Device for rapidly recycling precursor impregnation liquid and using method

Abstract

The invention discloses a device for rapidly recycling precursor impregnation liquid and a using method, and belongs to the technical field of precursor impregnation and pyrolysis processes. The device comprises a raw material chamber, an impregnation chamber and a raw material recovery chamber which are sequentially arranged from top to bottom, at least one steeping liquor container is arranged in the raw material chamber; a glass container is arranged in the impregnation chamber and used for containing a to-be-impregnated sample, and the impregnation chamber is connected with a vacuum pump; and at least one steeping liquor recovery container is arranged in the raw material recovery chamber. The device and the using method thereof are used for solving the technical problems of high cost of precursor impregnation liquid, difficulty in recycling the precursor impregnation liquid, low recycling efficiency, low impregnation efficiency and poor gradient modified composite material preparation effect in the existing PIP process.

Description

Technical Field

[0001] The present invention belongs to the technical field of precursor infiltration and pyrolysis processes, and particularly relates to a device and a use method for rapid recovery and recycling of a precursor impregnating solution. Background Art

[0002] Carbon-ceramic modified composites play an irreplaceable role in high-tech fields such as aerospace and national defense science and technology due to their excellent high-temperature resistance, high load-bearing capacity, and anti-ablative properties. The preparation of such materials largely depends on the precursor infiltration and pyrolysis process (PIP process). The PIP process is widely adopted because of its advantages such as simple material preparation process, convenient operation, ceramic phase precursor molecules can be designed as required, uniform distribution and high purity of ceramic phases, and the ability to achieve net shape forming of large-size and complex-shaped components.

[0003] In academic research, carbon-ceramic modified composites prepared by the PIP process have demonstrated excellent anti-ablative capabilities. For example, in the literature "Jiao X, He Q, Tan Q, et al. Ablation behavior of mullite modified C / C-SiC-HfC composites under oxyacetylene torch for single and cyclic ablations with two heat fluxes, (2023)", mullite modified C / C-HfC-SiC composites were prepared by the PIP technique, and it was found that this material could form a dense Hf-Si-Al-O multiphase layer to provide protection under low heat fluxes, while under high heat fluxes, stable HfO2 and HfSiO4 layers could effectively resist flame erosion. The literature "Li W, Lv J S, Li J T, et al. Superior ablation resistance of C / C-HfC-SiC composite sharp leading edges above 2500 °C prepared by precursor infiltration and pyrolysis (2025)" further verified the excellent anti-ablative performance of C / C-HfC-SiC sharp leading edge specimens prepared by the PIP technique at extremely high temperatures. These research results not only highlight the technical advantages of the PIP process but also provide a solid theoretical basis for the wide application of carbon-ceramic modified composites.

[0004] However, the PIP process faces numerous challenges in practical applications. The production process of the precursor impregnation solution is complex and costly, and there is no recycling procedure, resulting in waste. Key raw materials such as polycarbosilane and hafnium carbide precursors are expensive, making the cost of the entire preparation process high. In addition, as disclosed in a vacuum impregnation device and method for a silicon nitride composite material with the publication number CN 112194496 A provided by a Chinese invention, although the co-curing of the precursor impregnation solution and the specimen is achieved, a large amount of the precursor impregnation solution that has not penetrated into the specimen is wasted during this process, further exacerbating the cost problem. Currently, there is no effective solution for the rapid recovery and reuse of the precursor impregnation solution. The traditional pouring recovery method has the problem of splashing of the precursor impregnation solution, which not only easily causes direct contact between the skin and the precursor impregnation solution, increasing the risk of infection, but also poses a potential threat to human health after long-term exposure to such an environment, even when wearing intact protective facilities. At the same time, the precursor impregnation solution is prone to oxidation and failure when exposed to air for a long time, further reducing its utilization rate. The existing PIP process also has obvious deficiencies in terms of impregnation efficiency. Due to the premature intervention of the precursor impregnation solution, it is often difficult to ensure that there are no bubbles in the pores of the specimen to be impregnated during the vacuum pumping process, resulting in low impregnation efficiency and long impregnation time. This not only affects the production efficiency but also increases the energy consumption and cost. The existing PIP process is mainly applicable to the preparation of specimens for overall modification and has poor effects on the preparation of gradient-modified composite materials. In the area where the composite material undergoes low ablation, due to the introduction of excessive ultra-high temperature ceramics, not only the preparation cost is increased, resulting in waste of resources, but also the overall weight of the specimen is increased, reducing its performance in practical applications.

[0005] In summary, problems such as the high cost of the precursor impregnation solution in the existing PIP process, difficulties in recovering the precursor impregnation solution, low recovery and utilization efficiency, low impregnation efficiency, and poor preparation effects of gradient-modified composite materials need to be solved urgently. Summary of the Invention

[0006] In order to overcome the above-mentioned shortcomings of the prior art, the purpose of the present invention is to provide a device and a usage method for the rapid recovery and recycling of the precursor impregnation solution, so as to solve the technical problems of the high cost of the precursor impregnation solution in the existing PIP process, difficulties in recovering the precursor impregnation solution, low recovery and utilization efficiency, low impregnation efficiency, and poor preparation effects of gradient-modified composite materials.

[0007] To achieve the above purpose, the present invention adopts the following technical solutions: The present invention provides a device for rapidly recycling a precursor impregnating solution, which comprises a raw material chamber, an impregnation chamber, and a raw material recovery chamber arranged in sequence from top to bottom; at least one impregnating solution container is arranged in the raw material chamber; a glass container is arranged in the impregnation chamber, and the glass container is used for containing a sample to be impregnated. The impregnation chamber is connected to a vacuum pump; at least one impregnating solution recovery container is arranged in the raw material recovery chamber; the impregnating solution recovery container, the impregnating solution container, and the glass container are all connected to an air pipeline, and an air control valve is respectively arranged at the connection; the impregnating solution container is connected to the glass container through a first pipeline, the glass container is connected to the impregnating solution recovery container through a second pipeline, the impregnating solution recovery container is connected to a fourth pipeline through a third pipeline, and the fourth pipeline is connected to the impregnating solution container; a control valve is respectively arranged on the first pipeline, the second pipeline, and the third pipeline, and an impregnating solution reuse oil pump is arranged on the fourth pipeline.

[0008] In one embodiment, it further comprises an impregnating solution replenishing container, and the impregnating solution replenishing container is connected to the fourth pipeline through a fifth pipeline, and a control valve is arranged on the fifth pipeline.

[0009] In one embodiment, a storage rack is arranged below the glass container.

[0010] In one embodiment, a profiled porous glass tooling matching the sample to be impregnated is arranged in the glass container.

[0011] In one embodiment, the raw material chamber, the impregnation chamber, and the raw material recovery chamber are all sealed chambers. On the same side surface of the raw material chamber, the impregnation chamber, and the raw material recovery chamber, a warehouse door is respectively opened, and a transparent observation window is opened on the warehouse door.

