CN114096016A - Vacuum heating device and method - Google Patents

Abstract

The application provides a vacuum heating device and a vacuum heating method, and belongs to the technical field of vacuum heating. The heating table main body of the vacuum heating device comprises: sample mount, electrically conductive base station and first heating element. The conductive base station is connected with an anode wire holder; the conductive base station is provided with a positioning part for bearing and fixing the sample fixing frame. The first heating assembly comprises a tungsten wire and tungsten wire electrodes connected to two ends of the tungsten wire; the tungsten filament is fixed on the conductive base station and is opposite to the sample fixing frame without contact. The vacuum heating method is carried out by adopting a vacuum heating device and comprises the following steps of heating a metal sample: tungsten wire electrodes at two ends of a tungsten wire are connected with a positive electrode and a negative electrode of a direct-current power supply, so that the tungsten wire carries out thermal radiation heating on the metal sample; when the required heating temperature is higher than 600 ℃, the method also comprises the step of connecting the anode wire holder with the anode of a high-voltage power supply and connecting the tungsten wire with the cathode of the high-voltage power supply so as to enable electrons escaping from the surface of the tungsten wire to bombard and heat the metal sample. The equipment is simple, the cost is low, and different heating modes can be adopted.

Description

Vacuum heating device and method

Technical Field

The application relates to the technical field of vacuum heating, in particular to a vacuum heating device and method.

Background

Scanning tunneling microscopy, as a scanning probe microscopy tool, allows scientists to view and locate individual atoms with much higher resolution than its atomic force microscope of its same type. In order to make it easier to observe the single atoms on the surface of the material, it is necessary to pre-treat the sample before observation, i.e. to anneal the sample substrate in a high vacuum state to refine the grains, adjust the texture, and eliminate the texture defects, so as to obtain a clean and flat substrate.

Molecular beam epitaxy is a special vacuum coating process, is a new technology for preparing single crystal thin films, and is a method for growing thin films layer by layer along the crystal axis direction of a substrate material under a proper substrate and proper conditions. By controlling the temperature of the substrate, the growth rate of the film and the beam intensity can be controlled, and the components and the doping concentration of the film can be rapidly adjusted along with the change of the source. By the technology, single crystal films as thin as tens of atomic layers can be prepared, and ultrathin quantum microstructure materials formed by alternately growing films with different components and different doping can be prepared.

At present, for the vacuum heating operation, a laser heating mode and a radio frequency heating technology are generally adopted, the equipment is complex and high in cost, and the heating mode is single.

Disclosure of Invention

The application aims to provide a vacuum heating device and a method, which have the advantages of simple equipment and low cost and can adopt different heating modes.

The embodiment of the application is realized as follows:

in a first aspect, an embodiment of the present application provides a vacuum heating apparatus, including a heating stage main body, the heating stage main body includes: sample mount, electrically conductive base station and first heating element.

The conductive base station is connected with an anode wire holder; the conductive base station is provided with a positioning part for bearing and fixing the sample fixing frame.

The first heating assembly comprises a tungsten wire and tungsten wire electrodes connected to two ends of the tungsten wire; the tungsten filament is fixed on the conductive base station and is distributed in a non-contact way opposite to the sample fixing frame.

In the technical scheme, the tungsten wire and the tungsten wire electrode are arranged in the first heating assembly, and the anode wire holder is arranged on the conductive base platform, so that the structure is simple, and the cost is low. When the required heating temperature is lower, tungsten filament electrodes at two ends of a tungsten filament can be connected with the positive electrode and the negative electrode of a direct current power supply to carry out heat radiation heating; when the required heating temperature is higher, the anode wire holder is connected with the anode of the high-voltage power supply, and the tungsten filament is connected with the cathode of the high-voltage power supply to carry out electron bombardment heating, so that the heating table main body has different heating modes and can reach higher heating temperature.

In some embodiments, at least one of the following conditions (a) and (b) is satisfied: (a) the diameter of the tungsten filament is 0.2 mm-0.5 mm; (b) the tungsten wire extends along a helical path.

In the technical scheme, the tungsten filament is arranged according to a proper diameter specification and an extension path, and has a proper electron escape amount when being connected with a high-voltage power supply, so that a better bombardment heating effect is ensured.

In some embodiments, the sample holder comprises a first sample holder comprising a first sample carrying floor, a first sample pressing tab, and a first fastener; the first sample bearing bottom plate is used for placing and fixing the first sample bearing bottom plate on the positioning part, and a heating hole is formed in the middle of the first sample bearing bottom plate in a penetrating mode; the first fastener is used for fastening and connecting the first sample pressing sheet and the first sample carrying bottom plate.

In the technical scheme, the sample rack is simple in arrangement mode, and the sample is convenient to take, place and fix. Wherein, the sample is conveniently exposed in the setting of heating hole, conveniently carries out heat radiation and bombardment heating to the sample.

