Method and apparatus for closed cycle fluorine chemical vapor deposition of high purity materials

Abstract

The application discloses a method and a preparation device for closed-circuit fluorine compound chemical vapor deposition of high-purity materials, and belongs to the technical field of high-purity material preparation of semiconductors. The closed-circuit fluorine compound reduces the harm of fluorine element tail gas in the preparation of materials by chemical vapor deposition, and the fluorine element tail gas does not need to be collected and treated, so that the environment is friendly. Meanwhile, the application has high purification efficiency, is suitable for the purification of most refractory metals and the purification of some semiconductor transition metal elements, can purify crude-purity materials to high-purity materials in one step, can realize the purpose of quantitative feeding, prevents the reaction effect from being affected by the stacking of purified materials in a reaction kettle, provides a certain amplitude to a feeding bin, makes the purified materials in the feeding bin vibrate, so that the blocking condition can be prevented, the stability of the feeding bin in receiving the purified materials is improved, the blocking condition of the feeding box caused by the stacking of the purified materials is avoided, and the application of quantitative feeding is favorable to the sufficient reaction of the purified materials.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of semiconductor high-purity material preparation, and particularly relates to a closed-circuit fluorine compound chemical vapor deposition high-purity material preparation method and device. BACKGROUND

[0002] With the development of more advanced and more fine semiconductor processes, the purity of semiconductor materials is required to be higher and higher. In the chemical vapor deposition process for preparing high-purity semiconductor materials, the precursors are mostly fluorine-containing compounds such as WF6, MoF6 and AsF3. The fluorine compound contains halogen components, and the tail gas treatment cannot fundamentally eliminate the fluorine element hazards. The defects of the prior art are as follows:

[0003] 1. In the prior art of chemical vapor deposition for preparing high-purity materials, the utilization rate of fluorine elements is low, and the tail gas hazards are large.

[0004] 2. In the traditional chemical vapor deposition process for preparing high-purity materials, chlorine gas / bromine gas and other methods with high safety factor but high reaction energy consumption are used.

[0005] 3. In the prior art of chemical vapor deposition for preparing high-purity materials, the process needs to be carried out in a sealed environment. During the feeding process, the materials are prone to accumulate, causing blockage of the material pipe and failure to achieve the purpose of quantitative feeding. In addition, the materials and reactants cannot fully react, which is not conducive to the generation of products.

[0006] The application adopts a closed-circuit fluorine element recycling method, which is a closed-circuit fluorine compound chemical vapor deposition high-purity material preparation method. SUMMARY

[0007] In order to overcome the above defects, the application provides a closed-circuit fluorine compound chemical vapor deposition high-purity material preparation method and device, which solves the problem of fluorine element hazards in the chemical vapor deposition process using fluorine-containing precursors and achieves the purpose of recycling halogen compounds.

[0008] To achieve the above purpose, the application provides the following technical scheme: a closed-circuit fluorine compound chemical vapor deposition high-purity material preparation method, comprising the following steps:

[0009] S1. Feeding materials with a crude purity, and selecting a material to be purified with a purity of 99%-99.99%;

[0010] S2. Under a heating condition, fluorine gas reacts with the purified material to generate a binary fluorine compound;

[0011] S3. Purifying and separating the binary fluorine compound to separate out a target material containing fluorine compound;

[0012] S4. Under a heating condition, hydrogen gas reacts with the binary fluorine compound to reduce the purified material;

[0013] S5, the purified material is detected for purity, and if the product meets the standard, the product is qualified, and if the standard is not met, the material is repeatedly input into S2 process step;

[0014] S6, hydrogen fluoride generated by hydrogen reduction of binary fluoride in S4 is purified;

[0015] S7, the purified hydrogen fluoride in S6 is electrolyzed to prepare high-purity hydrogen and high-purity fluorine.

[0016] As a further scheme of the present application: in S2, the purity of fluorine gas is 99.999%-99.99999%, and in S4, the purity of hydrogen gas is 99.999%-99.99999%.

[0017] As a further scheme of the present application: in S7, fluorine gas is used for fluorination reaction in S2, and hydrogen gas is used for hydrogen reduction reaction in S4.

