Perovskite evaporation source crucible assembly

Abstract

The utility model belongs to the technical field of crucibles, and particularly relates to a perovskite evaporation source crucible assembly which comprises a quartz crucible with an opening at one end, at least one heat conduction piece arranged in the quartz crucible and a filtering piece arranged in the quartz crucible and located above the heat conduction piece. And the filtering piece covers the upper opening of the quartz crucible. According to the utility model, through the arrangement of the honeycomb-shaped heat conduction member and the filtering member, the original perovskite raw material is easier to volatilize, the loss of heating power is reduced, the time for stabilizing the deposition rate is shortened, and the large-scale mass production is facilitated; the filter screen is additionally arranged, so that raw materials are more conveniently prevented from splashing to pollute other raw materials, large blasting-boiling particles can be filtered out and splashed to a substrate in the evaporation process, a film layer grows finer and smoother, the quality is better, and defects caused to the film layer are avoided.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the crucible technical field, concretely is a kind of perovskite evaporation source crucible assembly and photovoltaic cell. BACKGROUND

[0002] Perovskite compound has multiple excellent physical and chemical properties, and its application in the field of photoelectric conversion is attracting more and more attention. Perovskite solar cells can be produced flexibly and in large areas due to their unique structure. However, in practical applications, how to improve the deposition rate of perovskite thin film is one of the key factors restricting the development of perovskite solar cells.

[0003] Currently, perovskite film preparation is generally divided into solution method and gas phase method. The gas phase method performs better than the solution method in uniformity, density and defect degree of perovskite film, which makes it have certain technical advantages in future large-scale production. Currently, the vacuum gas phase method mainly uses resistance wire to heat perovskite materials in a quartz crucible under certain vacuum conditions. The perovskite raw materials are directly filled into the quartz crucible, and the structure of the quartz crucible is not optimized. Specifically, the quartz crucible is heated by heating wire conduction to heat the perovskite materials inside the crucible. Due to the limitation of ordinary heating wire, the conduction heat efficiency of perovskite inorganic materials or organic materials is slow, so a long waiting period is required before the crystal oscillator film thickness meter can detect the change in film thickness. The conduction heat efficiency is slow. At the same time, it takes 10-25 minutes to start heating the crucible, which affects the actual deposition efficiency. Especially in the case of a large amount of raw materials, it takes a longer time to make the raw materials reach a stable state. In addition, when evaporating bulk perovskite organic crystalline materials, the problem of material spattering is particularly prominent.

[0004] Therefore, it is urgent to develop a new crucible assembly to improve the conduction heat efficiency of perovskite materials. SUMMARY

[0005] To solve the problems in the above background art, the utility model provides a perovskite evaporation source crucible assembly, which increases a heat-conducting piece with through holes in the interior of the quartz crucible, so that the deposition rate of perovskite materials reaches a stable state faster. At the same time, a filter is added to the opening of the quartz crucible to prevent raw materials from splashing into other sources.

[0006] The utility model provides a perovskite evaporation source crucible assembly, which includes a quartz crucible with an open end, at least one heat-conducting piece arranged in the quartz crucible, and a filter arranged in the quartz crucible above the heat-conducting piece. The heat-conducting piece is provided with a plurality of through holes that penetrate up and down, and the filter covers the upper opening of the quartz crucible.

[0007] Further, the heat-conducting pieces in the quartz crucible are stacked in multiple layers, one of the two adjacent heat-conducting pieces is provided with a limiting column, and the other is provided with a limiting hole matched with the limiting column.

[0008] Further, the limiting columns and limiting holes on the two adjacent heat-conducting pieces are provided in multiple, and the through holes on the two adjacent heat-conducting pieces are arranged one by one in correspondence.

[0009] Further, the heat-conducting piece in the quartz crucible comprises an inner heat-conducting piece and an outer heat-conducting piece sleeved with each other, the outer diameter of the inner heat-conducting piece is the same as the inner diameter of the outer heat-conducting piece, one of the inner heat-conducting piece and the outer heat-conducting piece is provided with a limiting guide groove, and the other is provided with a limiting block matched with the limiting guide groove.

[0010] Further, the through holes are arranged in a honeycomb shape.

[0011] Further, the filter is a filter screen, and the mesh number of the filter screen is 100-500.

[0012] Further, the cross section of the through hole is one of a circle, a polygon, a sector, and an ellipse.

