CN107794569B - A kind of method and device thereof of polysilicon chip straight forming - Google Patents
A kind of method and device thereof of polysilicon chip straight forming Download PDFInfo
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 41
- 229920005591 polysilicon Polymers 0.000 title claims description 36
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 119
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 117
- 239000010703 silicon Substances 0.000 claims abstract description 117
- 239000007788 liquid Substances 0.000 claims abstract description 57
- 238000007711 solidification Methods 0.000 claims abstract description 30
- 230000008023 solidification Effects 0.000 claims abstract description 30
- 238000000465 moulding Methods 0.000 claims abstract description 21
- 239000002210 silicon-based material Substances 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 47
- 238000009413 insulation Methods 0.000 claims description 45
- 229910002804 graphite Inorganic materials 0.000 claims description 42
- 239000010439 graphite Substances 0.000 claims description 42
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 239000013078 crystal Substances 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 21
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 229910052594 sapphire Inorganic materials 0.000 claims description 10
- 239000010980 sapphire Substances 0.000 claims description 10
- 230000009471 action Effects 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- 238000003698 laser cutting Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims 2
- 239000004575 stone Substances 0.000 claims 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 229910052571 earthenware Inorganic materials 0.000 claims 1
- 239000000284 extract Substances 0.000 claims 1
- 230000004927 fusion Effects 0.000 claims 1
- 235000012431 wafers Nutrition 0.000 abstract description 78
- 230000008569 process Effects 0.000 abstract description 22
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 230000015572 biosynthetic process Effects 0.000 abstract description 10
- 238000005266 casting Methods 0.000 abstract description 10
- 230000008018 melting Effects 0.000 abstract description 8
- 238000002844 melting Methods 0.000 abstract description 8
- 230000006911 nucleation Effects 0.000 abstract description 8
- 238000010899 nucleation Methods 0.000 abstract description 6
- 238000003825 pressing Methods 0.000 abstract description 2
- 238000004781 supercooling Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 6
- 229910052721 tungsten Inorganic materials 0.000 description 6
- 239000010937 tungsten Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 239000012774 insulation material Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000289 melt material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000011148 porous material Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- Crystallography & Structural Chemistry (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
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Abstract
本发明为一种多晶硅片直接成型的方法及其装置。该方法具体是:利用内部压力可控的坩埚,将已经熔化的硅液铸压到特定的铸模模腔内;定向凝固块的温度低于硅的熔点温度;硅液在定向凝固块的过冷度驱动下开始从上向下定向凝固并吸附在定向凝固块形成面上;该形成面具有精细的绒面结构,可控形核,生长出的晶粒尺寸小且均匀;凝固完成后,取出带有吸附硅片的定向凝固块;调节定向凝固块腔内的压力和温度将取出的硅片释放。本发明采用具有精细绒面结构的形成面生长硅片,替代复杂的湿法制绒工艺,减少了传统制造硅片的工艺流程,提高了硅材料的利用率,有效的降低了太阳能电池的制造成本。
The invention relates to a method and a device for direct molding of a polycrystalline silicon wafer. The method specifically includes: using a crucible with controllable internal pressure, casting and pressing the molten silicon liquid into a specific mold cavity; the temperature of the directional solidified block is lower than the melting point of silicon; the supercooling of the silicon liquid in the directional solidified block Driven by high speed, it starts directional solidification from top to bottom and adsorbs on the formation surface of the directional solidification block; the formation surface has a fine suede structure, controllable nucleation, and the grown grain size is small and uniform; after solidification, take out Oriented solidified block with adsorbed silicon chips; adjust the pressure and temperature in the cavity of the directional solidified block to release the taken out silicon chips. The invention adopts the formation surface with fine textured structure to grow silicon wafers, replaces the complex wet texturing process, reduces the traditional process of manufacturing silicon wafers, improves the utilization rate of silicon materials, and effectively reduces the manufacturing cost of solar cells .
Description
技术领域technical field
本发明涉及的是一种多晶硅片直接成型的方法,具体是将硅熔液从坩埚内部直接导出到特定的模腔内并在具有绒面结构的定向凝固块形成面上结晶成硅片。The invention relates to a method for direct molding of polycrystalline silicon wafers, specifically, silicon melt is directly exported from a crucible into a specific mold cavity and crystallized into silicon wafers on a directional solidified block forming surface with a textured structure.
背景技术Background technique
多晶硅片是制造太阳能电池的重要组成部分,其质量直接影响太阳能电池的光电转化效率。多晶硅片的制造成本制约光伏产业的发展,因此提高多晶片的质量以及降低其制造成本是发展太阳能的必经之路。Polycrystalline silicon wafer is an important part of manufacturing solar cells, and its quality directly affects the photoelectric conversion efficiency of solar cells. The manufacturing cost of polycrystalline silicon wafers restricts the development of the photovoltaic industry, so improving the quality of polycrystalline silicon wafers and reducing their manufacturing costs are the only way to develop solar energy.
传统的制造定向凝固多晶硅装置如图4所示,图中,1.不锈钢外壳、2.隔热笼、3.加热器、4.氩气、5.熔体硅、6.晶体硅、7.石英坩埚、8.石墨托盘、9.定向凝固块、10.支架。该装置采用自下向上定向凝固,方法是先让多晶硅料在坩埚内融化,通过坩埚底部降温,定向凝固形成多晶硅铸锭,利用金刚线或砂浆线切割多晶硅锭形成多晶硅片,再进行清洗制绒工艺形成制作太阳能电池所需的多晶硅片。首先由于凝固过程中熔体底部和侧面都与坩埚接触,致使凝固从侧面底部都有发生,其次凝固开始缺乏诱导,凝固开始时晶粒取向就不同。最终导致存在着晶粒取向不一致的不足。该方法得到的硅片晶粒尺寸比较大,且不均匀,结晶取向不一致。而且在其制造过程中有很多坩埚和硅料的浪费和环境污染问题。例如,每个多晶硅铸锭生长过程中所使用的石英坩埚仅能使用一次,在硅锭的切割工艺时会浪费很多硅料、金刚线或砂浆线。The traditional device for manufacturing directional solidified polysilicon is shown in Figure 4. In the figure, 1. Stainless steel shell, 2. Heat insulation cage, 3. Heater, 4. Argon gas, 5. Melt silicon, 6. Crystalline silicon, 7. Quartz crucible, 8. graphite tray, 9. directional solidified block, 10. bracket. The device adopts directional solidification from bottom to top. The method is to melt the polysilicon material in the crucible first, cool down through the bottom of the crucible, and directional solidify to form a polysilicon ingot, and use a diamond wire or a mortar wire to cut the polysilicon ingot to form a polysilicon wafer, and then clean the texture. The process forms the polycrystalline silicon wafers needed to make solar cells. First of all, because the bottom and side of the melt are in contact with the crucible during the solidification process, solidification occurs from the bottom of the side, and secondly, there is no induction at the beginning of solidification, and the grain orientation is different at the beginning of solidification. Eventually lead to the existence of inconsistent grain orientation. The crystal grain size of the silicon wafer obtained by the method is relatively large and uneven, and the crystal orientation is inconsistent. And there are a lot of waste and environmental pollution problems of crucible and silicon material in its manufacturing process. For example, the quartz crucible used in the growth process of each polysilicon ingot can only be used once, and a lot of silicon material, diamond wire or mortar wire will be wasted during the cutting process of the silicon ingot.
