KR20210031200A - Composition of polysiloxane composite and preparation method thereof - Google Patents

Abstract

The present invention relates to a polysiloxane composite composition and a method for preparing the same. More particularly, the present invention relates to a polysiloxane composite composition comprising a polysiloxane-based polymer, a conductive material, and a saturated fatty acid compound having 5 or more carbon atoms as a solvent, and a method for preparing the same. The polysiloxane composite composition of the present invention improves the conductivity and stability of the composition by improving the dispersibility of the conductive material, and enables application to various uses.

Description

Polysiloxane composite composition and its manufacturing method TECHNICAL FIELD [COMPOSITION OF POLYSILOXANE COMPOSITE AND PREPARATION METHOD THEREOF}

The present invention relates to a polysiloxane composite composition and a method for preparing the same.

Polydimethylsiloxane (PDMS) is a silicone polymer-based material having transparent properties, and has advantages such as flexibility, lubricity, and hydrophobicity, and has permeability to various liquids and vapors. It can stably adhere to various substrates that are not flat, and separation is easy because adhesion between polymers does not occur well when molding other polymers. In addition, since it is optically transparent to a thickness of 300 nm, it can be used as an optical element, and because it is an elastomer with very strong durability, it can be manufactured as a stamp and used repeatedly.

Polydimethylsiloxane having such excellent properties can be diversified in structure and function through mixing with other materials. Accordingly, in order to broaden the application field of polydimethylsiloxane, it is being used in combination with various materials.

In particular, the polysiloxane composite, which is a mixture of polydimethylsiloxane and a conductive material, is very practical because it can be used not only as a biological signal measuring electrode, an electrical stimulation electrode, and a biological material sensor, but also as an electrode and a substrate constituting a flexible device. Therefore, research on this is actively underway.

In general, carbon-based materials such as carbon nanotubes and carbon fibers are often used as conductive materials. In order to secure high conductivity, it is necessary to uniformly disperse these carbon-based materials in a solvent containing polydimethylsiloxane at a high concentration.

However, since most of the carbon-based materials consist of carbon-carbon bonds, it was difficult to disperse the conductive materials including these carbon-based materials in a solvent at a high concentration. For this reason, it is difficult to secure the effect of improving the physical properties of the composite according to the use of the conductive material.

Accordingly, various techniques have been proposed to solve the above-described problems and to improve the conductivity of the polysiloxane composite.

For example, Korean Patent Registration No. 10-1768153 discloses that a conductive filler is dispersed in a mixture of polydimethylsiloxane and a low viscosity methyl-ended polydimethylsiloxane, and ultrasonically treated during the dispersion, thereby improving the dispersibility of the conductive filler. It is disclosed that the conductivity of the material can be improved.

In addition, Korean Patent Registration No. 10-1406085 discloses that a graphene/PDMS composite with improved dispersion can be prepared by using tetrahydrofuran as a solvent and dispersing it through ultrasonic and heat treatment.

These prior literatures have improved the dispersibility of the conductive material to some extent by applying high energy or changing the solvent during dispersion, but the effect is not sufficient. In addition, as a separate process for dispersion is required, there is a problem in that the manufacturing process is complicated and the manufacturing cost is increased. Accordingly, there is a need for further development of a polysiloxane composite exhibiting excellent conductivity through a simple process.

Korean Patent Registration No. 10-1768153 (2017.08.08), conductive polymer composite material Republic of Korea Patent Registration No. 10-1406085 (2014.06.03), graphene/PDMS composite manufacturing method and graphene/PDMS composite manufactured thereby

Accordingly, the present inventors conducted various studies to solve the above problem. As a result, when the polysiloxane composite composition contains a saturated fatty acid compound having 5 or more carbon atoms as a solvent, the dispersibility of the conductive material is improved, so that excellent conductivity and stability can be secured. It was confirmed that the present invention was completed.

Accordingly, an object of the present invention is to provide a polysiloxane composite composition with improved dispersibility.

In addition, another object of the present invention is to provide a method for preparing the polysiloxane composite composition.

In order to achieve the above object, the present invention provides a polysiloxane composite composition comprising a polysiloxane-based polymer, a conductive material, a curing agent and a solvent, wherein the solvent includes a saturated fatty acid compound having 5 or more carbon atoms.

