TECHNICAL FIELD
[0001] 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
[0002] 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.
[0003] 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.
[0004] 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
[0005] 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.
[0006] 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.
[0007] As a further description of the aforementioned technical solution:
[0008] In the step 1), the graphite or graphene raw material is placed in a plasma cleaning
machine for cleaning.
[0009] As a further description of the aforementioned technical solution:
[0010] 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.
[0011] As a further description of the aforementioned technical solution:
[0012] 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.
[0013] As a further description of the aforementioned technical solution:
[0014] 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.
[0015] As a further description of the aforementioned technical solution:
[0016] 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.
[0017] 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.
[0018] 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
[0019] 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:
[0020] 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.
[0021] 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.
[0022] Various process parameters of Example 1 were shown in the table below:
| Electroplating process |
Component name |
Potion concentration |
Temperature |
Time |
|
| Activation |
sulfuric acid |
15% |
25°C |
3 minutes |
| Surfactant A (OP-10) |
0.10% |
| sodium dodecyl sulfate |
0.10% |
| Washing with pure water |
deionized water |
25°C |
20 seconds |
|
| Pre-plating of copper |
Copper ions |
50 g/l |
40°C |
20 minutes |
| sulfuric acid |
14% |
| Additive A (brightener) |
0.80% |
| Additive B (adjuvant) |
0.06% |
| Additive C (leveling agent) |
0.06% |
| Electroplating of copper |
Copper ions |
50 g/l |
40°C |
15 minutes |
| sulfuric acid |
14% |
| Additive A (brightener) |
0.80% |
| Additive B (adjuvant) |
0.06% |
| Additive C (leveling agent) |
0.06% |
| Cleaning with pure water |
deionized water |
25°C |
20 seconds |
| Protection 1 |
methyl benzotriazole |
5g/l |
25°C |
20 seconds |
| Protection 2 |
cetylpyridinium bromide |
0.5g/l |
25°C |
20 seconds |
| Drying |
drying oven |
80°C |
2 minutes |
Example 2
[0023] 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.
[0024] 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.
[0025] 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.
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;
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 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.
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
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 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.
7. 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 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.
Amended claims in accordance with Rule 137(2) EPC.
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;
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 being 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,
comprising: 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; and
8) drying the graphite or graphene raw material electroplated with the copper film
layer.
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 being 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
being 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
graphite or graphene raw material is subjected to the electroplating process twice
with an electroplating solution, and the electroplating solution 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
being 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 graphite or graphene raw material is electroplated with the electroplating solution
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
solution for the second time, the temperature is 40 celsius degrees and the time is
15 minutes.