CN102732252A - Novel aqua regia system ITO (indium tin oxide) etching solution and its preparation method - Google Patents
Novel aqua regia system ITO (indium tin oxide) etching solution and its preparation method Download PDFInfo
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Abstract
A novel aqua regia system ITO etching solution is characterized in that the etching solution comprises hydrochloric acid, nitric acid, pure water and additives, wherein the additives comprise a nitrate compound, a chlorine-based compound and a surfactant. A preparation method of the etching solution comprises the following steps: 1, adding a highly-acidic ion exchange resin to hydrochloric acid and nitric acid respectively, stirring to mix, filtering out the highly-acidic ion exchange resin, and controlling or removing impurity ions in the hydrochloric acid and the nitric acid; 2, weighing the hydrochloric acid, the nitric acid, the chlorine-based compound, the nitro-compound, the surfactant and the pure water according to a ratio; 3, dissolving the chlorine-based compound, the nitro-compound and the surfactant in water, and uniformly mixing the resulting solution with the nitric acid and the hydrochloric acid; and 4, letting the mixture obtained in step 3 in a filterer, and filtering to obtain the ITO etching solution. The etching solution has the advantages of stability, moderate etching efficiency, and good etching efficiency.
Description
Technical field
The chemical milling that the present invention relates to a kind of metallic substance is with compsn and preparation technology thereof, and being specifically related to be used for preparing liquid-crystal display/screen (LCD), plasma display/screen (PDP), field launcher/screen (FED), organic light emitting diode display/screen industries such as (OLED/PLED) is etching solution and preparation method as the etched novel chloroazotic acid of panel process indium tin oxide layer.
Background technology
It is low that indium tin oxide (ITO) conducting film has resistivity; Light transmission is good; High-temperature stability reaches preparation well and plurality of advantages such as the figure complete processing is simple, is a kind of ideal transparent electrode material, is widely used on the flat-panel monitors such as LCD, PDP, FED, OLED/PLED as transparency electrode.
For preparing needed electrode pattern, will carry out etching to the ITO conducting film.Etching is that material is used chemical reaction or physical shock effect and the technology that removes.Etching technique is divided into wet etching and dry etching, and wherein, wet etching is to adopt chemical reagent, reaches etched purpose via chemical reaction.Novel chloroazotic acid is an etching solution; Be colourless transparent liquid; Scent of is acid; In the prior art; Mainly made through the stirring and evenly mixing filtration by hydrochloric acid, nitric acid, additive and pure water, above-mentioned etching solution has been widely used in thin film field-effect liquid-crystal display/screen (LCD), plasma display/screen (PDP), field launcher/screen (FED), organic light emitting diode display/screen industries such as (OLED/PLED) as in indium tin oxide transparent conductive semiconductor film (ITO) etching in the panel process.But in reagent etching ITO materials process, general chloroazotic acid is the etch quantity that the ITO etching solution often is difficult to control etching angle and metal level on the market, and etching solution is unstable, but influence is the repeatability of effect.
In recent years; People are to the ever-increasing while of the demand of liquid-crystal display; Quality and picture precision to product are also had higher requirement, and etched effect can directly cause the quality of circuit board manufacturing process, influences the precision and the quality of high-density thin wire image.If will satisfy the requirements at the higher level of people to the precision of images and quality proposition, those skilled in the art make further improvement with regard to being necessary to the correlation technique of existing ITO etching solution.
Summary of the invention
One of the object of the invention is to overcome the deficiency in the existing ITO conductive film etching solution technology; Design a kind of high-quality, ITO etching solution cheaply; The etching solution of this prescription is stable, and etching efficiency is moderate, and etching efficiency is good; And the etching solution formula material is cheap and easy to get, thereby can effectively improve the yield of ITO conductive film.
Second purpose of the present invention is to overcome the deficiency among the existing ITO etching solution preparation technology, designs a kind of succinct, rational ITO etching solution preparation technology.
For realizing above-mentioned purpose; Technical scheme of the present invention is that a kind of novel chloroazotic acid of design is the ITO etchant; It is characterized in that said this etchant comprises hydrochloric acid, nitric acid, pure water and additive, wherein additive comprises nitrate compound, chlorine-based compound and tensio-active agent.
