CN107573446B - Boron nitride nanosheet and carbopol gel composite heat interfacial material and preparation method - Google Patents
Boron nitride nanosheet and carbopol gel composite heat interfacial material and preparation method Download PDFInfo
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- CN107573446B CN107573446B CN201610520064.3A CN201610520064A CN107573446B CN 107573446 B CN107573446 B CN 107573446B CN 201610520064 A CN201610520064 A CN 201610520064A CN 107573446 B CN107573446 B CN 107573446B
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 106
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 85
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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003999 initiator Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 150000002505 iron Chemical class 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 39
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 14
- 229910017083 AlN Inorganic materials 0.000 claims description 13
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 12
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 6
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 239000002356 single layer Substances 0.000 claims description 6
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- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 5
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- 239000002245 particle Substances 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
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- 238000000926 separation method Methods 0.000 claims 1
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- 239000000499 gel Substances 0.000 description 52
- 150000001875 compounds Chemical class 0.000 description 16
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- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical compound [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 description 6
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Abstract
The present invention provides a kind of boron nitride nanosheets and carbopol gel composite heat interfacial material and preparation method.The thermal interfacial material includes carbopol gel matrix and heat filling, and wherein carbopol gel matrix includes ferric ion-carbopol gel or modified silicon ball-carbopol gel, and heat filling includes boron nitride nanosheet.The thermal interfacial material the preparation method comprises the following steps: acrylic acid, water and trivalent iron salt or modified silicon ball are uniformly mixed, boron nitride nanosheet is added to be uniformly mixed, stirring, then it is stirred to react in the presence of initiator 30-40 minutes, it is reacted 40-48 hours in 35 ± 2 DEG C of standings again, obtains the thermal interfacial material.Thermal interfacial material provided by the invention is a kind of deformable and recoverable gel thermal interfacial material, it is with excellent heating conduction, and it can be closely adhered in the various surfaces that need to be radiated, make in the gap between heater element and spreader surface absolutely not air circulation.
Description
Technical field
The present invention relates to a kind of boron nitride nanosheets and carbopol gel composite heat interfacial material and preparation method thereof, belong to
In thermal interfacial material technical field.
Background technique
With the electronic products such as computer chip, high-power electronic device and photoelectric device, air-conditioning, TV, refrigerator, LED
Households and the industrial electric apparatus such as illumination, the modern transportations such as automobile, aircraft, steamer, high-speed rail equipment is to lightweight, miniaturization, height
Power direction development, the heat that unit area generates is higher and higher, and to heat control system, more stringent requirements are proposed.Therefore, such as
What quick, safety heat taken away on heater element becomes an important topic for restricting many industrial circles development.
In above-mentioned field, by taking integrated circuit as an example, with its various electronics and its related fields flourish and
Be widely used, how to solve the problems, such as the heat dissipation problem of integrated circuit become the field need solve it is main.Overheat will be big
Amplitude slows down the working efficiency of integrated circuit, in addition integrated circuit is caused it is badly damaged, and may be tired with the time
Product makes whole equipment eventual failure.Under normal circumstances, the problems of excessive heat of integrated circuit be by install additional on it radiator or
Fan is solved with helping its heat dissipation, and can also add thermal interfacial material in the gap of integrated circuit and radiator
(TIM) carry out heat transfer.
Existing thermal interfacial material mainly includes thermal paste, thermally conductive gel, phase-change thermal interface material, polymer-based compound
Several classes such as thermal interfacial material and metal heat interface material.Wherein, especially using aluminium oxide, boron nitride or aluminium nitride as heat filling
Thermal interfacial material be widely studied and develop.Compound of the boron nitride (Boron Nitride, BN) as similar graphite,
Material science research field has shown many noticeable characteristics, such as high intrinsic thermal conductivity, excellent chemical stability
With thermal stability, broad-band gap and good greasy property.Particularly, due to boron nitride nanosheet (boron nitride
Nanosheets, BNNS) aspect ratio (aspect ratio) with higher and specific surface area, compared with its block materials, table
Reveal more excellent material property.
