Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a precursor feeding system and a precursor feeding method for preparing a TaC coating by a chemical vapor deposition method, which are used for realizing stable sublimation, air flow homogenization and conveying control of a TaCl 5 precursor.
In order to achieve the above object, the invention provides a precursor feeding system for preparing TaC coating by chemical vapor deposition, which comprises a precursor tank, a primary buffer tank, a secondary buffer tank and a conveying pipeline, wherein the inner wall of the precursor tank is provided with an insulating layer, the precursor tank, the primary buffer tank and the secondary buffer tank are sequentially communicated through the conveying pipeline, wherein:
The outer side of the precursor tank is provided with a surrounding type heating device which comprises a feeding sublimation section, an air flow buffer section and an air flow steady flow section which are sequentially communicated, a heat conduction inert material is filled in the feeding sublimation section and used for improving the heat conduction of external precursor raw materials, a first flow equalizing disc used for reducing air flow fluctuation is arranged at the joint of the air flow buffer section and the air flow steady flow section, and a second flow equalizing disc used for reducing sublimation gas air flow fluctuation is arranged at the joint of the feeding sublimation section and the air flow buffer section;
the outlet end of the first-stage buffer tank is provided with a diversion weir for reducing the flow speed unevenness of the section;
The inside cellular water conservancy diversion core that is used for gaseous flow equalization steady voltage that is provided with of second grade buffer tank, second grade buffer tank exit end be connected with the conveying line of outside deposition furnace intercommunication.
In the feeding system, precursor TaCl 5 powder is mixed with the heat-conducting inert material in a feeding sublimation section, so that the heat transfer condition of a material bed is remarkably improved, uniform heating and stable sublimation of precursor TaCl 5 powder are realized, the fluctuation of the concentration of a TaCl 5 gas phase is reduced, and meanwhile, the fluctuation of the gas flow of the precursor gas phase is further reduced based on a first flow equalizing disc and a second flow equalizing disc;
The feeding system adopts a double-buffer structure of steady flow of the primary buffer tank and steady pressure of the secondary buffer tank, combines the design of the diversion weir and the honeycomb diversion core, effectively reduces the section flow velocity non-uniformity of the precursor gas phase, and further provides a guarantee for the continuity and uniformity of the subsequent TaC coating deposition process.
The precursor tank adopts a multi-point temperature control heating mode based on a surrounding type heating device to realize uniform temperature field of precursor raw materials.
The invention also provides a method for realizing precursor feeding based on the feeding system, which comprises the following steps:
s1, conveying precursor TaCl 5 powder into a precursor tank to be mixed with a heat-conducting inert material, sublimating the precursor TaCl 5 powder into a precursor gas phase through multi-point temperature control heating by a surrounding type heating device, and reducing the gas flow of the precursor gas phase through a first flow equalizing disc arranged in the precursor tank, wherein the mass ratio of the precursor TaCl 5 powder to the heat-conducting inert material is 3-5:1, and the heat-conducting inert material is one or more of quartz sand, carbon powder or alumina balls;
s2, enabling the precursor gas phase to enter a first-stage buffer tank through a conveying pipeline, and effectively reducing the section flow velocity of the precursor gas phase through a flow guiding weir arranged in the first-stage buffer tank so as to realize the steady flow of the precursor gas phase;
S3, the precursor gas phase enters a secondary buffer tank through a conveying pipeline, and under the action of the honeycomb flow guide core, the precursor gas phase is decomposed into a plurality of thin flows, so that pressure pulsation caused by local high-speed air flow is weakened, gas phase homogenization is realized, and then the precursor gas phase can be conveyed into an external deposition furnace through the conveying pipeline.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) The sublimation is uniform, namely, the heat conduction inert material mixed with the precursor TaCl 5 powder is filled in the precursor tank, so that the heat conduction of a material bed can be effectively improved, the evaporation rate of TaCl 5 is stable, and the technical problem of large evaporation rate fluctuation caused by uneven temperature field in the sublimation process in the prior art is solved;
(2) The air flow is stable, namely the interface flow speed non-uniformity of the precursor gas phase can be reduced to below 15 percent by arranging the double buffer structures of the primary buffer tank for stabilizing the flow and the secondary buffer tank for stabilizing the pressure, the air flow fluctuation is controlled within 5 percent, the continuity and the uniformity of the subsequent TaC coating deposition process are further ensured, the high-compactness TaC coating with the thickness uniformity of +/-3 percent can be obtained, the utilization rate and the deposition efficiency of raw materials are effectively improved by stabilizing air supply, the preparation period is shortened while the energy consumption is reduced, and the production cost is reduced;
(3) The mixing is uniform, namely, a diversion weir is arranged in the primary buffer tank, natural homogenization is carried out by utilizing the static pressure of the gas, and a honeycomb diversion core is arranged in the secondary buffer tank to decompose the jet flow at the inlet into uniform trickles, so that stirring-free homogenization is realized, secondary pollution is avoided, and the mixing uniformity of the multi-component gas is remarkably improved.