The solvent may contain a saturated fatty acid compound having 5 to 15 carbon atoms.

The solvent is pentanoic acid, 2-methylpentanoic acid, hexanoic acid, 2-methylhexanoic acid, 2-ethylhexanoic acid, 3,5,5-trimethylhexanoic acid, heptanoic acid, octanoic acid, nonanoic acid, decanoic acid, 4 ,4-dimethyldecanoic acid, 9,9-dimethyldecanoic acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, and pentadecanoic acid.

The solvent may be included in an amount of 50 to 99% by weight based on 100% by weight of the total polysiloxane composite composition.

The solvent may be included in an amount of 1,000 to 100,000 parts by weight based on 100 parts by weight of the conductive material.

The conductive material may include at least one selected from the group consisting of carbon nanotubes, carbon fibers, carbon black, graphite, graphene, graphite, and activated carbon.

The conductive material may be included in an amount of 0.1 to 10% by weight based on 100% by weight of the total polysiloxane composite composition.

The polysiloxane-based polymer may include one or more selected from the group consisting of polydimethylsiloxane, polyvinylsiloxane, and polyphenylmethylsiloxane.

The polysiloxane-based polymer may be included in an amount of 1 to 50% by weight based on 100% by weight of the total polysiloxane composite composition.

In addition, the present invention includes the steps of (a) preparing a siloxane sol solution by mixing a polysiloxane-based polymer, a curing agent, and a solvent, and (b) mixing a conductive material with the siloxane sol solution, wherein the solvent has 5 or more carbon atoms. It provides a method for preparing a polysiloxane composite composition containing a saturated fatty acid compound.

The polysiloxane composite composition according to the present invention includes a saturated fatty acid compound having 5 or more carbon atoms as a solvent, thereby improving the dispersibility of a conductive material including a carbon-based material, and thus, can greatly improve the stability as well as the conductivity of the composition. Accordingly, the polysiloxane composite composition of the present invention can be used for various purposes such as various sensors, electrochemical devices, electronic devices, and optical devices.

1 is a photograph of evaluation of polysiloxane solubility according to Experimental Example 1 of polysiloxane composite compositions according to Examples and Comparative Examples of the present invention ((a): Example 1, (b): Comparative Example 2).
2 is a photograph of a polysiloxane composite composition according to Examples and Comparative Examples of the present invention after being left at room temperature for 10 days according to Experimental Example 2 ((a): Example 3, (b): Comparative Example 4, (c) ): Comparative Example 5, (d): Comparative Example 6).

Hereinafter, the present invention will be described in more detail.

The terms or words used in the specification and claims should not be construed as being limited to their usual or dictionary meanings, and the inventor may appropriately define the concept of terms in order to describe his own invention in the best way. It should be interpreted as a meaning and concept consistent with the technical idea of the present invention based on the principle that there is.

The terms used in the present invention are used only to describe specific embodiments, and are not intended to limit the present invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In the present invention, terms such as'include' or'have' are intended to designate the presence of features, numbers, steps, actions, components, parts, or a combination thereof described in the specification, but one or more other features. It is to be understood that the presence or addition of elements or numbers, steps, actions, components, parts, or combinations thereof does not preclude in advance.

The term “composite” as used herein refers to a material that expresses more effective functions while forming different phases physically and chemically by combining two or more materials.

Polydimethylsiloxane (PDMS) is easy to process, has excellent optical and mechanical properties, and has advantages such as hydrophobicity, transparency, flexibility, lubricity and releasability, and is harmless to the human body and exhibits excellent biocompatibility. It is applied to various fields ranging from fields and materials/manufacturing fields, medical fields, biotechnology fields, and environment/energy fields.

For excellent conductivity, polydimethylsiloxane is mixed with a conductive material to form a composite, and it is difficult to secure uniform dispersibility and storage stability due to agglomeration of a carbon-based material mainly used as a conductive material.

However, in order to be used in various sensors, electrochemical devices, electronic devices, optical devices, etc., high conductivity must be secured, and thus a polysiloxane composite in which a conductive material having a high concentration is stably dispersed is required.