[0018] As a further scheme of the present application: S2 and S4 are step-by-step reactions of chemical vapor deposition:

[0019] S2 and S4 are separately reacted in separate chambers, that is, fluorination reaction is first carried out and then hydrogen reduction reaction is carried out;

[0020] S2 and S4 are reacted in one chamber, fluorination reaction is in a reaction zone, and hydrogen reduction is in a deposition zone.

[0021] As a further scheme of the present application: the purified material in S1 is a refractory metal or a transition metal, containing W, Mo, Ir, Rh, Nb, Ta, As, Te, Sb or Se, and the detection method in S5 includes GDMS or ICP-MS method.

[0022] A preparation device for closed-loop cycle fluoride chemical vapor deposition of high-purity material, the preparation device applied to feeding in S1 includes a reaction kettle, a discharge valve is arranged at the bottom of the reaction kettle, a feed bin is arranged above the reaction kettle, and a sealing cover is connected to the top of the feed bin;

[0023] Both sides of the bottom of the feed bin are fixedly connected with baffles, both baffles are fixed with the base, the base is fixedly connected with the top of the reaction kettle, the bottom of the feed bin is in communication with the feeding inlet of the reaction kettle through a feeding box, a quantitative feeding assembly is arranged in the feeding box, the bottom end of the quantitative feeding assembly is fixed with the base, both sides of the quantitative feeding assembly are respectively connected with knocking assemblies, the knocking assemblies are overlapped with the outer wall of the baffles, the side of the knocking assembly away from the baffle is fixedly connected with a supporting assembly, and the bottom of the supporting assembly is fixedly connected with the base.

[0024] As a further scheme of the present application: the quantitative feeding assembly comprises four grooves formed in the outer wall of the rotating roller, the included angle between the four grooves is 90 degrees, a connecting shaft is clamped in the middle of the rotating roller, and the two ends of the connecting shaft are fixedly connected with the rotating disc.

[0025] As a further scheme of the present application: the rotating disc is externally provided with two protrusions, one side of the protrusion is designed to be inclined, and the other side of the protrusion is designed to be vertical, one end of the connecting shaft is fixedly connected with the output shaft of the motor, a machine base is clamped outside the motor body, and the machine base is fixedly connected with the base.

[0026] As a further scheme of the present application: two groups of baffle plates are arranged on the two sides in the feeding box, and the number of each group of baffle plates is two, and the opposite two baffle plates are designed to be inversely V-shaped.

[0027] As a further scheme of the present application: the knocking assembly comprises a knocking plate, the inner side of the knocking plate is overlapped with the outer wall of the baffle plate, two connecting rods are fixedly connected to the side of the knocking plate close to the stock bin, and one end of the connecting rod is connected with a pulley.

[0028] As a further scheme of the present application: the two sides of the bottom of the knocking plate are fixedly connected with sliding plates, the positions corresponding to the sliding plates are provided with sliding rails on the base, the sliding plates are slidingly connected in the sliding rails, and the sliding plate and the sliding rail are designed to be T-shaped.

[0029] As a further scheme of the present application: the supporting assembly comprises a side plate, the bottom of the side plate is fixedly connected with the base, a spring is fixedly connected to the side of the side plate close to the stock bin, the spring is fixedly connected with the outer wall of the knocking plate, and the inner wall of the baffle plate is fixedly connected with the bottom of the stock bin through three inclined supporting rods.

[0030] Compared with the prior art, the present application has the following advantages:

[0031] 1. In the present application, the closed-circuit fluorine compound reduces the harm of fluorine element tail gas in the chemical vapor deposition preparation material, and the fluorine element tail gas does not need to be collected and treated, which is environmentally friendly. Meanwhile, the purification efficiency is high, the application range is wide, and it is suitable for the purification of most refractory metals and part of semiconductor transition metal elements. The crude purity material can be purified to high purity material in one step.

[0032] 2. In the present application, the stock bin is arranged to store the purified material, and the purified material in the stock bin falls into the groove. When the purified material is reacted, the motor is controlled to work, the output shaft of the motor drives the rotating roller to rotate through the connecting shaft, so that the purified material in the groove can be sent to the lower side of the feeding box, and the purified material falls into the reaction kettle, thereby achieving the purpose of quantitative feeding, preventing the purified material from being stacked in the reaction kettle to affect the reaction effect, and enabling the purified material to fully react.

