CN109898058B - Combined crucible for improving stability of evaporation beam by utilizing saturated vapor pressure and source furnace with crucible - Google Patents
Combined crucible for improving stability of evaporation beam by utilizing saturated vapor pressure and source furnace with crucible Download PDFInfo
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Abstract
The invention discloses a combined crucible for improving the stability of an evaporation beam by utilizing saturated vapor pressure and a source furnace with the combined crucible, and belongs to the technical field of film growth. The combined crucible comprises a crucible upper part and a crucible lower part, wherein the crucible upper part is connected with the crucible lower part through a supporting table, a movable current limiting assembly is arranged on the supporting table, the movable current limiting assembly is a detachable device, and a current limiting hole is arranged on the movable current limiting assembly. According to the invention, the current limiting assembly is placed in the support table, so that the crucible loading area reaches saturated vapor pressure, the evaporation rate is controlled to be completely dependent on the crucible temperature which can be stably controlled, the influence of the surface appearance change of an evaporation source material on the evaporation beam in the growth process is avoided, and the beam stability is greatly improved to prepare a film with higher quality.
Description
Technical Field
The invention relates to the technical field of film growth, in particular to a combined crucible for improving the stability of an evaporation beam by utilizing saturated vapor pressure and a source furnace with the crucible.
Background
Environment, energy, life and new materials are four major issues facing human beings currently, wherein the research on new materials requires that atoms can be manipulated, and thin film technology is a key entry point for manipulating atoms. A representative means of the thin film technology is molecular beam epitaxial thin film growth, in which a thin film is grown by irradiating an atomic or molecular beam generated by evaporation from a heat source onto a heated clean substrate. The development of this technology is to achieve increasingly high requirements for the technology of electronic devices, i.e. to achieve thin-layer-oriented planar structures with precisely controllable doping profiles. With Molecular Beam Epitaxy (MBE), ultra-thin epitaxial layers can be repeatedly grown to a thickness of only 4 angstroms, and the interface between the epitaxial layers can be precisely controlled for growth.
The molecular beam epitaxial film growth technology is one of the advanced means for developing new materials, and the generated film is not simple accumulation of evaporant, but requires atoms of the evaporant to carry out epitaxial growth on a substrate with atom precision according to a predetermined order. The representative application is the growth of nano-structure bodies such as quantum wells and quantum dots, and the quantum wells are already used for manufacturing semiconductor lasers, artificial intelligence materials and large-capacity storage devices; quantum dots are applied to single electron triodes. High-performance molecular beam epitaxy evaporation sources are required for atomic-level film growth and new material development. Therefore, the control of the stability of the molecular beam is crucial to the growth of high-quality materials.
The molecular beam epitaxial growth is realized by placing high-purity elemental metal source materials into crucibles of different spraying sources according to different elements, heating to corresponding temperature under the action of an external resistance wire, spraying molecular flow when each element reaches high vapor pressure in the crucibles, adsorbing the sprayed molecules or atoms on the surface of the substrate after the sprayed molecules or atoms reach the surface of the substrate according to the sequence and quantity controlled by a baffle, transferring, rearranging and the like, and finally staying at proper positions to form an epitaxial film layer by layer. However, in the actual production and research process, the crucible can not reach saturated vapor pressure, the evaporation rate is proportional to the surface area of the evaporation source material, and the change of the surface topography of the evaporation source material in the film growth process has obvious influence on the beam flow stability, thereby limiting the control precision of the film growth and the quality of the prepared film. The continuous development of electronic technology also puts higher requirements on the film preparation precision, and prompts people to actively explore the stability of the evaporation source beam, so that the improvement of crucible design is urgently needed to further improve the stability of the evaporation beam.
