CN111965078B - Melt diffusion device - Google Patents
Melt diffusion device Download PDFInfo
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- CN111965078B CN111965078B CN202010833448.7A CN202010833448A CN111965078B CN 111965078 B CN111965078 B CN 111965078B CN 202010833448 A CN202010833448 A CN 202010833448A CN 111965078 B CN111965078 B CN 111965078B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N2013/003—Diffusion; diffusivity between liquids
Abstract
The invention discloses a melt diffusion device, wherein a diffusion unit is detachably arranged in a rectangular cavity of a base; the diffusion unit comprises an upper limiting block, a lower limiting block and a diffusion table, wherein the upper limiting block and the lower limiting block are respectively and detachably arranged on the base, the diffusion table is formed by laminating a plurality of ceramic layers, the upper end and the lower end of a fixed positioning rod are respectively embedded into positioning holes of the upper limiting block and the lower limiting block through two left positioning rods and two right positioning rods respectively penetrating through two mounting grooves of the diffusion table, and the upper end and the lower end of the movable positioning rod are externally connected with a connecting frame; the plurality of ceramic plates of the diffusion table comprise a group of fixed ceramic plates which are fixedly arranged, a group of movable ceramic plates which can move left and right and a group of welding ceramic plates which can move left and right, and each movable ceramic plate is pushed to move left and right by pushing the connecting frame and matched with the left and right movement of the welding ceramic plates, so that the butt joint diffusion and the cutting of samples are realized. The invention has the advantages that: the installation and the disassembly are convenient and quick, and the test efficiency and the diffusion coefficient measurement accuracy are improved.
Description
Technical Field
The invention relates to a melt diffusion device which is used for measuring the mutual diffusion coefficient of binary and multi-element alloys or other nonmetallic materials in a molten state.
Background
The measurement of diffusion coefficient has been deeply focused by researchers at home and abroad. The diffusion coefficient measurement technology has been advanced under the efforts of a plurality of scholars at home and abroad, such as long capillary vessel technology, shearing unit technology, X-ray in-situ measurement technology, neutron scattering technology and the like. There are more and more means for measuring the diffusion coefficient of the alloy, and the measurement result is more and more accurate. Techniques for measuring diffusion coefficients are also receiving increasing attention from students.
It is very important to measure the diffusion coefficient of the metal melt. Diffusion is a very common phenomenon in nature and is seen everywhere in life. The nature of the diffusion phenomenon is a substance-oriented transport behavior, which is a substance migration behavior of substance particles due to thermal motion. The nature and characterization of atomic diffusion in molten metal is a fundamental and important physical problem in condensed state physics, and diffusion coefficient is an important parameter in characterizing the behavior of diffusion. The accurate diffusion coefficient also provides basic reference data for the atomic scale simulation process, provides reference basis for selection and improvement of potential functions, and can remarkably improve the accuracy of the simulation process. In addition, the diffusion data can also be used as basic input parameters of other simulation processes, so that possibility is provided for comprehensively knowing the properties of the alloy melt and the solidification process of the alloy melt, and the diffusion data is an important research aspect of computer-aided alloy composition design. The complex and ubiquitous diffusion behavior makes the computational measurement of diffusion coefficients an important research proposition that cannot be bypassed. In the design and preparation process of high-performance special alloy, the diffusion behavior of the multi-element system is researched, and the multi-element phase diffusion coefficient matrix is constructed in such a way, so that the multi-element phase diffusion coefficient matrix has important significance. For the research of diffusion and the measurement of the diffusion coefficient of the melt, the research time is short, the measured diffusion coefficient still has larger error, and different measurement methods are quite different.
The existing diffusion device has the defects of difficult clamping, easy loss, difficult elimination of the influence on diffusion in the cooling process and the like. The diffusion device is required to be detached from the diffusion furnace and taken out when diffusion experiments are carried out every time, after a diffusion sample is assembled, the whole diffusion device is placed into the diffusion furnace and is installed in a repositioning mode, a great deal of time and energy are required to be wasted in the process of detaching or assembling the whole diffusion device into the diffusion furnace, assembly is difficult, multiple assembly accuracy cannot be guaranteed, the success rate of the experiment is low, and the efficiency of the experiment is low. And the diffusion couple sample is still in a butt joint state in the cooling process of the original diffusion device, so that the influence of cooling on the experiment cannot be eliminated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a melt diffusion device so as to realize convenient and quick installation and disassembly, improve the test efficiency and the test success rate, reduce errors and improve the diffusion coefficient measurement precision.