In recent years, existing thermal interfacial material is not able to satisfy integrated level and power density in electronic technology already and further mentions
Height to heat dissipation requirement, and existing thermal interfacial material mechanical performance (including elasticity, viscosity, tensile strength etc. just
Face) still need to further increase, therefore develop it is a kind of novel using boron nitride nanosheet as the thermal interfacial material of heat filling, at
For one of this field urgent problem to be solved.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide a kind of boron nitride nanosheet and carbopol gels
Composite heat interfacial material and preparation method thereof.The thermal interfacial material is a kind of deformable and recoverable hot interface material of gel
Material, with excellent heating conduction, and can be closely adhered in the various surfaces that need to be radiated, makes heater element and radiator
Absolutely not air circulation in gap between surface.
In order to achieve the above objectives, present invention firstly provides a kind of boron nitride nanosheets and carbopol gel compound thermal circle
Plane materiel material, which includes carbopol gel matrix and heat filling, wherein the carbopol gel matrix
Boron nitride is included at least including ferric ion-carbopol gel or modified silicon ball-carbopol gel, the heat filling
Nanometer sheet.
In above-mentioned thermal interfacial material, it is preferable that the diameter of used boron nitride nanosheet is 200-2000nm, single layer
Thickness is about 0.8-1.2nm, and single-sheet thickness is about 5-15nm, and thermal conductivity is about 200-800W/mK.
In above-mentioned thermal interfacial material, it is preferable that prepare boron nitride nanosheet used by the thermal interfacial material and third
The mass ratio of olefin(e) acid is (1-5): 10.
In above-mentioned thermal interfacial material, it is preferable that the heat filling can further include aluminium oxide, aluminium nitride and
The combination of one or more of silicon carbide etc. prepares aluminium oxide used by the thermal interfacial material, aluminium nitride and silicon carbide
Deng one or more of combination and acrylic acid mass ratio be (0-5): 10, the mass ratio be preferably (1-5): 10.
In above-mentioned thermal interfacial material, it is preferable that prepare ferric ion used by the thermal interfacial material and propylene
The molar ratio of acid is (0.4-0.6): 100, which is more preferably (0.45-0.55): 100.
In above-mentioned thermal interfacial material, it is preferable that prepare modified silicon ball and acrylic acid used by the thermal interfacial material
Mass ratio be 0.09-0.11:100.The modification silicon ball may include vinyl silicon ball, and the diameter of the vinyl silicon ball can be
2.5-3.5nm。
Specific embodiment according to the present invention, it is preferable that above-mentioned boron nitride nanosheet and carbopol gel compound thermal
The thermal conductivity of boundary material is 1-3.5W/mK, complex viscosity 105-108Pas, tensile strength 20-40kPa, Applicable temperature
It is 0-120 DEG C.
Specific embodiment according to the present invention, it is preferable that above-mentioned boron nitride nanosheet and carbopol gel compound thermal
Boundary material is prepared by least following steps:
(1) acrylic acid, water and trivalent iron salt or modified silicon ball are uniformly mixed；
(2) boron nitride nanosheet is added, is uniformly mixed；
(3) stirring 8-12 hours after；
(4) it is then stirred to react in the presence of initiator 30-40 minutes, then stands reaction 35 ± 2 DEG C (in water-baths)
40-48 hours, obtain the boron nitride nanosheet and carbopol gel composite heat interfacial material.
Specific embodiment according to the present invention, it is preferable that compound in above-mentioned boron nitride nanosheet and carbopol gel
In the preparation step of thermal interfacial material, the mass ratio of used acrylic acid and water is 2:8-5:5, more preferably 2:8.
Specific embodiment according to the present invention, it is preferable that compound in above-mentioned boron nitride nanosheet and carbopol gel
The preparation step of thermal interfacial material further comprises step (5): boron nitride nanosheet described in constant temperature drying after step (4)
Reach required amount with the mass content of carbopol gel composite heat interfacial material to water therein.What the baking step obtained
The mass content of water can be carried out conventional adjustment by those skilled in the art in thermal interfacial material.
Specific embodiment according to the present invention, it is preferable that compound in above-mentioned boron nitride nanosheet and carbopol gel
In the preparation step of thermal interfacial material, the molar ratio of ferric ion and acrylic acid in used trivalent iron salt is (0.4-
0.6): 100, which is more preferably (0.45-0.55): 100.
Specific embodiment according to the present invention, it is preferable that compound in above-mentioned boron nitride nanosheet and carbopol gel
In the preparation step of thermal interfacial material, used trivalent iron salt includes iron chloride and/or ferric nitrate etc..
