CN115717681A - Steel cylinder for precursor solid source - Google Patents
Steel cylinder for precursor solid source Download PDFInfo
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- CN115717681A CN115717681A CN202211472550.4A CN202211472550A CN115717681A CN 115717681 A CN115717681 A CN 115717681A CN 202211472550 A CN202211472550 A CN 202211472550A CN 115717681 A CN115717681 A CN 115717681A
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- 239000007787 solid Substances 0.000 title claims abstract description 124
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 98
- 239000010959 steel Substances 0.000 title claims abstract description 98
- 239000002243 precursor Substances 0.000 title claims abstract description 28
- 239000012159 carrier gas Substances 0.000 claims abstract description 158
- 238000010438 heat treatment Methods 0.000 claims abstract description 121
- 238000007789 sealing Methods 0.000 claims description 73
- 239000007789 gas Substances 0.000 claims description 35
- 239000000523 sample Substances 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 11
- 230000001105 regulatory effect Effects 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 7
- 238000005019 vapor deposition process Methods 0.000 claims description 7
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 230000003749 cleanliness Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 10
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- 230000008569 process Effects 0.000 description 6
- 238000007740 vapor deposition Methods 0.000 description 6
- 230000003044 adaptive effect Effects 0.000 description 5
- 238000005485 electric heating Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 238000000859 sublimation Methods 0.000 description 4
- 230000008022 sublimation Effects 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 230000001174 ascending effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000005465 channeling Effects 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
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- 229920001774 Perfluoroether Polymers 0.000 description 1
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- PDPJQWYGJJBYLF-UHFFFAOYSA-J hafnium tetrachloride Chemical compound Cl[Hf](Cl)(Cl)Cl PDPJQWYGJJBYLF-UHFFFAOYSA-J 0.000 description 1
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- 238000010295 mobile communication Methods 0.000 description 1
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- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
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- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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Abstract
The invention discloses a steel cylinder for a precursor solid source, which comprises: the solid source steel cylinder main body is connected with a heating temperature control system; the source steel cylinder body is internally provided with a carrier gas channel, the side wall of the carrier gas channel is provided with an opening facing the bottom of the solid source steel cylinder and communicated with the outside, and the carrier gas channel is spirally arranged from the center to the outside at equal intervals; the heating temperature control system is positioned at the bottom of the solid source steel cylinder main body and comprises heaters, the heaters are spirally arranged from the center to the outer side at equal intervals, and the heaters correspond to the openings and extend into the openings; the circulation path of the carrier gas is prolonged in a limited space, and the carrying-out quantity of the carrier gas to the precursor chemical can be fully and effectively ensured. The heater extends into the side wall of the carrier gas channel for heating, so that uniform heating of the channel is ensured, the heating efficiency of chemicals is improved, and the overall size of the solid source steel cylinder is reduced.
Description
Technical Field
The invention relates to the field of chemical vapor deposition, in particular to a steel cylinder for a precursor solid source.
Background
The ultra-high purity ALD/CVD precursor product is one of the core raw materials of the whole electronic industry system, is widely applied to various aspects of manufacturing electronic devices such as computer chips, solar cells, mobile communication, satellite navigation, spacecrafts and the like, and plays a great role in the fields of aerospace, novel solar cells, electronic products and the like.
Currently, in the process of using a solid precursor source as a key process material in a vapor deposition technology, the operating characteristics of a vapor deposition system determine that the solid precursor source material needs to be converted into a vapor phase and transported into a reactor chamber of the system, so as to obtain the deposition of a target element. The key to solving the above problems is to solve the stability of the continuous sublimation of the solid source and how the carrier gas sufficiently carries out the mixed saturated vapor. In the currently widely implemented method, an integral source bottle is placed in a transportable system device, heat energy is given outside the source bottle, the heat energy is transferred into the bottle through the bottle wall, and a solid precursor source inside the bottle is indirectly heated, so as to meet the use requirement of the vapor of the solid precursor source required by the vapor deposition process. In view of such technical needs, the source bottle has a need for thermal energy, the solid precursor source is heated to volatilize, and vapor from the solid precursor source is carried along and transferred to the sublimation process of the entire solid source in the demand system under the flow of carrier gas.
