CN109810599A - A kind of anti-corrosion heat radiation coating and preparation method thereof - Google Patents
A kind of anti-corrosion heat radiation coating and preparation method thereof Download PDFInfo
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Abstract
A kind of anti-corrosion heat radiation coating, is made of the raw material of following weight percent: polyacrylic resin 74.9~82.9%, Nano diamond 5~10%, nano silica 4~7%, polyacrylic acid 0.7%, polyacrylamide 2.3%, coupling agent A-1100 2%, defoaming agent 7,500 0.1%, dimethlbenzene 3%.The invention also discloses preparation methods simultaneously.The present invention has corrosion resistant characteristic using nano silica and Nano diamond itself, is added into target coating, good supporting role can not only be played in coating gap, improve the hardness and wearability of coating.
Description
Technical field
The invention belongs to heat radiation coating technical fields more particularly to a kind of anti-corrosion heat radiation coating and preparation method thereof.
Background technique
The rapid development of science and technology, the intensive and miniaturization of the high frequency of electronic device, high speed and integrated circuit so that
The overall power density of unit volume electronic device and calorific value increase by a wide margin, to make the cooling problem and height of electronic device
Warm anti-corrosion becomes more and more prominent.The cooling capacity and corrosion resistance of conventional cooling system are greatly challenged, especially
In technical fields such as the energy, automobile, air-conditioning, agricultural, chemical industry, aerospace, microelectronics information, to raising radiating efficiency, anti-corrosion
The technologies such as erosion ability have higher requirement.Coating technology is applied to electronic field by researcher, to solve its heat dissipation problem,
Achieve good effect.Since coating technology meets electronic equipment lightweight, portable requirement, and coating well
The good results are evident for radiating and cooling, so coating technology have developed rapidly in electronic field.
Coating technology, which refers to, smears a coating in body surface (high heat flux regions), by the high thermal conductivity of coating, high spoke
Penetrating property achievees the purpose that flash heat transfer.Coating heat dissipation is by improving body surface radiation efficiency (especially raising infra-red radiation
Efficiency), augmented heat dissipation performance, have it is at low cost, implement the features such as simple.Heat loss through radiation High tailored coating is directly constructed
To the body surface for wanting radiating and cooling, can be reduced with heat of 8~13.5 μm of infrared wavelengths on airspace radiating object
Body surface and internal temperature, radiating and cooling are obvious.Coating heat dissipation is not influenced by surrounding medium, can be made in vacuum environment
With.
Base-material is the continuous film that coating is formed, and is the main matter of firm attachment on substrate surface.It radiates in anti-corrosion
In the preparation of coating, base-material is very important, it is necessary to be provided simultaneously with the performances such as anti-corrosion, weatherability and strong adhesive force.Coating
In commonly concentrate resin mainly and have acrylic resin, alkyd resin, aniline-formaldehyde resin, epoxy resin, polyester resin, poly- ammonia
Ester, vinylite, phthalic resin etc..Compared with other resins, acrylic resin is compared to other resins, propylene
Acid resin generally includes the advantages that good weatherability, moisture-proof, wearability, ultraviolet resistance irradiation, while having good attached
Put forth effort, good mechanical performance, good thermal conductivity and radiativity.
Using polyacrylic resin as matrix, by the way that the filler of high thermal conductivity and high radiation is added come thermally conductive, the spoke of strengthened coat
It penetrates and anti-corrosion ability, and then achievees the purpose that cooling and heat dissipation.Heat filling is divided into inorganic and organic two class, main inorganic thermally conductive
Filler has boron nitride, aluminium nitride, silicon carbide, aluminium oxide, magnesia etc.；And organic heat filling is mainly based on fiber, if not
Become rusty steel fibre, carbon fiber, graphite etc..The addition of these heat fillings can effectively improve the thermal coefficient of composite material, improve and dissipate
The thermal efficiency.
Although all achieving preferable achievement to the research of coating technology both at home and abroad, in field of electronic devices to painting
More stringent requirements are proposed for layer technology.Under special operation condition, coating needs higher hardness, higher corrosion resistance, good
Thermal diffusivity etc., but at present using polyacrylic resin as the coating of matrix cannot hardness, it is corrosion-resistant, in terms of it is preferably full
Foot is current to be needed.
Summary of the invention
The purpose of the present invention is to provide a kind of anti-corrosion heat radiation coatings, while it is of the invention another for providing preparation method
Goal of the invention.
Based on above-mentioned purpose, the present invention takes following technical scheme:
A kind of anti-corrosion heat radiation coating, is made of the raw material of following weight percent: polyacrylic resin 74.9~82.9%,
Nano diamond 5~10%, nano silica 4~7%, polyacrylic acid 0.7%, polyacrylamide 2.3%, coupling agent A-
1100 2%, defoaming agent AFE-7500 0.1%, dimethlbenzene 3%.
