KR20170086270A - Ti3SiC2 COATING COMPOSITION AND COATING METHOD USING THE SAME - Google Patents

Ti3SiC2 COATING COMPOSITION AND COATING METHOD USING THE SAME Download PDF

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KR20170086270A
KR20170086270A KR1020160005901A KR20160005901A KR20170086270A KR 20170086270 A KR20170086270 A KR 20170086270A KR 1020160005901 A KR1020160005901 A KR 1020160005901A KR 20160005901 A KR20160005901 A KR 20160005901A KR 20170086270 A KR20170086270 A KR 20170086270A
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coating
fiber
fibers
powder
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KR101816061B1 (en
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이현근
김원주
박지연
김대종
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한국원자력연구원
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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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
    • C09D5/4407—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained by polymerisation reactions involving only carbon-to-carbon unsaturated bonds
    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
    • C09D5/4419—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained otherwise than by polymerisation reactions only involving carbon-to-carbon unsaturated bonds
    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
    • C09D5/448—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications characterised by the additives used
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00—Electrophoretic coating characterised by the process
    • C25D13/02—Electrophoretic coating characterised by the process with inorganic material
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00—Electrophoretic coating characterised by the process
    • C25D13/12—Electrophoretic coating characterised by the process characterised by the article coated

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Abstract

The present invention relates to Ti 3 SiC 2 The present invention relates to a coating composition, and more particularly, to a coating composition using Ti 3 SiC 2 A solvent, a solvent, a solvent, and a solvent, wherein the solvent is selected from the group consisting of Ti 3 SiC 2 Composition for coating; And providing a SiC fiber connected to the cathode, providing a positive electrode spaced from the SiC fiber, the Ti 3 SiC 2 of the present invention Of SiC fibers by using a coating composition comprising the step of electrophoretic Ti 3 SiC 2 Coating method is provided.

Description

TECHNICAL FIELD [0001] The present invention relates to a Ti3SiC2 coating composition,

The present invention relates to Ti 3 SiC 2 The present invention relates to a coating composition and a coating method using the same, and more particularly to a coating composition comprising Ti 3 SiC 2 Coating suspension composition and a method of coating SiC fiber through electrophoresis using the same.

Max phases is used in a wide range of ceramic materials based on M n +1 AX n where M is a transition metal, A is Si, Al, Ge or Ga and X is C, N or B. The MAX phases are characterized by a low content of nonmetal atoms compared to metal atoms. US 5,942,455 discloses a process for producing bulk products having a solid phase or a single phase in the form of a mixture of M 3 X 1 Z 2 , which is characterized in that the powder mixture containing M, X and Z is heated to a temperature of approximately 1000 to 1800 ° C Lt; / RTI > The product thus formed is excellent in impact resistance, resistance to oxidation, and machinability.

On the other hand, SiC f / SiC composites are being investigated for applications as high temperature structural materials and next generation reactor reactor components due to their excellent performance at high temperatures and excellent radiation resistance. Of SiC f / SiC composite is woven SiC fiber and the SiC matrix (matrix), and consists of an interface image on the SiC fiber and the base, in particular SiC fiber surface is made be generated cracks is bent along the interface between SiC f / SiC composite It plays a very important role in improving fracture toughness. And the interfacial phase PyC and h-BN having a layered structure is coated on a SiC fiber is most widely used, due to the application when the layer structure as interphase fiber is easily within the composite pull-out (pull-out) is SiC f / SiC composite of the present invention exhibits improved fracture toughness.

However, PyC and h-BN have weak points of oxidation at high temperature, and mechanical properties of the material may decrease due to interfacial oxidation in an ultra-high temperature environment. Therefore, in order for the SiC f / SiC composite to be used as a high-temperature structural material or a high-temperature next-generation reactor reactor part, it is necessary to improve the oxidation resistance at the interface. The Ti 3 SiC 2 MAX phase is highly stable to high-temperature oxidation and thermal shock, and has a hexagonal structure, forming an anisotropic structure by forming a layered structure at the base. Therefore, SiC f / SiC composites with superior mechanical properties and oxidation resistance, such as cracking on the interface when the Ti 3 SiC 2 MAX phase is applied to the interface and fracture toughness being improved by easily pulling out the fibers in the composite, . ≪ / RTI >

Therefore, various studies have been conducted to coat the Ti 3 SiC 2 MAX phase, and in particular, studies using CVD (Chemical Vapor Deposition) have mainly been carried out. However, when the Ti 3 SiC 2 MAX phase is coated by CVD, the underlying surface is formed in a direction perpendicular to the substrate, and thus it does not contribute to improving the fracture toughness of the composite when applied on the interface of the composite. In addition, attempts have been made by various CVD methods, but no studies have been carried out to deposit layered structures parallel to the fibers.