Specific embodiment according to the present invention, it is preferable that compound in above-mentioned boron nitride nanosheet and carbopol gel
In the preparation step of thermal interfacial material, the mass ratio of used modified silicon ball and acrylic acid is 0.09-0.11:100.The modification
Silicon ball may include vinyl silicon ball, and the diameter of the vinyl silicon ball can be 2.5-3.5nm.
Specific embodiment according to the present invention, it is preferable that compound in above-mentioned boron nitride nanosheet and carbopol gel
In the preparation step of thermal interfacial material, the mass ratio of used boron nitride nanosheet and acrylic acid is (1-5): 10.
Specific embodiment according to the present invention, it is preferable that compound in above-mentioned boron nitride nanosheet and carbopol gel
In the preparation step of thermal interfacial material, used boron nitride nanosheet is through the following steps that be prepared: by boron nitride
Powder is put into water and/or alcohol ultrasound repeatedly and stirring, and makes total ultrasonic time control at 110-130 minutes；Then by water
And/or separate with the boron nitride powder after ultrasonic treatment (such as can be using making the side of water and/or alcohol explosive evaporation for alcohol
Formula), after the boron nitride powder after ultrasonic treatment is dried at 50-60 DEG C (can using baking oven carry out), obtain described
Boron nitride nanosheet.Wherein, the particle diameter of used boron nitride powder can be 1-100 μm, and obtained boron nitride is received
The diameter of rice piece is 200-2000nm, and thickness in monolayer is about 0.8-1.2nm, and single-sheet thickness is about 5-15nm, and thermal conductivity is about
200-800W/mK.The power of the ultrasound can be (120 ± 2) W, and frequency can be (40 ± 2) KHz.
Specific embodiment according to the present invention, it is preferable that above-mentioned boron nitride nanosheet and carbopol gel compound thermal
The preparation step of boundary material further include: when boron nitride nanosheet is added, be additionally added in aluminium oxide, aluminium nitride and silicon carbide etc.
One or more of combinations.Also, the combination of one or more of used aluminium oxide, aluminium nitride and silicon carbide etc. with
The mass ratio of acrylic acid is (0-5): 10, which is preferably (1-5): 10.
Specific embodiment according to the present invention, it is preferable that compound in above-mentioned boron nitride nanosheet and carbopol gel
In the preparation step of thermal interfacial material, used initiator includes ammonium persulfate, and the ammonium persulfate and acrylic acid being added
Molar ratio be (0.4-0.6): 100, the molar ratio be preferably (0.45-0.55): 100.
Specific embodiment according to the present invention, it is preferable that compound in above-mentioned boron nitride nanosheet and carbopol gel
In the preparation step of thermal interfacial material, at least step (4) carries out in a mold.In addition, step (1)-(3) can also be in mould
It is carried out in tool.It is put into mold that is, sufficient raw material can will be stirred, it can also be in ingredient just directly in mould
It is carried out in tool.And before initiator is added, can first it vacuumize so that the air in raw material is discharged；Initiator is being added and is stirring
After reaction 30-40 minutes, it can vacuumize, then seal mold again, be placed in 35 ± 2 DEG C of water-baths and stand reaction
40-48 hours.
Boron nitride nanosheet provided by the invention and carbopol gel composite heat interfacial material use ferric ion-
Carbopol gel or modified silicon ball-carbopol gel make polyacrylic acid chain and the iron in the thermal interfacial material as matrix
Ion or modified silicon ball are linked to each other, and form long-chain and reticular structure, substantially increase mechanical performance (including the bullet of gel
Property, viscosity, tensile strength etc.), its restorability is improved, its service life is extended.Wherein, modified silicon ball is as four
Valence object is capable of providing more hinged nodes to ensure better mechanical performance.Meanwhile thermal interfacial material of the invention is at least adopted
Use boron nitride nanosheet as heat filling, since boron nitride nanosheet has excellent heating conduction, so that heat of the invention
Boundary material thermal conductivity with higher.Therefore, thermal interfacial material provided by the invention is a kind of deformable and recoverable solidifying
Gluey thermal interfacial material can be restored to the original state with excellent self-healing properties and by control water content, also be had
There is excellent heating conduction, and can be closely adhered in the various surfaces that need to be radiated, makes between heater element and spreader surface
Gap in absolutely not air circulation, while it also has longer service life, repeatedly by cutting and again split into
After row self-healing, healing position still can bear higher stress and thermal conductivity is without being substantially reduced.
