CN113097361A - Method for improving structural stability of LED - Google Patents
Method for improving structural stability of LED Download PDFInfo
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- CN113097361A CN113097361A CN202110354775.9A CN202110354775A CN113097361A CN 113097361 A CN113097361 A CN 113097361A CN 202110354775 A CN202110354775 A CN 202110354775A CN 113097361 A CN113097361 A CN 113097361A
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- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 42
- 239000003607 modifier Substances 0.000 claims abstract description 38
- 229910052751 metal Inorganic materials 0.000 claims abstract description 30
- 239000002184 metal Substances 0.000 claims abstract description 30
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 16
- 238000001704 evaporation Methods 0.000 claims abstract description 13
- 238000002791 soaking Methods 0.000 claims abstract description 12
- 239000005416 organic matter Substances 0.000 claims abstract description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 9
- 125000003282 alkyl amino group Chemical group 0.000 claims description 8
- 125000004414 alkyl thio group Chemical group 0.000 claims description 8
- ZFNFNJYRZOQPJF-UHFFFAOYSA-N trimethoxy(sulfanyl)silane Chemical compound CO[Si](S)(OC)OC ZFNFNJYRZOQPJF-UHFFFAOYSA-N 0.000 claims description 8
- 150000001413 amino acids Chemical class 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- -1 carboxylic acid thiols Chemical class 0.000 claims description 5
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 5
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical class S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 238000007385 chemical modification Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 125000003396 thiol group Chemical class [H]S* 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 125000000008 (C1-C10) alkyl group Chemical group 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 61
- 239000002094 self assembled monolayer Substances 0.000 abstract description 2
- 239000013545 self-assembled monolayer Substances 0.000 abstract description 2
- 238000001338 self-assembly Methods 0.000 description 9
- 239000000758 substrate Substances 0.000 description 8
- 238000000151 deposition Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 5
- 230000006872 improvement Effects 0.000 description 4
- 238000003892 spreading Methods 0.000 description 4
- 230000007480 spreading Effects 0.000 description 4
- 229910007157 Si(OH)3 Inorganic materials 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011241 protective layer Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910002699 Ag–S Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- OGQYPPBGSLZBEG-UHFFFAOYSA-N dimethyl(dioctadecyl)azanium Chemical compound CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC OGQYPPBGSLZBEG-UHFFFAOYSA-N 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/36—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the electrodes
- H01L33/40—Materials therefor
- H01L33/42—Transparent materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0016—Processes relating to electrodes
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Led Devices (AREA)
Abstract
The invention provides a method for improving the structural stability of an LED, which comprises the following steps: soaking the ITO in a solution containing a chemical modifier to obtain modified ITO; the chemical modifier is an organic matter containing amino and/or sulfydryl; and then, evaporating a metal layer on the modified ITO surface. Compared with the prior art, the chemical modifier self-assembled monolayer is formed on the ITO surface, and the chemical modifier contains amino and/or sulfydryl and can be further modified, so that the evaporated metal and the amino and/or the sulfydryl form stable chemical bonds, the adhesion between the ITO and the metal layer is improved, and the structural stability of the LED is further improved.
Description
Technical Field
The invention belongs to the technical field of semiconductor devices, and particularly relates to a method for improving the structural stability of an LED.
Background
A Light Emitting Diode (LED) emits light by using an energy difference between N-type and P-type semiconductors, and emits light energy, which is different from a light emitting principle of an incandescent lamp, and thus is called a cold light source. Because of its advantages of high durability, long life, light weight and low power consumption, LEDs are used in many fields such as signal indicator lamps, lighting devices and display devices, however, their light emitting efficiency is one of the important factors that restrict the popularization of LEDs.
The light emitting efficiency of the LED is influenced by factors such as packaging materials, packaging structures, fluorescent powder excitation efficiency, transparent electrode light transmittance and substrate reflectivity.
In order to improve the light extraction efficiency of the LED, ITO is generally used as the transparent electrode. ITO is a transparent electrode material with high electrical conductivity, high visible light transmittance, high mechanical hardness and good chemical stability.
However, when an LED is manufactured, metal is directly evaporated on the ITO surface (see fig. 1, fig. 1 is a schematic structural diagram of a conventional flip-chip LED, where 1 is a growth substrate, 2 is an epitaxial structure, 3 is a transparent conductive layer ITO, 4 is a mirro layer, 5 is a barrier layer, 6 is a P current spreading bar, 7 is an N current spreading bar, 8 is an insulating protective layer, and 9 is a metal electrode), and the adhesion property between the metal layer and the ITO is poor, which causes the metal layer to easily fall off during the process of manufacturing the LED, and during the subsequent wire bonding or welding electrode test.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for improving the structural stability of an LED.