On the other hand, there has been studied a technique of coating a MAX-phase powder on a plate-shaped substrate through electrophoresis, but since this technique is difficult to apply directly to the interfacial coating of a SiC fiber fabric, It is expected that the technique will be widely applied in the related field if the technique of coating the entire 360 degrees uniformly and coating the SiC fibers inside the fabric as well as the SiC fibers outside the fabric is developed.

Accordingly, one aspect of the present invention is to provide a method of forming a Ti 3 SiC 2 And to provide a suspension composition for coating.

Another aspect of the present invention relates to the Ti 3 SiC 2 And a method of coating SiC fibers through electrophoresis using a suspension composition for coating.

According to one aspect of the present invention, Ti3SiC2 A solvent, a solvent, a solvent, a powder, a dispersant, and a remainder, wherein the solvent is selected from the group consisting of Ti3SiC2 A coating composition is provided.

According to another aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: providing SiC fibers connected to a cathode; Providing a positive electrode spaced from the SiC fiber; The Ti 3 SiC 2 of the present invention And a step of electrophoresis using a composition for coating, wherein the SiC fiber's Ti 3 SiC 2 Coating method is provided.

According to the present invention, it is possible to produce a composite excellent in high-temperature oxidation resistance while maintaining excellent mechanical properties by coating Ti 3 SiC 2 MAX phase on SiC fiber and using it as an interface phase of SiC f / SiC composite. SiC f / SiC composites which are excellent in high temperature oxidation resistance can be applied to high-temperature structural materials or reactor reactor parts to improve the life of these materials. In addition, the coating on the interface can be carried out through a liquid process rather than a CVD process, thereby shortening the coating time, and the process cost can be reduced as compared with the CVD process, so that the cost for manufacturing the composite can be reduced.

FIG. 1 is a photograph showing the effect of applied voltage and time for SiC fiber coating by electrophoresis using a Ti 3 SiC 2 suspension composition.
FIG. 2 is a photograph showing the effect of Ti 3 SiC 2 and PEI concentration on the SiC fiber coating by electrophoresis using a Ti 3 SiC 2 suspension composition. More specifically, FIG. 2 (a) shows the results of Comparative Example 2, and FIG. 2 (b) shows the results of Comparative Example 3.
FIG. 3 is a photograph showing the results of experiments on the addition of a binder component and the effect of application of a conductive paste.
Fig. 4 schematically shows an example of an electrophoresis apparatus for carrying out the coating method of the present invention.

Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings. However, the embodiments of the present invention can be modified into various other forms, and the scope of the present invention is not limited to the embodiments described below.

According to the present invention, Ti 3 SiC 2 to coat the Ti 3 SiC 2 MAX phase in SiC fiber A composition for coating is provided, wherein the Ti 3 SiC 2 When the electrophoresis is carried out by using the coating composition, unlike the conventional CVD coating method in which the layered structure is formed in a direction perpendicular to the fibers and the effect of improving the fracture toughness is not exhibited, the Ti 3 SiC 2 MAX powder exhibits an anisotropic form The coating may be carried out so as to exhibit a layered structure in a direction parallel to the SiC fibers. It is not possible to coat the spherical particles so as to exhibit a layered structure. When the particles are anisotropic, the layered structure may be formed in a parallel direction. In the present invention, And confirmed the possibility of performance.

In the present invention, "SiC fabric" or "SiC fabric" means a fabric woven with SiC fiber bundles, .

The Ti 3 SiC 2 The composition for coating is Ti 3 SiC 2 A powder, a dispersing agent and a residual solvent, wherein the solvent comprises ethanol and water.

