CN104992905A - Boron nitride substrate surface step etching method - Google Patents
Boron nitride substrate surface step etching method Download PDFInfo
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- CN104992905A CN104992905A CN201510307155.4A CN201510307155A CN104992905A CN 104992905 A CN104992905 A CN 104992905A CN 201510307155 A CN201510307155 A CN 201510307155A CN 104992905 A CN104992905 A CN 104992905A
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- boron nitride
- nitride substrate
- substrate surface
- hexagonal boron
- mask layer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
- H01L21/30612—Etching of AIIIBV compounds
Abstract
The invention provides a boron nitride substrate surface step etching method comprising the following steps: S1, providing a hexagonal boron nitride substrate; S2, forming a mask layer on the surface of the hexagonal boron nitride substrate, and forming a preset etching pattern exposing the surface of the hexagonal boron nitride substrate in the mask layer; S3, depositing a metal layer on the surface of the mask layer and in the preset etching pattern; S4, stripping the mask layer and the metal layer on the surface of the mask layer; and S5, annealing the hexagonal boron nitride substrate, and then removing the metal layer in the preset etching pattern to obtain a step on the surface of the hexagonal boron nitride substrate, wherein the thickness of the step is the thickness of a single layer of boron nitride atoms. By adopting the method of the invention, the shape and size of the hexagonal boron nitride pattern can be controlled, and the etching area can be selected. Moreover, the height of the etched step can be controlled through repeated etching, and the problem concerning graphical processing based on a hexagonal boron nitride film device is solved.
Description
Technical field
The invention belongs to technical field of semiconductors, relate to a kind of boron nitride substrate surface step lithographic method.
Background technology
Novel low-dimension nano material is as the discovery of Graphene, boron nitride, carbon nano-tube etc. and successfully prepare in recent years, become the focus of condensed state area research, along with their unique novel physicochemical properties gradually find by people, show huge application prospect in micro-nano field of electronic devices.
Hexagonal boron nitride (h-BN) is a kind of similar to SP graphene-structured
2the stratiform hexagonal lattice nano material of bonding, is commonly called as white graphite alkene.Hexagonal boron nitride and Graphene have similar physical property, as good thermal conductivity and stability, and high temperature resistant and corrosivity, high rigidity and chemical stability etc.Due to its have atomically flating surface, without dangling bonds, without electron adulterated, and be considered to a kind of desirable substrate of Graphene electronics device.Simultaneously due to the ion of hexagonal boron nitride become key mode and Graphene different, therefore also show the different physical property of Graphene as wide band gap, high resistivity, low-k etc.These excellent characteristics make boron nitride nanosheet have good application prospect in many aspects, the semiconductor microelectronics device such as, worked under being applied to high temperature, feds, high temperature heat transfer composite material, photoelectric material etc.
But relative to Graphene, the preparation method of boron nitride nanosheet is not a lot.This is mainly because have the feature of ionic bond between adjacent two lamellas in hexagonal boron nitride, this can cause the active force of its interlayer to be eager to excel than the Van der Waals force of graphite layers, is difficult to image-stone ink and is peeled away by hexagonal boron nitride by conventional method like that.
In order to meet demand prepared by h-BN device, the graphical processing technology of h-BN film seems particularly important.Current h-BN graphically etches the method adopting photoetching binding plasma etching more, or in chemical gas-phase deposition system, adopt gas to carry out reactive ion etching, and these methods can not control the number of plies or the thickness of etching well.
Therefore, how to provide a kind of boron nitride substrate surface step lithographic method, with make step etch the number of plies or thickness controlled, become the important technological problems that those skilled in the art are urgently to be resolved hurrily.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of boron nitride substrate surface step lithographic method, being applied to for solving h-BN in prior art the structure patterning problem that micro-nano electronics, photoelectric device and integrated circuit etc. run into.
For achieving the above object and other relevant objects, the invention provides a kind of boron nitride substrate surface step lithographic method, comprise the steps:
S1: a hexagonal boron nitride substrate is provided;
S2: form mask layer at described hexagonal boron nitride substrate surface, and in described mask layer, form the default etched features exposing described hexagonal boron nitride substrate surface;
S3: depositing metal layers in described mask layer surface and described default etched features;
S4: the metal level peeling off described mask layer and surface thereof;
S5: anneal to described hexagonal boron nitride substrate, then removes the metal level in described default etched features, obtains the step of single-layer silicon nitride boron atomic thickness at described hexagonal boron nitride substrate surface.
Alternatively, described mask layer comprises photoresist or hard mask plate.