[0012] In one embodiment, the device for rapidly recycling the precursor impregnating solution further comprises a cleaning solvent recycling part, and the cleaning solvent recycling part comprises at least one cleaning solvent container, at least one cleaning solvent recovery container, and at least one cleaning solvent replenishing container; The cleaning solvent container is arranged in the raw material chamber, the cleaning solvent recovery container is arranged in the raw material recovery chamber, the cleaning solvent recovery container and the cleaning solvent container are both connected to the air pipeline, and an air control valve is respectively arranged at the connection; the cleaning solvent container is connected to the glass container through a sixth pipeline, a solvent branch is opened on the second pipeline, the solvent branch is connected to the glass container and the cleaning solvent recovery container, the cleaning solvent recovery container is connected to a ninth pipeline through a seventh pipeline, the cleaning solvent replenishing container is connected to the ninth pipeline through an eighth pipeline, the ninth pipeline is connected to the cleaning solvent container, a control valve is respectively arranged on the sixth pipeline, the solvent branch, the seventh pipeline, and the eighth pipeline, and a cleaning solvent reuse oil pump is arranged on the ninth pipeline.

[0013] The present invention also provides a method for using the device for rapidly recycling the precursor impregnating solution, which comprises the following steps: S1: Open the air control valve at the connection between the impregnating solution container and the air pipeline, and turn on the vacuum pump until the impregnating chamber is in a near-vacuum state; open the control valve on the first pipeline, and deliver the precursor impregnating solution into the glass container. After the sample to be impregnated is submerged, close all the above-mentioned opened valves, and maintain the impregnation for a certain period of time, then turn off the vacuum pump; S2: Open the air control valves at the connections between the impregnating chamber and the impregnating solution recovery container and the air pipeline respectively, open the control valve on the second pipeline, deliver the precursor impregnating solution to the impregnating solution recovery container, and close all the above-mentioned opened valves; S3: Open the air control valve at the connection between the impregnating solution container and the air pipeline and the control valve on the third pipeline, and start the impregnating solution recycling oil pump to deliver the precursor impregnating solution in the impregnating solution recovery container to the impregnating solution container.

[0014] In one embodiment, the device for rapid recovery and recycling of the precursor impregnating solution further includes an impregnating solution supplement container, a fifth pipeline, and a control valve on the fifth pipeline; It further includes a supplement step, and the supplement step is as follows: If the precursor impregnating solution in the impregnating solution recovery container is insufficient, open the control valve on the fifth pipeline to supplement and deliver the precursor impregnating solution in the impregnating solution supplement container.

[0015] In one embodiment, it further includes a usage method of gradient impregnation, including the following steps: S101: Open the air control valve at the connection between the impregnating solution container and the air pipeline, and turn on the vacuum pump until the impregnating chamber is in a near-vacuum state; open the control valve on the first pipeline, and deliver the precursor impregnating solution into the glass container. After the sample to be impregnated is submerged, close all the above-mentioned opened valves; S102: Open the air control valve at the connection between the impregnating solution recovery container and the air pipeline and the control valve on the second pipeline at regular intervals, and wait until a certain amount of the precursor impregnating solution is recovered, then close all the above-mentioned opened valves; S103: Repeat S102 until all the precursor impregnating solution in the impregnating chamber is completely recovered, turn off the vacuum pump, open the air control valve at the connection between the impregnating chamber and the air pipeline until the impregnating chamber is at normal pressure, and then close it; S104: Open the air control valve at the connection between the impregnating solution container and the air pipeline and the control valve on the third pipeline, and start the impregnating solution recycling oil pump to deliver the precursor impregnating solution in the impregnating solution recovery container to the impregnating solution container; if the precursor impregnating solution in the impregnating solution recovery container is insufficient, open the control valve on the fourth pipeline to supplement and deliver the precursor impregnating solution in the impregnating solution supplement container.

[0016] In one embodiment, a profiling porous glass tooling matching the shaped sample to be impregnated is further arranged in the glass container; It also includes a method for using a gradient-impregnated special-shaped sample, which comprises the following steps: S111: Place the special-shaped sample to be impregnated into a profiled porous glass tooling to fix its position, and then place it into a glass container; S112: Open the air control valve at the connection between the impregnating solution container and the air pipeline, and turn on the vacuum pump until the impregnation chamber is in a near-vacuum state; open the control valve on the first pipeline, and the precursor impregnating solution is transported into the glass container. After the special-shaped sample to be impregnated is submerged, close all the above-mentioned opened valves; S113: Open the air control valve at the connection between the impregnating solution recovery container and the air pipeline and the control valve on the second pipeline at regular intervals. Wait until a certain amount of impregnating solution is recovered, and then close all the above-mentioned opened valves; S114: Repeat S112 until the precursor impregnating solution in the impregnation chamber is completely recovered. Turn off the vacuum pump, and open the air control valve at the connection between the impregnation chamber and the air pipeline until the impregnation chamber returns to normal pressure, and then close it; S115: Open the air control valve at the connection between the impregnating solution container and the air pipeline and the control valve on the third pipeline, and start the impregnating solution reuse oil pump to transport the precursor impregnating solution in the impregnating solution recovery container to the impregnating solution container; if the precursor impregnating solution in the impregnating solution recovery container is insufficient, open the control valve on the fourth pipeline to supplement and transport the precursor impregnating solution in the impregnating solution supplement container.

[0017] In one embodiment, it also includes a cleaning step carried out after S2. The cleaning step is as follows: S01: Open the air control valve at the connection between the cleaning solvent container and the air pipeline, and turn on the vacuum pump until the impregnation chamber is in a slightly negative pressure state; open the control valve on the sixth pipeline, and the cleaning solvent is transported into the glass container. After the sample to be impregnated is submerged, close all the above-mentioned opened valves and maintain for a certain period of time to remove the precursor impregnating solution adhering to the surface of the sample to be impregnated; S02: Open the air control valves at the connections between the impregnation chamber and the cleaning solvent recovery container and the air pipeline respectively, and open the control valve on the solvent branch. The cleaning solvent is transported to the cleaning solvent recovery container, and then close all the above-mentioned opened valves; S03: Open the air control valve at the connection between the cleaning solvent container and the air pipeline and the control valve on the seventh pipeline, and start the cleaning solvent reuse oil pump to transport the cleaning solvent in the cleaning solvent recovery container to the cleaning solvent container; if the cleaning solvent in the cleaning solvent recovery container is insufficient, open the control valve on the eighth pipeline to supplement and transport the cleaning solvent in the cleaning solvent supplement container.

[0018] Compared with the prior art, the present invention has the following beneficial effects: The present invention provides a device for rapidly recovering and recycling a precursor impregnating solution. Through the connection of an impregnating solution container, an impregnating solution recovery container and corresponding pipelines, and the setting of control valves, the impregnated precursor impregnating solution is recovered and reused, which can effectively reduce the preparation cost of the PIP process, achieve the rapid recovery of the precursor impregnating solution after impregnation, and avoid the waste and splashing problems caused by the traditional pouring recovery method. The impregnating solution container, the impregnating solution recovery container and their pipelines ensure the accurate recovery and reuse of the impregnating solution, re-transport the recovered impregnating solution to the impregnating solution container, realize the recycling of the impregnating solution, reduce the cost, and reduce the loss of the impregnating solution during the recovery process. The device also utilizes the height difference between the impregnation chamber and the recovery chamber, and the self-gravity of the liquid helps to completely recover the impregnating solution, avoiding the problem that the impregnating solution is oxidized and invalid due to exposure to the air. The vacuum pump and the impregnation chamber in the device can discharge the air bubbles in the internal pores of the specimen to be impregnated before the impregnation process, prompting the impregnating solution to quickly penetrate into the internal pores of the specimen to be impregnated, and improving the impregnation efficiency.

