CN112871397B - Nanoscale tungsten disulfide material and preparation method and device thereof - Google Patents
Nanoscale tungsten disulfide material and preparation method and device thereof Download PDFInfo
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- CN112871397B CN112871397B CN202011581264.2A CN202011581264A CN112871397B CN 112871397 B CN112871397 B CN 112871397B CN 202011581264 A CN202011581264 A CN 202011581264A CN 112871397 B CN112871397 B CN 112871397B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C21/00—Disintegrating plant with or without drying of the material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/12—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
Abstract
The invention discloses a nano-scale tungsten disulfide material and a preparation method and a device thereof, wherein the nano-scale tungsten disulfide material comprises the following raw material components in parts by weight: calcium chloride solution, sodium tungstate solution, cyclohexane solution, n-butane solution, hydrochloric acid and high-purity sulfur powder; the preparation method of the nano-scale tungsten disulfide material comprises the following steps: weighing raw materials according to a formula ratio, preparing calcium tungstate, preparing tungsten oxide, preparing tungsten disulfide, crushing and crushing; the device for the preparation method of the nanoscale tungsten disulfide material is used for crushing and crushing the tungsten disulfide material to prepare the nanoscale tungsten disulfide. The tungsten disulfide material disclosed by the invention is simple in preparation process, safe and reliable, simple to operate and good in preparation effect, and toxic gas is not used.
Description
Technical Field
The invention relates to a tungsten disulfide material, in particular to a nano-scale tungsten disulfide material and a preparation method and a device thereof.
Background
The tungsten disulfide has the molecular formula of WS2, the molecular weight of 247.97, fine crystals or powder with gray ribbon metallic luster, belongs to a hexagonal system, has semiconductivity and diamagnetism, and is prepared from natural minerals of wolframite, has a layered structure, is easy to dissociate and has lubricating property similar to graphite. As lubricants, e.g. for aerosols. The existing tungsten disulfide is prepared by reacting ammonium tungstate with hydrogen sulfide gas, the hydrogen sulfide gas is inflammable, the preparation process is leaked, the air is easily polluted, the personnel poisoning is caused, the existing tungsten disulfide powder is lack of pulverization, and the particles are too large and are not beneficial to use.
Aiming at the existing problems, a nano-scale tungsten disulfide material, a preparation method and a device thereof are designed.
Disclosure of Invention
The invention aims to provide a nanoscale tungsten disulfide material and a preparation method and a preparation device thereof, the nanoscale tungsten disulfide material is small in particles, convenient to use, simple and easy to obtain raw materials, safe and reliable, toxic hydrogen sulfide gas is not generated in the preparation process, a second rack on a crusher is matched with a second gear, a control ball body is used for crushing tungsten disulfide, the crushed tungsten disulfide is poured into the crusher to be crushed into powder and crushed into nanoscale particles, the nanoscale tungsten disulfide material is convenient to use, the tungsten disulfide material is placed on a movable frame to be conveniently moved, the structure is simple, and the operation is convenient.
The purpose of the invention can be realized by the following technical scheme:
the nanometer tungsten disulfide material comprises the following raw material components in parts by weight: 10-20 parts of calcium chloride solution, 10-20 parts of sodium tungstate solution, 50 parts of cyclohexane solution, 50 parts of n-butane solution, 20-40 parts of hydrochloric acid and 40-80 parts of high-purity sulfur powder.
Further, a preparation method of the nano-scale tungsten disulfide material comprises the following steps:
s1, weighing the raw materials according to the formula ratio.
S2 preparation of calcium tungstate
Respectively dripping a calcium chloride solution and a sodium tungstate solution into a cyclohexane solution and a normal butane solution, stirring for 30 minutes to obtain a microemulsion, mixing and stirring for 30 minutes, standing and precipitating for 1 hour to obtain a white precipitate, filtering, washing, and drying to obtain a calcium tungstate crystal.
S3 preparation of tungsten oxide
Adding calcium tungstate crystals into a hydrochloric acid solution, uniformly stirring for 1 hour to obtain tungstic acid and a precipitate, filtering to obtain a tungstic acid solution, and heating at the high temperature of 500 ℃ to obtain tungsten oxide.
S4, preparation
Placing high-purity sulfur powder in a container, placing tungsten oxide in a quartz boat, cleaning a substrate with an oxide layer on the surface, placing the substrate on the quartz boat, placing the quartz boat in the quartz tube, connecting one end of the quartz tube with the container and the other end with an air pump, and vacuumizing the quartz tube by using the air pump.