The Nano diamond particle size distribution range is 5~20nm, and the nano silica is club-like fiber, diameter
Range be 5~20nm, length range be 50~100nm, the present invention in, using club-like fiber nano silica with it is spherical
Nano silica is big compared to contact surface area, and mutually entangling between matrix material molecules can be improved in large specific surface area
Power is twined, while fibrous nano silica permeability also with higher itself and particle inner surface are more easier contact
Advantage easily occurs active reaction with the other ingredients of coating, mentions in this way, Nano diamond can be loaded and be transmitted along fiber
The stability and weatherability of high coating, are also improved from coating overall performance；In order to make the nano-silica of club-like fiber
SiClx plays better effect, and the thickness of film should be greater than the length of fiber, but be not more than 20%.
The preparation method of the anti-corrosion heat radiation coating, comprising the following steps:
1) 70~80 DEG C of water of 3 times of quality of coupling agent is first added into coupling agent A-1100 and stirs evenly, stands
30min is fully hydrolyzed coupling agent, adds Nano diamond and nano silica and stirs 30~35min under 1000rpm
Afterwards, the Nano diamond and nano silica that coupling agent is contained on surface are dried to obtain in 105 DEG C；
2) acrylic resin, polyacrylamide, polyacrylic acid are mixed to and are stirred under 800rpm revolving speed 20~30min,
The Nano diamond and nano silica of coupling agent are contained in the surface that step 1) is added, and side edged is turned with 500~600rpm's
Speed stirring after being added to coupling agent mixed solution, continues to keep revolving speed stirring 1h, while defoaming agent 7500 is added, stir
Dimethlbenzene is added afterwards to continue to stir 6h, makes material dispersion uniformly up to anti-corrosion heat radiation coating；
In step 1), the Nano diamond and nano silica must pass through following surface treatment:
A) silica is put into crucible, covers crucible cover, be put into Muffle furnace, heated up according to staged: room temperature arrives
120 DEG C, heating rate is 1 DEG C/min, keeps the temperature 30min, then be warming up to 400 DEG C by 120 DEG C, keeps the temperature 30min, then risen by 400 DEG C
Temperature keeps the temperature 1h, naturally cools to room temperature after heat preservation to 750 DEG C；Purpose is the size in order to remove silica surface,
Obtain pure surface；
B) concentrated sulfuric acid that concentration is 98% is added in cast iron autoclave, reaction kettle surface is passivated, so
Reaction kettle is cleaned with deionized water afterwards, until the pH value of aqueous solution is about 6.50~7.00 in reaction kettle；
C) be 5~10nm by particle size range, the Nano diamond of 100~150ct is put into above-mentioned autoclave, about
/ 10th of reaction kettle volume are added the deionized water of 8~10 times of Nano diamond quality, reaction kettle are carried out closed, put
Enter in thermostatic drying chamber and heat, using slow heating mode, 1 DEG C/min, is warming up to 120 DEG C, constant temperature 30min, natural cooling obtains
To Nano diamond turbid；
D) Nano diamond turbid is centrifuged 10min in the case where revolving speed is 8000~10000rpm, outwells supernatant liquor；
E) 600~6000g Nano diamond and nano silica gradually plasma modification: are put into Nanjing generation cutting edge of a knife or a sword
In the rectilinear plasma handling system of SF-Z-60L type, 30min is handled under the conditions of pure hydrogen, 200 DEG C for the treatment of temperature, hydrogen stream
Measure 60cm3/ min obtains the modified Nano diamond in surface or nano silica.The present invention is by making in hydrogen electric discharge machining in gas
For Hydrogen Separation at hydrogen ion and electronics, electron mass is small, can obtain energy more higher than free radical, and Nano diamond or receives
The oxygen atom of rice silica surface reacts, so that Nano diamond or nano-silica surface have more reactions
Free radical increases nano diamond nano silica surface activity, final to obtain the modified Nano diamond in surface or nanometer
Silica.
In application, by acetone, dibutyl phthalate with mass ratio 3:1 hybrid modulation at retarder thinner, and will add
Being added in above-mentioned coating adjusts its viscosity to 12~15s aerial spraying.The coating after dilution is sprayed with air gun
In processed substrate surface, air gun pressure is 0.5~0.7Mpa, and spray gun distance is 20~25cm, the mobile speed of spray gun
Degree is 30~40cm/s, and static 1~3min is put into high temperature oven after waiting levelling to be coated, and baking-curing forms a film at 145 DEG C,
It is acrylic resin composite coating that 30min or so, which takes out,.
