CN103966604A - LED (light-emitting diode) electrode removal solution and removal method - Google Patents
LED (light-emitting diode) electrode removal solution and removal method Download PDFInfo
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- CN103966604A CN103966604A CN201410221543.6A CN201410221543A CN103966604A CN 103966604 A CN103966604 A CN 103966604A CN 201410221543 A CN201410221543 A CN 201410221543A CN 103966604 A CN103966604 A CN 103966604A
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Abstract
The invention provides an LED (light-emitting diode) electrode removal solution and removal method. The method comprises the following steps: coating a negative photoresist, photoetching, immersing the electrode, carrying out vapor deposition on the electrode, and stripping the electrode. The electrode immersion is implemented by immersing the chip-bearing card plug into the electrode removal solution for 20-30 minutes, wherein the temperature of the solution is 40-50 DEG C. The electrode removal solution comprises 35-40 wt% of ferric chloride, 10-15 wt% of hydrochloric acid and the balance of water. The electrode removal method can effectively protect the SiO2 film layer and the TCL film layer without destroying the p-type GaN layer, thereby ensuring the quality of the product, saving the material cost and enhancing the production efficiency.
Description
Technical field
The present invention relates to the technical field that LED chip is manufactured, especially, the electrode that relates to a kind of LED chip is removed liquid and removal method.
Background technology
Photodiode (LED) is a kind of semiconductor diode, and it can be luminous energy by electric energy conversion.Its principle is that electric energy is many electronics and holes while causing than thermal equilibrium, meanwhile, due to compound electronics and the hole of reducing, causes new thermal equilibrium, and in recombination process, energy is emitted with the form of light.The substantive structure of photodiode is semi-conductor P-N knot, and it typically refers to, and the film that produces another kind of conduction type with diffusion, ion implantation or epitaxially grown method on a kind of crystal of conduction type makes.LED has been widely used in the every field such as street lamp, display screen, interior lighting, auto lamp.
The selected substrate material of LED chip roughly has three kinds at present, sapphire, silicon and silicon carbide, and sapphire is as comparative maturity of epitaxial substrate.Referring to Fig. 1; LED chip adopts the transparency conducting layer (transparentconductinglayer of high visible light transmissivity and low-resistivity; be abbreviated as TCL) as N-type GaN conductive layer, TCL rete top also has one deck to play a protective role and can increase the SiO of bright dipping
2film.Referring to Fig. 2, five kinds of metals of Ni/Al/Cr/Ni/AU form P electrode and N electrode in the mode of vacuum-evaporation successively.Two electrodes are positioned at the homonymy of chip, and P electrode is positioned at TCL top and part contacts with P layer, and N electrode directly contacts with N-GaN.
In actual production and R&D process, often there will be the situation that occurs quality abnormal or must do over again because of experiment demand because of reasons such as manual operation is ineffective, equipment failure, techniques.Such as finding that after evaporation metal electrode comes off or perk, electrode is scratched, electrode has pollution etc., now, for ensureing quality product, often needs the chip processing of doing over again.
At present, traditional removal technique is: remove SiO with chemical solution
2, electrode and TCL → evaporation TCL → TCL photoetching → TCL etching → removing photoresistance → alloy → deposition SiO
2→ PAD photoetching → SiO
2corrosion → electrode evaporation is also peeled off.There are two deficiencies in this kind of method:
1, rework step is more loaded down with trivial details, and production efficiency is low and wasted a large amount of Material Costs;
2, for the inert metal AU in lysis electrodes, the solution that the electrode of doing over again is at present used is all generally the acidic solution chloroazotic acid (mixing solutions that concentrated hydrochloric acid and concentrated nitric acid are made into by 3:1) by high density, chloroazotic acid is in corrosion target, corrode together with TCL rete, and chloroazotic acid can damage the P type GaN layer of chip surface, therefore, the voltage of chip after doing over again has the higher of greater probability, and the problem raising for alligatoring epitaxial wafer voltage is more obvious.Also have and adopt the slightly weak solution such as hydrochloric acid, sulfuric acid of corrosion strength as the electrode solution of doing over again, although can not damage GaN layer, but due to gold and the dissolution rate of nickel in the solution such as hydrochloric acid, sulfuric acid very slow, thereby the oversize production efficiency that affected of the time of doing over again.
