KR102397281B1 - Thermal adhesive composition capable of weight reduction and method for manufacturing the same - Google Patents

Abstract

Disclosed are a heat radiation adhesive composition capable of weight reduction and a method for manufacturing the same. A heat radiation adhesive composition capable of weight reduction according to one embodiment includes a main material including a binder resin, aluminum oxide, composite particles, and an additive, wherein composite particles may be prepared as particles in which aluminum hydroxide and aluminum oxide are bonded to each other.

Description

Heat dissipation adhesive composition capable of reducing weight and manufacturing method thereof

The present disclosure relates to a heat-dissipating adhesive composition capable of reducing weight and a method for manufacturing the same.

In recent years, electronic devices used in automobiles, electric/electronic fields, etc. are being pursued to be lightweight, ultra-thin, miniaturized, and multifunctional. These electronic devices generate more heat as they become highly integrated, and the emitted heat not only degrades the device's function, but also causes malfunctions of peripheral devices and substrate deterioration. Research is being done. In this regard, Korean Patent Registration No. 10-0307586 has a technology for a heat dissipation device for electronic products.

On the other hand, since the driving efficiency of an electric vehicle is improved as the weight is reduced, it is preferable that all parts applied to the electric vehicle be lightweight. It was on the high side with a score of 2.9 or higher.

If the content of the thermally conductive filler included in the heat dissipation composition is applied to 50% by weight or less to reduce the weight of the product, the specific gravity is adjusted to 2.0 or less and weight reduction is possible, but the thermal conductivity falls to 1W/mK or less there was Therefore, there is a demand for the development of a technology that can satisfy the weight reduction of the product while implementing the heat dissipation performance.

The technical idea of the present disclosure is to solve the above-described problems, and it is an object of the present disclosure to provide a technology capable of reducing the weight while implementing the heat dissipation performance of the product.

The problems to be solved by the present invention are not limited to the above problems, and other technical problems not mentioned will be clearly understood by those of ordinary skill in the art to which the present invention belongs from the following description.

In order to achieve this object, in one embodiment of the present invention, a lightweight heat dissipating adhesive composition is a binder resin, aluminum oxide, a subject including a composite particle and an additive; includes, wherein the composite particle is aluminum hydroxide and aluminum oxide It may be provided in the form of particles bonded to each other.

In addition, the composite particles may be provided in a structure in which aluminum oxide surrounds the surface of the aluminum hydroxide particles.

In addition, in the subject matter, the binder resin may be provided in an amount of 10-30 wt%, the aluminum oxide in an amount of 10-30 wt%, the composite particle in an amount of 15-30 wt%, and the additive in an amount of 10-40 wt%.

In addition, the binder resin may include at least one of a polyol, a silicone resin, an epoxy resin, and an acrylic resin.

In addition, the heat dissipation adhesive composition capable of reducing the weight further includes a curing agent, wherein the curing agent includes 10 to 30% by weight of a curing component causing a curing reaction with the binder resin; 10-30 wt% of aluminum oxide; 15-30 wt% of composite particles provided in a structure in which aluminum oxide surrounds the surface of aluminum hydroxide particles; and 10 to 40% by weight of additives.

In order to achieve this object, as another embodiment of the present invention, a method for preparing a light-weighted heat-dissipating adhesive composition includes: a subject preparation step of preparing a subject containing a binder resin, aluminum oxide, composite particles, and additives; and a curing agent preparation step of preparing a curing agent, wherein the composite particles may be prepared as particles in which aluminum hydroxide and aluminum oxide are combined with each other.

And, the preparation of the subject includes a composite particle manufacturing step of preparing the composite particles, wherein the composite particle manufacturing step includes an application step of applying aluminum hydroxide in a tray; While the tray is disposed on the metal belt, the metal belt is moved in one direction, and while the tray is moving, heat is applied to the aluminum hydroxide to form composite particles in the form of an aluminum oxide layer formed on the surface of the aluminum hydroxide composite particle formation step; a cooling step of cooling the composite particles; and a particle separation step of applying a physical impact to the composite particles adhering to each other to separate them into individual pieces.

In addition, in the composite particle forming step, the tray disposed on the metal belt passes through the inside of the heating unit and is heated by the heat source of the heating unit, and the heating unit is divided into first, second, and third areas in units of 1 meter. , a fourth region, a fifth region, a sixth region, and a seventh region, wherein the temperature is maintained at 300° C. in the first region, the temperature is maintained at 600° C. in the second region, and the third region The temperature is maintained at 1000°C in the region and the fourth region, the temperature is maintained at 600°C in the fifth region, and the temperature is maintained at 300°C in the sixth region and the seventh region, and the moving speed of the metal belt is It is maintained at 1 meter per minute, and argon or nitrogen gas may be supplied to the inside of the heating unit at a supply rate of 20 LPM.

