CN213231532U - Two-dimensional material purification device - Google Patents

Two-dimensional material purification device Download PDF

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CN213231532U
CN213231532U CN202021812486.6U CN202021812486U CN213231532U CN 213231532 U CN213231532 U CN 213231532U CN 202021812486 U CN202021812486 U CN 202021812486U CN 213231532 U CN213231532 U CN 213231532U
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tube
furnace
dimensional material
filter
heating
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喻学锋
喻彬璐
王佳宏
游志恒
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Hubei Mophos Technology Co ltd
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Shenzhen Zhongke Mophos Technology Co ltd
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Abstract

The utility model discloses a two-dimensional material purification device, the device include gas holder, heating furnace, boiler tube, flange, heating band, intermediate layer beaker, filter vacuum tube, vacuum pump. The device sequentially connects and assembles the gas storage tank, the heating furnace, the interlayer beaker, the filtering vacuum tube and the vacuum pump through the gas pipe. The utility model discloses can effectively purify the impurity of introducing in the two-dimensional material preparation process to acquire high-purity two-dimensional material.

Description

Two-dimensional material purification device
Technical Field
The utility model belongs to new material purification field especially relates to a two-dimensional material purification device.
Background
Since the appearance of graphene in a laboratory in 2004, various novel two-dimensional materials have been developed, the scientific research and the industrial field have been continuously and deeply researching two-dimensional materials, and the two-dimensional materials are full of huge imagination space for the future application of the two-dimensional materials, and the two-dimensional materials such as a black phosphorus simple substance, a molybdenum disulfide transition metal chalcogenide compound and the like are well known. Two-dimensional materials have potential to be widely applied in the field of advanced electronic devices because they exhibit excellent properties in the fields of light, heat, electricity, magnetism, and the like. The existing mature method for synthesizing the two-dimensional material comprises a solvothermal method, a chemical vapor transport method (CVT method) and a chemical vapor deposition method (CVD), wherein the solvothermal method inevitably needs various organic solvents, the chemical vapor transport method (CVT method) needs various halides as transport agents, and the chemical vapor deposition method (CVD) needs introduction of various volatile raw material sources, which are inevitably adsorbed or mixed in the two-dimensional material to influence the purity of the two-dimensional material, so that the performance of the two-dimensional material is influenced, and the development of the two-dimensional material is limited.
Disclosure of Invention
Introduce impurity to two-dimensional material in the field and lead to impure in the preparation process, the utility model aims at providing a two-dimensional material purification device, through continuous suction force quickly separating gaseous state impurity that provides, while rapid heating, keep an inert atmosphere and various impurity of effectual absorption, can realize that two-dimensional material purification process is harmless and the purification is high-efficient to material itself, can guarantee the harmless bad border of purification environment to operating personnel simultaneously, in addition, the component that this set of device involved can effectively enlarge, the operation is simple, low cost, be favorable to handling the purification of ton level above two-dimensional material, also have important promotion meaning to the large batch industrial production high quality two-dimensional material.
In order to achieve the above object, the utility model adopts the following technical scheme: a two-dimensional material purification device, characterized by: comprises a gas storage tank, a heating furnace, a furnace tube, an interlayer beaker, a filtering vacuum tube and a vacuum pump; the gas storage tank, the heating furnace, the furnace tube, the interlayer beaker, the filtering vacuum tube and the vacuum pump are sequentially connected and assembled through the gas tube.