The existing solid source steel cylinder cavity is too large, so that a large amount of channeling and hardening phenomena can be generated in the solid source in the using process, the heat energy supply mode of the solid source steel cylinder is the steel cylinder surface supply and supply mode, so that the position, close to the center, of the solid source steel cylinder cavity cannot obtain the heat energy meeting the sublimation of the solid source, the phenomenon that the solid source is heated unevenly occurs, and finally, a gas phase source cannot obtain stable output.
For example, a "solid precursor source sublimation apparatus and method for semiconductor processing" disclosed in chinese patent literature, the publication No. thereof: CN113529053B discloses a storage box, a plurality of trays installed in the storage box, and an electric heating temperature control plate installed at the bottom of the trays, wherein a plurality of storage tanks for loading solid precursor sources are densely distributed on the trays, the storage box forms a serpentine ventilation channel, a carrier gas inlet and a mixed steam outlet are arranged on the storage box, two ends of the ventilation channel are respectively communicated with the carrier gas inlet and the mixed steam outlet, but the steam pressure and uniform heating after heating are not guaranteed.
Disclosure of Invention
In order to solve the problems of insufficient saturated vapor pressure, uneven heating and channeling hardening of the solid source in the prior art, the invention provides the steel cylinder for the precursor solid source, which prolongs the flow path of the carrier gas, reduces the path diameter of the carrier gas and increases the heating area of the solid source.
In order to achieve the above purpose, the invention provides the following technical scheme:
a cylinder for a solid source of precursor, comprising: the solid source steel cylinder main body is connected with a heating temperature control system; a carrier gas channel is arranged in the source steel cylinder body, the side wall of the carrier gas channel is provided with an opening facing the bottom of the solid source steel cylinder and communicated with the outside, and the carrier gas channel is spirally arranged from the center to the outside at equal intervals; the heating temperature control system is positioned at the bottom of the solid source steel cylinder main body and comprises a heater, the heater is spirally arranged from the center to the outer side at equal intervals, and the heater corresponds to the opening and extends into the opening. The carrier gas channel is in a mosquito-repellent incense coil shape, the carrier gas channel is respectively provided with a carrier gas inlet transition groove and a carrier gas outlet transition groove at the center and the outer end of the mosquito-repellent incense coil, the upper side of the carrier gas channel is hollowed, the carrier gas channel wall between two adjacent carrier gas channels is hollowed downwards to form an opening, the openings in the downward opening direction and the carrier gas channels in the upward opening direction are alternately arranged, the flow path of carrier gas is prolonged in a limited space, and the carrying-out amount of carrier gas to the front body chemical can be fully and effectively ensured. The heater extends into the side wall of the carrier gas channel for heating, so that the uniform heating of the channel is ensured, the heating efficiency of chemicals is improved, and the overall size of the solid source steel cylinder is reduced.
Preferably, the solid source steel cylinder body comprises an upper sealing cover, the upper sealing cover is connected with a cylinder body, the upper sealing cover is connected with an air inlet part, the air inlet part is communicated with the cylinder body, and the cylinder body is connected with a heating temperature control system. The upper end surface of the bottle body and the upper end surface of the side wall of the carrier gas channel are positioned on the same horizontal plane; the main body of the solid source steel cylinder is of a circular cake-shaped structure; go up closing cap and bottle and pass through bolt fixed connection, the inside ascending gas reaction chamber of opening that is equipped with of bottle, carrier gas channel is located the gas reaction intracavity, and carrier gas channel's lateral wall runs through the gas reaction chamber downwards and communicates with the external world, and the lower terminal surface of going up the closing cap forms sealedly with carrier gas channel's the terminal butt of upside for go up the closing cap and constitute the cavity of carrier gas circulation jointly with carrier gas channel lateral wall, guarantee that the carrier gas circulates along carrier gas channel after getting into inside the solid source steel bottle.
Preferably, the heating temperature control system comprises an outer side temperature control part, the inner side lower end wall of the outer side temperature control part is connected with an inner side temperature control part, and the inner side temperature control part is used for preheating and automatically adjusting the heating temperature of the carrier gas before the carrier gas is introduced; the heater is arranged on the top of the inner temperature control part. Outside accuse temperature portion is used for heating the whole heat preservation of bottle from the outside, improves the bulk temperature, and inboard accuse temperature portion is used for heating carrier gas passageway, and inboard accuse temperature portion is used for automatically regulated heating temperature. Can heat the bottle body from the outside and inboard together, improve the result of use, reduce the heat and run off.
