CN107855923B - The polishing method of organic inorganic hybridization halide perovskite semiconductor crystal - Google Patents

The polishing method of organic inorganic hybridization halide perovskite semiconductor crystal Download PDF

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CN107855923B
CN107855923B CN201711083278.XA CN201711083278A CN107855923B CN 107855923 B CN107855923 B CN 107855923B CN 201711083278 A CN201711083278 A CN 201711083278A CN 107855923 B CN107855923 B CN 107855923B
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polishing
crystal
isopropanol
smooth
mapbbr
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CN107855923A (en
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徐亚东
刘欣
张滨滨
李乐琪
张洪健
介万奇
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NANJING GONGCHENG ENERGY SAVING NEW MATERIAL RESEARCH INSTITUTE Co.,Ltd.
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Northwest University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
    • B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/07—Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool
    • B24B37/10—Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool for single side lapping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
    • B24B7/20—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
    • B24B7/22—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
    • B24B7/228—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain for grinding thin, brittle parts, e.g. semiconductors, wafers

Abstract

The invention discloses a kind of polishing method of organic inorganic hybridization halide perovskite semiconductor crystal, the technical issues of the practicability is poor for solving existing semiconductor crystal polishing method.Technical solution is laid in rubber pad on two polishing disks；The MAPbBr that will be grown from solwution method3Crystal is placed on first polishing disk, and 1~3 milliliter of WD-40 polishing fluid is sprayed on rubber pad, is drawn " 8 " word with finger and is carried out grinding and polishing, polishes 300~1000 seconds to chip two sides, rinsed immediately with isopropanol respectively later；The crystal after WD-40 is polished is placed on second polishing disk again, 3~5ml of polishing fluid isopropanol is added dropwise, carries out chemical polishing in the same way, when smooth when plane of crystal, smooth, no marking, grinding and polishing is finished.It is rinsed immediately with isopropanol later, high pure nitrogen drying.Due to successively polishing using two kinds of polishing fluids, new residual will not be generated, practicability is good.