Wherein, said chlorine-based compound is the compound that can dissociate into cl ions.
At this; Etchant can comprise the hydrochloric acid of 10 to 30 wt %, the nitric acid of 0.5 to 10 wt %, the chlorine-based compound of 0.05 to 5 wt %; 0.05 nitro-compound to 5 wt %; This etching solution also contains tensio-active agent, is benchmark with the gross weight of etching solution, content 0.1% to the 10 wt % of said ionic surface active agent.
According to the present invention, said etching solution is the aqueous solution that contains hydrochloric acid, nitric acid, additive, wherein, contains tensio-active agent in this etching solution.
Said tensio-active agent can be conventional various tensio-active agents.The present invention is preferably AS and polyoxyethylene-type nonionogenic tenside; Said AS for example can be in X 2073, Witco 1298 Soft Acid, sodium alkyl sulfate, fatty alcohol sulphuric acid, sodium lauryl sulphate, the dodecyl sulphate one or several.Said polyoxyethylene-type nonionogenic tenside, for example one or several of AEO, TX10, polyoxyethylene carboxylate, polyoxyethylate amide, polyoxyethylene fatty amine, polyoxyethylene sorbitan monocarboxylate.Said AS further is preferably X 2073 and/or Witco 1298 Soft Acid, and the polyoxyethylene-type nonionogenic tenside further is preferably AEO and/or TX10.With etched total amount is benchmark, and the content of said tensio-active agent is 0.1% to 5 wt %, is preferably 0.1% to 3wt %.
Among the present invention; The weight percent of every kind of raw material is respectively in said six kinds of raw materials: the weight percent of every kind of raw material is respectively in said six kinds of raw materials: hydrochloric acid 10 to 30 wt %, nitric acid 0.5 to 10 wt %, nitro-compound 0.05 to 5 wt %, chlorine-based compound 0.05 to 5 wt %, pure water 60% to 89 wt %; After the purity of raw material changed, its proportioning should give adjustment.
Among the present invention, said hydrochloric acid, concentration of nitric acid are respectively: nitric acid 61.5%.Hydrochloric acid 38%.
Among the present invention, granularity is no more than 100 greater than the particle of 0.3 μ m in the said etching solution, and the impurity negatively charged ion is no more than 30ppb, and impurity cationic is no more than 0.05ppb.
Technical scheme of the present invention also comprises the preparation technology who designs a kind of ITO etching solution, it is characterized in that, said preparation technology comprises following procedure of processing:
The first step: strong-acid ion exchange resin is joined respectively in hydrochloric acid and the nitric acid, mix, leach strong-acid ion exchange resin then, the foreign ion in control or removal hydrochloric acid and the nitric acid;
Second step: with the configuration of weighing of hydrochloric acid, nitric acid, chlorine-based compound, nitro-compound, tensio-active agent, six kinds of proportioning raw materials of pure water;
The 3rd the step: with chlorine-based compound, nitro-compound, surfactant dissolves in water; Evenly get final product with nitric acid and mixed in hydrochloric acid again; Because will emit big calorimetric during the concentrated nitric acid dilution, therefore, preferably nitric acid slowly joined in the aqueous solution that contains tensio-active agent.
The 4th goes on foot: mixture is fed in the strainer filter, obtain said ITO etching solution.
Wherein, affiliated strongly acidic cationic exchange resin is a strongly acidic styrene type cation exchange resin.
Wherein, said strong-acid ion exchange resin mixes stirring with said hydrochloric acid and nitric acid be under the state of normal temperature and pressure, to carry out, and the speed of stirring is 65 ~ 85 rev/mins, and the mass ratio of resin and hydrochloric acid or nitric acid is 0.2 ~ 0.3, and churning time is 10 minutes.
Wherein, said nitrate compound is a saltpetre, and said saltpetre purity is higher than 99.5%; Chlorine-based compound is a Repone K, and said Repone K purity is higher than 99.5%.
Wherein, said filtering number of times is greater than twice, and the microfiltration membrane aperture of said strainer is 0.03~0.10 μ m.。
Wherein, said filtration granularity in air is no more than greater than the particle of 0.5 μ m in hundred grades of environment purifications of 100 and carries out.
Wherein, said stirring is mechanical stirring or magnetic agitation.