Through retrieval, the name of the invention is: a novel split type carbon-carbon crucible (application number: 201410566140.5, application date: 2014-10-21) adopts a split type carbon-carbon crucible structure, the upper portion of a crucible side and the middle portion of the crucible side are made of carbon materials, a crucible bottom is made of graphite materials, the split type structure is mainly used for facilitating an operator to disassemble a quartz crucible, the labor intensity of the operator is reduced, the furnace disassembling time is saved, the production efficiency is improved, and the production cost is reduced, but the split type carbon-carbon crucible cannot be applied to a molecular beam epitaxial film generation technology.
In addition, the name of the invention is as follows: a low-temperature vacuum evaporation source (application No. 201720550756.2 application No.: 2017-05-17) comprising: the temperature measuring system comprises a heating system, a cooling system, a temperature measuring system, a control system and a connecting assembly; in the device, the electrode is electrified to heat the filament of the heating system, so that the evaporation of alkali metal and organic compounds is realized; a thermocouple of the temperature measuring system detects the real-time evaporation temperature through the conduction of a thermocouple wire, and cooling water is introduced into a water inlet pipe of the cooling system to achieve the effect of low-temperature evaporation; the rotary baffle plate on the crucible opening can be adjusted and controlled by a manual lever to control whether the evaporated substance coats the substrate or not; but does not address the issue of evaporation beam flow stability.
Disclosure of Invention
1. Technical problem to be solved by the invention
The invention aims to overcome the defect that beam current is unstable due to the fact that the surface appearance of an evaporation source material is changed easily in the film preparation technology, and provides a combined crucible for improving the stability of the evaporation beam current by utilizing saturated vapor pressure and a source furnace with the combined crucible;
the combined crucible for improving the stability of the evaporation beam by using the saturated vapor pressure ensures that a crucible loading area reaches stable saturated vapor pressure by arranging the detachable small-hole current limiting device, overcomes the influence of the surface appearance change of an evaporation source material on the beam in the growth process of the film, greatly improves the stability of the beam, and can prepare a film with higher quality;
according to the source furnace for improving the stability of the evaporation beam, the influence of the surface appearance change of an evaporation source material on the beam in the growth process of the film is overcome by controlling the saturated vapor pressure of a crucible charging area, so that the evaporation rate completely depends on the temperature which can be stably controlled, the stability of the beam is greatly improved, and the film with higher quality can be prepared.
2. Technical scheme
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the combined crucible for improving the stability of the evaporation beam current by utilizing the saturated vapor pressure is characterized in that the crucible is sequentially provided with the upper part of the crucible and the lower part of the crucible from top to bottom, the upper part of the crucible is connected with the lower part of the crucible through a supporting table, a movable current limiting assembly is arranged on the supporting table, a current limiting hole is arranged on the movable current limiting assembly, and the current limiting hole is vertical to the surface of the movable current limiting assembly.
Preferably, the diameter of the upper surface of the supporting table is d1, the radius of the lower surface of the supporting table is d2, d1 is greater than d2, and the movable flow limiting component is movably arranged on the upper surface of the supporting table.
Preferably, the material of the movable current limiting component is hot-pressed boron nitride, aluminum oxide or tungsten.
Preferably, the diameter of the flow limiting hole is dr, the radius of the lower surface of the support table is d2, and 10dr is less than d 2.
Preferably, the number of the flow limiting holes is 1, and the flow limiting holes are arranged at the circle center of the movable flow limiting assembly; or a plurality of flow limiting holes are arranged, and the flow limiting holes are uniformly arranged around the circle center along the movable flow limiting assembly.
Preferably, the upper part and the lower part of the crucible are of a straight cylinder structure, and the diameter of the upper part of the crucible is d1The diameter of the lower part of the crucible is d2，d1＞d2。
The source furnace for improving the stability of the evaporation beam current comprises a crucible, an evaporation source and a heating unit, wherein the crucible is arranged in the evaporation source, the heating unit is arranged outside the crucible and used for heating the crucible, and the crucible is the crucible.
Preferably, the crucible is provided with a support table, and the support table is provided with a movable current limiting assembly.
Preferably, a beam baffle is arranged in the opening direction of the crucible.
