CN106298466A - The two-dimentional transient metal chalcogenide compound transfer method of adhesive tape is released based on heat - Google Patents
The two-dimentional transient metal chalcogenide compound transfer method of adhesive tape is released based on heat Download PDFInfo
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- CN106298466A CN106298466A CN201610828511.1A CN201610828511A CN106298466A CN 106298466 A CN106298466 A CN 106298466A CN 201610828511 A CN201610828511 A CN 201610828511A CN 106298466 A CN106298466 A CN 106298466A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/027—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34
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Abstract
The invention discloses a kind of two-dimentional transient metal chalcogenide compound transfer method releasing adhesive tape based on heat, it is loaded down with trivial details that the present invention solves tradition transfer method technique, the problem that transfer sample integrity is the highest, its implementation is: 1) carries out photoresist spin coating on the print that Grown has two-dimentional transient metal chalcogenide compound, and uses the KOH aqueous solution of 50～60 DEG C to perform etching print；2) release adhesive tape by heat to be close to through 1) process after print, peel off heat subsequently and release adhesive tape, obtain being followed successively by heat and release adhesive tape, photoresist and the stacked structure of two dimension transient metal chalcogenide compound, and the heat with this structure is released in the target substrate that adhesive tape is close to select in advance and cleaned；3) utilizing warm table heating to peel off heat and release adhesive tape, then remove the photoresist in target substrate with acetone and it dried up with nitrogen, transfer terminates.It is simple that the present invention has technique, and transfer is complete, requires low to print, and the advantage of the repeatable utilization of substrate can be used for the processing of two-dimension nano materials.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, be specifically related to the transfer method of two-dimensional material, can be used for nanometer
The processing of material.
Technical background
Continue the discovery of Graphene in 2004, and the research of two-dimensional topology material, also referred to as monolayer material constantly starts upsurge.Two dimension
The physicochemical characteristics of material uniqueness makes them have wide answering in light cell, quasiconductor, electrode and Water warfare field
Use prospect.Wherein study the significant advantages such as the most deep Graphene has intensity greatly, and electron mobility is high, but Graphene does not has
Having band gap, the transistor switch ratio made with it is less than 102, this significantly limit it and at large scale integration transistor and patrols
Collect the application in circuit.Therefore, find band gap tunable two-dimensional semiconductor material and become study hotspot, thus with MoS2For generation
The two-dimentional transient metal chalcogenide compound TMDs of table relies on its good electrostatic coupling, the adjustable band-gap that the number of plies relies on, directly
To indirectly band gap variation, good luminescence and detection performance, become field-effect transistor, collection optics, hypersensitization
Learn the object of study that sensor, flexible device and spintronics aspect receive much concern.As the foundation stone of application, the growth of material
Lasting concern and research has been obtained with transfer.Owing to chemical vapour deposition technique CVD can grow the large area that size is controlled
Monolayer TMDs material, is widely adopted.In order to process the monolayer material of CVD growth further, the most intactly turn
Shifting deeply characterizes its next step and element manufacturing has vital meaning.