The present invention also provides the preparations of a kind of above-mentioned boron nitride nanosheet and carbopol gel composite heat interfacial material
Method, the preparation method the following steps are included:
(1) acrylic acid, water and trivalent iron salt or modified silicon ball are uniformly mixed；
(2) boron nitride nanosheet is added, is uniformly mixed；
(3) stirring 8-12 hours after；
(4) it is then stirred to react in the presence of initiator 30-40 minutes, then stands reaction 35 ± 2 DEG C (in water-baths)
40-48 hours, obtain the boron nitride nanosheet and carbopol gel composite heat interfacial material.
In the above preparation method, it is preferable that the mass ratio of used acrylic acid and water is 2:8-5:5, more preferably
2:8。
Specific embodiment according to the present invention, it is preferable that further comprise after step (4) in above-mentioned preparation method
Step (5): with boron nitride nanosheet described in constant temperature drying and carbopol gel composite heat interfacial material to water therein
Mass content reaches required amount.The mass content of water can be by art technology in the thermal interfacial material that the baking step obtains
Personnel carry out conventional adjustment.
In the above preparation method, it is preferable that mole of ferric ion and acrylic acid in used trivalent iron salt
Than for (0.4-0.6): 100, which is more preferably (0.45-0.55): 100.
In the above preparation method, it is preferable that used trivalent iron salt includes iron chloride and/or ferric nitrate etc..
In the above preparation method, it is preferable that the mass ratio of used modified silicon ball and acrylic acid is 0.09-0.11:
100.The modification silicon ball may include vinyl silicon ball, and the diameter of the vinyl silicon ball can be 2.5-3.5nm.
In the above preparation method, it is preferable that the mass ratio of used boron nitride nanosheet and acrylic acid is (1-5):
10。
In the above preparation method, it is preferable that used boron nitride nanosheet is through the following steps that be prepared:
Boron nitride powder is put into water and/or alcohol ultrasound repeatedly and stirring, and makes total ultrasonic time control at 110-130 minutes；
Then separate water and/or alcohol with the boron nitride powder after ultrasonic treatment (such as can be steamed using making water and/or alcohol boil
The mode of hair), it (can be carried out), be obtained using baking oven after the boron nitride powder after ultrasonic treatment is dried at 50-60 DEG C
The boron nitride nanosheet.Wherein, the particle diameter of used boron nitride powder can be 1-100 μm, obtained nitrogen
The diameter for changing boron nanometer sheet is 200-2000nm, and thickness in monolayer is about 0.8-1.2nm, and single-sheet thickness is about 5-15nm, thermal conductivity
About 200-800W/mK.The power of the ultrasound can be (120 ± 2) W, and frequency can be (40 ± 2) KHz.
Specific embodiment according to the present invention, it is preferable that above-mentioned preparation method, which further includes steps of, to be added
When boron nitride nanosheet, it is additionally added the combination of one or more of aluminium oxide, aluminium nitride and silicon carbide etc..Also, it is used
The combination of one or more of aluminium oxide, aluminium nitride and silicon carbide etc. and the mass ratio of acrylic acid be (0-5): 10, the matter
Amount is than being preferably (1-5): 10.
In the above preparation method, it is preferable that used initiator includes ammonium persulfate, and the ammonium persulfate being added
Molar ratio with acrylic acid is (0.4-0.6): 100, which is preferably (0.45-0.55): 100.
In the above preparation method, it is preferable that at least step (4) carries out in a mold；In addition, step (1)-(3)
It can also carry out in a mold.It is put into mold that is, sufficient raw material can will be stirred, it can also be in ingredient
With regard to directly carrying out in a mold.And before initiator is added, can first it vacuumize so that the air in raw material is discharged；Draw in addition
Hair agent is simultaneously stirred to react after 30-40 minutes, can be vacuumized, then be sealed mold again, be placed in 35 ± 2 DEG C of water-baths
Stand reaction 40-48 hours.