Preferably, the evaporation source comprises a protective housing and a fixing base, wherein the protective housing is internally provided with an accommodating cavity, the fixing base is arranged at the bottom of the accommodating cavity, and the fixing base is used for fixing the lower part of the crucible.
3. Advantageous effects
Compared with the prior art, the technical scheme provided by the invention has the following remarkable effects:
(1) according to the combined crucible for improving the stability of the evaporation beam by utilizing the saturated vapor pressure, the movable current limiting assembly is creatively arranged on the middle part of the crucible side, the crucible charging area is ensured to reach the stable saturated vapor pressure through the current limiting hole on the movable current limiting assembly, the influence of the surface appearance change of the evaporation source material on the beam in the existing film growth process is overcome, the evaporation rate completely depends on the temperature which can be stably controlled, and the stability of the beam is greatly improved so as to prepare a film with higher quality;
(2) according to the combined crucible for improving the stability of the evaporation beam current by utilizing the saturated vapor pressure, the diameter of the upper surface of the support table is d1, the radius of the lower surface of the support table is d2, and d1 is larger than d2, so that the combined crucible is used for supporting the movable current limiting assembly, when the epitaxial film is prepared, the movable current limiting assembly is placed on the upper surface of the support table, and the evaporation source material and the crucible can be conveniently added and cleaned;
(3) according to the source furnace for improving the stability of the evaporation beam, the influence of opening or closing the beam baffle on the stability of the beam is reduced, the beam is controlled more stably to prepare a film with higher quality, and the higher requirement of the development of modern electronic devices on the film technology is met.
Drawings
FIG. 1 is a schematic view of the overall structure of a composite crucible of the present invention for improving the stability of an evaporation beam by utilizing the saturated vapor pressure;
FIG. 2 is a schematic diagram of the overall structure of the movable current limiting assembly;
FIG. 3 is a schematic structural view of a support stage according to embodiment 1;
FIG. 4 is a schematic structural view of a flow restriction orifice of embodiment 1;
FIG. 5 is a schematic view of the overall structure of a source furnace for improving the stability of the evaporation beam current according to the present invention.
The reference numerals in the schematic drawings illustrate:
100. a crucible; 110. the upper part of the crucible; 120. the lower part of the crucible; 130. a support table;
200. a movable current limiting assembly; 210. a flow restriction orifice;
300. an evaporation source; 310. a protective outer cover; 311. an accommodating chamber; 320. a fixed base; 321. a temperature measuring element; 322. a base positioning cylinder;
400. a heating unit;
500. and (4) a beam baffle.
Detailed Description
The detailed description and exemplary embodiments of the invention will be better understood when read in conjunction with the appended drawings, where the elements and features of the invention are identified by reference numerals.
The structure, proportion, size and the like shown in the drawings are only used for matching with the content disclosed in the specification, so that the person skilled in the art can understand and read the description, and the description is not used for limiting the limit condition of the implementation of the invention, so the method has no technical essence, and any structural modification, proportion relation change or size adjustment still falls within the scope of the technical content disclosed by the invention without affecting the effect and the achievable purpose of the invention. Meanwhile, the terms such as "upper", "lower", "left", "right" and "middle" used in the present specification are for clarity of description only, and are not used to limit the implementable scope, and the relative relationship changes or adjustments may be considered to be within the implementable scope of the present invention without substantial technical changes; in addition, the embodiments of the present invention are not independent of each other, but may be combined.
Example 1
As shown in fig. 1 and 2, in the combined crucible for improving the stability of the evaporation beam by using the saturated vapor pressure according to the present invention, a crucible 100 is provided with an upper crucible portion 110 and a lower crucible portion 120 in this order from top to bottom; the crucible upper part 110 is connected with the crucible lower part 120 through the supporting table 130, the supporting table 130 is provided with a movable current limiting assembly 200, a bayonet is arranged at the contact part of the movable current limiting assembly 200 and the supporting table 130, the movable current limiting assembly 200 is provided with a current limiting hole 210, the current limiting hole 210 is perpendicular to the surface of the movable current limiting assembly 200, and the emergent angle of beam current is adjusted by adjusting the direction of the bayonet. The invention improves the stability of the beam flow based on the theory of reducing the heat radiation, creatively installs the movable current limiting component 200 in the crucible 100, ensures the huge steam pressure difference in the crucible 100 by arranging the current limiting hole 210 on the movable current limiting component 200, further improves the stability of the evaporation beam flow and prepares a film with higher quality.