[0033] 3、The application, through the connecting shaft in the process of rotation can drive two rotating disc rotation, rotating disc rolling in the process of the pulley on the convex and pulley contact, the convex can push two pulley, make two pulley respectively through two connecting rod drive two knock plate away from each other and away from the baffle, when the convex on the rotating disc away from the pulley, through the spring force to support the knock plate, make knock plate can quickly close to the baffle, and knock the baffle, baffle can transmit the amplitude to the silo through the baffle and support rod after vibration, by providing a certain amplitude to the silo, make the silo in purification materials occur shaking, thus can prevent the emergence of jamming, improve the stability of the trough to accept purification materials, avoid the purification materials appear to cause the jamming of the feeding box, with the application of quantitative feeding, it is beneficial to the purification materials to carry on the full reaction;

[0034] 4、The application, through the pulley and rotating disc contact, reduce the friction between pulley and rotating disc, improve the stability of adjusting the position of knock plate, ensure that the knock plate can work stably for a long time, because the knock plate bottom connects the T-shaped slide plate, and the slide plate slides in the T-shaped slide rail, the slide rail can realize the purpose of slide plate limiting and guiding, make the slide plate not to separate from the slide rail, thus further improve the stability of knock plate work, because the baffle is connected with support rod, and the support rod is fixed with the bottom of the silo, enhance the effect of amplitude transmission, prevent the silo in purification materials jam. BRIEF DESCRIPTION OF DRAWINGS

[0035] Figure 1 The preparation device structure schematic diagram for the application S1 feeding is applied to;

[0036] Figure 2 The partial structure schematic diagram of the application; Figure 1

[0037] Figure 3 The structure schematic diagram of the feeding box and quantitative feeding assembly connection of the application;

[0038] Figure 4 The structure schematic diagram of the knock assembly and support assembly connection of the application;

[0039] Figure 5 The process flow chart of the application;

[0040] Figure 6 The flow reaction diagram of the application;

[0041] ​In the figure: 1, reaction kettle; 2, discharge valve; 3, silo; 4, sealing cover; 5, baffle; 6, base; 7, slide rail; 8, feeding box; 9, quantitative feeding assembly; 901, rotating roller; 902, connecting shaft; 903, trough; 904, motor; 905, machine base; 906, rotating disc; 10, blocking plate; 11, knocking assembly; 111, knocking plate; 112, sliding plate; 113, connecting rod; 114, pulley; 12, supporting assembly; 121, side plate; 122, spring; 13, supporting rod. DETAILED DESCRIPTION

[0042] The technical solutions of the present application will be further described in detail below in combination with specific embodiments.

[0043] As Figures 1-6 shown, the present application provides a technical solution: a method for closed-loop circulation fluorine chemical vapor deposition of high-purity materials, comprising the following steps:

[0044] S1, crude purity of the purified material is fed, and the purity of the material to be purified is selected to be 99%-99.99%;

[0045] S2, under heating conditions, fluorine gas reacts with the purified material to generate binary fluorides;

[0046] S3, binary fluorides are purified and separated, and the target material containing fluorine compounds is separated out;

[0047] S4, under heating conditions, hydrogen gas reacts with binary fluorides to reduce the purified material;

[0048] S5, the purity of the purified material is detected, and if it meets the standard, the product meets the standard, otherwise it is repeatedly fed into the S2 process link;

[0049] S6, the hydrogen fluoride generated by the hydrogen reduction of binary fluorides in S4 is purified;

[0050] S7, the purified hydrogen fluoride in S6 is electrolyzed to prepare high-purity hydrogen gas and high-purity fluorine gas.

[0051] In S2, the purity of fluorine gas is 99.999%-99.99999%, and in S4, the purity of hydrogen gas is 99.999%-99.99999%.

[0052] In S7, fluorine gas is used for fluorination reaction in S2, and hydrogen gas is used for hydrogen reduction reaction in S4.

