KR101425855B1 - Electroconductive ink composite including metal-organic precursor and method for Forming the metal line using the same - Google Patents
Electroconductive ink composite including metal-organic precursor and method for Forming the metal line using the same Download PDFInfo
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- KR101425855B1 KR101425855B1 KR1020130018523A KR20130018523A KR101425855B1 KR 101425855 B1 KR101425855 B1 KR 101425855B1 KR 1020130018523 A KR1020130018523 A KR 1020130018523A KR 20130018523 A KR20130018523 A KR 20130018523A KR 101425855 B1 KR101425855 B1 KR 101425855B1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Abstract
Description
TECHNICAL FIELD The present invention relates to a conductive ink composition and a method of forming a metal wiring using the conductive ink composition, and more particularly, to a conductive ink composition including a metal organic precursor that does not include particles and a method of forming a metal wiring using the conductive ink composition.
Metal wirings are used to electrically connect individual elements in a semiconductor device. As a conventional method of forming a metal wiring, a method using photolithography is widely used. However, the method of forming metal lines by photolithography involves complicated process steps and high manufacturing costs because expensive process equipment must be used. On the other hand, forming a metal pattern by printing conductive ink does not require a simple and expensive equipment, so it is possible to reduce the manufacturing cost of a product, and thus interest is increasing as a substitute for photolithography.
Nanoparticle inks are widely known in which metal is made into nanoscale and dispersed in a solvent by a method used to make conductive inks. However, when the ink is prepared with nanoparticles, the aggregation of the particles themselves can not be completely prevented, so that long-term preservation is difficult. In addition, transition metal nanoparticles other than noble metals are very vulnerable to oxidation, so that metal oxides are contained in the conductive ink, which causes the conductivity of the ink to deteriorate.
As a particle synthesis method for nanoparticle ink, a wet process is widely used. In the case of nanoparticle synthesis using a wet process, a cleaning process using a centrifuge or the like is performed in order to remove various chemicals and solvents used and recover only pure nanoparticle powders It is essential. This is the biggest obstacle to the mass production of nanoparticles.
In addition, organic substances such as surfactants and polymers are added to the nanoparticles in order to control particle size and prevent cohesion, which increases the manufacturing cost of the ink.
Conductive inks that do not contain particles have been proposed as an alternative to the problems of these nanoparticles. However, the development of conductive ink has been studied mostly for silver which has high standard reduction potential and excellent stability against oxidation, and which is relatively easy to develop. At present, it is urgent to develop a conductive ink using a dislocation metal rather than a conductive ink using silver because of an increase in price. As an alternative thereto, Korean Patent Laid-Open No. 10-2010-0066810 discloses an example in which copper flake is mixed with silver nanoparticles to improve resistivity and product unit cost. When the copper flake is used in the composition as described above, the resistivity and the unit cost can be reduced, which is relatively lower than that of a common metal. However, due to the characteristics of copper, it is easily oxidized and the resistivity is deteriorated due to the oxidation and oxidation of the ink composition, so that there is a limit to apply to a product requiring high quality and low non-resistance.
In addition, after metal wiring using a conductive ink composition is generally performed, firing is performed at high temperature to improve the resistivity characteristic. In the case of a conductive composition containing copper in this process, the resistivity characteristics are rather deteriorated due to the oxidation of copper. To prevent such a process, a change in the high-temperature firing process is inevitable.
Although studies on metal conductive inks that do not include the metal particles have been reported, most of them have an affinity with an organic solvent, and some have a disadvantage that a reducing agent such as a hydrogen gas is required to reduce the ink to a metal . Therefore, there is a demand for development of a technique capable of satisfying the storage stability of the composition, good printability and resistivity characteristics, and lowering the unit cost of the product.
An object of the present invention is to provide a metal nano-particle ink which is easy to be dispersed in a polar solvent and which can be easily dispersed, and which can overcome the limitations such as dispersion stability, To provide an ink composition.
