US20230070481A1

US20230070481A1 - Method for preparing heat dissipation component with high flexibility made of graphite or graphene material

Info

Publication number: US20230070481A1
Application number: US17/448,049
Authority: US
Inventors: Meixing Pang
Original assignee: Suzhou Ontap Precision Electronic Co Ltd
Current assignee: Suzhou Ontap Precision Electronic Co Ltd
Priority date: 2021-09-08
Filing date: 2021-09-18
Publication date: 2023-03-09
Also published as: JP2023039376A; TW202311157A; EP4148165A1; KR102631465B1; TWI777783B; JP7187069B1; CN113622007A; EP4148165B1; KR20230036941A

Abstract

The present disclosure disclose a method for preparing a heat dissipation component with high flexibility made of graphite or a graphene material, which includes that follow steps: 1) plasma cleaning a graphite or graphene raw material; 2) taking preparation materials of an activator; 3) continually cleaning the graphite or graphene raw material with the activator; 4) cleaning the graphite or graphene raw material with deionized water; 5) conducting a electroplating process on a surface of the graphite or graphene raw material to form a copper film layer; 6) continually cleaning the graphite or graphene raw material; 7) forming a protective film on the graphite or graphene raw material by soaking; 8) drying the graphite or graphene raw material electroplated with the copper film layer. The surface of graphite or graphene treated with the activator has a uniform copper film layer with good binding quality during electroplating.

Description

TECHNICAL FIELD

The present disclosure belong to the field of preparation of parts made of a graphite or graphene material, and particularly relate to a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material.

BACKGROUND

Graphite is a two-dimensional carbon nanomaterial presented with hexagonal honeycomb lattices and composed of carbon atoms in sp2 hybrid orbitals. Graphite has a very good thermal conduction performance. The pure and defect-free single-layer graphite has thermal conductivity up to 5300 W/mK, and is the carbon material with the highest thermal conductivity so far, and its thermal conductivity is higher than those of a single-walled carbon nanotube (3500 W/mK) and a multi-walled carbon nanotube (3000 W/mK). When it is used as a carrier, the thermal conductivity can also reach 600 W/MK. Furthermore, the ballistic thermal conductivity of graphite can lower the lower limit of the ballistic thermal conductivity of a carbon nanotube of unit circumference and length.
All kinds of electronic elements in electronic products need to dissipate heat. When traditional graphite or graphene is applied for heat dissipation of the electronic elements, it mainly fixes a metal layer on the surface of graphite or graphene, and in particular the metal layer is fixed onto graphite or graphene by bonding or electroplating, wherein electroplating is better than bonding in heat conduction efficiency.
In order to ensure the electroplating quality of the metal layer on the surface of graphite or graphene, it is usually necessary to subject the surface of graphite or graphene to multiple passes of cleaning processes before electroplating. During the cleaning process, after the surface of graphite or graphene is treated with an OP-10 surfactant, the smoothness of the surface of graphite or graphene is general, which leads to poor binding effect and uneven thickness of the metal layer electroplated on the surface of graphite or graphene, and thus affects the flexibility of the prepared heat dissipation component, and the surface of the heat dissipation component is easy to generate creases.