Alternatively, formed in the process of described default etched features in described mask layer, adopt uv-exposure method, electron beam exposure method, X-ray exposure method, ion beam exposure method or nano-imprint method in described mask layer, form the litho pattern of described default etched features.
Alternatively, described metal level is elemental metals Ni, Al, Zn, Mg, Fe, Sn, Pb or Co, or described metal level is the alloy of described elemental metals.
Alternatively, the thickness of described metal level is 2 ~ 100nm.
Alternatively, the method depositing described metal level is electron-beam vapor deposition method, sputtering method, ion assisted deposition method or pulsed laser deposition.
Alternatively, the atmosphere of described annealing is Ar/H
2mist, gas flow ratio is 200:100 ~ 200:20, and annealing region is 200 ~ 1000 DEG C, and annealing time is 2 ~ 8 hours.
Alternatively, the metal level in the described default etched features of wet etching removal is adopted.
Alternatively, described wet etching adopts HCl, (NH4)
2s
2o
8, HNO
3, H
2sO
4or acetic acid solution.
Alternatively, the concentration of described solution is 0.01 ~ 0.2mol/L, and wet etching soak time is 1min ~ 10hour.
Alternatively, described hexagonal boron nitride substrate adopts mechanical stripping or chemical vapour deposition technique to obtain.
Alternatively, after described step S5, repeating said steps S2 ~ S5 at least one times, obtains the step of preset thickness at described boron nitride substrate surface.
As mentioned above, boron nitride substrate surface step lithographic method of the present invention, there is following beneficial effect: boron nitride substrate surface step lithographic method of the present invention, etched features is preset by being formed in the mask layer on hexagonal boron nitride surface, plated metal subsequently, the hexagonal boron nitride underlayer surface in default etched features region is made to produce defect, then peel off preset mask layer around etched features and on metal, and described hexagonal boron nitride substrate is annealed, to promote that the dangling bonds on metal and destroyed hexagonal boron nitride surface are combined into key, solution removal is adopted to preset metal in etched features again, the hexagonal boron nitride atom that pre-etching region list layer is destroyed is taken away when metal is dissolved, form the step of individual layer atomic thickness.The method not only can control the patterned shape of hexagonal boron nitride, size, all right selective etching region, simultaneously through repeatedly etching, can control the height etching step, solving the graphical processing difficult problem based on hexagonal boron nitride thin-film device.
Accompanying drawing explanation
Fig. 1 is shown as the process chart of boron nitride substrate surface step lithographic method of the present invention.
Fig. 2 is shown as the structural representation of hexagonal boron nitride substrate in boron nitride substrate surface step lithographic method of the present invention.
Fig. 3 is shown as in boron nitride substrate surface step lithographic method of the present invention and forms mask layer at described hexagonal boron nitride substrate surface, and in described mask layer, form the schematic diagram exposing the default etched features of described hexagonal boron nitride substrate surface.
Fig. 4 is shown as the schematic diagram of depositing metal layers in described mask layer surface and described default etched features in boron nitride substrate surface step lithographic method of the present invention.
Fig. 5 is shown as the schematic diagram peeling off the metal level on described mask layer and surface thereof in boron nitride substrate surface step lithographic method of the present invention.
Fig. 6 is shown as in boron nitride substrate surface step lithographic method of the present invention the metal level removed in described default etched features, obtains the schematic diagram of the step of single-layer silicon nitride boron atomic thickness at described hexagonal boron nitride substrate surface.
Fig. 7 to be shown as in boron nitride substrate surface step lithographic method of the present invention repeating said steps S2 ~ S5 on the basis of structure shown in Fig. 6 and at least one times, to obtain the schematic diagram of the step of nitride multilayer boron atomic thickness at described boron nitride substrate surface.
Element numbers explanation
S1 ~ S5 step
1 hexagonal boron nitride substrate
2 mask layers
3 preset etched features
4 metal levels
5 steps
Embodiment
Below by way of specific instantiation, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Refer to Fig. 1 to Fig. 7.It should be noted that, the diagram provided in the present embodiment only illustrates basic conception of the present invention in a schematic way, then only the assembly relevant with the present invention is shown in graphic but not component count, shape and size when implementing according to reality is drawn, it is actual when implementing, and the kenel of each assembly, quantity and ratio can be a kind of change arbitrarily, and its assembly layout kenel also may be more complicated.