In the present invention, the Nano diamond of addition is a kind of novel nano material nontoxic to the human body, harmless, without side-effects
Material, it is high, wear-resisting with hardness, there is high thermal conductivity and heat dissipation performance；Nano silica be it is a kind of it is with high purity, nontoxic, harmless,
The material of high temperature resistant and good heat dissipation effect；The polyacrylic resin coating of Nano diamond and nano silica is added with good
Good adhesive force, good impact flexibility, good coefficient of heat transfer, good corrosion resistance and higher hardness, wherein nanometer
Diamond has good coefficient of heat transfer, is filled into coating gap of the invention, forms island-island structure, can be timely and effective
Export base-material heat, play good heat dissipation effect；Secondly, in plane, nano silica shape in acrylic resin
At random bridging mode；In solid, nano silica is uniformly distributed in acrylic resin, forms reticular structure, is prevented
The only creep of acrylic resin, while the heat of polyacrylic resin can be made to transmit outward by silica；
Since Nano diamond and nano silica have very low dielectric constant, can easily be penetrated by infrared,
Therefore the addition of Nano diamond and nano silica helps to improve the heat loss through radiation speed of polyacrylic resin
Therefore, compared with prior art, the invention has the following advantages: the present invention is using nano silica and receives
Rice diamond itself has corrosion resistant characteristic, is added into target coating, can not only play in coating gap very well
Supporting role, improve the hardness and wearability of coating.In target coating be added by the modified Nano diamond in surface with
Nano silica increases the roughness between substrate and base-material, improve adhesive force, while can also hinder oxidation material into
Enter wherein, improves the corrosion resistance of target coating.The polyacrylic resin of filler nanometer diamond and nano silica is added
Coating meets experimental standard and GB/T1732-1993 after salt mist experiment.Therefore, Nano diamond and nano-silica is added
The coating of SiClx has good corrosion resistance.
Detailed description of the invention
Fig. 1 is influence of the Nano diamond to impact resistance；
Fig. 2 is influence of the nano silica to impact resistance；
Fig. 3 is that Nano diamond influences radiation coefficient；
Fig. 4 is that nano silica influences radiation coefficient；
Fig. 5 is the influence of Nano diamond and nano silica to impact resistance；In figure, ND: Nano diamond；
Fig. 6 is that Nano diamond and nano silica influence radiation coefficient；In figure, ND: Nano diamond.
Specific embodiment
With specific embodiment, the present invention will be further described below.Ct is unit of weight, carat, 1g=5ct.
The nano silica of club dress fiber is by silica by techniques systems such as melting, wire drawing, ball milling, particle refinements
It is standby to obtain.
Embodiment 1-4
To keep specification brief, each component of embodiment 1-4 provides in table form.Specific each composition content is shown in Table 1
It is shown.
The content (mass fraction (%)) of 1 embodiment 1-3 each component of table
| Material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Performance |
| Polyacrylic resin | 82.9 | 79.9 | 77.9 | 74.9 | Base-material |
| Nano diamond | 5 | 5 | 10 | 10 | Filler |
| Nano silica | 4 | 7 | 4 | 7 | Filler |
| Polyacrylic acid | 0.7 | 0.7 | 0.7 | 0.7 | Levelling agent |
| Polyacrylamide | 2.3 | 2.3 | 2.3 | 2.3 | Dispersing agent |
| A-1100 | 2 | 2 | 2 | 2 | Coupling agent |
| 7500 | 0.1 | 0.1 | 0.1 | 0.1 | Defoaming agent |
| Dimethlbenzene | 3 | 3 | 3 | 3 | Preservative |
In embodiment 1-4, of length no more than 100nm of nano silica is more preferable in order to play nano silica
Effect, the thickness of film should be greater than the length of fiber, but not be preferably greater than 20%, therefore the thickness of film is set as 100 ± 20nm.