[0013] Further, the upper end of the filter is provided with a handle.

[0014] Further, the heat-conducting piece is made of one of stainless steel, tungsten, tantalum, and quartz or a plurality of materials.

[0015] Further, the height of the multiple stacked heat-conducting pieces is 3 / 5-4 / 5 of the internal depth of the quartz crucible.

[0016] Compared with the prior art, the utility model has the advantages that:

[0017] (1) The crucible assembly is provided with at least one heat-conducting piece in the quartz crucible, and the heat-conducting piece is provided with a plurality of through holes penetrating upward and downward, and a filter is arranged above the heat-conducting piece, the perovskite evaporation raw material is filled into the pores of the through holes, and a filter screen is added, then the quartz crucible is heated, the heat is rapidly transmitted to the heat-conducting piece, the heat-conducting piece contacts the perovskite to make the perovskite raw material more volatile, reduces the loss of heating power, and at the same time reduces the power consumption, shortens the time of stable deposition rate, and is more conducive to large-scale production; the filter screen is more convenient for protecting the raw material, avoiding the raw material from splashing and polluting other materials outside the quartz crucible in the heating process, and filtering large boiling particles in the evaporation process to avoid splashing on the substrate, making the film layer grow more delicate and better in quality, and avoiding defects on the film layer.

[0018] (2) The heat conducting pieces in the quartz crucible of the application are stacked in multiple layers, one of the two adjacent heat conducting pieces is provided with a limiting column, and the other is provided with a limiting hole matched with the limiting column, such as the upper end of the lower heat conducting piece is provided with a limiting column, and the lower end of the upper heat conducting piece is provided with a limiting hole; and when the limiting column is inserted into the limiting hole, the through hole on the upper heat conducting piece is arranged opposite to the through hole on the lower heat conducting piece. Thus, the heat conducting piece is matched with the quartz crucible of different heights, and the adaptability of the quartz crucible and the heat conducting piece is improved.

[0019] (3) The heat conducting piece in the quartz crucible of the application comprises an inner heat conducting piece and an outer heat conducting piece, the outer diameter of the inner heat conducting piece is the same as the inner diameter of the outer heat conducting piece, one of the inner heat conducting piece and the outer heat conducting piece is provided with a limiting guide groove, and the other is provided with a limiting block matched with the limiting guide groove; when it is needed to adapt to different diameter crucibles, the outer heat conducting piece can be sleeved on the inner heat conducting piece, so that the heat conducting piece is matched with the quartz crucible of different diameters, and the adaptability of the quartz crucible and the heat conducting piece is further improved. BRIEF DESCRIPTION OF DRAWINGS

[0020] In order to more clearly illustrate the technical solutions in the embodiments of the application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description are only some embodiments of the application, and for those skilled in the art, other drawings can also be obtained without creative labor on the basis of these drawings.

[0021] Figure 1 The overall structure diagram (one) of the crucible assembly provided by an embodiment of the application;

[0022] Figure 2 The overall structure diagram (two) of the crucible assembly provided by an embodiment of the application;

[0023] Figure 3 The sleeving structure diagram of the inner heat conducting piece and the outer heat conducting piece provided by an embodiment of the application;

[0024] Among them: 1-quartz crucible, 2-heat conducting piece, 21-through hole, 22-upper heat conducting piece, 23-lower heat conducting piece, 231-limiting column, 24-inner heat conducting piece, 241-limiting block, 25-outer heat conducting piece, 251-limiting guide groove, 3-filtering piece, 31-lifting handle. DETAILED DESCRIPTION

[0025] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application.

[0026] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application. Figure 1 The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application. Figure 3 The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application.

[0027] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application. Figures 1 to 3 The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application. The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application.

[0028] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application. The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application.