[0053] S2 and S4 are step-by-step reactions of chemical vapor deposition:

[0054] S2 and S4 are separately reacted in separate chambers, i.e., fluorination reaction is performed first and then hydrogen reduction reaction is performed;

[0055] S2 and S4 are reacted in one chamber, fluorination in the reaction zone and hydrogen reduction in the deposition zone.

[0056] The purified material in S1 is a refractory metal or a transition metal, including W, Mo, Ir, Rh, Nb, Ta, As, Te, Sb or Se, and the detection method in S5 includes GDMS or ICP-MS.

[0057] A preparation device for closed cycle fluorine chemical vapor deposition of high purity material, the preparation device applied to feeding in S1 includes a reaction kettle 1, a discharge valve 2 is arranged at the bottom of the reaction kettle 1, a feed bin 3 is arranged above the reaction kettle 1, and a sealing cover 4 is connected to the top of the feed bin 3. Because the sealing cover 4 is arranged, the feeding work and the reaction in the reaction kettle 1 are ensured to be in a sealed environment, so as to prevent liquid gas from leaking and affecting the reaction effect;

[0058] Two baffles 5 are fixedly connected to the bottom of the feed bin 3, the two baffles 5 are fixed with a base 6, the base 6 is fixedly connected with the top of the reaction kettle 1, the bottom of the feed bin 3 is communicated with the feeding inlet of the reaction kettle 1 through a feeding box 8, and a quantitative feeding assembly 9 is arranged in the feeding box 8. The quantitative feeding assembly 9 includes a rotating roller 901, four grooves 903 are arranged on the outer wall of the rotating roller 901, the included angle between the four grooves 903 is 90 degrees, a connecting shaft 902 is clamped in the middle of the rotating roller 901, and rotating discs 906 are fixedly connected to the two ends of the connecting shaft 902. Because the rotating roller 901 and the grooves 903 are arranged, the purified material in the grooves 903 can be sent to the lower side of the feeding box 8, the purified material falls into the reaction kettle 1, and thus the purpose of quantitative feeding is achieved, so as to prevent the purified material from being stacked in the reaction kettle 1 and affecting the reaction effect;

[0059] Two protrusions are arranged outside the rotating disc 906, one side of the protrusion is designed to be inclined, the other side of the protrusion is designed to be vertical, one end of the connecting shaft 902 is fixedly connected with the output shaft of a motor 904, a machine base 905 is clamped outside the body of the motor 904, and the machine base 905 is fixedly connected with the base 6. Because the protrusions are arranged outside the rotating disc 906, the protrusions can drive the two pulleys 114 to move, so that the two pulleys 114 drive the two knocking plates 111 to move away from each other and away from the baffles 5, so that the knocking plates 111 can perform knocking work subsequently.

[0060] A group of material blocking plates 10 are arranged on both sides in the feeding box 8, and the number of each group of material blocking plates 10 is two. The opposite two material blocking plates 10 are designed to be inversely V-shaped. Because the material blocking plates 10 are arranged, the material blocking plates 10 can scrape off the excess material protruding in the grooves 903, improve the effect of feeding the excess material, and prevent the excess material from being stuck in the gap between the rotating roller 901 and the feeding box 8, so as to prevent the rotating roller 901 from being stuck during rotation.

[0061] The bottom end of the quantitative feeding assembly 9 is fixed with the base 6, and the two sides of the quantitative feeding assembly 9 are respectively connected with a knocking assembly 11. The knocking assembly 11 comprises a knocking plate 111, the inner side of the knocking plate 111 is overlapped with the outer wall of the baffle 5, and the side of the knocking plate 111 close to the bin 3 is fixedly connected with two connecting rods 113. One end of the connecting rod 113 is connected with a pulley 114. Because the pulley 114 is provided, the pulley 114 is in contact with the rotating disc 906, the friction between the pulley 114 and the rotating disc 906 is reduced, the stability of adjusting the position of the knocking plate 111 is improved, and it is ensured that the knocking plate 111 can work stably for a long time.