At present, the main transfer method of two-dimensional TM Ds includes that electron beam resist PMMA substrate corrosion shifts, and water auxiliary turns
Move and heat releases adhesive tape transfer.It is good that PMMA substrate corrosion transfer method has film integrity, the feature that success rate is high, is current TEM
The main method that sample preparation and element manufacturing use, but the method sacrifices growth substrates and implementation process is complicated, and cost is high, no
It is beneficial to promote and large-area applications；The transfer of dripping of Yi-Hsien Lee et al. employing then make use of growth substrates (SiO2/Si)
Hydrophilic and MoS2The hydrophobicity of material realizes stripping and the transfer of material, and the most effectively, but this method is easily made
Become the broken of monolayer material, see (Yi-Hsien, Lee, Lili, Yu.Synthesis and Transfer of Single-
Layer Transition Metal Disulfides on Diverse Surfaces[J].Nano Letters,2013,
(13):1852-1857).The document describes the concrete steps of this method in detail；And heat is released adhesive tape rule and is originated from Graphene
Transfer process, realize peeling off transfer, Ziyuan by the difference of target material and substrate and the Young's modulus of Cu thin film
Lin et al. adopt carry out in this way original position transfer characteristic good, but the introducing of Cu can to semiconductor device make bring negative
Face rings, and sees (Ziyuan, Lin, Yang, Chai.Controllable Growth of Large Size
Crystalline MoS2 and Resist-Free Transfer Assisted with a Cu Thin Film[J]
.Scientific Reports,2015,(5)；srep18596)；In order to simplify transfer process further, it is ultrasonic that PMMA assists
Transfer is also suggested, and sees (Donglin, Ma, Zhongfan, Liu etc.A universal etching-free
transfer of MoS2 films for applications in photodetectors[J].Nano Research,
2015,11 (8): 3662-3672), but this method has damage to raw material, it is impossible to ensure sample thin film complete after transfer
Property, reduce the utilization rate of sample.
Summary of the invention
Present invention aims to above-mentioned the deficiencies in the prior art, it is provided that a kind of two dimension transient metal chalcogenide compound
The transfer method of material, to reduce in transfer process raw-material damage, it is ensured that the integrity of sample thin film after transfer, improves
The utilization rate of sample.
The key problem in technology realizing the present invention is: heat is released adhesive tape and is affixed on the growth print of spin coating photoresist, take heat off
Release adhesive tape, obtain being followed successively by heat and release adhesive tape, photoresist and two dimension transient metal chalcogenide compound stacked structure, then will be with this knot
The heat of structure is released adhesive tape and is affixed in target substrate and heats, and by controlling heating-up temperature, makes adhesive tape curling come off, removes photoresist
After, complete transfer.Its implementation is as follows:
(1) light Microscopic observation in Grown the print of two-dimensional layer material, demarcate transport zone and also shoot photograph
Sheet；
(2) clean print surface by nitrogen gun, and be placed on warm table and be heated to 100 DEG C～120 DEG C；
(3) 2 to 3 photoresists are dripped to print surface so that it is area coverage, slightly larger than the half of print surface area, then will
Print is placed in spin coating on spin coater, makes the photoresist on dripping be evenly distributed on print surface, print is placed in 160～180 subsequently
DEG C warm table on once heat after, again drip 2 photoresists to print surface, print carried out secondary spin coating and by it
It is placed on 160 DEG C～180 DEG C of warm tables and carries out post bake, from warm table, take off print afterwards；
(4), after print being placed in the KOH aqueous solution of 40～60 DEG C etching 4～8min, totally and nitrogen is used by pure water rinsing
Air gun is dried up, then heat is released adhesive tape is close on this print；
(5) select the substrate of surfacing no marking to do target substrate, use pure water, acetone, isopropanol successively they to be entered
Row ultrasonic cleaning 5～10min；
(6) heat is released adhesive tape slowly to tear along print edge, obtain being followed successively by heat and release adhesive tape, photoresist and two-dimensional layer material
The stacked structure of material, releases the heat with this structure adhesive tape subsequently and is close in the target substrate that step (5) obtains；
(7) target substrate posting heat and releasing adhesive tape is placed on warm table it is heated to 120 DEG C～140 DEG C, make heat release adhesive tape
Heated curling, separates with target substrate；
(8) target substrate is immersed in 40 DEG C～50 DEG C of acetone 3～5min, be then immersed in isopropanol 1～
3min, removes the photoresist on its surface, re-uses nitrogen gun and target substrate is dried up, and completes transfer.
Due to the fact that taking photoresist auxiliary heat releases the mode of adhesive tape, on the one hand this mode can effectively simplify stripping
From process, it is to avoid the breakage that raw-material hydrophobic property is brought in transfer, the integrity of transfer is effectively ensured；The opposing party
Face, this mode significantly reduces the etch period of KOH needed for transfer process, decreases KOH to SiO2With Sapphire Substrate table
The etching in face so that the substrate of growth two-dimensional layer material can be reused, environment-friendly high-efficiency, and reduces growth cost.