In some embodiments, the heating stage body further comprises a second heating assembly, the second heating assembly comprises a brush and a brush electrode connected to one end of the brush, the brush is fixed on one side of the conductive base platform, which faces away from the tungsten filament, and the other end of the brush is used for electrically contacting with the sample fixing frame.

In the technical scheme, the electric brush is arranged to be matched with the conductive base station, the direct-current power supply is connected between the electric brush and the conductive base station, the semiconductor can be heated quickly, the heating mode of the heating station main body is more diversified, and the heating of samples made of different materials can be better realized.

In some embodiments, the sample holder comprises a second sample holder, the second sample holder comprises a second sample-bearing bottom plate, a sample-supporting plate, a second sample-pressing plate and a second fastening piece, the second sample-bearing bottom plate is used for placing and fixing on the positioning portion, and the second fastening piece is sequentially arranged through the second sample-pressing plate, the sample-supporting plate and the second sample-bearing bottom plate; the sample support plate close to the electric brush comprises a flat plate part and a protruding part, and the protruding part is arranged at the top of the flat plate part in a protruding mode and is used for being in electric contact with the electric brush.

Optionally, the top of both ends of the protruding part in the length direction is provided with a chamfer structure.

Optionally, the chamfer structure satisfies at least one of the following conditions (c) to (e): (c) the included angle between the inclination direction of the chamfer structure and the length direction of the convex part is 10-30 degrees; (d) the ratio of the length of the chamfer structure in the inclined direction to the length of the bulge is (1-2): 10; (e) in the inclination direction of the chamfering structure, arc transition areas are arranged at two ends of the chamfering structure, and the distribution range of each arc transition area in the chamfering structure accounts for 10% -20%.

In the technical scheme, the sample rack is simple in arrangement mode, and the sample is convenient to take, place and fix. Wherein, the setting up of bulge is convenient to contact with the brush, and the convenience is through heating semiconductor sample fast to the brush.

Further, all be provided with the chamfer structure at the both ends top of bulge to dispose the chamfer structure according to certain requirement, be used for leading the dynamic fit of brush and bulge, so that the two can be better dynamic fit.

In some embodiments, the vacuum heating apparatus further comprises a mounting body; the mounting main body comprises a mounting base, a corrugated pipe and a connecting piece; the mounting base is provided with a fixed frame and a movable frame; the first end of the corrugated pipe is connected with the fixed frame and is provided with an installation piece which is used for being hermetically connected and communicated with the vacuum chamber; the second end of the corrugated pipe is connected with the movable frame; the connecting piece is arranged in the corrugated pipe in a penetrating mode, one end of the connecting piece is connected with the second end of the corrugated pipe, and the other end of the connecting piece penetrates out of the first end of the corrugated pipe and is connected with the conductive base station.

In above-mentioned technical scheme, through the control remove can the drive of frame connect in the electrically conductive base station of connecting piece, conveniently adjust the position of electrically conductive base station according to the heating needs. The corrugated pipe has good deformation adaptability, so that a vacuum environment can be well maintained in the heating vacuum cavity and the corrugated pipe.

In some embodiments, the movable rack is provided with a first driving member, a second driving member and a third driving member, the first driving member is used for driving the second end of the corrugated pipe to move in a first preset direction, the second driving member is used for driving the second end of the corrugated pipe to move in a second preset direction, and the third driving member is used for driving the second end of the corrugated pipe to move in a third preset direction; the first preset direction is the direction in which the fixed frame points to the movable frame; the second preset direction and the third preset direction are perpendicular to each other and both perpendicular to the first preset direction.

Optionally, the moving rack satisfies at least one of the following conditions (f) to (h): (f) the first driving piece is a screw rod driving structure; (g) the second driving piece is a micrometer handle; (h) the third driving piece is a micrometer handle.

In the technical scheme, the movable frame can drive the second end of the corrugated pipe to move in a three-axis three-dimensional coordinate system of an X, Y, Z shaft, so that the position can be adjusted conveniently and flexibly.

Further, the driving piece in the movable frame is provided with a specific driving form, so that the movable frame has proper adjusting precision in all directions and can better adapt to the adjusting requirement.

In some embodiments, the connector is rotatably connected to the second end of the bellows; the vacuum heating device also comprises a rotating mechanism, and the rotating mechanism is in transmission connection with the connecting piece.

In above-mentioned technical scheme, slewing mechanism's setting is convenient for control connection spare drive electrically conductive base station and is rotated, can heat and observe better.

In a second aspect, embodiments of the present application provide a vacuum heating method, which is performed by using the vacuum heating apparatus as provided in the first aspect.

The vacuum heating method comprises the following steps of heating a metal sample, wherein the heating of the metal sample comprises the following steps: tungsten wire electrodes at two ends of a tungsten wire are connected with the positive electrode and the negative electrode of a direct current power supply, so that the tungsten wire carries out thermal radiation heating on the metal sample; when the required heating temperature is higher than 600 ℃, the method also comprises the steps of connecting the anode wire holder with the anode of a high-voltage power supply and connecting the tungsten wire with the cathode of the high-voltage power supply so as to enable electrons escaping from the surface of the tungsten wire to bombard and heat the metal sample; optionally, the voltage of the high voltage power supply is 500V to 1000V.