现代技术中,有直接生长硅片技术的报道,其生长硅片的方法是利用特定的坩埚和吸附凝固装置直接从从硅的溶液里长出硅片,通过吸附凝固装置的抑制形核和限制热流的特性生长出大尺寸晶粒的硅片。该技术虽然在一定程度上减少了材料的浪费,但由于其结构简单,无法保证对温度和压力的掌控,制造的硅片的晶粒尺寸大,其内部的位错很多,光电转化效率较低,并且在硅片生长过程中硅片生长厚度不易控制。In modern technology, there are reports on the technology of directly growing silicon wafers. The method of growing silicon wafers is to use a specific crucible and an adsorption solidification device to directly grow silicon wafers from a silicon solution, and through the inhibition of nucleation and limitation of the adsorption solidification device The nature of heat flow grows silicon wafers with large grain sizes. Although this technology reduces the waste of materials to a certain extent, due to its simple structure, it cannot guarantee the control of temperature and pressure. The silicon wafers produced have a large grain size, many internal dislocations, and low photoelectric conversion efficiency. , and the silicon wafer growth thickness is not easy to control during the silicon wafer growth process.
发明内容Contents of the invention
本发明的目的是克服现有技术的不足,提供一种多晶硅片直接成型的方法。所述方法具体是:利用内部压力可控的坩埚,将已经熔化的硅液铸压到特定的模腔内;定向凝固块的温度低于硅的熔点温度;硅液在定向凝固块的过冷度驱动下开始从上向下定向凝固并吸附在定向凝固块形成面上;该形成面具有精细的绒面结构,可控形核,生长出的晶粒尺寸小且均匀;凝固完成后,取出带有吸附硅片的定向凝固块;调节定向凝固块腔内的压力和温度将取出的硅片释放。本发明采用具有精细绒面结构的形成面生长硅片,替代复杂的湿法制绒工艺,减少了传统制造硅片的工艺流程,提高了硅材料的利用率,有效的降低了太阳能电池的制造成本。The purpose of the present invention is to overcome the deficiencies of the prior art and provide a method for direct molding of polycrystalline silicon wafers. The method specifically includes: using a crucible with controllable internal pressure, casting and pressing the molten silicon liquid into a specific mold cavity; the temperature of the directional solidified block is lower than the melting point of silicon; the supercooling of the silicon liquid in the directional solidified block Driven by high speed, it starts directional solidification from top to bottom and adsorbs on the formation surface of the directional solidification block; the formation surface has a fine suede structure, controllable nucleation, and the grown grain size is small and uniform; after solidification, take out Oriented solidified block with adsorbed silicon slices; adjust the pressure and temperature in the cavity of the oriented solidified block to release the taken out silicon slices. The invention adopts the formation surface with fine textured structure to grow silicon wafers, replaces the complex wet texturing process, reduces the traditional process of manufacturing silicon wafers, improves the utilization rate of silicon materials, and effectively reduces the manufacturing cost of solar cells .
本发明解决该技术问题所采用的技术方案是:The technical solution adopted by the present invention to solve the technical problem is:
一种多晶硅片直接成型的方法,包括如下步骤:A method for direct molding of polycrystalline silicon wafers, comprising the steps of:
第一步,原料的加入The first step, the addition of raw materials
将多晶硅原料加入到所述的多晶硅片直接成型装置的坩埚中;Adding the polysilicon raw material into the crucible of the polysilicon sheet direct forming device;
第二步,原料的熔化The second step, the melting of raw materials
将上述晶体生长炉抽真空至1.33×10-4Pa~1.06×10-4Pa,启动加热器加热坩埚,在1785K~1835K,熔化坩埚中的硅料,当硅料完全融化后,保持温度20min-30min;同时设定定向凝固块腔内的温度为1685K~1690K,压强为1.33×10-4Pa~5.33×10-4Pa;Vacuum the above crystal growth furnace to 1.33×10 -4 Pa~1.06×10 -4 Pa, start the heater to heat the crucible, and melt the silicon material in the crucible at 1785K~1835K, when the silicon material is completely melted, keep the temperature for 20min -30min; at the same time, set the temperature in the cavity of the directional solidified block to be 1685K~1690K, and the pressure to be 1.33×10 -4 Pa~5.33×10 -4 Pa;
第三步,硅液的导流The third step, the diversion of silicon liquid
然后向坩埚内通氩气,使坩埚内气压在1.63×105Pa~1.83×105Pa,坩埚内的硅溶液在毛细作用和气体压力下通过导流管流入到上部的铸模模腔的容纳盒内;Then pass argon gas into the crucible so that the air pressure in the crucible is 1.63×10 5 Pa~1.83×10 5 Pa, and the silicon solution in the crucible flows into the upper part of the mold cavity through the guide tube under capillary action and gas pressure. inside the box;
第四步,定向凝固The fourth step, directional solidification
硅液填满容纳盒后,容纳盒顶部的溢流孔有硅液从硅液溢流口流出,此时降低上部定向凝固块腔内的温度和压强,使定向凝固块腔内温度1073K~1290K,压强1.33×10-4Pa~1.06×10-4Pa,则模腔内的硅液从上往下定向凝固;After the silicon liquid fills the holding box, the overflow hole on the top of the holding box has silicon liquid flowing out from the overflow port of the silicon liquid. At this time, the temperature and pressure in the upper directional solidified block cavity are lowered to make the temperature in the directional solidified block cavity 1073K~1290K , the pressure is 1.33×10 -4 Pa~1.06×10 -4 Pa, then the silicon liquid in the mold cavity is directional solidified from top to bottom;
第五步,提取定向凝固块The fifth step is to extract the directional solidified block
当降低到设定的温度和压力后10~30秒后,模腔内的硅液完全凝固后,取出底部吸附有多晶硅片的定向凝固块;After 10-30 seconds after lowering to the set temperature and pressure, after the silicon liquid in the mold cavity is completely solidified, take out the directional solidified block adsorbed on the bottom of the polysilicon wafer;
第六步,释放以及切割硅片Step 6, release and cut silicon wafer
将定向凝固块腔内的压强调至1.46×107Pa~1.66×107Pa,温度调至1480K~1500K,此时硅片在腔内压力的作用下被释放,然后使用激光切割硅片边缘部分,即可制得一种直接成型的多晶硅片。Adjust the pressure in the cavity of the directional solidified block to 1.46×10 7 Pa to 1.66×10 7 Pa, and adjust the temperature to 1480K to 1500K. At this time, the silicon wafer is released under the action of the pressure in the cavity, and then the edge of the silicon wafer is cut with a laser Part, you can make a direct molding polysilicon wafer.