The preparation method of anti-corrosion heat radiation coating described in embodiment 1-4, comprising the following steps:
1) first it is slowly added to 70~80 DEG C of water of 3 times of quality of coupling agent into coupling agent A-1100 and stirs evenly, it is quiet
Setting 30min is fully hydrolyzed coupling agent, add Nano diamond and nano silica stir 30 under 1000rpm~
After 35min, the Nano diamond and nano silica that coupling agent is contained on surface are dried to obtain in 105 DEG C；
2) acrylic resin, polyacrylamide, polyacrylic acid are mixed to and are stirred under 800rpm revolving speed 20~30min,
The Nano diamond and nano silica of coupling agent are contained in the surface that step 1) is added, and side edged is turned with 500~600rpm's
Speed stirring after being added to coupling agent mixed solution, continues to keep revolving speed stirring 1h, while defoaming agent 7500 is added, stir
Dimethlbenzene is added afterwards to continue to stir 6h, makes material dispersion uniformly up to anti-corrosion heat radiation coating；
In step 1), the Nano diamond and nano silica must pass through following surface treatment:
A) silica is put into crucible, covers crucible cover, be put into Muffle furnace, heated up according to staged: room temperature arrives
120 DEG C, heating rate is 1 DEG C/min, keeps the temperature 30min, then be warming up to 400 DEG C by 120 DEG C, keeps the temperature 30min, then risen by 400 DEG C
Temperature keeps the temperature 1h, naturally cools to room temperature after heat preservation to 750 DEG C；Purpose is the size in order to remove silica surface,
Obtain pure surface；
B) concentrated sulfuric acid that concentration is 98% is added in cast iron autoclave, reaction kettle surface is passivated, so
Reaction kettle is cleaned with deionized water afterwards, until the pH value of aqueous solution is about 6.50~7.00 in reaction kettle；
C) be 5~10nm by particle size range, the Nano diamond of 100~150ct is put into above-mentioned autoclave, about
/ 10th of reaction kettle volume are added the deionized water of 8~10 times of Nano diamond quality, reaction kettle are carried out closed, put
Enter in thermostatic drying chamber and heat, using slow heating mode, 1 DEG C/min, is warming up to 120 DEG C, constant temperature 30min, natural cooling obtains
To Nano diamond turbid；
D) Nano diamond turbid is centrifuged 10min in the case where revolving speed is 8000~10000rpm, outwells supernatant liquor；
E) 600~6000g Nano diamond and nano silica gradually plasma modification: are put into Nanjing generation cutting edge of a knife or a sword
In the rectilinear plasma handling system of SF-Z-60L type, 30min is handled under the conditions of pure hydrogen, 200 DEG C for the treatment of temperature, hydrogen stream
Measure 60cm3/ min obtains the modified Nano diamond in surface or nano silica.
1, performance detection
Testing coating sample each group component is as shown in table 2.
Table 2 detects coating each component content
In order to determine the optimum filling amount of Nano diamond and nano silica in polyacrylic resin, first to receiving
The influence of the performance of polyacrylic resin is studied in rice silica and the filling of Nano diamond single substance.It studies first
Influences of the different nano silica additive amounts to coating performance.
1) adhesive force detects
It is required according to ISO2409-2007, selects aluminium sheet as coating test substrate, coating is measured using F107 cross hatch device
Adhesive force.Coating coating before, need to pre-process substrate surface, key step have sand paper polishing derust, alkali cleaning
It deoils, acid pickling and rust removing, washing, drying.Remove the most iron rust of substrate surface；Using saponification, substrate table is removed with alkali cleaning
The greasy dirt in face；It is difficult to the rusty stain removed, strong acid is added using the reaction principle of acid and oxide and removes；Finally with distillation washing
Only, it dries.Aluminium sheet coating sample is prepared, marks the shape of cross grid on template with cross hatch device until aluminium sheet substrate；With hair
Brush is respectively brushed 5 times along the cornerwise direction of cross grid, is tightly attached on notch with adhesive tape and is pulled open rapidly；With amplification sem observation, repeat
Test of many times, the standard of 3 coating adhesion of the table of comparisons, determines the grade of coating adhesion.
The classification standard of 3 coating adhesion of table
Illustrate: 0 grade represents outstanding, and 1 grade represents and can satisfy industrial requirements, indicates that adhesive force is very poor after 2 grades, Bu Nengman
Sufficient coating use demand.
It is tested according to adhesive force of the above method to different target coating under room temperature, as shown in table 4:
The test of 4 paint adhesion of table
| Serial number | A | B | C | D | E | F | G | I | J | K | O |
| Adhesive force (grade) | 0 | 0 | 0 | 0 | 1 | 2 | 0 | 0 | 0 | 1 | 1 |
From testing result as can be seen that Nano diamond or nano silica are added in base-material to the adhesive force of coating
It has a certain impact, when not adding any filler in coating, the edge of the notch on coating is completely smooth, and grid edge does not have
There is any peeling, adhesive force grade is 0 grade.Nano diamond is added in coating, when Nano diamond additive amount be 1%~
When 10%, the edge of the cross recess of coating notch does not peel off aliquation phenomenon, and adhesive force grade is 0 grade；When filler nanometer gold
When hard rock additive amount is 15%, there is peeling at the edge or intersection of notch, and less than 5%, adhesive force grade is 1 grade；When filler is received
When rice diamond additive amount is 20%, there is peeling at the edge or intersection of notch, are greater than 5%, less than 15%, adhesive force grade is
2 grades.Nano silica is added in coating, when additive amount is 1%~7%, the side of the cross notch of coating notch
Edge does not have aliquation and peeling phenomenon, and adhesive force grade is 0 grade；When filler nanometer silica additive amount is 11% and 15%,
There is peeling at the edge or intersection of notch, and less than 5%, adhesive force grade is 1 grade.