The invention is realized by the following technical scheme:
the melt diffusion device comprises a base, wherein the base consists of a rear base and a front side plate which are detachably connected, a rectangular cavity which is communicated left and right is formed between the front side plate and the rear base, and a diffusion unit is detachably arranged in the rectangular cavity;
the diffusion unit comprises an upper limiting block, a lower limiting block and a diffusion table arranged between the upper limiting block and the lower limiting block, wherein the upper limiting block and the lower limiting block are respectively detachably arranged on a rear base, the diffusion table is formed by laminating a plurality of strip-shaped ceramic plates extending along the left-right direction, the left side and the right side of the diffusion table are respectively provided with a vertically through mounting groove, two positioning rods penetrate through the two mounting grooves of the diffusion table respectively through the left positioning rod and the right positioning rod, so that the ceramic plates are connected into a whole, the two positioning rods are respectively a fixed positioning rod and a movable positioning rod, the upper end and the lower end of the fixed positioning rod are respectively embedded into positioning holes of the upper limiting block and the lower limiting block, and the upper end and the lower end of the movable positioning rod are externally connected with a connecting frame;
the diffusion platform comprises a plurality of ceramic plates, a plurality of movable ceramic plates and a plurality of welding ceramic plates, wherein the fixed ceramic plates are fixedly arranged, the movable ceramic plates can move left and right, the welding ceramic plates can move left and right, the mounting grooves of the fixed ceramic plates and the fixed positioning rods are circular grooves, the mounting grooves of the movable ceramic plates and the movable positioning rods are kidney-shaped grooves, the mounting grooves of the movable ceramic plates and the fixed positioning rods are circular grooves, the mounting grooves of the movable ceramic plates and the movable positioning rods are kidney-shaped grooves, the movable ceramic plates are pushed to move left and right by pushing the connecting frame, and the welding ceramic plates are matched to move left and right, so that the change of the sample cavity inside the diffusion platform is realized, and then the butt joint diffusion and the cutting of samples are realized.
Further, in the diffusion table, the fused ceramic plate group is positioned in the middle of the diffusion table, the ceramic plates adjacent to the upper and lower parts of the fused ceramic plate group are respectively a first fixed ceramic plate and a second fixed ceramic plate, and the fixed ceramic plates and the movable ceramic plates are arranged above and below the fused ceramic plate group at intervals one by one;
the fixed ceramic plates and the movable ceramic plates are respectively provided with a first vertical through hole, the welding ceramic plates are respectively provided with a second vertical through hole, the top of the welding ceramic plate group is provided with a third vertical hole, the bottom of the welding ceramic plate group is provided with a fourth vertical hole, and the third vertical hole and the fourth vertical hole are not communicated with each other; the first fixed ceramic plate is also provided with a fifth vertical hole positioned on the right side of the first vertical through hole, the second fixed ceramic plate is also provided with a sixth vertical hole positioned on the right side of the first vertical through hole,
by moving the welded ceramic sheet set and the movable ceramic sheet set, three different status bits are obtained:
preheating status bit:
the right ends of the welding ceramic plate groups are protruded rightwards, and at the moment, the second vertical through holes on the welding ceramic plates, the fifth vertical holes on the first fixed ceramic plates and the sixth vertical holes on the second fixed ceramic plates are aligned and communicated on the same vertical position to form a welding sample cavity; the first vertical through holes of the fixed ceramic plates, the first vertical through holes of the movable ceramic plates, the third vertical holes of the welding ceramic plate groups and the fourth vertical holes of the welding ceramic plate groups are aligned at the same vertical position, and the upper sample cavity and the lower sample cavity which are coaxial up and down are respectively formed by blocking the welding ceramic plate groups;
welding state position:
each fixed ceramic plate and each movable ceramic plate are kept at the preheating state, the welding ceramic plate group moves leftwards until the left end of the welding ceramic plate group protrudes leftwards, and at the moment, the welding ceramic plate group penetrates through the upper sample cavity and the lower sample cavity through the second vertical through holes on each welding ceramic plate to form a welding state;
cooling status bit:
each fixed ceramic plate is kept on a welding state position, each movable ceramic plate moves rightwards, each welding ceramic plate moves rightwards until the first vertical through holes on each movable ceramic plate are staggered with the first vertical through holes on each fixed ceramic plate, and the second vertical through holes on each welding ceramic plate are staggered, so that the upper sample cavity, the lower sample cavity and the welding sample cavity are vertically divided into mutually independent column cavities.