Experiment shows, the present invention can have the two-dimensional layer material on the print of drug residue than more fully transfer, has
Effect improves the utilization rate of growth material.
Technical scheme and effect can be further illustrated by the following drawings and example.
Accompanying drawing explanation
Fig. 1 is the flowchart of the present invention；
Fig. 2 is two-dimensional layer MoS before and after present example 1 transfer2The light microscopic comparison diagram of material；
Fig. 3 is two-dimensional layer MoS before and after present example 2 transfer2The light microscopic comparison diagram of material；
Fig. 4 is two-dimensional layer WS before and after present example 3 transfer2The light microscopic comparison diagram of material；
Fig. 5 is two-dimensional layer MoS before and after present example 1 transfer2The Raman spectrum comparison diagram of material；
Detailed description of the invention
With reference to Fig. 1, the present invention provides following four embodiments:
Embodiment 1: to being grown in SiO2Two-dimensional layer MoS on/Si substrate2Transfer
Step one, at SiO2/ Si Grown two-dimensional layer MoS2The print spin coating photoresist of material and etching.
1a) at light Microscopic observation in SiO2/ Si Grown MoS2The print of stratified material, demarcates transport zone and claps
Take the photograph photo, and print nitrogen gun is blown off be placed on 120 DEG C of warm tables heating, take off print；
1b) drip 2 photoresists to print surface so that it is area coverage is slightly larger than the half of print surface area, then by sample
Sheet is placed in spin coating on spin coater, is 1000 turns/s at rotating speed, and rotary acceleration is 100 turns/s2Under conditions of spin coating 15s, make drip
On photoresist be evenly distributed on print surface, subsequently print is placed in after once heating on the warm table of 160 DEG C, then to
2 photoresists are dripped on print surface, print carries out secondary spin coating and is placed on 160 DEG C of warm tables and carries out post bake；
It is placed on after 1c) taking off print from hot plate in the KOH aqueous solution of 40 DEG C and slightly etches 4min, further take out print
Totally and nitrogen gun is used to be dried up by pure water rinsing afterwards.
Step 2, heat is released adhesive tape fill-in light photoresist, will be had two-dimensional layer MoS2Stacked structure transfer to target substrate.
2a) selecting the substrate of surfacing no marking to do target substrate, use deionized water, acetone, isopropanol surpasses successively
It is standby that sound cleans 5min；
2b) heat is released adhesive tape slowly to tear along print edge, obtain being followed successively by heat and release adhesive tape, photoresist and two-dimensional layer
MoS2Stacked structure, and the heat with this structure released adhesive tape be close in cleaned target substrate.
Step 3, the heat removed in target substrate releases adhesive tape and photoresist
3a) target substrate posting heat and releasing adhesive tape is placed on warm table it is heated to 120 DEG C, make heat release adhesive tape heated curling
After, separate with target substrate；
3b) target substrate is immersed in 3min in 40 DEG C of acetone, is then immersed in 1min in isopropanol, remove its table
The photoresist in face, re-uses nitrogen gun and target substrate is dried up, and completes transfer.
Embodiment 2: to the two-dimensional layer MoS grown on a sapphire substrate2Transfer
Step one, to growing two-dimensional layer MoS on a sapphire substrate2The print spin coating photoresist of material and etching.
First, at light Microscopic observation in Grown on Sapphire Substrates two-dimensional layer MoS2The print of material, demarcates transition range
Territory also shoots photo, and print nitrogen gun is blown off and be placed on the heating of 120 DEG C of warm tables, takes off print；
Then, 3 photoresists are dripped to print surface so that it is area coverage, slightly larger than the half of print surface area, then will
Print is placed in spin coating on spin coater, is 1000 turns/s at rotating speed, and rotary acceleration is 100 turns/s2Under conditions of spin coating 15s, make
Photoresist on Diing is evenly distributed on print surface, is placed in by print subsequently after once heating on the warm table of 180 DEG C, then
Drip 2 photoresists to print surface, print is carried out secondary spin coating and is placed on 180 DEG C of warm tables and carries out post bake；
Then, it is placed on after taking off print from hot plate in the KOH aqueous solution of 60 DEG C and slightly etches 8min, take out print
Totally and nitrogen gun is used to be dried up by pure water rinsing afterwards.