Description

The polishing method of organic inorganic hybridization halide perovskite semiconductor crystal
Technical field
The present invention relates to a kind of semiconductor crystal polishing method, in particular to a kind of organic inorganic hybridization halide perovskite The polishing method of semiconductor crystal.
Background technique
Organic inorganic hybridization halide perovskite MAPbX3Material is in LED, solar battery, photodetector, nuclear radiation The fields such as detection are widely used.Solwution method is generallyd use to prepare the halide perovskite crystal of hydridization.Solwution method is spontaneous The crystal of nucleation and seeded growth, due to the difference of growth conditions, the growth rate of different crystal faces has difference, and the crystal of acquisition is in Multiple rule three-dimensional configuration is unfavorable for the preparation of planar device.The large-sized crystal obtained, it is also desirable to prepare and advance in device Row is suitably cut out.The crystal that solwution method obtains, surface often have solution residual, and the volatilization of residual solution is easy to bring surface Crystallization causes surface irregularity.In addition, crystal the problems such as there may be the adhesions of crystal of solwution method preparation.
MAPbX3In crystal growth from solution and cutting process, many surface defects are brought, the macrostructure including growth Enrichment of the defect on surface, surface damage caused by polycrystalline, stray crystal and the contamination of surface deposition, the cutting of crystalline material etc..And The perovskite crystal of organic inorganic hybridization and common solvent, including water, ethyl alcohol, acetone etc. can all react, this gives crystal Following process, especially mill, throwing processing brings difficulty.Unprocessed or simple solvent-free mill, throwing, will lead to MAPbX3It is brilliant Light, the electrical property of body are degenerated, such as are reduced the transmitance of crystal, increased the leakage current of device, and the performance of its device is seriously affected. Therefore, develop a kind of novel solvent mill, throwing method for organic inorganic hybridization halide perovskite crystal late device Prepare most important.
Document 1 " Chinese patent that number of patent application is 201710277234.4 " discloses a kind of CdZnTe planar detector Surface treatment method, magnesia are effectively reduced as polishing fluid by the method for the surface treatments such as rough polishing, fine polishing, passivation The leakage current of CdZnTe wafer surface, improves energy resolution, improves the detection efficient of CdZnTe planar detector.
The document illustrates the necessity of crystal surface treatment, effectively reduces the leakage current of CdZnTe wafer surface, mentions High energy resolution, improves the detection efficient of CdZnTe planar detector.But about organic inorganic hybridization MAPbX3Crystal Surface solvent mill, throw method currently without report.
Summary of the invention
In order to overcome the shortcomings of existing semiconductor crystal polishing method, the practicability is poor, and it is miscellaneous that the present invention provides a kind of organic-inorganic Change the polishing method of halide perovskite semiconductor crystal.Rubber pad is laid on two polishing disks by this method；It will be from solution The MAPbBr that method is grown3Crystal is placed on first polishing disk, and 1~3 milliliter of WD-40 polishing fluid is sprayed on rubber pad, uses finger It draws " 8 " word and carries out grinding and polishing, chip two sides is polished 300~1000 seconds respectively, is rinsed immediately with isopropanol later；It will pass through again Crystal after WD-40 polishing is placed on second polishing disk, and 3~5ml of polishing fluid isopropanol is added dropwise, is changed in the same way Optical polishing, when smooth when plane of crystal, smooth, no marking, grinding and polishing is finished.It is rinsed immediately with isopropanol later, High Purity Nitrogen air-blowing It is dry.Due to successively polishing using two kinds of polishing fluids, new residual will not be generated, practicability is good.
The technical solution adopted by the present invention to solve the technical problems: a kind of organic inorganic hybridization halide perovskite is partly led The polishing method of body crystal, its main feature is that the following steps are included:
Rubber pad is laid on two polishing disks；The MAPbBr that will be grown from solwution method3Crystal is placed on first polishing On disk, 1~3 milliliter of WD-40 polishing fluid is sprayed on rubber pad, is drawn 8 words with finger and is carried out grinding and polishing, to MAPbBr3Crystal two sides point Pao Guang not be 300~1000 seconds, it is rinsed immediately with isopropanol later；Again by the MAPbBr after WD-40 is polished3Crystal is placed on On two polishing disks, 3~5ml of isopropanol polishing fluid is added dropwise, carries out chemical polishing in the same way, smooth to plane of crystal, It when smooth, no marking, is rinsed with isopropanol, high pure nitrogen drying, and is stored in vacuum desiccator.