Further, the welding ceramic sheet group comprises three welding ceramic sheets, namely a welding ceramic upper end sheet, a welding ceramic middle sheet and a welding ceramic lower end sheet from top to bottom in sequence, wherein a third vertical hole is formed in the welding ceramic upper end sheet, and a fourth vertical hole is formed in the welding ceramic lower end sheet.
Further, the installation groove for matching the middle welding ceramic plate with the movable positioning rod is a middle plate installation groove, the installation groove for matching the upper welding ceramic end plate, the lower welding ceramic end plate and the movable positioning rod is an end plate installation groove, and the inner ends of the middle plate installation groove and the inner ends of the two end plate installation grooves are not flush.
Further, in the upper sample cavity, an upper sealing ceramic plate, an upper graphite felt, upper ceramic particles and an upper sample are sequentially arranged from the top of the cavity to the bottom of the cavity; in the lower sample cavity, a lower closed ceramic plate, a lower graphite felt, lower ceramic particles and a lower sample are sequentially arranged from the bottom of the cavity to the top of the cavity.
Further, a plurality of heating holes which are vertically communicated are formed in the base, ceramic tubes are arranged in the heating holes, heating rods are arranged in the ceramic tubes, and adjacent heating rods are connected in series through connecting blocks.
Further, the back base is enclosed into a C-shaped frame structure by roof, posterior lateral plate, bottom plate jointly, preceding curb plate is located between roof and the bottom plate and is in the front side of posterior lateral plate, passes preceding curb plate, goes up the stopper back screw in posterior lateral plate in proper order through last mounting screw, passes preceding curb plate, lower stopper back screw in posterior lateral plate in proper order through lower mounting screw, realizes preceding curb plate, go up stopper, lower stopper and back base's detachable connection.
Further, the plurality of ceramic plates of the diffusion table are all boron nitride ceramic plates.
Compared with the prior art, the invention has the following advantages:
1. the invention provides a melt diffusion device which comprises a base composed of a rear base and a front side plate, wherein a diffusion unit is detachably arranged in a rectangular cavity of the base, the whole base can be placed in the diffusion furnace for a long time after being installed in the diffusion furnace, when diffusion experiments are carried out each time, the diffusion unit is only required to be taken out, after diffusion samples are installed, the assembled diffusion unit is placed in the rectangular cavity of the base, the base is not required to be detached and assembled back and forth, a great deal of time and effort are saved, assembly errors caused by back and forth detachment are avoided, assembly precision is improved, and therefore experimental efficiency and experimental success rate are improved.
2. The diffusion unit comprises an upper limiting block, a lower limiting block and a diffusion table, wherein the diffusion table is formed by stacking a plurality of ceramic layers, and can push each movable ceramic plate to move left and right by pushing a connecting frame and match with the left and right movement of a welding ceramic plate, so that a diffusion couple sample can be sheared into a plurality of columnar small particles, the atomic diffusion in the cooling process is effectively avoided, and the subsequent measurement of the diffusion coefficient of the diffusion couple sample is more accurate and reasonable.
3. According to the melt diffusion device provided by the invention, when the diffusion platform is in the preheating state, the upper end and the lower end of the welding sample cavity are overlapped with the upper sample cavity and the lower sample cavity in the vertical direction, so that when the subsequent welding ceramic wafer group moves leftwards to the welding state for welding diffusion, the butt joint surfaces are all the surfaces which are just cut, the condition that air holes appear in the middle of the samples during butt joint can be reduced to a great extent, the diffusion quality is ensured, and the follow-up diffusion coefficient measurement for diffusion couple samples is more accurate.