As can be seen here, urgently develop a kind of efficient, to chip surface epitaxial film without the reworking method destroying, to solve the existing LED chip problem existing in treatment process of doing over again.
Summary of the invention
The object of the invention is to provide a kind of electrode of LED chip to remove liquid and removal method, to solve existing reworking method, chip surface epitaxial film is destroyed the technical problem of serious and inefficiency.
For achieving the above object, the electrode that the invention provides a kind of LED chip is removed liquid, comprises iron(ic) chloride and hydrochloric acid, and wherein the massfraction of iron(ic) chloride is 35-40%, and the massfraction of hydrochloric acid is 10-15%, and all the other are water.
Preferably, the massfraction of iron(ic) chloride is 36-38%.
Preferably, the massfraction of hydrochloric acid is 11-13%.
The present invention also provides a kind of electrode removal method of LED chip, comprises and applies negativity photoresistance, photoetching, immersion electrode, electrode evaporation, stripping electrode step:
Wherein, applying negativity photoresistance step is: evenly apply DNR-L300-D1 negativity photoresistance at chip surface, carry out photoetching two electrodes are exposed; After even glue, carry out hot plate baking, baking condition is 105 DEG C, 90-120 second; After baking, within cooling 1 minute, expose, after exposure, again on hot plate, toast, baking condition is 110 DEG C, 70-80 second; After cooling 2 minutes, the jam that chip is housed is put into the beaker that fills developing solution and develop, development 70-80 second;
Soaking electrode step is: the jam that chip is housed is put into electrode removal liquid and soak 20-30 minute, the temperature of solution is at 40 DEG C～50 DEG C; Described electrode is removed liquid and is comprised iron(ic) chloride and hydrochloric acid, and wherein the massfraction of iron(ic) chloride is 35-40%, and the massfraction of hydrochloric acid is 10-15%, and all the other are water;
When immersion, assist and carry out sonic oscillation, sonic oscillation frequency is 30-35KHz, and power is 500W.
Preferably, electrode evaporation step is:
With the plated film mode electrode evaporation of electron beam vacuum-evaporation, in coating process, cavity pressure setting is 1.5 × 10-6Torr, and Temperature Setting is 0 DEG C.
Preferably, stripping electrode step is:
Chip is peeled off with blue film, then chip is put into temperature is that the glue-dispenser of 85 DEG C soaks 15-20 minute.
Preferably, while applying negativity photoresistance, by photoresistance gauge control at 2.8um～2.9um.
The present invention has following beneficial effect:
1, protection epitaxial film: present method owing to there being the protection of photoresistance, can effectively protect the SiO above TCL rete in the time removing electrode
2rete, and the P type GaN layer of chip surface can be not destroyed, do not affect for other parts of LED chip structure, is applicable to allly because of technical need, the situation that electrically bad or bad order need to be done over again, has ensured the quality of product.
2, the harmless electrode of repeatedly removing: the method for selective removal electrode of the present invention can coordinate PAD photoetching process to implement selective removal to two electrodes; Can also be applied in the middle of ICP etching; can repeatedly remove electrode harmlessly; coordinate MESA photoetching process protect and N layer is carried out to multiple etching P layer; after each etching, only need electrode evaporation just can carry out testing electrical property; thereby can obtain the electrical parameter under the same chip different etching degree of depth, due to SiO
2rete, TCL rete and P type GaN are not damaged, and therefore electrical property difference is only from the impact of ICP etching depth.
3, save operation: the inventive method step is simple, evaporation TCL rete, TCL photoetching, TCL etching, removing photoresistance, alloy, deposition SiO after having avoided doing over again
2, SiO
2the series of steps such as corrosion, can save material cost and enhance productivity.
Except object described above, feature and advantage, the present invention also has other object, feature and advantage.Below with reference to figure, the present invention is further detailed explanation.