The beneficial effects of the present invention are: rubber pad is laid on two polishing disks by this method；By what is grown from solwution method MAPbBr3Crystal is placed on first polishing disk, on rubber pad spray 1~3 milliliter of WD-40 polishing fluid, with finger draw " 8 " word into Row grinding and polishing polishes chip two sides respectively 300~1000 seconds, is rinsed immediately with isopropanol later；It again will be after WD-40 be polished Crystal be placed on second polishing disk, be added dropwise 3~5ml of polishing fluid isopropanol, chemical polishing is carried out in the same way, to crystalline substance Body surface face is smooth, smooth, no marking when, grinding and polishing finishes.It is rinsed immediately with isopropanol later, high pure nitrogen drying.Due to first Kind polishing fluid WD-40 slushing compound has antirust, dehumidifying, solution rust, lubrication, cleans, conductance six functions, and can be uniform It is distributed in plane of crystal, does not glue solid particle, keeps permanent lubrication so as to be attached to plane of crystal.In addition rubber polishing pad Use, reduce MAPbBr3The possibility of the secondary scuffing of perovskite crystal, reduces MAPbBr3Perovskite crystal burnishing surface is coarse Degree.In addition, because having used second of polishing fluid isopropanol that can remove the plane of crystal after the first polishing fluid WD-40 polishing The WD-40 of generation is remained, and the new residual that will not be generated leads to crystalline material penalty.The MAPbBr of acquisition3Plane of crystal Smooth, permeability is good, improves the resistivity of crystal, finds resistivity up to 10 after tested8Ω cm magnitude, practicability It is good.
It elaborates with reference to the accompanying drawings and detailed description to the present invention.
Detailed description of the invention
Fig. 1 is perovskite MAPbBr in embodiment of the present invention method 53The ultraviolet-visible light of crystal-near-infrared datagram.
Fig. 2 is perovskite MAPbBr in embodiment of the present invention method 53The IV characteristic curve of crystal.
Specific embodiment
Following embodiment referring to Fig.1-2.
Embodiment 1: rubber pad is laid on two polishing disks；The MAPbBr that will be grown from solwution method3Crystal is placed on On one polishing disk, 1 milliliter of WD-40 polishing fluid is sprayed on rubber pad, is drawn " 8 " word with finger and is carried out grinding and polishing, to chip two sides point Pao Guang not be 600 seconds, it is rinsed immediately with isopropanol later；The crystal after WD-40 is polished is placed on second polishing disk again, Polishing fluid isopropanol 5ml is added dropwise, carries out chemical polishing in the same way, when smooth when plane of crystal, smooth, no marking, mill Throwing finishes.It is rinsed with isopropanol, high pure nitrogen drying, and is stored in vacuum desiccator immediately later.
Embodiment 2: rubber pad is laid on two polishing disks；The MAPbBr that will be grown from solwution method3Crystal is placed on On one polishing disk, 3 milliliters of WD-40 polishing fluid are sprayed on rubber pad, are drawn " 8 " word with finger and are carried out grinding and polishing, to chip two sides point Pao Guang not be 600 seconds, it is rinsed immediately with isopropanol later；The crystal after WD-40 is polished is placed on second polishing disk again, Polishing fluid isopropanol 5ml is added dropwise, carries out chemical polishing in the same way, when smooth when plane of crystal, smooth, no marking, mill Throwing finishes.It is rinsed with isopropanol, high pure nitrogen drying, and is stored in vacuum desiccator immediately later.
Embodiment 3: rubber pad is laid on two polishing disks；The MAPbBr that will be grown from solwution method3Crystal is placed on On one polishing disk, 3 milliliters of WD-40 polishing fluid are sprayed on rubber pad, are drawn " 8 " word with finger and are carried out grinding and polishing, to chip two sides point Pao Guang not be 300 seconds, it is rinsed immediately with isopropanol later；The crystal after WD-40 is polished is placed on second polishing disk again, Polishing fluid isopropanol 4ml is added dropwise, carries out chemical polishing in the same way, when smooth when plane of crystal, smooth, no marking, mill Throwing finishes.It is rinsed with isopropanol, high pure nitrogen drying, and is stored in vacuum desiccator immediately later.
Embodiment 4: rubber pad is laid on two polishing disks；The MAPbBr that will be grown from solwution method3Crystal is placed on On one polishing disk, 2 milliliters of WD-40 polishing fluid are sprayed on rubber pad, are drawn " 8 " word with finger and are carried out grinding and polishing, to chip two sides point Pao Guang not be 1000 seconds, it is rinsed immediately with isopropanol later；The crystal after WD-40 is polished is placed on second polishing disk again On, polishing fluid isopropanol 4ml is added dropwise, carries out chemical polishing in the same way, when smooth when plane of crystal, smooth, no marking, Grinding and polishing finishes.It is rinsed with isopropanol, high pure nitrogen drying, and is stored in vacuum desiccator immediately later.
Embodiment 5: rubber pad is laid on two polishing disks；The MAPbBr that will be grown from solwution method3Crystal is placed on On one polishing disk, 2 milliliters of WD-40 polishing fluid are sprayed on rubber pad, are drawn " 8 " word with finger and are carried out grinding and polishing, to chip two sides point Pao Guang not be 1000 seconds, it is rinsed immediately with isopropanol later；The crystal after WD-40 is polished is placed on second polishing disk again On, polishing fluid isopropanol 3ml is added dropwise, carries out chemical polishing in the same way, when smooth when plane of crystal, smooth, no marking, Grinding and polishing finishes.It is rinsed with isopropanol, high pure nitrogen drying, and is stored in vacuum desiccator immediately later.
It will be seen from figure 1 that, because of the contact and influence of cooling oil, crystal permeability is bright in big crystal after cutting machine It is aobvious to reduce, after the present embodiment polishing treatment, MAPbBr3Plane of crystal is smooth, while remaining without polish line, penetrating Property is good.Figure it is seen that after the present embodiment polishing treatment, MAPbBr3Plane of crystal leakage current is lower, resistivity Up to 108Ω cm magnitude.
The WD-40 residual that plane of crystal after the polishing of WD-40 polishing fluid generates, by isopropanol polishing fluid polishing treatment Afterwards, MAPbBr3Plane of crystal is smooth, while remaining without polish line, and permeability is good, finds resistance by test I-V Rate is up to 108Ω cm magnitude.

