CN101660187B - Method for manufacturing submicron figure substrate based on preforming anode alumina - Google Patents
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- CN101660187B CN101660187B CN2009101923319A CN200910192331A CN101660187B CN 101660187 B CN101660187 B CN 101660187B CN 2009101923319 A CN2009101923319 A CN 2009101923319A CN 200910192331 A CN200910192331 A CN 200910192331A CN 101660187 B CN101660187 B CN 101660187B
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- 239000000758 substrate Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 35
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 46
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000004005 microsphere Substances 0.000 claims abstract description 40
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 11
- 238000005530 etching Methods 0.000 claims abstract description 8
- 239000004411 aluminium Substances 0.000 claims description 40
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 27
- 238000003475 lamination Methods 0.000 claims description 23
- 230000003647 oxidation Effects 0.000 claims description 23
- 238000007254 oxidation reaction Methods 0.000 claims description 23
- 229920002120 photoresistant polymer Polymers 0.000 claims description 20
- 238000005260 corrosion Methods 0.000 claims description 17
- 230000007797 corrosion Effects 0.000 claims description 17
- 239000011148 porous material Substances 0.000 claims description 17
- 229910052759 nickel Inorganic materials 0.000 claims description 15
- 239000004793 Polystyrene Substances 0.000 claims description 12
- 229920002223 polystyrene Polymers 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 229910052594 sapphire Inorganic materials 0.000 claims description 7
- 239000010980 sapphire Substances 0.000 claims description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000011806 microball Substances 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 238000001020 plasma etching Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000011135 tin Substances 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910017083 AlN Inorganic materials 0.000 claims description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 2
- -1 anodised time Substances 0.000 claims description 2
- 238000001311 chemical methods and process Methods 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 238000009834 vaporization Methods 0.000 abstract 3
- 230000008016 vaporization Effects 0.000 abstract 3
- 238000007747 plating Methods 0.000 abstract 2
- 238000007743 anodising Methods 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 230000003628 erosive effect Effects 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000001117 sulphuric acid Substances 0.000 description 3
- 235000011149 sulphuric acid Nutrition 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 125000002015 acyclic group Chemical group 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001459 lithography Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
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Abstract
The invention discloses a method for manufacturing a submicron figure substrate based on preforming anode alumina. The method comprises the following steps: firstly, plating an aluminum layer on a substrate; coating a microsphere structure layer on the surface of the aluminum layer evenly, plating erosion-resistance metal on the surface of a microsphere by vaporization, precipitating the erosion-resistance metal which is plated by vaporization on the surface of the aluminum layer by a clearance of the microsphere structure layer, and then removing the microsphere structure layer; eroding by dilute acid, forming a recess between the metal which is plated by vaporization on the aluminum layer and completing a preforming process; removing the erosion-resistance metal on the aluminum layer by concentrated acid; anodizing the aluminum layer and forming an alumina layer with a preset hole structure figure; taking the alumina layer as a mask and transferring the hole structure figure on the alumina layer onto the substrate by etching; and removing the alumina layer and obtaining the substrate with a submicron figure. The invention has the advantages of simple and quick operation, lower cost and controllable aperture.
Description
Technical field
The present invention relates to partly lead material growth field, relate in particular to a kind of method for manufacturing submicron figure substrate based on preforming anode alumina.
Background technology
The III-V group iii v compound semiconductor material is at photodiode, semiconductor laser, detector, and the electron device aspect has a wide range of applications.Solid state lighting is now popular topic, and gan (GaN) is a kind of important materials of solid state lighting, is exactly the core topic of solid state lighting and improve the light extraction efficiency.Wherein use graph substrate can effectively reduce between epitaxial film and the foreign substrate because the stress that lattice mismatch and thermal mismatching are brought gathers, improved the luminous efficiency of luminescent device.The graph substrate early stage of development,, generally adopt the figure of micron dimension owing to the restriction of Technology.Anodised aluminium (anodic aluminum oxide in recent years, AAO) technology constantly develops, can make the aperture is the following periodicity pore space structures of 500 nanometers, and is applied to by the mask lithography technology in the making of graph substrate, and the performance of luminescent device is effectively improved.
Traditional anodised aluminium is mainly realized by two step anodic oxidations.Because in the first step oxidation, hole produces randomly at alumina surface.This only causes the hole regularity of distribution of the aluminum oxide that obtains through oxidation step relatively poor.Adopt two step anodic oxidations can improve this situation.The first step oxidation is to form hole more clocklike on the aluminium surface.Earlier the zone of oxidation on aluminium surface is removed before the second step oxidation, that pitting clocklike will occur much on the aluminium surface, then carries out the second step oxidation.This step will form hole clocklike in whole zone of oxidation.