In addition, the composite particle manufacturing step further includes a layer thickness control step of adjusting the thickness of the aluminum oxide layer formed on the composite particle; in the layer thickness control step, the tray disposed on the metal belt is the first region, It passes through the second region, the third region, the fourth region, the fifth region, the sixth region, and the seventh region, and the temperature is maintained at 300° C. in the first region, and the second region, the third region and the third region In region 4, the temperature is maintained at 700°C, in the fifth region, the temperature is maintained at 300°C, in the sixth and seventh regions, the temperature is maintained at 25°C, and the moving speed of the metal belt is 1 per minute It is maintained by a meter, and argon or nitrogen gas may be supplied to the inside of the heating unit at a supply rate of 20 LPM.

In addition, the step of preparing the subject matter may further include a stirring step of stirring the binder resin, aluminum oxide, composite particles, and additives.

The means for solving the above-described problems are merely exemplary, and should not be construed as limiting the present invention. In addition to the exemplary embodiments described above, there may be additional embodiments described in the drawings and detailed description.

As described above, according to various embodiments of the present invention, there is an advantage in that the heat dissipation performance of the product to which the heat dissipation adhesive composition is applied is excellent, as well as the weight reduction of the product.

Effects of the present invention are not limited to the effects mentioned above, and other effects not mentioned will be clearly understood by those skilled in the art from the description of the claims.

1 is a flowchart illustrating a method of manufacturing a heat dissipation adhesive composition according to an embodiment of the present invention.
2 is a flowchart illustrating detailed steps of a composite particle manufacturing step according to an embodiment of the present invention.

A preferred embodiment of the present invention will be described in more detail with reference to the accompanying drawings, but already known technical parts will be omitted or compressed for the sake of brevity of description.

It should be noted that references to "one" or "an" embodiment of the invention herein are not necessarily to the same embodiment, and they mean at least one.

In the following examples, the singular expression includes the plural expression unless the context clearly dictates otherwise.

In the following embodiments, terms such as include or have means that the features or components described in the specification are present, and the possibility that one or more other features or components may be added is not excluded in advance.

In cases where certain embodiments may be implemented otherwise, a specific process sequence may be performed different from the described sequence. For example, two processes described in succession may be performed substantially simultaneously, or may be performed in an order opposite to the order described. That is, each step of the method described herein may be appropriately performed in any order unless otherwise stated in the specification or clearly contradicted by context.

As used herein, the term 'specific gravity' refers to the ratio of the mass of a substance to the mass of a standard of the same volume. In one embodiment, the specific gravity is obtained by dividing the density of a specific material by the density of water in a state of 4°C and 1 atm.

<Description of the heat dissipation adhesive composition capable of being lightweight>

The heat dissipation adhesive composition capable of being lightweight according to an embodiment of the present invention may include a main agent and a curing agent. In one embodiment, the subject may include a binder resin, aluminum oxide, composite particles, and additives.

According to one embodiment, the binder resin may be applied to at least one of polyol, silicone resin, epoxy resin, and acrylic resin. For example, the binder resin may be applied as polycaprolactone polyol, diethylene glycol, dipropylene glycol, polyethylene glycol, 2-hydroxypropyl acrylate or 2-hydroxyethyl methacrylate.

In one embodiment, examples of commercially available binder resins may include CAPA-2043 of First Top, but is not limited thereto.

The content of the binder resin according to an embodiment may be applied in an amount of 10 to 30% by weight. As a specific example, the content of the binder resin is 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, 15 wt%, 16 wt%, 17 wt%, 18 wt%, 19 wt%, 20 wt% %, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29% or 30% by weight. In addition, the content of the binder resin may be in the range of at least one of the above numerical values and less than or equal to one of the above numerical values.

For example, the content range of the binder resin may be provided in a range of 10 wt% to 20 wt%, 15 wt% to 25 wt%, 20 wt% to 30 wt%, or 10 wt% to 30 wt%.

In one embodiment, the content of aluminum oxide may be applied to 10 to 30% by weight. As a specific example, the content of aluminum oxide is 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, 15 wt%, 16 wt%, 17 wt%, 18 wt%, 19 wt%, 20 wt% %, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29% or 30% by weight. In addition, the content of aluminum oxide may be in the range of at least one of the above values and less than or equal to one of the above values.