4. According to the melt diffusion device provided by the invention, the heating rod is arranged in the base, so that the sample is heated more uniformly and rapidly, the temperature control is more stable, the experimental precision is improved, and the system error is reduced.
Drawings
Fig. 1 is an overall perspective view of the present invention.
Fig. 2 is a perspective exploded view of the present invention with the connector removed.
Fig. 3 is a perspective view of a diffusion unit of the present invention.
Fig. 4 is a perspective view of a diffusion stand of the present invention.
Fig. 5 is an exploded view of the diffusion station of the present invention.
Fig. 6 is an exploded view of adjacent fixed and movable ceramic plates of the present invention.
FIG. 7 is an exploded view of the fusion bonded ceramic sheet of the present invention and its upper and lower ceramic sheets.
FIG. 8 is a cross-sectional view of a diffusion stage of the present invention in a pre-heat state.
FIG. 9 is a cross-sectional view of a diffusion stand of the present invention in a fusion-bonded state.
FIG. 10 is a cross-sectional view of the diffusion stand of the present invention in a cooled state.
FIG. 11 is a sample of the CeAl system diffusion pair obtained in this example.
FIG. 12 is a graph showing the concentration profile and the fitted diffusion coefficient of a CeAl system diffusion couple sample obtained in this example
Reference numerals in the drawings: the ceramic device comprises a rear base, a front side plate, a 3 rectangular cavity, a 4 ceramic tube, a 5 heating rod, a 6 upper mounting screw, a 7 lower mounting screw, a 8 upper limiting block, a 9 lower limiting block, a 10 diffusion table, a 11 fixed positioning rod, a 12 movable positioning rod, a 13 mounting groove, a 14 connecting frame, a 15 fixed ceramic plate, a 16 movable ceramic plate, a 17 welded ceramic plate, a 18 first vertical through hole, a 19 second vertical through hole, a 20 third vertical hole, a 21 fourth vertical hole, a 22 fifth vertical hole, a 23 sixth vertical hole, a 24 welded sample cavity, a 25 upper sample cavity, a 26 lower sample cavity, a 27 pillar cavity, a 28 welded ceramic upper end plate, a 29 welded ceramic middle plate, a 30 welded ceramic lower end plate, a 31 middle plate mounting groove, a 32 end plate mounting groove, a 33 upper sealed ceramic plate, a 34 upper graphite felt, a 36 upper sample, a 37 lower sealed ceramic plate, a 38 lower sealed ceramic plate, a 39 lower ceramic particle, a 40 lower sample, a 41 welded sample cavity, a 42, a 43 first fixed ceramic plate, and a 44 second fixed ceramic plate.
Detailed Description
The following describes in detail the examples of the present invention, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of protection of the present invention is not limited to the following examples.
Referring to fig. 1 to 10, the present embodiment discloses a melt diffusion device, which comprises a base, wherein the base is composed of a rear base 1 and a front side plate 2 which are detachably connected, a rectangular cavity 3 which is penetrated from left to right is formed between the front side plate 2 and the rear base 1, and a diffusion unit is detachably arranged in the rectangular cavity 3. The base is provided with a plurality of heating holes which are vertically communicated, ceramic tubes 4 are arranged in the heating holes, heating rods 5 are arranged in the ceramic tubes 4, and adjacent heating rods 5 in the heating rods 5 are connected in series through connecting blocks 42. The rear base 1 is formed by enclosing a C-shaped frame structure together by a top plate, a rear side plate and a bottom plate, the front side plate 2 is positioned between the top plate and the bottom plate and is positioned at the front side of the rear side plate, the front side plate 2 and the upper limiting block 8 are sequentially penetrated through the upper mounting screw 6 and screwed into the rear side plate, the lower mounting screw 7 is sequentially penetrated through the front side plate 2 and the lower limiting block 9 and screwed into the rear side plate, and the detachable connection of the front side plate 2, the upper limiting block 8 and the lower limiting block 9 with the rear base 1 is realized.