SUMMARY

An objective of the present disclosure is to provide a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material, which includes the following steps: firstly, plasma cleaning a surface of graphite or graphene, and then treating the surface of graphite or graphene with an activator compounded by sulfuric acid, an OP-10 surfactant and sodium dodecyl sulfate, so that the surface of the material has good smoothness, and it ensures a copper film layer electroplated on the surface of graphite or graphene has good binding quality and uniform, and enhances the flexibility of the prepared heat dissipation component, and the surface of the heat dissipation component is not easy to generate creases.
In order to achieve the aforementioned objective, the present disclosure adopts the following technical solution: a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material, including the following steps:
1) plasma cleaning a graphite or graphene raw material;
2) taking preparation materials of an activator including the following components in percentage by weight: 10-20% of sulfuric acid, 0.05-1% of an OP-10 surfactant, 0.05-1% of sodium dodecyl sulfate, and the balance of water;
3) mixing the aforementioned components of the activator to prepare the activator, and continually cleaning the graphite or graphene raw material with the activator;
4) continually cleaning the graphite or graphene raw material with deionized water;
5) conducting a electroplating process on a surface of the graphite or graphene raw material to form a copper film layer;
6) continually cleaning the graphite or graphene raw material electroplated with the copper film layer on the surface thereof with deionized water;
7) forming a protective film on the graphite or graphene raw material by soaking; and
8) drying the graphite or graphene raw material electroplated with the copper film layer.
As a further description of the aforementioned technical solution:
In the step 1), the graphite or graphene raw material is placed in a plasma cleaning machine for cleaning.
As a further description of the aforementioned technical solution:
In the step 2), the activator includes the following components in percentage by weight: 12-16% of sulfuric acid, 0.05-0.5% of an OP-10 surfactant, 0.05-0.5% of sodium dodecyl sulfate, and the balance of water.
As a further description of the aforementioned technical solution:
in the step 2), the activator includes the following components in percentage by weight: 15% sulfuric acid, 0.1% of the OP-10 surfactant, 0.1% of sodium dodecyl sulfate, and the balance of water.
As a further description of the aforementioned technical solution:
in the step 5), the graphite or graphene raw material is subjected to the electroplating process twice with an electroplating potion, and the electroplating potion includes the following components in percentage by weight: 5% of copper ions; 14% of sulfuric acid; 0.8% of a brightener; 0.06% of an adjuvant; 0.06% of a leveling agent; and the balance of water.
As a further description of the aforementioned technical solution:
when the graphite or graphene raw material is electroplated with the electroplating potion for the first time, the temperature is 40 celsius degrees and the time is 20 minutes; and when the graphite or graphene raw material is electroplated with the electroplating potion for the second time, the temperature is 40 celsius degrees and the time is 15 minutes.
As a further description of the aforementioned technical solution:
in the step 6), the graphite or graphene raw material is firstly soaked in a 5 g/L methyl benzotriazole solution for 20-30 seconds to form a first layer of protective film, and then put into a 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second layer of protective film.
In view of the above, by employing the aforementioned technical solution, the present disclosure has the following beneficial effects.
1. in the present disclosure, the graphite or graphene raw material is firstly placed in a plasma cleaning machine for plasma cleaning, and then the surface of graphite or graphene is treated with an activator compounded by sulfuric acid, the OP-10 surfactant and sodium dodecyl sulfate. Sulphuric acid can wash away oil stains from the graphite or graphene raw material, the OP-10 surfactant improves the smoothness of the surface of the graphite or graphene raw material, and sodium dodecyl sulfate increases the dispersibility of graphite or graphene and further increases the smoothness of the surface of the graphite or graphene raw material, so that the electroplated copper film layer has good binding quality and is uniform, which enhances the flexibility of the prepared heat dissipation component, and the surface of the heat dissipation component is not easy to generate creases, and the heat dissipation and acid and alkali resistance performances of the heat dissipation component are improved.
2. In the present disclosure, after the copper film layer is formed on the graphite or graphene raw material by electroplating, the graphite or graphene raw material electroplated with the copper film layer is first soaked in a 5 g/L methyl benzotriazole solution for 20-30 seconds to form a first layer of protective film on the copper film layer, and then put into a 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second layer of protective film on the copper film layer, which effectively prevents the copper film layer from color changing.

DETAILED DESCRIPTION OF THE EMBODIMENTS

Exemplary examples of the present disclosure will be described in more detail below. Although exemplary examples of the present disclosure are shown, it should be understood that the present disclosure may be implemented in various forms, and should not be limited by the examples set forth herein. On the contrary, these embodiments are provided to enable a more thorough understanding of the present disclosure and to fully convey the scope of the disclosure to those skilled in the art.