Preferably, a sealing ring groove is arranged between the upper sealing cover and the bottle body, and the sealing ring grooves are respectively positioned on the corresponding surfaces of the upper sealing cover and the bottle body; the upper sealing cover is provided with an air passage penetrating through the upper sealing cover, and the tail end of the air passage is positioned at the bottom of the upper sealing cover and is provided with a particle filter screen. Be equipped with the sealing washer in the sealing washer groove, the sealing washer is used for being compressed after last closing cap and bottle locking and realizes sealed for gas can not be because of pressure backs down the sealing washer or flow out from the gap. The carrier gas is input into the carrier gas channel from the upper part of the bottle body through the gas channel, and impurity particles in the carrier gas can be filtered through the filter screen, so that the impurity particles are prevented from entering the carrier gas channel to cause blockage and pollution.
Preferably, the inner temperature control part comprises a heating controller, the heating controller is respectively connected with a temperature heater and a temperature probe, the temperature probe is connected with a temperature probe hole, and the temperature probe hole is positioned between two adjacent openings; the temperature heaters are positioned between two adjacent heaters. The heating controller receives a temperature signal of the temperature probe, the heating controller adjusts the power of the temperature heater according to the change of the temperature signal, the heater is controlled through the temperature heater, an adaptive function is established according to the feedback temperature of the temperature probe and the heat conversion working power of the heater, the heating power is output according to the adaptive function, the heating temperature adjustment in the working process is realized, and the heating stability of the whole solid source steel cylinder is ensured.
Preferably, the gas inlet part comprises a carrier gas inlet and a carrier gas outlet which are sequentially arranged at the top of the upper sealing cover, the carrier gas inlet is connected with a micro gas heater, the micro gas heater is connected with a flow regulating valve, and the gas inlet part further comprises a pressurizing port. The carrier gas inlet is communicated with the carrier gas inlet transition groove; realize the inside pressurization leak hunting function of bottle through the pressurization mouth, import the carrier gas through the carrier gas entry and to the carrier gas passageway, preheat through miniature gas heater simultaneously, realize the flow control before the carrier gas gets into through flow control valve.
Preferably, the bottom of the solid source steel cylinder body is provided with a fixing hole, the fixing hole faces the inner side temperature control part, the inner side temperature control part is provided with a fixing bolt, and the fixing bolt corresponds to the fixing hole. The inner side temperature control part is provided with a bottle body chassis heating device, the fixing bolt is positioned on the upper end surface of the bottle body chassis heating device, and the bottle body chassis heating device are in socket joint type matching through the fixing hole and the fixing bolt.
Preferably, the outer temperature control part comprises a heat-insulating heating sleeve, the source steel cylinder main body is positioned in the heat-insulating heating sleeve, and the heat-insulating heating sleeve is connected with the heating controller. The bottle body and the upper cover are covered by the heat-preservation heating sleeve, and the whole solid source steel cylinder main body can be heated and preserved.
Preferably, the material of the main body of the solid source steel cylinder is a material satisfying the cleanliness grade required by the vapor deposition process when heated for use. Ensuring that no extra impurities are generated at high temperature and high pressure.
The invention has the following advantages:
(1) The circulation path of the carrier gas is prolonged in a limited space, and the carrying-out quantity of the carrier gas to the precursor chemicals can be fully and effectively ensured. The heater extends into the side wall of the carrier gas channel for heating, so that the uniform heating of the channel is ensured, the heating efficiency of chemicals is improved, and the overall size of the solid source steel cylinder is reduced; (2) And the heating power is output according to the adaptive function, and the heating temperature adjustment in the working process is realized, so that the heating stability of the whole solid source steel cylinder is ensured.
Drawings
The drawings in the following description are merely exemplary, and it will be apparent to those of ordinary skill in the art that other embodiments can be derived from the provided drawings without inventive effort.
FIG. 1 is a schematic view showing an assembly structure of a solid source cylinder according to the present invention.