For example, the content range of aluminum oxide is 10% to 15% by weight, 12% to 17% by weight, 14% to 19% by weight, 15% to 20% by weight, 20% to 30% by weight or It may be provided in the range of 10 wt% to 30 wt%. Aluminum oxide according to an embodiment may maintain weight reduction and heat dissipation performance at an excellent level within the above range.

If the amount of aluminum oxide is less than 10% by weight, there is a risk that the thermal conductivity is lowered and the heat dissipation performance is lowered. It is preferable to be carried out within the range.

In an embodiment, the composite particles may be prepared as particles in which aluminum hydroxide and aluminum oxide are combined with each other. Specifically, the composite particles may be formed in a structure in which aluminum oxide surrounds the surface of the aluminum hydroxide particles.

In an embodiment, the average particle diameter of the composite particles may be 50 to 100 μm. As a specific example, the average particle diameter of the composite particles may be 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, or 100 μm. In addition, the average particle diameter of the composite particles may be in the range of at least one of the above numerical values and less than or equal to one of the above numerical values.

For example, the average particle diameter of the composite particles may be in the range of 50 μm to 70 μm, 60 μm to 80 μm, 70 μm to 100 μm, or 50 μm to 100 μm. The composite particle according to an embodiment may maintain weight reduction and heat dissipation performance at an excellent level within the above range.

If the average particle diameter of the composite particles is less than 50 μm, the viscosity of the adhesive composition increases and flowability is lowered, which may negatively affect the physical properties of the coating film, and if it exceeds 100 μm, the viscosity of the adhesive composition decreases and thixotropic As the (Thixotropic) property is lowered, the shape-retaining property is deteriorated after application of the adhesive, which may negatively affect the physical properties of the coating film. In an embodiment, the average particle diameter of the composite particles may be analyzed by a particle size analyzer (eg, Melvern Mastersizer 2000E) using a laser diffraction technique.

According to one embodiment, the content of the composite particles may be applied to 15 to 30% by weight. As a specific example, the content of the composite particles may be 15 wt%, 16 wt%, 17 wt%, 18 wt%, 19 wt%, 20 wt%, 21 wt%, 22 wt%, 23 wt%, 24 wt%, 25 wt% %, 26%, 27%, 28%, 29% or 30% by weight. Also, the content of the composite particles may be in the range of at least one of the above values and less than or equal to one of the above values.

For example, the content range of the composite particles may be provided in a range of 15 wt% to 20 wt%, 20 wt% to 25 wt%, 25 wt% to 30 wt%, or 15 wt% to 30 wt%. The composite particle according to an embodiment may maintain weight reduction and heat dissipation performance at an excellent level within the above range.

If the amount of the composite particles is less than 15% by weight, there is a risk that the heat dissipation performance may be lowered, and if it exceeds 30% by weight, the specific gravity increases and it is difficult to realize weight reduction. Therefore, the content of the composite particles is carried out within the above range It is preferable to be

Meanwhile, in one embodiment, the additive may include a dispersible additive and a flame retardant additive, and the content of the additive may include 10 to 40% by weight, but the content of the additive may be adjusted as necessary.

In one embodiment, the curing agent may include a curing component, aluminum oxide, composite particles, and additives. Here, the curing component causes a curing reaction with the binder resin, and in one embodiment, when the binder resin is applied as a polyol (eg, dipropylene glycol, polyethylene glycol, etc.), the curing component is an isocyanate compound (eg, polymeric) methylenediphenyl isocyanate, monomeric methylenediphenyl isocyanate, hexamethylene diisocyanate, etc.), and in another embodiment when the binder resin is applied as an acrylate (e.g. 2-hydroxypropyl acrylate, etc.) cures The component can be applied such as 4-hydroxydimethylacetophenone.

In one embodiment, the content of the curing component may be applied to 10 to 30% by weight. As a specific example, the content of the curing component is 10% by weight, 11% by weight, 12% by weight, 13% by weight, 14% by weight, 15% by weight, 16% by weight, 17% by weight, 18% by weight, 19% by weight, 20% by weight. %, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29% or 30% by weight. In addition, the content of the curing component may be in the range of at least one of the above values and less than or equal to one of the above values.

For example, the content range of the curing component may be provided in a range of 10 wt% to 20 wt%, 15 wt% to 25 wt%, 20 wt% to 30 wt%, or 10 wt% to 30 wt%.

In one embodiment, the content of aluminum oxide contained in the curing agent may be applied to 10 to 30% by weight. As a specific example, the content of aluminum oxide is 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, 15 wt%, 16 wt%, 17 wt%, 18 wt%, 19 wt%, 20 wt% %, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29% or 30% by weight. In addition, the content of aluminum oxide may be in the range of at least one of the above values and less than or equal to one of the above values.