In the technical scheme, when the required heating temperature is low, tungsten wire electrodes at two ends of a tungsten wire are connected to the positive electrode and the negative electrode of a direct-current power supply to carry out heat radiation heating; when the required heating temperature is higher, the anode wire holder and the tungsten filament are connected with a high-voltage power supply to perform bombardment heating by superposing a high-voltage electric field, the equipment is simple, the cost is low, different heating modes are provided, and higher heating temperature can be achieved.

In some embodiments, the vacuum heating apparatus is configured to: the heating table main body further comprises a second heating assembly, the second heating assembly comprises an electric brush and an electric brush electrode connected to one end of the electric brush, the electric brush is fixed on one side, back to the tungsten filament, of the conductive base table, and the other end of the electric brush is in electric contact with the sample fixing frame.

The vacuum heating method further includes heating the semiconductor sample, the heating the semiconductor sample including: and connecting the positive electrode and the negative electrode of the direct current power supply to the positive electrode wire holder and the electric brush electrode for heating the semiconductor sample.

In the technical scheme, the electric brush is arranged to heat the semiconductor sample, so that the semiconductor is heated quickly, the heating method is diversified, and the samples made of different materials can be heated better.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.

Fig. 1 is a schematic structural diagram of a vacuum heating apparatus provided in an embodiment of the present application at a first viewing angle;

fig. 2 is a schematic structural diagram of a vacuum heating apparatus provided in an embodiment of the present application at a second viewing angle;

fig. 3 is a partial schematic structural diagram of a vacuum heating apparatus provided in an embodiment of the present application at a first viewing angle;

fig. 4 is a partial structural schematic view of a vacuum heating apparatus provided in an embodiment of the present application at a second viewing angle;

FIG. 5 is a schematic structural diagram of a first sample holder according to an embodiment of the present disclosure;

FIG. 6 is a schematic structural diagram of a second sample holder according to an embodiment of the present disclosure;

fig. 7 is a sectional view of a rotating mechanism provided in an embodiment of the present application.

Icon: 10-vacuum heating device; 100-heating table body; 110-a sample holder; 111-a first sample holder; 1111-a first sample carrying backplane; 1112-first sample tableting; 1113-first fastener; 112-a second sample holder; 1121-second sample support floor; 1122-sample support plate; 11221-a flat plate portion; 11222-a projection; 11223-chamfer structure; 1123-second sample pellet; 1124-a second fastener; 1125-an insulator; 1126-height adjustment; 1127-molybdenum nuts; 120-a conductive submount; 121-anode wire holder; 122-a positioning section; 1221-sample holder chute; 1222-sample holder tabletting; 130-a first heating assembly; 131-tungsten filament; 132-tungsten wire electrode; 140-a second heating assembly; 141-a brush; 142-brush electrodes; 150-a bottom plate; 160-a connecting structure; 200-a mounting body; 210-mounting a base; 211-a holder; 212-a mobile rack; 2121-a first drive member; 2122-a second drive member; 2123-a third drive; 220-a bellows; 221-a mount; 230-a connector; 300-a rotation mechanism; 301-connecting flange; 302-central rotating shaft; 303-bearing sleeves; 304-external magnet holder; 305-internal magnet holder; 306-a sleeve; 307-tail fixation ring; 308-an external magnet; 309-internal magnet; a-a metal substrate; b-a semiconductor substrate.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations.

Thus, the following detailed description of the embodiments of the present application, presented in the accompanying drawings, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.

In the description of the present application, it is to be noted that the terms "center", "upper", "lower", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on orientations or positional relationships shown in the drawings or orientations or positional relationships conventionally laid out when products of the application are used, and are only used for convenience in describing the application and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the application. Furthermore, the terms "first," "second," and the like are used merely to distinguish one description from another, and are not to be construed as indicating or implying relative importance.

Furthermore, the terms "parallel", "vertical" and the like do not imply that the components are required to be absolutely horizontal or overhanging, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.

In the description of the present application, it is further noted that, unless expressly stated or limited otherwise, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present application can be understood in a specific case by those of ordinary skill in the art.

The inventor finds that the electric heating wire is adopted for heating, the equipment is simple, and the cost is low. However, the electric heating wire is generally used at a low temperature, and the metal material is generally not heated to the baking temperature. Further research shows that when the electric heating wire is used for heating, the electric heating wire made of specific materials is selected, and a proper electric field is added between the electric heating wire and a sample, so that electrons can effectively escape from the surface of the electric heating wire to bombard and heat the material, and the achievable heating temperature can be effectively increased.

Referring to fig. 1 to 4, in a first aspect, an embodiment of the present application provides a vacuum heating apparatus 10 including a heating stage main body 100. The heating stage main body 100 is used for placing into a vacuum chamber to heat a sample, and the heating stage main body 100 includes a sample holder 110, a conductive base 120, and a first heating assembly 130.

