CN108165237A - A kind of preparation method for improving Silica hydrogel composite wood heat conductivility - Google Patents
A kind of preparation method for improving Silica hydrogel composite wood heat conductivility Download PDFInfo
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- CN108165237A CN108165237A CN201810032016.9A CN201810032016A CN108165237A CN 108165237 A CN108165237 A CN 108165237A CN 201810032016 A CN201810032016 A CN 201810032016A CN 108165237 A CN108165237 A CN 108165237A
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
A kind of preparation method for improving Silica hydrogel composite wood heat conductivility, the present invention relates to thermal-conductive polymer matrix composites fields, and in particular to the preparation method of the polymer matrix composite of the lower obturator oriented alignment of magnetic material load technology and external magnetic field effect of diamond particle surfaces.The invention solves controllable preparation under magnetic fields qualitative arrangement Diamond/Si gel complex material prepare the technical issues of.Method：First prepare the diamond obturator particle of magnetic material load；Then using external magnetic field pair can the diamond particles of magnetic response be oriented arrangement to prepare composite material.The present invention proposes the preparation method of the Diamond/Si gel complex material of oriented alignment, the diamond particles oriented alignment of practical magnetic loading is characterized, oriented alignment significant effect, improves the thermal conductivity of Silica hydrogel composite sheet.
Description
Technical field
The present invention relates to thermal-conductive polymer matrix composites fields, and in particular to the magnetic material of diamond particle surfaces is born
The preparation method of the polymer matrix composite of load technology and the lower obturator oriented alignment of external magnetic field effect.
Background technology
At this stage, the fast development of the next-generation electronic device such as three dimensional integrated circuits (ICs) and hypervelocity high-capacity transistor
So that chip heat pipe reason becomes core technology, the application of electronic device of new generation is limited.If reduce GaN transistor temperature 10
DEG C, then its service life will extend one times；The reduction of silicon-base oxide semiconductor transistor operation temperature can improve integrated circuit
Clock speed.
Silica hydrogel is due to good elasticity, weatherability, chemical resistance and preferable temperature stability, usually
Basis material as electronic device thermal interfacial material.But be about 0.2W/mK since thermal conductivity of Silica hydrogel itself is relatively low, no
Suitable for being directly used as thermal interfacial material.In order to improve the thermal conductivity of Silica hydrogel, usual way is that filling is largely led thereto
Hot filler is to improve its thermal conductivity.In the prior art, medium thermal conductivity fillers such as aluminium oxide, boron nitride or aluminium nitride etc. (its heat
Conductance is 200-500W/mK), when needing more than 50% volume fraction of additive amount, the thermal conductivity of requirement can be reached；It is highly thermally conductive
Rate filler such as graphene, graphene nanometer sheet, carbon nanotube etc. (1000~2000W/mK of its thermal conductivity), this kind of heat filling
Price is typically relatively expensive, and since it with satisfactory electrical conductivity limits loading.Diamond is as a kind of electrical isolation
Material, thermal conductivity 2000W/mK, has had both high-termal conductivity and high-insulativity, is the excellent choosing of thermal interfacial material obturator
It selects.
Further to realize the preparation of high heat-conductive diamond Silica hydrogel thermal interfacial material, external magnetic field is selected to prepare orientation
The two-dimentional diamond Silica hydrogel composite material of arrangement has great importance, and magnetic field is considered as a kind of good external force of controllability
.But to the preparation problems of the diamond particles of external magnetic responsiveness and diamond how can be controlled to be oriented in magnetic field
The problems such as arrangement, is not resolved in thermal interfacial material preparation field.
Invention content
The invention solves skills prepared by the qualitative arrangement Diamond/Si gel complex material of controllable preparation under magnetic fields
Art problem, and a kind of preparation method for improving Silica hydrogel composite wood heat conductivility is provided.