Wherein, said stirring is under normal temperature, non-pressurized state, to carry out with mixing, and the time of said stirring is 3 ~ 4 hours, and the speed of stirring is 60 ~ 85 rev/mins.
Advantage of the present invention and beneficial effect are: because in the present invention, on the basis of the ITO etching solution that existing hydrochloric acid, nitric acid mix, add additive and tensio-active agent; Preparation technology through the etching solution of ITO described in the present invention mixes the etching solution that forms again, carves the liquid phase ratio with existing ITO, and not only ITO metal level etch-rate is moderate; Stable reaction; Noresidue, and can make the photoresist material of metal level top can break away from the ITO metal level slightly, make etching solution get into the photoresist material bottom easily; The ITO metal level is formed etching; Thereby the etching angle that makes formation does not have side etching phenomenon basically, and client device and personnel is not all had influence between 40 ~ 60 degree.Therefore, adopt etching solution provided by the invention and engraving method can obviously reduce the generation of side etching phenomenon.
Description of drawings
Fig. 1 is the product enlarged view after the 1 etching solution etching of the use embodiment of the invention.
Fig. 2 is the product enlarged view after the etching solution etching for commercially available common chloroazotic acid.
Fig. 3 is the product etching angle Electronic Speculum figure after the 1 etching solution etching of the use embodiment of the invention.
Embodiment
Below in conjunction with embodiment, specific embodiments of the invention further describes.Following examples only are used for technical scheme of the present invention more clearly is described, and can not limit protection scope of the present invention with this.
Embodiment 1
The present invention is that a kind of novel chloroazotic acid is the ITO etching solution, and this ITO etching solution is evenly formed by six kinds of raw materials mix such as hydrochloric acid, nitric acid, Repone K, saltpetre, tensio-active agent and pure water.
Wherein, the weight percent of raw material can be respectively in said six: 10 wt % hydrochloric acid, nitric acid 1wt %, saltpetre 0.1 wt %, Repone K 0.1wt %, X 2073 0.2wt %, and all the other are pure water; After the purity of raw material changed, its proportioning should give adjustment.Said hydrochloric acid, concentration of nitric acid are respectively: nitric acid 61.5%.Hydrochloric acid 38%; Said saltpetre purity is higher than 99.5%, and Repone K purity is higher than 99.5%.Said Repone K, all the other impurity components in the saltpetre raw material are the impurity that sodium-chlor, moisture and denier are insoluble to said etching liquid.
Wherein, granularity is no more than 100 greater than the particle of 0.3 μ m in the said etching solution, and the impurity negatively charged ion is no more than 30ppb, and impurity cationic is no more than 0.05ppb.
With above-mentioned chloroazotic acid is that the ITO etching solution is an example, and its step of preparation process is following:
The first step: strong-acid ion exchange resin is joined respectively in hydrochloric acid and the nitric acid, mix, leach strong-acid ion exchange resin then, the foreign ion in control or removal hydrochloric acid and the nitric acid;
Second step: with hydrochloric acid, nitric acid, chlorine-based compound, nitro-compound, tensio-active agent, six kinds of raw materials of pure water by the configuration of weighing of the said proportioning of claim 1;
The 3rd the step: with chlorine-based compound, nitro-compound, surfactant dissolves in water; Evenly get final product with nitric acid and mixed in hydrochloric acid again; Because will emit big calorimetric during the concentrated nitric acid dilution, therefore, preferably nitric acid slowly joined in the aqueous solution that contains tensio-active agent.
The 4th goes on foot: mixture is fed in the strainer filter, obtain said ITO etching solution.
In above-mentioned process step, said strongly acidic cationic exchange resin is a strongly acidic styrene type cation exchange resin.
In above-mentioned process step; Said strong-acid ion exchange resin mixes stirring with said hydrochloric acid and nitric acid be under the state of normal temperature and pressure, to carry out; The speed that stirs is 65 ~ 85 rev/mins, and the mass ratio of resin and hydrochloric acid or nitric acid is 0.25, and churning time is 10 minutes.
In above-mentioned process step, said filtering number of times is greater than twice, and the microfiltration membrane aperture of said strainer is 0.03~0.10 μ m.。
In the etching liquid hybrid technique, said filtration is carried out in granularity in every cubic metres of air is no more than hundred grades of environment purifications of 100 greater than the particle of 0.5 μ m.