The diffusion unit includes upper stopper 8, lower stopper 9, and the diffusion platform 10 of arranging in between upper stopper 8 and lower stopper 9, upper and lower stopper 9 detachably installs respectively on back base 1, and diffusion platform 10 is laminated the formation by a plurality of rectangular form potsherds that extend along left and right directions, and a plurality of potsherds of diffusion platform 10 adopt the boron nitride potsherds in this embodiment, and this boron nitride potsherd can not react with the sample under the high temperature to can improve experimental accuracy.
The left side and the right side of the diffusion platform 10 are respectively provided with a vertically through mounting groove 13, the left and the right positioning rods respectively penetrate through the two mounting grooves 13 of the diffusion platform 10, so that a plurality of ceramic plates are connected into a whole, the two positioning rods are respectively a fixed positioning rod 11 and a movable positioning rod 12, the upper end and the lower end of the fixed positioning rod 11 are respectively embedded into the positioning holes of the upper limiting block 9 and the lower limiting block 9, and the upper end and the lower end of the movable positioning rod 12 are externally connected with a C-shaped connecting frame 14.
The plurality of ceramic plates of the diffusion platform 10 comprise a group of fixed ceramic plates 15 which are fixedly arranged, a group of movable ceramic plates 16 which can move left and right, and a group of welding ceramic plates 17 which can move left and right, wherein the mounting grooves 13 of the fixed ceramic plates 15 and the fixed positioning rods 11 are circular grooves, the mounting grooves 13 of the movable positioning rods 12 are kidney-shaped grooves, the mounting grooves 13 of the movable ceramic plates 16 and the fixed positioning rods 11 are kidney-shaped grooves, the mounting grooves 13 of the movable positioning rods 12 are circular grooves, and the mounting grooves 13 at two ends of the welding ceramic plates 17 are kidney-shaped grooves, and the connecting frames 14 are pushed to push the movable ceramic plates 16 to move left and right and match the welding ceramic plates 17 to move left and right, so that the change of the sample cavity inside the diffusion platform 10 is realized, and the butt joint diffusion and the cutting of samples are realized.
In the diffusion stand 10, the fused ceramic sheet set is located in the middle of the diffusion stand 10, and the ceramic sheets adjacent to the upper and lower sides of the fused ceramic sheet set are a first fixed ceramic sheet 43 and a second fixed ceramic sheet 44, respectively, and above and below the fused ceramic sheet set, each fixed ceramic sheet 15 and each movable ceramic sheet 16 are arranged at a one-to-one interval.
The fixed ceramic plates 15 and the movable ceramic plates 16 are respectively provided with a first vertical through hole 18, the welding ceramic plates 17 are respectively provided with a second vertical through hole 19, the top of the welding ceramic plate group is provided with a third vertical hole 20, the bottom of the welding ceramic plate group is provided with a fourth vertical hole 21, and the third vertical hole 20 and the fourth vertical hole 21 are not communicated with each other; the first fixed ceramic sheet 43 is further provided with a fifth vertical hole 22 on the right side of the first vertical through hole 18, and the second fixed ceramic sheet 44 is further provided with a sixth vertical hole 23 on the right side of the first vertical through hole 18.
By moving the welded ceramic sheet set and the movable ceramic sheet set, three different status bits are obtained:
preheating status bit:
the right ends of the welding ceramic plate groups protrude rightwards, and at the moment, the second vertical through holes 19 on the welding ceramic plates 17, the fifth vertical holes 22 on the first fixed ceramic plates 43 and the sixth vertical holes 23 on the second fixed ceramic plates 44 are aligned and communicated at the same vertical position to form welding sample cavities 24; the first vertical through holes 18 of the respective fixed ceramic sheets 15, the first vertical through holes 18 of the respective movable ceramic sheets 16, the third vertical holes 20 of the fused ceramic sheet sets, and the fourth vertical holes 21 of the fused ceramic sheet sets are aligned at the same vertical position, and the upper sample chamber 25 and the lower sample chamber 26 which are coaxial up and down are respectively formed by the blocking of the fused ceramic sheet sets, and this state is shown in fig. 8.
Welding state position:
each fixed ceramic sheet 15 and each movable ceramic sheet 16 are kept in the preheating state, and the welding ceramic sheet group moves leftwards until the left end of the welding ceramic sheet group protrudes leftwards, at this time, the welding ceramic sheet group penetrates the upper sample cavity 25 and the lower sample cavity 26 through the second vertical through holes 19 on each welding ceramic sheet 17 to form a welding state, and the state is shown in fig. 9.