A kind of preparation method for improving Silica hydrogel composite wood heat conductivility, specifically carries out according to the following steps：
First, using soluble metallic salt and diamond particles as raw material, the diamond solution of particles of magnetic material load is prepared；
Wherein particles of magnetic material and diamond quality ratio are 1: (0.1~20)；
2nd, the diamond solution strong magnet washing and depositing for obtaining step 1 detaches supernatant liquor, with distilled water repeatedly
Washing precipitate, until the pH of eluting water is 7；Then sediment is dried in vacuo, obtains the diamond filling of magnetic material load
Body particle；
3rd, the diamond obturator particle that the magnetic material for obtaining Silica hydrogel and step 2 loads mixes, mechanical agitation
It mixes to uniform, then mixture is put into mold, deaeration 5~15 minutes, mold is taken out under vacuum condition, is placed on external
It in magnetic field, is fully cured, completes a kind of preparation method for improving Silica hydrogel composite wood heat conductivility.
The method that the diamond solution of particles of magnetic material load is prepared wherein in step 1 is as follows：
Soluble ferric iron salt is dissolved in water, adds in diamond particles under agitation, then heating water bath to 25 DEG C~
80 DEG C, under inert atmosphere argon gas or nitrogen protection, 10~20min is stirred, control mixing speed is 500-1000r/min,
Sodium hydroxide solution is added in using constant pressure titration funnel, then constant temperature stirring the reaction was continued 1~3h, obtains particles of magnetic material and bear
The diamond solution of load.
Alternatively, the method that the diamond solution of particles of magnetic material load is prepared wherein in step 1 is as follows：
Soluble metallic salt plus ethylene glycol are dissolved, add in diamond particles under agitation, is titrated and leaked using constant pressure
Bucket adds in sodium hydroxide solution, then adds in reducing agent and is restored, obtains the diamond solution of particles of magnetic material load.
Mixing of the soluble metallic salt for one or more of molysite, nickel salt and cobalt salt.
The beneficial effects of the invention are as follows：
1st, the load that rational technique carries out surface magnetism material is employed to monocrystalline or polycrystalline diamond particle, makes its table
Face covers one layer of uniform magnetic material, and magnetic material load capacity is controllable.
2nd, the preparation method for being oriented arrangement in Silica hydrogel to diamond using external magnetic field is proposed, to practical magnetic
Property load diamond particles oriented alignment characterized, oriented alignment significant effect improves Silica hydrogel composite sheet
Thermal conductivity.
The present invention is used to prepare the Silica hydrogel composite sheet for improving thermal conductivity.
Description of the drawings
Fig. 1 is the surface topography photo of diamond particles before one magnetic loading of embodiment；
Fig. 2 is the surface topography photo of diamond particles after one magnetic loading of embodiment；
Fig. 3 is the surface topography photo of diamond particle surfaces magnetic-particle after one magnetic loading of embodiment；
Fig. 4 is the diamond surface element composition Energy Dispersive X spectrogram of one magnetic material of embodiment load；
Fig. 5 is the X-ray diffraction spectrogram of diamond surface before and after the load of one magnetic material of embodiment；Wherein a is magnetic negative
Carry diamond, b Fe3O4, c is single-crystal diamond；
Fig. 6 is the hysteresis loop figure of diamond before and after the load of one magnetic material of embodiment；Wherein A is magnetic loading Buddha's warrior attendant
Stone, B are single-crystal diamond；
Fig. 7 is the shape appearance figure of one composite sheet inner section direction oriented alignment diamond of embodiment；
Fig. 8 is the shape appearance figure of direction oriented alignment diamond in one composite sheet inside face of embodiment.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it
Between arbitrary combination.
Specific embodiment one：A kind of preparation method for improving Silica hydrogel composite wood heat conductivility of present embodiment, specifically
It carries out according to the following steps：
First, using soluble metallic salt and diamond particles as raw material, the diamond solution of particles of magnetic material load is prepared；
The particles of magnetic material wherein generated is 1 with diamond quality ratio: (0.1~20)；
2nd, the diamond solution strong magnet washing and depositing for obtaining step 1 detaches supernatant liquor, with distilled water repeatedly
Washing precipitate, until the pH of eluting water is 7；Then sediment is dried in vacuo, obtains the diamond filling of magnetic material load
Body particle；
3rd, the diamond obturator particle that the magnetic material for obtaining Silica hydrogel and step 2 loads mixes, mechanical agitation
It mixes to uniform, then mixture is put into mold, deaeration 5~15 minutes, mold is taken out under vacuum condition, is placed on external
It in magnetic field, is fully cured, completes a kind of preparation method for improving Silica hydrogel composite wood heat conductivility.