Said stirring in the etching liquid technological process is mechanical stirring or magnetic agitation.
Said stirring in ITO etching solution mixing process is under normal temperature, non-pressurized state, to carry out with mixing, and the time of said stirring is 1.5 ~ 3 hours, and the speed of stirring is 60 ~ 85 rev/mins.
The ITO etching solution that embodiment 1 prepares is used for etching products; Its appearance is seen Fig. 1; Compare with the effect (see figure 2) of product after commercially available common chloroazotic acid is the etching solution etching; As can be seen from the figure, the residual commercial like product that obviously is less than of etching products of the present invention, promptly its etch effect obviously is superior to the commercially available prod.
The ITO etching solution that embodiment 1 prepares is used for etching products, and the etching angle is seen Fig. 3, as can beappreciated from fig. 3, and 43.3 ° of the etched product etching angles of present embodiment etching solution, and do not have side etching phenomenon basically.
Embodiment 2
The present invention is that a kind of novel chloroazotic acid is the ITO etching solution, and this ITO etching solution is evenly formed by six kinds of raw materials mix such as hydrochloric acid, nitric acid, Repone K, saltpetre, tensio-active agent and pure water.
Wherein, the weight percent of raw material can be respectively in said six: 30wt % hydrochloric acid, nitric acid 10wt %, saltpetre 5 wt %, Repone K 5wt %, TX10 3wt %, and all the other are pure water; After the purity of raw material changed, its proportioning should give adjustment.Said hydrochloric acid, concentration of nitric acid are respectively: nitric acid 61.5%.Hydrochloric acid 38%; Said saltpetre purity is higher than 99.5%, and Repone K purity is higher than 99.5%.Said Repone K, all the other impurity components in the saltpetre raw material are the impurity that sodium-chlor, moisture and denier are insoluble to said etching liquid.
Wherein, granularity is no more than 100 greater than the particle of 0.3 μ m in the said etching solution, and the impurity negatively charged ion is no more than 30ppb, and impurity cationic is no more than 0.05ppb.
With above-mentioned chloroazotic acid is that the ITO etching solution is an example, and its step of preparation process is following:
The first step: strong-acid ion exchange resin is joined respectively in hydrochloric acid and the nitric acid, mix, leach strong-acid ion exchange resin then, the foreign ion in control or removal hydrochloric acid and the nitric acid;
Second step: with hydrochloric acid, nitric acid, chlorine-based compound, nitro-compound, tensio-active agent, six kinds of raw materials of pure water by the configuration of weighing of the said proportioning of claim 1;
The 3rd the step: with chlorine-based compound, nitro-compound, surfactant dissolves in water; Evenly get final product with nitric acid and mixed in hydrochloric acid again; Because will emit big calorimetric during the concentrated nitric acid dilution, therefore, preferably nitric acid slowly joined in the aqueous solution that contains the tensio-active agent TX10.
The 4th goes on foot: mixture is fed in the strainer filter, obtain said ITO etching solution.
In above-mentioned process step, said strongly acidic cationic exchange resin is a strongly acidic styrene type cation exchange resin.
Remaining processing condition and process step and embodiment 1 are identical.
Embodiment 3
The present invention is that a kind of novel chloroazotic acid is the ITO etching solution, and this ITO etching solution is evenly formed by six kinds of raw materials mix such as hydrochloric acid, nitric acid, Repone K, saltpetre, tensio-active agent and pure water.
Wherein, the weight percent of raw material can be respectively in said six: 25wt % hydrochloric acid, nitric acid 8wt %, saltpetre 3 wt %, Repone K 3wt %, Witco 1298 Soft Acid 2wt %, and all the other are pure water; After the purity of raw material changed, its proportioning should give adjustment.Said hydrochloric acid, concentration of nitric acid are respectively: nitric acid 61.5%.Hydrochloric acid 38%; Said saltpetre purity is higher than 99.5%, and Repone K purity is higher than 99.5%.Said Repone K, all the other impurity components in the saltpetre raw material are the impurity that sodium-chlor, moisture and denier are insoluble to said etching liquid.