As shown in figure 3 of the drawings,the diameter of the upper surface of the supporting table 130 is d1, the radius of the lower surface of the supporting table 130 is d2, d1 is more than d2, the upper part 110 and the lower part 120 of the crucible are in a straight cylinder structure, and the diameter d of the upper part 110 of the crucible is1Equal to the diameter d1 of the upper surface of the support 130 and the diameter d of the lower part 120 of the crucible2Equal to the radius d2, d of the lower surface of the support table 1301＞d2The support table 130 is used to support the movable current limiting assembly 200. In the process of preparing the film, the saturated vapor pressure of the film during growth is very small relative to the atmospheric pressure, and the movable current limiting assembly 200 is placed on the upper surface of the support table 130, so that the disassembling steps of the movable current limiting assembly 200 are simplified, and the addition of the evaporation source material and the cleaning of the crucible 100 are facilitated. In the existing molecular beam epitaxy technology, the diameter of the upper part of the crucible is equal to that of the lower part of the crucible, and the invention provides a technical scheme with different conception for solving the problem of how to prepare a film with higher quality.
The molecular beam epitaxial growth film material is a non-equilibrium growth, the growth process is mainly controlled by molecular beam and crystal surface reaction kinetics, the molecular beam control has great influence on the growth, namely the accuracy of the molecular beam control determines the quality of the grown film, namely the atomic arrangement order. In the growth process of the film, the temperature of the molecular beam strictly corresponds to the temperature of the material source, wherein the equilibrium vapor pressure is one of the important factors influencing the molecular beam, and the theoretical basis is as follows: when atoms or molecules are released from a surface in a liquid or solid phase by heating the evaporation material, the kinetic energy corresponding to the velocity component perpendicular to the surface must be greater than the binding potential energy that atoms or molecules have for their mutual attraction. The kinetic energy depends on the thermal motion of the molecules, and thus, increasing the heating temperature can increase the number of particles released. The evaporation rate is proportional to the number of evaporation particles. However, the evaporation process comes at the cost of consuming the internal energy of the object, and in order not to lower the temperature of the object, the heat energy must be replenished; in addition, additional work is performed during evaporation due to the volume expansion that occurs during the transition from liquid or solid to gaseous state.
It is worth explaining that the change of the surface morphology of the evaporation source material in the growth process has a great influence on the stability of the molecular beam, thereby affecting the quality and the electrical properties of the film and the devices thereof. With the consumption of the evaporation source material, if the surface of the evaporation source material is uneven, the surface area of the evaporation source material changes, which can cause 1% order of magnitude change of molecular beam and even larger change, and has direct influence on the physical properties of impurities, stoichiometric ratio and other factors, and the quality of the film is directly influenced. In open crucibles used in the prior art, ions evaporated from the source material leave the surface directly, without reaching a dynamic equilibrium.
The invention creatively provides a combined crucible design adopting a small-hole flow limiting device to stabilize molecular beam flow, and further, a flow limiting hole 210 is formed in the movable flow limiting assembly 200, the diameter of the movable flow limiting assembly 200 is d200, the diameter of the flow limiting hole 210 formed in the movable flow limiting assembly 200 is dr, and 10dr is less than d2 (as shown in fig. 4). The flow restriction holes 210 are uniformly distributed on the movable flow restriction assembly 200, and the flow restriction holes 210 may be disposed at the center of the movable flow restriction assembly 200 or symmetrically distributed along the center of the movable flow restriction assembly 200.