A second object of the present invention is to provide a method of forming a metal wiring having a high conductivity by using a conductive ink composition comprising a metal organic precursor having an excellent dispersing ability in a polar solvent such as an alcohol or a polyol.
In order to accomplish one object of the present invention, a conductive ink composition according to embodiments of the present invention comprises 5.0 to 90% by weight of a metal organic precursor having a structure in which a metal-formate is complexed with an alkanolamine ligand, And an extra dispersion solution containing a solvent as a main component.
According to one embodiment, the metal organic precursor may be prepared by mixing a metal-formate with a liquid alkanolamine and a step of complexing the metal-formate with an alkanolamine as a ligand to form a liquid metal organic precursor And drying the liquid metal organic precursor.
According to one embodiment, the alkanolamine may use an organic compound having hydroxy and amino functional groups in the alkanabine. The alkanolamine may be selected from the group consisting of N-methylethanolamine, N-ethylethanolamine, N-propylethanolamine, N-butylethanolamine, diethanolamine, triethanolamine, N-methyldiethanolamine, Diisopropanolamine, triisopropanolamine, N-methylisopropanolamine, N-ethylisopropanolamine, N-propylisopropanolamine, 2-aminopropane-1-ol, N-methyl- Ol, N-methyl-1-aminopropane-3-ol, N-ethyl-1-aminopropane- 2-ol, N-methyl-1-aminobutan-2-ol, N-ethyl-1-aminobutan- 1-ol, N-methyl-3-aminobutan-1-ol, N-ethyl-3-aminobutane- 1-aminobutan-4-ol, N-methyl-1-aminobutan-4-ol, N-ethyl- 2-methylpropan-1-ol, 2-amino-4-methylpentan-1-ol, 2-aminohexane- Ol, 1-aminopropane-2,3-diol, 2-aminopropane-1-ol, 3-diol, tris (oxymethyl) aminomethane, 1,2-diaminopropane-3-ol, 1,3-diaminopropane- have.
According to one embodiment, the alkanolamine may be mixed in an equivalent ratio of 1.5 to 2.5 times the metal to be applied to the metal-formate.
According to one embodiment, the metal organic precursor is a metal-formate compound having an alkanolamine as a ligand, and the metal may be any one selected from the group consisting of copper, nickel, cobalt, and tin .
According to one embodiment, polar organic solvents such as alcohols, glycols and polyols may be used as the extra dispersion solution.
According to one embodiment, it may further comprise 1 to 20 wt% of a binder based on the total metal content.
According to another aspect of the present invention, there is provided a method of forming a metal line using a conductive ink composition, comprising: (a) providing a metal organic precursor containing a metal-formate compound having alkanolamine as a ligand in an amount of 5.0 to 90 wt% % And an extra dispersion solution on a surface of a substrate on which a metal wiring is to be formed, and drying the conductive ink composition printed on the substrate.
According to an embodiment, the substrate may be a printed circuit board, a semiconductor substrate, a plastic substrate, a wafer, or the like.
According to one embodiment, the metal wiring may be formed by reducing the metal organic precursor in the conductive ink composition to a metal film when the metal organic precursor is heat-treated and dried in a nitrogen atmosphere.
Since the conductive ink composition comprising the metal organic precursor according to the embodiments of the present invention is manufactured using a metal organic precursor which is easily dispersed in a polar solvent such as alcohol or polyol without containing particles, And has high dispersion stability compared to the electroconductive ink containing metal nanoparticles.