Specific embodiment two：The present embodiment is different from the first embodiment in that：Diamond particles in step 1
It is pre-processed：Diamond particles are screened using sieve, are then cleaned by ultrasonic in acetone, absolute ethyl alcohol, deionized water successively
10min, drying.It is other same as the specific embodiment one.
Specific embodiment three：The present embodiment is different from the first and the second embodiment in that：Diamond in step 1
Particle is monocrystalline or polycrystalline micro diamond particles, and average grain diameter is 1~100 μm.Other and specific embodiment one or two
It is identical.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：It is made in step 1
The method of the diamond solution of standby particles of magnetic material load is as follows：
Soluble ferric iron salt is dissolved in water, adds in diamond particles under agitation, then heating water bath to 25 DEG C~
80 DEG C, under inert atmosphere argon gas or nitrogen protection, 10~20min is stirred, control mixing speed is 500-1000r/min,
Sodium hydroxide solution is added in using constant pressure titration funnel, then constant temperature stirring the reaction was continued 1~3h, obtains particles of magnetic material and bear
The diamond solution of load.It is other identical with one of specific embodiment one to three.
Diamond solution prepared by present embodiment is the diamond aqueous solution of particles of magnetic material load.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：It is made in step 1
The method of the diamond solution of standby particles of magnetic material load is as follows：
Soluble metallic salt plus ethylene glycol are dissolved, add in diamond particles under agitation, is titrated and leaked using constant pressure
Bucket adds in sodium hydroxide solution, then adds in reducing agent and is restored, obtains the diamond solution of particles of magnetic material load.Its
One of it and specific embodiment one to four are identical.
Diamond solution prepared by present embodiment is the diamond ethylene glycol solution of particles of magnetic material load.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：The hydroxide
Sodium solution mass concentration is 30%, and the speed of addition is 0.1~10mL/min.Other phases one of with specific embodiment one to five
Together.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：The solubility
Mixing of the metal salt for one or more of molysite, nickel salt and cobalt salt.Other phases one of with specific embodiment one to six
Together.
Soluble metallic salt is molysite, nickel salt and cobalt salt in present embodiment when being a variety of mixing, by arbitrary ratio.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Magnetic in step 3
The diamond obturator particle of property material load accounts for the 1~60% of Silica hydrogel composite wood total volume.Other and specific embodiment
One of one to seven is identical.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：Step 3 China and foreign countries
The magnetic field intensity for putting magnetic field is 0.01~2T.It is other identical with one of specific embodiment one to eight.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：It is solid in step 3
Change the time for 10~for 24 hours.It is other identical with one of specific embodiment one to nine.
Present embodiment can shorten hardening time by heating.
Specific embodiment 11：Unlike one of present embodiment and specific embodiment one to ten：In step 3
Accelerate to cure by the way of heating.It is other identical with one of specific embodiment one to ten.
Beneficial effects of the present invention are verified using following embodiment：
Embodiment one：
A kind of preparation method for improving Silica hydrogel composite wood heat conductivility of the present embodiment, specifically carries out according to the following steps：
First, by FeCl3·6H2O and FeSO4·7H2The mixed aqueous solution of O, Fe2+With Fe3+Molar ratio is 1: 2, in stirring bar
Diamond particles are added under part, then heating water bath is to 60 DEG C, under nitrogen protection, stirs 10min, control mixing speed is
750r/min uses constant pressure titration funnel to add in mass concentration as 30% sodium hydroxide solution, and the speed of addition is 1mL/
Min, then constant temperature stirring the reaction was continued 1.5h, obtains the diamond solution of particles of magnetic material load；Wherein magnetic material
Grain is 1: 8 with diamond particles mass ratio；Diamond particles are monocrystalline micron order diamond particle；
2nd, the diamond solution strong magnet washing and depositing for obtaining step 1 detaches supernatant liquor, with distilled water repeatedly
Washing precipitate, until the pH of eluting water is 7；Then sediment is dried in vacuo, obtains the diamond filling of magnetic material load
Body particle；
3rd, the diamond obturator particle that the magnetic material for obtaining Silica hydrogel and step 2 loads mixes, mechanical agitation
It mixes to uniform, then mixture is put into Teflon mould, deaeration 10 minutes, mold is taken out under vacuum condition, is put
It puts in external magnetic field, magnetic field intensity 0.08T is fully cured, and completes a kind of raising Silica hydrogel composite wood heat conductivility
Preparation method.