FIG. 2 is a cross-sectional view of a solid source cylinder according to the present invention.
FIG. 3 is a diagram of a solid source cylinder body of the present invention.
FIG. 4 is a view showing a heating apparatus for a bottle body base in the present invention.
In the figure:
1-flow regulating valve; 2-micro gas heater; 3-heat preservation and heating jacket; 4, a temperature probe; 5-a temperature heater; 6-a heating controller; 7-carrier gas channel side wall; 8-a heater; 9-particle filter screen; 10-sealing ring groove; 11-temperature probe aperture; 12-carrier gas outlet transition groove; 13-a carrier gas channel; 14-heater power supply vias; 15-a pressurizing port; 16-carrier gas inlet; 17-a carrier gas outlet; 18-carrier gas inlet transition slot.
Detailed Description
The embodiments of the present invention are described below by specific examples, and all other examples obtained by those skilled in the art without any inventive work are within the scope of the present invention.
In a preferred embodiment, as shown in FIGS. 1-4, the present invention discloses a cylinder for a solid source of precursor, comprising: the solid source steel cylinder main body is connected with a heating temperature control system; a carrier gas channel 13 is arranged in the source steel cylinder body, the side wall 7 of the carrier gas channel 13 is provided with an opening facing the bottom of the solid source steel cylinder and communicated with the outside, and the carrier gas channel 13 is spirally arranged from the center to the outside at equal intervals; the heating temperature control system is located the bottom of the solid source steel cylinder main body and comprises a heater 8, the heater 8 is spirally arranged from the center to the outer side at equal intervals, and the heater 8 corresponds to the opening and extends to the inside of the opening. The carrier gas channel 13 is in a mosquito coil shape, the carrier gas channel 13 is respectively provided with a carrier gas inlet 16 transition groove and a carrier gas outlet 17 transition groove 12 at the center and the outer end of the mosquito coil, the upper side of the carrier gas channel 13 is hollowed, the wall of the carrier gas channel 13 between two adjacent carrier gas channels 13 is hollowed downwards to form an opening, the openings in the downward opening direction and the carrier gas channels 13 in the upward opening direction are alternately arranged, the flow path of the carrier gas is prolonged in a limited space, and the carrying-out amount of the carrier gas to the precursor chemical can be fully and effectively ensured. The heater extends into the side wall of the carrier gas channel 13 for heating, so that the uniform heating of the channel is ensured, the heating efficiency of chemicals is improved, and the overall size of the solid source steel cylinder is reduced.
When in use, the mosquito-repellent incense coil channel wall is hollow and is opened from the bottom end of the bottle body, and the heater is in the shape of a convex mosquito-repellent incense coil; the hollow part is a concave mosquito-repellent incense coil-shaped channel when being observed from the outer lower end of the bottle body; the heater and the opening form letter socket type matching, the heater can heat the carrier gas channel from head to tail, the left side, the right side and the lower side of the carrier gas channel are heated, and the left side, the right side and the lower side of the solid source are heated.
The solid source steel cylinder main body comprises an upper sealing cover, the upper sealing cover is connected with a cylinder body, the upper sealing cover is connected with an air inlet part, the air inlet part is communicated with the cylinder body, and the cylinder body is connected with a heating temperature control system. The upper end surface of the bottle body and the upper end surface of the side wall of the carrier gas channel 13 are positioned on the same horizontal plane; the main body of the solid source steel cylinder is of a circular cake-shaped structure; go up closing cap and bottle and pass through bolt fixed connection, the inside ascending gas reaction chamber of opening that is equipped with of bottle, carrier gas channel 13 is located the gas reaction intracavity, and carrier gas channel 13's lateral wall runs through the gas reaction chamber downwards and communicates with the external world, and the lower terminal surface of going up the closing cap forms sealedly with carrier gas channel 13's the terminal butt of upside for go up closing cap and carrier gas channel 13 lateral wall 7 constitute the cavity of carrier gas circulation jointly, guarantee that the carrier gas circulates along carrier gas channel 13 after getting into inside the solid source steel bottle.
