CN116550784A - Preparation method of semiconductor material arm array - Google Patents
Preparation method of semiconductor material arm array Download PDFInfo
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- CN116550784A CN116550784A CN202210106772.8A CN202210106772A CN116550784A CN 116550784 A CN116550784 A CN 116550784A CN 202210106772 A CN202210106772 A CN 202210106772A CN 116550784 A CN116550784 A CN 116550784A
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- 239000000463 material Substances 0.000 title claims abstract description 169
- 239000004065 semiconductor Substances 0.000 title claims abstract description 131
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000001125 extrusion Methods 0.000 claims abstract description 90
- 238000000034 method Methods 0.000 claims description 39
- 239000000758 substrate Substances 0.000 claims description 30
- 239000013590 bulk material Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052711 selenium Inorganic materials 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910002909 Bi-Te Inorganic materials 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 238000005553 drilling Methods 0.000 description 10
- 238000005520 cutting process Methods 0.000 description 9
- 229910000831 Steel Inorganic materials 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000010959 steel Substances 0.000 description 8
- 238000003491 array Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/02—Making uncoated products
- B21C23/04—Making uncoated products by direct extrusion
- B21C23/14—Making other products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C25/00—Profiling tools for metal extruding
- B21C25/02—Dies
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C29/00—Cooling or heating work or parts of the extrusion press; Gas treatment of work
- B21C29/003—Cooling or heating of work
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C35/00—Removing work or waste from extruding presses; Drawing-off extruded work; Cleaning dies, ducts, containers, or mandrels
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Pressure Sensors (AREA)
Abstract
The invention relates to a preparation method of a semiconductor material arm array. Specifically, a semiconductor block material is firstly placed on the surface of an extrusion die, then the semiconductor block material and the extrusion die are placed in a pressure-resistant sleeve, the semiconductor block material is subjected to plastic deformation through extrusion and is filled in holes arranged in an array on the surface of the extrusion die, and then the semiconductor material arm array is obtained after demolding.
Description
Technical Field
The invention relates to a preparation method of a semiconductor material arm array, and belongs to the technical field of semiconductor materials and devices.
Background
The small-size semiconductor device has wide application prospects in various fields (such as the micro thermoelectric device realizes accurate temperature control in micro-area active refrigeration and self-energy supply of wearable equipment), but with microminiaturization of the semiconductor device, preparation of core functional elements, namely high-density high-integration n-type and p-type semiconductor material arms and arrays thereof, faces a plurality of difficulties. On the one hand, with miniaturization of devices, the size of semiconductor material arms is greatly reduced, and efficient preparation thereof becomes a great problem. The arms of semiconductor material are conventionally obtained by cutting blocks of semiconductor material. When the size of the material arm is reduced to the sub-millimeter level, the cutting yield is obviously reduced, the cutting workload and line loss are greatly improved, and the preparation difficulty and the cost are greatly increased. For brittle thermoelectric semiconductor materials, the dicing process is essentially infeasible when the material arm size is less than 0.3 mm; on the other hand, with miniaturization of devices, it will be difficult to efficiently complete the arrangement of the material arm array with the conventional process. Taking a micro thermoelectric device as an example, at present, array arrangement is generally realized by picking up and transferring single n-type and p-type thermoelectric material arms obtained by cutting to a preset die one by one. When the size of the thermoelectric legs is reduced from the traditional few mm to 0.3mm or even below 0.1mm, the difficulty of picking up and transferring hundreds to thousands of thermoelectric legs is very high and the cost is very high by adopting the traditional method. Meanwhile, as the distance between adjacent thermoelectric legs in the array is greatly reduced, the inherent gap between the thermoelectric legs and a preset die can obviously influence the array arrangement precision, so that the quality of the device is difficult to effectively control.
Moreover, there are a number of disadvantages to the prior art in the fabrication of conventional mm-or cm-scale arrays of arms of semiconductor material. On one hand, the prior art prepares the semiconductor material arm based on a cutting method, and has the defects of low cutting speed of a single machine, limited productivity, large-scale production, purchase of a large number of cutting machines, corresponding operators, and high equipment and labor cost. In addition, the cutting process causes considerable material loss and environmental pollution. On the other hand, the prior art mainly utilizes a positioning template to pick up and transfer semiconductor material arms one by one manually to realize array arrangement, so that the productivity is difficult to be greatly improved, and the product quality is difficult to be effectively controlled.