At this time, the Ti 3 SiC 2 The average particle diameter of the powder is preferably 1 占 퐉 or less, more preferably 0.1 to 1 占 퐉, and further preferably 0.1 to 0.5 占 퐉. The Ti 3 SiC 2 When the average particle diameter of the powder exceeds 1 탆, there is a problem that the powder is hardly uniformly adhered to the surface of the round SiC fiber to be coated.

The dispersant is at least one component selected from the group consisting of nonionic surfactants such as polyethyleneimine (PEI), polyethylene oxide (PEO), polyethylene glycol (PEG) .

On the other hand, the Ti 3 SiC 2 The powder was Ti 3 SiC 2 It is preferably contained in an amount of 0.01 to 1% by weight based on the total weight of the coating composition, more preferably 0.03 to 0.2 % ≪ / RTI > by weight. The Ti 3 SiC 2 When the amount of the powder is less than 0.01% by weight, the coating is insufficient on the entire surface of the SiC fiber. If the amount of the powder is more than 1% by weight, the addition amount of the dispersant for dispersing the Ti 3 SiC 2 powder is greatly increased The properties of the composition for coating Ti 3 SiC 2 may not be suitable for carrying out the coating by electrophoresis.

The dispersant may be Ti 3 SiC 2 Is preferably contained in an amount of 0.1 to 5% by weight, more preferably 0.3 to 1.5% by weight, based on the total weight of the coating composition. When the dispersing agent is contained in an amount of less than 0.1% by weight, Ti 3 SiC 2 The dispersibility of the powder may be lowered and aggregation may occur. If it is contained in an amount exceeding 5% by weight, the viscosity of the prepared composition for coating with Ti 3 SiC 2 may greatly increase, or the zeta potential value may become remarkably small. A problem that is difficult to perform the coating may occur.

The solvent used in the present invention includes ethanol and water. The solvent preferably has a weight ratio of ethanol: water of 1: 0.5 to 1: 5, more preferably water in an amount of not less than the weight of ethanol, More preferably, water is contained in an amount exceeding ethanol, and the weight ratio of ethanol: water is more than 1: 1 to 1: 5. On the other hand, water is when included in an amount of less than 0.5 parts by weight per ethanol, 1 part by weight, the movement of the character and Ti 3 SiC 2 powder electrolytic composition for coating Ti 3 SiC 2 is also not good, the characteristics do not coating is not smooth A problem may arise.

The dispersant and Ti 3 SiC 2 The powder was Ti 3 SiC 2 Powder: dispersant = 1: 3 to 30% by weight, and the dispersant is preferably contained in a ratio of Ti 3 SiC 2 When if it is included in not more than three times the weight of the powder is performed by using this, a coating of SiC fiber Ti 3 SiC 2 The coating composition tends to be laminated between SiC fibers without being coated with the SiC fibers, and when the dispersant is Ti 3 SiC 2 When the weight of the SiC fiber is more than 30 times the weight of the powder, the coating amount of the SiC fiber may be too high to increase the viscosity of the composition for coating the Ti 3 SiC 2 , There is a problem that the uniformity of the Ti 3 SiC 2 powder coating is reduced.

On the other hand, the Ti 3 SiC 2 PH of the coating composition is 2 to 9.4, preferably 6 to 8, will, pH is less than 2 when Ti 3 SiC 2, there is a greater volume of the anion of the acidic substance to be added to lower the pH of the coating composition for the Ti 3 SiC 2 coating is uneven. When the pH exceeds 9.4, the zeta potential of the composition for coating Ti 3 SiC 2 becomes negative, which may result in a problem of coating on electrodes other than the SiC fabric.

The Ti 3 SiC 2 The coating composition may further comprise at least one binder selected from the group consisting of polyvinyl butyral (PVB), polycarbosilane (PCS), polyvinyl alcohol (PVA) and the like, preferably polyvinyl butyrate Lt; / RTI > (PVB). When such a binder is Ti 3 SiC 2 When included in the coating composition, Ti 3 SiC 2 It is expected that the coating uniformity of the SiC single fiber can be improved due to the increase of the tackiness of the powder and even more uniform coating layer can be formed in the entire SiC fabric.