The heating temperature control system comprises an outer side temperature control part, the inner side lower end wall of the outer side temperature control part is connected with an inner side temperature control part, and the inner side temperature control part is used for preheating and automatically adjusting the heating temperature of the carrier gas before the carrier gas is introduced; the heater is positioned at the top of the inner temperature control part. The outer side temperature control part is used for heating and insulating the whole bottle body from the outer side to improve the whole temperature, the inner side temperature control part is used for heating the carrier gas channel 13, and the inner side temperature control part is used for automatically adjusting the heating temperature. Can heat the bottle body from the outside and inboard together, improve the result of use, reduce the heat and run off.
A sealing ring groove 10 is arranged between the upper sealing cover and the bottle body, and the sealing ring groove 10 is respectively positioned on the corresponding surfaces of the upper sealing cover and the bottle body; the upper sealing cover is provided with an air channel penetrating through the upper sealing cover, and the tail end of the air channel is positioned at the bottom of the upper sealing cover and is provided with a particle filter screen 9. The sealing ring is arranged in the sealing ring groove 10, and the sealing ring is used for being compressed to realize sealing after the upper sealing cover and the bottle body are locked, so that gas cannot push the sealing ring open due to pressure or flow out from a gap. The carrier gas is input into the carrier gas channel 13 from the upper part of the bottle body through the gas channel, and impurity particles in the carrier gas can be filtered through the filter screen, so that the impurity particles are prevented from entering the carrier gas channel 13 to cause blockage and pollution.
When the sealing ring is used, after the bolt is screwed down, the half sealing ring groove 10 on the lower end surface of the upper sealing cover and the half sealing ring groove 10 on the upper end surface of the bottle body form a complete sealing ring groove 10, and the sealing ring is compressed to the size of the sealing ring groove 10 to realize sealing. The carrier gas passes through the particle filter screen 9 to realize impurity filtration before entering the gas reaction cavity through the gas channel.
The inner side temperature control part comprises a heating controller 6, the heating controller 6 is respectively connected with a temperature heater 5 and a temperature probe 4, the temperature probe 4 is connected with a temperature probe 4 hole, and the temperature probe 4 hole is positioned between two adjacent openings; the temperature heater 5 is located between two adjacent heaters. The hole of the temperature probe 4 is positioned, the temperature probe 4 is used for detecting the temperature of the lower side of the carrier gas channel 13, the hole of the temperature probe 4 is positioned in the bottle body of the lower side of the carrier gas channel 13, the heating controller 6 receives the temperature signal of the temperature probe 4, the heating controller 6 adjusts the power of the temperature heater 5 according to the change of the temperature signal, the heater is controlled through the temperature heater 5, an adaptive function is established according to the feedback temperature of the temperature probe 4 and the heat conversion working power of the heater, the heating power is output according to the adaptive function, the heating temperature adjustment in the working process is realized, and therefore the heating stability of the whole solid source steel bottle is ensured.
In use, the temperature probe 4 detects the temperature of the solid source at the bottom of the carrier gas channel 13, the temperature probe 4 sends a temperature signal to the heating controller 6, and the heating effect of the heater in the side wall 7 of the carrier gas channel 13 is controlled by the heating controller 6.
The air inlet part comprises a carrier gas inlet 16 and a carrier gas outlet 17 which are sequentially arranged at the top of the upper sealing cover, the carrier gas inlet 16 is connected with a micro gas heater 2, the micro gas heater 2 is connected with a flow regulating valve 1, and the air inlet part further comprises a pressurizing port 15. The carrier gas inlet 16 is communicated with the transition groove of the carrier gas inlet 16; the pressure filling leakage detection function inside the bottle body is realized through the pressure filling port 15, the carrier gas is input into the carrier gas channel 13 through the carrier gas inlet 16, the preheating is carried out through the micro gas heater 2, and the flow regulation before the carrier gas enters is realized through the flow regulating valve 1.
When the device is used, carrier gas enters the carrier gas inlet 16 through the flow regulating valve 1 and the micro gas heater 2, the flow and the temperature of the carrier gas are regulated, the carrier gas enters the carrier gas channel 13 through the transition groove of the carrier gas inlet 16, the sublimation gas of the solid source is mixed and then enters the carrier gas outlet 17 through the transition groove 12 of the carrier gas outlet 17, and the mixed steam is discharged through the carrier gas outlet 17. The fluid inlet and outlet can be controlled by the main valve or the external valve.