On one hand, the movable current limiting assembly 200 creates a relatively closed space for the crucible lower part 120, the saturated vapor pressure refers to the vapor pressure of the vapor phase when the dynamic balance between the vapor phase and the solid phase or between the vapor phase and the liquid phase is achieved, which can be achieved in the closed space generally, so as to ensure that the crucible charging area achieves stable saturated vapor pressure, overcome the influence of the surface appearance change of the evaporation source material on the beam in the existing film growth process, ensure that the evaporation rate completely depends on the temperature which can be stably controlled, and greatly improve the stability of the beam to prepare a film with higher quality; on the other hand, the diameter of the flow limiting hole 210 is far smaller than that of the lower part 120 of the crucible, so that huge steam pressure difference is realized in the upper and lower areas of the crucible 100 divided by the separation blade, the lower end is ensured to reach saturated steam pressure, the influence of the surface appearance change of an evaporation source material on the beam in the existing film growth process is overcome, the evaporation rate completely depends on the temperature which can be stably controlled, the stability of the beam is greatly improved to prepare a film with higher quality, and the higher requirement of the development of modern electronic devices on the film technology is met.
Further, the material of the movable current limiting assembly 200 is the same as that of the crucible 100, the material of the movable current limiting assembly 200 can be hot-pressed boron nitride, aluminum oxide or tungsten, the material has a smooth surface and good compactness, can work under ultrahigh vacuum, has stable physical and chemical properties, and does not react with the evaporation source material.
Example 2
As shown in fig. 5, the source furnace for improving the stability of the evaporation beam current of the embodiment includes a crucible 100, an evaporation source 300, and a heating unit 400, wherein the crucible 100 is disposed in the evaporation source 300, the heating unit 400 is disposed outside the crucible 100, the heating unit 400 is used for heating the crucible 100, the heating unit 400 is a resistance wire, and the crucible 100 is the crucible 100 of embodiment 1. A beam current baffle 500 (shown in fig. 3) is provided in the opening direction of the crucible 100. The invention accurately controls the layer-by-layer growth of the film by alternately opening and closing the beam baffles 500 at the top end of the crucible 100, and the change of the surface appearance of the evaporation source material can influence the beam stability, thereby influencing the quality and the electrical property of the film and devices thereof. According to the invention, by improving the crucible 100 in the MBE technology and using a brand-new technical scheme, more stable temperature and beam control are obtained, so that the influence of opening or closing the beam baffle 500 on the temperature stability is avoided, and the quality of the film is improved.
Further, the evaporation source 300 includes a protective housing 310 and a fixing base 320, wherein an accommodating cavity 311 is formed in the protective housing 310, the fixing base 320 is disposed at the bottom of the accommodating cavity 311, and the fixing base 320 is used for fixing the crucible lower part 120. The containing cavity 311 is used for containing the crucible 100, the inner diameter of the containing cavity 311 is larger than the outer diameter of the crucible 100, namely, the outer wall of the crucible 100 is not contacted with the containing cavity 311; the fixed base 320 is provided with a temperature measuring element 321, the temperature measuring element 321 is used for detecting the temperature of the crucible 100 so as to detect the temperature of the crucible 100 at any time, the fixed base 320 is provided with a base positioning cylinder 322, the base positioning cylinder 322 is used for being matched with the bottom of the crucible 100, the outer diameter of the base positioning cylinder 322 is smaller than the inner diameter of the accommodating cavity 311, and the base positioning cylinder 322 is not contacted with the inner wall of the accommodating cavity 311.
The invention has been described in detail hereinabove with reference to specific exemplary embodiments thereof. It will, however, be understood that various modifications and changes may be made without departing from the scope of the invention as defined in the appended claims. The detailed description and drawings are to be regarded as illustrative rather than restrictive, and any such modifications and variations are intended to be included within the scope of the present invention as described herein. Furthermore, the background is intended to be illustrative of the state of the art as developed and the meaning of the present technology and is not intended to limit the scope of the invention or the application and field of application of the invention.