Diamond particles are pre-processed in step 1：Diamond particles are screened using sieve, then successively in acetone, nothing
It is cleaned by ultrasonic 10min in water-ethanol, deionized water, dries up.
When to measure in Silica hydrogel composite wood manufactured in the present embodiment diamond volume content be 14%, thermal conductivity is
1.4W/mK。
The surface topography photo of diamond particles is as shown in Figure 1 before the present embodiment magnetic loading；
The surface topography photo of diamond particles is as shown in Figure 2 after the present embodiment magnetic loading；
The surface topography photo of diamond particle surfaces magnetic-particle is as shown in Figure 3 after the present embodiment magnetic loading；
The diamond surface element composition Energy Dispersive X spectrogram of the present embodiment magnetic material load is as shown in Figure 4；
The X-ray diffraction spectrogram of diamond surface is as shown in Figure 5 before and after the load of the present embodiment magnetic material；Wherein a is magnetic
Property load diamond, b Fe3O4, c is single-crystal diamond；
The hysteresis loop figure of diamond is as shown in Figure 6 before and after the load of the present embodiment magnetic material；Wherein A is magnetic loading gold
Hard rock, B are single-crystal diamond；
The shape appearance figure of the present embodiment composite sheet inner section direction oriented alignment diamond is as shown in Figure 7；
The shape appearance figure of direction oriented alignment diamond is as shown in Figure 8 in the present embodiment composite sheet inside face.
It can be obtained by above-mentioned test result：
1. nanoscale ferriferrous oxide particles uniform fold on single-crystal diamond surface；
2. the diamond particles of supported magnetic ferroferric oxide can respond external magnetic field, corresponding magnetic is generated
Square；
3. the diamond particles of magnetic loading can prolong magnetic direction under the action of external magnetic field is oriented arrangement, shape
Into cylindrical particle beam, this structure can be fixed in Silica hydrogel solidification process.
4. the thermal conductivity of oriented diamond/Silica hydrogel of volume fraction 14% reaches 1.4W/mK, Silica hydrogel is significantly improved
Thermal conductivity.
Embodiment two：
A kind of preparation method for improving Silica hydrogel composite wood heat conductivility of the present embodiment, specifically carries out according to the following steps：
First, by NiCl2·6H2O adds in ethylene glycol dissolving, adds in diamond particles under agitation, is titrated using constant pressure
Funnel adds in the sodium hydroxide solution that mass concentration is 30%, and the speed of addition is 1mL/min, then adds in the water-soluble of hydrazine hydrate
Liquid is restored, and obtains the diamond solution of particles of magnetic material load；Wherein particles of magnetic material and diamond quality ratio are 1
∶4；
2nd, the diamond solution strong magnet washing and depositing for obtaining step 1 detaches supernatant liquor, with distilled water repeatedly
Washing precipitate, until the pH of eluting water is 7；Then sediment is dried in vacuo, obtains the diamond filling of magnetic material load
Body particle；
3rd, the diamond obturator particle that the magnetic material for obtaining Silica hydrogel and step 2 loads mixes, mechanical agitation
It mixes to uniform, then mixture is put into Teflon mould, deaeration 10 minutes, mold is taken out under vacuum condition, is put
It puts in external magnetic field, magnetic field intensity 0.2T is fully cured, and completes a kind of raising Silica hydrogel composite wood heat conductivility
Preparation method.