[0019] Furthermore, to fully ensure the life and health of scientific research and production personnel, reduce the preparation cost of the PIP process, and realize the rational recycling of resources, etc., the outside of the device communicates with the outdoor environment, and each compartment door is closed. During the impregnation and recovery processes, there is basically no excessive contact with the precursor impregnating solution and the organic cleaning solvent, which can effectively reduce the risk of scientific research and production personnel inhaling and contacting the precursor impregnating solution and the organic cleaning solvent, and provide protection for the life and health of personnel.

[0020] The present invention also provides a method for using a device for rapidly recovering and recycling a precursor impregnating solution. This method is highly integrated and easy to operate. Since the impregnation chamber is in a vacuum state in advance, the precursor impregnating solution quickly enters the internal pores of the specimen to be impregnated, with high impregnation efficiency, greatly improving the impregnation cycle and reducing the production cost. Additionally, by controlling the impregnation duration at different positions in the thickness direction of the specimen to be impregnated, the ceramic gradient of the specimen to be impregnated can be effectively achieved, realizing the preparation of modified composite materials with low cost and lightweight.

[0021] Furthermore, by controlling the impregnation duration at different positions in the thickness direction of the specimen to be impregnated, the ceramic gradient of the specimen to be impregnated can be effectively achieved. Also, by placing the special-shaped specimen to be impregnated in a profiled porous tooling, the ceramic gradient of the special-shaped specimen to be impregnated can be achieved (for example, if the sharp leading edge is inverted, a specimen with more ceramic at the head and less at the tail can be prepared). Description of the Drawings

[0022] Figure 1 It is an external schematic diagram of the device for rapidly recovering and recycling the precursor impregnating solution; Figure 2 It is a connection schematic diagram of the impregnating solution recovery and utilization part of the device for rapidly recovering and recycling the precursor impregnating solution; Figure 3 Schematic connection diagram of the impregnating solution recycling part and the cleaning solvent recycling part of the device for rapid recycling of the precursor impregnating solution; Figure 4 Graph showing the change of the density of the specimens in the examples and comparative examples with the impregnation cycle (each cycle of impregnation and curing three times followed by heat treatment at 1500 - 1700 °C is recorded as one impregnation cycle); Figure 5 XRD pattern of the C / C-ZrC-SiC composite material prepared in Example 1; Figure 6 Scanning electron micrograph of the C / C-ZrC-SiC composite material prepared in Example 1; Figure 7 Scanning electron micrograph of the C / C-ZrC-SiC composite material prepared in Example 2; Figure 8 Scanning electron micrograph of the C / C-ZrC-SiC composite material prepared in Example 3.

[0023] Among them, 1 - raw material chamber; 2 - impregnation chamber; 3 - raw material recovery chamber; 4 - electric control integrated device; 5 - cleaning solvent recovery container; 51 - cleaning solvent recovery control valve; 52 - cleaning solvent recovery air control valve; 53 - cleaning solvent reuse control valve; 6 - impregnating solution recovery container; 61 - impregnating solution recovery control valve; 62 - impregnating solution recovery air control valve; 63 - impregnating solution reuse control valve; 7 - impregnating solution container; 71 - impregnating solution control valve; 72 - impregnating solution air control valve; 8 - cleaning solvent container; 81 - cleaning solvent control valve; 82 - cleaning solvent air control valve; 9 - impregnation chamber air control valve; 10 - vacuum pump; 11 - specimen to be impregnated; 12 - glass container; 13 - storage rack; 14 - cleaning solvent supplementary container; 141 - cleaning solvent supplementary container control valve; 15 - impregnating solution supplementary container; 151 - impregnating solution supplementary control valve; 16 - cleaning solvent reuse oil pump; 17 - impregnating solution reuse oil pump. Detailed implementation manners

[0024] In order to enable those skilled in the art to better understand the solution of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts shall fall within the protection scope of the present invention.

[0025] It should be noted that the terms "first", "second", etc. in the specification, claims and the above-mentioned drawings of the present invention are used to distinguish similar objects, and do not necessarily describe a specific order or sequence. It should be understood that the data used in this way can be interchanged under appropriate circumstances, so that the embodiments of the present invention described here can be implemented in an order other than those illustrated or described here. In addition, the terms "comprising" and "having" and any variations thereof are intended to cover non-exclusive inclusion. For example, a process, method, system, product or device comprising a series of steps or units does not necessarily have to be limited to those steps or units clearly listed, but may include other steps or units not clearly listed or inherent to these processes, methods, products or devices.

[0026] The present invention will be further described in detail below with reference to the drawings: In view of the problems in the PIP process such as the high cost of the precursor impregnation solution, the difficulty in recovering the precursor impregnation solution, the low recovery efficiency, the low impregnation efficiency, and the poor preparation effect of the gradient modified composite material, it is particularly important to develop a device and method for rapid recovery and recycling of the precursor impregnation solution that are efficient, environmentally friendly, and economical. The present invention provides a device and method for rapid recovery and recycling of the precursor impregnation solution, which can not only significantly reduce the preparation cost of the carbon-ceramic modified composite material, improve the production efficiency, but also reduce resource waste, reduce the risk to human life and health, and environmental pollution, providing a more solid support for the wide application of the carbon-ceramic modified composite material.

[0027] See Figure 1 and Figure 2 As shown in and, the present invention provides a device for rapid recovery and recycling of the precursor impregnation solution. The structure of the device includes a raw material chamber 1, an impregnation chamber 2, and a raw material recovery chamber 3 arranged in sequence from top to bottom. The raw material chamber 1, the impregnation chamber 2, and the raw material recovery chamber 3 are all sealed chambers. On the same side surface of the raw material chamber 1, the impregnation chamber 2, and the raw material recovery chamber 3, a hatch door is respectively opened, and a transparent observation window is opened on the hatch door.

[0028] See Figure 2 As shown in, at least one impregnation solution container 7 is provided in the raw material chamber 1. A glass container 12 is provided in the impregnation chamber 2, and this glass container 12 is used to hold the specimen to be impregnated 11, and the impregnation chamber 2 is connected to a vacuum pump 10. At least one impregnation solution recovery container 6 is provided in the raw material recovery chamber 3.

[0029] The impregnation solution recovery container 6, the impregnation solution container 7, and the glass container 12 are all connected to an air pipeline, and an air control valve is respectively provided at each connection, namely an impregnation solution recovery air control valve 62, an impregnation solution air control valve 72, and an impregnation chamber air control valve 9.

[0030] The impregnating solution container 7 is connected to the glass container 12 through the first pipeline, the glass container 12 is connected to the impregnating solution recovery container 6 through the second pipeline, the impregnating solution recovery container 6 is connected to the fourth pipeline through the third pipeline, and the fourth pipeline is connected to the impregnating solution container 7. A control valve is provided on each of the first pipeline, the second pipeline, and the third pipeline, which are respectively the impregnating solution control valve 71, the impregnating solution recovery control valve 61, and the impregnating solution reuse control valve 63. An impregnating solution reuse oil pump 17 is provided on the fourth pipeline.