Claims (1)

1. a kind of polishing method of organic inorganic hybridization halide perovskite semiconductor crystal, it is characterised in that including following step It is rapid:
Rubber pad is laid on two polishing disks；The MAPbBr that will be grown from solwution method3Crystal is placed on first polishing disk, 1~3 milliliter of WD-40 polishing fluid is sprayed on rubber pad, is drawn 8 words with finger and is carried out grinding and polishing, to MAPbBr3Crystal two sides polishes respectively It 300~1000 seconds, is rinsed immediately with isopropanol later；Again by the MAPbBr after WD-40 is polished3Crystal is placed on second throwing On CD, 3~5ml of isopropanol polishing fluid is added dropwise, carries out chemical polishing in the same way, smooth to plane of crystal, smooth, nothing It when scratch, is rinsed with isopropanol, high pure nitrogen drying, and is stored in vacuum desiccator；The MAPbBr that this method obtains3Crystal Surface is smooth, and resistivity is up to 108Ω cm magnitude.
CN201711083278.XA 2017-11-07 2017-11-07 The polishing method of organic inorganic hybridization halide perovskite semiconductor crystal Active CN107855923B (en)

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CN112525940B (en) * 2020-11-19 2023-07-04 西北工业大学 All-inorganic halide perovskite CsPbBr 3 Method for displaying secondary phase particles on wafer surface
CN113001376A (en) * 2021-02-25 2021-06-22 上海大学 MAPbI3Method for polishing crystal
CN115056042B (en) * 2022-05-30 2023-11-14 西北工业大学 Reduce full inorganic CsPbBr 3 Surface treatment method for leakage current of perovskite device
CN116120839B (en) * 2023-04-04 2023-08-29 中国科学技术大学 Magnetorheological fluid for perovskite semiconductor material and magnetorheological polishing method

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CN107121446A (en) * 2017-04-25 2017-09-01 大连交通大学 A kind of Cross-section transmission tem sample mechanical pre-thinning method
CN107123698A (en) * 2017-04-25 2017-09-01 西北工业大学 CdZnTe planar detector surface treatment methods

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Publication number Priority date Publication date Assignee Title
CN1970665A (en) * 2006-12-07 2007-05-30 西北工业大学 Polishing liquid and method for polishing II-VI compound semiconductor wafer
CN105158033A (en) * 2015-07-23 2015-12-16 成都航天龙宇质检技术有限公司 Fabrication method for compact tension specimen used for performance testing of material
CN106409818A (en) * 2016-10-17 2017-02-15 北京工业大学 Method of acquiring flexible ferroelectric thin film capacitor nondestructively
CN107121446A (en) * 2017-04-25 2017-09-01 大连交通大学 A kind of Cross-section transmission tem sample mechanical pre-thinning method
CN107123698A (en) * 2017-04-25 2017-09-01 西北工业大学 CdZnTe planar detector surface treatment methods

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