To this end, in the prior art, a method of dispersing by applying energy from outside such as heat or ultrasonic treatment has been proposed, or a method such as introducing a functional group that increases dispersibility on the surface of a conductive material has been proposed, but the conductive material could not be sufficiently dispersed. In addition, it has the disadvantage of being inefficient due to the complicated process and high cost.

Accordingly, the present invention provides a polysiloxane composite composition using a saturated fatty acid compound having 5 or more carbon atoms as a solvent in order to improve the problem of low dispersibility of the conductive material and secure the effect of improving the conductivity of the polysiloxane composite including the same.

Specifically, the polysiloxane composite composition according to the present invention includes a polysiloxane-based polymer, a conductive material, a curing agent, and a solvent, and the solvent includes a saturated fatty acid compound having 5 or more carbon atoms.

The polysiloxane composite composition of the present invention is characterized in that it contains a saturated fatty acid compound having 5 or more carbon atoms as a solvent.

In the present invention, the solvent serves to evenly disperse the conductive material together with the polysiloxane-based polymer. Specifically, the conductive material of the present invention tends to strongly agglomerate as it contains a carbon-based material, which is caused by the van der Waals force to form a bundle and agglomerate to make interfacial contact with the solvent. It is an action to minimize the surface energy by minimizing. In order to improve the problem of aggregation of the conductive material and the problem of lowering the dispersibility and stability due to this, the present invention includes an aliphatic hydrocarbon chain having solubility in a polysiloxane-based polymer and a carboxylic acid group that helps disperse the conductive material, having 5 or more carbon atoms. A saturated fatty acid compound is included as a solvent.

In order to improve the dispersibility of a conductive material including a carbon-based material, the case of using an organic acid compound such as sulfonic acid or carboxylic acid as an additive is already known in the prior art. However, there is no known effect of improving the dispersibility of a conductive material by forming a siloxane sol into which a carboxylic acid group is introduced by applying it as a solvent of a polysiloxane composite composition as in the present invention.

The organic acid compound used in the prior art is used as an additive and serves to promote dispersion, and the solubility of polysiloxane could not be secured. On the other hand, in the case of the present invention, when a saturated fatty acid compound having 5 or more carbon atoms is used as a solvent, there is an advantage of simultaneously obtaining an effect of improving the dispersibility of the conductive material together with the polysiloxane solubility at room temperature.

In the present invention, the solvent contains a fatty acid compound having 5 or more carbon atoms, preferably 5 to 15 carbon atoms, which is a chain-shaped saturated monocarboxylic acid. In this case, when using a mixture of two or more solvents, a fatty acid compound having 15 or more carbon atoms may also be included. In addition, the fatty acid compound may be both straight chain and branched.

For example, the solvent is pentanoic acid, 2-methylpentanoic acid, hexanoic acid, 2-methylhexanoic acid, 2-ethylhexanoic acid (2-ethylhexanoic acid), 3,5,5-trimethylhexanoic acid, heptanoic acid, octanoic acid, nonanoic acid, decanoic acid (decanoic acid), 4,4-dimethyldecanoic acid, 9,9-dimethyldecanoic acid, undecanoic acid, dodecanoic acid , Tridecanoic acid, tetradecanoic acid, and pentadecanoic acid. Preferably, the solvent may be one or more selected from the group consisting of pentanoic acid, hexanoic acid, 2-ethylhexanoic acid, heptanoic acid and octanoic acid, and more preferably, the solvent is pentanoic acid, hexanoic acid and It may contain one or more selected from the group consisting of 2-ethylhexanoic acid.

The solvent may be included in an amount of 50 to 99% by weight, preferably 80 to 99% by weight, based on 100% by weight of the total polysiloxane composite composition. If the content of the solvent is less than the above range, a problem may occur in the solubility of the siloxane sol. Conversely, if the content of the solvent exceeds the above range, the dispersibility of the conductive material may decrease.

In addition, the solvent may be included in an amount of 1,000 to 100,000 parts by weight, preferably 2,000 to 10,000 parts by weight, based on 100 parts by weight of the conductive material. When the content of the solvent is outside the above-described range, a problem may occur in dispersibility, so it is preferable to determine an appropriate content within the above-described range.