Detailed Description
The "range" disclosed herein is defined in terms of lower and upper limits, with the given range being defined by the selection of a lower and an upper limit, the selected lower and upper limits defining the boundaries of the particular range. Ranges that are defined in this way can be inclusive or exclusive of the endpoints, and any combination can be made, i.e., any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a particular parameter, it is understood that ranges of 60-110 and 80-120 are also contemplated. Furthermore, if minimum range values 1 and 2 are listed, and if maximum range values 3,4, and 5 are listed, then the following ranges are all contemplated as 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5. In the present application, unless otherwise specified, the resin range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, the resin range "0-5" means that all real numbers between "0-5" have been listed throughout, and "0-5" is only a shorthand representation of these resin combinations. When a certain parameter is expressed as an integer of 2 or more, it is disclosed that the parameter is, for example, an integer of 2,3,4, 5, 6, 7, 8, 9, 10, 11, 12 or the like.
The terms "comprising" and "including" as used herein mean open ended or closed ended, unless otherwise noted. For example, the terms "comprising" and "comprises" may mean that other components not listed may be included or included, or that only listed components may be included or included.
The term "or" is inclusive in this application, unless otherwise specified. For example, the phrase "a or B" means "a, B, or both a and B. More specifically, either condition satisfies the condition "A or B" that A is true (or present) and B is false (or absent), that A is false (or absent) and B is true (or present), or that both A and B are true (or present).
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way.
As shown in fig. 1 to 3, the application provides a precursor feeding system for preparing a TaC coating by a chemical vapor deposition method, which comprises a precursor tank 100, a primary buffer tank 200, a secondary buffer tank 300 and a conveying pipeline 400, wherein the inner walls of the precursor tank 100, the primary buffer tank 200 and the secondary buffer tank 300 are all provided with heat insulation layers, and the precursor tank 100, the primary buffer tank 200 and the secondary buffer tank 300 are sequentially communicated through the conveying pipeline 400, wherein:
The outer side of the precursor tank 100 is provided with a surrounding type heating device 110 which comprises a feeding sublimation section 120, an air flow buffer section 130 and an air flow steady flow section 140 which are sequentially communicated, a heat conduction inert material is filled in the feeding sublimation section 120 and used for improving the heat conduction of external precursor raw materials, a first flow equalizing disc 150 used for reducing air flow fluctuation is arranged at the joint of the air flow buffer section 130 and the air flow steady flow section 140, and a second flow equalizing disc 160 used for reducing sublimation gas air flow fluctuation is arranged at the joint of the feeding sublimation section 120 and the air flow buffer section 130;
The outlet end of the primary buffer tank 200 is provided with a diversion weir 210 for reducing the cross-sectional flow velocity unevenness;
The inside cellular water conservancy diversion core 310 that is used for gaseous flow equalization steady voltage that is provided with of second grade buffer tank 300, and the delivery line 400 that is connected with outside deposition furnace intercommunication is connected to second grade buffer tank 300 outlet end.
The feeding system adopts a double-buffer structure with steady flow of the primary buffer tank 200 and steady pressure of the secondary buffer tank 300, and combines the design of the diversion weir 210 and the honeycomb diversion core 310, so that the cross-section flow velocity non-uniformity of the precursor gas phase is effectively reduced, and further, the continuity and uniformity of the subsequent TaC coating deposition process are ensured.
As shown in fig. 4, the present application further provides a method for implementing precursor feeding based on the feeding system, which includes the following steps:
S1, conveying precursor TaCl 5 powder into a precursor tank 100 to be mixed with a heat-conducting inert material, sublimating the precursor TaCl 5 powder into a precursor gas phase through multi-point temperature control heating by a surrounding type heating device 110, and reducing the gas flow of the precursor gas phase through a first flow equalizing plate 150 arranged in the precursor tank 100, wherein the mass ratio of the precursor TaCl 5 powder to the heat-conducting inert material is 3-5:1, and the heat-conducting inert material is one or more of quartz sand, carbon powder or alumina balls;
It should be noted that in other embodiments, the precursor gas phase further reduces gas flow fluctuations via a second flow equalization plate 160 disposed within the precursor tank 100, wherein the second flow equalization plate 160 is disposed at the junction of the feed sublimation section 120 and the gas flow buffer section 130.