Example 1

This example of the present disclosure provided a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material, including the following steps:
1) placing a graphite or graphene raw material in a plasma cleaning machine for plasma cleaning, wherein the plasma cleaning machine had an air pressure of 2 MPa and a power of 550-600 W, and the time for the plasma cleaning was 30 min;
2) taking preparation materials of an activator including the following components in percentage by weight: 15% of sulfuric acid, 0.1% of an OP-10 surfactant, 0.1% of sodium dodecyl sulfate, and the balance of water;
3) mixing the aforementioned components of the activator to prepare the activator, and continually cleaning the graphite or graphene raw material with the activator;
4) continually cleaning the graphite or graphene raw material with deionized water;
5) conducting a electroplating process on a surface of the graphite or graphene raw material twice to form a copper film layer;
6) continually cleaning the graphite or graphene raw material electroplated with the copper film layer on the surface thereof with deionized water;
7) firstly, soaking the graphite or graphene raw material plated with the copper film layer in a 5 g/L methyl benzotriazole solution for 20-30 seconds to form a first layer of protective film on the copper film layer, and then putting into a 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second layer of protective film on the copper film layer to effectively prevent the copper film from color changing;
8) drying the graphite or graphene raw material electroplated with the copper film layer.
In the step 5), it included two electroplating procedures: firstly, the graphite or graphene raw material was subjected to primary electroplating with an electroplating potion; and secondly, the graphite or graphene raw material was subjected to secondary electroplating with the electroplating potion. The electroplating potion included the following components in percentage by weight: 5% of copper ions; 14% of sulfuric acid; 0.8% of a brightener; 0.06% of an adjuvant; 0.06% of a leveling agent; and the balance of water. During the electroplating process, pickling could be carried out at the same time, so that the flatness of the heat dissipation component was good.
Various process parameters of Example 1 were shown in the table below:


		Potion
Electroplating	Component	concen-
process	name	tration	Temperature	Time

Activation	sulfuric acid	15%	25° C.	3 minutes
	Surfactant A	0.10%
	(OP-10)
	sodium dodecyl	0.10%
	sulfate

Washing with	deionized water	25° C.	20 seconds
pure water

Pre-plating of	Copper ions	50 g/l	40° C.	20 minutes
copper	sulfuric acid	14%
	Additive A	0.80%
	(brightener)
	Additive B	0.06%
	(adjuvant)
	Additive C	0.06%
	(leveling agent)
Electroplating	Copper ions	50 g/l	40° C.	15 minutes
of	sulfuric acid	14%
copper	Additive A	0.80%
	(brightener)
	Additive B	0.06%
	(adjuvant)
	Additive C	0.06%
	(leveling agent)

Cleaning with	deionized water	25° C.	20 seconds
pure water

Protection 1	methyl	5 g/l	25° C.	20 seconds
	benzotriazole
Protection 2	cetylpyridinium	0.5 g/l	25° C.	20 seconds
	bromide

Drying	drying oven	80° C.	2 minutes

Example 2

This example of the present disclosure provided a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material, including the following steps:
1) placing a graphite or graphene raw material in a plasma cleaning machine for plasma cleaning, wherein the plasma cleaning machine had an air pressure of 2 MPa and a power of 550-600 W, and the time for the plasma cleaning was 30 min;
2) taking preparation materials of an activator including the following components in percentage by weight: 16% of sulfuric acid, 0.2% of an OP-10 surfactant, 0.2% of sodium dodecyl sulfate, and the balance of water;
3) mixing the aforementioned components of the activator to prepare the activator, and continually cleaning the graphite or graphene raw material with the activator;
4) continually cleaning the graphite or graphene raw material with deionized water;
5) conducting a electroplating process on a surface of the graphite or graphene raw material twice to form a copper film layer;
6) continually cleaning the graphite or graphene raw material electroplated with the copper film layer on the surface thereof with deionized water;
7) firstly, soaking the graphite or graphene raw material plated with the copper film layer in a 5 g/L methyl benzotriazole solution for 20-30 seconds to form a first layer of protective film on the copper film layer, and then putting into a 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second layer of protective film on the copper film layer to effectively prevent the copper film from color changing;
8) drying the graphite or graphene raw material electroplated with the copper film layer.
In view of the above, compared with the prior art, the method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material as provided by the aforementioned examples has the following advantages. The graphite or graphene raw material is firstly placed in a plasma cleaning machine for plasma cleaning, and then the surface of graphite or graphene is treated with an activator compounded by sulfuric acid, the OP-10 surfactant and sodium dodecyl sulfate. Sulphuric acid can wash away oil stains from the graphite or graphene raw material, the OP-10 surfactant improves the smoothness of the surface of the graphite or graphene raw material, and sodium dodecyl sulfate increases the dispersibility of graphite or graphene and further increases the smoothness of the surface of the graphite or graphene raw material, so that the electroplated copper film layer has good binding quality and is uniform, which enhances the flexibility of the prepared heat dissipation component, and the surface of the heat dissipation component is not easy to generate creases, and the heat dissipation and acid and alkali resistance performances of the heat dissipation component are improved. After the copper film layer is formed on the graphite or graphene raw material by electroplating, the graphite or graphene raw material electroplated with the copper film layer is first soaked in a 5 g/L methyl benzotriazole solution for 20-30 seconds to form a first layer of protective film on the copper film layer, and then put into a 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second layer of protective film on the copper film layer, which effectively prevents the copper film layer from color changing.
The aforementioned description is only preferred specific embodiments of the present disclosure, and the claimed scope of the present disclosure is not limited thereto. Equivalent substitutions or modifications can be made by those of skills in the art according to the technical solution and inventive concept of the present disclosure, without departing from the technical scope disclosed by the present disclosure. These substitutions or modifications all fall within the claimed scope of the present disclosure.