It follows that the preparation of an array of arms of semiconductor material is an inefficient, pollution and labor intensive process based on the prior art. The prior art has a plurality of defects in preparing the conventional-size semiconductor material arm array, and is more difficult in preparing the micro-size semiconductor material arm array. Therefore, the development of a novel preparation method of the semiconductor material arm array realizes high-quality, low-cost and large-scale preparation of the semiconductor material arm array, and has important value for promoting the development of semiconductor devices with conventional sizes and promoting the development of devices to small (micro) sizes.
Disclosure of Invention
In view of the above, the present invention provides an array of arms of semiconductor material and a method for making the same.
On one hand, the invention provides a preparation method of a semiconductor material arm array, which is characterized in that a semiconductor block material is firstly placed on the surface of an extrusion die, then the semiconductor block material and the extrusion die are placed in a pressure-resistant sleeve, the semiconductor block material is subjected to plastic deformation along the pressure direction by extrusion and is filled in holes arranged on the surface of the extrusion die in an array manner, and the semiconductor material arm array is obtained after demolding.
Preferably, the extrusion die includes: a rigid substrate, and an array of holes distributed in the rigid substrate; the method comprises the steps of carrying out a first treatment on the surface of the The hard substrate is a metal substrate (e.g., a steel substrate) or a ceramic substrate.
Preferably, the shape of the projection of the hole on the plane parallel to the surface of the hard substrate is a circle, rectangle, triangle, trapezoid or sector, and the shape of the projection of the hole on the direction perpendicular to the surface of the hard substrate is a rectangle or trapezoid.
Preferably, when the shape of the projection of the hole in the direction perpendicular to the surface of the hard substrate is trapezoid, the base angle of the trapezoid is more than 90 degrees and less than or equal to 135 degrees, and preferably 92-100 degrees. The meaning of the range is as follows: on one hand, the corresponding thermoelectric arm is slightly tapered, so that the demolding is convenient; on the other hand, the taper of the thermoelectric legs is not large, so that the size difference of the thermoelectric legs at different positions along the height direction of the thermoelectric legs is small, and the complexity of the structure and performance design of the thermoelectric device is avoided.
Preferably, the size of the projection of the holes on a plane parallel to the surface of the rigid substrate is 1 μm to 20mm, preferably 1 μm to 3000 μm, more preferably 30 μm to 500 μm.
Preferably, the shortest distance between the centers of adjacent holes is 3 μm to 20mm, preferably 50 μm to 800 μm.
Preferably, the depth of the holes is 1 μm to 50mm, preferably 10 μm to 3mm.
Preferably, the relative deviation between the diameters of the semiconductor block material and the extrusion die and the inner diameter dimension of the pressure-resistant sleeve is less than or equal to 5%, and preferably, the absolute deviation between the diameters of the semiconductor block material and the extrusion die and the inner diameter dimension of the pressure-resistant sleeve is less than or equal to 0.2mm. In the extrusion process, plastic deformation of the material occurs in the pressure-resistant sleeve, and the diameters of the bulk material and the extrusion die are equal to the inner diameter dimension of the pressure-resistant sleeve (the relative deviation is less than or equal to 5 percent and the absolute deviation is less than or equal to 0.2 mm), so that the deformation of the bulk material mainly occurs in the pressure direction in the extrusion process.
According to the invention, the semiconductor material arm and the semiconductor material array are integrally formed through an extrusion process based on the plasticity of the semiconductor bulk material, so that the high-quality, low-cost and large-scale preparation of the semiconductor material arm array is realized.
Preferably, the semiconductor bulk material is a semiconductor material having intrinsic plasticity, a composite material having plasticity prepared from a semiconductor material having intrinsic plasticity and a semiconductor material having intrinsic non-plasticity, or a paste-like mixture prepared based on an intrinsic non-plastic semiconductor material. Preferably, the semiconductor bulk material has a composition selected from the group consisting of Ag-based semiconductor materials (Ag 2 S x M 1-x M is Se or Te, x is more than or equal to 0 and less than or equal to 1), and Cu-based semiconductor material (Cu) 2-y Ag y Se 1-z M z Y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, M element is S or Te), bi-Te based semiconductor material, and mud-like mixture taking Bi-Te based semiconductor material as main component.