The conductive base 120 is connected with an anode wire holder 121; the conductive base 120 is provided with a positioning portion 122 for supporting and fixing the sample holder 110. The first heating assembly 130 includes a tungsten wire 131 and tungsten wire electrodes 132 connected to both ends of the tungsten wire 131; the tungsten filament 131 is fixed on the conductive base 120 and disposed opposite to the sample holder 110 in a non-contact manner, that is, the tungsten filament 131 and the sample holder 110 are disposed opposite to each other and do not contact each other. The tungsten filament 131 and the sample holder 110 are not in contact with each other, and may be distributed with a gap therebetween, or may be distributed with a spacer disposed therebetween; in the case where the spacer is provided, the material of the spacer is, for example, molybdenum or tantalum, which has a high thermal conductivity.

The conductive base 120 has a plate-like structure as a whole, and the top thereof serves as a table top. The conductive base 120 is made of a conductive material to realize the conductive function. As an example, the conductive base 120 is machined from molybdenum. The molybdenum has higher hardness and better supporting effect; the molybdenum has low thermal expansion coefficient, high melting point (up to 2662 ℃) and high thermal conductivity, namely has good high temperature resistance and thermal conductivity, and can be better applied to a heating structure.

The positioning portion 122 has a function of supporting the sample holder 110, for example, has a sample holder sliding slot 1221 opened on the conductive base 120, and is used for slidably accommodating the sample holder 110 therein. The positioning portion 122 also has a function of fixing the sample holder 110, and for example, is provided with a sample holder pressing piece 1222 corresponding to the slide slot for pressing the sample holder 110 in the sample holder slide slot 1221. As an example, the sample holder pressing piece 1222 is made of a tantalum sheet, has good toughness, and can fix the sample holder 110 with a certain friction force, so that the sample holder 110 can be stably fixed in the sample holder sliding groove 1221 when the heating stage main body 100 rotates during the heating process.

The tungsten wire 131 is fixed to the conductive base 120 in an unlimited manner, and is fixed below the conductive base 120 by, for example, a molybdenum screw and a molybdenum nut 1127, and is disposed opposite to the sample holder sliding groove 1221 in the positioning portion 122 thereof.

In the present application, the tungsten wire 131 and the tungsten wire electrode 132 are disposed in the first heating element 130, and the anode wire holder 121 is disposed on the conductive base 120, which has a simple structure and a low cost, and has different heating methods and can reach a high heating temperature. The heating principle of the heating table main body 100 is as follows:

when the required heating temperature is lower (for example, less than or equal to 600 ℃), the tungsten wire electrodes 132 at the two ends of the tungsten wire 131 are connected with the positive electrode and the negative electrode of the direct-current power supply, so that the tungsten wire 131 can be used for conveniently heating the sample by heat radiation. The tungsten filament 131 has high melting point, low escape attack, small evaporation rate, stable heat emission and good ion bombardment resistance, and when the required heating temperature is higher (for example, more than 600 ℃), the anode wire holder 121 is connected with the anode of a high-voltage power supply, and the tungsten filament 131 is connected with the cathode of the high-voltage power supply, so that an electric field is superposed between the tungsten filament 131 and a sample, and electrons escaping from the surface of the tungsten filament 131 can bombard and heat the sample (metal sample, semiconductor sample such as silicon chip and the like); wherein, under the condition that the voltage of the high-voltage power supply is 500V-1000V, the maximum heating temperature can reach more than 1000 ℃ and even more than 1200 ℃.

As an example, the tungsten wire 131 may have a diameter of 0.2mm to 0.5mm, or 0.3mm to 0.4mm, and a cargo space of 0.35mm to 0.4mm, for example, 0.375 mm. The tungsten filament 131 with the specification has proper electron escape amount when being connected with a high-voltage power supply, and better bombardment heating effect is ensured; meanwhile, the tungsten wire 131 with the specification is convenient to process and form.

As an example, the tungsten wire 131 extends along a spiral path, which is, for example, a double-wound structure and has an elliptical shape in cross section; wherein the central axis of the helical path is optionally parallel to the surface of the conductive submount 120. The tungsten filament 131 has a proper distribution density and a large corresponding area with the conductive base 120, and has a proper electron escape amount when a high-voltage power supply is connected, so that a good bombardment heating effect is ensured.

In view of the above-described heating stage main body 100 provided by the present application, the heating of the metal sample can be preferably performed mainly by the heat radiation heating and the bombardment heating of the first heating member 130. In actual operation, sometimes the semiconductor needs to be heated, so a heating assembly capable of rapidly heating the semiconductor sample is added to the heating table main body 100, so that the heating mode of the heating table main body 100 is more diversified, and the heating of samples of different materials can be better realized.