Claims

1. A method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material, comprising the following steps:

1) plasma cleaning a graphite or graphene raw material to obtain a first cleaned graphite or graphene raw material;

2) taking preparation materials of an activator comprising the following components in percentage by weight: 10-20% of sulfuric acid, 0.05-1% of an OP-10 surfactant, 0.05-1% of sodium dodecyl sulfate, and the balance of water;

3) mixing the aforementioned components of the activator to prepare the activator, and continually cleaning the first cleaned graphite or graphene raw material with the activator to obtain a second cleaned graphite or graphene raw material;

4) continually cleaning the graphite or graphene raw material with deionized water to obtain a third cleaned graphite or graphene raw material;

5) conducting an electroplating process on a surface of the third cleaned graphite or graphene raw material to form a copper film layer on the surface of the third cleaned graphite or graphene raw material to obtain an electroplated graphite or graphene raw material;

6) continually cleaning the electroplated graphite or graphene raw material with deionized water to obtain a fourth cleaned graphite or graphene raw material;

7) forming a protective film on the fourth cleaned graphite or graphene raw material by soaking to obtain a fifth graphite or graphene raw material covered by the protective film, wherein said forming the protective film on the fourth cleaned graphite or graphene raw material comprises:

soaking the fourth cleaned graphite or graphene raw material in a 5 g/L methyl benzotriazole solution for 20-30 seconds to form a first layer of protective film, and

putting the fourth cleaned graphite or graphene raw material with the first layer of protective film into a 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second layer of protective film; and

8) drying the fifth graphite or graphene raw material.

2. The method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material according to claim 1, wherein in the step 1), the graphite or graphene raw material is placed in a plasma cleaning machine for cleaning.

3. The method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material according to claim 1, wherein in the step 2), the activator comprises the following components in percentage by weight: 12-16% of sulfuric acid, 0.05-0.5% of the OP-10 surfactant, 0.05-0.5% of sodium dodecyl sulfate, and the balance of water.

4. The method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material according to claim 3, wherein in the step 2), the activator comprises the following components in percentage by weight: 15% sulfuric acid, 0.1% of the OP-10 surfactant, 0.1% of sodium dodecyl sulfate, and the balance of water.

5. The method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material according to claim 1, wherein in the step 5), the third cleaned graphite or graphene raw material is subjected to the electroplating process twice with an electroplating potion, and the electroplating potion comprises the following components in percentage by weight: 5% of copper ions; 14% of sulfuric acid; 0.8% of a brightener; 0.06% of an adjuvant; 0.06% of a leveling agent; and the balance of water.

6. The method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material according to claim 5, wherein in the step 5), when the third cleaned graphite or graphene raw material is electroplated with the electroplating potion for the first time, the temperature is 40 celsius degrees and the time is 20 minutes; and when the third cleaned graphite or graphene raw material is electroplated with the electroplating potion for the second time, the temperature is 40 celsius degrees and the time is 15 minutes.

7. (canceled)