It sees from the above, when filler nanometer diamond or nano silica additional amount are 1%, to the adhesive force of coating
Very little is influenced, but with the increase of filler additive amount, the adhesive force of coating is still 0 grade, but when excessive addition filler nanometer gold
Hard rock and nano silica then reduce the adhesive force of target coating.Filler nanometer Buddha's warrior attendant is added this is mainly due to a small amount of
Stone or nano silica increase the roughness between base-material and substrate, increase the foundation area of coating and substrate, therefore
The adhesive force of coating is not influenced.When excessive Nano diamond or nano silica is added, reunited, in base
When coating on material, the contact area of polyacrylic resin and substrate in coating is reduced, reduces the adhesive force of coating.Therefore,
With the increase of filling adding amount, adhesive force is gradually decreased.
2) hardness determination
The coating hardness that target coating is formed is also one of ability of resistance to deformation, i.e. coating surface is to being applied to it
The resistance that object is showed.It is measured according to GB/T6739-2006 using pencil, the hardness level of pencil is by soft to hard: 5B
To 5H.One section of the pencil wood for pruning about 5~6mm leaves to scratch smooth cylindrical pencil pen core.Pencil is consolidated by clip
After fixed, pencil is pressed downward on the coating surface under the load of 750g ± 10g with 45° angle, with the speed of 0.5mm/s~1mm/s
At least distance of 7mm is pushed towards the direction for leaving operator, scratch result is evaluated using 6~10 times of magnifying glass.If super
The scratch for crossing 3mm, the hardness for reducing pencil repeats to test, until the scratch of 3mm no longer occurs.With do not occur 3mm and
The hardness of the most hard pencil of the above scratch indicates the hardness of coating.Testing result is as shown in table 5.
5 Hardness results of table
| Serial number | A | B | C | D | E | F | G | I | J | K | O |
| Pencil hardness | B | HB | F | F | H | 2H | HB | HB | F | F | H |
From testing result as can be seen that Nano diamond or nano silica are added in base-material the hardness of coating
Certain influence, when not adding any filler in coating, coating quality is softer, cannot be marked on its surface using B grades of pencils
Scratch.When the additional amount of Nano diamond is 1%, the hardness of coating is HB grades；When Nano diamond additional amount be 5~
When 10%, the hardness of coating is F grades；When Nano diamond additional amount is 20%, coating hardness is 2H grades.Diamond is due to tool
There are the characteristics such as high rigidity, high abrasion, is added in coating as filler, the hardness of coating is increased, therefore, with Nano diamond
Additional amount increase, the hardness of coating increases therewith.
When the additional amount of nano silica is 1%, the hardness of coating is HB grades；When the additional amount of nano silica
When being 4%, the hardness of coating is HB grades；When nano silica additional amount is 7~11%, coating hardness is F grades；Work as nanometer
When the additional amount of silica is 15%, the hardness of coating is H grades.Although the hardness of the not no diamond of silica is high, due to
It is club-like, and more short and small, therefore rigidity with higher, is mutually interconnected by the coupling agent of silica surface with base-material
It connects, forms " skeleton " in base-material, increase the hardness of coating, therefore, with the increase of the additional amount of nano silica, apply
The hardness of layer increases therewith.
3) the impact resistance detection of target coating
Impact resistance is the ability measured material and resist impact load.According to the requirement of GB/T1732-93, rushed using paint film
Device is hit to be measured coating.The sample for preparing steel plate coating, steel plate is placed on impactor, falls within weight in template as far as possible
The heart, coating is face-up, and weight (standard weights is 1kg) is freely fallen by some height, and each Height Impact 3~5 times tests are used
Whether 4 times of amplification sem observation paint films cracked, phenomena such as peeling off, and such as without obvious crackle and peeling phenomenon, increases the height fallen
Degree, is tested again, until cracked or peeling, not cause the maximum height of breakdown of coating to indicate, unit is: cm.Examination
It is as depicted in figs. 1 and 2 to test result.
As can be known from Fig. 1, the additive amount of Nano diamond has large effect to the impact resistance of coating material, with
The increase of Nano diamond content, the impact resistance height of polyacrylic resin coating first increases to be gradually decreased afterwards.Polyacrylic acid
When being free of Nano diamond in resin, impact resistance height is 60cm；When the addition mass percent of Nano diamond is 1%,
The impact resistance height of target paint coatings is 61cm, improves 1.7%；When the addition mass percent of Nano diamond is 5%
When, the impact resistance height of target paint coatings is 65cm, 8.3% is improved, with the increase of additive amount, Nano diamond addition
Amount is 5~10%, and coating impact resistance height reaches maximum value, there is a stable additive amount, and impact resistance height is 65cm；Work as nanometer
When diamond additive amount is 15%, the impact resistance height of coating is 50cm, 16.7% is reduced, when Nano diamond additive amount is
When 20%, the impact resistance height of coating is 48cm, reduces 20%, has not met coatings industry production standard.