S5 preparation of tungsten disulfide
Heating the quartz tube to heat the container to obtain sulfur vapor, introducing the sulfur vapor into the quartz tube, reacting tungsten oxide with the sulfur vapor to generate tungsten disulfide and oxygen, and recovering the oxygen and the redundant sulfur vapor by the air pump.
S6, crushing
And taking the substrate out of the quartz tube, taking the tungsten disulfide on the substrate down, and crushing to generate tungsten disulfide powder.
S7, crushing
And (3) crushing the tungsten disulfide powder for 30 minutes to prepare the nano-scale tungsten disulfide.
Further, the drying temperature is 90-100 ℃.
Further, the heating temperature of the quartz tube is 1400-1800 ℃.
The utility model provides a device of nanometer tungsten disulfide material preparation method, the device includes the workstation, the workstation is fastened and is equipped with the removal frame that is used for placing tungsten disulfide, and the workstation is fastened and is equipped with the breaker, and it is equipped with the carriage release lever that is used for tungsten disulfide breakage to slide on the breaker, and the workstation is fastened and is equipped with the kibbling rubbing crusher that is used for tungsten disulfide, and the rubbing crusher is fastened and is equipped with the casing, fixes being equipped with the inserted bar that is used for fixed high breaker on the workstation.
The crusher is characterized in that a first mounting groove for mounting the crusher is formed in the workbench, a spring for damping is fixedly arranged in the first mounting groove, a jack for mounting an insert rod is arranged in the first mounting groove, a sliding groove is formed in the workbench, a first rack is tightly arranged in the sliding groove, and a second mounting groove for mounting the crusher is formed in the workbench.
Further, the movable frame comprises two sliding blocks, a first gear is arranged on one side of each sliding block in a rotating mode, a first motor is fixedly arranged on the other side of each sliding block, the output end of the first motor is fixedly connected with the first gear, a hydraulic rod is fixedly arranged on each sliding block, the output end of the hydraulic rod is fixedly connected with a first mounting plate, a second mounting plate is arranged on one side of the first mounting plate in a rotating mode, a second motor is arranged on the other side of each first mounting plate, the output end of the second motor is fixedly connected with the second mounting plate, a double-headed screw rod is rotatably arranged between the second mounting plates, a first guide rod is fixedly arranged between the second mounting plates, a third motor is fixedly arranged on one side of each second mounting plate, the output end of the third motor is fixedly connected with the double-headed screw rod, symmetrically distributed is arranged on the first guide rod, the double-headed screw rod penetrates through the movable plate and is in threaded fit with the movable plate, clamping blocks are arranged on one side of the movable plate, and a placing piece is fixedly arranged between the clamping blocks.
Further, the slider is matched with the sliding groove, and the first gear is matched with the first rack.
Further, the breaker includes the fixed plate, is equipped with the fixed slot on the fixed plate, and the fixed plate sets firmly the processing platform, and the processing bench is equipped with the standing groove, and the fixed mounting bracket that is equipped with on the fixed plate rotates on the mounting bracket and is equipped with first lead screw, fixedly on the mounting bracket being equipped with second guide arm and fourth motor, and the output and the first lead screw fastening of fourth motor are connected, are equipped with the sliding plate on the second guide arm, and first lead screw runs through the sliding plate and with sliding plate screw-thread fit.
The sliding plate is fixedly provided with a vertical plate, the vertical plate is provided with a through groove, a second lead screw is arranged in the through groove in a rotating mode, a fifth motor is fixedly arranged on the vertical plate, the output end of the fifth motor is fixedly connected with the second lead screw, a moving block is arranged in the through groove in a sliding mode, the second lead screw penetrates through the moving block and is in threaded fit with the moving block, a connecting rod is arranged on one side of the moving block, a second gear is arranged on one side of the vertical plate in a rotating mode, a swing rod is arranged on one side of the second gear in a fastening mode, a through groove is formed in the swing rod, a push block is arranged in the through groove in a sliding mode, one end of the connecting rod is connected with the moving block in a rotating mode, the other end of the connecting rod is connected with the push block in a rotating mode, a shaft sleeve used for leakage prevention is fixedly arranged on the sliding plate, and a limiting groove is formed in the shaft sleeve.
Furthermore, a second rack is fixedly arranged on the moving rod, a limiting block is arranged on the moving rod, and a ball body for crushing tungsten disulfide is fixedly arranged at one end of the moving rod.
The movable rod is matched with the shaft sleeve, the limiting block is matched with the limiting groove, and the second rack is matched with the second gear.