Further, since the metal organic precursor is used, the conductive ink composition of the present invention is easy to mass-produce by a simple synthesis method and is excellent in a solvent having polarity such as alcohol or polyol. Since it has high solubility in solvents such as alcohols and polyols, it shows excellent performance in the printing process using PDMS (Polydimethylsiloxane). In addition, since the metal organic precursor has a structure in which alkanolamine is complexed with a ligand in a salt of a metal formate, alkanolamine acts as a secondary reducing agent to assist reduction of the metal formate, so that a separate reducing agent is not required Do not. This results in lowering the thermal decomposition temperature of the metal formate, so that it is possible to perform the printing firing to form metal wiring at a relatively low temperature. However, the effects of the present invention are not limited thereto, and various modifications may be made without departing from the spirit and scope of the present invention.
1 is a graph showing a TGA analysis result of a conductive ink prepared according to Example 1 of the present invention.
2 is a photograph showing a conductive ink applied to Example 2 of the present invention.
3 is a graph showing the results of XRD analysis of a copper metal wiring according to Example 2 of the present invention.
Hereinafter, a conductive ink composition according to an embodiment of the present invention and a method of forming a metal wiring using the conductive ink composition will be described in detail. While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are further described in the text. It should be understood, however, that the invention is not intended to be limited to the particular forms disclosed, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention. The terms first, second, etc. may be used to describe various components, but the components should not be limited by the terms. The terms are used only for the purpose of distinguishing one component from another. For example, without departing from the scope of the present invention, the first component may be referred to as a second component, and similarly, the second component may also be referred to as a first component.
The terminology used in this application is used only to describe a specific embodiment and is not intended to limit the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In this application, the terms "comprises", "having", and the like are used to specify that a feature, a number, a step, an operation, an element, a part or a combination thereof is described in the specification, But do not preclude the presence or addition of one or more other features, integers, steps, operations, components, parts, or combinations thereof.
On the other hand, unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the contextual meaning of the related art and are to be interpreted as either ideal or overly formal in the sense of the present application Do not.
Conductive ink composition
The conductive ink composition according to the present invention mainly comprises a metal organic precursor and a dispersion solution used for dispersing the metal organic precursor in an ink state. Preferably from 5 to 90% by weight of a metal organic precursor having an aldoloamine as a ligand and an extra dispersion solvent comprising a polar solvent. In this embodiment, the amount of the metal organic precursor or the dispersing solvent may vary greatly depending on the viscosity of the ink and the printing method of the ink.
As an example, the metal organic precursor applied to the conductive ink composition to which the present invention is applied is a metal-formate compound having an alkanolamine as a ligand, and can be prepared by performing the following steps.
In order to prepare a metal-formate compound having an alkanolamine as a ligand that is a metal organic precursor, an alkanolamine is added and mixed in a metal formate as a first step. As an example, the mixing of the metal formate and the alkanolamine may be carried out by mechanical stirring such as ultrasonic or ball milling.
In a second step, the metal-formate is then complexed with the alkanolamine as a ligand to form a liquid metal-organic precursor. The metal organic precursor is a metal-formate compound having an alkanolamine as a ligand, and the metal may include any one transition metal selected from the group consisting of copper, nickel, cobalt, and tin.
The metal formate used to form the metal organic precursor is reduced to metal as shown in Reaction Equation 1 and Reaction Scheme 2 shown below to generate volatile CO2, CO, and H2O as decomposition products. However, these metal formates have been known to be unsuitable for use in the production of conductive inks because they are soluble only in water and are insoluble in most other solvents.
M (HCOO) 2 - > M + CO + CO2 + H2O -
M (HCOO) 2 - > M + 2CO2 + H2 - (Scheme 2)
(In the above Schemes 1 and 2, M is a dislocation metal and may be copper, nickel, cobalt or tin.
To solve this problem, in the present invention, alkanolamine is complexed with a ligand to convert a solid metal-formate into a liquid metal-organic precursor. In particular, since the alkanolamine is applied as a ligand, the metal organic precursor can have solubility in the polar organic solvent, making it usable in the production of conductive ink.