The polysiloxane composite composition of the present invention includes a polysiloxane-based polymer and a conductive material together with the above-described solvent.

The polysiloxane-based polymer is any variety of compounds that alternately contain silicon and oxygen atoms in a linear or cyclic arrangement in which one or two organic groups are attached to each silicon atom, and is not particularly limited, and known ones may be used.

The polysiloxane-based polymer may include at least one selected from the group consisting of polydimethylsiloxane (PDMS), polyvinylsiloxane, and polyphenyl methylsiloxane. Preferably, the polysiloxane-based polymer may be polydimethylsiloxane.

The weight average molecular weight (M _w ) of the polysiloxane-based polymer is not particularly limited. When considering the dispersibility of the conductive material and the conductivity of the composition to be described later, it may be 10,000 to 200,000, preferably 20,000 to 100,000.

In addition, the viscosity of the polysiloxane-based polymer is not particularly limited, but may be 200 to 60,000 cst (25° C.), preferably 1,000 to 30,000 cst (25° C.) from the viewpoint of dispersibility and stability of the conductive material.

The polysiloxane-based polymer may be included in an amount of 1 to 50% by weight, preferably 1 to 20% by weight, based on 100% by weight of the total polysiloxane composite composition. If the content of the polysiloxane-based polymer is less than the above range, the dispersibility of the conductive material decreases, and if the content exceeds the above range, on the contrary, a problem may occur in the solubility of the siloxane sol. Therefore, it is preferable to determine an appropriate content within the above-described range. Do.

The conductive material is a material used to impart conductivity to the composition according to the present invention, and includes a carbon material.

The conductive material may include carbon nanotubes (CNTs) such as single-walled carbon nanotubes (SWCNTs) and multi-walled carbon nanotubes (MWCNTs); Carbon fibers such as graphite nanofibers (GNF), carbon nanofibers (CNF), and activated carbon fibers (ACF); Carbon blacks such as denka black, acetylene black, ketjen black, channel black, furnace black, lamp black, and summer black; Graphite; Graphene; It may include one or more selected from the group consisting of graphite, such as natural graphite, artificial graphite, and expanded graphite, and activated carbon. Preferably, the conductive material may be at least one selected from the group consisting of carbon nanotubes, carbon fibers, and graphene, and more preferably, the conductive material may be carbon fiber.

In one embodiment of the present invention, when the conductive material is a carbon fiber, the diameter of the carbon fiber is not particularly limited, but in general, the average diameter may be 10 to 1,000 nm, preferably 50 to 500 nm. In addition, the length of the carbon fiber is not particularly limited, but may be 2 µm or more, preferably 5 to 50 µm, for securing dispersibility and conductivity. In addition, the aspect ratio (length: diameter) of the carbon fiber may be 10 to 1,000, preferably 100 to 1,000.

The conductive material may be included in an amount of 0.1 to 10% by weight, preferably 0.5 to 5% by weight, based on 100% by weight of the total polysiloxane composite composition. If the content of the conductive material is less than the above range, the conductivity is lowered. Conversely, if the content of the conductive material exceeds the above range, a problem may occur in dispersion of the conductive material. Therefore, it is preferable to determine an appropriate content within the above-described range.

The curing agent is not particularly limited in the present invention, and any one that can be used in the technical field to which the present invention pertains may be applied without limitation.

In addition to the above-described composition, the polysiloxane composite composition of the present invention may additionally include additives commonly used for the purpose of improving its function in the relevant technical field, if necessary. For example, the additive may include a metal catalyst.

The polysiloxane composite composition according to the present invention includes a polysiloxane-based polymer, a conductive material, and a solvent, wherein the solvent includes a saturated fatty acid compound having 5 or more carbon atoms, thereby forming a polysiloxane composite in which the conductive material is evenly dispersed in the polysiloxane-based polymer. In particular, the polysiloxane composite composition of the present invention improves the dispersibility of the conductive material and can contain the conductive material at a high concentration of 1 to 100 mg/ml. Long-term stability can be improved. Accordingly, the polysiloxane composite composition of the present invention can be used in various fields requiring conductivity from bio to electronic materials.