Further, be equipped with the collecting vat that is used for collecting nanometer tungsten disulfide powder on the rubbing crusher, be equipped with the installation piece on the rubbing crusher, be equipped with the feed port on the installation piece and be used for the screw hole of fixed casing, installation piece one side is rotated and is equipped with the pivot, the fixed sixth motor that is equipped with of opposite side, the output and the pivot fastening connection of sixth motor, the crushing blade that array distributes has set firmly in the pivot, the one end and the installation piece of pivot rotate to be connected, the other end and lower flitch fastening connection, installation piece one side is equipped with the deflector, it is equipped with the casing to slide on the deflector, the fixed block has set firmly on the casing, be equipped with the feeder hopper on the fixed block, feeder hopper and feed port intercommunication, be equipped with the through hole on the fixed block.
The screw rod penetrates through the through hole to be matched with the threaded hole.
The invention has the beneficial effects that:
1. the nano-grade tungsten disulfide material has small particles, is convenient to use, has a simple and easily-obtained raw material, does not generate toxic hydrogen sulfide gas in the preparation process, and is safe and reliable;
2. according to the device for preparing the nano-grade tungsten disulfide material, the second rack on the crusher is matched with the second gear, the ball is controlled to crush tungsten disulfide, the tungsten disulfide is crushed into powder and then poured into the crusher to be crushed into nano-grade particles, and the device is convenient to use.
3. According to the device for preparing the nano-grade tungsten disulfide material, the tungsten disulfide is placed on the movable frame, so that the device is convenient to move, simple in structure and convenient to operate.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic view of the structure of a production apparatus of the present invention;
FIG. 2 is a schematic view of the table of the present invention;
FIG. 3 is a schematic view of the structure of the mobile frame of the present invention;
FIG. 4 is an enlarged schematic view of the structure at A in FIG. 3;
FIG. 5 is a schematic view of the crusher of the present invention;
FIG. 6 is an enlarged view of the structure at B in FIG. 5;
FIG. 7 is a schematic view of the travel bar configuration of the present invention;
figure 8 is a schematic illustration of the exploded structure of the shredder of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A nano-scale tungsten disulfide material comprises the following raw material components in parts by weight: 10-20 parts of calcium chloride solution, 10-20 parts of sodium tungstate solution, 50 parts of cyclohexane solution, 50 parts of n-butane solution, 20-40 parts of hydrochloric acid and 40-80 parts of high-purity sulfur powder.
A preparation method of a nano-scale tungsten disulfide material comprises the following steps:
s1, weighing the raw materials according to the formula ratio.
S2 preparation of calcium tungstate
Respectively dripping a calcium chloride solution and a sodium tungstate solution into a cyclohexane solution and a normal butane solution, stirring for 30 minutes to obtain a microemulsion, mixing and stirring for 30 minutes, standing and precipitating for 1 hour to obtain a white precipitate, filtering and washing, and drying at the temperature of 90-100 ℃ to obtain a calcium tungstate crystal.
S3 preparation of tungsten oxide
Adding calcium tungstate crystals into a hydrochloric acid solution, uniformly stirring for 1 hour to obtain tungstic acid and a precipitate, filtering to obtain a tungstic acid solution, and heating at the high temperature of 500 ℃ to obtain tungsten oxide.
S4, preparation
Placing high-purity sulfur powder in a container, placing tungsten oxide in a quartz boat, cleaning a substrate with an oxide layer on the surface, placing the substrate on the quartz boat, placing the quartz boat in the quartz tube, connecting one end of the quartz tube with the container and the other end with an air pump, and vacuumizing the quartz tube by using the air pump.
S5 preparation of tungsten disulfide
Heating the quartz tube to 1400-1800 ℃, heating the container to obtain sulfur vapor, introducing sulfur vapor into the quartz tube, reacting tungsten oxide with the sulfur vapor to generate tungsten disulfide and oxygen, and recovering the oxygen and the redundant sulfur vapor by the air pump.
S6, crushing
And taking the substrate out of the quartz tube, taking the tungsten disulfide on the substrate down, and crushing to generate tungsten disulfide powder.
S7, crushing
And (3) crushing the tungsten disulfide powder for 30 minutes to prepare the nano-scale tungsten disulfide.
The invention is further described below by reference to several examples.
Example 1
S1, weighing the calcium chloride solution 10, the sodium tungstate solution 10, the cyclohexane solution 50, the n-butane solution 50, the hydrochloric acid 20 and the high-purity sulfur powder 40.
S2 preparation of calcium tungstate
Respectively dripping a calcium chloride solution and a sodium tungstate solution into a cyclohexane solution and a normal butane solution, stirring for 30 minutes to obtain a microemulsion, mixing and stirring for 30 minutes, standing and precipitating for 1 hour to obtain a white precipitate, filtering and washing, and drying at the temperature of 90 ℃ to obtain a calcium tungstate crystal.