In the present invention, the use of the alkanolamine for converting the metal formate into the metal organic precursor allows easy formation of coordination bonds with the metal ion in the amino group contained in the alkanolamine, so that the solid metal- And is easily dispersed in polar solvents such as alcohols and polyols which are polarized by hydroxy groups not participating in coordination bond after coordination bond. Further, in addition to the reaction of the metal organic precursor to thermal oxidation of the amino group to imine and nitrile upon thermal decomposition, the oxidation reaction of the primary alcohol included in the alkanolamine to the aldehyde, carboxylic acid and carbon dioxide is added to help reduce the metal ion You can do it together.
As an example, the alkanolamine refers to an organic compound having hydroxy and amino functional groups in the alkane succinic acid. Specific examples of alkanolamide that can be used in the present invention include N-methylethanolamine, N-ethylethanolamine, N-propylethanolamine, N-butylethanolamine, diethanolamine, triethanolamine, Diisopropanolamine, N-methylisopropanolamine, N-ethylisopropanolamine, N-propylisopropanolamine, 2-aminopropane-1-ol, N- 1-ol, N-methyl-1-aminopropane-3-ol, N-ethyl- 1-aminobutane-2-ol, N-ethyl-1-aminobutan-2-ol, 2-aminobutane- Ol, N-methyl-2-aminobutan-1-ol, N-ethyl- , N-ethyl-3-aminobutan-1-ol, 1-aminobutan- Amino-2-methylpropan-2-ol, 2-amino-2-methylpropan-1-ol, 1-aminopentane Ol, 2-amino-4-methylpentan-1-ol, 2-aminohexan-1-ol, 3- 1,3-diol, tris (oxymethyl) aminomethane, 1,2-diaminopropan-3-ol, 1,3- 2-ol, 2- (2-aminoethoxy) ethanol and the like. They may be used alone or in combination of two or more.
The amount of the alkanolamine to be mixed with the metal-formate is preferably used in consideration of the coordination number of the metal ion. As an example, the amount of alkanolamine to be mixed with the metal-formate can be mixed in an equivalent ratio of 1.5 to 2.5 times of the applied metal.
For example, copper has six coordinateable sites. In the case of copper formate, one formate molecule is bonded to the copper atom in a bidentate form to occupy two coordination sites. Since the copper formate has two formates, in this case, it is preferable to add two equivalents of the alkanolamine to the metal, since there are two possible coordination sites on the copper metal atom.
Next, as the third step, the liquid metal organic precursor obtained in the second step is dried.
In the third step, the drying step is performed to remove water through a vacuum oven when the metal film applied to form the metal organic precursor is a hydrate. In this process, it is also possible to remove the alkanolamine which has not coordinated with the metal formate. In addition, when the solvent is used in the synthesis, the step of removing the solvent is included.
The dispersion solvent to be used for forming the conductive ink composition of the present invention may contain a polar organic solvent as a main component. Examples of these solvents include alcohols, glycols, polyols and the like, which may be used alone or in admixture of two or more. In this embodiment, the amount of the dispersion solvent containing a polar organic solvent as a main component may vary greatly depending on the viscosity of the ink and the printing method of the ink.
The dispersion solution of the present invention is used for the purpose of dissolving a metal organic precursor and adjusting the viscosity of the ink in the preparation of the ink composition to form an ink according to a desired printing technique. The dispersion solution is used as a binder (adhesive) But also for dispersing the additive. In addition, it is possible to selectively use a solvent suitable for use in PDMS due to the characteristics of the present invention having considerable affinity to alcohol, polyol, and the like.
In a conductive ink composition according to one embodiment, the conductive ink composition may further comprise 1 to 20% by weight of a binder. As an example, the binder may be used in an amount of 1 to 20 wt% based on the metal content of the organometallic precursor used. The binder improves the adhesion of the metal and acts on the surface of the metal to form a coating film when the metal of the conductive ink is printed on the target to form the metal wiring. It also plays an important role in improving the printability in accordance with selective use because it imparts the rheological characteristics of the ink.