[0031] The usage method of the device for rapid recovery and recycling of the precursor impregnating solution includes the following steps: S1: Open the impregnating solution air control valve 72, turn on the vacuum pump 10 until the impregnation chamber 2 is in a near-vacuum state; open the impregnating solution control valve 71 on the first pipeline, and the precursor impregnating solution is transported into the glass container 12. After the sample to be impregnated 11 is submerged, close the above-mentioned impregnating solution control valve 71 and impregnating solution air control valve 72 in sequence, and maintain the impregnation for a certain time and then turn off the vacuum pump 10; S2: Open the impregnation chamber air control valve 9 and the impregnating solution recovery air control valve 62 respectively, open the impregnating solution recovery control valve 61 on the second pipeline, and the precursor impregnating solution is transported to the impregnating solution recovery container 6, and then close the above-mentioned impregnation chamber air control valve 9, impregnating solution recovery air control valve 62, and impregnating solution recovery control valve 61; S3: Open the impregnating solution air control valve 72 and the impregnating solution reuse control valve 63 on the third pipeline, and start the impregnating solution reuse oil pump 17 to transport the precursor impregnating solution in the impregnating solution recovery container 6 to the impregnating solution container 7.

[0032] Furthermore, the impregnating solution container 7 is connected to the impregnating solution recovery container 6 and the impregnating solution replenishing container 15; specifically, the device further includes an impregnating solution replenishing container 15, and the impregnating solution replenishing container 15 is connected to the fourth pipeline through the fifth pipeline. A control valve is provided on the fifth pipeline, and this control valve is the impregnating solution replenishing control valve 151.

[0033] Based on the above usage method, there is further a supplementary step, and the supplementary step is as follows: If the precursor impregnating solution in the impregnating solution recovery container 6 is insufficient, open the impregnating solution replenishing control valve 151 on the fifth pipeline to supplement and transport the precursor impregnating solution in the impregnating solution replenishing container 15.

[0034] Furthermore, a storage rack 13 is provided below the glass container 12; a profiling porous glass tooling matching the sample to be impregnated 11 is provided in the glass container 12.

[0035] Further, after S1, the impregnation duration at different positions in the thickness direction of the specimen to be impregnated 11 is regulated by controlling the impregnation liquid recovery control valve 61. By making the impregnation durations at different positions different, gradient modified composite materials can be prepared.

[0036] Inserting a profiled porous glass tooling in S1 can be used to prepare profiled composite materials with gradient modification, such as profiled specimens with sharp leading edges, isothermal flow spherical column specimens and other profiled specimens for which it is difficult to control the specimen stability.

[0037] Further, on the basis of the above usage method, there is also a usage method for gradient impregnation, including the following steps: S101: Open the air control valve at the connection between the impregnation liquid container 7 and the air pipeline, and open the vacuum pump 10 until the impregnation chamber 2 is in a near-vacuum state; open the control valve on the first pipeline, and convey the precursor impregnation liquid into the glass container 12. After the precursor impregnation liquid submerges the specimen to be impregnated 11, close all the above opened valves. S102: Open the air control valve at the connection between the impregnation liquid recovery container 6 and the air pipeline and the control valve on the second pipeline at regular intervals. After a certain amount of the precursor impregnation liquid is recovered, close all the above opened valves. S103: Repeat S102 until the precursor impregnation liquid in the impregnation chamber 2 is completely recovered. Close the vacuum pump 10, and open the air control valve at the connection between the impregnation chamber 2 and the air pipeline until the impregnation chamber 2 returns to normal pressure and then close it. S104: Open the air control valve at the connection between the impregnation liquid container 7 and the air pipeline and the control valve on the third pipeline, and start the impregnation liquid reuse oil pump 17 to convey the precursor impregnation liquid in the impregnation liquid recovery container 6 to the impregnation liquid container 7; if the precursor impregnation liquid in the impregnation liquid recovery container 6 is insufficient, open the control valve on the fourth pipeline to supplement and convey the precursor impregnation liquid in the impregnation liquid supplement container 15.

[0038] Further, a profiled porous glass tooling matching the specimen to be impregnated 11 is also arranged in the glass container 12. On the basis of the above usage method, there is also a usage method for gradient impregnation of profiled parts, including the following steps: S111: Place the profiled specimen to be impregnated into the profiled porous glass tooling to fix its position, and then place it into the glass container 12. S112: Open the air control valve at the connection between the impregnation liquid container 7 and the air pipeline, and open the vacuum pump 10 until the impregnation chamber 2 is in a near-vacuum state; open the control valve on the first pipeline, and convey the precursor impregnation liquid into the glass container 12. After the precursor impregnation liquid submerges the specimen to be impregnated 11, close all the above opened valves. S113: Open the air control valve at the connection between the impregnation liquid recovery container 6 and the air pipeline and the control valve on the second pipeline every once in a while, and wait until a certain amount of impregnation liquid is recovered, then close all the opened valves mentioned above; S114: Repeat S112 until all the precursor impregnation liquid in the impregnation chamber 2 is completely recovered. Then close the vacuum pump 10, open the air control valve at the connection between the impregnation chamber 2 and the air pipeline until the impregnation chamber 2 is at normal pressure, and then close it; S115: Open the air control valve at the connection between the impregnation liquid container 7 and the air pipeline and the control valve on the third pipeline, and start the impregnation liquid reuse oil pump 17 to transport the precursor impregnation liquid in the impregnation liquid recovery container 6 to the impregnation liquid container 7; If the precursor impregnation liquid in the impregnation liquid recovery container 6 is insufficient, open the control valve on the fourth pipeline to supplement and transport the precursor impregnation liquid in the impregnation liquid supplement container 15.

[0039] Further, referring to Figure 3 , the device for rapid recovery and recycling of the precursor impregnation liquid further includes a cleaning solvent recovery and utilization part, and the cleaning solvent recovery and utilization part includes at least one cleaning solvent container 8, at least one cleaning solvent recovery container 5 and at least one cleaning solvent supplement container 14; The cleaning solvent container 8 is arranged in the raw material chamber 1, the cleaning solvent recovery container 5 is arranged in the raw material recovery chamber 3, both the cleaning solvent recovery container 5 and the cleaning solvent container 8 are connected to the air pipeline, and an air control valve is respectively arranged at the connection, which are the cleaning solvent recovery air control valve 52 and the cleaning solvent air control valve 82; The cleaning solvent container 8 is connected to the glass container 12 through the sixth pipeline, a solvent branch is opened on the second pipeline, and the solvent branch connects the glass container 12 and the cleaning solvent recovery container 5. The cleaning solvent container 8 is connected to the cleaning solvent recovery container 5 and the cleaning solvent supplement container 14. The cleaning solvent recovery container 5 is connected to the ninth pipeline through the seventh pipeline, and the cleaning solvent supplement container 14 is connected to the ninth pipeline through the eighth pipeline. The ninth pipeline is connected to the cleaning solvent container 8. A control valve is respectively arranged on the sixth pipeline, the solvent branch, the seventh pipeline and the eighth pipeline, which are the cleaning solvent control valve 81, the cleaning solvent recovery control valve 51, the cleaning solvent reuse control valve 53 and the cleaning solvent supplement container control valve 141. A cleaning solvent reuse oil pump 16 is arranged on the ninth pipeline.