Compared with traditional thermal interfacial material, the advantage of thermal interfacial material of the invention is specifically included that
(1) compared to conventional solid thermal interfacial material
Conventional solid thermal interfacial material often is faced with the problem of gap between can not filling the surface that full two need heat transfer,
The air retained in gap will significantly reduce its heating conduction.Compared to conventional solid thermal interfacial material, gel heat of the invention
Boundary material be it is soft and deformable, can fit closely in any coarse or curved surface or gap, make to send out
Absolutely not air enters in gap between thermal element and spreader surface, and then shows relatively high heat-conductive characteristic,
It can be used in helping cooling integrated and play a protective role to integrated circuit and its related device.
(2) compared to liquid thermal interfacial material
Liquid thermal interfacial material has mobility, in some instances it may even be possible to can add up as the temperature rises and using the time
And it volatilizees or is lost.Compared to liquid thermal interfacial material, gel thermal interfacial material of the invention can be formed, and
It will not flow or deform under wider temperature range, unless it absorbs a certain amount of moisture；And thermal interfacial material of the invention
The problem of will not volatilizing, and then reducing heat-conductive characteristic there is no significant its of the volatilization of thermal interfacial material；Therefore, of the invention solidifying
Gluey thermal interfacial material is capable of fixing in various types of gaps.
(3) compared to traditional disposable thermal boundary material
Compared to traditional disposable thermal boundary material, gel thermal interfacial material of the invention can in different application quilt
Longer service life is reused and has, which is a kind of environment friendly material.
In conclusion boron nitride nanosheet provided by the invention and carbopol gel composite heat interfacial material are that one kind can
Deformation and recoverable gel thermal interfacial material.Since with deformability, which can be transformed into different
Shape, therefore its heater element surface that can satisfy different situations or spreader surface (such as coarse or curved surface)
Requirement, and can be closely adhered in a variety of different surfaces that need to be radiated, make various types of heater element and dissipate
Absolutely not air circulation in gap between hot device surface, that is, have for different types of surface and gap splendid suitable
Ying Xing, and then improve heating conduction.The thermal interfacial material has recoverability simultaneously, can be restored by control water content
Original state, and there are excellent self-healing properties, after repeatedly being cut and split carries out self-healing again, healing position is still
Higher stress so can be born and thermal conductivity is without being substantially reduced, by water suction, drying and arbitrary shape can also be become come quilt
It reuses, therefore the thermal interfacial material can be reused in different application and have longer service life.In addition,
Since using boron nitride nanosheet, as heat filling, which has excellent heating conduction.Therefore, the present invention mentions
The boron nitride nanosheet and carbopol gel composite heat interfacial material of confession not only show excellent heat-conductive characteristic, are also solid
Body heat boundary material generally can not be fitted closely from different surfaces and liquid thermal interfacial material would generally volatilize or be lost and mention
Solution is supplied.Gel thermal interfacial material of the invention mainly can be applied in the heat dissipation of various integrated circuits, such as
The heat dissipation of CPU and relay, can be used for other needs the field of heat transfer.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention
Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
Embodiment 1
Present embodiments provide a kind of boron nitride nanosheet and carbopol gel composite heat interfacial material, be by with
What lower step was prepared:
(1) boron nitride powder is put into water and/or alcohol ultrasound repeatedly and stirring, and makes total ultrasonic time control 2
Hour, and the power of ultrasound can be 120W, frequency can be 40KHz；It then, will be ultrasonic by water and/or alcohol explosive evaporation
Treated, and boron nitride powder is put into baking oven after 50 DEG C of drying, obtains boron nitride nanosheet；Wherein, used boron nitride
The particle diameter of powder is 1-20 μm, and the diameter of obtained boron nitride nanosheet is 200-2000nm, and thickness in monolayer is about
1nm, single-sheet thickness are about 10nm, and thermal conductivity is about 300 ± 100W/mK；
(2) acrylic acid, water and iron chloride are uniformly mixed；Wherein, the mass ratio of acrylic acid and water is 2:8, iron chloride
Molar ratio with acrylic acid is 0.5:100；
(3) boron nitride nanosheet that step (1) is prepared is added, is uniformly mixed；Wherein, the boron nitride nanometer of addition
The mass ratio of piece and acrylic acid is 5:10；
(4) stirring 8-12 hours after；
(5) sufficient raw material will be stirred to be put into mold, vacuumized so that the air in raw material is discharged；Then it is added and draws
Hair agent ammonium persulfate is simultaneously stirred to react 0.5 hour, is vacuumized, is then sealed mold again, is placed in 35 DEG C of water-baths and stands
Reaction makes raw material sufficiently react molding in 48 hours, obtains the thick of boron nitride nanosheet and carbopol gel composite heat interfacial material
Product；Wherein, the molar ratio of the ammonium persulfate and acrylic acid of addition is 0.5:100；
(6) crude product of obtained gel thermal interfacial material is taken out, is cut, weighed, control quality then with 30 DEG C
The mass content of constant temperature drying water into thermal interfacial material crude product obtains the boron nitride nanosheet and polypropylene to 40%
Acid gel composite heat interfacial material.