[0029] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application. Figure 2 The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the protection scope of the present application. Figure 1As shown, the upper end of the lower heat-conducting member 23 of the two adjacent heat-conducting members 2 is provided with two limiting columns 231, and the two limiting columns 231 are symmetrically arranged. The lower end of the upper heat-conducting member 22 is provided with two limiting holes, and the two limiting holes are also symmetrically arranged. When the limiting column 231 is inserted into the limiting hole, the through hole on the upper heat-conducting member 22 and the through hole on the lower heat-conducting member 23 are arranged one-to-one. In another example, the upper end of the lower heat-conducting member 23 of the two adjacent heat-conducting members 2 is provided with three limiting columns 231, and the three limiting columns 231 are circumferentially uniformly arranged. The lower end of the upper heat-conducting member 22 is provided with three limiting holes, and the three limiting holes are also circumferentially uniformly arranged. When the three limiting columns 231 are respectively inserted into the three limiting holes, the through hole on the upper heat-conducting member 22 and the through hole on the lower heat-conducting member 23 are arranged one-to-one. The present application realizes the matching of the heat-conducting member 2 and the quartz crucible 1 with different heights through the arrangement of the limiting column and the limiting hole, improves the adaptability of the quartz crucible 1 and the heat-conducting member 2, and also makes the assembly of the stacked multiple heat-conducting members 2 more convenient.

[0030] Referring to Figure 3 In some other embodiments, the heat-conducting member 2 in the quartz crucible 1 comprises an inner heat-conducting member 24 and an outer heat-conducting member 25 sleeved outside the inner heat-conducting member 24. The outer diameter of the inner heat-conducting member 24 is the same as the inner diameter of the outer heat-conducting member 25. One of the inner heat-conducting member 24 and the outer heat-conducting member 25 is provided with a limiting guide groove 251, and the other is provided with a limiting block 241 matched with the limiting guide groove 251. For example, at least two limiting blocks 241 axially extending are arranged on the outer side wall of the inner heat-conducting member 24, and the outer heat-conducting member 25 is provided with a limiting guide groove 251 corresponding to the limiting block 241. When it is necessary to adapt to quartz crucibles 1 with different diameters, the outer heat-conducting member 25 can be sleeved outside the inner heat-conducting member 24, so as to realize the matching of the heat-conducting member 2 and the quartz crucible 1 with different diameters, and further improve the adaptability of the quartz crucible 1 and the heat-conducting member 2. In order to improve the capacity of the evaporation source, a plurality of through holes 21 are circumferentially arranged on the outer heat-conducting member 25 in the present embodiment. When the inner heat-conducting member 24 and the outer heat-conducting member 25 are assembled into one, the distribution of the through holes 21 is more uniform.

[0031] In some embodiments, the filter 3 is a filter screen, and the mesh number of the filter screen is 100-500 meshes. It can be understood that the higher the mesh number of the filter screen is, the greater the inhibition on the evaporation rate will be. Therefore, the mesh number of the filter screen of the present application is preferably between 100 meshes and 500 meshes.

[0032] In some embodiments, the cross section of the through hole 21 is one or more of circular, polygonal, sector, elliptical; preferably, the cross section of the through hole 21 is hexagonal, which can increase the contact area of the heat conducting piece 2 with the material and quickly transfer the heat on the heat conducting piece 2 to the material. The purpose of the through hole 21 in the present application is to form a plurality of small evaporation areas in the quartz crucible 1, so that the heat of the quartz crucible 1 is quickly transferred to the evaporation source, and the conduction heat efficiency of the evaporation source is improved. The shape and size of the through hole 21 are not limited in the present application, as long as the evaporation source can be accommodated.

[0033] In some embodiments, the plurality of through holes 21 on the heat conducting piece 2 are arranged in a honeycomb shape, which makes the through holes on the heat conducting piece 2 more dense and the divided evaporation areas more, so that the heat transfer can be better achieved.

[0034] In some embodiments, the upper end of the filter 3 is provided with a handle, which is used to facilitate the installation and removal of the filter when the filter 3 is vertically placed in the quartz crucible 1 and is relatively fixed with the quartz crucible 1. When the filter 3 is connected in the quartz crucible 1 and is relatively fixed with the quartz crucible 1, the handle 31 is also used to facilitate the movement of the entire quartz crucible 1.

[0035] In some embodiments, the heat conducting piece 2 is made of one of stainless steel, tungsten, tantalum, and quartz, and the material for making the heat conducting piece 2 requires that the gasification melting temperature under vacuum should not be lower than that of the perovskite raw material, and the heat conductivity should be good; the filter 3 is made of stainless steel, but is not limited thereto, and can also be made of other high-temperature resistant materials, but the material for making the filter 3 should not react with and corrode the perovskite raw material.

[0036] In some embodiments, in order to match the charging capacity of the quartz crucible 1 and leave installation space for the filter 3, the height of the plurality of heat conducting pieces 2 arranged in a stack is 3 / 5-4 / 5 of the internal depth of the quartz crucible 1.

