CN104528664B - The preparation method of two dimension telluride gallium material - Google Patents

The preparation method of two dimension telluride gallium material Download PDF

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CN104528664B
CN104528664B CN201410819701.8A CN201410819701A CN104528664B CN 104528664 B CN104528664 B CN 104528664B CN 201410819701 A CN201410819701 A CN 201410819701A CN 104528664 B CN104528664 B CN 104528664B
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CN104528664A (en
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王涛
赵清华
介万奇
谢涌
何杰
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Northwestern Polytechnical University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/007—Tellurides or selenides of metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size

Abstract

The invention discloses a kind of preparation method of two-dimentional telluride gallium material, for solving the little technical problem of telluride gallium material area prepared by existing preparation method.Technical scheme is based on existing micromechanics stripping method, in transfer process, introduces the parameters such as temperature and pressure, improves the size of two-dimentional GaTe material.On the basis of original micromechanics stripping method stripping-transfer step, devise stripping-transfer-peel off three step micromechanics stripping methods again.During transfer, 10 5anneal is carried out under the impressed pressure of pa and 90-110 DEG C of condition.Finally use the high adhesive tape of think of to carry out strip operation again, realize the thinning further of GaTe thin slice.Due to the annealing process procedure under introducing impressed pressure in transition phase and follow-up peel off thinning process again, stablely obtain large-area two-dimentional GaTe material.Two dimension GaTe scantling brings up to 200-600 μm by 5-60 μm of background technology.