Wherein, granularity is no more than 100 greater than the particle of 0.3 μ m in the said etching solution, and the impurity negatively charged ion is no more than 30ppb, and impurity cationic is no more than 0.05ppb.
With above-mentioned chloroazotic acid is that the ITO etching solution is an example, and its step of preparation process is following:
The first step: strong-acid ion exchange resin is joined respectively in hydrochloric acid and the nitric acid, mix, leach strong-acid ion exchange resin then, the foreign ion in control or removal hydrochloric acid and the nitric acid;
Second step: with hydrochloric acid, nitric acid, chlorine-based compound, nitro-compound, tensio-active agent, six kinds of raw materials of pure water by the configuration of weighing of the said proportioning of claim 1;
The 3rd the step: with chlorine-based compound, nitro-compound, surfactant dissolves in water; Evenly get final product with nitric acid and mixed in hydrochloric acid again; Because will emit big calorimetric during the concentrated nitric acid dilution, therefore, preferably nitric acid slowly joined in the aqueous solution that contains Witco 1298 Soft Acid.
The 4th goes on foot: mixture is fed in the strainer filter, obtain said ITO etching solution.
In above-mentioned process step, said strongly acidic cationic exchange resin is a strongly acidic styrene type cation exchange resin.
Remaining processing condition and process step and embodiment 1 are identical.
Through above-mentioned technology mainly is that the chloroazotic acid that rectification process is processed is the ITO etching solution, and its physical and chemical performance index can be controlled in:
Concentration is 38% hydrochloric acid, premium grads, and its index is following:
1.1 physical property
Characteristic | Be controlled to be |
Content (%) | 38 |
Particle (>=0.5um, individual/ml) | ≤100 |
Colourity (Hazen), | ≤10 |
Ignition residue (in SO4); PPm | ≤3 |
Free chlorine (Cl2); PPm | ≤0.5 |
Ammonium salt (NH4); PPm | ≤2 |
Phosphoric acid salt (PO4); PPm | ≤0.05 |
Vitriol (SO4); PPm | ≤0.3 |
Sulphite (SO3); PPm | ≤1 |
1.2 trace impurity content
Impurity ppb max | Q/320281-A-15 |
Aluminium (Al) | ≤0.01 |
Arsenic (As) | ≤0.01 |
Silver (Ag) | ≤0.01 |
Gold (Au) | ≤0.01 |
Barium (Ba) | ≤0.01 |
Bismuth (Bi) | ≤0.01 |
Boron (B) | ≤0.01 |
Calcium (Ca) | ≤0.01 |
Cadmium (Cd) | ≤0.01 |
Cobalt (Co) | ≤0.01 |
Chromium (Cr) | ≤0.01 |
Copper (Cu) | ≤0.01 |
Gallium (Ga) | ≤0.01 |
Germanium (Ge) | ≤0.01 |
Iron (Fe) | ≤0.01 |
Potassium (K) | ≤0.01 |
Lithium (Li) | ≤0.01 |
Magnesium (Mg) | ≤0.01 |
Manganese (Mn) | ≤0.01 |
Molybdenum (Mo) | ≤0.01 |
Sodium (Na) | ≤0.01 |
Nickel (Ni) | ≤0.01 |
Plumbous (Pb) | ≤0.01 |
Silicon (Si) | ≤0.01 |
Strontium (Sr) | ≤0.01 |
Tin (Sn) | ≤0.01 |
Titanium (Ti) | ≤0.01 |
Zinc (Zn) | ≤0.01 |
When concentration of nitric acid be 61.5% the time, its physical and chemical performance index is following:
1.1 physical property
Characteristic | Q/320281-A-10 |
Nitric acid wt% | 61.5 |
Colourity (Hazen) | ≤5 |
Cl (ppm) | ≤0.5 |
PO4 (ppm) | ≤0.5 |
SO4 (ppm) | ≤0.5 |
Particle>0.1um (individual/ml) | ≤250 |
Particle>0.2um (individual/ml) | ≤50 |
1.2 trace impurity
Impurity ppm max | Q/320281-A-22 |
Aluminium | ≤0.01 |
Silver | ≤0.01 |
Arsenic | ≤0.01 |
Barium | ≤0.01 |
Beryllium | ≤0.01 |
Cadmium | ≤0.01 |
Cobalt | ≤0.01 |
Chromium | ≤0.01 |
Copper | ≤0.01 |
Iron | ≤0.01 |
Gallium | ≤0.01 |
Potassium | ≤0.01 |
Lithium | ≤0.01 |
Magnesium | ≤0.01 |
Manganese | ≤0.01 |
Sodium | ≤0.01 |
Nickel | ≤0.01 |
Plumbous | ≤0.01 |
Strontium | ≤0.01 |
Titanium | ≤0.01 |
Vanadium | ≤0.01 |
Zinc | ≤0.01 |
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from know-why of the present invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (10)
1. a novel chloroazotic acid is the ITO etching solution, it is characterized in that: said this etchant comprises hydrochloric acid, nitric acid, pure water and additive, and wherein additive comprises nitrate compound, chlorine-based compound and tensio-active agent.