As an example, the heating stage main body 100 further includes a second heating assembly 140, the second heating assembly 140 includes a brush 141 and a brush electrode 142 connected to one end of the brush 141, the brush 141 is fixed to a side of the conductive base 120 facing away from the tungsten wire 131, and is fixed above the conductive base 120 and insulated from the conductive base by alumina ceramic, for example; the other end of the brush 141 is used for electrical contact with the sample holder 110. When the semiconductor sample needs to be heated, the sample holder 110 is fixed to the positioning portion 122, so that the brush 141 and the sample holder 110 are electrically contacted, and then the positive and negative poles of the dc power supply are connected to the positive electrode holder 121 and the brush electrode 142, so as to rapidly heat the semiconductor sample.

Since the brush 141 and the sample holder 110 are in dynamic contact at the stage of relative movement of the sample holder 110, and the like, and the high-temperature environment is handled under the working state, optionally, the brush 141 is formed by laser cutting a tantalum sheet. The tantalum has high melting point (reaching 2995 ℃), moderate hardness, high ductility, small thermal expansion coefficient and extremely high corrosion resistance, and can better adapt to the working environment and meet the working requirements.

In the present application, the sample holder 110 is not limited to be disposed in any manner as long as the sample can be taken, placed and fixed. In the present application, the number of the sample holders 110 is also not limited, and may be set to one or more. The structures of the plurality of sample holders 110 may be the same, and may be used to hold a plurality of identical samples to be heated; the plurality of sample holders 110 may also have different structures, and may be used to hold a plurality of different samples to be heated, such as a metal sample and a semiconductor sample, respectively.

Referring to fig. 5, as a first example, the sample holder 110 includes a first sample holder 111, which is exemplarily used for holding a metal sample. Such as a metal substrate a. The first sample holder 111 includes a first sample carrying base plate 1111, a first sample pressing plate 1112, and a first fastening member 1113. The first sample-bearing bottom plate 1111 is used for placing and fixing on the positioning portion 122; the middle part of the sample box is provided with a heating hole in a penetrating way, so that the sample can be conveniently exposed, and the sample can be conveniently heated by heat radiation and bombardment. The first fastener 1113 is used to fasten the first sample wafer 1112 and the first sample carrying base 1111.

Referring to fig. 6, as a second example, the sample holder 110 further includes a second sample holder 112, which is illustratively used to hold semiconductor samples. Such as semiconductor substrate B. The sample holder 110 includes a second sample holder 112, the second sample holder 112 includes a second sample supporting bottom plate 1121, a sample supporting plate 1122, a second sample pressing plate 1123 and a second fastening member 1124, and the second fastening member is sequentially inserted through the second sample pressing plate 1123, the sample supporting plate 1122 and the second sample supporting bottom plate 1121. The second sample support bottom plate 1121 is used for placing and fixing to the positioning portion 122, and the sample support plate 1122 and the second sample wafer 1123 are used for holding the semiconductor substrate B. The sample support plate 1122 near the brush 141 includes a flat plate portion 11221 and a projection 11222, and the second sample pad 1123 is attached to the top of the flat plate portion 11221; the protruding portion 11222 protrudes from the top of the flat plate portion 11221 and is used for electrically contacting the brush 141, so that the semiconductor sample can be heated quickly by the brush 141.

Wherein, in each sample holder 110: the sample support floor 150 is illustratively slidably received in the sample rack chute 1221 and secured by the sample rack preforms 1222, the sample support floor 150 being machined from, for example, molybdenum; the sample preforms are arranged, for example, in two, which are arranged opposite one another and are each machined, for example, from tantalum sheets.

In the first sample holder 111, the first fastener 1113 only needs to fasten the first sample pressing plate 1112 and the first sample carrying base plate 1111, which is, for example, a screw structure, such as a molybdenum screw.

In the second sample holder 112, on the side close to the brush 141, the top of the second sample wafer 1123 is provided with, for example, an insulator 1125 for insulation; the insulator 1125, such as an alumina ceramic spacer, fits over the second fastener 1124 and is pressed against the top of the second sample wafer 1123 by the second fastener 1124. Further, in order to maintain the balance of the height, the second sample wafer 1123 of the other side is provided with a height adjusting member 1126; the height adjustment member 1126 is, for example, a molybdenum shim, optionally positioned on the top or bottom of the second sample wafer 1123, and secured by a corresponding second fastener 1124. Since the second fastening member 1124 is required to fasten and connect the sample support plate 1122, the second sample pressing sheet 1123, the second sample supporting bottom plate 1121, the insulating member 1125, the height adjusting member 1126, etc., it is, for example, a stud structure, such as a molybdenum stud, in order to achieve good connection; furthermore, a nut is arranged to be matched with the molybdenum stud, such as the molybdenum nut 1127, so that the fastening connection effect of the molybdenum stud is guaranteed, and shaking can be effectively prevented.