Preferably, the extrusion temperature is 5-500 ℃, preferably 30-250 ℃, and the extrusion temperature is higher than or equal to the softening temperature of the semiconductor bulk material; the extrusion pressure is 1 MPa-10 GPa, preferably 100 MPa-1 GPa; the dwell time of the extrusion is 1 to 100 minutes, preferably 10 to 40 minutes; the temperature of the demolding is greater than the softening temperature of the semiconductor bulk material, preferably 10-170 ℃. Wherein the semiconductor bulk material is subjected to an extrusion treatment, and the temperature of the extrusion treatment is continuously increased from room temperature until the semiconductor bulk material is plastically deformed without breaking, the temperature being defined as a softening temperature of the semiconductor material. Proper extrusion temperature and pressure are set according to the requirements, so that the extrusion of the semiconductor material is ensured to be in place, and the cost (energy consumption and die loss) is reduced.
In yet another aspect, the present invention provides an array of arms of semiconductor material prepared according to the preparation method described above, comprising: an arm of semiconductor material, and an array integrally formed with the arm of semiconductor material. The size, arrangement and pattern design of the semiconductor material arm array are in one-to-one correspondence with the holes in the extrusion die.
The beneficial effects are that:
in the invention, the plasticity of the semiconductor material is fully utilized, the thermoelectric arms of the same material are formed by extrusion, and the size of the semiconductor material arm depends on the size of a hole in an extrusion die, so that: a) Compared with various cutting processes, the limit of the mechanical property of the semiconductor material on the size of the material arm is broken through, and the size of the material arm can be conveniently reduced to be 0.3mm or even below 0.1 mm; b) Compared with various deposition processes, the method can prepare the semiconductor material arm with the micron-millimeter level at low cost and high efficiency, has a large adjustment range of the height-diameter ratio of the material arm, and is beneficial to optimizing the performance of the semiconductor device.
In the invention, the array of the same semiconductor material arms is integrally formed by extrusion, rather than sequentially picking up independent material arms for one-to-one transfer arrangement. Thus: a) The array forming process is greatly simplified, and low-cost and large-scale preparation can be realized; b) The quality control of the array is very convenient (different arrays extruded by the same die, and the shapes and the arrangement of material arms are identical); c) The method can break through the limitation of the traditional preparation method on the positioning precision of the semiconductor material arm in the array, and is beneficial to the further miniaturization of the corresponding device.
Compared with the traditional method, the method has less material loss in the array preparation process, and the advantage is more obvious along with the reduction of the array size. This is because the material loss in the fabrication process of the present invention, which is independent of the height and cross-sectional dimensions of the semiconductor material arms, is easily controlled by the need to remove the substrate material associated with the array. Whereas the material loss in conventional dicing methods is related to the semiconductor material arm height and cross-sectional area. As the material arm size decreases, the material loss duty cycle will inevitably rise rapidly.
The material arm array extrusion molding technology provided by the invention has a wide application range. In terms of materials, the method can be used for preparing a corresponding semiconductor material arm array by the materials which have intrinsic plasticity under certain conditions or can show plasticity through certain treatment; in terms of size, the semiconductor material arm size can be realized from microscopic (μm-scale) to macroscopic (mm-cm-scale) as long as the extrusion die of the corresponding size can be prepared.
Drawings
FIG. 1 is a schematic top view of an array of arms of semiconductor material described in example 1 (schematic top view of an array of arms of semiconductor material described in examples 2,4-7 is similar);
FIGS. 2a and 2b are extrusion dies used in examples 1 and 4-5, respectively (the extrusion dies used in the remaining examples are similar in appearance to FIG. 2 a);
FIG. 3 shows the pressure sleeves and pressure heads used in examples 1-4 and 6-7;
FIGS. 4a, 4b and 4c are, respectively, the arrays of arms of semiconductor material obtained in examples 1, 2 and 6 using the preparation method of the present invention;
FIGS. 5a and 5b are, respectively, an extrusion die used in example 3 and an array of arms of semiconductor material obtained by the preparation method of the present invention;
FIGS. 6a and 6b are, respectively, an extrusion die and its fittings (inside and outside circles) used in example 4, and an array of arms of semiconductor material obtained by the preparation method of the present invention;
fig. 7a, 7b and 7c are respectively an extrusion die before extrusion, a semiconductor bulk material placed thereon, a semiconductor material and an extrusion die after extrusion without using a pressure-resistant sleeve, and an array of semiconductor material arms obtained after demolding in example 5;
fig. 8a and 8b are, respectively, an array of extrusion die holes before extrusion and an array of extrusion die holes after extrusion, which resulted in a large amount of breakage residues of the semiconductor material arms due to an excessively low release temperature.