一种多晶硅片直接成型装置,该装置包括定向凝固块、铸模模腔、保温屏、加热器、坩埚、石墨支架和隔热笼;A polycrystalline silicon chip direct forming device, the device comprises a directional solidified block, a casting mold cavity, a thermal insulation screen, a heater, a crucible, a graphite support and a thermal insulation cage;
其中,定向凝固块的正下方为铸模模腔;定向凝固块的下半部和铸模模腔一同置于保温屏之中;保温屏固定在隔热笼的顶盖上;隔热笼的内部,隔热笼的底板上为石墨支架,石墨支架上放置有坩埚;坩埚的顶部与隔热笼的顶盖下部相连,周围设置有加热器,并设置有通氩气孔到隔热笼外;Among them, the mold cavity is directly below the directional solidified block; the lower half of the directional solidified block and the mold cavity are placed in the insulation screen together; the insulation screen is fixed on the top cover of the heat insulation cage; inside the heat insulation cage, The bottom plate of the heat insulation cage is a graphite support, and a crucible is placed on the graphite support; the top of the crucible is connected to the lower part of the top cover of the heat insulation cage, and a heater is arranged around it, and an argon hole is provided to the outside of the heat insulation cage;
所述的定向凝固块的主体是空腔体,空腔体的顶部设置有钢罩;空腔体的外壁的中部固定有限位装置;空腔体的底部为石墨层,石墨层的下表面为形成面,所述的形成面的材质为蓝宝石材料,厚度为3~4μm,上面分布有大小相同、塔顶向下的金字塔状凸起,金字塔高为2~4μm,塔基为正方形,边长为3~5μm,金字塔状凸起之间的间隙为1~2μm,覆盖率为85~90%;The main body of the described directional solidified block is a hollow body, and the top of the hollow body is provided with a steel cover; the middle part of the outer wall of the hollow body is fixed with a limiting device; the bottom of the hollow body is a graphite layer, and the lower surface of the graphite layer is The forming surface, the material of the forming surface is sapphire material, the thickness is 3-4 μm, and there are pyramid-shaped protrusions with the same size and the top of the tower facing down, the pyramid height is 2-4 μm, the tower base is square, and the side length is 3-5 μm, the gap between the pyramid-shaped protrusions is 1-2 μm, and the coverage rate is 85-90%;
所述的铸模模腔的组成包括容纳盒和其下部的调温器;容纳盒的结构呈正方形漏斗状,漏斗的倾角角度为10°~15°;容纳盒的顶部与每一个侧壁顶部中间各有一个开口,前后对称的开口是硅液填满后的硅液溢流口,左右对称的开口是硅液流入口,每个硅液流入口均安装有一个用于传输硅液的导流管,导流管向下,穿过隔热笼的顶盖,通入到坩埚的底部;The composition of the mold cavity includes a storage box and a temperature regulator at its lower part; the structure of the storage box is a square funnel, and the inclination angle of the funnel is 10° to 15°; the top of the storage box is in the middle of the top of each side wall Each has an opening, and the front and rear symmetrical openings are the silicon liquid overflow ports after the silicon liquid is filled, and the left and right symmetrical openings are the silicon liquid inflow inlets, and each silicon liquid inflow inlet is equipped with a guide for transferring the silicon liquid Tube, the guide tube goes down, passes through the top cover of the heat insulation cage, and leads to the bottom of the crucible;
铸模模腔中容纳盒的高度为230μm~250μm。The height of the containing box in the cavity of the casting mold is 230 μm to 250 μm.
所述的石墨层的孔隙率为1%~80%;石墨层厚度为150mm~160mm。The porosity of the graphite layer is 1%-80%; the thickness of the graphite layer is 150mm-160mm.
本发明的实质性特点为:Substantive features of the present invention are:
本发明中定向凝固块为自上向下凝固装置,其形成面具有精细的绒面结构,形成面生长硅片,替代复杂的湿法制绒工艺,减少了传统制造硅片的切片、制绒等工艺流程。其中,铸模模腔与定向凝固块的使用为关键,铸模模腔与形成面具有四种特性,高纯度、耐高温、高熔点、高强度。定向凝固块底部具有特定孔隙的石墨层控制形成面压力。在定向凝固块形成面与硅熔体接触期间,形成面与硅材料不容易发生反应,形成面压力小于硅熔体材料表面的压力,控制定向凝固块温度小于熔点时,硅熔体吸附凝固在定向凝固块形成面上。在定向凝固块形成面与硅片分离时应控制形成面的压力大于硅材料表面的压力,使得形成的硅片容易与形成面彻底分离。In the present invention, the directional solidification block is a top-down solidification device, and its forming surface has a fine textured structure, and silicon wafers are grown on the forming surface, which replaces the complicated wet texturing process, and reduces the slicing and texturing of traditional silicon wafers. process flow. Among them, the use of the mold cavity and directional solidified block is the key. The mold cavity and the forming surface have four characteristics, high purity, high temperature resistance, high melting point, and high strength. A graphite layer with specific pores at the bottom of the directional solidified block controls the forming surface pressure. During the contact between the forming surface of the directional solidified block and the silicon melt, the forming surface and the silicon material are not easy to react, the pressure of the forming surface is lower than the pressure on the surface of the silicon melt material, and when the temperature of the directional solidified block is controlled to be lower than the melting point, the silicon melt is adsorbed and solidified at Directional solidification blocks form on the face. When the formation surface of the directional solidification block is separated from the silicon wafer, the pressure on the formation surface should be controlled to be greater than the pressure on the surface of the silicon material, so that the formed silicon wafer can be easily and completely separated from the formation surface.