At this time, the binder is Ti 3 SiC 2 If it is desirable, and include less than 0.01% by weight which comprises the entire weight of the coating composition in an amount of 0.01 to 5% by weight basis, it may be minimal, the effect of adding the binder, if it exceeds 5% by weight, Ti 3 SiC 2 coating may increase the viscosity of the coating composition, which may result in difficulty in coating or the problem of coagulation of the Ti 3 SiC 2 powder.

Further, according to the present invention, the Ti 3 SiC 2 Ti 3 SiC 2 of SiC fiber using coating composition A coating method is provided, and the SiC fiber of the present invention, Ti 3 SiC 2 The coating method includes the steps of: providing SiC fibers connected to a cathode; Providing a positive electrode spaced from the SiC fiber; And the Ti 3 SiC 2 of the present invention And electrophoresis using the composition for coating.

The Ti 3 SiC 2 The technical content of the coating composition is as described above, and the SiC fiber can be provided as a SiC fabric woven with a SiC fiber bundle.

The SiC fibers preferably have an average diameter of 4 to 50 mu m, and the average thickness of the SiC fiber bundles is preferably 50 to 500 mu m.

Wherein when the average diameter of the SiC fiber is less than 4 μm had a problem that the SiC fiber diameter that is smaller Ti 3 SiC 2 powder is not uniformly coated, preferably to the preparation of a complex comprising a SiC fiber than 50 μm one upper The average thickness of the bundles of SiC fibers is preferably not less than 50 占 퐉 in the manufacturing process, but the lower limit is not limited thereto, and in the case of more than 500 占 퐉, the bundles of SiC fibers may be subjected to electrophoresis There is a problem that uniform coating is difficult to be performed inside the SiC fabric.

Preferably, the anode comprises two anodes arranged in parallel to the SiC fibers, and the two anodes disposed on both sides of the SiC fiber are preferably spaced equidistant from the SiC fibers.

Meanwhile, the electrophoresis is preferably performed for a period of 10 minutes to 4 hours or less under an applied voltage of more than 5 V but less than 20 V, and when the applied voltage is 5 V or less, the coating is not uniformly roughened And if it is 20 V or more, there is a problem that the SiC fabric is coated thickly only on the surface thereof. On the other hand, when the coating time is less than 10 minutes, the coating of Ti 3 SiC 2 is not sufficiently coated. If the coating time exceeds 4 hours, the coating of SiC fabric is coated with Ti 3 SiC 2 powder, A problem may occur that is not performed.

The ratio (V / d) of the applied voltage (V) to the distance (d) between the SiC fiber and the anode is preferably 2.5 to 10 V / cm, and the applied voltage (V / d) is less than 2.5 V / cm, there is a problem that the coating is not uniformly roughened. When the ratio (V / d) is more than 10 V / cm, there is a problem that the surface is thickly coated only on the surface of the SiC fabric Lt; / RTI >

Furthermore, the SiC fiber of the present invention, Ti 3 SiC 2 In the coating method, the step of treating the edges of the SiC fibers with a conductive paste may further include the step of forming a more uniform coating layer in the SiC fiber fabric. That is, the conductive paste reduces the resistance between the positive electrode and the SiC fibers and between the respective SiC fibers so that a more uniform coating can be performed.

The conductive paste is preferably at least one selected from the group consisting of a carbon paste, a metal paste, and a conductive epoxy paste. Preferably, carbon paste is used. The carbon paste can be used, for example, by diluting the carbon paste to acetone by about 1 to 100 times. The conductive paste can uniformly impregnate the end portion of the SiC fabric to the inside of the SiC fabric.

As described above, according to the present invention, a TiC 3 SiC 2 MAX phase can be coated on SiC fibers and utilized as an interface phase of a SiC f / SiC composite to produce a composite having excellent high temperature oxidation resistance while maintaining excellent mechanical properties. SiCf / SiC composites which are excellent in high temperature oxidation resistance can be applied to high-temperature structural materials or reactor reactor parts to improve the life of these materials.

FIG. 4 schematically shows an example of an electrophoresis apparatus for carrying out the coating method of the present invention,

The SiC fabric connected to the cathode of the power supply device and the anodes located on both sides thereof are disposed in the chamber containing the Ti 3 SiC 2 coating composition of the present invention wherein the SiC fabric can be fixed with a fixing member between the conductive plates, In particular, the edges of the SiC fabric (fabric) can be treated with a conductive paste as shown in Fig. However, the electrophoresis apparatus that can be used in the present invention is not limited thereto.

