Rhenium transportation and recovery system

Abstract

The invention provides a rhenium transportation and recovery system. The rhenium transportation and recovery system comprises a rhenium precursor steam transportation and metal rhenium condensation recovery device. A chassis liquid bath cavity is installed at the bottom of the reaction cavity, carrier gas carrying rhenium precursor steam enters the reaction cavity through the chassis liquid bath cavity through an inlet conveying pipeline and reaches the surface of a workpiece through a spraying hole pipeline, and the rhenium precursor steam not deposited on the workpiece enters a collecting hole pipe in the reaction cavity and reaches a tail gas pipeline through the chassis liquid bath cavity. The tail gas conveying pipeline is connected with the condensation recovery cavity through the pipeline liquid bath cavity; the rhenium precursor steam is condensed and recycled in the condensation recycling cavity, and the remaining carrier gas is exhausted through the exhaust pipe. Through the designed base plate liquid bath cavity structure, heat preservation of the inlet conveying pipeline in the area where the heating belt cannot be wound is achieved, and meanwhile the rotation requirement of a workpiece in the reaction cavity is not affected. And the condensation recovery cavity realizes efficient recovery of the rhenium precursor through three-stage condensation.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical vapor deposition equipment, and in particular relates to a rhenium transport and recovery system. Background Art

[0002] Rhenium is a rare metal with an extremely high melting point, which is as high as 3180℃. Rhenium still has high mechanical properties at high temperatures, strong resistance to heat shock, and excellent corrosion and wear resistance. Due to its series of excellent properties, rhenium is one of the extremely important raw materials for the development of modern high-tech fields such as aerospace and electronics industry. It is widely used in missile propulsion systems, ultra-high temperature emitters and wear-resistant erosion coatings. Compared with other process methods, the metal rhenium film prepared by chemical vapor deposition has higher mechanical properties and density, and can prepare ultra-high purity metal rhenium film. Due to the technical characteristics of chemical vapor deposition, it can prepare film structures with precise dimensions and complex shapes, and the rhenium film layer is firmly bonded to the substrate and has good uniformity.

[0003] The currently commonly used metal rhenium chemical vapor deposition is based on the decomposition of rhenium chloride precursor vapor at high temperature. The difficulty in gas transportation of rhenium chloride precursor vapor is to ensure that condensation does not occur, that is, to ensure that there are no low-temperature locations in all pipelines. Once low-temperature condensation occurs at a certain location, the pipeline will be blocked due to rhenium accumulation. The conventional pipeline heating method uses heating tape winding and multi-point thermocouple arrangement. On the one hand, due to the poor contact of the heating tape winding process, local low-temperature condensation occurs. On the other hand, it is difficult to wrap the heating tape around some special parts. For example, the connection between the rhenium precursor pipeline and the reaction chamber is several centimeters long and cannot be wrapped with the heating tape. How to more stably and conveniently achieve the heating and high-temperature maintenance of the transportation pipeline in special parts is a difficult problem for rhenium precursor transportation.

[0004] Due to the high cost of rhenium metal, after rhenium is deposited on the workpiece, the remaining rhenium precursor vapor needs to be effectively recovered. It is necessary to design an effective heating device for the pipeline so that the rhenium precursor can be recovered. How to design a recovery system and stably transport the remaining rhenium precursor vapor to the recovery system is a key problem in reducing the cost of metal rhenium chemical vapor deposition. Summary of the invention

[0005] In order to solve the problems of the existing technology, the patent of this invention proposes a rhenium transportation and recovery system in view of the extremely high requirements of rhenium precursors for high-temperature pipeline transportation. It can reliably and evenly heat and insulate the key parts of the rhenium chloride vapor transportation process, reduce the risks of condensation and blockage, and greatly improve the long-term operation stability of the equipment.

[0006] The rhenium transport and recovery system provided by the present invention comprises a rhenium precursor vapor transport and metal rhenium condensation recovery device. A bottom plate liquid bath chamber (105) is installed at the bottom of a reaction chamber (100). A carrier gas carrying rhenium precursor vapor enters the reaction chamber (100) through an inlet transport pipe (101) outside the reaction chamber (100) and the bottom plate liquid bath chamber (105), passes through a spray hole pipe (107) and reaches the surface of a workpiece (109). The rhenium precursor vapor not deposited on the workpiece (109) enters a collection hole pipe (114) inside the reaction chamber (100), enters an exhaust gas transport pipe (119) through the bottom plate liquid bath chamber (105), and reaches a condensation recovery chamber (132) for recovery. The remaining carrier gas is discharged from an exhaust pipe.