本发明的有益效果为:The beneficial effects of the present invention are:
传统的多晶硅片制造方法是先让多晶硅料在坩埚内融化,通过坩埚底部降温,定向凝固形成多晶硅铸锭,利用金刚线或砂浆线切割多晶硅锭形成多晶硅片,再进行清洗制绒工艺形成制作太阳能电池所需的多晶硅片。本发明采用精细的绒面结构,替代复杂湿法制绒工艺,减少了传统制造硅片的切片、制绒等工艺流程。The traditional method of manufacturing polysilicon wafers is to first melt the polysilicon material in the crucible, cool down the bottom of the crucible, and directional solidify to form a polysilicon ingot, then use a diamond wire or a mortar wire to cut the polysilicon ingot to form a polysilicon wafer, and then perform a cleaning process to form a solar energy. Polycrystalline silicon wafers required for batteries. The invention adopts a fine textured texture, replaces the complex wet textured process, and reduces the traditional technological processes of slicing and texturing for silicon wafers.
与现有技术相比,本发明的优点在于,精细的绒面结构,替代复杂湿法制绒工艺,减少了传统制造硅片的工艺流程,提高了硅材料的利用率,有效的降低了太阳能电池的制造成本。与传统工艺相比,新工艺省去了晶体生长过程和成品的制绒、切片等加工过程的长时间电力控制,总共的电耗不到传统工艺的三分之二;水耗只有四分之一,使制作太阳能电池的成本降低了约四成。Compared with the prior art, the present invention has the advantages that the fine textured structure replaces the complex wet texturing process, reduces the traditional process flow for manufacturing silicon wafers, improves the utilization rate of silicon materials, and effectively reduces the cost of solar cells. manufacturing cost. Compared with the traditional process, the new process saves the long-term power control during the crystal growth process and the finished product's texturing, slicing and other processing processes, and the total power consumption is less than two-thirds of the traditional process; water consumption is only one-fourth First, the cost of making solar cells has been reduced by about 40%.
附图说明Description of drawings
图1为本发明一种多晶硅片直接成型的方法整体结构示意图。FIG. 1 is a schematic diagram of the overall structure of a method for direct molding of polycrystalline silicon wafers according to the present invention.
图2为本发明一种多晶硅片直接成型的方法所用装置中的定向凝固块结构示意图。Fig. 2 is a schematic diagram of the structure of a directional solidified block in a device used in a method for direct molding of a polycrystalline silicon wafer according to the present invention.
图3为本发明一种多晶硅片直接成型的方法所用装置中的铸模模腔示意图。3 is a schematic diagram of a mold cavity in a device used in a method for direct molding of polycrystalline silicon wafers according to the present invention.
图4为本发明一种多晶硅片直接成型的方法所用装置中的多晶硅铸锭炉炉体结构。Fig. 4 is a structure of a polycrystalline silicon ingot furnace body in a device used in a method for direct molding of polycrystalline silicon wafers according to the present invention.
图5为实施例1中得到的多晶硅片绒面结构图。FIG. 5 is a structure diagram of the textured surface of the polycrystalline silicon wafer obtained in Example 1. FIG.
具体实施方式Detailed ways
下面结合实施例和附图对本发明做进一步说明。The present invention will be further described below in conjunction with the embodiments and accompanying drawings.
请参阅图1至图3,为一种多晶硅片直接成型装置(简称晶体生长炉)的结构示意图,图1所示实施例表明,该装置包括定向凝固块1、铸模模腔2、保温屏3、加热器7、坩埚8、石墨支架9和隔热笼10;Please refer to Fig. 1 to Fig. 3, it is a kind of structure schematic diagram of polysilicon wafer direct molding device (abbreviation crystal growth furnace), and the embodiment shown in Fig. , heater 7, crucible 8, graphite support 9 and heat insulation cage 10;
其中,定向凝固块1的正下方为铸模模腔2;定向凝固块1的下半部和铸模模腔2一同置于保温屏3之中;保温屏3固定在隔热笼10的顶盖上;隔热笼10的内部,隔热笼10的底板上为石墨支架9,石墨支架9上放置有坩埚8;坩埚8的顶部与隔热笼10的顶盖下部相连,周围设置有加热器7,并设置有通氩气孔5到隔热笼10外;Wherein, directly below the directional solidification block 1 is the casting mold cavity 2; the lower half of the directional solidification block 1 and the casting mold cavity 2 are placed in the insulation screen 3 together; the insulation screen 3 is fixed on the top cover of the heat insulation cage 10 ; Inside the heat-insulating cage 10, the base plate of the heat-insulating cage 10 is a graphite support 9, and a crucible 8 is placed on the graphite support 9; , and is provided with the argon vent 5 to the outside of the heat insulation cage 10;
所述的定向凝固块1主体是材质为钢的空腔体12,空腔体12的水平截面为正方形,顶部设置有钢罩11,用于通入氩气和抽真空,控制空腔内部压力;空腔体12的外壁的中部固定有限位装置13(即限位板),限位装置13安装在保温屏3的顶部,在定向凝固块取出和放入过程中的限位装置13,用于固定定向凝固块的可拆卸装置;空腔体12的底部为石墨层14,石墨层14的下表面为形成面15,所述的形成面15的材质为蓝宝石材料,厚度为3.5μm,上面均匀分布有相同材质、大小相同、塔顶向下的金字塔状凸起,金字塔高为3μm,塔基为正方形,边长为5μm,金字塔状凸起之间的间隙为1~2μm,覆盖率为85~90%。The main body of the directional solidification block 1 is a hollow body 12 made of steel, the horizontal section of the hollow body 12 is a square, and the top is provided with a steel cover 11 for feeding argon and vacuuming to control the internal pressure of the cavity The middle part of the outer wall of the cavity body 12 is fixed with a limiter 13 (i.e. a limit plate), and the limiter 13 is installed on the top of the insulation screen 3, and the limiter 13 in the process of taking out and putting into the directional solidified block is used A detachable device for fixing and directional solidified blocks; the bottom of the cavity body 12 is a graphite layer 14, and the lower surface of the graphite layer 14 is a forming surface 15, and the material of the forming surface 15 is sapphire material with a thickness of 3.5 μm. There are evenly distributed pyramid-shaped protrusions of the same material and size with the top of the tower downward. The height of the pyramid is 3 μm, the base of the tower is square, and the side length is 5 μm. The gap between the pyramid-shaped protrusions is 1-2 μm. The coverage rate is 85-90%.