Diamond particles are pre-processed in step 1：Diamond particles are screened using sieve, then successively in acetone, nothing
It is cleaned by ultrasonic 10min in water-ethanol, deionized water, dries up.
Embodiment three：
A kind of preparation method for improving Silica hydrogel composite wood heat conductivility of the present embodiment, specifically carries out according to the following steps：
First, by Fe (NO3)3·9H2O adds in ethylene glycol dissolving, diamond particles is added under agitation, using constant pressure
It titrates funnel and adds in the sodium hydroxide solution that mass concentration is 30%, the speed of addition is 1mL/min, then adds in sodium borohydride
Aqueous solution restored, obtain particles of magnetic material load diamond solution；Wherein particles of magnetic material and diamond matter
Amount is than being 1: 4；
2nd, the diamond solution strong magnet washing and depositing for obtaining step 1 detaches supernatant liquor, with distilled water repeatedly
Washing precipitate, until the pH of eluting water is 7；Then sediment is dried in vacuo, obtains the diamond filling of magnetic material load
Body particle；
3rd, the diamond obturator particle that the magnetic material for obtaining Silica hydrogel and step 2 loads mixes, mechanical agitation
It mixes to uniform, then mixture is put into Teflon mould, deaeration 10 minutes, mold is taken out under vacuum condition, is put
It puts in external magnetic field, magnetic field intensity 0.2T is fully cured, and completes a kind of raising Silica hydrogel composite wood heat conductivility
Preparation method.
Diamond particles are pre-processed in step 1：Diamond particles are screened using sieve, then successively in acetone, nothing
It is cleaned by ultrasonic 10min in water-ethanol, deionized water, dries up.
Example IV：
A kind of preparation method for improving Silica hydrogel composite wood heat conductivility of the present embodiment, specifically carries out according to the following steps：
First, by CoC4H6O4·4H2O adds in ethylene glycol dissolving, diamond particles is added under agitation, using perseverance
Pressure titration funnel adds in the sodium hydroxide solution that mass concentration is 30%, and the speed of addition is 1mL/min, then adds in hydrazine hydrate
Aqueous solution restored, obtain particles of magnetic material load diamond solution；Wherein particles of magnetic material and diamond matter
Amount is than being 1: 4；
2nd, the diamond solution strong magnet washing and depositing for obtaining step 1 detaches supernatant liquor, with distilled water repeatedly
Washing precipitate, until the pH of eluting water is 7；Then sediment is dried in vacuo, obtains the diamond filling of magnetic material load
Body particle；
3rd, the diamond obturator particle that the magnetic material for obtaining Silica hydrogel and step 2 loads mixes, mechanical agitation
It mixes to uniform, then mixture is put into Teflon mould, deaeration 10 minutes, mold is taken out under vacuum condition, is put
It puts in external magnetic field, magnetic field intensity 0.2T is fully cured, and completes a kind of raising Silica hydrogel composite wood heat conductivility
Preparation method.
Diamond particles are pre-processed in step 1：Diamond particles are screened using sieve, then successively in acetone, nothing
It is cleaned by ultrasonic 10min in water-ethanol, deionized water, dries up.
Claims (10)
1. it is a kind of improve Silica hydrogel composite wood heat conductivility preparation method, it is characterised in that this method specifically according to the following steps into
Row：
First, using soluble metallic salt and diamond particles as raw material, the diamond solution of particles of magnetic material load is prepared；Wherein
The particles of magnetic material of generation is 1 with diamond quality ratio: (0.1~20)；
2nd, the diamond solution strong magnet washing and depositing for obtaining step 1 detaches supernatant liquor, is washed repeatedly with distilled water
Sediment, until the pH of eluting water is 7；Then sediment is dried in vacuo, obtains the diamond obturator of magnetic material load
Grain；
3rd, the diamond obturator particle that the magnetic material for obtaining Silica hydrogel and step 2 loads mixes, mechanical agitation mixing
It is put into mold to uniform, then by mixture, deaeration 5~15 minutes, mold is taken out under vacuum condition, is placed on external magnetic field
In, it is fully cured, completes a kind of preparation method for improving Silica hydrogel composite wood heat conductivility.