[0062] The two sides of the bottom of the knocking plate 111 are fixedly connected with sliding plates 112, and the base 6 is provided with sliding rails 7 corresponding to the positions of the sliding plates 112. The sliding plates 112 are slidingly connected in the sliding rails 7, and the sliding plates 112 and the sliding rails 7 are both T-shaped designs. Through the cooperation between the sliding plates 112 and the sliding rails 7, the sliding plates 112 slide in the T-shaped sliding rails 7, the sliding rails 7 can realize the purpose of limiting and guiding the sliding plates 112, the sliding plates 112 will not be separated from the sliding rails 7, and thus the stability of the working of the knocking plate 111 is further improved.

[0063] The knocking assembly 11 is overlapped with the outer wall of the baffle 5, and the side of the knocking assembly 11 away from the baffle 5 is fixedly connected with a supporting assembly 12. The bottom of the supporting assembly 12 is fixedly connected with the base 6. The supporting assembly 12 comprises a side plate 121, the bottom of the side plate 121 is fixedly connected with the base 6, and the side of the side plate 121 close to the bin 3 is fixedly connected with a spring 122. The outer wall of the spring 122 is fixedly connected with the knocking plate 111. The inner wall of the baffle 5 is fixedly connected with the bottom of the bin 3 through three obliquely designed supporting rods 13. The baffle 5 is connected with the supporting rods 13, and the supporting rods 13 are fixed with the bottom of the bin 3, so that the effect of vibration amplitude transmission is enhanced, and the purified material in the bin 3 is prevented from being blocked.

[0064] Through the cooperation between the spring 122 and the knocking plate 111, the elastic force of the spring 122 supports the knocking plate 111, so that the knocking plate 111 can quickly approach the baffle 5 and knock the baffle 5. After the baffle 5 is vibrated, the vibration amplitude can be transmitted to the bin 3 through the baffle 5 and the supporting rods 13. By providing a certain vibration amplitude to the bin 3, the purified material in the bin 3 is shaken, so that the blocking condition can be prevented.

[0065] Embodiment:

[0066] The flow reaction steps of the present application are as follows:

[0067] Step one: 2N crude purity tungsten feeding, tungsten material is powder material, particle size size is 0.1-1mm;

[0068] Step two: under the condition of 450℃, fluorine gas reacts with tungsten material to generate tungsten hexafluoride, and the purity of fluorine gas is 99.9999%.

[0069] Step three: separation and purification of tungsten hexafluoride;

[0070] Step four: under the condition of 500 DEG C, hydrogen and tungsten hexafluoride are reacted to reduce tungsten into tungsten element, and the purity of hydrogen is 99.9999%;

[0071] Step five: the purified material is detected by ICP-MS, and the product meets the standard if the standard is met;

[0072] Step six: hydrogen fluoride generated by hydrogen reduction of tungsten hexafluoride in step four is purified, and the purity of hydrogen fluoride is 99.9999%;

[0073] Step seven: the purified hydrogen fluoride in step six is electrolyzed to prepare high-purity hydrogen and high-purity fluorine, wherein the fluorine is used in the fluorination reaction in step two, the hydrogen is used in the hydrogen reduction reaction in step four, and the purity of the purified fluorine is 99.9999%, and the purity of the purified hydrogen is 99.9999%.

[0074] Advantages compared with prior art:

[0075] In the preparation of high-purity materials by chemical vapor deposition, the utilization rate of fluorine element is low, and the tail gas is harmful, the method provided by the application has 100% utilization rate of fluorine element, and the tail gas does not contain fluorine component

[0076] In the preparation of high-purity materials by traditional chemical vapor deposition process, chlorine gas / bromine gas and other methods with high safety factor but high reaction energy consumption are used, the method provided by the application eliminates the hidden danger of fluorine gas tail gas emission and reduces the energy consumption in the preparation process

[0077] Because fluorine gas has active chemical properties, the purification field to which the application is applied is more extensive than the field of chemical vapor deposition of high-purity materials by chlorine gas / bromine gas.