Hereinafter, the present invention will be described more specifically by way of specific examples. The following examples are provided to aid understanding of the present invention, and the scope of the present invention is not limited thereto.

Example

One. Ti 3 SiC 2 Preparation of coating compositions

Example  One

The commercial Ti 3 SiC 2 powder (MAXTHAL 312, Sanvik AB, Sweden) was ball milled through a planetary ball-mill to grind the powder size to below 1 μm. 0.3 wt% of PEI (branched polyethlyeneimine) having a molecular weight of 10,000 was used as a dispersing agent. 0.03 wt% of Ti 3 SiC 2 powder was mixed with ethanol, and 0.03 wt% of the powder was mixed with ethanol and water at a ratio of 1: 1 Suspension compositions were prepared with one solvent.

Example  2

A suspension composition was prepared in the same manner as in Example 1, except that 0.1 wt% of Ti 3 SiC 2 powder, 1.0 wt% of PEI and 0.1 wt% of polyvinyl butyral (PVB) binder were added.

Comparative Example  One

A suspension composition was prepared by the same procedure as in Example 1 except that no dispersing agent was used.

Comparative Example  2

Same as Example 1 except that the ratio of Ti 3 SiC 2 powder and dispersant was adjusted to 1: 3 by using 0.1 wt% of Ti 3 SiC 2 powder together with 0.3 wt% of a branched polyethlyeneimine (PEI) dispersant having a molecular weight of 10,000. To prepare a suspension composition.

Comparative Example  3

Having a molecular weight of 10,000 PEI (branched Polyethlyeneimine) a dispersant with 1.0 wt% Ti 3 SiC 2 powder of 0.5 using a wt% Ti 3 SiC 2 powder and the proportion of the dispersing agent 1: the same as in Example 1 except that the adjustment to the two To prepare a suspension composition.

2. Ti 3 SiC 2 Using the coating composition SiC  Coating of fibers

The zeta potential of the Ti 3 SiC 2 suspension composition obtained in the above step 1 was measured to coat the SiC Ti 3 SiC 2 powder by electrophoresis.

The cathode was connected to the SiC fiber and the electrode was installed on both sides parallel to the fiber at a distance of 20 mm from the SiC fiber, and the anode was connected. Ti 3 SiC 2 was to be to indicate the zeta potential is a positive value of the suspension composition to adjust the pH of the suspension composition of Ti 3 SiC 2 to move the Ti 3 SiC 2 powder as the negative electrode with the SiC fiber.

The Ti 3 SiC 2 suspension composition of Comparative Example 1 in which the dispersant was not mixed showed a zeta potential value of 0 at a pH of 7.5 and a positive zeta potential value at a decrease of pH. The values were negative.

In the case of Example 1, in which 0.3 wt% of PEI was mixed with the dispersing agent, the zeta potential value was 0 at pH 9.4, and a positive value when the pH was decreased and a negative value when the pH was increased.

After setting the pH of the Ti 3 SiC 2 suspension composition to 7, the SiC fiber fabric is mounted with the electrode in the center of the electrophoresis apparatus, and a voltage of 5 to 20 V is applied And then electrophoresed for 2 hr.

At this time, the SiC fiber fabric was formed by bundling SiC single fibers having an average diameter of 8 탆 and having a thickness of about 150 탆, and woven fabrics were used.

While the concentration of the dispersant PEI in the Ti 3 SiC 2 suspension composition was increased from 0.1 wt.% To 1.5 wt.%, The zeta potential value was above 12 mV when the pH of the Ti 3 SiC 2 suspension composition was 7, Ti 3 SiC 2 powder was able to migrate to the electrode.

3. Analysis of influence of applied voltage and time in electrophoresis

1 (c) and FIG. 1 (d), when the SiC fiber was coated with the Ti 3 SiC 2 suspension composition of Example 1 at an applied voltage of 10 V for 2 hours, 3 SiC 2 powder was coated on the surface of the SiC powder, and it was confirmed that the layered structure of anisotropic Ti 3 SiC 2 powder was coated parallel to the SiC fiber.