Detailed Description
The invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof.
In the invention, the preparation process of the semiconductor material arm array comprises the following main steps: and designing and preparing an extrusion die. An array of n (p) semiconductor material arms is integrally formed and de-molded using an extrusion process. By adopting the method, the semiconductor material arm and the semiconductor material arm array can be integrally formed, and the high-quality, low-cost and large-scale preparation of the semiconductor material arm array is realized.
Suitable materials are selected for the preparation of the extrusion die. The material of the extrusion die has enough compressive strength, and deformation in the repeated heating and cooling and extrusion process is avoided, so that array accuracy is prevented from being influenced. According to the extrusion technological parameters of different semiconductor materials, the corresponding die materials can be steel materials such as hard alloy steel, high-speed steel, die steel, stainless steel and the like, can also be metal materials such as W, mo, nb, ti and the like, and can also be ZrO 2 、Al 2 O 3 、AlN、Si 3 N 4 The ceramic material can also be other inorganic or organic materials with required compressive strength and processing performance. In a preferred embodiment, the mold material is mold steel. The extrusion die further comprises a press head and the like.
And processing a corresponding hole array on the surface of the die material according to parameters obtained by the semiconductor material arm and the array. Specifically, according to parameters of the semiconductor material arm array, such as the shape, the spacing and the arrangement of the material arms, corresponding hole arrays are prepared on the surface of the die material by adopting technologies such as mechanical drilling, laser drilling or corrosion hole forming. The holes in the mold may be circular, rectangular, triangular, trapezoidal, fan-shaped or other irregular shape in the horizontal direction, and rectangular, trapezoidal or other irregular shape in the vertical direction (vertical direction). For easy demoulding, the inner wall of the hole should be smooth as much as possible, the projection of the hole on the plane perpendicular to the surface of the mould can be rectangular or trapezoid, and the base angle can be 90-135 degrees, preferably 92-100 degrees. The size of the projection of the holes on a plane parallel to the surface of the rigid substrate may be 1 μm to 20mm, preferably 1 μm to 3000 μm, more preferably 30 μm to 200 μm. The shortest distance between the centers of adjacent holes may be 3 μm to 20mm, preferably 50 μm to 800 μm. The depth of the holes may be 1 μm to 50mm, preferably 10 μm to 3mm.
In a preferred embodiment, the array of holes is prepared using laser drilling, with the bottom of the holes having a diameter of about 70 μm and a depth of about 200 μm, and the projected trapezoid base angle being about 92 °. In another preferred embodiment, the hole array is prepared by mechanical drilling, the hole bottom diameter is about 200 μm, the hole depth is about 500 μm, the projected trapezoid base angle is about 92 °, and the center-to-center distance between nearest neighbor holes is about 707 μm. In another preferred embodiment, the hole array is prepared using mechanical drilling with a hole bottom diameter of about 150 μm and a hole depth of about 300 μm with a projected trapezoidal base angle of about 100 °. In another preferred embodiment, the array of holes is prepared using mechanical drilling, the holes having a diameter of about 200 μm and a depth of about 600 μm, the holes being rectangular in projection on a plane perpendicular to the mold surface.
The n (p) semiconductor block material is arranged on the hole array of the extrusion die, the semiconductor block material and the extrusion die are arranged in a pressure-resistant sleeve with the inner diameter equal to or slightly larger than that of the semiconductor block material (the relative deviation of the size is less than or equal to 5 percent, and the absolute deviation is less than or equal to 0.2 mm), and the material is subjected to plastic deformation through extrusion. During the extrusion process, the pressure-resistant sleeve constrains the lateral deformation of the semiconductor material, causing the material deformation to occur (mainly) in the direction of the pressure so as to fill all the holes. The proper extrusion temperature, pressure and dwell time are set according to the specific semiconductor material properties, which ensures that the material is extruded in place (filling the holes), reduces costs (energy consumption and die loss), and minimizes the impact of extrusion on the material properties.