Description

The preparation method of two dimension telluride gallium material
Technical field
The present invention relates to a kind of preparation method of telluride gallium material, particularly relate to a kind of preparation method of two-dimentional telluride gallium material.
Background technology
The two-dimensional functional material being representative with Graphene, magnesium-yttrium-transition metal chalcogenide relies on unique physics, chemical property and huge researching value thereof, receives the extensive concern of people.Wherein two-dimentional GaTe material belongs to III-VII A compound semiconductor, has larger ordination number and suitable energy gap, and at opto-electronic device, there is very high using value in the field such as radiation detection and solar cell.The acquisition of large-area two-dimensional GaTe material can meet large-scale integrated circuit constructs multiple MOSFET structure continuously requirement in less region, have compressed cost further while improving electronics performance, is the prerequisite realizing commercial application.But up to now, the stable preparation of large-area two-dimensional GaTe material remains a general difficult problem.
Document 1 " NovoselovKS, GeimAK, MorozovSV, etal.ElectricFieldEffectinAtomicallyThinCarbonFilms.Scie nce, 2004; 306:666-669 " report and adopt micromechanics stripping method to peel off expanded graphite to have prepared two-dimensional graphene material, the two-dimensional graphene of document report is of a size of 60 μm * 20 μm.
Document 2 " JonathanN.Coleman, MnstafaLotya, etal.Two-DimensionalNanosheetsProducedbyLiquidExfoliatio nofLayeredMaterials.Science, 2011; 331:568-571 " report and adopt organic solvent stripping method to prepare MoS 2, WS 2, MoSe 2etc. multiple two-dimensional material, the overall dimension of the two-dimensional material of document report is 5 μm.
Document 3 " Yi-HsienLee, Xin-QuanZhang, WenJingZhang, Lain-JongLi, etal.SynthesisofLarge-AreaMoS 2atomicLayerswithChemicalVaporDeposition.AdvanceMaterials, 2012; 24:2320-2325 " report adopt chemical Vapor deposition process prepared two-dimentional MoS 2material, the two-dimentional MoS of document report 2material is of a size of 20 μm.
Above method has all prepared proper two-dimensional material, but its size is all below 100 μm, still can not meet the requirement of large-area two-dimensional material.
Summary of the invention
In order to overcome the little deficiency of telluride gallium material area prepared by existing preparation method, the invention provides a kind of preparation method of two-dimentional telluride gallium material.The method, based on existing micromechanics stripping method, in transfer process, is introduced the parameters such as temperature and pressure, is improve the size of two-dimentional GaTe material.On the basis of original micromechanics stripping method stripping-transfer step, devise stripping-transfer-peel off three step micromechanics stripping methods again.During transfer, 10 5anneal is carried out under the impressed pressure of pa and 90-110 DEG C of condition.Finally use the high adhesive tape of think of to carry out strip operation again, realize the thinning further of GaTe thin slice, prepared telluride gallium material area can be increased.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of two-dimentional telluride gallium material, is characterized in adopting following steps:
Step one, adopt vertical bridgeman crystal growth method, Ga:Te is prepared burden than 1:1 by amount of substance, preparation GaTe single crystal.
In step 2, that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, choose the GaTe body material of bulk smooth surface corrugationless, and be separated into polylith along natural cleavage plane.
In step 3, that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, use and think high adhesive tape and tears off from the GaTe block materials surface that top layer light, damage are less the GaTe thin slice that one piece of thickness is about 6-8 μm.
In step 4, that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, the high adhesive tape of think of with GaTe thin slice is repeatedly bonded separation, until tape surface is no longer bright, successfully adheres to the GaTe lamella of comparatively intensive hundreds of nano thickness.In order to protect GaTe body material even curface, GaTe surface during stripping, should be made fully to contact with tape surface.In adhesive tape sepn process, one direction slowly to carry out.
Step 5, select tape surface stratiform GaTe distribution comparatively intensive and cull is less region is shifted, transfer to by the GaTe thin slice on adhesive tape the SiO that thickness is 300nm 2substrate surface.Use weight to apply 10 simultaneously 5the pressure of Pa and at 90 DEG C-110 DEG C anneal 22-24h.
Step 6, GaTe lamella thinning, namely peels off again.Utilize 3M to think the adhesion repeatedly of high adhesive tape, the GaTe being attached to silica sphere is peeled off further, re-use the cull of the cotton balls erasing substrate surface being moistened with acetone.
The invention has the beneficial effects as follows: the method, based on existing micromechanics stripping method, in transfer process, is introduced the parameters such as temperature and pressure, improve the size of two-dimentional GaTe material.On the basis of original micromechanics stripping method stripping-transfer step, devise stripping-transfer-peel off three step micromechanics stripping methods again.During transfer, 10 5anneal is carried out under the impressed pressure of pa and 90-110 DEG C of condition.Finally use the high adhesive tape of think of to carry out strip operation again, realize the thinning further of GaTe thin slice.Due to the annealing process procedure under introducing impressed pressure in transition phase and follow-up peel off thinning process again, stablely obtain large-area two-dimentional GaTe material.Two dimension GaTe scantling brings up to 200-600 μm by 5-60 μm of background technology.
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
Accompanying drawing explanation
Fig. 1 is the optical microphotograph pattern picture of the two-dimentional GaTe material prepared by the inventive method embodiment 2.
Fig. 2 is the EDS collection of illustrative plates that the two-dimentional GaTe material composition prepared by the inventive method embodiment 2 is analyzed.
Fig. 3 is the atomic force microscope observation picture of the two-dimentional GaTe material prepared by the inventive method embodiment 2.
Embodiment
Following examples are with reference to Fig. 1-3.
Embodiment 1:
Step one, adopts vertical bridgeman crystal growth method, is prepared burden by Ga:Te by amount of substance than 1:1, the GaTe single crystal of preparation.
Step 2, in that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, chooses the GaTe body material of bulk smooth surface corrugationless, and is separated into 2 pieces along natural cleavage plane.
Step 3, in that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, uses the GaTe block materials surface that the high adhesive tape of think of is bright from top layer, damage is less to tear off the GaTe thin slice that one piece of thickness is about 6 μm.
4th step, in that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, bonds separation 15 times by the high adhesive tape of think of with GaTe thin slice, until tape surface is no longer bright, successfully adheres to the GaTe lamella of comparatively intensive 200nm thickness.In order to protect GaTe body material even curface, GaTe surface during stripping, should be made fully to contact with tape surface.In adhesive tape sepn process, one direction slowly to carry out.
5th step, selects tape surface stratiform GaTe distribution comparatively intensive and cull is less region is shifted, and transfers to by the GaTe thin slice on adhesive tape the SiO that thickness is 300nm 2substrate surface.Use weight to apply 10 simultaneously 5the pressure of Pa and at 90 DEG C anneal 24h.
6th step, GaTe lamella thinning, namely peels off again.Utilize 3M to think the adhesion repeatedly of high adhesive tape, the GaTe being attached to silica sphere is peeled off further, re-use the cull of the cotton balls erasing substrate surface being moistened with acetone.
Two-dimentional GaTe material prepared by the present embodiment is of a size of 300 μm.
Embodiment 2:
Step one, adopts vertical bridgeman crystal growth method, is prepared burden by Ga:Te by amount of substance than 1:1, the GaTe single crystal of preparation.
Step 2, in that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, chooses the GaTe body material of bulk smooth surface corrugationless, and is separated into 3 pieces along natural cleavage plane.
Step 3, in that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, uses the GaTe block materials surface that the high adhesive tape of think of is bright from top layer, damage is less to tear off the GaTe thin slice that one piece of thickness is about 8 μm.
4th step, in that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, bonds separation 15 times by the high adhesive tape of think of with GaTe thin slice, until tape surface is no longer bright, successfully adheres to the GaTe lamella of comparatively intensive 210nm thickness.In order to protect GaTe body material even curface, GaTe surface during stripping, should be made fully to contact with tape surface.In adhesive tape sepn process, one direction slowly to carry out.
5th step, selects tape surface stratiform GaTe distribution comparatively intensive and cull is less region is shifted, and transfers to by the GaTe thin slice on adhesive tape the SiO that thickness is 300nm 2substrate surface.Use weight to apply 10 simultaneously 5the pressure of Pa and at 100 DEG C anneal 23h.
6th step, GaTe lamella thinning, namely peels off again.Utilize 3M to think the adhesion repeatedly of high adhesive tape, the GaTe being attached to silica sphere is peeled off further, re-use the cull of the cotton balls erasing substrate surface being moistened with acetone.
The optical microphotograph pattern picture of the two-dimentional GaTe material of Fig. 1 prepared by embodiment 2.Can be seen by figure, prepared two-dimentional GaTe material is of a size of 600 μm.
The EDS collection of illustrative plates that the two-dimentional GaTe material composition of Fig. 2 prepared by embodiment 2 is analyzed.The EDS data that the two-dimentional GaTe material composition of table 1 prepared by embodiment 2 is analyzed.Can be seen by Fig. 2 and table 1, Ga and the Te atom content of prepared two-dimentional GaTe material is respectively 49.41% and 50.59%, close to 1:1, intactly saves the composition of GaTe body material.
The atomic force microscope observation picture of the two-dimentional GaTe material of Fig. 3 prepared by embodiment 2.Can be seen by figure, the thickness of prepared two-dimentional GaTe material is 2.5nm.
The EDS data that the two-dimentional GaTe material composition of table 1 is analyzed
Element Quality % Atom %
Ga 34.80 49.41
Te 65.20 50.59
Amount to 100 100
Embodiment 3:
Step one, adopts vertical bridgeman crystal growth method, is prepared burden by Ga:Te by amount of substance than 1:1, the GaTe single crystal of preparation.
Step 2, in that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, chooses the GaTe body material of bulk smooth surface corrugationless, and is separated into 4 pieces along natural cleavage plane.
Step 3, in that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, uses the GaTe block materials surface that the high adhesive tape of think of is bright from top layer, damage is less to tear off the GaTe thin slice that one piece of thickness is about 7 μm.
4th step, in that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, bonds separation 15 times by the high adhesive tape of think of with GaTe thin slice, until tape surface is no longer bright, successfully adheres to the GaTe lamella of comparatively intensive 210nm thickness.In order to protect GaTe body material even curface, GaTe surface during stripping, should be made fully to contact with tape surface.In adhesive tape sepn process, one direction slowly to carry out.
5th step, selects tape surface stratiform GaTe distribution comparatively intensive and cull is less region is shifted, and transfers to by the GaTe thin slice on adhesive tape the SiO that thickness is 300nm 2substrate surface.Use weight to apply 10 simultaneously 5the pressure of Pa and at 110 DEG C anneal 22h.
6th step, GaTe lamella thinning, namely peels off again.Utilize 3M to think the adhesion repeatedly of high adhesive tape, the GaTe being attached to silica sphere is peeled off further, re-use the cull of the cotton balls erasing substrate surface being moistened with acetone.
Two-dimentional GaTe material prepared by the present embodiment is of a size of 400 μm.