[0007] The inlet transport pipeline (101) is connected to the chassis liquid bath chamber (105) through the inlet pipeline flange 1 (103), and is connected to the spray hole pipeline (107) through the inlet pipeline flange 2 (106); the exhaust gas transport pipeline (119) is connected to the chassis liquid bath chamber (105) through the outlet pipeline flange 1 (116), and is connected to the collection hole pipe (114) through the outlet pipeline flange 2 (115).

[0008] In addition, the chassis liquid bath chamber (105) includes a liquid bath chamber liquid inlet (104), a liquid bath chamber liquid outlet (117), and a rotating shaft fixing component (112). The outer shell of the chassis liquid bath chamber (105) and the rotating shaft fixing component (112) form an annular chamber. High-temperature liquid enters the annular chamber in the chassis liquid bath chamber (105) through the liquid bath chamber liquid inlet (104), flows through the outer walls of the inlet transport pipeline (101) and the exhaust gas transport pipeline (119), and flows out through the liquid bath chamber liquid outlet (117).

[0009] The rhenium transport and recovery system provided by the present invention further comprises a condensation recovery chamber (132), comprising a front recovery baffle (124), a rear recovery baffle 1 (126), a rear recovery baffle 2 (127) and a condensation recovery laminate (133). A front recovery baffle cold water pipe (125) is installed on the front recovery baffle (124), and a condensation recovery laminate cold water pipe 1 (128), a condensation recovery laminate cold water pipe 2 (129), a condensation recovery laminate cold water pipe 3 (130), and a condensation recovery laminate cold water pipe 4 (131) are installed on the condensation recovery laminate (133). A condensation recovery chamber inlet heating belt (123) is installed at the end of the tail gas transport pipeline (119) near the inlet of the condensation recovery chamber (132).

[0010] Furthermore, an inlet pipeline heating belt (102) is installed on the inlet transport pipeline (101), an exhaust gas pipeline heating belt (118) is installed on the exhaust gas transport pipeline (119), and a pipeline liquid bath chamber (120) is installed at the turning point of the pipeline. High-temperature liquid enters the inner cavity of the pipeline liquid bath chamber (120) through the pipeline liquid bath chamber liquid inlet (121) and surrounds the outer periphery of the exhaust gas transport pipeline (119), and flows out through the pipeline liquid bath chamber liquid outlet (122).

[0011] Furthermore, a support platform rotating shaft (111) is installed at the center of the rotating shaft fixing component (112), and a support platform (110) and a workpiece (109) are installed on the supporting platform rotating shaft (111) in sequence.

[0012] Furthermore, a chlorine concentration detector (135) is provided between the reaction chamber (100) and the condensation recovery chamber (132), which can rapidly and continuously monitor the chlorine concentration of the tail gas transport pipeline (119) online, and can calculate the reaction amount of the precursor per unit time.

[0013] The advantages of the present invention are: through the designed chassis liquid bath chamber (105) structure, the heat preservation of the inlet transport pipeline (101) in the area where the heating belt cannot be wound is achieved, and at the same time, the rotation requirement of the workpiece (109) in the reaction chamber (100) is not affected. The condensation recovery chamber (132) realizes efficient recovery of rhenium precursor through three-stage condensation. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 It is a schematic diagram of the structure of the rhenium transport and recovery system of the present invention.

[0015] Figure 2 It is a bottom view schematic diagram of the reaction chamber liquid bath chassis of the present invention.

[0016] Figure 3 It is a top view schematic diagram of the condensation recovery device of the present invention.