[0040] Further, it also includes a cleaning step carried out after S1~S3, S101~S104, S111~S115. The cleaning step is as follows: S01: Open the cleaning solvent air control valve 82, and turn on the vacuum pump 10 until the impregnation chamber 2 is in a slightly negative pressure state; open the cleaning solvent control valve 81 on the sixth pipeline, and transport the cleaning solvent into the glass container 12. After the cleaning solvent submerges the sample 11 to be impregnated, close the above-mentioned cleaning solvent control valve 81, cleaning solvent air control valve 82, and vacuum pump 10 in sequence, and maintain for a certain period of time to remove the precursor impregnation liquid adhered to the surface of the sample 11 to be impregnated. S02: Open the impregnation chamber air control valve 9, and let air flow into the impregnation chamber 2 until it reaches atmospheric pressure. Open the cleaning solvent recovery air control valve 52 to ensure that the cleaning solvent recovery container 5 reaches atmospheric pressure. Open the cleaning solvent recovery control valve 51 on the solvent branch, and transport the cleaning solvent to the cleaning solvent recovery container 5. Then close the above-mentioned impregnation chamber air control valve 9, cleaning solvent recovery control valve 51, and cleaning solvent recovery air control valve 52. S03: Open the cleaning solvent air control valve 82 and the cleaning solvent reuse control valve 53 on the seventh pipeline, and start the cleaning solvent reuse oil pump 16 to transport the cleaning solvent in the cleaning solvent recovery container 5 to the cleaning solvent container 8; if the cleaning solvent in the cleaning solvent recovery container 5 is insufficient, open the cleaning solvent supply container control valve 141 on the eighth pipeline to supplement and transport the cleaning solvent in the cleaning solvent supply container 14.

[0041] The present invention provides a device for rapid recovery and recycling of precursor impregnation liquid, which mainly includes a raw material chamber 1, an impregnation chamber 2, a raw material recovery chamber 3, and an electric control integrated device 4. The device is divided into a raw material chamber 1, an impregnation chamber 2, and a raw material recovery chamber 3 from top to bottom. Multiple solenoid valves are arranged inside the raw material chamber 1 and the raw material recovery chamber 3 to control the rapid recovery of precursor impregnation liquid or cleaning organic solvents.

[0042] Among them, the raw material chamber 1 contains an impregnating solution container 7 for holding the precursor impregnating solution, a solenoid valve for controlling the delivery of the precursor impregnating solution to the impregnating chamber 2, i.e., the impregnating solution control valve 71, and a solenoid valve for maintaining the normal pressure state of the impregnating solution container 7, i.e., the impregnating solution air control valve 72, a container for cleaning the organic cleaning solvent of the precursor impregnating solution, i.e., the cleaning solvent container 8, a solenoid valve for controlling the delivery of the organic solvent for cleaning the precursor impregnating solution to the impregnating chamber 2, i.e., the cleaning solvent control valve 81, and a solenoid valve for maintaining the normal pressure state of the cleaning solvent container 8, i.e., the cleaning solvent air control valve 82; the impregnating chamber 2 contains a glass container 12 for holding the specimen to be impregnated 11, and the glass container 12 is supported by a rack 13 below; the internal devices of the raw material recovery chamber 3 and the raw material chamber 1 are substantially the same, which are respectively an impregnating solution recovery container 6 and a cleaning solvent recovery container 5 for cleaning the organic solvent of the precursor impregnating solution. Among them, the impregnating solution recovery control valve 61 controls the delivery of the precursor impregnating solution in the impregnating chamber 2 to the impregnating solution recovery container 6, and the impregnating solution recovery air control valve 62 maintains the normal pressure state of the impregnating solution recovery container 6. The cleaning solvent recovery control valve 51 controls the delivery of the organic solvent for cleaning the precursor impregnating solution in the impregnating chamber 2 to the cleaning solvent recovery container 5, and the cleaning solvent recovery air control valve 52 maintains the normal pressure state of the cleaning solvent recovery container 5. An impregnating chamber air control valve 9 for exhausting the impregnating chamber 2 and a vacuum pump 10 for evacuating the impregnating chamber 2 are provided on the outside of the device. The electric control integration device 4 is used to control the solenoid valves, the cleaning solvent recovery control valve 51, the cleaning solvent recovery air control valve 52, the cleaning solvent reuse control valve 53, the impregnating solution recovery control valve 61, the impregnating solution recovery air control valve 62, the impregnating solution reuse control valve 63, the impregnating solution control valve 71, the impregnating solution air control valve 72, the cleaning solvent control valve 81, the cleaning solvent air control valve 82, the impregnating chamber air control valve 9, the vacuum pump 10, the cleaning solvent replenishing container control valve 141, the impregnating solution replenishing control valve 151, the cleaning solvent reuse oil pump 16, the impregnating solution reuse oil pump 17, as well as the on / off and the degree of on / off of these valves. The pipeline connection method is as Figure 2 and Figure 3 shown.

[0043] The electric control integration device 4 is respectively connected to all the solenoid valves and pumps; the electric control integration device 4 can select the PLC operating system.

[0044] According to factors such as the experimental environment and cost, the solenoid valves can be replaced by ordinary valves, or the existing vacuum impregnation box can be improved to this device.

[0045] This device can be further improved. For example, the container bottles in the raw material recovery area can be directly sent back to the raw material area through a suction filter pump, realizing the rapid recycling of the solution, and the factory effect is obvious.

[0046] On the other hand, the present invention provides a method of using a device for rapid recovery and recycling of a precursor impregnating solution. The specific steps are as follows: Step 1: Prepare the sample 11 to be impregnated, the required solution, connect the pipelines, and close the doors of each area bin.

[0047] Step 2: Open the impregnating solution air control valve 72 to ensure that the impregnating solution container 7 is at normal pressure, and open the vacuum pump 10 until the impregnation chamber 2 is in a near-vacuum state; Step 3: Open the impregnating solution control valve 71 to control the slow delivery of the precursor impregnating solution into the glass container 12. After covering the sample 11 to be impregnated, close the impregnating solution control valve 71 and the impregnating solution air control valve 72 in sequence, and maintain the impregnation for a certain time and then close the vacuum pump 10; Step 4: Open the impregnation chamber air control valve 9, let air flow into the impregnation chamber 2 until it is at normal pressure, open the impregnating solution recovery air control valve 62 to ensure that the impregnating solution recovery container 6 is at normal pressure, open the impregnating solution recovery control valve 61, and use the self-gravity of the liquid to make the precursor impregnating solution flow into the impregnating solution recovery container 6; Step 5: After all the precursor impregnating solution is delivered to the impregnating solution recovery container 6, close the impregnation chamber air control valve 9, the impregnating solution recovery air control valve 62, and the impregnating solution recovery control valve 61; Step 6: Open the cleaning solvent air control valve 82 to ensure that the cleaning solvent container 8 is at normal pressure, and open the vacuum pump 10 until the impregnation chamber 2 is in a slightly negative pressure state; Step 7: Open the cleaning solvent control valve 81 to control the slow delivery of the cleaning solvent into the glass container 12. After covering the sample 11 to be impregnated, close the cleaning solvent control valve 81, the cleaning solvent air control valve 82, and the vacuum pump 10 in sequence, and maintain for ~1 min to fully remove the precursor impregnating solution adhered to the surface of the sample 11 to be impregnated and avoid blocking the pores of the impregnated sample due to the adhered precursor impregnating solution; Step 8: Open the impregnation chamber air control valve 9, let air flow into the impregnation chamber 2 until it is at normal pressure, open the cleaning solvent recovery air control valve 52 to ensure that the cleaning solvent recovery container is at normal pressure, open the cleaning solvent recovery control valve 51, and use the self-gravity of the liquid to make the cleaning solvent flow into the cleaning solvent recovery container 5; Step 9: After all the cleaning solvent is delivered to the cleaning solvent recovery container 5, close the impregnation chamber air control valve 9, the cleaning solvent recovery control valve 51, and the cleaning solvent recovery air control valve 52.