The bottom of the solid source steel cylinder body is provided with a fixing hole, the fixing hole faces to the inner side temperature control part, the inner side temperature control part is provided with a fixing bolt, and the fixing bolt corresponds to the fixing hole. The inner side temperature control part is provided with a bottle body chassis heating device, the fixing bolt is positioned on the upper end surface of the bottle body chassis heating device, and the bottle body chassis heating device are in socket joint type matching through the fixing hole and the fixing bolt.
The outer temperature control part comprises a heat preservation heating sleeve 3, the source steel cylinder main body is positioned in the heat preservation heating sleeve 3, and the heat preservation heating sleeve 3 is connected with a heating controller 6. The heat preservation heating jacket 3 covers the bottle body and the upper cover in a whole manner, and can heat and preserve heat of the whole solid source steel cylinder main body.
When using, carry out the temperature setting to the heating protective sheath, whether accord with operation requirement through temperature probe 4 detection temperature, when not being conform to operation requirement, carry out temperature regulation to the heating protective sheath through temperature controller.
The material of the solid source steel cylinder main body is a material which meets the cleanness grade required by the vapor deposition process when being heated and used. Ensuring that no extra impurities are generated at high temperature and high pressure. The sealing ring of the solid source steel cylinder is made of perfluoroether, polytetrafluoroethylene or winding type soft material which meets the requirement of the cleanness grade required by the vapor deposition process; the upper sealing cover of the solid source steel cylinder is made of metal or nonmetal, and the inside of the upper sealing cover has a clean grade meeting the requirement of a vapor deposition process; the bottle body is made of metal or nonmetal, and the inside of the bottle body is provided with a clean grade meeting the requirement of a vapor deposition process.
When in use, the invention comprises the following steps: a. a precursor solid source is filled in a bottle body mosquito coil type channel of a solid source steel bottle; b. sequentially mounting an upper sealing cover of the solid source steel cylinder and a heating device of a bottom plate of the cylinder body on the cylinder body of the solid source steel cylinder; c. filling helium gas into the solid source steel cylinder body from the pressurizing port 15, and carrying out tightness detection on the sealing cover on the solid source steel cylinder and the flange connection part of the cylinder body by using a handheld helium detector; d. covering a steel cylinder heat-preservation heating sleeve 3 on a solid source steel cylinder; e. connecting a carrier gas inlet and a mixed steam outlet to a pipeline of a vapor deposition system, and introducing carrier gas into the carrier gas inlet; f. the electric heating temperature control plate is electrified and is provided with a heating device for heating, the electric heating temperature control plate heats the solid precursor source in the storage tank, and when the heating temperature reaches the set temperature; g. and opening a carrier gas inlet valve and a carrier gas outlet valve to introduce carrier gas so as to bring the vapor of the solid precursor source into the vapor deposition system.
In a second embodiment, comprising: the solid source steel cylinder comprises a solid source steel cylinder body, a solid source steel cylinder heating device and a temperature control system. The solid source steel cylinder main body mainly comprises: the upper sealing cover and the bottle body of the solid source steel cylinder are connected through the flange face bolt, after the bolt is locked, firstly, the sealing washer placed in the sealing groove is extruded to form sealing for the whole flange, and therefore the sealing effect of the whole solid source steel cylinder is achieved. Moreover, the end face of the upper sealing cover of the solid source steel cylinder is tightly attached to the carrier gas channel to form sealing, so that the carrier gas is ensured to flow along the carrier gas channel after entering the solid source steel cylinder; the upper sealing cover is mainly provided with a carrier gas inlet, a carrier gas outlet, a pressurizing port, a flow regulating valve and a micro gas heater, a particle filter screen is arranged on the flange surface of each interface, the gas filtering function is achieved, carrier gas enters the solid source steel cylinder from the carrier gas inlet and then flows out from the carrier gas outlet, and the pressurizing port is used for pressurizing and detecting leakage after the upper sealing cover of the solid source steel cylinder is connected with the bottle body.