S3 preparation of tungsten oxide
Adding calcium tungstate crystals into a hydrochloric acid solution, uniformly stirring for 1 hour to obtain tungstic acid and a precipitate, filtering to obtain a tungstic acid solution, and heating at the high temperature of 500 ℃ to obtain tungsten oxide.
S4, preparation
Placing high-purity sulfur powder in a container, placing tungsten oxide in a quartz boat, cleaning a substrate with an oxide layer on the surface, placing the substrate on the quartz boat, placing the quartz boat in the quartz tube, connecting one end of the quartz tube with the container and the other end with an air pump, and vacuumizing the quartz tube by using the air pump.
S5 preparation of tungsten disulfide
Heating the quartz tube to 1400 ℃, heating the container to obtain sulfur vapor, introducing sulfur vapor into the quartz tube, reacting tungsten oxide with the sulfur vapor to generate tungsten disulfide and oxygen, and recovering the oxygen and the redundant sulfur vapor by the air pump.
S6, crushing
And taking the substrate out of the quartz tube, taking the tungsten disulfide on the substrate down, and crushing to generate tungsten disulfide powder.
S7, crushing
And (3) crushing the tungsten disulfide powder for 30 minutes to prepare the nano-scale tungsten disulfide.
Example 2
S1, weighing the calcium chloride solution 15, the sodium tungstate solution 15, the cyclohexane solution 50, the n-butane solution 50, the hydrochloric acid 30 and the high-purity sulfur powder 60.
S2 preparation of calcium tungstate
Respectively dripping a calcium chloride solution and a sodium tungstate solution into a cyclohexane solution and a normal butane solution, stirring for 30 minutes to obtain a microemulsion, mixing and stirring for 30 minutes, standing and precipitating for 1 hour to obtain a white precipitate, filtering and washing, and drying at the temperature of 95 ℃ to obtain a calcium tungstate crystal.
S3 preparation of tungsten oxide
Adding calcium tungstate crystals into a hydrochloric acid solution, uniformly stirring for 1 hour to obtain tungstic acid and a precipitate, filtering to obtain a tungstic acid solution, and heating at the high temperature of 500 ℃ to obtain tungsten oxide.
S4, preparation
Placing high-purity sulfur powder in a container, placing tungsten oxide in a quartz boat, cleaning a substrate with an oxide layer on the surface, placing the substrate on the quartz boat, placing the quartz boat in the quartz tube, connecting one end of the quartz tube with the container and the other end with an air pump, and vacuumizing the quartz tube by using the air pump.
S5 preparation of tungsten disulfide
Heating the quartz tube to 1600 ℃, heating the container to prepare sulfur vapor, introducing sulfur vapor into the quartz tube, reacting tungsten oxide with the sulfur vapor to generate tungsten disulfide and oxygen, and recovering the oxygen and the redundant sulfur vapor by the air pump.
S6, crushing
And taking the substrate out of the quartz tube, taking the tungsten disulfide on the substrate down, and crushing to generate tungsten disulfide powder.
S7, crushing
And (3) crushing the tungsten disulfide powder for 30 minutes to prepare the nano-scale tungsten disulfide.
Example 3
S1, weighing the calcium chloride solution 18, the sodium tungstate solution 18, the cyclohexane solution 50, the n-butane solution 50, the hydrochloric acid 35 and the high-purity sulfur powder 70.
S2 preparation of calcium tungstate
Respectively dripping a calcium chloride solution and a sodium tungstate solution into a cyclohexane solution and a normal butane solution, stirring for 30 minutes to obtain a microemulsion, mixing and stirring for 30 minutes, standing and precipitating for 1 hour to obtain a white precipitate, filtering and washing, and drying at the temperature of 98 ℃ to obtain a calcium tungstate crystal.
S3 preparation of tungsten oxide
Adding calcium tungstate crystals into a hydrochloric acid solution, uniformly stirring for 1 hour to obtain tungstic acid and a precipitate, filtering to obtain a tungstic acid solution, and heating at the high temperature of 500 ℃ to obtain tungsten oxide.
S4, preparation
Placing high-purity sulfur powder in a container, placing tungsten oxide in a quartz boat, cleaning a substrate with an oxide layer on the surface, placing the substrate on the quartz boat, placing the quartz boat in the quartz tube, connecting one end of the quartz tube with the container and the other end with an air pump, and vacuumizing the quartz tube by using the air pump.