The invention provides a method for improving the structural stability of an LED, which comprises the following steps:
soaking the ITO in a solution containing a chemical modifier to obtain modified ITO; the chemical modifier is an organic matter containing amino and/or sulfydryl;
and then, evaporating a metal layer on the modified ITO surface.
Preferably, the chemical modifier is selected from one or more of aminosilane, mercaptosilane, carboxylic acid thiol compound and amino acid amphoteric molecule.
Preferably, the chemical modifier is selected from compounds represented by formula (I) and/or formula (II):
wherein R is1And R3Each independently selected from amino, alkylamino, mercapto or alkylmercapto; r2Is C1-C10 alkyl; n is an integer of 1 to 20.
Preferably, the number of carbon atoms in the alkylamino group and the alkylmercapto group is preferably 1 to 10 independently; r2Is C2-C4 alkyl; n is an integer of 1 to 10.
Preferably, the number of carbon atoms in the alkylamino group and the alkylmercapto group is preferably 3 to 4 independently; r2Is C2-C3 alkyl; n is an integer of 1 to 4.
Preferably, the chemical modifier is selected from 3-aminopropyltriethoxysilane and/or mercaptotrimethoxysilane.
Preferably, the concentration of the chemical modifier in the solution containing the chemical modifier is 0.1-2 mol/L.
Preferably, the soaking time is 10-60 min.
Preferably, the metal layer is a nickel layer, a silver layer, a gold layer or a chromium layer.
Preferably, the thickness of the metal layer is
The invention provides a method for improving the structural stability of an LED, which comprises the following steps: soaking the ITO in a solution containing a chemical modifier to obtain modified ITO; the chemical modifier is an organic matter containing amino and/or sulfydryl; and then, evaporating a metal layer on the modified ITO surface. Compared with the prior art, the chemical modifier self-assembled monolayer is formed on the ITO surface, and the chemical modifier contains amino and/or sulfydryl and can be further modified, so that the evaporated metal and the amino and/or the sulfydryl form stable chemical bonds, the adhesion between the ITO and the metal layer is improved, and the structural stability of the LED is further improved.
Drawings
FIG. 1 is a schematic diagram of a conventional flip-chip LED;
FIG. 2 is a schematic diagram of the self-assembly of the chemical modifier of the present invention when it is aminosilane and/or mercaptosilane;
FIG. 3 is a schematic diagram of the self-assembly of the chemical modifier of the present invention in the form of carboxylic acid thiol compound and/or amino acid amphiphile;
fig. 4 is a schematic view of a manufacturing process of the flip LED chip provided by the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for improving the structural stability of an LED, which comprises the following steps: soaking the ITO in a solution containing a chemical modifier to obtain modified ITO; the chemical modifier is an organic matter containing amino and/or sulfydryl; and then, evaporating a metal layer on the modified ITO surface.
In the present invention, the sources of all raw materials are not particularly limited, and they may be commercially available.
Soaking ITO in a solution containing a chemical modifier; in the invention, the ITO can be ITO plated on glass or on the surface of a semiconductor epitaxial structure; the chemical modifier is preferably one or more of aminosilane, mercaptosilane, carboxylic acid thiol compounds and amino acid amphoteric molecules, and is more preferably a compound represented by formula (I) and/or formula (II):
wherein R is1And R3Each independently is amino, alkylamino, mercapto or alkylmercapto; the number of carbon atoms in the alkylamino group and the alkylmercapto group is preferably 1 to 10, more preferably 2 to 8, still more preferably 2 to 6, and most preferably 3 to 4.
R2Is an alkyl group of C1-C10, preferably an alkyl group of C1-C8, more preferably an alkyl group of C1-C6, still more preferably an alkyl group of C2-C4, most preferably an alkyl group of C2-C3; n is an integer of 1 to 20, preferably an integer of 1 to 15, more preferably an integer of 1 to 10, more preferably an integer of 1 to 6, and most preferably an integer of 1 to 4.
Most preferably in the present invention, the chemical modifier is 3-aminopropyltriethoxysilane and/or mercaptotrimethoxysilane.