For example, the content range of aluminum oxide is 10% to 15% by weight, 12% to 17% by weight, 14% to 19% by weight, 15% to 20% by weight, 20% to 30% by weight or It may be provided in the range of 10 wt% to 30 wt%. Aluminum oxide according to an embodiment may maintain weight reduction and heat dissipation performance at an excellent level within the above range.

If the amount of aluminum oxide is less than 10% by weight, there is a fear that the thermal conductivity is lowered and the heat dissipation performance is lowered. It is preferably carried out within the above-described range.

In one embodiment, the composite particles included in the curing agent may be formed in a structure in which aluminum oxide surrounds the surface of the aluminum hydroxide particles.

According to one embodiment, the content of the composite particles included in the curing agent may be applied to 15 to 30% by weight. As a specific example, the content of the composite particles may be 15 wt%, 16 wt%, 17 wt%, 18 wt%, 19 wt%, 20 wt%, 21 wt%, 22 wt%, 23 wt%, 24 wt%, 25 wt% %, 26%, 27%, 28%, 29% or 30% by weight. Also, the content of the composite particles may be in the range of at least one of the above values and less than or equal to one of the above values.

For example, the content range of the composite particles may be provided in a range of 15 wt% to 20 wt%, 20 wt% to 25 wt%, 25 wt% to 30 wt%, or 15 wt% to 30 wt%. The composite particle according to an exemplary embodiment may have excellent heat resistance and moisture resistance within the above range, and may maintain weight reduction and heat dissipation performance at an excellent level.

If the composite particle is less than 15% by weight, there is a risk that the heat dissipation performance may be lowered, and if it exceeds 30% by weight, the specific gravity of the adhesive increases when the curing agent is mixed with the main agent, so that it is difficult to realize weight reduction. The content is preferably carried out within the above-mentioned range.

In one embodiment, the content of the additive included in the curing agent may be applied in an amount of 10 to 40% by weight, but the content of the additive may be adjusted as necessary. In addition, the additive in the curing agent may include a dispersible additive and a flame retardant additive.

<Description of the manufacturing method of the heat-dissipating adhesive composition capable of being lightweight>

A method of manufacturing a heat dissipation adhesive composition according to an embodiment of the present invention will be described according to the flowcharts shown in FIGS. 1 and 2 , but for convenience, they will be described in order.

1. Topic preparation step <S101>

In this step, a process of preparing a subject including binder resin, aluminum oxide, composite particles, and additives may be performed. According to an embodiment, the step of preparing the subject may include a step of preparing the composite particles and a step of stirring.

1-1. Composite particle manufacturing step <S1011>

In this step, a process of manufacturing composite particles to be included in the subject matter may be performed. Here, the composite particles are particles in which aluminum hydroxide and aluminum oxide are combined with each other, and the aluminum hydroxide particles may be transformed into composite particles by a series of special processes. The manufacturing of the composite particles according to an embodiment may include an application step, a composite particle formation step, a cooling step, a particle separation step, and a layer thickness control step.

1-1A. Application step <S10111>

In this step, aluminum hydroxide may be applied to a certain thickness (eg, 3 mm) in a heat-resistant tray. The aluminum hydroxide input to the tray in this step may be aluminum hydroxide powder, or a slurry in which aluminum hydroxide and a solvent (eg, caustic soda solution) are mixed.

1-1B. Composite particle formation step <S10112>

In this step, the tray is placed on the metal belt, and the metal belt is moved in one direction, but heat can be applied to the aluminum hydroxide in the tray while the tray is moving. In this step, through the process of applying heat to the aluminum hydroxide, composite particles in the form of an aluminum oxide layer formed on the surface of the aluminum hydroxide can be made.

According to one embodiment, the tray may move in one direction along the metal belt, and may be heated by the heat source of the heating unit while passing through the inside of the heating unit (eg, infrared oven) provided with the heat source. In one embodiment, the heating unit may include a first area, a second area, a third area, a fourth area, a fifth area, a sixth area, and a seventh area divided in units of 1 meter, each area The temperature conditions may be set differently. In addition, the first to seventh regions may be sequentially arranged along the moving direction of the belt.

According to one embodiment, the temperature is maintained at 300°C in the first region of the heating unit, the temperature is maintained at 600°C in the second region, and the temperature is maintained at 1000°C in the third and fourth regions, and the fifth The temperature may be maintained at 600° C. in the region, and the temperature may be maintained at 300° C. in the sixth and seventh regions. According to one embodiment, defects due to thermal expansion in the manufacture of composite particles can be minimized by heating the tray stepwise, raising the temperature to 1000° C., and cooling stepwise.