Because the sample holder 110 and the brush 141 are in dynamic contact during relative movement such as mounting the sample holder 110, and the brush 141 made of tantalum sheet has strong toughness, the brush 141 is usually deviated downward by a small angle to ensure good close contact between the two. In order to facilitate the brushes 141 to be in good dynamic contact with the protruding portion 11222, as an example, both end tops of the protruding portion 11222 in the length direction are provided with chamfered structures 11223, which facilitate guiding the sliding movement of the brushes 141 located at both ends of the top of the protruding portion 11222 toward the middle of the top end of the protruding portion 11222.

As an example, the chamfered structure 11223 satisfies at least one of the following conditions: an included angle between the inclined direction of the chamfered structure 11223 and the length direction of the protruding portion 11222 is 10-30 degrees, for example, the included angle is 20 degrees; the ratio of the length of the chamfered structure 11223 in the oblique direction to the length of the protrusion 11222 is (1-2): 10, for example, the ratio is 1: 10; in the inclined direction of the chamfered structure 11223, both ends of the chamfered structure 11223 have arc transition areas, and each arc transition area is distributed in the chamfered structure 11223 in a range of 10% to 20%, for example, 10%. It is understood that, in the present application, the direction of inclination of the chamfer structure 11223 refers to the direction in which the chamfer starting end points to the chamfer ending end.

In the present application, the heating table main body 100 may be provided with other structures as needed, for example, the heating table main body 100 may be further provided with a bottom plate 150 and a connecting structure 160 for facilitating installation of the heating table main body 100 in a working environment. The bottom plate 150 is disposed at the bottom of the conductive base 120, and is used for mounting the conductive base 120; a support column is connected between the bottom plate 150 and the conductive base 120 for supporting the conductive base 120. The connection structure 160 is, for example, a connection screw, which is optionally processed from SUS304, and the connection portion thereof is a screw of M6, which facilitates assembly.

It is understood that, in the present application, in order to facilitate the installation or driving of the heating table main body 100 to better adapt to the heating requirement in the vacuum cavity, the vacuum heating apparatus 10 may further be provided with an installation structure and/or a driving structure as required.

In some alternative embodiments, the vacuum heating apparatus 10 further includes a mounting body 200, and the mounting body 200 includes a mounting base 210, a bellows 220, and a connector 230.

The mounting base 210 is provided with a fixed frame 211 and a movable frame 212.

A first end of the bellows 220 is connected to the fixing frame 211, and is provided with a mounting member 221 for hermetically connecting and communicating with the vacuum chamber; the mounting 221 is, for example, a CF35 flange, the CF35 flange sealing the connection to the vacuum chamber, for example, by an oxygen-free copper gasket. The second end of the bellows 220 is connected to the moving frame 212 for following the movement of the moving frame 212.

A connection 230, illustratively a cylindrical connecting rod, is disposed through the bellows 220. One end of the connection member 230 is connected to the second end of the bellows 220 for following the movement of the second end of the bellows 220; the other end of the connecting member 230 passes through the first end of the bellows 220 and is connected to the conductive base 120, for example, the connecting structure 160 of the heating stage main body 100 is connected to the conductive base 120.

In the above technical solution, the second end of the corrugated tube 220 can move along with the moving frame 212, the connecting member 230 can move along with the second end of the corrugated tube 220, and the conductive base 120 connected to the connecting member 230 can be driven by controlling the moving frame 212, so that the position of the conductive base 120 can be conveniently adjusted according to the heating requirement. The bellows 220 has a good deformation adaptability, so that a vacuum environment can be well maintained in the heating vacuum cavity and the bellows 220 when the position of the conductive base station 120 is adjusted.

It is understood that the direction and manner of the moving member moving the second end of the bellows 220 and the connecting member 230 are not limited, and can be selected according to the requirement.

As an example, the moving frame 212 is provided with a first driving element 2121, a second driving element 2122 and a third driving element 2123, wherein the first driving element 2121 is used for driving the second end of the bellows 220 to move in a first preset direction, the second driving element 2122 is used for driving the second end of the bellows 220 to move in a second preset direction, and the third driving element 2123 is used for driving the second end of the bellows 220 to move in a third preset direction. Wherein, the first predetermined direction is a direction in which the fixed frame 211 points to the movable frame 212; the second preset direction and the third preset direction are perpendicular to each other and both perpendicular to the first preset direction. The arrangement mode enables the moving frame 212 to drive the second end of the bellows 220 to move in the X, Y, Z-axis three-dimensional coordinate system, so that the position adjustment is convenient and flexible.

Optionally, the first driving member 2121 is a screw driving structure, the second driving member 2122 is a micrometer handle, and the third driving member 2123 is a micrometer handle, which has suitable adjustment precision in various directions, and can better adapt to the adjustment requirement.