However, in the case of performing electrophoresis at an applied voltage of 20 V, as shown in FIG. 1 (a), even when the coating time is maintained for 1 hour, Ti 3 SiC 2 powder is laminated thickly on the surface of the SiC fabric, Was not performed.

In addition, when the coating time by electrophoresis was maintained for 2 hours at an applied voltage of 5 V, it was confirmed that the Ti 3 SiC 2 powder was plated on the SiC fiber as shown in FIG. 1 (b).

4. Electrophoresis Ti 3 SiC 2  And PEI  Impact analysis by concentration

Comparative Example 2 in which 0.1 wt% of Ti 3 SiC 2 and 0.3 wt% of PEI as a dispersant were added, and Comparative Example 2 in which 0.5 wt% of Ti 3 SiC 2 and 1.0 wt% of PEI as a dispersant were added was used SiC fiber.

2 (a), which is the result of Comparative Example 2, and Fig. 2 (b), which is the result of Comparative Example 3, the SiC fabric is not coated on the SiC fiber even when coated at an applied voltage of 10 V for 2 hours. It was confirmed that Ti 3 SiC 2 powder was laminated between the inner SiC fibers.

That is, Ti 3 SiC 2 and the weight ratio is 1 PEI: In 10 Suspension compositions been made a smooth coating on the SiC fiber, Ti 3 SiC a weight ratio of 2 and PEI 1: 3 or less, the Ti 3 SiC 2 powder, SiC And it was confirmed that they were laminated between SiC fibers without being coated with fibers.

5. Ti 3 SiC 2  Analysis of effect of addition of binder in suspension composition

The Ti 3 SiC 2 suspension composition of Example 2 was applied at an applied voltage of 10 V for 2 hours.

In the case of the suspension composition in which polyvinyl butyral (PVB, polyvinylbutyral) was further added as a binder as in Example 2, the uniformity of coating of Ti 3 SiC 2 on the entire SiC single fibers and the SiC fabric was increased, The coating uniformity of the SiC single fibers and the coating uniformity of the entire SiC fabric were improved due to the increase in the tackiness of the Ti 3 SiC 2 powder.

6. SiC fabric  Analysis of the effect of conductive paste application on the edge

In order to improve the uniformity of the coating, conductive paste was applied to the edge of the SiC fabric specimen during electrophoresis. More specifically, a carbon paste is applied to the edge portion of the SiC fiber fabric, which is connected to the electrode, by immersing the end portion of the edge of the SiC fiber fabric in a conductive composition in which the carbon paste is diluted 10 times with acetone, So that the conductive material can penetrate evenly to the inside, and as a result, the resistance between the electrodes and the SiC fibers, and furthermore, the resistance between the SiC fibers decreases.

As shown in FIG. 3, when the conductive paste was applied to the edge of the SiC fabric and coated with the Ti 3 SiC 2 suspension composition of Example 2 at an applied voltage of 10 V for 2 hours, the uniformity of the Ti 3 SiC 2 coating of the SiC fabric Was significantly improved. It was also confirmed that the coating uniformity for each SiC fiber in the SiC fabric was also improved.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, It will be obvious to those of ordinary skill in the art.

National R & D project supporting this invention

Assignment number: 2015M2A8A4001841

Department: Future Creation Science Division

Research Management Institution: Korea Research Foundation

Research Project Name: Nuclear R & D Project

Research title: Development of SiC composite for extreme environments

Contribution rate: 100%

Organization: Korea Atomic Energy Research Institute

Research period: 2015.3.1 ~ 2016.2.2.29

Claims (18)