In one embodiment, since the moving speed of the metal belt is maintained at 1 meter per minute, the time for the tray to pass through each area of the heating unit may be applied as 1 minute per each area. If the time the tray passes through each region of the heating unit is less than 1 minute, the smooth formation of aluminum oxide on the surface of the aluminum hydroxide may be limited, and if it exceeds 1 minute, the entire aluminum hydroxide particles are converted to aluminum oxide. Composite particles can be tricky to implement.

In one embodiment, argon or nitrogen gas may be supplied to the inside of the heating unit at a supply rate of 20 LPM (liter per minute). Formation of composite particles may be limited if the feed rate of the inert gas is less than or greater than 20 LPM.

1-1C. Cooling step <S10113>

In this step, the composite particles prepared in step S10112 may be cooled. According to an embodiment, in this step, the tray may be cooled at room temperature (eg, 25° C.) for a predetermined time.

1-1D. Particle separation step <S10114>

In this step, the composite particles adhering to each other can be separated into individual particles by applying a physical impact. In one embodiment, the composite particles may be separated into each other by injecting the composite particles into the air jet mill equipment and spraying compressed air of 1 to 10 bar.

1-1E. Layer thickness adjustment step <S10115>

In this step, the thickness of the aluminum oxide layer formed on the composite particles can be adjusted. That is, the thickness of the aluminum oxide layer formed on the surface of the aluminum hydroxide can be adjusted to a desired level by controlling the time for applying heat at a constant temperature to the aluminum hydroxide particles.

In one embodiment, the tray disposed on the metal belt moving in one direction sequentially passes through the first region, the second region, the third region, the fourth region, the fifth region, the sixth region, and the seventh region. can At this time, the temperature is maintained at 300° C. in the first region, the temperature is maintained at 700° C. in the second, third, and fourth regions, and the temperature is maintained at 300° C. in the fifth region, and the sixth region and In the seventh region, the temperature may be maintained at room temperature (eg, 25° C.).

In one embodiment, the moving speed of the metal belt is maintained at 1 meter per minute, and argon or nitrogen gas may be supplied to the inside of the heating unit at a supply rate of 20 LPM. The final thickness of the aluminum oxide layer formed on the composite particles through this step may be 1 to 5 μm.

1-2. Stirring step <S1012>

In this step, the binder resin, aluminum oxide, composite particles and additives may be stirred. In one embodiment, the binder resin, the catalyst, and the dispersible additive may be mixed and the first stirred product may be prepared by first stirring at 500 RPM for 10 minutes. After that, the flame-retardant additive, aluminum oxide and composite particles are added into the primary agitation, and the secondary agitation can be made by second stirring at 800 RPM for 30 minutes. And, while stirring the secondary stirred material at 1000RPM at high speed, it can be defoamed for 60 minutes.

2. Curing agent preparation step <S102>

In this step, a process of preparing a curing agent may be performed. For example, in this step, the curing agent may be prepared by stirring the curing component, aluminum oxide, composite particles, and additives. In one embodiment, the first stirring may be made by mixing the curing component and the dispersible additive and first stirring at 500 RPM for 10 minutes. After that, the flame-retardant additive, aluminum oxide and composite particles are added into the primary agitation, and the secondary agitation can be made by second stirring at 800 RPM for 30 minutes. And, while stirring the secondary stirred material at 1000RPM at high speed, it can be defoamed for 60 minutes.

Hereinafter, the present invention will be described in more detail through specific examples and experimental examples. Since the following Examples and Experimental Examples are merely examples to help the understanding of the present invention, the scope of the present invention is not limited or limited thereto.