S5 preparation of tungsten disulfide
Heating the quartz tube to 1700 ℃, heating the container to obtain sulfur steam, introducing sulfur steam into the quartz tube, reacting tungsten oxide with the sulfur steam to generate tungsten disulfide and oxygen, and recovering the oxygen and the redundant sulfur steam by the air pump.
S6, crushing
And taking the substrate out of the quartz tube, taking the tungsten disulfide on the substrate down, and crushing to generate tungsten disulfide powder.
S7, crushing
And (3) crushing the tungsten disulfide powder for 30 minutes to prepare the nano-scale tungsten disulfide.
Example 4
S1, weighing the calcium chloride solution 20, the sodium tungstate solution 20, the cyclohexane solution 50, the n-butane solution 50, the hydrochloric acid 40 and the high-purity sulfur powder 80.
S2 preparation of calcium tungstate
Respectively dripping a calcium chloride solution and a sodium tungstate solution into a cyclohexane solution and a normal butane solution, stirring for 30 minutes to obtain a microemulsion, mixing and stirring for 30 minutes, standing and precipitating for 1 hour to obtain a white precipitate, filtering and washing, and drying at the temperature of 100 ℃ to obtain a calcium tungstate crystal.
S3 preparation of tungsten oxide
Adding calcium tungstate crystals into a hydrochloric acid solution, uniformly stirring for 1 hour to obtain tungstic acid and a precipitate, filtering to obtain a tungstic acid solution, and heating at the high temperature of 500 ℃ to obtain tungsten oxide.
S4, preparation
Placing high-purity sulfur powder in a container, placing tungsten oxide in a quartz boat, cleaning a substrate with an oxide layer on the surface, placing the substrate on the quartz boat, placing the quartz boat in the quartz tube, connecting one end of the quartz tube with the container and the other end with an air pump, and vacuumizing the quartz tube by using the air pump.
S5 preparation of tungsten disulfide
Heating the quartz tube to 1800 ℃, heating the container to prepare sulfur vapor, introducing sulfur vapor into the quartz tube, reacting tungsten oxide with the sulfur vapor to generate tungsten disulfide and oxygen, and recovering the oxygen and the redundant sulfur vapor by the air pump.
S6, crushing
Taking out the substrate from the quartz tube, taking off the tungsten disulfide on the substrate, and crushing to generate tungsten disulfide powder
S7, crushing
And (3) crushing the tungsten disulfide powder for 30 minutes to prepare the nano-scale tungsten disulfide.
The device comprises a workbench 1, as shown in figure 1, a moving frame 2 for placing tungsten disulfide is fixedly arranged on the workbench 1, a crusher 3 is fixedly arranged on the workbench 1, a moving rod 4 for crushing tungsten disulfide is slidably arranged on the crusher 3, a pulverizer 5 for pulverizing tungsten disulfide is fixedly arranged on the workbench 1, a shell 6 is fixedly arranged on the pulverizer 5, and an insert rod 7 for fixing the high crusher 3 is fixedly arranged on the workbench 1.
As shown in fig. 2, a first mounting groove 11 for mounting the crusher 3 is provided on the table 1, a spring 12 for damping is fixedly provided in the first mounting groove 11, an insertion hole 13 for mounting the insertion rod 7 is provided in the first mounting groove 11, a sliding groove 14 is provided on the table 1, a first rack 15 is tightly provided in the sliding groove 14, and a second mounting groove 16 for mounting the crusher 5 is provided on the table 1.
As shown in fig. 3 and 4, the moving frame 2 includes two sliding blocks 21, one side of the sliding block 21 is rotatably provided with a first gear 22, the other side is fixedly provided with a first motor 20, the output end of the first motor 20 is fixedly connected with the first gear 22, the sliding block 21 is fixedly provided with a hydraulic rod 23, the output end of the hydraulic rod 23 is fixedly connected with a first mounting plate 24, one side of the first mounting plate 24 is rotatably provided with a second mounting plate 25, the other side is provided with a second motor 240, the output end of the second motor 240 is fixedly connected with the second mounting plate 25, a double-head screw 26 is rotatably arranged between the second mounting plates 25, a first guide rod 27 is fixedly arranged between the second mounting plates 25, one side of the second mounting plate 25 is fixedly provided with a third motor 260, the output end of the third motor 260 is fixedly connected with the double-head screw 26, the first guide rod 27 is provided with symmetrically distributed moving plates 28, the double-head screw 26 penetrates through the moving plate 28 and is in threaded fit with the moving plate 28, clamping blocks 29 are arranged on one side of the moving plate 28, and a placing piece 200 is fixedly arranged between the clamping blocks 29.
