CN105274530B - The nickel photoetching corrosion formula of liquid and caustic solution that a kind of suitable multilayer film circuit makes - Google Patents
The nickel photoetching corrosion formula of liquid and caustic solution that a kind of suitable multilayer film circuit makes Download PDFInfo
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- CN105274530B CN105274530B CN201510594064.3A CN201510594064A CN105274530B CN 105274530 B CN105274530 B CN 105274530B CN 201510594064 A CN201510594064 A CN 201510594064A CN 105274530 B CN105274530 B CN 105274530B
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Abstract
The nickel photoetching corrosion formula of liquid and caustic solution that a kind of suitable multilayer film circuit makes, formula include hydrofluoric acid, nitric acid and deionized water；The volume ratio of each component is as follows：Hydrofluoric acid：Nitric acid：Deionized water=(0.8 1.2)：(2.5‑3.5)：2.Using the multilayer film circuit nickel layer of inventive formulation corrosion 40 × micro- Microscopic observation, lines side wall is smooth, steep, and no metallic diaphragm inside contracts, no zigzag protrusion or indent；The front and rear comparison film adhesion of corrosion is without significant change, phenomena such as no film layer warps, comes off；Through up to a hundred corrosion verifications, line quality is good, and corrosion process is easy to control, and etching process is relatively stable.
Description
Technical field
The present invention relates to a kind of nickel photoetching corrosion formula of liquid.
Background technology
Ni layers are used as a kind of proper alignment metallic diaphragm, in microwave multilayer film circuit (such as (Ta2N)-NiCr-Ni-Au) system
The effect of barrier layer and the solder of resistance to SnPb welding is primarily served in work, manufacture craft includes the physical vapor deposition of nickel film layer
The figure of (magnetron sputtering) and nickel layer corrodes.In practical applications, technologists determine the magnetron sputtering of complete set
(Ta2N) the production method of-NiCr-Ni-Au film layer structures, but to realize the multilayer film circuit graphic making that lines are neat, steep
When, need to use the method for mask pattern transfer into spin coating on film substrate, exposure, development, corrode successively Au, Ni, NiCr,
Ta2N.In corrosion system, Au, NiCr, Ta2The corrosive liquid of N is more mature, suitable for multilayer film circuit graphic making technique, but
It is that Ni corrosive liquids are difficult to search out suitable technical recipe in multilayer film circuit making.
By data check and investigation, common Ni corrosive liquids be mainly nitric acid with ammonium ceric nitrate, nitric acid and nitric acid pick cerium,
The mixed aqueous solutions such as nitric acid and ammonium persulfate find that corrosive effect is poor after carrying out the corrosion of figure using above-mentioned several formulas,
Line edge is substantially irregular after showing as corrosion, is serrated, it is impossible to meet examination and test of products standard and aerospace product high quality
Making demand.Main cause is：On the one hand, there is Local map on same circuit wafer for Ni layers often in the process in corrosion in corrosive liquid
Shape corrodes halfway phenomenon, treats to corrode clean, other positions excessive erosion at last；On the other hand, conventional corrosion liquid
It is not strong to the corrosion process selectivity of Ni and NiCr, while corroding Ni layers, also it can corrode NiCr layers with faster corrosion rate,
Ni layers are caused not etch completely also, the NiCr layers of bottom have occurred and that apparent lateral erosion, and the lines of product figure is caused to make
It is second-rate.
The content of the invention
The technology of the present invention solves the problems, such as：A kind of suitable multilayer film circuit system is overcome the deficiencies of the prior art and provide
The nickel photoetching corrosion formula of liquid and caustic solution of work.
The present invention technical solution be：The nickel photoetching corrosion formula of liquid that a kind of suitable multilayer film circuit makes, including
Hydrofluoric acid solution, salpeter solution and deionized water；The volume ratio of each component is as follows：
Hydrofluoric acid solution：Salpeter solution：Deionized water=(0.8-1.2)：(2.5-3.5)：2.
The optimal volume ratio of hydrofluoric acid solution, salpeter solution and deionized water is 1：3：2.
A kind of nickel photoetching corrosion method that suitable multilayer film circuit makes, step are as follows：
(1) under ventilation condition, according to above-mentioned formula rate, the deionization that hydrofluoric acid addition has been pre-metered first
In water, then add in nitric acid, stirred after addition, stand, cool down after obtain corrosive liquid；
(2) the multilayer film circuit full wafer of the nickel layer to be corroded by photoresist protection is immersed to the corrosive liquid in step (1)
In corroded, forThe Ni layers of thickness, etching time 3-7 seconds, 25 DEG C -35 DEG C of corrosion temperature are rotten
The relative motion of holding circuit and corrosive liquid during erosion.