Preparation of heat dissipating adhesive composition

<Examples 1-3 and Comparative Examples 1-2>

In a heat-resistant tray, aluminum hydroxide powder with an average particle diameter of 50 to 100 μm is applied to a thickness of 3 mm, a tray containing aluminum hydroxide powder is placed on a metal belt, and the tray is heated while maintaining the moving speed of the metal belt at 1 meter per minute moved in the negative direction. The heating unit is subdivided into 1st area, 2nd area, 3rd area, 4th area, 5th area, 6th area, and 7th area divided by 1 meter unit. The temperature is maintained at 600°C in the second region, the temperature is maintained at 1000°C in the third and fourth regions, the temperature is maintained at 600°C in the fifth region, and the sixth and seventh regions In the furnace, the temperature was maintained at 300 °C, and argon gas was supplied to the inside of the heating unit at a supply rate of 20 LPM. After that, the tray is cooled at room temperature (for example, 25° C.) for 2 hours, the cooled composite particles are put into the air jet mill equipment, and compressed air of 1 to 10 bar is sprayed to separate the composite particles attached to each other. separated. Then, the composite particles were put back into the tray, and the tray was passed through the inside of the heating unit using a metal belt maintaining a moving speed of 1 meter per minute. That is, the tray sequentially passed through the first region, the second region, the third region, the fourth region, the fifth region, the sixth region, and the seventh region of the heating unit, and the temperature was maintained at 300°C in the first region, , the temperature was maintained at 700 °C in the second, third and fourth regions, the temperature was maintained at 300 °C in the fifth region, and the temperature was maintained at 25 °C in the sixth and seventh regions, and heating Argon gas was supplied to the inside of the part at a feed rate of 20 LPM to complete the manufacture of the composite particles.

After that, the binder resin and the dispersible additive are mixed and the first stirred product is made by first stirring at 500 RPM for 10 minutes, then the flame retardant additive, aluminum oxide and composite particles are put in the first stirring material, and the second time at 800 RPM for 30 minutes A secondary stirred product was prepared by stirring, and the secondary stirred product was defoamed for 60 minutes while stirring at a high speed at 1000 RPM to complete the preparation of the main agent.

To prepare a curing agent, a curing component and a dispersible additive are mixed, and a primary stirring is made by first stirring at 500 RPM for 10 minutes, and then, a flame retardant additive, aluminum oxide and composite particles are put in the first stirring, and then, at 800 RPM for 30 minutes Secondary stirring was performed to make a secondary stirred material, and the secondary stirred material was defoamed for 60 minutes while stirring at a high speed at 1000RPM to complete the preparation of the curing agent. The contents of each component added during stirring of the main agent and the contents of each component added during stirring of the curing agent are as described in Table 1.

division Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 subject ¹ binder resin 30 30 30 30 25 ² aluminum oxide 10 20 30 0 40 ³ Composite Particles 30 30 30 30 25 ⁴ Dispersible Additives 15 10 5 20 5 ⁵ Flame Retardant Additives 15 10 5 20 5 hardener ⁶ hardening ingredients 30 30 30 30 25 ² aluminum oxide 10 20 30 0 40 ³ Composite Particles 30 30 30 30 25 ⁴ Dispersible Additives 15 10 5 20 5 ⁵ Flame Retardant Additives 15 10 5 20 5 main)
1: Binder resin - CAPA-2043 (Perstop Corporation)
2: Aluminum oxide - SPA-70 (CMP)
3: Composite particles (CK EM solution)
4: Dispersible additive - BYK-2152 (BYK)
5: Flame retardant additive - PNF-100R (Universal Chemtech)
6: Curing component - hexamethylene diisocyanate (Wanhua)

<Examples 4-7 and Comparative Examples 3-4>

The content of each component added during stirring of the main agent and the content of each component added during stirring of the curing agent were applied as described in Table 2, and the rest of the conditions were set the same as in Example 1 to prepare the subject and curing agent.

division Example 4 Example 5 Example 6 Example 7 Comparative Example 3 Comparative Example 4 subject ¹ binder resin 30 30 30 30 30 25 ² aluminum oxide 30 30 30 30 30 30 ³ Composite Particles 15 20 25 30 10 35 ⁴ Dispersible Additives 12.5 10 7.5 5 15 5 ⁵ Flame Retardant Additives 12.5 10 7.5 5 15 5 hardener ⁶ hardening ingredients 30 30 30 30 30 25 ² aluminum oxide 30 30 30 30 30 30 ³ Composite Particles 15 20 25 30 10 35 ⁴ Dispersible Additives 12.5 10 7.5 5 15 5 ⁵ Flame Retardant Additives 12.5 10 7.5 5 15 5 main)
1: Binder resin - CAPA-2043 (Perstop Corporation)
2: Aluminum oxide - SPA-70 (CMP)
3: Composite particles (CK EM solution)
4: Dispersible additive - BYK-2152 (BYK)
5: Flame retardant additive - PNF-100R (Universal Chemtech)
6: Curing component - hexamethylene diisocyanate (Wanhua)

Test and evaluation methods

Experimental environment conditions

The experimental environment, that is, the place where the experiment is conducted, is a place where there is no direct sunlight and very little gas, steam, dust and ventilation at a temperature of 20±2℃ and a humidity of 65±5% (hereinafter referred to as ‘room temperature’). proceeded.

specific gravity measurement

After putting the subject and curing agent of each Example and Comparative Example into a two-component ejector and mixing them, apply them on a PET film under the conditions of a length of 5mm, a width of 5mm, and a thickness of 5mm, and after preparing a specimen cured at room temperature for 48 hours, specific gravity measurement The specific gravity of the specimen was measured using the equipment (Mirage's SD-200L). The measured results are as described in Tables 3 and 4.