[0017] Description of reference numerals: 100 reaction chamber, 101 inlet transport pipeline, 102 inlet pipeline heating belt, 103 inlet pipeline flange one, 104 liquid inlet of liquid bath chamber, 105 chassis liquid bath chamber, 106 inlet pipeline flange two, 107 spray hole pipeline, 108 rhenium precursor reaction chamber pipeline outlet hole, 109 workpiece, 110 support platform, 111 support platform rotating shaft, 112 rotating shaft fixing component, 113 rhenium precursor reaction chamber pipeline outlet hole, 114 collecting hole tube, 115 outlet pipeline flange two, 116 outlet pipeline flange one, 117 liquid outlet of liquid bath chamber, 118 exhaust pipeline heating belt, 119 exhaust gas transport pipeline, 120 pipeline liquid bath chamber, 121 pipeline liquid bath chamber liquid inlet, 122 liquid outlet of pipeline liquid bath chamber, 123 heating belt of condensation recovery chamber inlet, 124 front recovery baffle, 125 front recovery baffle cold water pipe, 126 rear recovery baffle one, 127 rear recovery baffle two, 128 condensation recovery laminate cold water pipe one, 129 condensation recovery laminate cold water pipe two, 130 condensation recovery laminate cold water pipe three, 131 condensation recovery laminate cold water pipe four, 132 condensation recovery chamber, 133 condensation recovery laminate, 134 exhaust pipe, 135 chlorine gas concentration detector. Implementation

[0018] Example: Figure 1-3 As shown, the rhenium transport and recovery system provided by the present invention includes a rhenium precursor vapor transport and metal rhenium condensation recovery device. A bottom of the reaction chamber 100 is installed with a bottom plate liquid bath chamber 105, and the inlet transport pipeline 101 is connected to the bottom plate liquid bath chamber 105 through the inlet pipeline flange 103, and is connected to the spray hole pipeline 107 through the inlet pipeline flange 2 106; wherein the tail gas transport pipeline 119 is connected to the bottom plate liquid bath chamber 105 through the outlet pipeline flange 116, and is connected to the collection hole pipe 114 through the outlet pipeline flange 2 115.

[0019] The chassis liquid bath chamber 105 includes a liquid bath chamber liquid inlet 104, a liquid bath chamber liquid outlet 117, and a rotating shaft fixing component 112. The outer shell of the chassis liquid bath chamber 105 and the rotating shaft fixing component 112 form an annular chamber. High-temperature oil heated to 450°C enters the annular chamber in the chassis liquid bath chamber 105 through the liquid bath chamber liquid inlet 104, flows through the outer wall of the inlet delivery pipeline 101 and the exhaust gas delivery pipeline 119, and flows out through the liquid bath chamber liquid outlet 117. The high-temperature oil is circulated in the chassis night bath chamber 105 by a high-temperature oil pump.

[0020] The carrier gas carrying the rhenium precursor vapor enters the reaction chamber 100 through the inlet transport pipe 101 outside the reaction chamber 100 and the bottom plate liquid bath chamber 105, and reaches the surface of the workpiece 109 through the nozzle pipe 107. The rhenium precursor vapor not deposited on the workpiece 109 enters the collection hole pipe 114 inside the reaction chamber 100, enters the tail gas transport pipe 119 through the bottom plate liquid bath chamber 105, and reaches the condensation recovery chamber 132 for recovery, and the remaining carrier gas is discharged from the exhaust pipe. The system includes a condensation recovery chamber 132. The condensation recovery chamber 132 includes a front recovery baffle 124, a rear recovery baffle 1 126, a rear recovery baffle 2 127 and a condensation recovery stack 133. The front recovery baffle 124 is provided with a front recovery baffle cold water pipe 125, and the condensation recovery lamination 133 is provided with a condensation recovery lamination cold water pipe 1 128, a condensation recovery lamination cold water pipe 2 129, a condensation recovery lamination cold water pipe 3 130, and a condensation recovery lamination cold water pipe 4 131. The end of the tail gas transport pipeline 119 near the entrance of the condensation recovery chamber 132 is provided with a condensation recovery chamber entrance heating belt 123.

[0021] Preferably, an inlet pipeline heating belt 102 is installed on the inlet transport pipeline 101, and the heating and insulation temperature of the inlet pipeline heating belt 102 is set to 450°C. An exhaust pipeline heating belt 118 is installed on the exhaust gas transport pipeline 119, and the heating and insulation temperature of the exhaust pipeline heating belt 118 is set to 450°C, and a pipeline liquid bath cavity 120 is installed at the pipeline turning point. The high-temperature oil heated to 450°C enters the inner cavity of the pipeline liquid bath cavity 120 through the pipeline liquid bath cavity liquid inlet 121 and surrounds the outer periphery of the exhaust gas transport pipeline 119, and flows out through the pipeline liquid bath cavity liquid outlet 122. The high-temperature oil is circulated in the pipeline liquid bath cavity 120 by a high-temperature oil pump.