In an alternative embodiment, the semiconductor bulk material is an Ag-based semiconductor material Ag 2 S x M 1-x M elementThe element is Se or Te, x is more than or equal to 0 and less than or equal to 1, the extrusion temperature can be 5-170 ℃, the extrusion pressure can be 100 MPa-1 GPa, and the pressure maintaining time can be 10-60 minutes. In a preferred embodiment, ag 2 The extrusion temperature of the S material is 20 ℃, the pressure is 1.5GPa, and the dwell time is 10min. In another preferred embodiment, ag 2 The extrusion temperature of the S material is 80 ℃, the pressure is 500MPa, and the pressure maintaining time is 40min. In another preferred embodiment, ag 2 The extrusion temperature of the S material is 140 ℃, the pressure is 200MPa, and the pressure maintaining time is 60min.
In an alternative embodiment, the semiconductor bulk material may be a Cu-based semiconductor material (Cu 2-y Ag y Se 1-z M z Y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, M element is S or Te), the extrusion temperature can be 180-300 ℃, the extrusion pressure can be 300 MPa-1.5 GPa, and the pressure maintaining time can be 10-60 minutes. In a preferred embodiment, cu 2 The extrusion temperature of Se material is 250 ℃, the pressure is 1GPa, and the dwell time is 40min.
After the extrusion is completed, the semiconductor material arms and the extrusion die are separated by demolding, and the semiconductor material arm array which is formed by n (p) type semiconductor material arms with the same shape as the holes and is consistent with the die hole array is obtained. In this process, an appropriate demolding temperature needs to be set according to the properties of the semiconductor bulk material. The demolding temperature should be slightly above the softening temperature of the material, typically 10 to 50℃above it. The temperature is too low, the thermoelectric arms are easy to be pulled and brittle to break in the demolding process, and broken thermoelectric arms remain in holes of the extrusion die, so that the die is scrapped, and meanwhile, a complete thermoelectric arm array cannot be obtained. The temperature is too high, and the material is too soft and is easy to be pulled and deformed and even broken. And after demolding, obtaining a semiconductor material arm array connected with the substrate material, wherein the shape and array arrangement of the material arms are completely consistent with those of the die hole array.
In an alternative embodiment, the semiconductor bulk material is an Ag-based semiconductor material Ag 2 S x M 1-x The M element is Se or Te, x is more than or equal to 0 and less than or equal to 1, and the demoulding temperature after extrusion is finished can be 10-80 ℃, preferably 20-40 ℃.
In an alternative embodimentThe semiconductor bulk material may be a Cu-based semiconductor material (Cu 2-y Ag y Se 1-z M z Y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, M element is S or Te, and the demoulding temperature after extrusion is finished can be 130-220 ℃, preferably 150-170 ℃.
By appropriate processing of the end faces of the semiconductor material arms in the array, subsequent end face metallization and integration of semiconductor devices is facilitated.
In the invention, the obtained semiconductor material arms are connected with the substrate material, the shape of the semiconductor material arms is the same as that of the die holes, and the array arrangement of the material arms is consistent with that of the die holes.
The present invention will be further illustrated by the following examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1
An array of holes as shown in fig. 1 and 2a was prepared on the surface of a die steel (hrc=60) using a mechanical drilling process, the bottom hole diameter was about 200 μm, the hole depth was about 500 μm, the projection of the holes on a plane perpendicular to the die surface was trapezoidal, and the bottom angle was about 92 °.
Ag with 2 S material is processed into blocks with the diameter of 9.90mm and the thickness of 1mm, the blocks are placed on an extrusion die hole array, and the material and the extrusion die are placed in a pressure-resistant sleeve with the inner diameter of 10mm in sequence. Pressurizing to 1.5GPa at 20deg.C and at a pressure increasing rate of 0.2GPa/s, maintaining for 10min, removing pressure, and demolding at 20deg.C to obtain Ag connected with substrate material 2 An array of S thermoelectric arms is shown in fig. 4 a.
Example 2
A mechanical drilling process was used to prepare an array of micro-holes similar to that shown in fig. 1 on the surface of a die steel (hrc=50), with a bottom aperture of about 150 μm and a hole depth of about 300 μm, the holes being trapezoidal in projection in a plane direction perpendicular to the die surface, with a base angle of about 100 °.