Thermal conductivity measurement

After putting the subject and curing agent of each Example and Comparative Example into a two-component ejector and mixing them, they were applied on a PET film under the conditions of a length of 50 mm, a width of 50 mm, and a thickness of 5 mm. After preparing a specimen cured at room temperature for 48 hours, thermal conductivity The thermal conductivity (unit: W/mK) of the specimen was measured using a measuring device (Hotdisk's TPS-3500). The measured results are as described in Tables 3 and 4.

Shear strength measurement

After putting the main agent and curing agent of each Example and Comparative Example into a two-component ejector and mixing them, they are coated on a steel panel with a length of 25.4 mm, a width of 25.4 mm, and a thickness of 0.3 mm, and then a separate steel panel is laminated and attached thereon. After preparing a specimen hardened at room temperature for 48 hours, the shear strength was measured according to ASTM D 1002. Pull and measure the dynamic shear strength (unit: MPa). The measured results are as described in Tables 3 and 4.

Adhesion measurement

After putting the subject and curing agent of each Example and Comparative Example into a two-component ejector and mixing them, they were applied on a steel panel under the conditions of 125 mm in length, 10 mm in width, and 0.3 mm in thickness, and then a separate PET film was laminated and attached thereon. After preparing a dried specimen by curing at room temperature for 48 hours, the peel strength (unit: gf/cm) was measured according to ASTM D 3330 using a universal tester, but the evaluation speed when measuring the peel strength was 300 mm/min. . The measured results are as described in Tables 3 and 4.

hardness measurement

After putting the subject and curing agent of each Example and Comparative Example into a two-component ejector and mixing them, using a jig to apply under the conditions of a thickness of 10 mm and a diameter of 25 mm, and curing at room temperature for 48 hours to prepare a dried specimen, Shore hardness The hardness of the coating film was evaluated by measuring the Shore D hardness of each specimen according to ISO 868 using a shore hardness tester. The measured results are as described in Tables 3 and 4.

Heat resistance and moisture resistance measurement

Except for putting the specimen in a chamber with a temperature of 85° C. and a relative humidity of 85%, and measuring the shear strength, adhesion and hardness of the specimen after 1000 hours, the method for preparing and measuring each specimen is the shear strength, adhesive force described above. And the hardness measurement method was performed in the same way, and the resultant value measured after placing the specimen in the chamber and the result value measured before placing the specimen in the chamber were compared, and the rate of change derived by deriving the rate of change according to Equation 1 below was 5% In the case of the following, it was evaluated that the heat resistance and moisture resistance were excellent, and when it exceeded 5%, the heat resistance and moisture resistance were evaluated as poor. The measured results are as described in Tables 3 and 4.

[Equation 1]

Rate of change = (Measured before placing the specimen in the chamber - Measured after placing the specimen in the chamber) / Measured before placing the specimen in the chamber * 100%

division Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 importance 1.88 1.93 1.97 1.81 2.2 thermal conductivity 1.21 1.33 1.45 0.89 1.44 shear strength 10.5 10.8 11 9.5 11 adhesion 2610 2500 2350 2850 1980 Hardness 60 63 65 45 75 Heat and moisture resistance Great Great Great Great Great

As shown in Table 3, it can be confirmed that Examples 1 to 3 of the present invention are at an overall excellent level in terms of specific gravity, thermal conductivity, shear strength, adhesion, hardness, heat resistance and moisture resistance, whereas Comparative Examples 1 to 2 Through the experimental results, when the content of aluminum oxide contained in the adhesive composition exceeds or is less than the input amount range, it can be confirmed that the decrease in physical properties occurs relatively compared to the Examples.

division Example 4 Example 5 Example 6 Example 7 Comparative Example 3 Comparative Example 4 importance 1.83 1.95 1.97 1.98 1.81 2.18 thermal conductivity 1.21 1.32 1.43 1.54 0.95 1.58 shear strength 10.8 11.2 11.8 11.4 9.2 11.9 adhesion 2230 2490 2510 2480 1950 2520 Hardness 63 63 65 66 49 66 Heat and moisture resistance Great Great Great Great Great Great

As shown in Table 4, it can be seen that Examples 4 to 7 of the present invention are at an overall excellent level in terms of specific gravity, thermal conductivity, shear strength, adhesion, hardness, heat resistance and moisture resistance, whereas Comparative Examples 3 to 4 Through the experimental results, when the content of the composite particles included in the adhesive composition exceeds or is less than the input amount range, it can be confirmed that the decrease in physical properties occurs relatively compared to the Examples.