There are some shortcomings in the method that two-step oxidation is made anodised aluminium: one is exactly the more about several microns of size of hole, and the aperture is difficult to control; Second be exactly time of needing long.New technology is used in carries out pretreated method and has substituted for the first time that oxidation improves these shortcomings on the aluminium surface.One of them method is the array that carves the hexagon small salient point with beamwriter lithography on the single-crystal silicon carbide disk, is going out hexagonal pitting as mould at aluminium surface coining with this array.Through after the anodic oxidation, the position of these pittings will become hole.The big I of shape and size of the resulting hole of this a kind of method is determined by mould.The pretreated method that another control hole forms is exactly that elder generation carves pitting with focused ion beam (FIB) on the Al surface, forms anodised aluminium based on this.The preformed method of above-mentioned some, the technology cost is more expensive, is not suitable for large batch of industrialization growth.How adopting the cheap material and the graphic structure of prepared sub-micrometer scale, is a problem that the important application meaning is arranged.
Summary of the invention
At the shortcoming of prior art, the purpose of this invention is to provide a kind of simple to operate, quick, cost is lower, the method for manufacturing submicron figure substrate based on preforming anode alumina of controllable aperture.
For achieving the above object, technical scheme of the present invention is: a kind of method for manufacturing submicron figure substrate based on preforming anode alumina, and it may further comprise the steps: (1) plates an aluminium lamination earlier on substrate; (2) evenly apply a micro-sphere structure layer on the aluminium lamination surface, and in microsphere surface evaporation corrosion resistant metal, the corrosion resistant metal of evaporation will be deposited on the aluminium lamination surface by the micro-sphere structure lamellar spacing, the micro-sphere structure layer be removed again; (3) corrode with diluted acid, between the metal of institute's evaporation on the aluminium lamination, form pit, finish preformed process; (4) utilize concentrated acid that the corrosion resistant metal on the aluminium lamination is removed; (5) aluminium lamination is carried out anodic oxidation, form alumina layer with default pore space structure figure; (6) utilize alumina layer as mask, by etching with the pore space structure figure transfer on the alumina layer to substrate; (7) remove alumina layer, obtain the substrate of submicron figure.
Described substrate is sapphire, silicon, silicon carbide, gan, aluminium nitride, zinc oxide or gallium arsenide.
Described micro-sphere structure layer is made of polystyrene, silicon oxide or epoxy third lipoid microsphere.
Hole size is by the size decision of microballoon, by chemical process corrosion or plasma etching method control diameter of micro ball and size at interval.
By oxygen ICP etching micro-sphere structure layer, change diameter of micro ball, the size of regulating microballoon.
In the step (5), place polyprotonic acid feeding certain voltage to carry out oxidation substrate and aluminium lamination, polyprotonic acid is 5% phosphoric acid, 10% sulfuric acid or 5% oxalic acid, and its corresponding voltage is 100V～130V, 25～27V or 30～50V.
In the step (2), be coated with one deck photoresist material on the aluminium lamination surface earlier, again the spin coating of micro-sphere structure layer mixing water got on, afterwards its heating is dried,, when removing the micro-sphere structure layer photoresist material is removed simultaneously so that the micro-sphere structure layer is attached on the photoresist material.
In the step (2), described corrosion resistant metal is gold, nickel, chromium or tin.
In the step (5), periodically the aperture of pore space structure changes by the method for the diameter of regulating polystyrene microsphere, anodised time, acid strength, and the pore space structure degree of depth was regulated by the anodised time.
In the step (6), the figure of anodic oxidation rear oxidation aluminium lamination is a pore space structure periodically, its by wet chemical or dry plasma etch with figure transfer to substrate.
Compared with prior art, the present invention has following advantage:
The present invention's fabrication cycle or acyclic figure.Utilize the method for anodised aluminium fabrication techniques graphic structure with respect to other, this method is through a preliminary shaping and an anode aluminaization submicron figure to be transferred on the semiconductor epitaxial material, has simple to operate, quick, cost is lower, advantages such as controllable aperture.
Description of drawings
Fig. 1～7th, the whole process flow side schematic view of making sapphire graphical substrate among the embodiment 1
About accompanying drawing, 1 represents substrate among the figure, and 2 represent aluminium lamination, and 3 represent the micro-sphere structure layer, and 4 represent the corrosion resistant metal layer, and 5 representatives are through anodic oxidation rear oxidation aluminium.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in detail.