[0022] Preferably, a support platform rotating shaft 111 is installed at the center of the rotating shaft fixing component 112 , and a support platform 110 and a workpiece 109 are installed on the support platform rotating shaft 111 in sequence.

[0023] Preferably, a chlorine concentration detector 135 is provided between the cavity 100 and the condensation recovery cavity 132, which can quickly and continuously monitor the chlorine concentration of the tail gas transport pipeline 119 online, and can calculate the reaction amount of the precursor per unit time.

[0024] The above embodiments mainly illustrate the rhenium transport and recovery method proposed by the present invention. Although only one embodiment of the present invention is described, the present invention can be implemented in many other ways without departing from its purpose and scope. Therefore, it should be understood that the above embodiments are not limited to the present invention, and all modifications, substitutions, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A rhenium transport and recovery system, characterized in that: A bottom plate liquid bath chamber (105) is installed at the bottom of the reaction chamber (100). The carrier gas carrying rhenium precursor vapor enters the reaction chamber (100) through the inlet transport pipe (101) outside the reaction chamber (100) and the bottom plate liquid bath chamber (105), and reaches the surface of the workpiece (109) through the spray hole pipe (107). The rhenium precursor vapor not deposited on the workpiece (109) enters the collection hole pipe (114) inside the reaction chamber (100), and enters the tail gas transport pipe (119) through the bottom plate liquid bath chamber (105). ), and reaches the condensation recovery chamber (132) for recovery, and the remaining carrier gas is discharged from the exhaust pipe (134). The inlet transport pipeline (101) is connected to the chassis liquid bath chamber (105) through the inlet pipeline flange 1 (103), and is connected to the spray hole pipeline (107) through the inlet pipeline flange 2 (106); the exhaust gas transport pipeline (119) is connected to the chassis liquid bath chamber (105) through the outlet pipeline flange 1 (116), and is connected to the collection hole pipe (114) through the outlet pipeline flange 2 (115). The chassis liquid bath chamber (105) comprises a liquid bath chamber liquid inlet (104), a liquid bath chamber liquid outlet (117), and a rotating shaft fixing component (112). The outer shell of the chassis liquid bath chamber (105) and the rotating shaft fixing component (112) form an annular chamber. High-temperature liquid enters the annular chamber in the chassis liquid bath chamber (105) through the liquid bath chamber liquid inlet (104), flows through the outer walls of the inlet transport pipeline (101) and the exhaust gas transport pipeline (119), and flows out through the liquid bath chamber liquid outlet (117). The condensation recovery chamber (132) comprises a front recovery baffle (124), a rear recovery baffle one (126), a rear recovery baffle two (127) and a condensation recovery stack (133); a front recovery baffle cold water pipe (125) is installed on the front recovery baffle (124); a condensation recovery stack cold water pipe one (128), a condensation recovery stack cold water pipe two (129), a condensation recovery stack cold water pipe three (130) and a condensation recovery stack cold water pipe four (131) are installed on the condensation recovery stack (133); and a condensation recovery chamber inlet heating belt (123) is installed at the end of the exhaust gas transport pipeline (119) near the inlet of the condensation recovery chamber (132).

2. A rhenium transport and recovery system according to claim 1, characterized in that: The inlet transport pipeline (101) is provided with an inlet pipeline heating belt (102), the exhaust gas transport pipeline (119) is provided with an exhaust gas pipeline heating belt (118), and a pipeline liquid bath chamber (120) is provided at the turning point of the pipeline. High-temperature liquid enters the inner cavity of the pipeline liquid bath chamber (120) through the pipeline liquid bath chamber liquid inlet (121) and surrounds the outer periphery of the exhaust gas transport pipeline (119), and flows out through the pipeline liquid bath chamber liquid outlet (122).

3. A rhenium transport and recovery system according to claim 1, characterized in that: A support platform rotating shaft (111) is installed at the center of the rotating shaft fixing component (112), and a support platform (110) and a workpiece (109) are installed in sequence on the support platform rotating shaft (111).

4. A rhenium transport and recovery system according to claim 1, characterized in that: A chlorine concentration detector (135) is provided between the reaction chamber (100) and the condensation recovery chamber (132), which can rapidly and continuously monitor the chlorine concentration of the tail gas transport pipeline (119) online, and can calculate the reaction amount of the precursor per unit time.

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