As described above, according to various embodiments of the present invention, there is an advantage in that the heat dissipation performance of the product to which the heat dissipation adhesive composition is applied (eg, a battery for an electric vehicle) is excellent, and the weight of the product can be reduced.

In addition, according to various embodiments of the present invention, it is possible to implement a core-shell structure without a separate adhesive or adhesive layer between the aluminum hydroxide and the aluminum oxide in the composite particles, and the aluminum hydroxide and aluminum oxide are combined in the composite particles. Since an adhesive is not used for this purpose, it is easier to control the average particle diameter of the composite particles compared to a technique for bonding aluminum hydroxide and aluminum oxide using an adhesive, and costs can be reduced.

And, according to various embodiments of the present invention, when the main agent and the curing agent are mixed, the filler component (aluminum oxide, composite particles) of the main agent and the filler component (aluminum oxide, composite particles) of the curing agent are set in a weight ratio of 1:1, The specific gravity of the main agent and the curing agent is the same, the viscosity of the adhesive composition can be easily controlled, the mixing is smooth, so that the application is easy, and the content can be prevented from settling after application.

In addition, according to various embodiments of the present invention, as the aluminum hydroxide particles move in one direction along the metal belt and are heated step by step to form composite particles, a continuous process is possible compared to a heating method by a general furnace, so that the composite particles mass production is made quickly, and defects of particles due to thermal expansion can be minimized by performing a step-by-step temperature increase and cooling process.

As described above, the detailed description of the present invention has been made by way of examples, but since the above-described exemplary embodiments have only been described with preferred examples of the present invention, it should not be understood that the present invention is limited only to the above examples. No, the scope of the present invention should be understood as the following claims and their equivalents.

Claims (10)

delete delete delete delete delete A subject preparation step of preparing a subject containing a binder resin, aluminum oxide, composite particles and additives; and
Including; a curing agent preparation step of preparing a curing agent;
The composite particles are prepared in the form of particles in which aluminum hydroxide and aluminum oxide are combined with each other,
The topic preparation step is
Including; a composite particle manufacturing step of preparing the composite particle;
The composite particle manufacturing step is
Application step of applying aluminum hydroxide in the tray;
While the tray is disposed on the metal belt, the metal belt is moved in one direction, and while the tray is moving, heat is applied to the aluminum hydroxide to form composite particles in the form of an aluminum oxide layer formed on the surface of the aluminum hydroxide composite particle formation step;
a cooling step of cooling the composite particles; and
Including; a particle separation step of separating into individual particles by applying a physical impact to the composite particles adhering to each other;
In the composite particle forming step, the tray disposed on the metal belt is heated by the heat source of the heating unit while passing through the inside of the heating unit, and the heating unit includes a first area, a second area, a third area divided by 1 meter; It includes a fourth region, a fifth region, a sixth region, and a seventh region, wherein the temperature is maintained at 300°C in the first region, and the temperature is maintained at 600°C in the second region, and the third region and The temperature is maintained at 1000°C in the fourth region, the temperature is maintained at 600°C in the fifth region, and the temperature is maintained at 300°C in the sixth and seventh regions, and the moving speed of the metal belt is It is maintained at 1 meter, and argon or nitrogen gas is supplied to the inside of the heating unit at a supply rate of 20 LPM,
The composite particle manufacturing step is
A layer thickness control step of controlling the thickness of the aluminum oxide layer formed on the composite particles; further comprising,
In the layer thickness adjustment step, the tray disposed on the metal belt passes through the first region, the second region, the third region, the fourth region, the fifth region, the sixth region, and the seventh region, and the first region The temperature is maintained at 300°C in the second region, the third region, and the fourth region is maintained at 700°C, the temperature is maintained at 300°C in the fifth region, and the sixth and seventh regions In the region, the temperature is maintained at 25° C., the moving speed of the metal belt is maintained at 1 meter per minute, and argon or nitrogen gas is supplied to the inside of the heating unit at a supply rate of 20 LPM.
A method of manufacturing a heat-dissipating adhesive composition capable of reducing weight. delete delete delete 7. The method of claim 6,
The topic preparation step is
A stirring step of stirring the binder resin, aluminum oxide, composite particles and additives; characterized in that it further comprises
A method of manufacturing a heat-dissipating adhesive composition capable of reducing weight.

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