Brief description of the drawings
The accompanying drawing that forms the application's a part is used to provide a further understanding of the present invention, and schematic description and description of the present invention is used for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 is the LED chip epitaxial layer structure schematic diagram of the preferred embodiment of the present invention;
Fig. 2 is the electrode structure schematic diagram of the preferred embodiment of the present invention;
Wherein, 1, P electrode, 2, SiO
2rete, 3, TCL rete, 4, P type GaN layer, 5, N-type GaN layer, 6, N electrode, 7, substrate, 8, Ni metal level, 9, Al metal level, 10, Cr metal level, 11, Au metal level.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are elaborated, but the multitude of different ways that the present invention can limit and cover according to claim is implemented.
Referring to Fig. 1, Fig. 2, LED chip structure generally comprises from bottom to up: substrate 7, N-type GaN layer 5, N electrode 6, P type GaN layer 4, TCL rete 3, SiO
2rete 2 and P electrode 1; 6, P electrode 1 and N electrode comprise five layers from bottom to up: Ni metal level 8, Al metal level 9, Cr metal level 10, Ni metal level 8 and Au metal level 11.
A kind of electrode removal method that the invention discloses LED chip, comprises step:
A, photoetching: specific operation process is as follows:
1, even glue: control photoresistance thickness at 2.8um～2.9um;
2, soft roasting: to adopt hot plate soft roasting, 100 DEG C～105 DEG C of soft roasting temperature, 90 seconds～120 seconds soft roasting time;
3, exposure: exposure energy 80～90mj/cm
2;
4, firmly roasting: to adopt hot plate firmly roasting, 108 DEG C～112 DEG C of firmly roasting temperature, firmly roasting 60 seconds～90 seconds time;
5, develop: adopt developer for positive photoresist, when development, the jam that installs chip is put into the beaker that fills developing solution, when development, shake jam to guarantee to develop fully, development time 70 seconds～90 seconds;
6, bath is put into drier for 5 minutes again and is dried.
B, removal electrode:
The electrode that employing comprises iron(ic) chloride, hydrochloric acid and water is removed liquid, wherein the massfraction of iron(ic) chloride is 35-40%, the massfraction of hydrochloric acid is 10-15%, all the other are water, this solution does not have destruction to the GaN layer of chip surface, and remove the speed of electrode, within 20 minutes, just electrode can be removed clean.
Operating process and parameter while removing electrode are as follows:
The jam that chip is housed is put into electrode removal liquid soaks, control the temperature of solution at 40 DEG C～50 DEG C, when immersion, ceaselessly shake jam, simultaneously assisting ultrasonic vibration in immersion process, so that solution and nickel, aluminium lamination bottom electrode have and good contact and chemical reaction occurs.
The gold layer of top of electrodes and chromium layer can not be removed liquid reaction with electrode, when immersion, solution reacts with nickel, the aluminium lamination of electrode bottom from the sidewall of electrode, along with the carrying out of reaction, solution corrodes to the inside from sidewall, finally nickel, the aluminium lamination of electrode bottom is eroded completely, and electrode is now in hollow out state, electrode in hollow out state is easy to come off under the physical force of shake and sonic oscillation, thereby reaches the object of removing electrode.
Chemical equation is as follows:
Al+FeCl
3＝AlCl
3+Fe
2Al+6HCl＝2AlCl
3+3H
2
Ni+2F
eCl
3＝NiCl
2+2F
eCl
2
C, stripping electrode:
Concrete steps and parameter are as follows:
1, with blue film, chip is peeled off, to peel off metal and photoresistance;
2, chip being put into temperature is that the glue-dispenser of 80～90 DEG C soaks 15 minutes, to remove residual photoresistance;
3, bath is put into drier for 5 minutes again and is dried.
Be below the embodiment of the present invention, wherein adopted respectively the listed electrode of following table to remove the operation that liquid is removed electrode.
| Massfraction | Hydrochloric acid | Iron(ic) chloride | Water |
| Embodiment mono- | 10 | 35 | 55 |
| Embodiment bis- | 11 | 36 | 53 |
| Embodiment tri- | 12 | 37 | 51 |
| Embodiment tetra- | 13 | 38 | 49 |
| Embodiment five | 14 | 39 | 47 |
| Embodiment six | 15 | 40 | 45 |
Respectively with reworking method of the present invention and existing traditional reworking method 100 chips of doing over again, experimental result finds, the chip voltage mean value of reworking method of the present invention is lower 0.1 volt than the chip voltage mean value of existing reworking method.