[0048] The precursor impregnating solution includes, but is not limited to, a mixed solution of one or more precursors such as polycarbosilane, zirconium carbide precursor, hafnium carbide precursor, etc. and an organic solvent xylene, or other solutions that can be used for impregnation. The organic solvents used for cleaning the precursor impregnating solution include, but are not limited to, xylene, etc.

[0049] The sample 11 to be impregnated can be all materials applicable to the precursor impregnation and pyrolysis process, such as low-density C / C composites, low-density C / SiC composites, low-density SiC / SiC composites, etc.

[0050] According to the different precursor impregnation solutions required for the sample, multiple corresponding container bottles can be arranged in the raw material area and the raw material recycling area to quickly replace the precursor impregnation solution.

[0051] In one implementation process, after the container solution in the raw material recycling area is full, the containers in the raw material area and the raw material recycling area can be exchanged and reused.

[0052] The following is further described in conjunction with specific embodiments: Example 1: Step 1: Prepare the sample 11 to be impregnated (~1.2 g / cm 3 C / C composite), the required solution (the precursor impregnation solution is a mixed solution of zirconium carbide precursor and polycarbosilane, and the organic solvent is xylene), connect the pipelines, and close the doors of each area.

[0053] Step 2: Open the impregnating liquid air control valve 72 to ensure that the impregnating liquid container 7 is at normal pressure, and open the vacuum pump 10 to make the impregnation chamber 2 in a near-vacuum state; Step 3: Open the impregnating liquid control valve 71 to control the slow delivery of the precursor impregnating liquid into the glass container 12. After covering the sample 11 to be impregnated, close the impregnating liquid control valve 71 and the impregnating liquid air control valve 72 in sequence, and maintain the impregnation for 30 min and then close the vacuum pump 10; Step 4: Open the impregnation chamber air control valve 9 to allow air to flow into the impregnation chamber 2 to normal pressure. Open the impregnating liquid recovery air control valve 62 to ensure that the impregnating liquid recovery container 6 is at normal pressure. Open the impregnating liquid recovery control valve 61, and use the self-gravity of the liquid to make the precursor impregnation solution flow into the impregnating liquid recovery container 6; Step 5: After all the precursor impregnating liquid is delivered to the impregnating liquid recovery container 6, close the impregnation chamber air control valve 9, the impregnating liquid recovery air control valve 62, and the impregnating liquid recovery control valve 61; Step 6: Open the cleaning solvent air control valve 82 to ensure that the cleaning solvent container 8 is at normal pressure, and open the vacuum pump 10 to make the impregnation chamber 2 in a slightly negative pressure state; Step 7: Open the cleaning solvent control valve 81 to control the slow delivery of the cleaning solvent into the glass container 12. After covering the sample 11 to be impregnated, close the cleaning solvent control valve 81, the cleaning solvent air control valve 82, and the vacuum pump 10 in sequence, and maintain for ~1 min to fully remove the precursor impregnating liquid adhered to the surface of the impregnated sample and avoid the blocked pores of the impregnated sample caused by the adhered precursor impregnating liquid; Step 8: Open the air control valve 9 of the impregnation chamber, allow air to flow into the impregnation chamber 2 until it reaches atmospheric pressure. Open the air control valve 52 for cleaning solvent recovery to ensure that the cleaning solvent recovery container 5 is at atmospheric pressure. Open the cleaning solvent recovery control valve 51, and use the self-gravity of the liquid to transfer the cleaning solvent to the cleaning solvent recovery container 5; Step 9: After all the cleaning organic solvents are transferred to the cleaning solvent recovery container 5, close the air control valve 9 of the impregnation chamber, the cleaning solvent recovery control valve 51, and the air control valve 52 for cleaning solvent recovery.

[0054] Repeat Steps 1 to 9, and perform curing (in an air environment, maintained at 60 °C for 12 h) three times. Conduct a high-temperature heat treatment at 1500 - 1700 °C. Consider this process as one impregnation cycle, and repeat several impregnation cycles until the preparation of the C / C-ZrC-SiC composite material is completed.

[0055] Example 2: Step 1: Prepare the sample to be impregnated 11 (~1.2 g / cm 3 C / C composite material), the required solutions (the precursor impregnation solution is a mixed solution of zirconium carbide precursor and polycarbosilane, and the organic solvent is xylene), connect the pipelines, and close the doors of each area compartment.

[0056] Step 2: Open the air control valve 72 of the impregnation liquid to ensure that the impregnation liquid container 7 is at atmospheric pressure. Open the vacuum pump 10 until the impregnation chamber 2 is in a near-vacuum state; Step 3: Open the impregnation liquid control valve 71 to control the slow transfer of the precursor impregnation liquid into the glass container 12. After covering the sample to be impregnated 11, close the impregnation liquid control valve 71 and the air control valve 72 of the impregnation liquid in sequence, and maintain impregnation for 45 min, then close the vacuum pump 10; Step 4: Open the air control valve 9 of the impregnation chamber, allow air to flow into the impregnation chamber 2 until it reaches atmospheric pressure. Open the air control valve 62 for impregnation liquid recovery to ensure that the impregnation liquid recovery container 6 is at atmospheric pressure. Open the impregnation liquid recovery control valve 61, and use the self-gravity of the liquid to transfer the precursor impregnation solution to the impregnation liquid recovery container 6; Step 5: After all the precursor impregnation liquid is transferred to the impregnation liquid recovery container 6, close the air control valve 9 of the impregnation chamber, the air control valve 62 for impregnation liquid recovery, and the impregnation liquid recovery control valve 61; Step 6: Open the air control valve 82 of the cleaning solvent to ensure that the cleaning solvent container 8 is at atmospheric pressure. Open the vacuum pump 10 until the impregnation chamber 2 is in a slightly negative pressure state; Step 7: Open the cleaning solvent control valve 81 to control the slow transfer of the cleaning solvent into the glass container 12. After covering the sample to be impregnated 11, close the cleaning solvent control valve 81, the air control valve 82 of the cleaning solvent, and the vacuum pump 10 in sequence, and maintain for ~1 min to fully remove the precursor impregnation liquid adhering to the surface of the impregnated sample, and avoid the precursor impregnation liquid adhering to block the pores of the impregnated sample; Step Eight: Open the air control valve 9 of the impregnation chamber, allow air to flow into the impregnation chamber 2 until it reaches atmospheric pressure. Open the cleaning solvent recovery air control valve 52 to ensure that the cleaning solvent recovery container 5 is at atmospheric pressure. Open the cleaning solvent recovery control valve 51, and use the self-gravity of the liquid to transfer the cleaning solvent to the cleaning solvent recovery container 5; Step Nine: After all the cleaning organic solvents are transferred to the cleaning solvent recovery container 5, close the air control valve 9 of the impregnation chamber, the cleaning solvent recovery control valve 51, and the cleaning solvent recovery air control valve 52.

[0057] Repeat Steps One to Nine, and cure (in an air environment, maintain at 80 °C for 18 h) three times. Conduct a high-temperature heat treatment at 1500 - 1700 °C once, and regard this process as one impregnation cycle. Repeat several impregnation cycles until the preparation of the C / C-ZrC-SiC composite material is completed.