More specifically, although exemplary embodiments of the invention have been described herein, the invention is not limited to these embodiments, but includes any and all embodiments modified, omitted, combined (e.g., between various embodiments), adapted and/or substituted as would be recognized by those skilled in the art from the foregoing detailed description. The limitations in the claims are to be interpreted broadly based the language employed in the claims and not limited to examples described in the foregoing detailed description or during the prosecution of the application, which examples are to be construed as non-exclusive. For example, in the present invention, the term "preferably" is not exclusive, and it means "preferably, but not limited to" herein. Any steps recited in any method or process claims may be executed in any order and are not limited to the order presented in the claims. The scope of the invention should, therefore, be determined only by the appended claims and their legal equivalents, rather than by the descriptions and examples given above.
Claims (8)
1. A combined crucible for improving the stability of an evaporation beam by utilizing the saturated vapor pressure is characterized in that: the crucible (100) is sequentially provided with an upper crucible part (110) and a lower crucible part (120) from top to bottom, the upper crucible part (110) is connected with the lower crucible part (120) through a support table (130), a movable flow limiting assembly (200) is arranged on the support table (130), a flow limiting hole (210) is arranged on the movable flow limiting assembly (200), and the flow limiting hole (210) is vertical to the surface of the movable flow limiting assembly (200); the diameter of the flow limiting hole (210) is dr, the radius of the lower surface of the support table (130) is d2, 10dr is less than d2, the flow limiting holes (210) are uniformly distributed on the movable flow limiting assembly (200), the number of the flow limiting holes (210) is 1, and the flow limiting holes (210) are arranged at the center of the circle of the movable flow limiting assembly (200); or a plurality of flow limiting holes (210) are arranged, and the flow limiting holes (210) are uniformly arranged around the circle center along the movable flow limiting assembly (200).
2. The combination crucible as claimed in claim 1, wherein the combination crucible is used for improving the stability of the evaporation beam flow by using the saturated vapor pressure, and is characterized in that: the diameter of the upper surface of the support table (130) is d1, the radius of the lower surface of the support table (130) is d2, d1 is larger than d2, and the movable current limiting assembly (200) is movably arranged on the upper surface of the support table (130).
3. The combination crucible as claimed in claim 1, wherein the combination crucible is used for improving the stability of the evaporation beam flow by using the saturated vapor pressure, and is characterized in that: the movable current limiting assembly (200) is made of hot-pressed boron nitride, aluminum oxide or tungsten.
4. A composite crucible as claimed in claim 2 or 3, wherein the combination crucible is used for improving the stability of the evaporation beam by using the saturated vapor pressure, and is characterized in that: the upper part (110) and the lower part (120) of the crucible are of a straight cylinder structure, and the diameter of the upper part (110) of the crucible is d1The diameter of the lower part (120) of the crucible is d2，d1＞d2。
5. A source furnace for improving the stability of an evaporation beam flow is characterized in that: the crucible (100) is arranged in the evaporation source (300), the heating unit (400) is arranged outside the crucible (100), the heating unit (400) is used for heating the crucible (100), and the crucible (100) is the crucible (100) according to any one of claims 1 to 4.
6. The source furnace for improving the stability of the evaporation beam current as claimed in claim 5, wherein: a supporting platform (130) is arranged on the crucible (100), and a movable current limiting assembly (200) is arranged on the supporting platform (130).
7. The source furnace for improving the stability of the evaporation beam current as claimed in claim 5, wherein: a beam baffle (500) is arranged in the opening direction of the crucible (100).
8. A source furnace for improving the stability of an evaporation beam flow according to any one of claims 5 to 7, wherein: the evaporation source (300) comprises a protective outer cover (310) and a fixed base (320), an accommodating cavity (311) is formed in the protective outer cover (310), the fixed base (320) is arranged at the bottom of the accommodating cavity (311), and the fixed base (320) is used for fixing the lower part (120) of the crucible.
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