As follows at the lower specific embodiment that uses the inventive method to do over again of multiple different operating modes (PAD photoetching, ICP etching and other manipulable);
Embodiment 1:
1) evenly apply DNR-L300-D1 negativity photoresistance at chip surface, carry out photoetching, so that two electrodes expose, and other place is protected by photoresistance.The full-automatic sol evenning machine of SVS that adopts precision and have good uniformity carries out even glue, and photoresistance thickness is 2.8um; After even glue, carry out hot plate baking, baking condition is 105 DEG C, 90 seconds; Baking cooling 1 minute afterwards then exposes under DNK Full-automatic exposure machine, and exposure energy is set as 90mj/cm
2; After exposure, again on hot plate, toast, baking condition is 110 DEG C, 80 seconds; After cooling 2 minutes, the jam that chip is housed is put into the beaker that fills developing solution and develop, develops 70 seconds, when development, shake jam so that develop abundant; Wash by water and after 5 minutes, put into drier and dry.
2) jam that chip is housed being put into iron(ic) chloride and hydrochloric acid massfraction is respectively 35% and 10% electrode and removes liquid and soak 20 minutes, the temperature of controlling solution is 45 DEG C, when immersion, ceaselessly shake jam assisting ultrasonic vibration, electrode is removed totally completely.Sonic oscillation frequency is 30KHz, and power is 500W.
3) with the plated film mode electrode evaporation of electron beam vacuum-evaporation, in coating process, cavity pressure setting is 1.0 × 10-6Torr, and Temperature Setting is 0 DEG C, and plated film power setting is 18%, and plated film rate setting was 6 dust/seconds.
4) with blue film, chip is peeled off, to peel off metal and photoresistance, then chip is put into temperature is that the glue-dispenser of 85 DEG C soaks 15 minutes, to remove residual photoresistance, washes by water and within 5 minutes, puts into drier again and dry.
Embodiment 2:
1) evenly apply DNR-L300-D1 negativity photoresistance at chip surface, carry out photoetching, so that two electrodes expose, and other place is protected by photoresistance.The full-automatic sol evenning machine of SVS that adopts precision and have good uniformity carries out even glue, and photoresistance thickness is 2.9um; After even glue, carry out hot plate baking, baking condition is 105 DEG C, 120 seconds; Baking cooling 1 minute afterwards then exposes under DNK Full-automatic exposure machine, and exposure energy is set as 85mj/cm2; After exposure, again on hot plate, toast, baking condition is 110 DEG C, 70 seconds; After cooling 2 minutes, the jam that chip is housed is put into the beaker that fills developing solution and develop, develops 80 seconds, when development, shake jam so that develop abundant; Wash by water and after 5 minutes, put into drier and dry.
2) jam that chip is housed being put into iron(ic) chloride and hydrochloric acid massfraction is respectively 38% and 13% electrode and removes liquid and soak 20 minutes, the temperature of controlling solution is 48 DEG C, when immersion, ceaselessly shake jam assisting ultrasonic vibration, electrode is removed totally completely.Sonic oscillation frequency setting is 35KHz, and power is 500W.
3) with the plated film mode electrode evaporation of electron beam vacuum-evaporation, in coating process, cavity pressure setting is 1.5 × 10-6Torr, and Temperature Setting is 0 DEG C, and plated film power setting is 15%, and plated film rate setting was 5 dust/seconds.
4) with blue film, chip is peeled off, to peel off metal and photoresistance, then chip is put into temperature is that the glue-dispenser of 85 DEG C soaks 15 minutes, to remove residual photoresistance, washes by water and within 5 minutes, puts into drier again and dry.
Taking 100 chips of doing over again as example, the inventive method comprises PAD photoetching, removes electrode, electrode evaporation, four operations such as peels off, and wherein PAD photoetching takes 2 hours, removes electrode and takes altogether half an hour, and electrode evaporation takes 2 hours, peels off and takes altogether half an hour.Whole flow process takes 5 hours.