The slider 21 cooperates with the runner 14 and the first gear 22 cooperates with the first rack 15.
As shown in fig. 5 and 6, the crusher 3 includes a fixed plate 31, a fixed groove 311 is disposed on the fixed plate 31, a processing table 32 is fixedly disposed on the fixed plate 31, a placement groove 33 is disposed on the processing table 32, an installation frame 31 is fixedly disposed on the fixed plate 31, a first lead screw 36 is rotatably disposed on the installation frame 31, a second lead screw 35 and a fourth motor 30 are fixedly disposed on the installation frame 31, an output end of the fourth motor 30 is fixedly connected with the first lead screw 36, a sliding plate 37 is disposed on the second lead screw 35, the first lead screw 36 penetrates through the sliding plate 37 and is in threaded engagement with the sliding plate 37, a vertical plate is fixedly disposed on the sliding plate 37, a through groove 372 is disposed on the vertical plate 371, a second lead screw 373 is rotatably disposed in the through groove 372, a fifth motor 370 is fixedly disposed on the vertical plate 371, an output end of the fifth motor 370 is fixedly connected with the second lead screw 373, a moving block 38 is slidably disposed in the through groove 372, the second lead screw 373 is in threaded engagement with the moving block 38, a connecting rod 380 is arranged on one side of the moving block 38, a second gear 39 is rotatably arranged on one side of the vertical plate 371, a swing rod 391 is fixedly arranged on one side of the second gear 39, a through groove 392 is formed in the swing rod 391, a push block 381 is slidably arranged in the through groove 392, one end of the connecting rod 380 is rotatably connected with the moving block 38, the other end of the connecting rod 380 is rotatably connected with the push block 381, a shaft sleeve 374 for preventing leakage is fixedly arranged on the sliding plate 37, and a limiting groove 375 is formed in the shaft sleeve 374.
As shown in fig. 7, a second rack 41 is fixedly arranged on the moving rod 4, a limiting block 42 is arranged on the moving rod 4, and a ball 43 for crushing tungsten disulfide is fixedly arranged at one end of the moving rod 4.
The travel bar 4 engages the sleeve 374, the stop 42 engages the stop slot 375, and the second rack 41 engages the second gear 39.
As shown in fig. 8, a collecting tank 51 for collecting nano tungsten disulfide powder is disposed on the pulverizer 5, a mounting block 52 is disposed on the pulverizer 5, a feeding hole 53 and a threaded hole 54 for fixing the housing 6 are disposed on the mounting block 52, a rotating shaft 55 is rotatably disposed on one side of the mounting block 52, a sixth motor 50 is fixedly disposed on the other side of the mounting block 50, an output end of the sixth motor 50 is fixedly connected with the rotating shaft 55, crushing blades 56 distributed in an array are fixedly disposed on the rotating shaft 55, one end of the rotating shaft 55 is rotatably connected with the mounting block 52, the other end of the rotating shaft is fixedly connected with a blanking plate 58, a guide plate 57 is disposed on one side of the mounting block 52, the housing 6 is slidably disposed on the guide plate 57, a fixing block 61 is fixedly disposed on the housing 6, a feeding hopper 62 is disposed on the fixing block 61, the feeding hopper 62 is communicated with the feeding hole 53, and a through hole 63 is disposed on the fixing block 61.
The screw rod passes through the through hole 63 to be matched with the threaded hole 54.