The mosquito-repellent incense coil type carrier gas channel is arranged inside the bottle body, and has the advantages that the circulation path of the carrier gas is well prolonged, the carrying-out of the precursor chemicals by the carrier gas is fully and effectively guaranteed, the mosquito-repellent incense coil type channel wall is designed to be hollowed out outwards through an opening, and the hollowed-out part is a concave mosquito-repellent incense coil type channel when observed from the outer lower end of the bottle body. The solid source steel cylinder heating and temperature control system mainly comprises: the heating device of the bottle body chassis heating device is in a convex mosquito-repellent incense coil shape in appearance and forms primary-secondary socket type matching with the lower end face of the bottle body, and the matching has the advantages of ensuring uniform heating of a channel, improving the heating efficiency of chemicals and reducing the overall size of the solid source steel cylinder; besides, the whole body of the steel cylinder is provided with a heating and heat-insulating sleeve for heating and insulating the whole solid source steel cylinder; the heating and heat-preserving device has the functions of temperature setting and temperature regulation, the heating device heats the solid source steel cylinder through the set temperature, the temperature probe feeds the temperature of the solid source steel cylinder back to the controller, and the heating temperature regulation is carried out according to the temperature fed back by the temperature probe, so that the heating stability of the whole solid source steel cylinder is ensured.
Because the end surface of the upper sealing cover of the solid source steel cylinder is tightly attached to the carrier gas channel to form sealing, the carrier gas is heated by the micro gas heater after the flow regulation is finished by the flow regulating valve, enters the carrier gas inlet transition groove in the solid source steel cylinder, and flows to the carrier gas outlet transition groove along the mosquito coil-shaped channel to flow out;
the solid source is placed in a mosquito coil type channel of a solid source steel bottle body, the solid source is sublimated by heating a bottle body base plate, and then the sublimated solid source is taken into equipment by carrier gas;
the pressurizing port is used for sealing and leakage detection of the joint of the solid source steel cylinder body and the upper sealing cover, and can be set at any part outside the mosquito-repellent incense coil shape of the cylinder body according to the space of a machine table at a use end.
Fig. 1 is a schematic diagram illustrating assembly of a solid source steel cylinder in this embodiment, the solid source steel cylinder is divided into a solid source steel cylinder main body, a solid source steel cylinder heating device and a temperature control system, and the upper portion of the solid source steel cylinder includes: an upper sealing cover and a bottle body; the lower part and the outer layer of the solid source steel cylinder are provided with a solid source steel cylinder heating device and a temperature control system. The upper sealing cover of the solid source steel cylinder is provided with a flow regulating valve 1 and a micro gas heater 2 which are arranged at the front end of a carrier gas inlet 16; a carrier gas outlet 17 and a pressurizing port 15 are respectively positioned at the two sides of the carrier gas inlet 16; the solid source steel cylinder heating device, the temperature control system bottle body chassis heating device, the solid source steel cylinder heating insulation sleeve 3, the temperature probe 4 and the temperature heater 5 are connected to the temperature heating controller 6, and the heating, temperature monitoring and adjusting functions of the solid source steel cylinder are achieved.
FIG. 2 is a sectional view of a solid source steel cylinder, wherein a particle filter screen 9 is arranged at three interfaces of an upper sealing cover, a heating device of an upper sealing cover, a bottle body and a bottle body chassis are connected through flange bolts, a sealing ring groove 10 is formed at the flange connecting end of the upper sealing cover and the bottle body, a temperature probe hole 11 is formed at the lower end of the bottle body, a heater power supply through hole 14 is formed at the lower end of the heating device of the bottle body chassis, the section shows that a mosquito coil type carrier gas channel wall is designed to be a hollow channel wall 7, and a heater 8 of the heating device of the bottle body chassis is inserted into the hollow channel wall 7 from the bottom of the bottle body, so that a solid source can be heated most directly and efficiently.
Fig. 3 is a top view of a solid source steel cylinder body, a mosquito coil type carrier gas channel 13 is arranged in the cylinder body, the solid source is arranged in the carrier gas channel 13, the central position of the channel is a carrier gas inlet transition groove 18, and the tail end of the channel is a carrier gas outlet transition groove 12.
FIG. 4 is a top view of the bottle body chassis heating device, wherein the heater 8 is shaped like a mosquito coil and is in concave-convex surface socket fit with the carrier gas channel 7.