所述的石墨层的孔隙率为1%~80%;石墨层厚度为150mm~160mm;The porosity of the graphite layer is 1%-80%; the thickness of the graphite layer is 150mm-160mm;
为了更容易使硅片取出,所述的铸模模腔2的组成包括容纳盒和其下部的调温器18;容纳盒的结构呈正方形漏斗状,漏斗的倾角角度为10°~15°;容纳盒的顶部与每一个侧壁顶部中间各有一个开口,前后对称的开口是硅液填满后的硅液溢流口16(高度为40μm,宽度为100mm),左右对称的开口是硅液流入口17(高度为30μm,宽度为100mm),每个硅液流入口17均安装有一个用于传输硅液的导流管4,导流管4向下,穿过隔热笼10的顶盖,通入到坩埚8的底部;In order to make it easier to take out the silicon wafer, the composition of the mold cavity 2 includes a holding box and a temperature regulator 18 at its lower part; the structure of the holding box is a square funnel, and the inclination angle of the funnel is 10° to 15°; There is an opening in the middle of the top of the box and the top of each side wall. The front and rear symmetrical openings are the silicon liquid overflow ports 16 (height is 40 μm, and the width is 100 mm) after the silicon liquid is filled. The left and right symmetrical openings are the silicon liquid flow. Inlet 17 (height is 30 μm, width is 100mm), each silicon liquid inflow port 17 is all equipped with a guide pipe 4 for transferring silicon liquid, guide pipe 4 is downward, passes through the top cover of heat insulation cage 10 , pass into the bottom of the crucible 8;
铸模模腔2中容纳盒的高度为250μm。The height of the housing box in the mold cavity 2 was 250 μm.
所述的定向凝固块1,空腔内的压强通过通入的氩气调节是从顶部通入,其底部有一层孔隙率为1%~80%的石墨层14,在压强范围为1.33×10-4Pa~5.33×10-4Pa下,氩气可以通过石墨层,硅液不可以通过石墨层,在石墨层下表面装有一层由蓝宝石材料,制成的间隔金字塔状凸起结构的形成面15,该形成面能够承受硅熔体的高温环境,且不与硅熔体发生化学反应。当定向凝固块腔内处于低温低压状态时(温度1273K,压强为1.33×10-4Pa),由于石墨材料相比蓝宝石材料导热性强,硅液会首先吸附在金字塔状间隙的石墨层表面,然后进行形核和生长,每一个金字塔间隙都是一个形核中心,该形核中心细小且均匀,最后硅液定向凝固成为晶粒尺寸小且均匀的具有金字塔绒面的硅片。In the directional solidified block 1, the pressure in the cavity is adjusted from the top by the argon gas introduced, and there is a graphite layer 14 with a porosity of 1% to 80% at the bottom, and the pressure range is 1.33×10 -4 Pa~5.33×10 -4 Pa, argon gas can pass through the graphite layer, silicon liquid can not pass through the graphite layer, and a layer of sapphire material is installed on the lower surface of the graphite layer to form a pyramid-shaped convex structure at intervals Surface 15, the forming surface can withstand the high temperature environment of the silicon melt, and does not chemically react with the silicon melt. When the cavity of the directional solidified block is in a state of low temperature and low pressure (temperature 1273K, pressure 1.33×10 -4 Pa), since the thermal conductivity of graphite material is stronger than that of sapphire material, the silicon liquid will first be adsorbed on the surface of the graphite layer in the pyramid-shaped gap, Then carry out nucleation and growth, each pyramid gap is a nucleation center, the nucleation center is small and uniform, and finally the silicon liquid is directional solidified into a silicon wafer with a small and uniform grain size and a pyramid texture.
所述坩埚为钨坩埚。The crucible is a tungsten crucible.
所述隔热笼为石墨碳毡复合材料。The heat insulation cage is graphite carbon felt composite material.
所述连接铸模模腔与坩埚的导流管用钨材料导流管,其周围被保温材料包围。The guide tube connecting the mold cavity and the crucible is made of a tungsten material guide tube surrounded by heat-insulating materials.
所述铸模模腔为钨材料制成,其内表面非常光滑,底部连接控温模块。The cavity of the casting mold is made of tungsten material, its inner surface is very smooth, and the bottom is connected with a temperature control module.
下面给出本发明一种多晶硅片直接成型的方法的具体实施例,具体实施例仅用于详细说明本发明,并不限制本发明申请权利要求的保护范围。A specific embodiment of a method for direct molding of a polycrystalline silicon wafer according to the present invention is given below. The specific embodiment is only used to describe the present invention in detail, and does not limit the protection scope of the claims of the present invention.