Ti 3 SiC 2 A powder, a dispersing agent and a residual solvent,
The solvent is selected from the group consisting of Ti 3 SiC 2 ≪ / RTI >
The method of claim 1, wherein the Ti 3 SiC 2 The average particle diameter of the powder is not more than 1 占 퐉, Ti 3 SiC 2 ≪ / RTI >
The method of claim 1, wherein the dispersant is at least one component selected from the group consisting of nonionic surfactants comprising polyethyleneimine (PEI), polyethylene oxide (PEO), and polyethylene glycol (PEG). Ti 3 SiC 2 ≪ / RTI >
The method of claim 1, wherein the Ti 3 SiC 2 The powder was Ti 3 SiC 2 A coating composition comprising Ti 3 SiC 2 in an amount of 0.01 to 1% by weight, based on the total weight of the coating composition, ≪ / RTI >
The method of claim 1, wherein the dispersant is Ti 3 SiC 2 A coating composition comprising Ti 3 SiC 2 , which is contained in an amount of 0.1 to 1.5% by weight based on the total weight of the coating composition, ≪ / RTI >
The composition for coating a Ti 3 SiC 2 according to claim 1, wherein the solvent is ethanol: water in a weight ratio of 1: 0.5 to 1: 5.
The method of claim 1, wherein the dispersant and Ti 3 SiC 2 The powder was Ti 3 SiC 2 Powder: dispersant = Ti 3 SiC 2 ≪ / RTI >
The method of claim 1, wherein the Ti 3 SiC 2 The pH of the coating composition is 2 to 9.4 Ti 3 SiC 2 ≪ / RTI >
The method of claim 1, wherein the Ti 3 SiC 2 The composition for coating further comprises at least one binder selected from the group consisting of polyvinyl butyral (PVB), polycarbosilane (PCS) and polyvinyl alcohol (PVA), Ti 3 SiC 2 ≪ / RTI >
The method of claim 9, wherein the binder is Ti 3 SiC 2 A coating composition comprising 0.01 to 5% by weight, based on the total weight of the coating composition, of Ti 3 SiC 2 ≪ / RTI >
Providing SiC fibers connected to the cathode;
Providing a positive electrode spaced from the SiC fiber; And
A composition comprising the Ti 3 SiC 2 of any one of claims 1 to 10 Electrophoresis using a coating composition
Of, SiC fiber, which comprises a Ti 3 SiC 2 Coating method.
12. The method of claim 11, wherein the SiC fibers are of, SiC fibers in a SiC provided a fabric woven with SiC fiber bundles Ti 3 SiC 2 Coating method.
According to claim 11, wherein an average diameter of 4 to 50 μm of the SiC fibers, Ti 3 SiC of the SiC fiber bundle has an average thickness of 50 to 500 μm, SiC fibers 2 Coating method
According to claim 11, wherein the positive electrode is Ti 3 SiC of, SiC fibers of two anodes arranged and spaced in parallel with the SiC fiber 2 Coating method
According to claim 11, wherein the electrophoresis is greater than 5 V, SiC fibers is carried out for a period of less than 1 hour 3 hours under an applied voltage of less than 20V Ti 3 SiC 2 Coating method.
12. The method of claim 11 wherein the ratio of the applied voltage (V) for a distance (d) of the SiC fiber and the positive (V / d) is 2.5 to 10 V / cm is, the SiC fiber Ti 3 SiC 2 Coating method.
12. The method of claim 11, further comprising treating the edges of the SiC fibers with a conductive paste, wherein the SiC fiber's Ti 3 SiC 2 Coating method.
According to claim 17, wherein the conductive paste is Ti 3 SiC of at least one of, SiC fiber is selected from the group consisting of carbon (carbon) paste, metal paste, and conductive epoxy paste 2 Coating method.
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CN114561680A (en) * 2022-03-21 2022-05-31 上海大学 Ti on metal bipolar plate3SiC2Preparation method of ceramic coating and metal bipolar plate

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FR2907117B1 (en) 2006-10-17 2010-09-24 Snecma Propulsion Solide PROCESS FOR MANUFACTURING A COMPOSITE MATERIAL PART WITH A CERAMIC MATRIX CONTAINING CRACKING MATRIX PHASES AND A CRACKING DEVIATOR
WO2011136136A1 (en) 2010-04-30 2011-11-03 独立行政法人物質・材料研究機構 Max-phase oriented ceramic and production method therefor

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KR20190085255A (en) * 2018-01-10 2019-07-18 영남대학교 산학협력단 Preparation method of Ti3AlC2 tape and the joining method of silicon carbide using the same
CN114561680A (en) * 2022-03-21 2022-05-31 上海大学 Ti on metal bipolar plate3SiC2Preparation method of ceramic coating and metal bipolar plate
CN114561680B (en) * 2022-03-21 2024-04-12 上海大学 Ti on metal bipolar plate 3 SiC 2 Preparation method of ceramic coating and metal bipolar plate

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