Step 2, heat is released adhesive tape fill-in light photoresist, will be had two-dimensional layer MoS2Stacked structure transfer to target substrate.
First, selecting the substrate of surfacing no marking to do target substrate, use deionized water, acetone, isopropanol is successively
Ultrasonic cleaning 10min is standby；
Then, heat is released adhesive tape and slowly tears along print edge, obtain being followed successively by heat and release adhesive tape, photoresist and two-dimensional layer
MoS2Stacked structure, and the heat with this structure released adhesive tape be close in cleaned target substrate.
Step 3, the heat removed in target substrate releases adhesive tape and photoresist.
First, the target substrate posting heat and releasing adhesive tape is placed on warm table and is heated to 140 DEG C, make heat release adhesive tape by hot rolling
Qu Hou, separates with target substrate；
Then, target substrate is immersed in 5min in 60 DEG C of acetone, is then immersed in 3min in isopropanol, removes it
The photoresist on surface, re-uses nitrogen gun and target substrate is dried up, and completes transfer.
Embodiment 3: to being grown in SiO2Two-dimensional layer WS on/Si substrate2Transfer
Step A, at SiO2/ Si Grown two-dimensional layer WS2The print spin coating photoresist of material and etching.
A1) at light Microscopic observation in SiO2/ Si Grown two-dimensional layer WS2The print of material, demarcates transport zone also
Shooting photo, and print nitrogen gun is blown off be placed on the heating of 110 DEG C of warm tables, take off print；
A2) 2 photoresists are dripped to print surface so that it is area coverage is slightly larger than the half of print surface area, then by sample
Sheet is placed in spin coating on spin coater, is 1000 turns/s at rotating speed, and rotary acceleration is 100 turns/s2Under conditions of spin coating 15s, make drip
On photoresist be evenly distributed on print surface, subsequently print is placed in after once heating on the warm table of 170 DEG C, then to
2 photoresists are dripped on print surface, print carries out secondary spin coating and is placed on 170 DEG C of warm tables and carries out post bake；
A3) it is placed on after taking off print from hot plate in the KOH aqueous solution of 50 DEG C and slightly etches 6min, after taking out print
Totally and nitrogen gun is used to be dried up by pure water rinsing.
Step B, heat releases adhesive tape fill-in light photoresist, will be containing two-dimensional layer WS2Stacked structure transfer to target substrate.
B1) selecting the substrate of surfacing no marking to do target substrate, use deionized water, acetone, isopropanol surpasses successively
It is standby that sound cleans 8min；
B2) heat is released adhesive tape slowly to tear along print edge, obtain being followed successively by heat and release adhesive tape, photoresist and two-dimensional layer
WS2Stacked structure, and the heat with this structure released adhesive tape be close in cleaned target substrate.
Step C, the heat removed in target substrate releases adhesive tape and photoresist.
C1) target substrate posting heat and releasing adhesive tape is placed on warm table it is heated to 130 DEG C, make heat release adhesive tape heated curling
After, separate with target substrate；
C2) target substrate is immersed in 4min in 45 DEG C of acetone, is then immersed in 2min in isopropanol, removes its table
The photoresist in face, re-uses nitrogen gun and target substrate is dried up, and completes transfer.
Embodiment 4: to the two-dimensional layer WS grown on a sapphire substrate2Transfer
The first step, to growing two-dimensional layer WS on a sapphire substrate2The print spin coating photoresist of material and etching.