The concentration of the chemical modifier in the solution containing the chemical modifier is preferably 0.1-2 mol/L, more preferably 0.1-1.5 mol/L, and still more preferably 0.5-1 mol/L; in the embodiment provided by the invention, the concentration of the chemical modifier in the solution containing the chemical modifier is specifically 0.5 mol/L; the solvent in the solution comprising the chemical modification agent is preferably water.
The soaking time is preferably 10-60 min, more preferably 20-50 min, and still more preferably 30-40 min. The chemical adsorption on the ITO surface can be completed by soaking, and the chemical modifier can form a stable and ordered monomolecular layer on the ITO surface through self-assembly. Referring to fig. 2 and fig. 3, fig. 2 is a schematic diagram of self-assembly when the chemical modifier is aminosilane and/or mercaptosilane, and fig. 3 is a schematic diagram of self-assembly when the chemical modifier is carboxylic acid thiol compound and/or amino acid amphiprotic molecule. The chemical modifier may be further modified because it has an amino group and/or a thiol group at its end.
Then, evaporating a metal layer on the modified ITO surface; the evaporation method is vacuum evaporation known to those skilled in the art, and is not particularly limited; the thickness of the metal layer is preferably
More preferably
Further preferred is
Most preferably
The metal layer is preferably a nickel layer, a silver layer, a gold layer or a chromium layer; the ITO surface self-assembled chemical modification molecules can be chelated with metal in the metal layer to form covalent bonds, so that the adhesion between the ITO and the metal layer is enhanced, and the stability of the ITO surface self-assembled chemical modification molecules is improved. With 3-aminopropyltriethoxysilane (APTES, H)2N(CH2)3Si(OC2H5)3) For example, the reaction of depositing an Ag layer on the ITO surface is as follows: h2N(CH2)3Si(OC2H5)3→H2N(CH2)3Si(OH)3→H2N(CH2)3Si(O-)3(ITO surface self-assembly forms ordered monomolecular layer) → Ag-N (CH)2)3Si(O-)3→Ag┄Ag-N(CH2)3Si(O-)3；
Similarly, 3-aminopropyltriethoxysilane (APTES, H)2N(CH2)3Si(OC2H5)3) For example, the reaction of depositing a Ni layer on the surface of ITO is as follows: h2N(CH2)3Si(OC2H5)3→H2N(CH2)3Si(OH)3→H2N(CH2)3Si(O-)3(ITO surface self-assembly forming ordered monolayer) → Ni-N (CH)2)3Si(O-)3→Ni┄Ni-N(CH2)3Si(O-)3；
Taking mercapto trimethoxy silane as an example, the reaction of evaporating an Ag layer on the ITO surface is as follows: HS (CH)2)3Si(OCH3)3→HS(CH2)3Si(OH)3→HS(CH2)3Si(O-)3(ITO surface self-assembly forms ordered monomolecular layer) → Ag-S (CH)2)3Si(O-)3→Ag┄Ag-S(CH2)3Si(O-)3。
In the embodiment provided by the present invention, specifically, taking preparation of a flip-chip LED chip as an example, see fig. 4, and fig. 4 is a schematic view of a preparation flow of the flip-chip LED chip, where 1 is a schematic view of a structure of an existing flip-chip LED, where 1 is a growth substrate, 2 is an epitaxial structure, 3 is a transparent conductive layer ITO, 4 is a chemical modifier, 5 is a mirro layer, 6 is a barrier layer, 7 is a P current spreading strip, 8 is an N current spreading strip, 9 is an insulating protective layer, and 10 is a metal electrode; a is to provide the growth substrate, B is to form the epitaxial structure and etch and expose the N type layer, C is to make transparent conducting layer ITO, D is to make the self-assembly chemical modifier, E is to make the mirror layer, F is to make the barrier layer, G is to make P, N extension strip, H is to make the chip insulating protective layer, I is to make P, N electrode.
In order to further illustrate the present invention, the following describes a method for improving the structural stability of the LED according to the present invention in detail with reference to the following embodiments.
The reagents used in the following examples are all commercially available.
Example 1
S1) providing a sapphire growth substrate.
S2) forming an epitaxial structure N-type GaN layer (with the thickness of 3 mu m) and a P-type GaN layer (with the thickness of 400nm) on the surface of the growth substrate and etching to expose the N-type layer.