[0058] Example 3: Step One: Prepare the sample to be impregnated 11 (~1.2 g / cm 3 C / C composite material), the required solutions (the precursor impregnation solution is a mixed solution of zirconium carbide precursor and polycarbosilane, and the organic solvent is xylene), connect the pipelines, and close the doors of each area bin.

[0059] Step Two: Open the air control valve 72 of the impregnation liquid to ensure that the impregnation liquid container 7 is at atmospheric pressure. Open the vacuum pump 10 until the impregnation chamber 2 is in a near-vacuum state; Step Three: Open the impregnation liquid control valve 71 to control the slow transfer of the precursor impregnation liquid into the glass container 12. After covering the sample to be impregnated 11, close the impregnation liquid control valve 71 and the air control valve 72 of the impregnation liquid in sequence, and maintain the impregnation for 1 h, then close the vacuum pump 10; Step Four: Open the air control valve 9 of the impregnation chamber, allow air to flow into the impregnation chamber 2 until it reaches atmospheric pressure. Open the impregnation liquid recovery air control valve 62 to ensure that the impregnation liquid recovery container 6 is at atmospheric pressure. Open the impregnation liquid recovery control valve 61, and use the self-gravity of the liquid to transfer the precursor impregnation solution to the impregnation liquid recovery container 6; Step Five: After all the precursor impregnation liquid is transferred to the impregnation liquid recovery container 6, close the air control valve 9 of the impregnation chamber, the impregnation liquid recovery air control valve 62, and the impregnation liquid recovery control valve 61; Step Six: Open the air control valve 82 of the cleaning solvent to ensure that the cleaning solvent container 8 is at atmospheric pressure. Open the vacuum pump 10 until the impregnation chamber 2 is in a slightly negative pressure state; Step 7: Open the cleaning solvent control valve 81 to control the slow delivery of the cleaning solvent into the glass container 12. After the cleaning solvent submerges the sample to be impregnated 11, close the cleaning solvent control valve 81, the cleaning solvent air control valve 82, and the vacuum pump 10 in sequence, and maintain for ~1 min to fully remove the precursor impregnation solution adhering to the surface of the impregnated sample, and avoid the pores of the impregnated sample being blocked by the adhering precursor impregnation solution; Step 8: Open the impregnation chamber air control valve 9 to allow air to flow into the impregnation chamber 2 to atmospheric pressure. Open the cleaning solvent recovery air control valve 52 to ensure that the cleaning solvent recovery container 5 is at atmospheric pressure. Open the cleaning solvent recovery control valve 51, and utilize the self-gravity of the liquid to deliver the cleaning solvent to the cleaning solvent recovery container 5; Step 9: After all the cleaning organic solvent is delivered to the cleaning solvent recovery container 5, close the impregnation chamber air control valve 9, the cleaning solvent recovery control valve 51, and the cleaning solvent recovery air control valve 52.

[0060] Repeat Steps 1 to 9, and cure (in an air environment, maintain at 100 °C for 12 h) three times, and conduct a high-temperature heat treatment at 1500 - 1700 °C once. Regard this process as one impregnation cycle, and repeat several impregnation cycles until the preparation of the C / C-ZrC-SiC composite material is completed.

[0061] Comparative Example Impregnate using the existing PIP technology, that is, put the sample to be impregnated 11 (~1.2 g / cm 3 C / C composite material) into the precursor impregnation solution (a mixed solution of zirconium carbide precursor and polycarbosilane), take it out after vacuum impregnation for 45 min, clean the surface of the sample with an organic solvent (xylene), and cure at 80 °C for 18 h in an air environment. Repeat impregnation and curing three times, and record it as one impregnation cycle after one heat treatment at 1500 - 1700 °C until the preparation of the C / C-ZrC-SiC composite material is completed.

[0062] See Figure 4 . After 13 impregnation cycles in the example, the density of the sample basically maintained a stable state, indicating that the limit value of the PIP process had been reached, while the comparative example reached the same density level after 16 impregnation cycles. Through comparison, it can be seen that using the equipment provided by the present invention can effectively improve the impregnation efficiency.

[0063] Figure 7 It is the scanning electron microscope image of the C / C-ZrC-SiC composite material prepared in Example 2 (the black phase is the carbon fiber / pyrolytic carbon matrix, the gray phase is SiC, and the bright white phase is ZrC); Figure 8 It is the scanning electron microscope image of the C / C-ZrC-SiC composite material prepared in Example 3 (the black phase is the carbon fiber / pyrolytic carbon matrix, the gray phase is SiC, and the bright white phase is ZrC).

[0064] See Figures 5 to 8 It can be seen that the preparation of the C / C-ZrC-SiC composite material is completed by the above-mentioned device and its use method. Additionally, the present invention provides a method of gradient impregnation. In step three, after the precursor impregnation solution submerges the sample 11 to be impregnated, the impregnation solution recovery air control valve 62 is opened at regular intervals, and the impregnation solution recovery control valve 61 is controlled to convey a certain height of the precursor impregnation solution into the impregnation solution recovery container 6 by means of the self-gravity of the liquid. Through this operation, the impregnation time at different positions in the thickness direction of the sample 11 to be impregnated can be made different, thereby controlling the ceramic content introduced in each impregnation, and thus achieving ceramic gradient in the thickness direction.

[0065] Additionally, the present invention provides a method of gradient impregnation for special-shaped samples. In step one, a profiled porous glass tooling is introduced to maintain the stability of the special-shaped sample 11 to be impregnated (such as an inverted sharp leading-edge part, that is, the head is downward). In step three, after the precursor impregnation solution submerges the sample 11 to be impregnated, the impregnation solution recovery air control valve 62 is opened at regular intervals, and the impregnation solution recovery control valve 61 is controlled to convey a certain height of the precursor impregnation solution into the impregnation solution recovery container 6 by means of the self-gravity of the liquid. Through this operation, the impregnation time at different positions in the thickness direction of the sample to be impregnated can be made different, thereby controlling the ceramic content introduced in each impregnation, and thus achieving ceramic gradient in the thickness direction (such as more ceramic content at the head of the sharp leading edge and less at the tail).

[0066] The above content is only to illustrate the technical idea of the present invention and cannot be used to limit the protection scope of the present invention. Any modification made on the basis of the technical solution according to the technical idea proposed by the present invention falls within the protection scope of the claims of the present invention.

Claims

1. An apparatus for rapid recovery and recycling of a precursor impregnation solution, characterized in that, It includes a raw material chamber (1), an impregnation chamber (2), and a raw material recovery chamber (3) arranged successively from top to bottom; at least one impregnation liquid container (7) is provided in the raw material chamber (1); a glass container (12) is provided in the impregnation chamber (2), and the glass container (12) is used to hold the specimen to be impregnated (11), and the impregnation chamber (2) is connected to a vacuum pump (10); at least one impregnation liquid recovery container (6) is provided in the raw material recovery chamber (3); the impregnation liquid recovery container (6), the impregnation liquid container (7), and the glass container (12) are all connected to an air pipeline, and an air control valve is respectively provided at the connection; the impregnation liquid container (7) is connected to the glass container (12) through a first pipeline, the glass container (12) is connected to the impregnation liquid recovery container (6) through a second pipeline, the impregnation liquid recovery container (6) is connected to a fourth pipeline through a third pipeline, and the fourth pipeline is connected to the impregnation liquid container (7); a control valve is respectively provided on the first pipeline, the second pipeline, and the third pipeline, and an impregnation liquid reuse oil pump (17) is provided on the fourth pipeline.