1.1) at light Microscopic observation in Grown on Sapphire Substrates two-dimensional layer WS2The print of material, demarcates transport zone
And shoot photo, and print nitrogen gun is blown off be placed on 105 DEG C of warm tables heating, take off print；
1.2) 2 photoresists are dripped to print surface so that it is area coverage is slightly larger than the half of print surface area, then by sample
Sheet is placed in spin coating on spin coater, makes the photoresist on dripping be evenly distributed on print surface, print is placed in the heating of 175 DEG C subsequently
After once heating on platform, then drip 2 photoresists to print surface, print is carried out secondary spin coating and is placed on 175 DEG C
Carrying out post bake on warm table, wherein the technological parameter of spin coating is as follows:
Rotating speed is 1000 turns/s, and rotary acceleration is 100 turns/s2, spin-coating time is 15s；
1.3) it is placed on after taking off print from hot plate in the KOH aqueous solution of 50 DEG C and slightly etches 6min, take out print
Totally and nitrogen gun is used to be dried up by pure water rinsing afterwards.
Second step, heat releases adhesive tape fill-in light photoresist, will be containing two-dimensional layer WS2Stacked structure transfer to target substrate.
2.1) selecting the substrate of surfacing no marking to do target substrate, use deionized water, acetone, isopropanol surpasses successively
It is standby that sound cleans 8min；
2.2) heat is released adhesive tape slowly to tear along print edge, obtain being followed successively by heat and release adhesive tape, photoresist and two-dimensional layer
WS2Stacked structure, and the heat with this structure released adhesive tape be close in cleaned target substrate.
3rd step, the heat removed in target substrate releases adhesive tape and photoresist.
Implementing of this step is identical with the step 3 of embodiment 3.
The effect of the present invention can be further illustrated by following measured result.
Actual measurement 1, the two-dimensional layer MoS before and after utilizing optical microscope that embodiment 1 is shifted2Material is observed, result
As shown in Figure 2.Wherein, Fig. 2 (a) is under amplifying 50 times, is grown in SiO2Two-dimensional layer MoS on/Si substrate2Material shifts
Front light microscopic figure；Fig. 2 (b) is under amplifying 50 times, transfers to the MoS in target substrate2Light microscopic figure；Fig. 2 (c) is to amplify
Under 500 times, it is grown in SiO2Two-dimensional layer MoS on/Si substrate2Light microscopic figure before transfer；Fig. 2 (d) is under amplifying 500 times,
Transfer to MoS in target substrate2Light microscopic figure.
Actual measurement 2, the two-dimensional layer MoS before and after utilizing optical microscope that embodiment 2 is shifted2Material is observed, result
As shown in Figure 3.Wherein, 3 (a) is under amplifying 50 times, the two-dimensional layer MoS of Grown on Sapphire Substrates before transfer2Light microscopic figure；
Fig. 3 (b) is under amplifying 50 times, transfers to the MoS in target substrate2Light microscopic figure；Fig. 3 (c) is under amplifying 500 times, blue
The two-dimensional layer MoS of gem Grown2Light microscopic figure；Fig. 3 (d) is under amplifying 500 times, transfers in target substrate
MoS2Light microscopic figure.
Actual measurement 3, the two-dimensional layer WS before and after utilizing optical microscope that embodiment 3 is shifted2Material is observed, and result is such as
Shown in Fig. 4, wherein Fig. 4 (a) is under amplifying 100 times, is grown in SiO2Two-dimensional layer WS on/Si substrate2Light microscopic before transfer
Figure；Fig. 4 (b) is under amplifying 200 times, transfers to the WS in target substrate2Light microscopic figure；Fig. 4 (c) is under amplifying 500 times, raw
Long at SiO2WS on/Si substrate2Light microscopic figure before sample transfer；Fig. 4 (d) is under amplifying 500 times, transfers to target substrate
Upper WS2Light microscopic figure.
From the test result of Fig. 2 it can be seen that the present invention can be to being grown in SiO2Two-dimensional layer MoS on/Si substrate2
Material carries out complete transfer.