In some alternative embodiments, the vacuum heating apparatus 10 further comprises a connecting member 230 rotatably connected to the second end of the bellows 220; the vacuum heating apparatus 10 further comprises a rotating mechanism 300, wherein the rotating mechanism 300 is in transmission connection with the connecting member 230. The rotation mechanism 300 is provided to facilitate the control connection member 230 to drive the conductive base 120 to rotate, so as to better perform heating and observation. Wherein, through direct drive connecting piece 230 pivoted mode, compare with drive bellows 220 drive connecting piece 230 pivoted mode, still be favorable to avoiding bellows 220 to lead to the problem that bellows 220 leaks gas, life shortens easily because of multi-angle rotating.

In the present application, the rotating mechanism 300 is not limited to be disposed, and is, for example, a magnetic rotating shaft.

Referring to fig. 7, the magnetic shaft includes a connection flange 301, a central shaft 302, a bearing housing 303, an outer magnet holder 304, an inner magnet holder 305, a shaft housing 306, a tail fixing ring 307, an outer magnet 308, an inner magnet 309, and a connection rod.

Wherein the connecting flange 301 is, for example, a CF35 flange, for connecting with the second end of the bellows 220. The central rotating shaft 302 is rotatably arranged in the connecting flange 301 in a penetrating way; the central rotating shaft 302 comprises a first shaft section and a second shaft section, wherein the first shaft section is positioned on one side of the connecting flange 301 close to the corrugated pipe 220 and is connected with the connecting piece 230; the second shaft section is located on one side of the connecting flange 301 far away from the bellows 220 and is sleeved in the shaft sleeve 306. The inner magnet holder 305 is sleeved outside the second shaft section and is made of, for example, SUS430 magnetic stainless steel; the internal magnet 309 is disposed within the internal magnet holder 305. The external magnet holder 304 is sleeved outside the internal magnet holder 305, and is made of, for example, SUS430 magnetic stainless steel; the external magnet 308 is disposed in the external magnet holder 304 and corresponds to the internal magnet 309.

The tail fixing ring 307 is optionally processed with a screw hole for passing a screw member such as a screw to fix the shaft and the outer sleeve of the magnetic shaft relatively. When the rotating shaft rotates to a certain fixed angle, the rotating shaft and the outer sleeve are relatively fixed by the hand-screwed screw, so that the heating table main body 100 maintains a certain fixed angle.

In a second aspect, embodiments of the present application provide a vacuum heating method, which is performed by using the vacuum heating apparatus 10 as provided in the first aspect.

The vacuum heating method comprises the following steps of heating a metal sample, wherein the heating of the metal sample comprises the following steps:

when the required heating temperature is lower (for example, less than or equal to 600 ℃), the tungsten wire electrodes 132 at the two ends of the tungsten wire 131 are connected with the positive electrode and the negative electrode of the direct-current power supply, so that the tungsten wire 131 carries out heat radiation heating on the metal sample. By controlling the current of the direct current power supply, different metal samples can be heated, and the highest heating temperature can reach 600 ℃.

When the required heating temperature is higher (for example, more than 600 ℃, especially more than 1000 ℃), the method also comprises the steps of connecting the positive electrode of the high-voltage power supply to the anode wire holder 121 and connecting the negative electrode of the high-voltage power supply to the tungsten wire 131, so that electrons escaping from the surface of the tungsten wire 131 bombard and heat the metal sample. It can be understood that the high-voltage power supply is connected to the positive electrode of the positive electrode wire holder 121, and the high-voltage power supply is connected to the negative electrode of the tungsten filament 131, which means that the tungsten filament electrodes 132 at the two ends of the tungsten filament 131 are kept connected to the positive and negative electrodes of the direct-current power supply, that is, a high-voltage electric field is superimposed while the tungsten filament 131 is heated by direct-current thermal radiation.

Optionally, the voltage of the high-voltage power supply is 500V to 1000V, or 600V to 1000V, or 700V to 900V, or 800V, and the high-voltage electric field of the specific standard enables the tungsten filament 131 to have a proper electron emission amount, so that a good bombardment heating effect is ensured, and the maximum heating temperature can reach more than 1000 ℃ and even more than 1200 ℃.

Where the heat block assembly is further configured with a second heating assembly 140 and associated structures, the vacuum heating method further includes heating the semiconductor sample. The operation of heating the semiconductor sample includes: the positive and negative poles of the dc power supply are connected to the positive electrode holder 121 and the brush electrode 142, and heat the semiconductor sample. Since the semiconductor resistance is large, when the positive and negative poles of the dc power supply are connected to the positive electrode holder 121 and the brush electrode 142, the semiconductor sample can be heated quickly.

The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. A vacuum heating apparatus, comprising a heating stage main body, the heating stage main body comprising:

a sample holder;

the conductive base station is connected with an anode wire holder; the conductive base station is provided with a positioning part for bearing and fixing the sample fixing frame; and

the first heating assembly comprises a tungsten wire and tungsten wire electrodes connected to two ends of the tungsten wire; the tungsten filament is fixed on the conductive base station and is distributed in a non-contact manner relative to the sample fixing frame.

2. The vacuum heating apparatus according to claim 1, wherein at least one of the following conditions (a) and (b) is satisfied:

(a) the diameter of the tungsten wire is 0.2 mm-0.5 mm;

(b) the tungsten wire extends along a helical path.