Ni layers etch after immediately using deionized water surface washing is clean.
The present invention has the beneficial effect that compared with prior art：
Using the multilayer film circuit nickel layer of inventive formulation corrosion 40 × micro- Microscopic observation, lines side wall is smooth, steep
Directly, no metallic diaphragm inside contracts, no zigzag protrusion or indent；The front and rear comparison film adhesion of corrosion is without significant change, no film layer
Phenomena such as warping, coming off；Through up to a hundred corrosion verifications, line quality is good, and corrosion process is easy to control, and etching process is more
Stablize.
Description of the drawings
Fig. 1 is schematic diagram before corrosion；
Fig. 2,3 be corrosion process of the present invention diagrammatic cross-section.
Specific embodiment
The present invention proposes a kind of new Ni film layer corrosive liquids for being suitble to nickeliferous multilayer film circuit, to solving film applications
The etching problem of common Ni sputtered layers is highly effective.Ni film layers are that the thickness obtained by magnetically controlled sputter method is aboutFibre structure columnar grain film, the target used is 99.99%Ni targets.
After the sputtering parameter of Ni determines, in terms of Ni film layer photoetching corrosions, a large amount of in-depth study work have been carried out.By
Inquire about the chemical corrosion liquid list of various metallic elements, it is known that the optimal caustic solution of the Ni film layers is oxidation corrosion, using nitre
The acid solutions such as acid or hydrofluoric acid can realize such corrosion of metal.Different Ni corrosive liquids experiments such as following table.
In experiment 1., room temperature corrosionThe Ni film layers of thickness, after corroding 40s-50s, Ni layers of corrosion
Thoroughly, but line edge sideetching is serious；Line edge remains substantial amounts of Ni layers and (is seen under 40 × microscope during less than 40s
It examines).
In experiment 2., room temperature corrosionNi film layers the etching time about 90s, Local residues Ni of thickness
Layer, and corrosion photoresist is peeling-off for a long time, lines sideetching is serious.
In experiment 3., water-bath adds in Ni layers of corrosion, and etching time about 4-15s, fine lines sideetching is tight after corrosion
Weight, 40 × micro- Microscopic observation, Ni layers etch latter NiCr layers and are also corroded.
In experiment 4., etching time about 4min, corrosion rate is slower, film layer darkly color after corrosion, after further corroding
Figure is serrated.
In experiment 5., etching time about 4min, corrosion rate is slower, film layer darkly color after corrosion, after further corroding
Local figure still has residual film layer.
The present invention with conventional several etch recipes by having carried out lots of comparing experiments, mainly to the details such as lines of corrosion
Adhesive force Weaken degree, the stability of etching process after the steep degree of side, corrosion are compared research；By to formula
It continues to optimize, for stringent graphical quality requirement, a large amount of adjustment has been carried out to the fine scale of several ingredients in corrosive liquid, have been made
Reached optimal corrosive effect.Meanwhile in definite Ni corrosion is also formulated, it has been found that if hydrofluoric acid ratio liter
Height after nitric acid ratio reduces, reacts more violent, process control is poor, and lines sideetching is tight after corrosion in corrosion process
Weight；If hydrofluoric acid ratio is too low, after the rise of nitric acid ratio, excessive nitric acid can then participate in NiCr layers of corrosion, cause localized membrane
Layer is difficult to thoroughly corrosion totally, and there are burr phenomenas for line edge.Therefore, suitable for the specific corruption of Ni layers of multilayer film circuit
It is as follows to lose formula of liquid：
Hydrofluoric acid：Nitric acid：Deionized water (volume ratio)=(0.8-1.2)：(2.5-3.5)：2.
Optimal etch recipe is：Hydrofluoric acid, nitric acid and deionized water (volume ratio)=1：3：2.
Wherein, hydrofluoric acid is 40% content (mass percent), and nitric acid is 70% content (mass percent).
After determining formula, by largely testing and determining using the correct caustic solution step under the formula such as
Under：
(1) under ventilation condition, according to above-mentioned formula rate, the deionization that hydrofluoric acid addition has been pre-metered first
In water, simultaneously because nitric acid is also easy to produce heat release after being dissolved in solution, nitric acid should be eventually adding, is slowly added on a small quantity, is stirred after addition,
It stands, cooling rear can be used.
After being etched using the corrosive liquid, it is necessary to corrosion is positioned in plastic containers and is sealed, often corrode 2-3
Batch (every batch of by 15 calculating) must replace corrosive liquid, Ni layers etch after must use substantial amounts of deionized water immediately
Surface washing is clean.