实施例1Example 1
A.多晶硅片直接成型所用的晶体生长炉A. Crystal growth furnace for direct molding of polycrystalline silicon wafers
多晶硅片直接成型所用的晶体生长炉的结构如上所述,主要包括石墨支架、隔热笼、坩埚、加热器、导流管、模腔、定向凝固块;隔热笼是用石墨碳毡和钢罩制成,有很好的保温隔热作用;加热器缠绕在坩埚的外表面;导流管连接坩埚和模腔,其外部被保温材料包围;铸模模腔的侧面带有溢流孔,底部有调节温度的加热器电极;定向凝固块在凝固硅片时放在模腔顶部,其侧面带有限位装置,内部填充压力可调的氩气,底部是由多孔石墨和蓝宝石材料制成;The structure of the crystal growth furnace used for direct molding of polycrystalline silicon wafers is as above, mainly including graphite support, heat insulation cage, crucible, heater, draft tube, mold cavity, directional solidification block; heat insulation cage is made of graphite carbon felt and steel It is made of a hood, which has a good thermal insulation effect; the heater is wound on the outer surface of the crucible; the guide tube connects the crucible and the mold cavity, and its exterior is surrounded by thermal insulation materials; the side of the mold cavity has overflow holes, and the bottom There is a heater electrode to adjust the temperature; the directional solidification block is placed on the top of the mold cavity when the silicon wafer is solidified, and its side is equipped with a limit device, and the interior is filled with argon gas with adjustable pressure, and the bottom is made of porous graphite and sapphire materials;
其中,坩埚容积为0.2m3;空腔体高度为32cm,底边边长为16cm;容纳盒高度为250μm,底面积为15.6cm×15.6cm。以下实施例同。Among them, the volume of the crucible is 0.2m 3 ; the height of the cavity is 32cm, and the length of the bottom side is 16cm; the height of the containing box is 250μm, and the bottom area is 15.6cm×15.6cm. The following examples are the same.
B.操作步骤B. Operation steps
第一步,原料的加入The first step, the addition of raw materials
将400kg多晶硅原料加入到A所述的多晶硅片直接成型所用晶体生长炉的钨坩埚中,然后进行炉体密封(即使用碳毡对坩埚和石墨支架的间隙进行填充密封,与此同时关掉导流管和通氩气孔,以下实施例同);Add 400kg polysilicon raw material into the tungsten crucible of the crystal growth furnace used for the direct molding of polycrystalline silicon wafers described in A, and then seal the furnace body (that is, use carbon felt to fill and seal the gap between the crucible and the graphite support, and at the same time turn off the guide Flow tube and argon hole, the following examples are the same);
第二步,原料的熔化The second step, the melting of raw materials
将上述晶体生长炉的坩埚8内抽真空至1.33×10-4Pa,启动A所述的加热器加热晶体生长炉中的专用坩埚,其加热功率为105KW,加热温度达到1785K连续加热15小时,完全熔化第一步中加热专用坩埚中的硅料,然后继续维持20分钟;同时,设定定向凝固块腔内的温度为1685K,压强为1.33×10-4Pa。Vacuumize the crucible 8 of the above-mentioned crystal growth furnace to 1.33×10 -4 Pa, start the heater described in A to heat the special crucible in the crystal growth furnace, the heating power is 105KW, and the heating temperature reaches 1785K for continuous heating for 15 hours. Completely melt the silicon material in the special heating crucible in the first step, and then maintain it for 20 minutes; at the same time, set the temperature in the cavity of the directional solidified block to 1685K and the pressure to 1.33×10 -4 Pa.
第三步,硅液的导流The third step, the diversion of silicon liquid
当硅料完全融化后,向坩埚内通氩气,使坩埚内气压在1.63×105Pa,坩埚内的硅溶液在毛细作用和气体压力下通过导流管流入到上部的铸模平台的模腔内;When the silicon material is completely melted, pass argon gas into the crucible so that the pressure in the crucible is 1.63×10 5 Pa, and the silicon solution in the crucible flows into the mold cavity of the upper casting mold platform through the guide tube under capillary action and gas pressure Inside;
第四步,定向凝固The fourth step, directional solidification
硅液填满模腔后,顶部的溢流孔有硅液流出,此时关闭导流管,阻止硅液的继续流入。降低上部定向凝固块腔内的温度和压强(通过保温屏3的调温作用来降低腔内温度,并向腔内通入氩气来改变腔内压强,进而达到晶体生长所需条件。)使定向凝固块腔内温度1273K,压强1.33×10-4Pa,模腔内的硅液从上往下定向凝固;After the silicon liquid fills the mold cavity, the silicon liquid flows out from the overflow hole on the top. At this time, the guide tube is closed to prevent the silicon liquid from continuing to flow in. Reduce the temperature and pressure in the cavity of the upper directional solidified block (the temperature in the cavity is reduced by the temperature adjustment effect of the insulation screen 3, and argon gas is introduced into the cavity to change the pressure in the cavity, so as to achieve the required conditions for crystal growth.) The temperature in the directional solidified block cavity is 1273K, the pressure is 1.33×10 -4 Pa, and the silicon liquid in the mold cavity is directional solidified from top to bottom;
第五步,提取定向凝固块The fifth step is to extract the directional solidified block
在降温降压20秒后,模腔内的硅液已经完全凝固后,取出形成面上吸附有多晶硅片的定向凝固块;After lowering the temperature and reducing the pressure for 20 seconds, after the silicon liquid in the mold cavity has completely solidified, take out the directional solidified block on which the polysilicon wafer is adsorbed on the formed surface;
第六步,释放以及切割硅片Step 6, release and cut silicon wafer
将定向凝固块腔内的压强调至1.66×107Pa,温度调至1480K,此时硅片在腔内压力和高温的作用下被释放,然后使用激光切割硅片边缘部分激光切割修整硅片四周的毛边,然后进行抛光处理,即可制得一种直接成型的多晶硅片。得到的硅片厚度为200μm~210μm。Adjust the pressure in the cavity of the directional solidified block to 1.66×10 7 Pa, and adjust the temperature to 1480K. At this time, the silicon wafer is released under the action of the pressure and high temperature in the cavity, and then laser cutting is used to trim the edge of the silicon wafer. The surrounding burrs are then polished to produce a direct-molded polysilicon wafer. The obtained silicon wafer has a thickness of 200 μm to 210 μm.
得到的多晶硅片绒面结构如图5所示,从图中可以看到制绒率接近90%,符合预期的结果。由于定向凝固块的蓝宝石材质形成面在晶体生长过程中充当形核位点,起到了诱导形核的作用,从而形成均匀的小尺寸晶粒。众所周知,小尺寸晶粒形成的晶界多、位错少。综合位错和晶界的影响,小尺寸的均匀的柱状晶所制造的太阳能电池的光电转化效率更高。The textured structure of the obtained polycrystalline silicon wafer is shown in Figure 5, and it can be seen from the figure that the textured rate is close to 90%, which is in line with the expected result. Since the sapphire material formation surface of the directional solidified block acts as a nucleation site during the crystal growth process, it plays a role in inducing nucleation, thereby forming uniform small-sized grains. It is well known that small-sized grains form more grain boundaries and fewer dislocations. Combined with the influence of dislocations and grain boundaries, the photoelectric conversion efficiency of solar cells manufactured by small-sized uniform columnar crystals is higher.