Embodiment 1
Referring to Fig. 7, be the epitaxially grown graph substrate side schematic view that can be used for of final molding.Wherein comprise Sapphire Substrate 1.Wherein Sapphire Substrate can change other substrates into, and as silicon (Si), silicon carbide (SiC), gan (GaN), aluminium nitride (AlN), zinc oxide (ZnO), gallium arsenide (GaAs) substrate, or other are used for the substrate material of nitride material growth.
With the Sapphire Substrate is example, and the preparation method of graph substrate shown in Figure 1 may further comprise the steps:
A, elder generation are with Sapphire Substrate chemical solution and pure water, and ultrasonic cleaning is clean.On substrate 1, plate the aluminium lamination 2 of 2～5 μ m.Then its phosphoric acid with 5% was polished 5 minutes down at 5 ℃, voltage is 100V, as shown in Figure 1.
B, microballoon and ethanol are hybridly prepared into mixing solutions, and mixing solutions is spin-coated on the aluminium lamination surface.Polystyrene microsphere will be gathered into unit molecule micro-sphere structure layer, as shown in Figure 2.Described micro-sphere structure layer is made of polystyrene, silicon oxide or epoxy third lipoid microsphere.Present embodiment adopts polystyrene microsphere.
C, deposit corrosion resistant metal on the micro-sphere structure layer, described corrosion resistant metal is gold, nickel, chromium or tin, and present embodiment adopts the nickel metal, and its thickness is 10nm.Because exist the gap between the microballoon, the pairing substrate in gap will deposit last layer nickel, as shown in Figure 3.Then substrate, aluminium lamination and micro-sphere structure layer are immersed in the DI water, the micro-sphere structure layer are separated with aluminium lamination by the method for ultrasonic vibration.And clean with organic solvent and pure water ultrasonic cleaning, as shown in Figure 4.
D, substrate and the aluminium lamination that has a metal are immersed in 10% dilute sulphuric acid the inside 2 minutes because nickel has solidity to corrosion to dilute sulphuric acid aluminium easily with the dilute sulphuric acid reaction, so there is not that a part of aluminium of nickel protection to be gone down the formation pit by corrosion fast.Will form default pore space structure like this, can be designed to periodically or acyclic pore space structure, as shown in Figure 5 according to actual needs.
E, sample carry out oxidation 2～10 hour at 5%, 100 ℃ of phosphoric acid under with the voltage of 100V through cleaning the back.After oxidation, can obtain tens alumina layers, as shown in Figure 6 to the hundreds of nanometer.This step can prolong or the minimizing time as required, and obtains the different hole diameter and the degree of depth.
F, utilize this formable layer anodised aluminium as mask, on ICP,, the periodic pattern on the anodised aluminium is transferred on the substrate with Ar gas plasma etching, so just on substrate, obtain periodically pore space structure, as shown in Figure 7.
G, erode the anodised aluminium mask layer.
H, sample are clean with ultrasonic cleaning.
To this step, just can obtain having the periodically substrate of pore space structure, as Fig. 7.Grown epitaxial layer in the above.
Similar to embodiment 1, because introduce nickel preformed the time as mask being Al,, can between steps d, e, add the step of removing nickel in order to eliminate the influence that nickel may be introduced in subsequent step.Rafifinal passivation can occur at the sulfuric acid of concentration more than 80%, has solidity to corrosion, and nickel does not then have solidity to corrosion.Utilize above said characteristic, nickel can be removed, and less to the influence of aluminium.
Specific implementation method is: the steps d in embodiment 1, e add following steps between the step:
Sample is immersed at normal temperatures in 98% the vitriol oil 10～30 minutes.The concrete time is according to the thickness decision of nickel dam.
Directly polystyrene microsphere and alcoholic acid mixing solutions are spin-coated on the surface of Al, the bonding strength that might occur between microballoon and the Al is not enough, and causes the microballoon position problem that moves to occur.In order to address this is that, can be coated with one deck photoresist material on the Al surface earlier, again the spin coating of microballoon mixing water is got on.This step can not be used organic solution, and organic solution can be influential to photoresist material.Afterwards its heating is dried, microballoon will be attached on the photoresist material.With acetone or glue-dispenser photoresist material and microballoon are together removed at last.