In addition, the present invention provides a method for preparing the polysiloxane composite composition.

The method for preparing a polysiloxane composite composition according to the present invention includes (a) preparing a siloxane sol solution by mixing a polysiloxane-based polymer, a curing agent, and a solvent, and (b) mixing a conductive material with the siloxane sol solution; and In this case, the solvent includes a saturated fatty acid compound having 5 or more carbon atoms.

As described above, in the conventional manufacturing process of the polysiloxane composite composition, separate dispersion through heating or ultrasonic waves, surface treatment of the conductive material, and addition of a dispersant were performed to improve the dispersibility of the conductive material, but the dispersion characteristics of the conductive material The improvement effect was low. In comparison, the method for preparing a polysiloxane composite composition of the present invention uses a saturated fatty acid compound having 5 or more carbon atoms as a solvent to evenly disperse a conductive material in a polysiloxane polymer to form a composite, thereby preparing a polysiloxane composite. As the prepared polysiloxane composite composition improves the dispersibility and stability of the conductive material, it can exhibit excellent conductivity when used in various sensors and electrical devices.

Hereinafter, each step will be described.

First, in step (a), a polysiloxane-based polymer, a curing agent, and a solvent are mixed to prepare a siloxane sol solution.

The polysiloxane-based polymer used in step (a) is as described above.

In particular, the solvent used in step (a) is a saturated fatty acid compound having 5 or more carbon atoms, and other characteristics are as described in the polysiloxane composite composition.

The curing agent used in step (a) is not particularly limited as it is commonly used in the relevant technical field.

The siloxane sol solution containing the above-described polysiloxane-based polymer, a curing agent and a solvent containing a saturated fatty acid compound having 5 or more carbon atoms is 1 to 100% by weight, preferably 1 to 50% by weight of the polysiloxane-based polymer based on 100% by weight of the solvent. %, more preferably 1 to 25% by weight. When the concentration of the siloxane sol solution is out of the above-described range, a problem may occur in solubility, so it is preferable to determine an appropriate content within the above-described range.

The mixing of step (a) may be performed according to a conventional method known in the art. The mixing is to increase the degree of mixing between the above-described materials, and may be performed using a stirring device commonly used in the art. At this time, the mixing time and speed may also be selectively adjusted according to the content and conditions of each composition.

Subsequently, in step (b), a conductive material is mixed with the siloxane sol solution prepared in step (a).

The step (b) is a process of compounding a polysiloxane-based polymer and a conductive material. In this case, mixing may be performed according to a conventional method known in the art as described in step (a), and the mixing condition is also dependent on the conditions. It can be selectively adjusted accordingly.

The manufacturing method of the polysiloxane composite composition according to the present invention has the advantage of being able to manufacture a polysiloxane composite composition exhibiting excellent dispersibility, stability, and conductivity without a simple process, easy commercial application, and no additional additives or processes. . The polysiloxane composite composition prepared by the above-described manufacturing method can be applied on a substrate to form a coating film, wherein the coating film exhibits excellent conductivity by showing a low surface resistance of 10 ohm/sq or less, and various sensors, electrochemical devices , Electronic devices, optical devices, and the like.

Hereinafter, a preferred embodiment is presented to aid in the understanding of the present invention, but it is obvious to those skilled in the art that various changes and modifications are possible within the scope of the present invention and the scope of the technical idea, but the following examples are only illustrative of the present invention, It is natural that such modifications and modifications fall within the scope of the appended claims.

Examples and Comparative Examples

[Example 1]

To 10 ml of pentanoic acid (manufactured by Sigma Aldrich), 1 g of polydimethylsiloxane (Sylgard 184, manufactured by Dow Corning) was added as a curing agent (Sylgard 184 curing agent, manufactured by Dow Corning). ) And 10:1 weight ratio and sufficiently stirred to dissolve.

To the siloxane sol solution, 0.1 g of carbon fiber (VGCF-H, manufactured by Showa Denko Carbon) was added and stirred at 300 rpm for 2 hours to prepare a polysiloxane composite composition.

[Example 2]

To 10 ml of hexanoic acid (manufactured by Sigma Aldrich), 1 g of polydimethylsiloxane (Sylgard 184, manufactured by Dow Corning) was added as a curing agent (Sylgard 184 curing agent, manufactured by Dow Corning). ) And 10:1 weight ratio and sufficiently stirred to dissolve.