However, the use of excessive binder resin is a cause of inhibiting the resistivity property, so use caution is necessary. Can be used to improve adhesion. Examples of the binder may include PDMS (Polydimethylsiloxane), a polymer containing an acrylic group, a copolymer containing an acryl group, a polymer containing a urethane group, a copolymer containing a urethane group, and a mixture thereof.
If the content of the binder exceeds 20% by weight, the viscosity may increase and the resistivity characteristic may be poor after the metal wiring printing. Therefore, when the binder is used, the content of the binder is in the range of 1 to 20% by weight, more preferably in the range of 3 to 10% by weight.
As another example, depending on the nature of the ink composition, the binder resin may not be used depending on the use of the solvent.
The conductive ink composition may further include an optional additive component. Surfactants, viscosity modifiers, pH adjusting agents, antioxidants, conductivity modifiers, and the like.
Method for forming metal wiring using conductive ink composition
First, the conductive ink composition according to the present invention is printed on a target substrate.
The conductive ink composition according to the present invention has a composition comprising from 5.0 to 90% by weight of a metal organic precursor comprising a metal-formate compound having an alkanolamine as a ligand and an extra dispersion solution. The composition of the conductive ink composition including the metal organic precursor and the description thereof have been described in detail above, and are omitted in order to avoid duplication.
The target substrate includes a semiconductor substrate, a wafer, a printed circuit board, a plastic substrate, and the like. The conductive ink composition may be screen printed or printed on one or both sides of the target substrate. The printing is not limited thereto and can be carried out by any conventional method.
Subsequently, the conductive ink composition printed on the target substrate is dried to form a metal wiring. The drying process is performed to finally form a metal wiring by performing thermal decomposition of the precursor by the provided heat. That is, the formation of the metal wiring is formed by reducing the metal organic precursor in the conductive ink composition to the metal film due to thermal decomposition by heat in a nitrogen atmosphere. The drying may be performed at a temperature of about 150 to 280 ° C.
The metal wiring thus formed may have a resistance of about 0.05? / Cm to 0.15? / Cm and also have excellent adhesion to the substrate.
Hereinafter, the components and technical features of the present invention will be described in more detail with reference to the following examples. However, the following examples are intended to illustrate the present invention in detail, but do not limit the scope of the present invention to those exemplified in these embodiments.
Example 1
Amino-2-methylpropan-1-ol was added to 10 g of copper formate tetrahydrate and the mixture was sonicated for 2 hours to obtain 2-amino-2-methylpropan-1- Ol (alkanolamine) was complexed. Thereafter, it was dried in a vacuum oven at 60 DEG C for one day to obtain 15 g of a copper organic precursor. At this time, copper formate tetrahydrate and unreacted alkanolamine were removed during the drying of the vacuum oven.
Evaluation example 1
The TGA (pyrolysis) analysis of the copper organic precursor obtained in Example 1 and the results are shown in FIG.
Referring to FIG. 1, TGA analysis of the copper organic precursor in Example 1 revealed that the copper organic precursor at 190 占 폚 was completely reduced, and the amount of the copper remaining after the reduction was 2-amino-2-methyl Propan-1-ol was found to be a complex, 19.4%, which is similar to the calculated theoretical value of 19.3%.
Example 2
The copper organic precursor obtained in Example 1 was dissolved in 50% by weight of isopropanol to form a conductive ink composition as shown in Fig. 2, and then the conductive ink composition was printed on the surface of a glass substrate. Thereafter, the substrate on which the conductive ink composition was printed was heat treated at about 350 캜 for about 30 minutes to form a copper metal wiring. The copper metallization had a surface resistance of 0.089? / Cm.
Evaluation example 2
The copper wiring formed on the organic substrate in Example 2 was subjected to XRD analysis, and the results are shown in Fig. 3.
As can be seen from the graph of FIG. 3, it can be confirmed that the copper wiring formed of the ink composition is a pure copper wiring free of copper oxide.