With the increase of the additive amount of Nano diamond in polyacrylic resin, the impact resistance height of target paint coatings is first
It is reduced after raising, the main reason for this phenomenon occur is: when the additive amount of Nano diamond is no more than 10%, target coating
Roughness between coating and substrate increases, and the increase of roughness is conducive to increase the contact area between base-material and substrate, from
And increase the adhesive force of coating, and then improve the impact resistance height of coating.When Nano diamond incrementss be 15~
When 20%, since in coating preparation process, Nano diamond is filled into acrylic resin crosslinking gap, strand is hindered
Movement, and then increase the hardness of coating, when being impacted, be easy to happen cracking；Excessive Nano diamond is rolled into a ball
It is poly-, the foundation area of base-material and substrate is reduced instead, as a result leads to falling off for coating.Therefore, when the addition of Nano diamond
When amount is 5~10%, the impact resistance height of acrylic resin coating reaches maximum value, and is most stability range.
From fig. 2 it can be seen that the different additive amounts of nano silica have the impact resistance of coating material
Different influences, when being free of Nano diamond in polyacrylic resin, impact resistance height is 60cm；When adding for nano silica
When to add mass percent be 1%, the impact resistance height of target paint coatings is 62cm, improves 3.3%；Work as nano silica
Addition mass percent when being 4~7%, the impact resistance height of target paint coatings is 67cm, improves 11.7%, is reached most
Stationary value；When nano silica additive amount is 11%, the impact resistance height of coating is 53cm, reduces 11.7%；When receiving
When rice silica additive amount is 15%, the impact resistance height of coating is 52cm, reduces 13.3%.
With the increase of the additive amount of nano silica, the impact resistance height of target paint coatings in polyacrylic resin
First increase reduces afterwards, the main reason for this phenomenon occurs and is: generating this phenomenon mainly because prepared by polyacrylic resin
In the process, it is nano-silica filled into acrylic resin gap when random shape, and fiber surface coupling agent is presented
It is cross-linked to form a random reticular structure with acrylic resin, and then enhances the toughness and hardness of coating material, simultaneously
The roughness between target paint coatings and substrate is increased, the increase of roughness is conducive to increase connecing between base-material and substrate
Contacting surface product, so that the adhesive force of coating be made to increase, and then improves the impact resistance height of coating.When the nano silica of addition
When excessive, the impact resistance height of coating reduces suddenly, mainly since excessive nano silica is reunited, base-material and base
Roughness between material becomes uneven, and contact area reduces, while also causing the hardness of coating uneven, the adhesive force of coating
Decline, impact resistance height are greatly reduced in turn.Therefore, when the additive amount of nano silica is 4~7%, polypropylene tree
The impact resistance height of rouge coating reaches maximum value, and is most stability range.
4) measurement of heat dissipation effect
The content of Nano diamond has thermal dispersant coatings heat dissipation performance from the content size of nano silica different
It influences, according to the experiment condition consistency principle, the addition of single filler various concentration gradient is measured first.
It is measured using cooling effect of the furnace temperature tester to target paint coatings, model SMT-7-128-500-K,
Match aestheticism High Seience Technology Co., Ltd. in Beijing.Working principle is that temperature signal is changed into thermo-electromotive force by thermocouple, using electrical
Instrument comes out the temperature display that this electromotive force is changed into measured matter.Subjects are LED radiator or CPU radiating fin.Through
The workpiece for crossing different disposal is placed in 145 DEG C of insulating boxs, constant temperature 1h, takes out, its cooling is measured in the case where free convection
Curve, cooling extent of the temperature difference for the 15min that cools down as coating, measurement result are as shown in table 6.
The additional amount of the different fillers of table 6 and the cooling extent of corresponding coating
In table as can be seen that when single filler is Nano diamond, the cooling effect of target coating, with nanometer Buddha's warrior attendant
The increase of the additive amount of stone, when the mass percent of nano-diamond filler is 10%, cooling extent reaches maximum value 15.5
DEG C, it is far longer than 4.5 DEG C of the coating for not adding Nano diamond, but as Nano diamond additive amount increases, work as incrementss
When being 15%, cooling extent starts to become smaller.This mainly when Nano diamond additive amount is few, can be uniformly distributed in target and fill out
Expect uniformly distribute heat in coating；When Nano diamond additive amount excess, Nano diamond forms reunion, heat
Amount transmitting is uneven, also just can not timely and effectively give out heat.
It is found that the addition of nano silica also has a certain impact to the cooling effect of target coating in table 6, this master
If being in the coating in unordered mixed and disorderly distribution, forming random netted, nanometer titanium dioxide since nano silica is club-like
Silicon has good thermal coefficient, therefore can play a positive role to the heat dissipation of coating, but the nanometer two excessive with addition
The cooling extent of silica, target coating gradually increases, and when nanometer titanium dioxide silicone content increases to 7%, target coating is most
9.7 DEG C of big cooling extent, but continuing growing with nanometer titanium dioxide silicone content, the cooling extent of target coating gradually drop
It is low, this is mainly due to being excessively added for nano silica, cause to form reunion in the coating, heat dissipation is uneven, can not
Effective export heat, plays its heat dissipation effect.