Specifically, a first flange and a second flange are installed at two ends of the furnace tube, an air inlet communicated with the furnace tube is formed in the first flange, an air outlet communicated with the furnace tube is formed in the second flange, the air inlet is connected with an air storage tank through an air pipe, and the air outlet is connected with the interlayer beaker through the air pipe.
Specifically, the filtering vacuum tube comprises a first filtering vacuum tube and a second filtering vacuum tube, the first filtering vacuum tube and the second filtering vacuum tube are connected with each other in a sealing mode through a hoop and a rubber ring, and the two vacuum tubes are connected with the air tube through the hoop, the rubber ring and a pagoda joint; and the first filtering vacuum pipe and the second filtering vacuum pipe are respectively filled with a filter I and a filter II.
Specifically, the heating belts are arranged on the parts, which are not covered by the heating furnace, of the two ends of the furnace tube, and are used for carrying out auxiliary heating on the furnace tube outside the heating furnace, wherein the temperature range is 200-300 ℃, and the furnace tube outside the furnace body is subjected to auxiliary heating, so that gaseous impurities are prevented from being condensed and accumulated on the tube wall.
Specifically, the gas in the gas storage tank is inert gas, such as nitrogen, argon, helium or neon, and provides purging and ensures that the furnace tube is in inert atmosphere.
Specifically, the heating furnace is a single-temperature-zone tube furnace or a multi-temperature-zone tube furnace; the furnace tube is made of quartz, high borosilicate, ceramic, alumina or zirconia.
Specifically, the materials of the interlayer beaker and the filter vacuum tube are stainless steel, glass or ceramic; the filter I comprises one or more of anhydrous copper sulfate, anhydrous calcium chloride, anhydrous calcium sulfate, silica gel and active alumina, and has a moisture absorption function; the filter II comprises one or a combination of more of a molecular sieve and activated carbon and has the function of adsorbing other gaseous impurities.
Specifically, the vacuum pump is a water ring vacuum pump, a reciprocating vacuum pump or a rotary vane vacuum pump, and maintains a negative pressure environment to provide pumping force.
Specifically, the air pipe is made of epoxy resin, polyvinyl chloride, polyethylene or stainless steel.
In particular, two-dimensional materials that can be used for purification include black phosphorus, transition metal chalcogenides, silicon phosphorus compounds, metal phosphides, metal nitrides, metal borides, or metal carbides.
Drawings
FIG. 1 is a schematic view of a purification apparatus in example 1;
FIG. 2 is the XRD pattern of the black phosphorus crystals before purification in example 1;
FIG. 3 is the XRD pattern of the purified black phosphorus crystals of example 1;
in the figure: 1-gas storage tank, 2-heating furnace, 3-furnace tube, 31-first flange, 32-second flange, 33-heating belt, 4-sandwich beaker, 5-filtering vacuum tube, 51-first filtering vacuum tube, 51 a-filter I, 52-second filtering vacuum tube, 52 b-filter II, 53-clamp, 6-vacuum pump and 7-gas tube.
Detailed Description
For a better understanding of the present invention, the following further illustrates the present invention with reference to specific examples and drawings, but the present invention is not limited to the following examples.
Example 1
a. Assembling the purification device: the gas storage tank 1, the heating furnace 2, the furnace tube 3, the first flange 31, the second flange 32, the heating belt 33, the interlayer beaker 4, the filtering vacuum tube 5 and the vacuum pump 6 are connected in sequence through a gas tube 7, and the inner diameter of the gas tube is
Figure BDA0002651902560000021
The material is selected from PVC. Specifically, a first flange 31 and a second flange 32 are installed at two ends of the furnace tube 3, an air inlet communicated with the furnace tube 3 is formed in the first flange 31, an air outlet communicated with the furnace tube 3 is formed in the second flange 32, the air inlet is connected with the air storage tank 1 through an air pipe 7, and the air outlet is connected with the interlayer beaker 4 through the air pipe 7.
The furnace tube 3 leaks out of the furnace body part of the heating furnace 2 and is wound by a heating belt 33, and the heating belt 33 can be directly plugged on a 220V power supply. The two filter vacuum tubes 5 are provided, namely a first filter vacuum tube 51 and a second filter vacuum tube 52, wherein anhydrous copper sulfate is selectively filled in a filter I51 a in the first filter vacuum tube 51; the filter II 52b in the second filtering vacuum tube 52 is selectively filled with molecular sieve, the two vacuum tubes are connected with each other through a clamp 53 and a rubber ring, the two vacuum tubes are connected with the air tube 7 through the clamp 53, the rubber ring and a pagoda joint, the clamp 53 can be selected as a KF25 clamp, and the schematic diagram of the device is shown in FIG. 1.