S2, the precursor gas phase enters the first-stage buffer tank 200 through the conveying pipeline 400, and the flow velocity of the cross section of the precursor gas phase is effectively reduced through the flow guiding weir 210 arranged in the first-stage buffer tank 200, so that the steady flow of the precursor gas phase is realized;
S3, the precursor gas phase enters the secondary buffer tank 300 through the conveying pipeline, and is decomposed into a plurality of fine flows under the action of the honeycomb flow guide cores 310, so that pressure pulsation caused by local high-speed air flow is weakened, gas phase homogenization is realized, and then the precursor gas phase can be conveyed into an external deposition furnace through the conveying pipeline 400.
To further illustrate the principles and technical effects of the present invention, a precursor vapor phase is provided to an external CVD deposition furnace based on the feed system and feed method as follows.
Example 1
400G of precursor tantalum pentachloride (TaCl 5) powder with the average grain diameter of 140-160 mu m is taken, the taken precursor tantalum pentachloride (TaCl 5) powder is sent into a precursor feeding system, and TaCl 5 is supplied to an external CVD deposition furnace through a conveying pipeline 400 after being processed by the precursor feeding system–Ar mixture and depositing TaC coating on the graphite substrate, the specific steps are as follows:
(1) Mixing the obtained precursor TaCl 5 powder with quartz sand according to a ratio of 4:1, loading the mixture into a feeding sublimation section 120, heating the mixture by a multi-point temperature control heating mode of a surrounding type heating device 110, controlling the temperature of the feeding sublimation section 120 to be 180+/-10 ℃, controlling the temperature of an airflow buffer section 130 to be 200+/-10 ℃, and controlling the temperature of an airflow steady flow section 140 to be 210+/-10 ℃, so as to realize step-by-step uniform sublimation of TaCl 5;
(2) The sublimated TaCl 5 gas phase passes through the flow guiding weir 210 arranged at the outlet of the primary buffer tank 200, so that the flow speed unevenness of the section of the TaCl 5 gas phase is reduced to 15%, and then passes through the honeycomb flow guiding core 310 arranged in the secondary buffer tank 300, so that inlet air flow pulsation is eliminated, and the steady flow and pressure stabilization of the TaCl 5 gas phase are realized.
(3) The TaCl 5 gas phase after pressure stabilization and current stabilization passes through the conveying pipeline 400 and–Ar is mixed and then enters an external CVD deposition furnace, and is deposited on the surface of the graphite substrate for 5 hours at 1300 ℃ and 2kPa, so as to form the TaC coating with the thickness of 40 mu m.
Example 2
Unlike example 1, in example 2, precursor TaCl 5 powder was mixed with quartz sand at a 3:1 ratio.
Example 3
Unlike example 1, in example 3, precursor TaCl 5 powder was mixed with quartz sand at a ratio of 5:1.
The fluctuation of the gas flow rate during the deposition in the external CVD deposition furnace and the uniformity of the thickness of the TaC coating after the deposition in examples 1 to 3 were examined, respectively, and the examination results are shown in Table 1.
TABLE 1 detection of fluctuation in gas flow rate during deposition in an external CVD deposition furnace and TaC coating thickness uniformity after deposition in examples 1-3
As can be seen from table 1, the precursor feed systems of examples 1-3 each provided a gas flow rate fluctuation of less than 4.2% for the mixed gas, and the thickness uniformity of the TaC coating deposited in the external CVD deposition furnace based on the mixed gas was within ±3%. Therefore, the precursor feeding system and method provided by the invention can realize stable sublimation, air flow homogenization and conveying control of the TaCl 5 precursor.
It should be noted that, in the above embodiment, the delivery pipe 400 is a stainless steel pipe, and the insulating layer is an electric heating belt wrapped around the precursor tank 100, the primary buffer tank 200, the secondary buffer tank 300, and the delivery pipe 400.
The precursor feeding system and the precursor feeding method for preparing the TaC coating by the chemical vapor deposition method provided by the application are described in detail. The principles and embodiments of the present application have been described herein with reference to specific examples, the description of which is intended only to facilitate an understanding of the core concepts of the application. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the application can be made without departing from the principles of the application and these modifications and adaptations are intended to be within the scope of the application as defined in the following claims.