3. The vacuum heating apparatus according to claim 1, wherein the sample holder comprises a first sample holder comprising a first sample carrying base plate, a first sample pressing sheet, and a first fastener; the first sample bearing bottom plate is used for placing and fixing the first sample bearing bottom plate on the positioning part, and a heating hole is formed in the middle of the first sample bearing bottom plate in a penetrating mode; the first fastener is used for fastening and connecting the first sample pressing sheet and the first sample carrying bottom plate.

4. The vacuum heating apparatus according to claim 1, wherein the heating stage main body further comprises a second heating unit, the second heating unit comprises a brush and a brush electrode connected to one end of the brush, the brush is fixed to a side of the conductive base opposite to the tungsten wire, and the other end of the brush is used for electrically contacting with the sample holder.

5. The vacuum heating apparatus according to claim 4, wherein the sample holder comprises a second sample holder, the second sample holder comprises a second sample-bearing bottom plate, a sample-supporting plate, a second sample-pressing plate and a second fastening member, the second sample-bearing bottom plate is used for placing and fixing on the positioning portion, and the second fastening member is sequentially inserted through the second sample-pressing plate, the sample-supporting plate and the second sample-bearing bottom plate; the sample support plate close to the electric brush comprises a flat plate part and a protruding part, and the protruding part is arranged at the top of the flat plate part in a protruding mode and is used for being in electric contact with the electric brush;

optionally, the top parts of both ends of the protruding part in the length direction are provided with a chamfer structure;

optionally, the chamfer structure satisfies at least one of the following conditions (c) to (e):

(c) the included angle between the inclination direction of the chamfer angle structure and the length direction of the convex part is 10-30 degrees;

(d) the ratio of the length of the chamfer structure in the inclined direction to the length of the bulge is (1-2): 10;

(e) in the inclination direction of the chamfering structure, arc transition areas are arranged at two ends of the chamfering structure, and the distribution range of each arc transition area in the chamfering structure accounts for 10% -20%.

6. The vacuum heating apparatus according to any one of claims 1 to 5, further comprising a mounting body; the mounting main body comprises a mounting base, a corrugated pipe and a connecting piece; the mounting base is provided with a fixed frame and a movable frame; the first end of the corrugated pipe is connected to the fixing frame and is provided with an installation piece which is used for being hermetically connected and communicated with the vacuum chamber; the second end of the corrugated pipe is connected with the movable frame; the connecting piece is arranged in the corrugated pipe in a penetrating mode, one end of the connecting piece is connected with the second end of the corrugated pipe, and the other end of the connecting piece penetrates out of the first end of the corrugated pipe and is connected with the conductive base platform.

7. The vacuum heating apparatus according to claim 6, wherein the moving frame is provided with a first driving member for driving the second end of the corrugated tube to move in a first predetermined direction, a second driving member for driving the second end of the corrugated tube to move in a second predetermined direction, and a third driving member for driving the second end of the corrugated tube to move in a third predetermined direction;

the first preset direction is the direction in which the fixed frame points to the movable frame; the second preset direction and the third preset direction are perpendicular to each other, and both the second preset direction and the third preset direction are perpendicular to the first preset direction;

optionally, the moving rack satisfies at least one of the following conditions (f) to (h):

(f) the first driving piece is a screw rod driving structure;

(g) the second driving piece is a micrometer handle;

(h) the third driving piece is a micrometer handle.

8. The vacuum heating apparatus according to claim 6, wherein the connecting member is rotatably connected to the second end of the bellows; the vacuum heating device further comprises a rotating mechanism, and the rotating mechanism is in transmission connection with the connecting piece.

9. A vacuum heating method using the vacuum heating apparatus according to claim 1, the vacuum heating method comprising heating a metal sample, the heating a metal sample comprising:

the tungsten wire electrodes at two ends of the tungsten wire are connected with the positive electrode and the negative electrode of a direct current power supply, so that the tungsten wire carries out thermal radiation heating on the metal sample;

when the required heating temperature is higher than 600 ℃, the positive pole of a high-voltage power supply is connected to the anode wire holder, and the negative pole of the high-voltage power supply is connected to the tungsten wire, so that electrons escaping from the surface of the tungsten wire bombard and heat the metal sample; optionally, the voltage of the high voltage power supply is 500V to 1000V.

10. The vacuum heating method according to claim 9,

the vacuum heating apparatus is configured to: the heating table main body further comprises a second heating assembly, the second heating assembly comprises an electric brush and an electric brush electrode connected to one end of the electric brush, the electric brush is fixed on one side, back to the tungsten filament, of the conductive base table, and the other end of the electric brush is in electrical contact with the sample fixing frame;

the vacuum heating method further includes heating the semiconductor sample, the heating the semiconductor sample including: and the anode wire holder and the brush electrode are connected with the anode and the cathode of a direct current power supply and used for heating the semiconductor sample.

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