b. Preparing black phosphorus: 100g of low-purity red phosphorus, 15g of bismuth powder and 10g of iodine simple substance are placed in a place with the length of about 19cm and the inner diameter
Figure BDA0002651902560000031
The stainless steel pipe is vacuumized until the pressure in the pipe is about 1Pa, and the pipe is fastened through a hoop. The sealed stainless steel tube raw material end is arranged in a high-temperature area in a double-temperature-area furnace body, and the other end is arranged in a low-temperature area in the double-temperature-area furnace body. The high temperature section and the low temperature section are heated to target temperatures of 490 ℃ and 480 ℃ respectively in the same time, the temperature is kept for 18h, and then the temperature is reduced, and the reaction temperature rise rate and the reaction temperature reduction rate have no special influence on the yield of the black phosphorus and are not particularly described. About 95g of black phosphorus was obtained, and XRD results are shown in FIG. 2, with a significant impurity peak of bismuth iodide at the 12.86 ℃ position.
c. And (3) purifying black phosphorus: and (b) putting the black phosphorus crystal obtained in the step (b) into a furnace tube, selecting a single-temperature-zone tube furnace as a heating furnace, sequentially connecting the purification components according to the step (a), setting the temperature of the heating furnace to be 350 ℃, setting the temperature of a heating zone to be 200 ℃, selecting a water ring vacuum pump as a vacuum pump, working in the whole reaction period, simultaneously selecting nitrogen for a gas storage tank to purge, wherein the reaction time is 12h, and XRD results are shown in figure 3, only characteristic peaks of black phosphorus and all positions of miscellaneous peaks disappear, so that the high efficiency of the purification device is fully proved.
Example 2
a. The assembly of the purification device was completed as in example 1.
b. Molybdenum diphosphide (MoP)2) The preparation of (1): taking 0.96g molybdenum (Mo) powder, 0.7g red phosphorus powder, length about 10cm, inner diameter
Figure BDA0002651902560000032
The quartz tube is vacuumized until the pressure in the quartz tube is about 1Pa, the quartz tube is sealed by an oxyhydrogen machine, the sealed quartz tube is placed in a box-type furnace, the temperature is set to 700 ℃, the temperature is kept for 18h, and then the temperature is reduced, wherein the reaction temperature rise rate and the temperature reduction rate have no special influence on products.
c. Molybdenum diphosphide (MoP)2) Purification of (2): taking stepsAnd (c) putting the molybdenum phosphide obtained in the step (b) into a furnace tube, selecting a single-temperature-zone tube furnace as a heating furnace, sequentially connecting the purification components according to the step (a), setting the temperature of the heating furnace to be 500 ℃, setting the temperature of a heating belt to be 300 ℃, selecting a reciprocating vacuum pump as a vacuum pump, working in the whole reaction period, simultaneously selecting argon as a gas storage tank for purging, and successfully removing phosphorus and phosphorus oxides attached to the product for 10 hours.
Example 3
a. The assembly of the purification device was completed as in example 1.
b. Tin diselenide (SnSe)2) The preparation of (1): adding 45mL of ethylene glycol and 3mL of ethylenediamine into a beaker respectively, and then adding 3mmol of SnCl2Fully stirring and uniformly mixing the hydrate and 3mmol of sodium selenite, pouring the mixture into a polytetrafluoroethylene reaction kettle with the volume of 100ml, and reacting for 7 hours at 180 ℃ to obtain SnSe2And (3) sampling.
c. Tin diselenide (SnSe)2) Purification of (2): and (b) putting the molybdenum phosphide obtained in the step (b) into a furnace tube, selecting a single-temperature-zone tube furnace as a heating furnace, sequentially connecting the purification components according to the step (a), setting the temperature of the heating furnace to be 400 ℃, setting the temperature of a heating zone to be 260 ℃, selecting a reciprocating vacuum pump as a vacuum pump, working in the whole reaction period, simultaneously selecting argon as a gas storage tank for purging, and successfully removing the organic matters attached to the product for 12 hours.