Cooling status bit:
referring to fig. 10, each of the fixed ceramic sheets 15 is held in a fusion state position, and the connecting frame 14 is pushed to the right, so that each of the movable ceramic sheets 16 is pushed to the right, each of the fusion ceramic sheets 17 is pushed to the right until the first vertical through holes 18 on each of the movable ceramic sheets 16 are offset from the first vertical through holes 18 on each of the fixed ceramic sheets 15, and the second vertical through holes 19 on each of the fusion ceramic sheets 17 are offset, so that the upper sample chamber 25, the lower sample chamber 26, and the fusion sample chamber 24 are vertically divided into mutually independent column chambers 27, as shown in fig. 10.
The welding ceramic sheet group comprises three welding ceramic sheets 17, namely a welding ceramic upper end sheet 28, a welding ceramic middle sheet 29 and a welding ceramic lower end sheet 30 from top to bottom, wherein a third vertical hole 20 is formed in the welding ceramic upper end sheet 28, and a fourth vertical hole 21 is formed in the welding ceramic lower end sheet 30. The installation groove 13 for matching the welding ceramic middle plate 29 with the movable positioning rod 12 is a middle plate installation groove 31, the installation groove 13 for matching the welding ceramic upper end plate 28, the welding ceramic lower end plate 30 and the movable positioning rod 12 is an end plate installation groove 32, the inner ends of the middle plate installation groove 31 and the inner ends of the two end plate installation grooves 32 are not flush, and the structural design can ensure that the second vertical through holes 19 on the adjacent welding ceramic plates 17 in the cooling state are staggered in the vertical direction.
An upper closed ceramic plate 33, an upper graphite felt 34, upper ceramic particles 35 and an upper sample 36 are arranged in the upper sample cavity 25 in sequence from the top of the cavity to the bottom of the cavity; in the lower sample chamber 26, a lower closed ceramic plate 37, a lower graphite felt 38, lower ceramic particles 39 and a lower sample 40 are arranged in sequence from the bottom of the chamber to the top of the chamber; through the arrangement, the device is used for sealing the upper end and the lower end of the sample to form a pressurizing effect, so that the influence of surface tension on the free surface in the diffusion process on a diffusion system is effectively reduced, and the device has a particularly remarkable effect on improving the measurement accuracy.
When a diffusion experiment is required, an upper sample 36, a welded sample 41 and a lower sample 40 are placed in the upper sample chamber 25, the welded sample chamber 24 and the lower sample chamber 26, respectively, wherein the welded sample 41 and the lower sample 40 have the same composition. After the sample is assembled, the fixed positioning rod 11 and the movable positioning rod 12 respectively penetrate through the mounting grooves 13 on the left side and the right side of the diffusion table 10, then the upper limiting block 8 and the lower limiting block 9 are respectively arranged at the upper end and the lower end of the diffusion table 10, the upper end and the lower end of the fixed positioning rod 11 are respectively embedded into the positioning holes of the upper limiting block 9 and the lower limiting block 9, and the upper end and the lower end of the movable positioning rod 12 are externally connected with the connecting frame 14, so that the assembly of the diffusion unit is completed. And then the assembled diffusion unit is placed into the rectangular cavity 3 of the base, the diffusion unit sequentially penetrates through the front side plate 2 and the upper limiting block 8 through the two upper mounting screws 6 and then is screwed into the rear side plate, and the diffusion unit sequentially penetrates through the front side plate 2 and the lower limiting block 9 through the two lower mounting screws 7 and then is screwed into the rear side plate, so that the connection between the front side plate 2, the upper limiting block 8 and the lower limiting block 9 and the rear base 1 is realized, and the assembly of the whole diffusion device is completed. And then placing the assembled diffusion device into a diffusion furnace, and installing and positioning the base of the diffusion device and the diffusion furnace, so that the subsequent diffusion operation can be performed. After the diffusion operation is completed, only the two upper mounting screws 6 and the two lower mounting screws 7 are required to be disassembled, diffusion units in the rectangular cavity 3 can be taken out, diffusion couple samples are taken out, the whole diffusion device is not required to be disassembled, the disassembly and assembly time is greatly saved, and the test efficiency is improved.