The invention provides a kind of boron nitride substrate surface step lithographic method, refer to Fig. 1, be shown as the process chart of the method, comprise the steps:
S1: a hexagonal boron nitride substrate is provided;
S2: form mask layer at described hexagonal boron nitride substrate surface, and in described mask layer, form the default etched features exposing described hexagonal boron nitride substrate surface;
S3: depositing metal layers in described mask layer surface and described default etched features;
S4: the metal level peeling off described mask layer and surface thereof;
S5: anneal to described hexagonal boron nitride substrate, then removes the metal level in described default etched features, obtains the step of single-layer silicon nitride boron atomic thickness at described hexagonal boron nitride substrate surface.
Technical scheme of the present invention is described in detail below by concrete example.
Embodiment one
First refer to Fig. 2, perform step S1: provide a hexagonal boron nitride substrate 1.
Concrete, described hexagonal boron nitride substrate 1 can adopt mechanical stripping or chemical vapour deposition technique to obtain.
Mechanical stripping method is generally: be pasted onto on adhesive tape by hexagonal boron nitride block, repeatedly doubling adhesive tape, peels off boron nitride block layer by layer, until adhesive tape leaves thinner hexagonal boron nitride film, and is transferred to target substrate as SiO
2, quartz or flexible substrate on.
Chemical vapour deposition technique is generally: adopt metal catalytic substrate, as Cu, Ni or Pt etc., with BH
3nH
3, (HBNH)
3, (HBNCl)
3or (ClNH)
3deng being growth source, under preset process condition, obtain hexagonal boron nitride film in the growth of metal catalytic substrate surface.This is well known to those skilled in the art, and repeats no more herein.
Then refer to Fig. 3, perform step S2: form mask layer 2 on described hexagonal boron nitride substrate 1 surface, and in described mask layer 2, form the default etched features 3 exposing described hexagonal boron nitride substrate 1 surface.
Concrete, according to the type of device that will make and the position controlling described default etched features flexibly can be required, i.e. selective etching region.The shape of described default etched features and size are arranged by changing litho pattern equally.
Concrete, described mask layer 2 can be photoresist or hard mask version.In the present embodiment, described mask layer 2 is preferably photoresist, and it is formed by photoetching processes such as linging, spin coating photoresists.In described mask layer 2, form the litho pattern presetting etched features subsequently through photoetching processes such as aiming at exposure, then through development, obtain described default etched features 3.Described exposure can adopt the methods such as uv-exposure method, electron beam exposure method, X-ray exposure method, ion beam exposure method or nano impression.
Then refer to Fig. 4, perform step S3: depositing metal layers 4 in described mask layer 2 surface and described default etched features 3.
Concrete, described metal level 4 is elemental metals Ni, Al, Zn, Mg, Fe, Sn, Pb or Co, or described metal level 4 is the alloy of described elemental metals.The thickness of described metal level 4 is 2 ~ 100nm.The method depositing described metal level 4 is electron-beam vapor deposition method, sputtering method, ion assisted deposition method or pulsed laser deposition.
Electron-beam vapor deposition method is the one of vacuum vapor plating, is to utilize electron beam to carry out direct heating evaporation material under vacuum, makes evaporating materials gasify and transport to substrate, film forming method that substrate is condensed.In electron beam heater, be positioned in the mandarin orange whirlpool of water-cooled by the material heated, evaporating materials and mandarin orange can be avoided to bring disaster upon wall and react and affect the quality of film, therefore, electron beam vapor deposition method can prepare high purity films.Electron beam evaporation can evaporate materials with high melting point, higher than the general resistance heating evaporation heat efficiency, beam current density is large, evaporation rate is fast, and the film purity made is high, quality good, and thickness can control more exactly.
Sputtering (sputtering) is the one of PVD film preparing technology, is mainly divided into four large classes: direct current sputtering, interchange sputtering, reactive sputtering and magnetron sputtering.Sputtered film is normally produced in the plasma of inert gas (as argon).The principle of sputtering use charged particle bombardment target, and during the Ions Bombardment surface of solids of acceleration, generation surface atom collides and the transfer of energy and momentum occurs, and makes target atom overflow from surface and be deposited on the process backing material.Because sputter procedure contains the conversion of momentum, so the particle sputtered is directive.Utilize sputtering that substrate material surface can be made to obtain metal, alloy or thin dielectric film.Adopt sputtering technology to have substrate temperature low, film matter is pure, and even tissue is closely knit, fastness and high repeatability and other advantages.
Ion assisted deposition (ion assisted deposition) is electron beam evaporation or deposition while, and the surface grown with certain energy, kind, ion beam bombardment that stream is strong is to improve a kind of method of film quality.