Ag with 2 S material is processed into blocks with the diameter of 9.90mm and the thickness of 1mm, the blocks are placed on an extrusion die hole array, and the material and the extrusion die are placed in a pressure-resistant sleeve with the inner diameter of 10mm in sequence. Heating the material and the die to 80 ℃ at a heating rate of 10 ℃/min, preserving heat for 5min, then pressurizing to 500MPa at a pressurizing rate of 0.2GPa/s, maintaining the pressure for 40min, removing the pressure, and demolding at 20 ℃ to obtain the Ag connected with the substrate material 2 An array of S thermoelectric arms as shown in fig. 4 b.
Example 3 (70 μm)
The laser drilling process was used to prepare an array of micro-holes as shown in fig. 5a in the surface of a die steel (hrc=50), with a bottom aperture of about 70 μm and a hole depth of about 200 μm, the holes being projected in a trapezoid shape with a base angle of about 92 ° in a plane direction perpendicular to the die surface.
Ag with 2 S material is processed into blocks with the diameter of 9.9mm and the thickness of 1mm, and the blocks are placed on an extrusion die hole array and then sequentially placed into a pressure-resistant sleeve with the inner diameter of 10 mm. Heating to 140deg.C at 20deg.C/min, maintaining the temperature for 10min, pressurizing to 0.2GPa at 0.1GPa/s, maintaining the pressure for 60min, removing pressure, and demolding at 20deg.C to obtain Ag connected with substrate material 2 An array of S thermoelectric arms as shown in fig. 5 b.
Example 4 (rectangle)
A mechanical drilling process was used to prepare an array of micro-holes similar to that shown in fig. 1, with a pore diameter of about 220 μm and a pore depth of about 600 μm, on the surface of a die steel (hrc=50), the projection of the holes in a plane direction perpendicular to the die surface being rectangular.
Ag with 2 The S material was processed into blocks 9.9mm in diameter and 1mm thick, placed over the array of extrusion die holes and surrounding extrusion fittings (as shown in FIG. 6 a), and then placed in sequence in a 10mm inner diameter pressure sleeve. Heating the material and the die to 80 ℃ at a heating rate of 10 ℃/min, preserving heat for 5min, then pressurizing to 500MPa at a pressurizing rate of 0.2GPa/s, maintaining the pressure for 40min, removing the pressure, and demolding at 20 ℃ to obtain the Ag connected with the substrate material 2 S thermoelectricAn array of arms as shown in figure 6 b.
Example 5 (no pressure sleeve, array deformation)
Ag with 2 The S material was processed into a 9.9mm diameter block of 1mm thickness and placed over the array of extrusion die holes described in example 4 without the use of a pressure resistant sleeve, as shown in FIG. 7 a. Heating the material and the die to 80 ℃ at a heating rate of 10 ℃/min, preserving heat for 5min, then pressurizing to 500MPa at a pressurizing rate of 0.2GPa/s, maintaining the pressure for 40min, and removing the pressure, so that the material block is obviously deformed transversely, as shown in figure 7 b. Demolding at 20deg.C to obtain Ag connected with substrate material 2 S array of thermoelectric legs, but the thermoelectric legs in the array are severely deformed as shown in FIG. 7 c.
Example 6 (Cu) 2 Se)
Cu is added with 2 Se material was processed into blocks of 9.9mm diameter and 1mm thickness, placed over the array of extrusion die holes described in example 1, and then placed in sequence in a pressure-resistant sleeve of 10mm inside diameter. Pressurizing at 250deg.C with a pressure increasing rate of 0.2GPa/s to 1GPa, maintaining the pressure for 40min, removing pressure, and demolding at 160deg.C to obtain Cu connected with base material 2 S thermoelectric arm array as shown in FIG. 4c
Example 7 (Cu) 2 Se cleavage
Cu is added with 2 The S material was processed into blocks of 9.9mm diameter and 1mm thickness, placed over the array of extrusion die holes described in example 1, and then placed in sequence in a pressure sleeve of 10mm inside diameter. Pressurizing to 1GPa at 250 ℃ at a pressure increasing rate of 0.2GPa/s, maintaining the pressure for 40min, removing the pressure, demolding at 120 ℃, breaking the root of the thermoelectric arm in the demolding process, and leaving a large amount of thermoelectric arm in the hole of the extrusion die, as shown in figure 8 b. The array preparation failed and the extrusion die was scrapped.