Test obtains the thermal conductivity of boron nitride nanosheet provided in this embodiment Yu carbopol gel composite heat interfacial material
Rate is 3.1981W/mK, complex viscosity 341291Pas, tensile strength 40.087kPa, and Applicable temperature is 0-120 DEG C.
Boron nitride nanosheet provided in this embodiment is cut with carbopol gel composite heat interfacial material and is spelled again
After conjunction, healing position can bear at least stress of 10kPa, and thermal conductivity just has slight after cutting and healing three times
It reduces, thermal conductivity about reduces 10% or so.As it can be seen that the present embodiment is using boron nitride nanosheet and ferric ion-poly- third
The compound obtained thermal interfacial material of olefin(e) acid gel has excellent self-healing performance, heating conduction and reusable performance.
Embodiment 2
Present embodiments provide a kind of boron nitride nanosheet and carbopol gel composite heat interfacial material, the hot interface material
The preparation step of material is substantially the same manner as Example 1, the difference is that: the boron nitride nanosheet of addition and the mass ratio of acrylic acid
For 2:10.
Test obtains the thermal conductivity of boron nitride nanosheet provided in this embodiment Yu carbopol gel composite heat interfacial material
Rate is 1.5898W/mK, complex viscosity 343962Pas, tensile strength 32.227kPa, and Applicable temperature is 0-120 DEG C.
Comparative example 1
This comparative example provides a kind of ferric ion-carbopol gel, the preparation step and 1 base of embodiment of the gel
This is identical, the difference is that: it is added without boron nitride nanosheet.
Ferric ion-carbopol gel thermal conductivity that test obtains the offer of this comparative example is 0.8553W/mK, multiple
Number viscosity is 128818Pas, tensile strength 21.302kPa.
Comparative example 2
This comparative example provides a kind of boron nitride nanosheet and carbopol gel composite heat interfacial material, the hot interface material
The preparation step of material is substantially the same manner as Example 1, the difference is that: it is added without iron chloride.
Test obtains the boron nitride nanosheet of this comparative example offer and the thermal conductivity of carbopol gel composite heat interfacial material
Rate is 3.0072W/mK, complex viscosity 605.047Pas, tensile strength 3.186kPa.
Application examples
Product prepared by embodiment 1 and comparative example 1 is separately connected the same coarse ceramic bottom board and two panels is separated
Coarse potsherd, baseplate temp are 65 DEG C, and the initial temperature for the potsherd that embodiment 1 is connected with product prepared by comparative example 1 is equal
It is 23 DEG C.It has been observed that as time goes by, it is real when the temperature of the potsherd of product connection prepared by comparative example 1 is 47 DEG C
The temperature for applying the potsherd of the product connection of the preparation of example 1 has reached 54 DEG C, it is seen that the potsherd of product connection prepared by embodiment 1
Obvious heating faster, illustrates that the thermal conductivity of the product is more excellent.
Claims (14)
1. a kind of boron nitride nanosheet and carbopol gel composite heat interfacial material, which includes polypropylene acid cure
Matrix body and heat filling, wherein the carbopol gel matrix includes ferric ion-carbopol gel, it is described to lead
Hot filler includes at least boron nitride nanosheet；
The mass ratio for preparing boron nitride nanosheet used by the thermal interfacial material and acrylic acid is (1-5): 10.
2. boron nitride nanosheet according to claim 1 and carbopol gel composite heat interfacial material, wherein used
Boron nitride nanosheet diameter be 200-2000nm, thickness in monolayer 0.8-1.2nm, single-sheet thickness 5-15nm, thermal conductivity
For 200-800W/mK.