Pulsed laser deposition (Pulsed Laser Deposition, PLD), be also referred to as pulse laser ablation (pulsed laserablation, PLA), that one utilizes laser to bombard object, then by bombardment species precipitate out on different substrates, to be precipitated or a kind of means of film.PLD generally can be divided into following four-stage: the interaction stage of laser emission and target, the movement segment of melted material, melted material at depositional phase of substrate and film at the nucleation (nucleation) of substrate surface and generation phase.Pulsed laser deposition has good guarantor's composition, deposition rate is high, the test period is short, underlayer temperature requires that film that is low, preparation is even, technological parameter regulates arbitrarily, to advantages such as the kind of target do not limit.
Exemplarily, sputtering method body structure surface deposit thickness shown in Fig. 3 is adopted to be the W metal of 10nm.
Especially, in plated metal process, due to the impact of energetic atom or ion, hexagonal boron nitride substrate 1 surface in described default etched features 3 can produce defect, thus destroys hexagonal boron nitride surface structure.
Refer to Fig. 5 again, perform step S4: the metal level 4 peeling off described mask layer 2 and surface thereof.
Because described mask layer 2 adopts photoresist, be easy to be stripped, the metal level 4 on it also can be pulled away in photoresist stripping process, only leaves the metal level in default etched features region.
Finally refer to Fig. 6, perform step S5: described hexagonal boron nitride substrate is annealed, then removes the metal level 4 in described default etched features 3, obtain the step 5 of single-layer silicon nitride boron atomic thickness on described hexagonal boron nitride substrate 1 surface.
Especially, the object of annealing promotes that the dangling bonds on metal and destroyed hexagonal boron nitride surface are combined into key, well can remove the hexagonal boron nitride atom on top layer simultaneously, realize the corrasion to hexagonal boron nitride substrate when being beneficial to follow-up removal metal.
Concrete, the atmosphere of described annealing is Ar/H
2mist, gas flow ratio is 200:100 ~ 200:20, and annealing region is 200 ~ 1000 DEG C, and annealing time is 2 ~ 8 hours.In the present embodiment, in CVD stove, preferably adopt 600 DEG C of low pressure annealing 2 ~ 6 hours.
Concrete, adopt the metal level 4 in the described default etched features 3 of wet etching removal.Described wet etching adopts HCl, (NH4)
2s
2o
8, HNO
3, H
2sO
4or acetic acid solution.The concentration of described solution is 0.01 ~ 0.2mol/L, and wet etching soak time is 1min ~ 10hour.
Exemplarily, structure shown in annealed Fig. 5 is put into the NH4 that concentration is 0.02%)
2s
2o
8in solution, soak at room temperature 1 hour, makes the metal on h-BN surface dissolve completely.
Because metal is in deposition process, meeting effects on surface h-BN atomic layer forms destruction to a certain degree, thus forming dangling bonds on hexagonal boron nitride surface, annealing process makes this layer of destroyed hexagonal boron nitride and metal form chemical bond, or dissolving is in a metal.Therefore, in the process of wet etching dissolution of metals layer, one deck hexagonal boron nitride atomic layer below metal level will be pulled away thus obtain the described step 5 of single-layer silicon nitride boron atomic thickness.
Especially, owing to there is adhesion between top layer hexagonal boron nitride atom destroyed below the described metal level 4 of graphics field and metal, therefore in the process of dissolution of metals layer, one deck h-BN atomic layer below metal level will be pulled away (be similar to when sand washes away by rainwater and also taken away mud sticky on sand), thus obtains the described step 5 of single-layer silicon nitride boron atomic thickness.
So far, the step of single-layer silicon nitride boron atomic thickness is obtained in described hexagonal boron nitride substrate surface etching.
Embodiment two
Refer to Fig. 7, the present embodiment repeating said steps S2 ~ S5 on the basis of embodiment one at least one times, obtains the step of preset thickness at described boron nitride substrate surface.
Concrete, in the process of repeating said steps S2, can use same photomask, form mask lithography figure above original step, technique is simple, and can not increase mask costs.