2. a kind of novel chloroazotic acid according to claim 1 is the ITO etching solution, it is characterized in that: each material mass proportioning is following in the said component:
Hydrochloric acid 10 to 30 wt %, nitric acid 0.5 to 10 wt %, nitro-compound 0.05 to 5 wt %, chlorine-based compound 0.05 to 5 wt %, tensio-active agent 0.1-10 wt %; Surplus is a pure water;
Said hydrochloric acid, concentration of nitric acid are respectively: nitric acid 61.5%, hydrochloric acid 38%.
3. be the ITO etching solution according to the described a kind of novel chloroazotic acid of one of claim 1-2, it is characterized in that: said tensio-active agent is AS or polyoxyethylene-type nonionogenic tenside.
4. a kind of novel chloroazotic acid according to claim 3 is the ITO etching solution, it is characterized in that: said AS is one or several in X 2073, Witco 1298 Soft Acid, sodium alkyl sulfate, fatty alcohol sulphuric acid, sodium lauryl sulphate, the dodecyl sulphate;
Said polyoxyethylene-type nonionogenic tenside is one or several of AEO, TX10, polyoxyethylene carboxylate, polyoxyethylate amide, polyoxyethylene fatty amine, polyoxyethylene sorbitan monocarboxylate.
5. a kind of novel chloroazotic acid according to claim 2 is the ITO etching solution, it is characterized in that: the content of said tensio-active agent is 0.1% to 3wt %.
6. a kind of novel chloroazotic acid according to claim 1 is the ITO etching solution, it is characterized in that: said chlorine-based compound is the compound that can dissociate into cl ions.
7. a kind of novel chloroazotic acid according to claim 1 is the ITO etching solution, it is characterized in that: said nitrate compound is a saltpetre, and said saltpetre purity is higher than 99.5%; Chlorine-based compound is a Repone K, and said Repone K purity is higher than 99.5%.
8. the method that to prepare the described a kind of novel chloroazotic acid of one of claim 1-7 be the ITO etching solution, it is characterized in that: said preparation technology comprises following procedure of processing:
The first step: strong-acid ion exchange resin is joined respectively in hydrochloric acid and the nitric acid, mix, leach strong-acid ion exchange resin then, the foreign ion in control or removal hydrochloric acid and the nitric acid;
Second step: with hydrochloric acid, nitric acid, chlorine-based compound, nitro-compound, tensio-active agent, six kinds of raw materials of pure water by the proportioning configuration of weighing;
The 3rd step: chlorine-based compound, nitro-compound, surfactant dissolves in water, are evenly got final product with nitric acid and mixed in hydrochloric acid again, preferably nitric acid is slowly joined in the aqueous solution that contains tensio-active agent;
The 4th goes on foot: mixture is fed in the strainer filter, obtain said ITO etching solution.
9. the preparation method that a kind of novel chloroazotic acid according to claim 8 is the ITO etching solution; It is characterized in that: said strong-acid ion exchange resin mixes stirring with said hydrochloric acid and nitric acid be under the state of normal temperature and pressure, to carry out; The speed that stirs is 65 ~ 85 rev/mins; The mass ratio of resin and hydrochloric acid or nitric acid is 0.2 ~ 0.3, and churning time is 10 minutes.
10. the preparation method that a kind of novel chloroazotic acid according to claim 9 is the ITO etching solution is characterized in that: said strongly acidic cationic exchange resin is a strongly acidic styrene type cation exchange resin.
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