And existing traditional method comprises and removes SiO with chemical solution
2, electrode and ITO → evaporation TCL (taking 2 hours) → TCL photoetching (taking 2 hours) → TCL etching and removing photoresistance (taking 1 hour) → alloy (taking 1 hour) → deposition SiO
2(taking half an hour) → PAD photoetching → SiO
2corrosion (taking half an hour) → electrode evaporation → peel off, has more evaporation TCL, TCL photoetching, TCL etching and removing photoresistance, alloy, deposition SiO than the present invention
2, SiO
2corrosion totally six operations, multiplex 7 hours, 12 hours consuming time altogether.Be existing method consuming time be 2.4 times of the inventive method.
And, respectively with reworking method of the present invention and existing traditional reworking method 100 chips of doing over again, found that, lower 0.1 volt than existing reworking method chip voltage mean value after treatment through reworking method of the present invention chip voltage mean value after treatment, chip quality is significantly increased.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. the electrode of LED chip is removed a liquid, it is characterized in that, comprise iron(ic) chloride and hydrochloric acid, wherein the massfraction of iron(ic) chloride is 35-40%, and the massfraction of hydrochloric acid is 10-15%, and all the other are water.
2. the electrode of a kind of LED chip according to claim 1 is removed liquid, it is characterized in that, the massfraction of iron(ic) chloride is 36-38%.
3. the electrode of a kind of LED chip according to claim 1 is removed liquid, it is characterized in that, the massfraction of hydrochloric acid is 11-13%.
4. the electrode removal method of a LED chip, is characterized in that, comprises and applies negativity photoresistance, photoetching, immersion electrode, electrode evaporation, stripping electrode step:
Wherein, applying negativity photoresistance step is: evenly apply DNR-L300-D1 negativity photoresistance at chip surface, carry out photoetching two electrodes are exposed; After even glue, carry out hot plate baking, baking condition is 105 DEG C, 90-120 second; After baking, within cooling 1 minute, expose, after exposure, again on hot plate, toast, baking condition is 110 DEG C, 70-80 second; After cooling 2 minutes, the jam that chip is housed is put into the beaker that fills developing solution and develop, development 70-80 second;
Soaking electrode step is: the jam that chip is housed is put into electrode removal liquid and soak 20-30 minute, the temperature of solution is at 40 DEG C～50 DEG C; Described electrode is removed liquid and is comprised iron(ic) chloride and hydrochloric acid, and wherein the massfraction of iron(ic) chloride is 35-40%, and the massfraction of hydrochloric acid is 10-15%, and all the other are water;
When immersion, assist and carry out sonic oscillation, sonic oscillation frequency is 30-35KHz, and power is 500W.
5. the electrode removal method of a kind of LED chip according to claim 4, is characterized in that, electrode evaporation step is:
With the plated film mode electrode evaporation of electron beam vacuum-evaporation, in coating process, cavity pressure setting is 1.5 × 10-6Torr, and Temperature Setting is 0 DEG C.
6. the electrode removal method of a kind of LED chip according to claim 4, is characterized in that, stripping electrode step is:
Chip is peeled off with blue film, then chip is put into temperature is that the glue-dispenser of 85 DEG C soaks 15-20 minute.
7. the electrode removal method of a kind of LED chip according to claim 4, is characterized in that, while applying negativity photoresistance, by photoresistance gauge control at 2.8um～2.9um.
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|---|---|---|---|
| CN201410221543.6A CN103966604A (en) | 2014-05-23 | 2014-05-23 | LED (light-emitting diode) electrode removal solution and removal method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112928020A (en) * | 2021-02-08 | 2021-06-08 | 江苏艾森半导体材料股份有限公司 | Etching method of gold-nickel film and application thereof |
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| CN103046050A (en) * | 2011-10-17 | 2013-04-17 | 关东化学株式会社 | Etching liquid composition and etching method |
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| JP2010138451A (en) * | 2008-12-11 | 2010-06-24 | Ulvac Japan Ltd | Etchant and etching method |
| CN102108512A (en) * | 2009-12-25 | 2011-06-29 | 比亚迪股份有限公司 | Chemical etching liquid for metals and etching method |
| CN101944562A (en) * | 2010-09-03 | 2011-01-12 | 湘能华磊光电股份有限公司 | Method for removing light-emitting diode (LED) chip electrode |
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