抽真空，直至真空度为1×10-2Pa后，封管。将封口后的石英管置于加热炉内，以9℃/min的速率升温至400℃，保温2h；再以5℃/min的速率升温至950℃，保温1h；然后以5℃/min的速率升温至1180℃，保温2.5h。当温度升至1180℃时，采用竖直60度左右摇摆的方式将石英管中的物料混匀，所述混匀的时间为2.5h。之后，将炉腔的温度自然冷却至25～35℃后，出料，得到碲化亚铜。Mix 1.5kg of 5N copper grains and 5N tellurium blocks at a molar ratio of 2:1, put them into a platinum-coated quartz tube, vacuumize the quartz tube until the vacuum degree reaches 1×10 -2 Pa, and then seal it. Tube. Place the sealed quartz tube in a heating furnace, raise the temperature to 400°C at a rate of 9°C/min, and keep it for 2 hours; then raise the temperature to 950°C at a rate of 5°C/min, and keep it for 1 hour; Raise the temperature to 1180°C and keep it warm for 2.5h. When the temperature rises to 1180° C., the materials in the quartz tube are mixed evenly by swinging about 60 degrees vertically, and the mixing time is 2.5 hours. Afterwards, after the temperature of the furnace cavity is naturally cooled to 25-35° C., the material is discharged to obtain cuprous telluride.
实施例6Example 6
对实施例1～5得到的碲化亚铜的纯度进行检测：Detect the purity of the cuprous telluride that embodiment 1～5 obtains:
采用电感耦合等离子体质谱仪(ICP-MS，生产厂家为PE公司，型号为DRC-II)进行检测，该设备的检测的条件为：温度为18℃～28℃，相对湿度为30％～70％，洁净度为1000级。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。检测结果见表1所示。Adopt inductively coupled plasma mass spectrometer (ICP-MS, manufacturer is PE company, model is DRC-II) to detect, the detection condition of this equipment is: temperature is 18 ℃～28 ℃, relative humidity is 30%～70 %, the cleanliness is class 1000. Detection method of inductively coupled plasma mass spectrometer: After the element to be measured is ionized by high-temperature plasma, it enters the mass analyzer in the form of positive charge, and is received by the detector according to the difference in mass/charge ratio to generate a signal. The ratio of the signal generated by the analyte to the signal of the element in the standard substance gives the content of the analyte. The test results are shown in Table 1.
表1实施例1～5得到的碲化亚铜含有的杂质及其含量(单位：ppm)Table 1 The impurities contained in the cuprous telluride obtained in Examples 1-5 and their contents (unit: ppm)
从表1可以看出，实施例1～5制备的碲化亚铜中所含有的杂质种类及含量较少，纯度较高，均在5N以上。It can be seen from Table 1 that the types and contents of impurities contained in the cuprous telluride prepared in Examples 1-5 are relatively small, and the purity is relatively high, all of which are above 5N.
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。The descriptions of the above embodiments are only used to help understand the method and core idea of the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention will not be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
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