实施例2Example 2
A.多晶硅片直接成型所用的晶体生长炉A. Crystal growth furnace for direct molding of polycrystalline silicon wafers
多晶硅片直接成型所用的晶体生长炉的结构主要包括石墨支架、隔热笼、坩埚、加热器、导流管、模腔、定向凝固块;隔热笼是用石墨碳毡和钢罩制成,有很好的保温隔热作用;加热器缠绕在坩埚的外表面;导流管连接坩埚和模腔,其外部被保温材料包围;铸模模腔的侧面带有溢流孔,底部有调节温度的加热器电极;定向凝固块在凝固硅片时放在模腔顶部,其侧面带有限位装置,内部填充压力可调的氩气,底部是由多孔石墨和蓝宝石材料制成;The structure of the crystal growth furnace used for direct molding of polycrystalline silicon wafers mainly includes graphite brackets, heat insulation cages, crucibles, heaters, draft tubes, mold cavities, and directional solidified blocks; heat insulation cages are made of graphite carbon felt and steel covers. It has a good thermal insulation effect; the heater is wound on the outer surface of the crucible; the guide tube connects the crucible and the mold cavity, and its exterior is surrounded by thermal insulation materials; the side of the mold cavity has an overflow hole, and the bottom has a temperature adjustment Heater electrode; the directional solidification block is placed on the top of the mold cavity when the silicon wafer is solidified, and its side is equipped with a limit device, and the interior is filled with argon gas with adjustable pressure, and the bottom is made of porous graphite and sapphire materials;
B.操作步骤B. Operation steps
第一步,原料的加入The first step, the addition of raw materials
将400kg多晶硅原料加入到A所述的多晶硅片直接成型所用晶体生长炉的钨坩埚中,然后进行炉体密封;Add 400kg of polysilicon raw material into the tungsten crucible of the crystal growth furnace used for the direct molding of polysilicon wafers described in A, and then seal the furnace body;
第二步,原料的熔化The second step, the melting of raw materials
将上述晶体生长炉的坩埚8内抽真空至1.33×10-4Pa,启动A所述的加热器加热晶体生长炉中的专用坩埚,其加热功率为105KW,加热温度达到1785K连续加热15小时,完全熔化第一步中加热专用坩埚中的硅料,然后继续维持20分钟;同时,设定定向凝固块腔内的温度为1685K,压强为1.33×10-4Pa。Vacuumize the crucible 8 of the above-mentioned crystal growth furnace to 1.33×10 -4 Pa, start the heater described in A to heat the special crucible in the crystal growth furnace, the heating power is 105KW, and the heating temperature reaches 1785K for continuous heating for 15 hours. Completely melt the silicon material in the special heating crucible in the first step, and then maintain it for 20 minutes; at the same time, set the temperature in the cavity of the directional solidified block to 1685K and the pressure to 1.33×10 -4 Pa.
第三步,硅液的导流The third step, the diversion of silicon liquid
当硅料完全融化后,向坩埚内通氩气,使坩埚内气压在1.63×105Pa,坩埚内的硅溶液在毛细作用和气体压力下通过导流管流入到上部的铸模平台的模腔内;When the silicon material is completely melted, pass argon gas into the crucible so that the pressure in the crucible is 1.63×10 5 Pa, and the silicon solution in the crucible flows into the mold cavity of the upper casting mold platform through the guide tube under capillary action and gas pressure Inside;
第四步,定向凝固The fourth step, directional solidification
硅液填满模腔后,顶部的溢流孔有硅液流出,此时关闭导流管,阻止硅液的继续流入。降低上部定向凝固块腔内的温度和压强(通过保温屏3的调温作用来降低腔内温度,并向腔内通入氩气来改变腔内压强,进而达到晶体生长所需条件。)使定向凝固块腔内温度1173K,压强1.06×10-4Pa,模腔内的硅液从上往下定向凝固;After the silicon liquid fills the mold cavity, the silicon liquid flows out from the overflow hole on the top. At this time, the guide tube is closed to prevent the silicon liquid from continuing to flow in. Reduce the temperature and pressure in the cavity of the upper directional solidified block (the temperature in the cavity is reduced by the temperature adjustment effect of the insulation screen 3, and argon gas is introduced into the cavity to change the pressure in the cavity, so as to achieve the required conditions for crystal growth.) The temperature in the directional solidified block cavity is 1173K, the pressure is 1.06×10 -4 Pa, and the silicon liquid in the mold cavity is directional solidified from top to bottom;
第五步,提取定向凝固块The fifth step is to extract the directional solidified block
在降温降压15秒后,模腔内的硅液已经完全凝固后,取出形成面上吸附有多晶硅片的定向凝固块;After lowering the temperature and reducing the pressure for 15 seconds, after the silicon liquid in the mold cavity has completely solidified, take out the directional solidified block on which the polysilicon wafer is adsorbed on the formed surface;
第六步,释放以及切割硅片Step 6, release and cut silicon wafer
将定向凝固块腔内的压强调至1.66×107Pa,温度调至1480K,此时硅片在腔内压力和高温的作用下被释放,然后使用激光切割硅片边缘部分激光切割修整硅片四周的毛边,然后进行抛光处理,即可制得一种直接成型的多晶硅片。得到的硅片厚度为200μm~210μm。Adjust the pressure in the cavity of the directional solidified block to 1.66×10 7 Pa, and adjust the temperature to 1480K. At this time, the silicon wafer is released under the action of the pressure and high temperature in the cavity, and then laser cutting is used to trim the edge of the silicon wafer. The surrounding burrs are then polished to produce a direct-molded polysilicon wafer. The obtained silicon wafer has a thickness of 200 μm to 210 μm.
得到的多晶硅片绒面结构同实施例1。The textured structure of the obtained polycrystalline silicon wafer is the same as in Example 1.