[0078] The working principle of the application is:

[0079] When in use, the bunker 3 is used to store the purified material, and the purified material in the bunker 3 falls into the trough 903, when the purified material is reacted, the motor 904 is controlled to work, so that the output shaft of the motor 904 drives the rotating roller 901 to rotate through the connecting shaft 902, so that the purified material in the trough 903 can be sent to the lower side of the feeding box 8, and the purified material falls into the reaction kettle 1;

[0080] The connecting shaft 902 can drive the two rotating discs 906 to rotate in the process of rotation, and the pulleys 114 can roll on the outer wall of the rotating disc 906 in the process of rotation of the rotating disc 906, when the protrusions on the rotating disc 906 are in continuous contact with the pulleys 114, the protrusions can drive the two pulleys 114 on both sides to move away from each other and away from the baffle 5 through the two connecting rods 113;

[0081] When the protrusion on the rotating disc 906 is separated from the pulley 114, the knocking plate 111 is supported by the elastic force of the spring 122, so that the knocking plate 111 can quickly approach the baffle 5 and knock the baffle 5, and the baffle 5 can transmit the vibration to the hopper 3 through the baffle 5 and the supporting rod 13, so that the purified material in the hopper 3 is shaken by providing a certain amplitude to the hopper 3;

[0082] The reaction kettle 1 is under heating condition, the fluorine gas reacts with the purified material to generate binary fluoride, the binary fluoride is purified and separated, the target material containing fluorine compound is separated out, under heating condition, the hydrogen gas reacts with the binary fluoride to reduce the purified material, the purified material is detected for purity, if the product meets the standard, the product is qualified, if not, the purified hydrogen fluoride generated by the hydrogen reduction of the binary fluoride in S4 is purified, and the purified hydrogen fluoride in S6 is electrolyzed to prepare high-purity hydrogen gas and high-purity fluorine gas.

[0083] From the above, it can be seen that:

[0084] The hopper 3 is arranged to store the purified material, and the purified material in the hopper 3 falls into the chute 903, when the purified material is reacted, the motor 904 is controlled to work, so that the output shaft of the motor 904 drives the rotating roller 901 to rotate through the connecting shaft 902, so that the purified material in the chute 903 can be sent to the lower side of the feeding box 8, and the purified material falls into the reaction kettle 1, so that the purpose of quantitative feeding is achieved, the reaction effect is prevented from being affected by the stacking of the purified material in the reaction kettle 1, and the purified material can be fully reacted.

[0085] The purpose of quantitative feeding is achieved, the reaction effect is prevented from being affected by the stacking of the purified material in the reaction kettle 1, and the purified material can be fully reacted.

[0086] The hopper 3 is arranged to store the purified material, and the purified material in the hopper 3 falls into the chute 903, when the purified material is reacted, the motor 904 is controlled to work, so that the output shaft of the motor 904 drives the rotating roller 901 to rotate through the connecting shaft 902, so that the purified material in the chute 903 can be sent to the lower side of the feeding box 8, and the purified material falls into the reaction kettle 1, so that the purpose of quantitative feeding is achieved, the reaction effect is prevented from being affected by the stacking of the purified material in the reaction kettle 1, and the purified material can be fully reacted.

[0087] In the description of the present application, it should be noted that unless otherwise specified and limited, the terms "mounting", "connecting", "connecting" should be understood in a broad sense, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected, it can be mechanically connected, or electrically connected, it can be directly connected, or indirectly connected through an intermediate medium, or the internal communication of two elements. For ordinary skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0088] The preferred embodiments of the present application have been described in detail, but the present application is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present application.