3. boron nitride nanosheet according to claim 1 and carbopol gel composite heat interfacial material, wherein described to lead
Hot filler still further comprises the combination of one or more of aluminium oxide, aluminium nitride and silicon carbide, prepares the hot interface material
The combination of one or more of aluminium oxide used by expecting, aluminium nitride and silicon carbide and the mass ratio of acrylic acid are (0-5):
10。
4. boron nitride nanosheet according to claim 3 and carbopol gel composite heat interfacial material, wherein preparation institute
State the combination of one or more of aluminium oxide, aluminium nitride used by thermal interfacial material and silicon carbide and the mass ratio of acrylic acid
For (1-5): 10.
5. boron nitride nanosheet according to claim 1 and carbopol gel composite heat interfacial material, wherein preparation institute
The molar ratio for stating ferric ion and acrylic acid used by thermal interfacial material is (0.4-0.6): 100.
6. boron nitride nanosheet according to claim 5 and carbopol gel composite heat interfacial material, wherein preparation institute
The molar ratio for stating ferric ion and acrylic acid used by thermal interfacial material is (0.45-0.55): 100.
7. boron nitride nanosheet according to claim 1 and carbopol gel composite heat interfacial material, wherein the heat
The thermal conductivity of boundary material is 1-3.5W/mK, complex viscosity 105-108Pas, tensile strength 20-40kPa, Applicable temperature
It is 0-120 DEG C.
8. boron nitride nanosheet according to claim 1 and carbopol gel composite heat interfacial material, wherein the heat
Boundary material is prepared by least following steps:
(1) acrylic acid, water and trivalent iron salt are uniformly mixed；
(2) boron nitride nanosheet is added, is uniformly mixed；
(3) stirring 8-12 hours after；
(4) it is then stirred to react in the presence of initiator 30-40 minutes, then is reacted 40-48 hours in 35 ± 2 DEG C of standings, obtained
To the boron nitride nanosheet and carbopol gel composite heat interfacial material.
9. boron nitride nanosheet according to claim 8 and carbopol gel composite heat interfacial material, wherein used
Trivalent iron salt include iron chloride and/or ferric nitrate；
Used initiator includes ammonium persulfate, and the molar ratio for the ammonium persulfate and acrylic acid being added is (0.4-0.6):
100。
10. boron nitride nanosheet according to claim 9 and carbopol gel composite heat interfacial material, wherein be added
Ammonium persulfate and acrylic acid molar ratio be (0.45-0.55): 100.
11. boron nitride nanosheet according to claim 8 and carbopol gel composite heat interfacial material, wherein adopted
Boron nitride nanosheet is through the following steps that be prepared: boron nitride powder being put into water and/or alcohol surpasses repeatedly
Sound and stirring, and make total ultrasonic time control at 110-130 minutes；Then by the nitridation after water and/or alcohol and ultrasonic treatment
Boron powder separation obtains the boron nitride nanometer by the boron nitride powder after ultrasonic treatment after 50-60 DEG C is dried
Piece；Wherein, the particle diameter of used boron nitride powder is 1-100 μm, and the diameter of obtained boron nitride nanosheet is
200-2000nm, thickness in monolayer 0.8-1.2nm, single-sheet thickness 5-15nm, thermal conductivity 200-800W/mK.
12. boron nitride nanosheet according to claim 8 and carbopol gel composite heat interfacial material, wherein described
The preparation step of thermal interfacial material further include: when boron nitride nanosheet is added, be additionally added in aluminium oxide, aluminium nitride and silicon carbide
One or more of combinations；Also, the combination of one or more of used aluminium oxide, aluminium nitride and silicon carbide and third
The mass ratio of olefin(e) acid is (0-5): 10.
13. boron nitride nanosheet according to claim 12 and carbopol gel composite heat interfacial material, wherein adopted
The combination of one or more of aluminium oxide, aluminium nitride and silicon carbide and the mass ratio of acrylic acid are (1-5): 10.
14. a kind of described in any item boron nitride nanosheets of claim 1-13 and carbopol gel composite heat interfacial material
Preparation method, wherein the preparation method the following steps are included:
(1) acrylic acid, water and trivalent iron salt are uniformly mixed；
(2) boron nitride nanosheet is added, is uniformly mixed；
(3) stirring 8-12 hours after；
(4) it is then stirred to react in the presence of initiator 30-40 minutes, then is reacted 40-48 hours in 35 ± 2 DEG C of standings, obtained
To the boron nitride nanosheet and carbopol gel composite heat interfacial material.
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