Claims (9)

1. A two-dimensional material purification device, characterized by: comprises a gas storage tank (1), a heating furnace (2), a furnace tube (3), an interlayer beaker (4), a filtering vacuum tube (5) and a vacuum pump (6); the gas storage tank (1), the heating furnace (2), the furnace tube (3), the interlayer beaker (4), the filtering vacuum tube (5) and the vacuum pump (6) are sequentially connected and assembled through a gas tube (7); filter vacuum tube (5) and include first filter vacuum tube (51) and second filter vacuum tube (52), first filter vacuum tube (51) and second filter vacuum tube (52) pass through clamp (53) and rubber circle sealing connection, all connect through clamp (53), rubber circle and pagoda joint between two vacuum tubes and trachea (7), pack filter I (51a) and filter II (52b) in first filter vacuum tube (51) and the second filter vacuum tube (52) respectively.
2. The two-dimensional material purification apparatus of claim 1, wherein: the furnace tube (3) is characterized in that a first flange (31) and a second flange (32) are respectively installed at two ends of the furnace tube (3), an air inlet communicated with the furnace tube (3) is formed in the first flange (31), an air outlet communicated with the furnace tube (3) is formed in the second flange (32), the air inlet is connected with the air storage tank (1) through an air pipe (7), and the air outlet is connected with the interlayer beaker (4) through the air pipe (7).
3. The two-dimensional material purification apparatus of claim 1, wherein: the heating device is characterized in that heating belts (33) are arranged on the parts, which are not covered by the heating furnace (2), at the two ends of the furnace tube (3), the heating belts are used for carrying out auxiliary heating on the furnace tube (3) outside the heating furnace (2), and the temperature range is 200-300 ℃.
4. The two-dimensional material purification apparatus of claim 1, wherein: the gas in the gas storage tank (1) is inert gas, and is nitrogen, argon, helium or neon.
5. The two-dimensional material purification apparatus of claim 1, wherein: the heating furnace (2) is a single-temperature-zone tube furnace or a multi-temperature-zone tube furnace; the furnace tube (3) is made of quartz, high borosilicate, ceramic, alumina or zirconia.
6. The two-dimensional material purification apparatus of claim 1, wherein: the interlayer beaker (4) and the filter vacuum tube (5) are made of stainless steel, glass or ceramic.
7. The two-dimensional material purification apparatus of claim 1, wherein: the vacuum pump (6) is a water ring vacuum pump, a reciprocating vacuum pump or a rotary vane vacuum pump.
8. The two-dimensional material purification apparatus of claim 1, wherein: the material of the air pipe (7) is epoxy resin, polyvinyl chloride, polyethylene or stainless steel.
9. The two-dimensional material purification apparatus of claim 1, wherein: two-dimensional materials for purification include black phosphorus, transition metal chalcogenides, silicon phosphorus compounds, metal phosphides, metal nitrides, metal borides or metal carbides.
CN202021812486.6U 2020-08-26 2020-08-26 Two-dimensional material purification device Active CN213231532U (en)

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Effective date of registration: 20231206

Address after: 443007 No. 66-2 Ting Ting Road, Ting Ting District, Yichang, Hubei

Patentee after: HUBEI MOPHOS TECHNOLOGY Co.,Ltd.

Address before: 518111 602-4, 6th floor, building B, Baoneng zhichuanggu, no.6, Fukang Road, Pinghu street, Longgang District, Shenzhen City, Guangdong Province

Patentee before: SHENZHEN ZHONGKE MOPHOS TECHNOLOGY Co.,Ltd.

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