Specific implementation method is to carry out following steps after step a:
A, apply the photoresist material of 600nm after will sample cleaning in the above, the thickness of photoresist material does not need very high, mainly be requirement entire sample surface-coated evenly.Sample is placed on the hot plate with 100 ℃ of heating 30 seconds, and purpose is only to make the photoresist material surface cure.
B, polystyrene microsphere and water are hybridly prepared into mixing solutions, and mixing solutions is spin-coated on the photoresist material surface.Polystyrene microsphere will be gathered into the unimolecular layer structure.Sample is being placed on the hot plate with 100 ℃ of heating 2 minutes.Microballoon will some imbed the photoresist material the inside like this, and this just reaches the fixedly purpose of microballoon.
C, sample is being used the oxygen etching on ICP.That a part of photoresist material that does not have microballoon to stop so can be etched into.The oxygen etching be requirement will not be blocked the part photoresist material all remove, until the Al layer till.
D, the nickel of 10nm on the evaporation in the above, that is nickel on the position that does not have photoresist material will deposit.
E, photoresist material is removed with acetone or glue-dispenser.Microballoon also can be along with photoresist material removes together.Use organic solvent and pure water ultrasonic cleaning clean at last.Till this step, just can obtain the sample that step c obtains among the embodiment 1.
F, following step just can be carried out according to steps d～g among the embodiment 1.
Because the size of microballoon is that standard, fixed are arranged, so the aperture in hole, hole just can not be regulated arbitrarily.Can after applying polystyrene microsphere, promptly behind the step b of embodiment 1,, diameter of micro ball be diminished, regulate the size of microballoon with oxygen ICP etching.To realize to hole and adjusting at interval.Then carry out step c again.
Claims (8)
1. method for manufacturing submicron figure substrate based on preforming anode alumina is characterized in that may further comprise the steps:
(1) on substrate, plates an aluminium lamination earlier;
(2) evenly apply a micro-sphere structure layer on the aluminium lamination surface, and in microsphere surface evaporation corrosion resistant metal, the corrosion resistant metal of evaporation will be deposited on the aluminium lamination surface by the micro-sphere structure lamellar spacing, the micro-sphere structure layer be removed again; Described corrosion resistant metal is gold, nickel, chromium or tin;
(3) corrode with diluted acid, between the metal of institute's evaporation on the aluminium lamination, form pit, finish preformed process;
(4) utilize concentrated acid that the corrosion resistant metal on the aluminium lamination is removed;
(5) aluminium lamination is carried out anodic oxidation, form alumina layer with default pore space structure figure;
(6) utilize alumina layer as mask, by etching with the pore space structure figure transfer on the alumina layer to substrate;
(7) remove alumina layer, obtain the substrate of submicron figure.
2. making method according to claim 1 is characterized in that: described substrate is sapphire, silicon, silicon carbide, gan, aluminium nitride, zinc oxide or gallium arsenide.
3. making method according to claim 1 is characterized in that: described micro-sphere structure layer is made of polystyrene, silicon oxide or epoxy third lipoid microsphere.
4. making method according to claim 3 is characterized in that: hole size is by the size decision of microballoon, by chemical process corrosion or plasma etching method control diameter of micro ball and size at interval.
5. making method according to claim 3 is characterized in that: by oxygen ICP etching micro-sphere structure layer, change diameter of micro ball, the size of regulating microballoon.
6. according to each described making method of claim 1 to 5, it is characterized in that: in the step (2), earlier be coated with one deck photoresist material on the aluminium lamination surface, again the spin coating of micro-sphere structure layer mixing water is got on, afterwards its heating is dried, so that the micro-sphere structure layer is attached on the photoresist material, when removing the micro-sphere structure layer photoresist material is removed simultaneously.
7. making method according to claim 1, it is characterized in that: in the step (5), micro-sphere structure is made of polystyrene, default pore space structure is the periodicity pore space structure, periodically the aperture of pore space structure changes by the method for the diameter of regulating polystyrene microsphere, anodised time, acid strength, and the pore space structure degree of depth was regulated by the anodised time.
8. making method according to claim 1 is characterized in that: in the step (6), the figure of anodic oxidation rear oxidation aluminium lamination is a pore space structure periodically, its by wet chemical or dry plasma etch with figure transfer to substrate.
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| US8513780B2 (en) | 2010-06-22 | 2013-08-20 | Institute of Microelectronics, Chinese Academy of Sciences | Semiconductor device having inter-level dielectric layer with hole-sealing and method for manufacturing the same |
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