Claims

1. A method of closed circuit fluorine chemical vapor deposition of high purity materials, characterized in that, The method comprises the following steps: S1, the crude purity of the material is put into the reactor, and the purity of the material to be purified is selected to be 99%-99.99%; S2, under the condition of heating, fluorine gas reacts with the purified material to generate binary fluoride; S3, the binary fluoride is purified and separated, and the target material containing fluorine compound is separated out; S4, under the condition of heating, hydrogen gas reacts with the binary fluoride to reduce the purified material; S5, the purity of the purified material is detected, and if it meets the standard, the product meets the standard, otherwise, it is repeated in the S2 process; S6, the hydrogen fluoride generated by the hydrogen reduction of the binary fluoride in S4 is purified; S7, the purified hydrogen fluoride in S6 is electrolyzed to prepare high-purity hydrogen gas and high-purity fluorine gas; The preparation device applied to the feeding in S1 comprises a reaction kettle (1), a discharge valve (2) is arranged at the bottom of the reaction kettle (1), a feed bin (3) is arranged above the reaction kettle (1), and a sealing cover (4) is connected to the top of the feed bin (3); Both sides of the bottom of the feed bin (3) are fixedly connected with baffles (5), the two baffles (5) are fixed with a base (6), the base (6) is fixedly connected with the top of the reaction kettle (1), the bottom of the feed bin (3) is communicated with the feeding inlet of the reaction kettle (1) through a feeding box (8), a quantitative feeding assembly (9) is arranged in the feeding box (8), the bottom end of the quantitative feeding assembly (9) is fixed with the base (6), both sides of the quantitative feeding assembly (9) are respectively connected with knocking assemblies (11), the knocking assemblies (11) are overlapped with the outer wall of the baffle (5), and the side, away from the baffle (5), of the knocking assembly (11) is fixedly connected with a supporting assembly (12), and the bottom of the supporting assembly (12) is fixedly connected with the base (6); The quantitative feeding assembly (9) comprises a rotating roller (901), four grooves (903) are arranged on the outer wall of the rotating roller (901), the included angle between the four grooves (903) is 90 degrees, a connecting shaft (902) is arranged in the middle of the rotating roller (901), both ends of the connecting shaft (902) are fixedly connected with rotating discs (906), two protrusions are arranged outside the rotating disc (906), one side of the protrusion is designed to be inclined, the other side of the protrusion is designed to be perpendicular, one end of the connecting shaft (902) is fixedly connected with the output shaft of a motor (904), a motor base (905) is arranged outside the motor (904), and the motor base (905) is fixedly connected with the base (6); A group of material blocking plates (10) are arranged on both sides in the feeding box (8), the number of each group of material blocking plates (10) is two, the opposite two material blocking plates (10) are designed to be inversely V-shaped, the knocking assembly (11) comprises a knocking plate (111), the inner side of the knocking plate (111) is overlapped with the outer wall of the baffle (5), two connecting rods (113) are fixedly connected with the side, close to the feed bin (3), of the knocking plate (111), and one end of the connecting rod (113) is connected with a pulley (114); Both sides of the bottom of the knocking plate (111) are fixedly connected with sliding plates (112), the base (6) is provided with sliding rails (7) corresponding to the positions of the sliding plates (112), the sliding plates (112) are slidingly connected in the sliding rails (7), and the sliding plates (112) and the sliding rails (7) are both T-shaped in design; The support assembly (12) comprises a side plate (121), the bottom of the side plate (121) is fixedly connected with the base (6), one side of the side plate (121) close to the stock bin (3) is fixedly connected with a spring (122), the spring (122) is fixedly connected with the outer wall of the knocking plate (111), and the inner wall of the baffle (5) is fixedly connected with the bottom of the stock bin (3) through three obliquely designed supporting rods (13).

2. The method of claim 1, wherein: In the S2, the purity of fluorine gas is 99.999%-99.99999%, and in the S4, the purity of hydrogen gas is 99.999%-99.99999%.

3. The method of claim 1, wherein: In the S7, fluorine gas is used for the fluorination reaction in the S2, and hydrogen gas is used for the hydrogen reduction reaction in the S4.

4. The method of claim 1, wherein the method is a closed cycle fluorine chemical vapor deposition of high purity material. The S2 and the S4 are step reactions of chemical vapor deposition: The S2 and the S4 are separately reacted in separate chambers, that is, the fluorination reaction is first carried out, and then the hydrogen reduction reaction is carried out. The S2 and the S4 are reacted in one chamber, the fluorination reaction is carried out in a reaction zone, and the hydrogen reduction is carried out in a deposition zone.

5. The method of claim 1, wherein: the method is a closed cycle fluorine chemical vapor deposition method of high purity materials. In the S1, the purified material is a refractory metal or a transition metal, containing W, Mo, Ir, Rh, Nb, Ta, As, Te, Sb or Se, and the detection method in the S5 comprises a GDMS or ICP-MS method.

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