To the siloxane sol solution, 0.1 g of carbon fiber (VGCF-H, manufactured by Showa Denko Carbon) was added and stirred at 300 rpm for 2 hours to prepare a polysiloxane composite composition.

[Example 3]

To 10 ml of 2-ethylhexanoic acid (manufactured by Sigma Aldrich), 1 g of polydimethylsiloxane (Sylgard 184, manufactured by Dow Corning) was added as a curing agent (Sylgard 184 curing agent, Dow Corning). ) Company product) and 10:1 weight ratio, and sufficiently stirred to dissolve.

To the siloxane sol solution, 0.1 g of carbon fiber (VGCF-H, manufactured by Showa Denko Carbon) was added and stirred at 300 rpm for 2 hours to prepare a polysiloxane composite composition.

[Comparative Example 1]

To 10 ml of methanesulfonic acid (manufactured by Sigma Aldrich), 1 g of polydimethylsiloxane (Sylgard 184, manufactured by Dow Corning) was added as a curing agent (Sylgard 184 curing agent, Dow Corning). Product) and 10:1 weight ratio, and sufficiently stirred to dissolve.

To the siloxane sol solution, 0.1 g of carbon fiber (VGCF-H, manufactured by Showa Denko Carbon) was added and stirred at 300 rpm for 2 hours to prepare a polysiloxane composite composition.

[Comparative Example 2]

1 g of polydimethylsiloxane (Sylgard 184, manufactured by Dow Corning) was added to 10 ml of acetic acid (manufactured by Daejeonghwa Gold) and 10:1 weight with a curing agent (Sylgard 184 curing agent, manufactured by Dow Corning). The mixture was mixed at a rate and sufficiently stirred to dissolve.

To the siloxane sol solution, 0.1 g of carbon fiber (VGCF-H, manufactured by Showa Denko Carbon) was added and stirred at 300 rpm for 2 hours to prepare a polysiloxane composite composition.

[Comparative Example 3]

To 10 ml of propanoic acid (manufactured by Dow Corning), 1 g of polydimethylsiloxane (Sylgard 184, manufactured by Dow Corning) was mixed with a curing agent (Sylgard 184 curing agent, manufactured by Dow Corning) and 10:1. The mixture was mixed at a weight ratio and sufficiently stirred to dissolve.

To the siloxane sol solution, 0.1 g of carbon fiber (VGCF-H, manufactured by Showa Denko Carbon) was added and stirred at 300 rpm for 2 hours to prepare a polysiloxane composite composition.

[Comparative Example 4]

1 g of polydimethylsiloxane (Sylgard 184, manufactured by Dow Corning) was added to 10 ml of chloroform (manufactured by Daejeonghwa Geum) and 10:1 weight with a curing agent (Sylgard 184 curing agent, manufactured by Dow Corning). The mixture was mixed at a rate and sufficiently stirred to dissolve.

To the siloxane sol solution, 0.1 g of carbon fiber (VGCF-H, manufactured by Showa Denko Carbon) was added and stirred at 300 rpm for 2 hours to prepare a polysiloxane composite composition.

[Comparative Example 5]

To 10 ml of dimethylformamide (manufactured by Daejeonghwa Geum Corporation), 1 g of polydimethylsiloxane (Sylgard 184, manufactured by Dow Corning) was added as a curing agent (Sylgard 184 curing agent, manufactured by Dow Corning) and 10: The mixture was mixed at a weight ratio of 1 and sufficiently stirred to dissolve.

To the siloxane sol solution, 0.1 g of carbon fiber (VGCF-H, manufactured by Showa Denko Carbon) was added and stirred at 300 rpm for 2 hours to prepare a polysiloxane composite composition.

[Comparative Example 6]

Toluene (manufactured by Sigma Aldrich), 1 g of polydimethylsiloxane (Sylgard 184, manufactured by Dow Corning) was added as a curing agent (Sylgard 184 curing agent, manufactured by Dow Corning). And 10:1 weight ratio, and sufficiently stirred to dissolve.