Claims (10)
Wherein the metal organic precursor comprises an excess of dispersion solution,
The alkanolamine
The metal-formate can be reacted with N-methylethanolamine, N-ethylethanolamine, N-propylethanolamine, N-butylethanolamine, N-methyldiethanolamine, N- ethyldiethanolamine, isopropanolamine, diisopropanolamine, Propyl isopropanolamine, 2-aminopropane-1-ol, N-methyl-2-aminopropane-1-ol, N-ethyl- Ol, N-methyl-1-aminopropane-3-ol, N-ethyl-1-aminopropane- Ol, N-methyl-2-aminobutan-1-ol, N-methyl-1-aminobutan- 3-aminobutane-1-ol, N-ethyl-3-aminobutan-1-ol, 1-amino Ol, N-methyl-1-aminobutan-4-ol, N-ethyl-1-aminobutan- Ol, 2-amino-4-methylpentan-1-ol, 2-aminohexan-1-ol, 3-aminoheptan- 1-aminopropane-1,3-diol, tris (oxymethyl) aminomethane, 1, One of the liquid alkanolamines selected from the group consisting of 2-diaminopropane-3-ol, 1,3-diaminopropane-2-ol, 2- (2-aminoethoxy) ethanol, Mixing;
Complexing the metal-formate with an alkanolamine as a ligand to form a liquid metal organic precursor; And
And drying the liquid metal organic precursor. The conductive ink composition according to claim 1, wherein the metal organic precursor comprises a metal organic precursor.
And drying the conductive ink composition printed on the substrate to form a metal wiring.
Wherein when the metal organic precursor in the conductive ink composition is heat-treated under the condition that nitrogen gas is supplied, the metal organic precursor is pyrolyzed and reduced to a metal.
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| KR101549672B1 (en) | 2014-08-26 | 2015-09-03 | 주식회사 코윈디에스티 | Display reparing device and method using conductive ink |
| KR101782799B1 (en) | 2015-08-11 | 2017-09-28 | (주)창성 | Method for preparation of copper-amine co-complex and conductive ion ink comprising the same and the fine pattern electrode using the same |
| KR101785617B1 (en) * | 2016-11-23 | 2017-10-20 | 창성나노텍 주식회사 | Electrically conductive metal ink composition for light sintering and Method for preparing the same |
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| KR20200004947A (en) | 2018-07-05 | 2020-01-15 | 재단법인 다차원 스마트 아이티 융합시스템 연구단 | Conductive pattern preparation method using multi-walled carbon nanotube filler-blended metal-organic decomposition ink and conductive pattern composition comprising the same |
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| KR101549672B1 (en) | 2014-08-26 | 2015-09-03 | 주식회사 코윈디에스티 | Display reparing device and method using conductive ink |
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| KR20170124660A (en) * | 2016-05-02 | 2017-11-13 | 서울대학교산학협력단 | Electroconductive ink composite including metal-organic precursor and polyhydric alcohol capable of heating in the air and method for forming the metal line using the same |
| KR101855121B1 (en) | 2016-05-02 | 2018-06-11 | 서울대학교산학협력단 | Electroconductive ink composite including metal-organic precursor and polyhydric alcohol capable of heating in the air and method for forming the metal line using the same |
| KR101785617B1 (en) * | 2016-11-23 | 2017-10-20 | 창성나노텍 주식회사 | Electrically conductive metal ink composition for light sintering and Method for preparing the same |
| KR20200004947A (en) | 2018-07-05 | 2020-01-15 | 재단법인 다차원 스마트 아이티 융합시스템 연구단 | Conductive pattern preparation method using multi-walled carbon nanotube filler-blended metal-organic decomposition ink and conductive pattern composition comprising the same |
| CN111417848A (en) * | 2018-08-03 | 2020-07-14 | 株式会社Lg化学 | Method for measuring insoluble materials in polymer solutions |
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