(2) the multilayer film circuit full wafer of the nickel layer to be corroded by photoresist protection is immersed to the corrosive liquid in step (1)
In corroded, forThe Ni layers of thickness, etching time 3-7 seconds, 25 DEG C -35 DEG C of corrosion temperature, corrosion
The relative motion of holding circuit and corrosive liquid in the process.
As shown in Figure 1, 2, 3, successively corroded after using photoresist protection for multilayer film circuit, such as first
Using existing corrosive liquid and caustic solution corrosion outermost layer gold, when nickel layer is eroded to, corrosive liquid of the present invention and corrosion are utilized
Method is corroded.
Embodiment 1
Corrosive liquid：Hydrofluoric acid：Nitric acid：Deionized water (volume ratio)=0.8：3.5：2, etching time 7s, corrosion temperature 25
DEG C -35 DEG C, corrode (Ta2N) the nickel layer in-NiCr-Ni-Au multilayer film circuits.
Local line edge slightly has micro black film layer particle residue after the corrosion of 40 × micro- sem observation, and lines are steep,
Film adhesion is good, film layer without warp, obscission, a delivery-check qualified rate reaches 88% after corrosion.
Embodiment 2
Etch recipe is：Hydrofluoric acid, nitric acid and deionized water (volume ratio)=1：3：2, etching time 4-5s, corrosion temperature
25℃-35℃.Corrode (Ta2N) the nickel layer in-NiCr-Ni-Au multilayer film circuits.
Lines are smooth, steep after the corrosion of 40 × micro- sem observation, and no zigzag, no metallic diaphragm inside contracts, no excessive residual
Metallic particles, film adhesion is good, film layer without warp, obscission, corrosion primary delivery-check qualified rate reaches 95%.
Embodiment 3
Hydrofluoric acid：Nitric acid：Deionized water (volume ratio)=1.2：2.5：When 2, etching time 3s, 25 DEG C -35 of corrosion temperature
DEG C, corrode (Ta2N) the nickel layer in-NiCr-Ni-Au multilayer film circuits.
Experiment finds that corrosion rate is very fast, and local line edge slightly has sideetching and shows after the corrosion of 40 × micro- sem observation
As, no excess metal film layer residual, film adhesion is good, and nothing warps, obscission,.Corrosion primary delivery-check qualified rate reaches
85%.
Unspecified part of the present invention belongs to common sense well known to those skilled in the art.
Claims (4)
1. a kind of nickel photoetching corrosion formula of liquid that suitable multilayer film circuit makes, it is characterised in that：Corrosion liquid formula is suitable for adopting
The Ni film layers obtained with magnetically controlled sputter method, including hydrofluoric acid, nitric acid and deionized water；The volume ratio of each component is as follows：
Hydrofluoric acid：Nitric acid：Deionized water=(0.8-1.2)：(2.5-3.5)：2, wherein, hydrofluoric acid is that mass percent is 40%
Hydrofluoric acid, nitric acid be mass percent be 70% nitric acid.
2. the nickel photoetching corrosion formula of liquid that a kind of suitable multilayer film circuit according to claim 1 makes, it is characterised in that：
The optimal volume ratio of hydrofluoric acid, nitric acid and deionized water is 1：3：2.
3. a kind of nickel photoetching corrosion method that suitable multilayer film circuit makes, it is characterised in that step is as follows：
(1) under ventilation condition, according to the formula rate described in claim 1, hydrofluoric acid addition is pre-metered first
Deionized water in, then add in nitric acid, stirred after addition, stand, cool down after obtain corrosive liquid；
(2) will by the corrosive liquid in multilayer film circuit full wafer immersion step (1) of nickel layer corrode of photoresist protection into
Row corrosion, forThe Ni layers of thickness, etching time 3-7 seconds, 25 DEG C -35 DEG C of corrosion temperature, corrosion process
The relative motion of middle holding circuit and corrosive liquid.
4. the nickel photoetching corrosion method that a kind of suitable multilayer film circuit according to claim 3 makes, it is characterised in that：Ni
Layer is clean by surface washing using deionized water immediately after etching.
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| JP2003147552A (en) * | 2001-08-27 | 2003-05-21 | Mitsubishi Gas Chem Co Inc | Peeling solution for nickel or nickel alloy |
| CN101597760A (en) * | 2009-06-26 | 2009-12-09 | 上海工程技术大学 | A kind of etching reagent with Ni-based braze material as solder |
| CN104419931A (en) * | 2013-08-26 | 2015-03-18 | 广州三星通信技术研究有限公司 | Etching solution |
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