From the test result of Fig. 3 it can be seen that the present invention can be to growth two-dimensional layer MoS on a sapphire substrate2
Material carries out complete transfer.
From the observed result of Fig. 4 it can be seen that the present invention can be to growth two-dimensional layer WS on a sapphire substrate2Material
Material carries out complete transfer.
Comprehensive above test result can obtain, and the present invention has transfer characteristic the most in situ.
Actual measurement 4, utilizes Raman spectrum analysis instrument, the two-dimensional layer MoS before and after shifting embodiment 12Material is tested,
Result is as shown in Figure 5.Wherein, the two-dimensional layer MoS before Fig. 5 (a) is embodiment 1 transfer2The Raman spectrum of material, Fig. 5 (b) is
Two-dimensional layer MoS after embodiment 1 transfer2The Raman spectrum of material.
Comparison diagram 5 (a) and Fig. 5 (b) can obtain, before comparing transfer, and MoS after transfer2The raman characteristic peak E of material1 2gAnd A1gAll
There occurs blue shift, show transfer process may have occurred certain Stress Release；And E in Fig. 5 (a) and Fig. 5 (b)1 2gAnd A1gTwo
Peak separation maintains 20cm-1Left and right, shows effectively control chemical contamination in transfer process and be folded mechanically, it is ensured that sample
The quality of material.
Claims (5)
1. release a two-dimentional transient metal chalcogenide compound transfer method for adhesive tape based on heat, comprise the steps:
(1) light Microscopic observation in Grown the print of two-dimentional transient metal chalcogenide compound, demarcate transport zone also
Shooting photo；
(2) clean print surface by nitrogen gun, and be placed on warm table and be heated to 100 DEG C～120 DEG C；
(3) 2 to 3 photoresists are dripped to print surface so that it is area coverage is slightly larger than the half of print surface area, then by print
It is placed in spin coating on spin coater, makes the photoresist on dripping be evenly distributed on print surface, subsequently print is placed in 160～180 DEG C
After once heating on warm table, again drip 2 photoresists to print surface, print is carried out secondary spin coating and is placed on
Carry out post bake on 160 DEG C～180 DEG C of warm tables, from hot plate, take off print afterwards；
(4), after print being placed in the KOH aqueous solution of 40～60 DEG C etching 4～8min, totally and nitrogen gun is used by pure water rinsing
Dried up, then heat is released adhesive tape be close on this print；
(5) select the substrate of surfacing no marking to do target substrate, use pure water, acetone, isopropanol successively they to be surpassed
Sound cleans 5～10min；
(6) heat is released adhesive tape slowly to tear along print edge, obtain being followed successively by heat and release adhesive tape, photoresist and two dimension Transition Metal Sulfur
Belong to the stacked structure of compound, subsequently the heat with this structure is released adhesive tape and is close in the target substrate that step (5) obtains；
(7) target substrate posting heat and releasing adhesive tape is placed on warm table it is heated to 120 DEG C～140 DEG C, make heat release adhesive tape and be heated
Curling, separates with target substrate；
(8) target substrate is immersed in 40 DEG C～50 DEG C of acetone 3～5min, is then immersed in isopropanol 1～3min,
Remove the photoresist on its surface, re-use nitrogen gun and target substrate is dried up, complete transfer.
2., according to the method described in claims 1, wherein print in step (1), including grown two-dimensional layer MoS2Material
Print and grown two-dimensional layer WS2The print of material.
3., according to the method described in claims 1, wherein substrate used by step (1) print, including SiO2/ Si substrate and indigo plant are precious
At the bottom of stone lining.
4. according to the method described in claims 1, wherein the process conditions of step (3) spin coater spin coating photoresist are as follows: turn
Speed is 1000 turns/s, and rotary acceleration is 100 turns/s2, spin-coating time is 15s.
5., according to the method described in claims 1, wherein KOH aqueous solution in step (4), is by adding in 50ml pure water
The liquid KOH configuration of 5ml forms.
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