The applicant carried out a diffusion test using the diffusion device of this embodiment, wherein the upper sample 36 had a composition of Ce75Al25, the lower sample 40 and the welded sample 41 had a composition of Ce85Al15, and the diffusion stage 10 had been made of thirty boron nitride ceramic plates, and correspondingly, thirty diffusion couple samples were obtained after the diffusion test, and a physical diagram of thirty celi diffusion couple samples obtained in this embodiment were embedded in a graphite tank as shown in fig. 11. As shown in fig. 12, a concentration profile and a fitted diffusion coefficient graph of a celi system diffusion couple sample obtained in this example are shown.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (6)
1. A melt diffusion apparatus comprising a base, characterized in that: the base is composed of a rear base (1) and a front side plate (2) which are detachably connected, a rectangular cavity (3) which is communicated left and right is formed between the front side plate (2) and the rear base (1), and a diffusion unit is detachably arranged in the rectangular cavity (3);
the diffusion unit comprises an upper limit block (8), a lower limit block (9) and a diffusion table (10) arranged between the upper limit block (8) and the lower limit block (9), wherein the upper limit block and the lower limit block (9) are respectively and detachably arranged on a rear base (1), the diffusion table (10) is formed by laminating a plurality of strip-shaped ceramic layers extending along the left-right direction, the left side and the right side of the diffusion table (10) are respectively provided with a vertically through mounting groove (13), the left side and the right side of the diffusion table respectively penetrate through the two mounting grooves (13) of the diffusion table (10) through the left positioning rod and the right positioning rod, so that a plurality of ceramic plates are connected into a whole, the two positioning rods are respectively a fixed positioning rod (11) and a movable positioning rod (12), and the upper end and the lower end of the fixed positioning rod (11) are respectively embedded into the positioning holes of the upper limit block and the lower limit block (9), and the upper end and the lower end of the movable positioning rod (12) are externally connected with a connecting frame (14);
the plurality of ceramic plates of the diffusion platform (10) comprise a group of fixed ceramic plates (15) which are fixedly arranged, a group of movable ceramic plates (16) which can move left and right, and a group of welding ceramic plates (17) which can move left and right, wherein the mounting grooves (13) of the fixed ceramic plates (15) and the fixed positioning rods (11) are circular grooves, the mounting grooves (13) of the movable ceramic plates (16) and the movable positioning rods (12) are kidney-shaped grooves, the mounting grooves (13) of the movable ceramic plates (16) and the fixed positioning rods (11) are circular grooves, the mounting grooves (13) of the two ends of the welding ceramic plates (17) are kidney-shaped grooves, and the connecting frames (14) are pushed so as to push the movable ceramic plates (16) to move left and right, and the welding ceramic plates (17) are matched to move left and right, so that the change of the internal sample cavity of the diffusion platform (10) is realized, and the butt joint and the splitting of the sample are realized;
in the diffusion table (10), a welding ceramic plate group is positioned in the middle of the diffusion table (10), ceramic plates adjacent to the upper part and the lower part of the welding ceramic plate group are a first fixed ceramic plate (43) and a second fixed ceramic plate (44) respectively, and the fixed ceramic plates (15) and the movable ceramic plates (16) are arranged above and below the welding ceramic plate group at intervals;
the fixed ceramic plates (15) and the movable ceramic plates (16) are respectively provided with a first vertical through hole (18), the welding ceramic plates (17) are respectively provided with a second vertical through hole (19), the tops of the welding ceramic plate groups are provided with a third vertical hole (20), the bottoms of the welding ceramic plate groups are provided with a fourth vertical hole (21), and the third vertical hole (20) and the fourth vertical hole (21) are not communicated with each other; a fifth vertical hole (22) is further formed in the right side of the first vertical through hole (18) on the first fixed ceramic sheet (43), a sixth vertical hole (23) is further formed in the right side of the first vertical through hole (18) on the second fixed ceramic sheet (44),
by moving the welded ceramic sheet set and the movable ceramic sheet set, three different status bits are obtained:
preheating status bit:
the right ends of the welding ceramic plate groups are protruded rightwards, and at the moment, the second vertical through holes (19) on the welding ceramic plates (17), the fifth vertical holes (22) on the first fixed ceramic plates (43) and the sixth vertical holes (23) on the second fixed ceramic plates (44) are aligned and communicated at the same vertical position to form welding sample cavities (24); the first vertical through holes (18) of the fixed ceramic plates (15), the first vertical through holes (18) of the movable ceramic plates (16), the third vertical holes (20) of the welding ceramic plate groups and the fourth vertical holes (21) of the welding ceramic plate groups are aligned at the same vertical position, and an upper sample cavity (25) and a lower sample cavity (26) which are coaxial up and down are respectively formed by blocking the welding ceramic plate groups;
welding state position:
each fixed ceramic plate (15) and each movable ceramic plate (16) are kept at the preheating state, the welding ceramic plate group moves leftwards until the left end of the welding ceramic plate group protrudes leftwards, and at the moment, the upper sample cavity (25) and the lower sample cavity (26) are communicated by the welding ceramic plate group through second vertical through holes (19) on each welding ceramic plate (17) to form a welding state;
cooling status bit:
each fixed ceramic plate (15) is kept at a welding state position, each movable ceramic plate (16) moves rightwards, each welding ceramic plate (17) moves rightwards until a first vertical through hole (18) on each movable ceramic plate (16) is staggered with a first vertical through hole (18) on each fixed ceramic plate (15), and a second vertical through hole (19) on each welding ceramic plate (17) is staggered, so that an upper sample cavity (25), a lower sample cavity (26) and a welding sample cavity (24) are vertically divided into mutually independent column cavities (27);
the welding ceramic sheet group comprises three welding ceramic sheets (17), wherein a welding ceramic upper end sheet (28), a welding ceramic middle sheet (29) and a welding ceramic lower end sheet (30) are sequentially arranged from top to bottom, a third vertical hole (20) is formed in the welding ceramic upper end sheet (28), and a fourth vertical hole (21) is formed in the welding ceramic lower end sheet (30).
2. A melt diffusion apparatus according to claim 1, wherein: the installation groove (13) for matching the welding ceramic middle plate (29) with the movable positioning rod (12) is a middle plate installation groove (31), the installation groove (13) for matching the welding ceramic upper end plate (28), the welding ceramic lower end plate (30) with the movable positioning rod (12) is an end plate installation groove (32), and the inner ends of the middle plate installation groove (31) and the inner ends of the two end plate installation grooves (32) are not flush.
3. A melt diffusion apparatus according to claim 1, wherein: an upper closed ceramic plate (33), an upper graphite felt (34), upper ceramic particles (35) and an upper sample (36) are sequentially arranged in the upper sample cavity (25) from the top of the cavity to the bottom of the cavity; in the lower sample cavity (26), a lower sealing ceramic plate (37), a lower graphite felt (38), lower ceramic particles (39) and a lower sample (40) are sequentially arranged from the bottom of the cavity to the top of the cavity.
4. A melt diffusion apparatus according to claim 1, wherein: the base is provided with a plurality of heating holes which are vertically communicated, ceramic tubes (4) are arranged in the heating holes, heating rods (5) are arranged in the ceramic tubes (4), and among the heating rods (5), adjacent heating rods (5) are connected in series through connecting blocks (42).
5. A melt diffusion apparatus according to claim 1, wherein: the rear base (1) is jointly enclosed into a C-shaped frame structure by a top plate, a rear side plate and a bottom plate, the front side plate (2) is positioned between the top plate and the bottom plate and is positioned on the front side of the rear side plate, the front side plate (2) and the upper limit block (8) are sequentially penetrated through an upper mounting screw (6), the rear side plate is screwed in, the lower limit block (9) is sequentially penetrated through a lower mounting screw (7), and the rear side plate is screwed in, so that the detachable connection of the front side plate (2), the upper limit block (8), the lower limit block (9) and the rear base (1) is realized.
6. A melt diffusion apparatus according to claim 1, wherein: the plurality of ceramic plates of the diffusion table (10) are boron nitride ceramic plates.
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