When the tungsten disulfide mill is used, tungsten disulfide prepared in S5 is taken down and placed in the placing piece 200, the moving frame 2 is moved to the crusher 3, the hydraulic rod 23 contracts, the clamping block 29 and the placing piece 200 are placed in the placing groove 33, the first lead screw 36 rotates, the sliding plate 37 moves until the shaft sleeve 374 is attached to the processing table 32, the second lead screw 373 rotates to reciprocate the moving block 38, the swing rod 391 rotates to drive the moving rod 4 to reciprocate the second gear 39, the ball 43 performs S6 crushing operation on tungsten disulfide, the moving frame 2 moves to the crusher 5, the second motor 240 rotates the second mounting plate 25, tungsten disulfide powder in the placing piece 200 is poured into the feed hopper 62, the rotating shaft 55 rotates to grind the tungsten disulfide powder by the grinding blade 56, the S7 grinding operation is performed, after 30 minutes, the nano-scale tungsten disulfide is prepared, the shell 6 is opened, the blanking plate 58 pushes out the nano-scale tungsten disulfide in the shell 6 and falls into the collecting tank 51.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (8)
1. The preparation method of the nanometer tungsten disulfide material is characterized in that the nanometer tungsten disulfide material comprises the following raw material components in parts by weight: 10-20 parts of calcium chloride solution, 10-20 parts of sodium tungstate solution, 50 parts of cyclohexane solution, 50 parts of n-butane solution, 20-40 parts of hydrochloric acid and 40-80 parts of high-purity sulfur powder;
the preparation method comprises the following steps:
s1, weighing the raw materials according to the formula ratio;
s2 preparation of calcium tungstate
Respectively dripping a calcium chloride solution and a sodium tungstate solution into a cyclohexane solution and a normal butane solution, stirring for 30 minutes to obtain a microemulsion, mixing and stirring for 30 minutes, standing and precipitating for 1 hour to obtain a white precipitate, filtering, washing, and drying to obtain a calcium tungstate crystal;
s3 preparation of tungsten oxide
Adding calcium tungstate crystals into a hydrochloric acid solution, uniformly stirring for 1 hour to obtain tungstic acid and a precipitate, filtering to obtain a tungstic acid solution, and heating at a high temperature of 500 ℃ to obtain tungsten oxide;
s4, preparation
Placing high-purity sulfur powder in a container, placing tungsten oxide in a quartz boat, cleaning a substrate with an oxide layer on the surface, placing the substrate on the quartz boat, placing the quartz boat in a quartz tube, connecting one end of the quartz tube with the container and the other end with an air pump, and vacuumizing the quartz tube by using the air pump;
s5 preparation of tungsten disulfide
Heating the quartz tube to heat the container to obtain sulfur vapor, introducing the sulfur vapor into the quartz tube, reacting tungsten oxide with the sulfur vapor to generate tungsten disulfide and oxygen, and recovering the oxygen and the redundant sulfur vapor by the air pump;
s6, crushing
Taking the substrate out of the quartz tube, taking the tungsten disulfide on the substrate down, and crushing to generate tungsten disulfide powder;
s7, crushing
Crushing the tungsten disulfide powder for 30 minutes to prepare nano-scale tungsten disulfide;
the device for preparing the nanoscale tungsten disulfide material comprises a workbench (1), wherein a moving frame (2) for placing tungsten disulfide is fixedly arranged on the workbench (1), a crusher (3) is fixedly arranged on the workbench (1), a moving rod (4) for crushing tungsten disulfide is slidably arranged on the crusher (3), a pulverizer (5) for pulverizing tungsten disulfide is fixedly arranged on the workbench (1), a shell (6) is fixedly arranged on the pulverizer (5), and an inserting rod (7) for fixing the high crusher (3) is fixedly arranged on the workbench (1);
be equipped with first mounting groove (11) that are used for installing breaker (3) on workstation (1), first mounting groove (11) internal fixation is equipped with and is used for absorbing spring (12), is equipped with jack (13) that are used for installing inserted bar (7) in first mounting groove (11), is equipped with spout (14) on workstation (1), and the fastening is equipped with first rack (15) in spout (14), is equipped with second mounting groove (16) that are used for installing rubbing crusher (5) on workstation (1).
2. The method for preparing the nano-scale tungsten disulfide material according to claim 1, wherein the drying temperature in the S2 is 90-100 ℃.
3. The method for preparing nano-scale tungsten disulfide material according to claim 1, wherein the heating temperature of the quartz tube is 1400-1800 ℃.
4. The device for preparing the nano-scale tungsten disulfide material according to claim 1, wherein the moving frame (2) comprises two sliding blocks (21), one side of each sliding block (21) is rotatably provided with a first gear (22), the other side of each sliding block is fixedly provided with a first motor (20), the output end of each first motor (20) is fixedly connected with the first gear (22), a hydraulic rod (23) is fixedly arranged on each sliding block (21), the output end of each hydraulic rod (23) is fixedly connected with a first mounting plate (24), one side of each first mounting plate (24) is rotatably provided with a second mounting plate (25), the other side of each first mounting plate is provided with a second motor (240), the output end of each second motor (240) is fixedly connected with the second mounting plate (25), a double-head screw (26) is rotatably arranged between the second mounting plates (25), and a first guide rod (27) is fixedly arranged between the second mounting plates (25), second mounting panel (25) one side is fixed and is equipped with third motor (260), the output and double-end lead screw (26) fastening connection of third motor (260), is equipped with symmetric distribution's movable plate (28) on first guide arm (27), double-end lead screw (26) run through movable plate (28) and with movable plate (28) screw-thread fit, movable plate (28) one side is equipped with clamp splice (29), fixedly between clamp splice (29) be equipped with place piece (200).