[0037] The use steps of the crucible assembly are as follows:

[0038] S1: The cleaned quartz crucible 1 is prepared in advance, for example, the outer diameter of the quartz crucible 1 is 12 mm and the height is 25 mm, and the heat conducting piece 2 with the through hole 21 corresponding to the quartz crucible 1 is selected, the height of the heat conducting piece 2 is 20 mm, the outer diameter is 10 mm, and the through hole 21 is in a hexagonal structure, and the width of the hexagonal structure is 1.8 mm. The heat conducting piece 2 is placed in the quartz crucible 1. It should be noted that the heat conducting piece 2 is cleaned by ultrasonic cleaning with isopropyl alcohol and treated by UV light before being placed, and the heat conducting piece 2 can be a heat conducting piece in an assembled form, which can match the quartz crucible 1.

[0039] S2: fill the perovskite evaporation raw materials such as PbI2, PbCl2, PbBr2, CsI, CsBr, etc. in the quartz crucible 1 filled with honeycomb structure, try to make the raw materials enter the through hole 21 when filling, then add a filter screen above the heat conducting part 2, the mesh number of the filter screen can be selected between 100 and 500.

[0040] S3: heat the evaporation source; the present application takes PbI2 as the evaporation source for test description, through comparison, it can be known that when the deposition rate of the evaporation source is 4A / s, the power-up power of the quartz crucible 1 without filling the heat conducting part 2 with through hole is 48.1%; the power-up power of the quartz crucible filled with the heat conducting part 2 with through hole is reduced to 44.2%, reduced by about 4%, which greatly reduces the power-up loss, and the crystal oscillator and the actual test film thickness do not change, which achieves the expected effect; at the same time, due to the reduction of power and the increase of conduction heat effect, the pre-deposition rate stable time is reduced by about 5 minutes, the overall cycle is reduced, and the utilization rate of raw materials is improved.

[0041] The above further describes the present application with specific embodiments, but it should be understood that the specific description here should not be understood as limiting the essence and scope of the present application, and various modifications of the above embodiments made by those skilled in the art after reading the present specification all belong to the scope protected by the present application.

Claims

1. A perovskite evaporation source crucible assembly, characterized in that, The quartz crucible comprises an open end, at least one heat-conducting member arranged in the quartz crucible, and a filter arranged in the quartz crucible and above the heat-conducting member, wherein the heat-conducting member is provided with a plurality of through holes penetrating from top to bottom, and the filter covers the open end of the quartz crucible.

2. The perovskite evaporation source crucible assembly of claim 1, wherein, The heat-conducting members are stacked in multiple layers, one of the two adjacent heat-conducting members is provided with a limiting column, and the other is provided with a limiting hole matched with the limiting column.

3. The perovskite evaporation source crucible assembly of claim 2, wherein, The limiting column and the limiting hole are provided in multiple sets on the two adjacent heat-conducting members, and the through holes on the two adjacent heat-conducting members are arranged in one-to-one correspondence when the limiting column is inserted into the limiting hole.

4. The perovskite evaporation source crucible assembly of claim 2, wherein, The heat-conducting member in the quartz crucible comprises an inner heat-conducting member and an outer heat-conducting member sleeved with each other, the outer diameter of the inner heat-conducting member is the same as the inner diameter of the outer heat-conducting member, one of the inner heat-conducting member and the outer heat-conducting member is provided with a limiting guide groove, and the other is provided with a limiting block matched with the limiting guide groove.

5. The perovskite evaporation source crucible assembly of claim 1, wherein, The plurality of through holes are arranged in a honeycomb shape.

6. The perovskite evaporation source crucible assembly of claim 1, wherein, The filter is a filter screen, and the mesh number of the filter screen is 100-500.

7. The perovskite evaporation source crucible assembly of claim 1, wherein, The cross section of the through hole is one or more of a circle, a polygon, a sector, and an ellipse.

8. The perovskite evaporation source crucible assembly of claim 1, wherein, The upper end of the filter is provided with a handle.

9. The perovskite evaporation source crucible assembly of claim 1, wherein, The heat-conducting member is made of one of stainless steel, tungsten, tantalum, and quartz.

10. The perovskite evaporation source crucible assembly of claim 2, wherein, The height of the plurality of stacked heat-conducting members is 3 / 5-4 / 5 of the internal depth of the quartz crucible.

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