Claims (1)

1. a preparation method for two-dimentional telluride gallium material, is characterized in that comprising the following steps:
Step one, adopt vertical bridgeman crystal growth method, Ga:Te is prepared burden than 1:1 by amount of substance, preparation GaTe single crystal;
In step 2, that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, choose the GaTe block materials of bulk smooth surface corrugationless, and be separated into polylith along natural cleavage plane;
In step 3, that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, use and think high adhesive tape and tears off from the GaTe block materials surface that top layer light, damage are less the GaTe thin slice that one piece of thickness is 6-8 μm;
In step 4, that Universal2440-750 glove box of meter Kai Luo under an ar atmosphere, the high adhesive tape of think of with GaTe thin slice is repeatedly bonded separation, until tape surface is no longer bright, successfully adheres to the GaTe lamella of comparatively intensive hundreds of nano thickness; In order to protect GaTe block materials even curface, GaTe surface during stripping, should be made fully to contact with tape surface; In adhesive tape sepn process, one direction slowly to carry out;
Step 5, select tape surface stratiform GaTe distribution comparatively intensive and cull is less region is shifted, transfer to by the GaTe thin slice on adhesive tape the SiO that thickness is 300nm 2substrate surface; Use weight to apply 10 simultaneously 5the pressure of Pa and at 90 DEG C-110 DEG C anneal 22-24h;
Step 6, GaTe lamella thinning, namely peels off: utilize 3M to think the adhesion repeatedly of high adhesive tape, peeled off further by the GaTe being attached to silica sphere again, re-uses the cull of the cotton balls erasing substrate surface being moistened with acetone.
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CN106702320B (en) * 2015-11-13 2019-02-05 中国科学院物理研究所 Heterogeneous two-dimentional crystalline film material of a kind of superconductor-insulator-metal and preparation method thereof
CN107123599A (en) * 2017-04-12 2017-09-01 西北工业大学 Vacuum annealing method based on two-dimentional telluride gallium material FET
CN106953231B (en) * 2017-05-02 2019-05-10 中山大学 A method of realizing telluride gallium (GaTe) two-dimensional material exciton Laser emission
CN107167424A (en) * 2017-06-09 2017-09-15 华东师范大学 A kind of device for preparing two-dimensional layer material automatically based on shearing force
CN107994099B (en) * 2017-11-23 2019-08-09 西北工业大学 Based on two-dimentional gallium selenide material field effect transistor preparation method

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