Claims (13)
1. A preparation method of a semiconductor material arm array is characterized in that a semiconductor block material is firstly placed on the surface of an extrusion die, then the semiconductor block material and the extrusion die are placed in a pressure-resistant sleeve, plastic deformation is carried out on the semiconductor block material through extrusion, the semiconductor block material is filled in holes arranged on the surface of the extrusion die in an array mode, and then the semiconductor material arm array is obtained after demolding.
2. The method of manufacturing according to claim 1, wherein the extrusion die comprises: a rigid substrate, and an array of holes distributed in the rigid substrate; the hard substrate is a metal substrate or a ceramic substrate.
3. The method of claim 2, wherein the holes have a circular, rectangular, triangular, trapezoidal, or fan-shaped projection on a plane parallel to the surface of the rigid substrate, and a rectangular, or trapezoidal projection on a plane perpendicular to the surface of the rigid substrate.
4. A method of producing according to claim 3, wherein the holes have a trapezoid shape in projection perpendicular to the surface of the rigid substrate, the base angle of the trapezoid being > 90 ° and 135 °, preferably 92 ° to 100 °.
5. The method of claim 2, wherein the size of the projection of the holes on a plane parallel to the surface of the rigid substrate is 1 μm to 20mm, preferably 1 μm to 3000 μm, more preferably 30 μm to 500 μm.
6. The preparation method according to any one of claims 1 to 5, wherein the shortest distance between adjacent hole centers is 3 μm to 20mm, preferably 50 μm to 800 μm.
7. The method of any one of claims 1-5, wherein the holes have a depth of 1 μm to 50mm, preferably 10 μm to 3mm.
8. The method of any one of claims 1 to 7, wherein the relative deviation of the diameters of the semiconductor block and the extrusion die from the inner diameter dimension of the pressure jacket is less than or equal to 5%, preferably the absolute deviation of the diameters of the semiconductor block and the extrusion die from the inner diameter dimension of the pressure jacket is less than or equal to 0.2mm.
9. The method of any one of claims 1 to 8, wherein the semiconductor bulk material is a semiconductor material having intrinsic plasticity, a composite material having plasticity prepared from a semiconductor material having intrinsic plasticity and a semiconductor material having intrinsic non-plasticity, or a paste-like mixture prepared based on an intrinsic non-plastic semiconductor material.
10. The method according to claim 9, wherein the semiconductor bulk material has a composition selected from the group consisting of Ag-based semiconductor materials (Ag 2 S x M 1-x M is Se or Te, x is more than or equal to 0 and less than or equal to 1), and Cu-based semiconductor material (Cu) 2-y Ag y Se 1-z M z Y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, M element is S or Te), bi-Te based semiconductor material, and mud-like mixture taking Bi-Te based semiconductor material as main component.
11. The method of any one of claims 1 to 10, wherein the extrusion temperature is 5 to 500 ℃, preferably 20 to 250 ℃, and the extrusion temperature is at or above the softening temperature of the semiconductor bulk material; the extrusion pressure is 1 MPa-10 GPa, preferably 100 MPa-1.5 GPa; the dwell time of the extrusion is 1 to 100 minutes, preferably 10 to 60 minutes.
12. The method of any one of claims 1 to 11, wherein the temperature of the demolding > the softening temperature of the semiconductor bulk material, preferably 10 to 170 ℃.
13. An array of arms of semiconductor material prepared according to the preparation method of any one of claims 1 to 12, comprising: a semiconductor material arm substrate, and an array of semiconductor material arms integrally formed with the semiconductor material arm substrate.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210106772.8A CN116550784A (en) | 2022-01-28 | 2022-01-28 | Preparation method of semiconductor material arm array |
| PCT/CN2023/071690 WO2023143076A1 (en) | 2022-01-28 | 2023-01-10 | Preparation method for semiconductor material arm array and batch preparation method for semiconductor material arm array interface layer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210106772.8A CN116550784A (en) | 2022-01-28 | 2022-01-28 | Preparation method of semiconductor material arm array |
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| CN116550784A true CN116550784A (en) | 2023-08-08 |
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| CN202210106772.8A Pending CN116550784A (en) | 2022-01-28 | 2022-01-28 | Preparation method of semiconductor material arm array |
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