5. The apparatus for preparing nano-scale tungsten disulfide material according to claim 4, wherein the slider (21) is engaged with the chute (14), and the first gear (22) is engaged with the first rack (15).
6. The device for preparing the nano-scale tungsten disulfide material according to claim 1, wherein the crusher (3) comprises a fixed plate (31), a fixed groove (311) is formed in the fixed plate (31), a processing table (32) is tightly fixed on the fixed plate (31), a placing groove (33) is formed in the processing table (32), a mounting frame is fixedly arranged on the fixed plate (31), a first lead screw (36) is rotatably arranged on the mounting frame, a second guide rod (35) and a fourth motor (30) are fixedly arranged on the mounting frame, an output end of the fourth motor (30) is tightly connected with the first lead screw (36), a sliding plate (37) is arranged on the second guide rod (35), and the first lead screw (36) penetrates through the sliding plate (37) and is in threaded fit with the sliding plate (37);
a vertical plate (371) is fixedly arranged on the sliding plate (37), a through groove (372) is arranged on the vertical plate (371), a second lead screw (373) is rotationally arranged in the through groove (372), a fifth motor (370) is fixedly arranged on the vertical plate (371), the output end of the fifth motor (370) is fixedly connected with the second lead screw (373), a moving block (38) is arranged in the through groove (372) in a sliding manner, the second lead screw (373) penetrates through the moving block (38) and is in threaded fit with the moving block (38), a connecting rod (380) is arranged on one side of the moving block (38), a second gear (39) is rotationally arranged on one side of the vertical plate (371), a swing rod (391) is fixedly arranged on one side of the second gear (39), a through groove (392) is arranged on the swing rod (391), a pushing block (381) is arranged in the through groove (392) in a sliding manner, one end of the connecting rod (380) is rotationally connected with the moving block (38), and the other end is rotationally connected with the pushing block (381), a shaft sleeve (374) for leakage prevention is fixedly arranged on the sliding plate (37), and a limit groove (375) is arranged in the shaft sleeve (374).
7. The device for preparing the nano-scale tungsten disulfide material according to claim 6, wherein the moving rod (4) is fixedly provided with a second rack (41), the moving rod (4) is provided with a limiting block (42), and one end of the moving rod (4) is tightly provided with a ball (43) for crushing tungsten disulfide;
the moving rod (4) is matched with the shaft sleeve (374), the limiting block (42) is matched with the limiting groove (375), and the second rack (41) is matched with the second gear (39).
8. The device for preparing the nano-scale tungsten disulfide material according to claim 1, wherein a collecting groove (51) for collecting nano-scale tungsten disulfide powder is arranged on the pulverizer (5), a mounting block (52) is arranged on the pulverizer (5), a feeding hole (53) and a threaded hole (54) for fixing the shell (6) are arranged on the mounting block (52), a rotating shaft (55) is rotatably arranged on one side of the mounting block (52), a sixth motor (50) is fixedly arranged on the other side of the mounting block (5), the output end of the sixth motor (50) is tightly connected with the rotating shaft (55), crushing blades (56) distributed in an array are fixedly arranged on the rotating shaft (55), one end of the rotating shaft (55) is rotatably connected with the mounting block (52), the other end of the rotating shaft is tightly connected with the blanking plate (58), a guide plate (57) is arranged on one side of the mounting block (52), the shell (6) is slidably arranged on the guide plate (57), a fixed block (61) is fixedly arranged on the shell (6), a feed hopper (62) is arranged on the fixed block (61), the feed hopper (62) is communicated with the feed hole (53), and a through hole (63) is arranged on the fixed block (61);
the screw rod passes through the through hole (63) to be matched with the threaded hole (54).
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| CN103641173B (en) * | 2013-11-04 | 2016-03-02 | 江苏大学 | The preparation method of one kind Graphene tungsten disulfide nano slices |
| CN104449708B (en) * | 2014-11-20 | 2016-10-05 | 重庆文理学院 | The preparation method of synthesizing high lumineseent intensity artificial schellite crystallite under a kind of room temperature |
| CN106811731A (en) * | 2016-11-17 | 2017-06-09 | 北京交通大学 | A kind of controllable method for preparing of tungsten disulfide |
| CN107416905B (en) * | 2017-06-22 | 2019-03-08 | 河南大学 | A kind of preparation method of oil-soluble tungsten disulfide nano slices |
| CN107557754B (en) * | 2017-07-21 | 2019-09-20 | 杭州电子科技大学 | A kind of preparation method of tungsten disulfide film |
| CN108046327B (en) * | 2017-12-26 | 2020-05-05 | 佛山科学技术学院 | Preparation method of tungsten disulfide nanotube |
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