A kind of 2. preparation method for improving Silica hydrogel composite wood heat conductivility according to claim 1, it is characterised in that step
Diamond particles are pre-processed in rapid one：Using sieve screen diamond particles, then successively in acetone, absolute ethyl alcohol, go
It is cleaned by ultrasonic 10min in ionized water, dries up.
A kind of 3. preparation method for improving Silica hydrogel composite wood heat conductivility according to claim 1, it is characterised in that step
Diamond particles are monocrystalline or polycrystalline micro diamond particles in rapid one, and average grain diameter is 1~100 μm.
A kind of 4. preparation method for improving Silica hydrogel composite wood heat conductivility according to claim 1, it is characterised in that step
The method that the diamond solution of particles of magnetic material load is prepared in rapid one is as follows：
Soluble ferric iron salt is dissolved in water, adds in diamond particles under agitation, then heating water bath is to 25 DEG C~80 DEG C,
Under inert atmosphere argon gas or nitrogen protection, 10~20min is stirred, control mixing speed is 500-1000r/min, using perseverance
Pressure titration funnel adds in sodium hydroxide solution, and then constant temperature stirring the reaction was continued 1~3h, obtains the gold of particles of magnetic material load
Hard rock solution.
A kind of 5. preparation method for improving Silica hydrogel composite wood heat conductivility according to claim 1, it is characterised in that step
The method that the diamond solution of particles of magnetic material load is prepared in rapid one is as follows：
Soluble metallic salt plus ethylene glycol are dissolved, add in diamond particles under agitation, is added using constant pressure titration funnel
Enter sodium hydroxide solution, then add in reducing agent and restored, obtain the diamond solution of particles of magnetic material load.
6. a kind of preparation method for improving Silica hydrogel composite wood heat conductivility according to claim 4 or 5, it is characterised in that
The sodium hydroxide solution mass concentration is 30%, and the speed of addition is 0.1~10mL/min.
A kind of 7. preparation method for improving Silica hydrogel composite wood heat conductivility according to claim 5, it is characterised in that institute
State mixing of the soluble metallic salt for one or more of molysite, nickel salt and cobalt salt.
A kind of 8. preparation method for improving Silica hydrogel composite wood heat conductivility according to claim 1, it is characterised in that step
The diamond obturator particle that magnetic material loads in rapid three accounts for the 1~60% of Silica hydrogel composite wood total volume.
A kind of 9. preparation method for improving Silica hydrogel composite wood heat conductivility according to claim 1, it is characterised in that step
The magnetic field intensity of external magnetic field is 0.01~2T in rapid three.
A kind of 10. preparation method for improving Silica hydrogel composite wood heat conductivility according to claim 1, it is characterised in that step
In rapid three hardening time for 10~for 24 hours.
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| CN112976438A (en) * | 2021-01-28 | 2021-06-18 | 华中科技大学 | Preparation method and product of directionally interconnected high-thermal-conductivity interface material |
| CN116462971A (en) * | 2023-04-24 | 2023-07-21 | 宁波能之光新材料科技股份有限公司 | Preparation method of heat-conducting insulating silicon gel composite material for lithium battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110117484A (en) * | 2019-06-11 | 2019-08-13 | 哈尔滨工业大学 | A kind of preparation method having directive thermal conductive silicon Gel composite sheets material |
| CN112457821A (en) * | 2020-12-09 | 2021-03-09 | 中国科学院深圳先进技术研究院 | Heat-conducting gel containing diamond and liquid metal and preparation and application thereof |
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| CN112976438B (en) * | 2021-01-28 | 2022-07-12 | 华中科技大学 | Preparation method and product of directionally interconnected high-thermal-conductivity interface material |
| CN116462971A (en) * | 2023-04-24 | 2023-07-21 | 宁波能之光新材料科技股份有限公司 | Preparation method of heat-conducting insulating silicon gel composite material for lithium battery |
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