When the invention is used, a precursor HfCL4 solid source is filled in a mosquito coil type channel of a bottle body of a solid source steel bottle by taking a solid source such as hafnium tetrachloride (HfCL 4) as an example.
And sequentially arranging the upper sealing cover of the solid source steel cylinder and the heating device of the bottom plate of the cylinder body on the cylinder body of the solid source steel cylinder.
Helium is filled into the solid source steel cylinder body from the pressurizing port, and the sealing performance of the joint of the sealing cover on the solid source steel cylinder and the flange of the solid source steel cylinder body is detected by using a handheld helium detector.
And covering the solid source steel cylinder with a steel cylinder heat-insulating heating jacket.
And connecting a carrier gas inlet and a mixed vapor outlet to a pipeline of the vapor deposition system, wherein the carrier gas is introduced into the carrier gas inlet.
And the electric heating temperature control plate is electrified, the heating temperature of the heating device is set according to the temperature required by the saturated vapor pressure of HfCL4 for heating, the electric heating temperature control plate heats the solid precursor source in the storage tank, and when the heating temperature reaches the set temperature, the carrier gas inlet valve and the carrier gas outlet valve are opened to introduce carrier gas so as to bring the vapor of the solid precursor source into the vapor deposition system.
Although the invention has been described in detail with respect to the general description and the specific embodiments, it will be apparent to those skilled in the art that modifications and improvements may be made based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. A cylinder for a solid source of precursor, comprising: the solid source steel cylinder main body is connected with a heating temperature control system; the source steel cylinder body is internally provided with a carrier gas channel, the side wall of the carrier gas channel is provided with an opening facing the bottom of the solid source steel cylinder and communicated with the outside, and the carrier gas channel is spirally arranged from the center to the outside at equal intervals; the heating temperature control system is positioned at the bottom of the solid source steel cylinder main body and comprises heaters, the heaters are spirally arranged from the center to the outside at equal intervals, and the heaters correspond to the openings and extend into the openings.
2. The cylinder of claim 1, wherein the cylinder body comprises an upper cover, the upper cover is connected to a body, the upper cover is connected to a gas inlet, the gas inlet is connected to the body, and the body is connected to a heating and temperature control system.
3. The steel cylinder for the precursor solid source according to claim 1 or 2, wherein the heating temperature control system comprises an outer temperature control part, an inner temperature control part is connected to the inner lower end wall of the outer temperature control part, and the inner temperature control part is used for preheating and automatically adjusting the heating temperature of the carrier gas before the carrier gas is introduced; the heater is positioned at the top of the inner side temperature control part.
4. The cylinder of claim 2, wherein a sealing ring groove is provided between the upper cover and the body, the sealing ring groove being located on the corresponding surface of the upper cover and the body; the upper sealing cover is provided with an air passage penetrating through the upper sealing cover, and the tail end of the air passage is positioned at the bottom of the upper sealing cover and is provided with a particle filter screen.
5. The cylinder of claim 3, wherein the inner temperature control part comprises a heating controller, the heating controller is connected with a temperature heater and a temperature probe, the temperature probe is connected with a temperature probe hole, and the temperature probe hole is located between two adjacent openings; the temperature heater is positioned between two adjacent heaters.
6. The cylinder as claimed in claim 2 or 4, wherein the gas inlet includes a carrier gas inlet and a carrier gas outlet sequentially arranged on the top of the upper cover, the carrier gas inlet is connected with a micro gas heater, the micro gas heater is connected with a flow regulating valve, and the gas inlet further includes a pressurizing port.
7. The cylinder of claim 5, wherein the bottom of the cylinder body has a fixing hole facing the inner temperature control unit, and the inner temperature control unit has a fixing pin corresponding to the fixing hole.
8. The cylinder of claim 5, wherein the outer temperature control portion comprises a thermally insulated heating jacket, the source cylinder body being disposed within the thermally insulated heating jacket, the thermally insulated heating jacket being connected to a heating controller.
9. The cylinder as claimed in any one of claims 1 to 8, wherein the body of the cylinder is made of a material that meets the required cleanliness class of vapor deposition process when heated for use.
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| CN202211472550.4A CN115717681B (en) | 2022-11-18 | 2022-11-18 | Steel cylinder for precursor solid source |
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| CN115717681B (en) | 2023-12-29 |
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