S3) depositing a transparent conductive layer ITO (with the thickness of being equal to that of the epitaxial structure P-type GaN layer
) And then soaking the ITO layer in a mercaptotrimethoxysilane solution with the concentration of 0.5mol/L for 30min, taking out and drying to obtain the ITO modified by mercaptotrimethoxysilane.
S4) ion beam evaporation of a metal silver layer on the ITO surface modified by mercaptotrimethoxysilane is carried out, and the evaporation thickness is
Then evaporating and plating TiW/Pt/TiW with the total thickness of AgTiW/Pt/TiW
Then Ti/Pt/Ti/Pt/Ti/Pt/Ti/Pt is deposited on the surface as barrier layer with the deposition thickness of
S5) finally, respectively manufacturing a P expansion strip and an N expansion strip on the surfaces of the barrier layer and the exposed N-type layer to obtain the flip LED.
The performance of the flip LED obtained in the example 1 is tested by wire bonding, the phenomenon that the electrodes of ITO and a metal layer fall off can occur in the flip LED chip before improvement (namely, the flip LED chip is not soaked in a mercaptotrimethoxysilane solution, and the rest steps are the same as those in the example 1), the phenomenon that the electrodes of the ITO and the metal layer fall off is not generated in the chip after improvement obtained in the example 1, and the inference value of the average thrust is 5-10 g higher than that of the flip LED chip without improvement.
Example 2
S1) providing a sapphire growth substrate.
S2) forming an epitaxial structure N-type GaN layer (with the thickness of 3 mu m) and a P-type GaN layer (with the thickness of 400nm) on the surface of the growth substrate and etching to expose the N-type layer.
S3) depositing a transparent conductive layer ITO (with the thickness of being equal to that of the epitaxial structure P-type GaN layer
) And then soaking the ITO layer in a 3-aminopropyltriethoxysilane solution with the concentration of 0.3mol/L for 40min, taking out and drying to obtain the ITO modified by 3-aminopropyltriethoxysilane.
S4) depositing a metal Ni layer on the ITO surface ion beam modified by 3-aminopropyltriethoxysilane by evaporation with the thickness of
Then evaporating AlTiPtTiPtAu, wherein the total thickness of NiAlTiPtTiPtAu is
S5) finally depositing a passivation layer on the surface of the LED chip to obtain the normally-installed LED.
By utilizing the performance of the normally-installed LED obtained in the embodiment 2 through routing test, the electrode dropping phenomenon of ITO and a metal layer can occur on the normally-installed LED chip before improvement (namely the chip is not soaked in a 3-aminopropyltriethoxysilane solution, and other steps are the same as those in the embodiment 2), the electrode dropping phenomenon of ITO and the metal layer does not occur on the improved chip obtained in the embodiment 2, and the inference value of the average thrust is 3-5 g higher than that of the normally-installed LED chip which is not improved.
Claims (10)
1. A method for improving structural stability of an LED, comprising:
soaking the ITO in a solution containing a chemical modifier to obtain modified ITO; the chemical modifier is an organic matter containing amino and/or sulfydryl;
and then, evaporating a metal layer on the modified ITO surface.
2. The method of claim 1, wherein the chemical modifier is selected from one or more of aminosilanes, mercaptosilanes, carboxylic acid thiols, and amino acid amphiphiles.
3. The method of claim 1, wherein the chemical modification agent is selected from compounds of formula (I) and/or formula (II):
wherein R is1And R3Each independently selected from amino, alkylamino, mercapto or alkylmercapto; r2Is C1-C10 alkyl; n is an integer of 1 to 20.
4. The method according to claim 3, wherein the number of carbon atoms in the alkylamino group and the alkylmercapto group is preferably 1 to 10; r2Is C2-C4 alkyl; n is an integer of 1 to 10.
5. According to the rightThe method according to claim 3, wherein the number of carbon atoms in the alkylamino group and the alkylmercapto group is preferably 3 to 4; r2Is C2-C3 alkyl; n is an integer of 1 to 4.
6. The method of claim 1, wherein the chemical modifier is selected from the group consisting of 3-aminopropyltriethoxysilane and/or mercaptotrimethoxysilane.
7. The method according to claim 1, wherein the concentration of the chemical modifier in the solution containing the chemical modifier is 0.1-2 mol/L.
8. The method according to claim 1, wherein the soaking time is 10-60 min.
9. The method of claim 1, wherein the metal layer is a nickel layer, a silver layer, a gold layer, or a chromium layer.
10. The method of claim 1, wherein the metal layer has a thickness of
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