To the siloxane sol solution, 0.1 g of carbon fiber (VGCF-H, manufactured by Showa Denko Carbon) was added and stirred at 300 rpm for 2 hours to prepare a polysiloxane composite composition.

Experimental Example 1. Evaluation of polysiloxane solubility

Polysiloxane solubility in the manufacturing process of the polysiloxane composite compositions prepared in Examples 1 and 2 and Comparative Examples 1 to 3 was visually evaluated. The results obtained at this time are shown in FIG. 1.

In FIG. 1, (a) corresponds to Example 1, and (b) corresponds to Comparative Example 2. Referring to FIG. 1, in the case of Example 1, it is transparent, but in the case of Comparative Example 2, it can be seen that polysiloxane is not dissolved and is present in the supernatant. From these results, it can be seen that in the case of the polysiloxane composite composition according to the embodiment, the polysiloxane is completely dissolved and appears in a transparent sol form, whereas in the case of Comparative Examples 1 to 3, it can be confirmed that the polysiloxane is not dissolved and separated.

Experimental Example 2. Conductive material dispersibility evaluation

While the polysiloxane composite compositions prepared in Example 3 and Comparative Examples 4 to 6 were allowed to stand at room temperature (about 25° C.), the degree of dispersion was observed with the naked eye. Figure 2 shows the state after 10 days.

In FIG. 2, (a) corresponds to Example 3, (b) corresponds to Comparative Example 4, and (c) corresponds to Comparative Example 5 and (d) corresponds to Comparative Example 6, respectively. As shown in FIG. 2, in the case of Example 3, specifically, in the case of the composition according to Example 3, precipitation does not occur and the dispersed state is maintained even after 10 days, whereas the composition according to Comparative Examples 4 to 6 is conductive. It can be seen that the precipitation of the material has occurred. From these results, it can be confirmed that the polysiloxane composite composition according to the present invention has excellent dispersibility in the conductive material.

Claims (11)

Including a polysiloxane-based polymer, a conductive material, a curing agent and a solvent,
The solvent is a polysiloxane composite composition comprising a saturated fatty acid compound having 5 or more carbon atoms. The method of claim 1,
The solvent comprises a saturated fatty acid compound having 5 to 15 carbon atoms, polysiloxane composite composition. The method of claim 1,
The solvent is pentanoic acid, 2-methylpentanoic acid, hexanoic acid, 2-methylhexanoic acid, 2-ethylhexanoic acid, 3,5,5-trimethylhexanoic acid, heptanoic acid, octanoic acid, nonanoic acid, decanoic acid, 4 ,4-dimethyldecanoic acid, 9,9-dimethyldecanoic acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid and pentadecanoic acid, comprising at least one selected from the group consisting of, polysiloxane composite composition. The method of claim 1,
The solvent comprises 50 to 99% by weight based on 100% by weight of the total polysiloxane composite composition, polysiloxane composite composition. The method of claim 1,
The solvent comprises 1,000 to 100,000 parts by weight based on 100 parts by weight of a conductive material, polysiloxane composite composition. The method of claim 1,
The conductive material includes at least one selected from the group consisting of carbon nanotubes, carbon fibers, carbon black, graphite, graphene, graphite, and activated carbon. The method of claim 1,
The conductive material comprises 0.1 to 10% by weight based on 100% by weight of the total polysiloxane composite composition, polysiloxane composite composition. The method of claim 1,
The polysiloxane-based polymer comprises at least one selected from the group consisting of polydimethylsiloxane, polyvinylsiloxane and polyphenylmethylsiloxane, polysiloxane composite composition. The method of claim 1,
The polysiloxane-based polymer comprises 1 to 50% by weight based on 100% by weight of the total polysiloxane composite composition, polysiloxane composite composition. (a) preparing a siloxane sol solution by mixing a polysiloxane-based polymer, a curing agent, and a solvent, and
(b) mixing a conductive material in the siloxane sol solution,
The solvent is a method for producing a polysiloxane composite composition comprising a saturated fatty acid compound having 5 or more carbon atoms. The method of claim 10,
The siloxane sol solution contains 1 to 100% by weight of a polysiloxane-based polymer based on 100% by weight of a solvent.

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