2. The device for rapid recovery and recycling of the precursor impregnation liquid according to claim 1, characterized in that, It further includes an impregnation liquid supplement container (15), and the impregnation liquid supplement container (15) is connected to the fourth pipeline through a fifth pipeline, and a control valve is provided on the fifth pipeline.

3. The device for rapid recovery and recycling of the precursor impregnation solution according to claim 1, characterized in that, A storage rack (13) is provided below the glass container (12).

4. The device for rapid recovery and recycling of the precursor impregnating solution according to claim 1, wherein A profiling porous glass tooling matching the specimen to be impregnated (11) is provided in the glass container (12).

5. The device for rapid recovery and recycling of the precursor impregnation solution according to claim 1, characterized in that, The raw material chamber (1), the impregnation chamber (2), and the raw material recovery chamber (3) are all sealed chambers, and a warehouse door is respectively opened on the same side of the raw material chamber (1), the impregnation chamber (2), and the raw material recovery chamber (3), and a transparent observation window is opened on the warehouse door.

6. The device for rapid recovery and recycling of the precursor impregnation solution according to claim 1, wherein The device for rapid recovery and recycling of the precursor impregnation liquid further includes a cleaning solvent recovery and utilization part, and the cleaning solvent recovery and utilization part includes at least one cleaning solvent container (8), at least one cleaning solvent recovery container (5), and at least one cleaning solvent supplement container (14); The cleaning solvent container (8) is arranged in the raw material chamber (1), the cleaning solvent recovery container (5) is arranged in the raw material recovery chamber (3), the cleaning solvent recovery container (5) and the cleaning solvent container (8) are both connected to an air pipeline, and an air control valve is respectively provided at the connection; the cleaning solvent container (8) is connected to the glass container (12) through a sixth pipeline, a solvent branch is opened on the second pipeline, and the solvent branch connects the glass container (12) and the cleaning solvent recovery container (5), the cleaning solvent recovery container (5) is connected to a ninth pipeline through a seventh pipeline, the cleaning solvent supplement container (14) is connected to the ninth pipeline through an eighth pipeline, the ninth pipeline is connected to the cleaning solvent container (8), a control valve is respectively provided on the sixth pipeline, the solvent branch, the seventh pipeline, and the eighth pipeline, and a cleaning solvent reuse oil pump (16) is provided on the ninth pipeline.

7. A method for using a device for rapid recovery and recycling of a precursor impregnation solution, characterized in that, Based on the device for rapid recovery and recycling of the precursor impregnation liquid according to any one of claims 1 to 6, it includes the following steps: S1: Open the air control valve at the connection between the impregnating solution container (7) and the air pipeline, and turn on the vacuum pump (10) until the impregnation chamber (2) is in a near-vacuum state; open the control valve on the first pipeline to deliver the precursor impregnating solution into the glass container (12). After the sample to be impregnated (11) is submerged, close all the opened valves mentioned above, and maintain the impregnation for a certain period of time before turning off the vacuum pump (10). S2: Open the air control valves at the connections between the impregnation chamber (2) and the impregnating solution recovery container (6) and the air pipeline respectively, and open the control valve on the second pipeline to deliver the precursor impregnating solution to the impregnating solution recovery container (6), and then close all the opened valves mentioned above. S3: Open the air control valve at the connection between the impregnating solution container (7) and the air pipeline and the control valve on the third pipeline, and start the impregnating solution reuse oil pump (17) to deliver the precursor impregnating solution in the impregnating solution recovery container (6) to the impregnating solution container (7).

8. The method of using the device for rapid recovery and recycling of the precursor impregnating solution according to claim 7, characterized in that, The device for rapid recovery and recycling of the precursor impregnating solution further includes an impregnating solution replenishing container (15), a fifth pipeline, and a control valve on the fifth pipeline. It further includes a replenishing step, which is as follows: If the precursor impregnating solution in the impregnating solution recovery container (6) is insufficient, open the control valve on the fifth pipeline to replenish and deliver the precursor impregnating solution in the impregnating solution replenishing container (15).

9. The method of using the device for rapid recovery and recycling of the precursor impregnation solution according to claim 8, characterized in that, It further includes a usage method for gradient impregnation, including the following steps: S101: Open the air control valve at the connection between the impregnating solution container (7) and the air pipeline, and turn on the vacuum pump (10) until the impregnation chamber (2) is in a near-vacuum state; open the control valve on the first pipeline to deliver the precursor impregnating solution into the glass container (12). After the sample to be impregnated (11) is submerged, close all the opened valves mentioned above. S102: Open the air control valve at the connection between the impregnating solution recovery container (6) and the air pipeline and the control valve on the second pipeline at regular intervals, and wait until a certain amount of the precursor impregnating solution is recovered before closing all the opened valves mentioned above. S103: Repeat S102 until all the precursor impregnating solution in the impregnation chamber (2) is completely recovered. Turn off the vacuum pump (10), and open the air control valve at the connection between the impregnation chamber (2) and the air pipeline until the impregnation chamber (2) returns to atmospheric pressure and then close it. S104: Open the air control valve at the connection between the impregnating solution container (7) and the air pipeline and the control valve on the third pipeline, and start the impregnating solution reuse oil pump (17) to deliver the precursor impregnating solution in the impregnating solution recovery container (6) to the impregnating solution container (7); if the precursor impregnating solution in the impregnating solution recovery container (6) is insufficient, open the control valve on the fourth pipeline to replenish and deliver the precursor impregnating solution in the impregnating solution replenishing container (15).

10. The method of using the device for rapid recovery and recycling of the precursor impregnating solution according to claim 8, characterized in that, A profiling porous glass tooling matching the profiled sample to be impregnated (11) is also provided in the glass container (12). It further includes a usage method for gradient impregnation of profiled parts, including the following steps: S111: Place the profiled sample to be impregnated (11) into the profiling porous glass tooling to fix its position, and then place it into the glass container (12). S112: Open the air control valve at the connection between the impregnation liquid container (7) and the air pipeline, and turn on the vacuum pump (10) until the impregnation chamber (2) is in a near-vacuum state; open the control valve on the first pipeline to convey the precursor impregnation liquid into the glass container (12), and close all the opened valves after the special-shaped sample to be impregnated (11) is submerged. S113: Open the air control valve at the connection between the impregnation liquid recovery container (6) and the air pipeline and the control valve on the second pipeline at regular intervals, and close all the opened valves after a certain amount of impregnation liquid is recovered. S114: Repeat S112 until all the precursor impregnation liquid in the impregnation chamber (2) is recovered, turn off the vacuum pump (10), and open the air control valve at the connection between the impregnation chamber (2) and the air pipeline until the impregnation chamber (2) returns to normal pressure and then close it. S115: Open the air control valve at the connection between the impregnation liquid container (7) and the air pipeline and the control valve on the third pipeline, and start the impregnation liquid reuse oil pump (17) to convey the precursor impregnation liquid in the impregnation liquid recovery container (6) to the impregnation liquid container (7); if the precursor impregnation liquid in the impregnation liquid recovery container (6) is insufficient, open the control valve on the fourth pipeline to supplement and convey the precursor impregnation liquid in the impregnation liquid supplementary container (15).

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