In sum, boron nitride substrate surface step lithographic method of the present invention, etched features is preset by being formed in the mask layer on hexagonal boron nitride surface, plated metal subsequently, the hexagonal boron nitride underlayer surface in default etched features region is made to produce defect, then peel off preset mask layer around etched features and on metal, and described hexagonal boron nitride substrate is annealed, to promote that the dangling bonds on metal and destroyed hexagonal boron nitride surface are combined into key, solution removal is adopted to preset metal in etched features again, the hexagonal boron nitride atom that pre-etching region list layer is destroyed is taken away when metal is dissolved, form the step of individual layer atomic thickness.The method not only can control the patterned shape of hexagonal boron nitride, size, all right selective etching region, simultaneously through repeatedly etching, can control the height etching step, solving the graphical processing difficult problem based on hexagonal boron nitride thin-film device.So the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (12)
1. a boron nitride substrate surface step lithographic method, is characterized in that, comprise the steps:
S1: a hexagonal boron nitride substrate is provided;
S2: form mask layer at described hexagonal boron nitride substrate surface, and in described mask layer, form the default etched features exposing described hexagonal boron nitride substrate surface;
S3: depositing metal layers in described mask layer surface and described default etched features;
S4: the metal level peeling off described mask layer and surface thereof;
S5: anneal to described hexagonal boron nitride substrate, then removes the metal level in described default etched features, obtains the step of single-layer silicon nitride boron atomic thickness at described hexagonal boron nitride substrate surface.
2. boron nitride substrate surface step lithographic method according to claim 1, is characterized in that: described mask layer comprises photoresist or hard mask version.
3. boron nitride substrate surface step lithographic method according to claim 2, it is characterized in that: formed in the process of described default etched features in described mask layer, adopt uv-exposure method, electron beam exposure method, X-ray exposure method, ion beam exposure method or nano-imprint method in described mask layer, form the litho pattern of described default etched features.
4. boron nitride substrate surface step lithographic method according to claim 1, it is characterized in that: described metal level is elemental metals Ni, Al, Zn, Mg, Fe, Sn, Pb or Co, or described metal level is the alloy of described elemental metals.
5. boron nitride substrate surface step lithographic method according to claim 1, is characterized in that: the thickness of described metal level is 2 ~ 100nm.
6. boron nitride substrate surface step lithographic method according to claim 1, is characterized in that: the method depositing described metal level is electron-beam vapor deposition method, sputtering method, ion assisted deposition method or pulsed laser deposition.
7. boron nitride substrate surface step lithographic method according to claim 1, is characterized in that: the atmosphere of described annealing is Ar/H
2mist, gas flow ratio is 200:100 ~ 200:20, and annealing region is 200 ~ 1000 DEG C, and annealing time is 2 ~ 8 hours.
8. boron nitride substrate surface step lithographic method according to claim 1, is characterized in that: adopt the metal level in the described default etched features of wet etching removal.
9. boron nitride substrate surface step lithographic method according to claim 8, is characterized in that: described wet etching adopts HCl, (NH4)
2s
2o
8, HNO
3, H
2sO
4or acetic acid solution.
10. boron nitride substrate surface step lithographic method according to claim 9, is characterized in that: the concentration of described solution is 0.01 ~ 0.2mol/L, and wet etching soak time is 1min ~ 10hour.
11. boron nitride substrate surface step lithographic methods according to claim 1, is characterized in that: described hexagonal boron nitride substrate adopts mechanical stripping or chemical vapour deposition technique to obtain.
12. boron nitride substrate surface step lithographic methods according to claim 1 ~ 11 any one, it is characterized in that: after described step S5, repeating said steps S2 ~ S5 at least one times, obtains the step of preset thickness at described boron nitride substrate surface.
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| CN105575789A (en) * | 2015-12-23 | 2016-05-11 | 昆山工研院新型平板显示技术中心有限公司 | Method for patterning thin film |
| CN106835074A (en) * | 2017-01-19 | 2017-06-13 | 杭州电子科技大学 | A kind of method of boron nitride etching |
| CN109202297A (en) * | 2018-08-01 | 2019-01-15 | 南京理工大学 | A kind of laser wet etch process suitable for arbitrary surface transparent dielectric material |
| CN111421390A (en) * | 2020-02-29 | 2020-07-17 | 湖南大学 | Ion beam polishing processing method for manufacturing micro-nano step array structure |
| CN113233431A (en) * | 2021-04-30 | 2021-08-10 | 桂林电子科技大学 | Two-dimensional material film forming method |
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| CN105575789A (en) * | 2015-12-23 | 2016-05-11 | 昆山工研院新型平板显示技术中心有限公司 | Method for patterning thin film |
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| CN111421390A (en) * | 2020-02-29 | 2020-07-17 | 湖南大学 | Ion beam polishing processing method for manufacturing micro-nano step array structure |
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| CN113233431A (en) * | 2021-04-30 | 2021-08-10 | 桂林电子科技大学 | Two-dimensional material film forming method |
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