实施例3Example 3
A.多晶硅片直接成型所用的晶体生长炉A. Crystal growth furnace for direct molding of polycrystalline silicon wafers
多晶硅片直接成型所用的晶体生长炉的结构主要包括石墨支架、隔热笼、坩埚、加热器、导流管、模腔、定向凝固块;隔热笼是用石墨碳毡和钢罩制成,有很好的保温隔热作用;加热器缠绕在坩埚的外表面;导流管连接坩埚和模腔,其外部被保温材料包围;铸模模腔的侧面带有溢流孔,底部有调节温度的加热器电极;定向凝固块在凝固硅片时放在模腔顶部,其侧面带有限位装置,内部填充压力可调的氩气,底部是由多孔石墨和蓝宝石材料制成;The structure of the crystal growth furnace used for direct molding of polycrystalline silicon wafers mainly includes graphite brackets, heat insulation cages, crucibles, heaters, draft tubes, mold cavities, and directional solidified blocks; heat insulation cages are made of graphite carbon felt and steel covers. It has a good thermal insulation effect; the heater is wound on the outer surface of the crucible; the guide tube connects the crucible and the mold cavity, and its exterior is surrounded by thermal insulation materials; the side of the mold cavity has an overflow hole, and the bottom has a temperature adjustment Heater electrode; the directional solidification block is placed on the top of the mold cavity when the silicon wafer is solidified, and its side is equipped with a limit device, and the interior is filled with argon gas with adjustable pressure, and the bottom is made of porous graphite and sapphire materials;
B.操作步骤B. Operation steps
第一步,原料的加入The first step, the addition of raw materials
将400kg多晶硅原料加入到A所述的多晶硅片直接成型所用晶体生长炉的钨坩埚中,然后进行炉体密封;Add 400kg of polysilicon raw material into the tungsten crucible of the crystal growth furnace used for the direct molding of polysilicon wafers described in A, and then seal the furnace body;
第二步,原料的熔化The second step, the melting of raw materials
将上述晶体生长炉的坩埚8内抽真空至1.33×10-4Pa,启动A所述的加热器加热晶体生长炉中的专用坩埚,其加热功率为105KW,加热温度达到1785K连续加热15小时,完全熔化第一步中加热专用坩埚中的硅料,然后继续维持20分钟;同时,设定定向凝固块腔内的温度为1685K,压强为1.33×10-4Pa。Vacuumize the crucible 8 of the above-mentioned crystal growth furnace to 1.33×10 -4 Pa, start the heater described in A to heat the special crucible in the crystal growth furnace, the heating power is 105KW, and the heating temperature reaches 1785K for continuous heating for 15 hours. Completely melt the silicon material in the special heating crucible in the first step, and then maintain it for 20 minutes; at the same time, set the temperature in the cavity of the directional solidified block to 1685K and the pressure to 1.33×10 -4 Pa.
第三步,硅液的导流The third step, the diversion of silicon liquid
当硅料完全融化后,向坩埚内通氩气,使坩埚内气压在1.63×105Pa,坩埚内的硅溶液在毛细作用和气体压力下通过导流管流入到上部的铸模平台的模腔内;When the silicon material is completely melted, pass argon gas into the crucible so that the pressure in the crucible is 1.63×10 5 Pa, and the silicon solution in the crucible flows into the mold cavity of the upper casting mold platform through the guide tube under capillary action and gas pressure Inside;
第四步,定向凝固The fourth step, directional solidification
硅液填满模腔后,顶部的溢流孔有硅液流出,此时关闭导流管,阻止硅液的继续流入。降低上部定向凝固块腔内的温度和压强(通过保温屏3的调温作用来降低腔内温度,并向腔内通入氩气来改变腔内压强,进而达到晶体生长所需条件。)使定向凝固块腔内温度1073K,压强1.33×10-4Pa,模腔内的硅液从上往下定向凝固;After the silicon liquid fills the mold cavity, the silicon liquid flows out from the overflow hole on the top. At this time, the guide tube is closed to prevent the silicon liquid from continuing to flow in. Reduce the temperature and pressure in the cavity of the upper directional solidified block (the temperature in the cavity is reduced by the temperature adjustment effect of the insulation screen 3, and argon gas is introduced into the cavity to change the pressure in the cavity, so as to achieve the required conditions for crystal growth.) The temperature in the directional solidified block cavity is 1073K, the pressure is 1.33×10 -4 Pa, and the silicon liquid in the mold cavity is directional solidified from top to bottom;
第五步,提取定向凝固块The fifth step is to extract the directional solidified block
在降温降压10秒后,模腔内的硅液已经完全凝固后,取出形成面上吸附有多晶硅片的定向凝固块;After lowering the temperature and reducing the pressure for 10 seconds, after the silicon liquid in the mold cavity has completely solidified, take out the directional solidified block on which the polysilicon wafer is adsorbed on the formed surface;
第六步,释放以及切割硅片Step 6, release and cut silicon wafer
将定向凝固块腔内的压强调至1.66×107Pa,温度调至1480K,此时硅片在腔内压力和高温的作用下被释放,然后使用激光切割硅片边缘部分激光切割修整硅片四周的毛边,然后进行抛光处理,即可制得一种直接成型的多晶硅片。得到的硅片厚度为200μm~210μm。Adjust the pressure in the cavity of the directional solidified block to 1.66×10 7 Pa, and adjust the temperature to 1480K. At this time, the silicon wafer is released under the action of the pressure and high temperature in the cavity, and then laser cutting is used to trim the edge of the silicon wafer. The surrounding burrs are then polished to produce a direct-molded polysilicon wafer. The obtained silicon wafer has a thickness of 200 μm to 210 μm.
得到的多晶硅片绒面结构同实施例1。The textured structure of the obtained polycrystalline silicon wafer is the same as in Example 1.
以上所述具体实施例对本发明的技术方案和实施办法做了进一步地详细说明,以上实例并不仅用于本发明,凡是在本发明的精神和原则之内进行的同等修改、等效替换、改进等均应该在本发明的保护范围之内。The specific embodiments described above have further described the technical solutions and implementation methods of the present invention in detail. The above examples are not only used in the present invention, and all equivalent modifications, equivalent replacements, and improvements are carried out within the spirit and principles of the present invention. etc. should be within the protection scope of the present invention.
本发明未尽事宜为公知技术。Matters not covered in the present invention are known technologies.
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