5) measurement of radiation coefficient
Radiation coefficient (also known as radiance, emissivity, coefficient of blackness, heat emissivity coefficient etc.) is the basic ginseng of the hot physical property of material
One of number, refers to the ratio between actual object and the radiation of black matrix under the same terms (temperature, wavelength and geometrical condition):
In formula: ε (λ, T) is emissivity of the sample in temperature T, and M (λ, T) is that spectral radiance of the sample in temperature T goes out
Degree, M0(λ, T) is spectral radiance out-degree of the black matrix in temperature T.
Radiance measurement is carried out to coating sample using IR-2 type two waveband emissivity measurement instrument, measurement wave band is 1~22 μ
M, blackbody temperature are set as 145 DEG C, after black matrix is stablized, and wave band is different, need to use optical filter, and using the reference sample of known radiance
Plate is corrected at the corresponding temperature.Test result is as shown in Figure 3 and Figure 4.
When not having filler in polyacrylic resin, the radiation coefficient of target coating is 0.67, with Nano diamond content
Increase, the trend constantly increased is presented in the radiation coefficient of coating.When the content of filler nanometer diamond is 5~10%, apply
The radiation coefficient of layer reaches maximum value, is 0.84, radiation coefficient improves 25.4%；With the increase of Nano diamond, when adding
Dosage be 15% when, radiation coefficient improves 20.8%, compared to Nano diamond additive amount be 10% when, reduce 4.7%；
When additive amount be 20% when, radiation coefficient improves 22.4%, compared to Nano diamond additive amount be 10% when, reduce
3.5%.Therefore, when the additive amount of Nano diamond is 5~10%, the radiation coefficient of polyacrylic resin reaches maximum value.
When to add filler in acrylic resin be nano silica, with the increase of filler nanometer dioxide-containing silica,
The radiation coefficient of coating shows the trend of first increases and then decreases.When the content of filler nanometer silica is 1%, coating
Radiation coefficient is 0.70, and radiation coefficient improves 4.5%, when the content of filler nanometer silica is 7%, the radiation of coating
Coefficient reaches maximum value, is 0.79, radiation coefficient improves 17.9%；With the increase of nano silica, when additive amount is
When 11%, radiation coefficient improves 11.9%, compared to nano silica additive amount be 7% when, reduce 5.1%；When adding
Dosage be 15% when, radiation coefficient improves 10.4%, compared to nano silica additive amount be 7% when, reduce
6.3%.Therefore, when the additive amount of nano silica is 4~7%, the radiation coefficient of polyacrylic resin reaches maximum value.
In polyacrylic resin preparation process, it is nano-silica filled into acrylic resin gap when present it is random
State, and fiber surface coupling agent and acrylic resin are cross-linked to form a random reticular structure；Nano diamond is equal
It is even to be dispersed in polyacrylic resin, the structure on " island-bridge-island " is formed with nano silica；Due to Nano diamond and receive
Rice silica improves the radiation coefficient of target coating due to light transmission with higher, wave.
2, containing the coating preparation of compounded mix
By research Nano diamond and nano silica respectively as single filler to polyacrylic resin coating
Heat dissipation performance influence, it has been determined that when as single filler, the adding proportion model of Nano diamond and nano silica
It encloses.According to the above results, when preparing while adding Nano diamond and nano silica filler, to polyacrylic resin coating
Heat dissipation performance influence, paint ingredient is as shown in table 7 below, and experimental index and examination criteria are as shown in table 8.
7 compounded mix each component content of table
8 experimental index of table and examination criteria
| Project | Testing index | Examination criteria |
| Adhesive force (grade) | ≤1 | GB1720 |
| Hardness (Mitsubishi's pencil) | ≥F | GB/T6739 |
| Impact resistance (cm.Kg) | 50 | GB/T1732-1993 |
1) the impact resistance detection of target coating
Impact resistance is the ability measured material and resist impact load.According to the requirement of GB/T1732-93, rushed using paint film
Device is hit to be measured coating.The sample for preparing steel plate coating, steel plate is placed on impactor, falls within weight in template as far as possible
The heart, coating is face-up, and weight (standard weights is 1kg) is freely fallen by some height, and each Height Impact 3~5 times tests are used
Whether 4 times of amplification sem observation paint films cracked, phenomena such as peeling off, and such as without obvious crackle and peeling phenomenon, increases the height fallen
Degree, is tested again, until cracked or peeling, unit is: cm, test results are shown in figure 5.
As can be known from Fig. 5, without addition Nano diamond and nano silica filler in coating, the impact resistance of coating is high
Degree is 60cm, when Nano diamond additive amount is 5%, and nano silica additive amount is 4%, the resistance to punching of target paint coatings
Hitting height is 65cm, and the impact resistance height of target paint coatings improves 8.3%；When Nano diamond additive amount be 5%, nanometer
When silica additive amount is 7%, the impact resistance height of target paint coatings is 66cm, the impact resistance height of target paint coatings
Improve 10%.When Nano diamond additive amount is 10%, and nano silica additive amount is 4%, target paint coatings
Impact resistance height is 64cm, and the impact resistance height of target paint coatings improves 6.7%,；When Nano diamond additive amount is
10%, when nano silica additive amount is 7%, the impact resistance height of target paint coatings is 63cm, target paint coatings
Impact resistance height improves 5%.
From above-mentioned experimental data as can be seen that when one timing of Nano diamond additive amount, the resistance to punching of target coating coating
Height is hit to increase with the increase of the additive amount of nano silica；When nanometer titanium dioxide silicone content is certain, target coating
The impact resistance height of coating is increased with the increase of the additive amount of Nano diamond.
From above-mentioned conclusion, we have observed that Nano diamond and nano silica are received in polyacrylic resin coating
Rice silica forms dimensional network structure, is dispersed throughout in entire coating material, and Nano diamond is filled in coating gap,
Collaboration mutually, improves the hardness of coating, increases the roughness between paint coatings and substrate, improve what coating was hit
Highly.By experiment Testing index table 8 it is found that the target coating of above-mentioned different component filler meets industrial production application standard.
2) hardness determination
The coating hardness that target coating is formed is also one of ability of resistance to deformation, i.e. coating surface is to being applied to it
The resistance that object is showed.It is measured according to GB/T6739-2006 using pencil, the hardness level of pencil is by soft to hard: 5B
To 5H.One section of the pencil wood for pruning about 5~6mm leaves to scratch smooth cylindrical pencil pen core.Pencil is consolidated by clip
After fixed, pencil is pressed downward on the coating surface under the load of 750g ± 10g with 45° angle, with the speed of 0.5mm/s~1mm/s
At least distance of 7mm is pushed towards the direction for leaving operator, scratch result is evaluated using 6~10 times of magnifying glass.If super
The scratch for crossing 3mm, the hardness for reducing pencil repeats to test, until the scratch of 3mm no longer occurs.With do not occur 3mm and
The hardness of the most hard pencil of the above scratch indicates the hardness of coating.Testing result is as shown in table 9.
9 Hardness results of table
| Serial number | L | M | N | P |
| Pencil hardness | F | H | H | H |
From testing result as can be seen that addition Nano diamond and nano silica increase the hard of coating in base-material
Degree, when the additive amount of Nano diamond is 5%, and the additive amount of nano silica is 4%, the hardness of target coating is F grades；
When the additive amount of Nano diamond is 5%, and the additive amount of nano silica is 7%, it is H that the hardness of target coating, which increases,
Grade；When the additive amount of Nano diamond is 10%, and the additive amount of nano silica is 4%, the hardness of target coating is H
Grade；When the additive amount of Nano diamond is 10%, and the additive amount of nano silica is 7%, the hardness of target coating is H
Grade.
Nano diamond has the characteristics such as high rigidity, high abrasion, although the hardness of the not no diamond of silica is high, due to being
Club-like, and it is more short and small, therefore rigidity with higher, it is connected with each other by the coupling agent and base-material of silica surface,
" skeleton " is formed in base-material, the two mutually cooperates with the hardness for improving coating jointly.
3) adhesive force detects
It is required according to ISO2409-2007, selects aluminium sheet as coating test substrate, coating is measured using F107 cross hatch device
Adhesive force.Coating coating before, need to pre-process substrate surface, key step have sand paper polishing go, alkali cleaning is gone
Oil, acid pickling and rust removing, washing, drying.Remove the most iron rust of substrate surface；Using saponification, substrate surface is removed with alkali cleaning
Greasy dirt；It is difficult to the rusty stain removed, strong acid is added using the reaction principle rust of acid and oxide and removes；Finally with distillation washing
Only, it dries.Aluminium sheet coating sample is prepared, marks the shape of cross grid on template with cross hatch device until aluminium sheet substrate；With hair
Brush is respectively brushed 5 times along the cornerwise direction of cross grid, is tightly attached on notch with adhesive tape and is pulled open rapidly；With amplification sem observation, repeat
Test of many times, the standard of 5 coating adhesion of the table of comparisons determine that the grade of coating adhesion, test result are as shown in table 10:
The test of 10 paint adhesion of table
| Serial number | L | M | N | P |
| Adhesive force (grade) | 0 | 0 | 0 | 0 |
It sees from the above, the additive amount range of filler nanometer diamond is 5~10%, nano silica additional amount model
It encloses when being 4~7%, the adhesive force of coating is 0 grade, does not reduce the adhesive force of coating in this filler addition range.This is mainly
Since nano silica forms irregular reticular structure in coating, Nano diamond is filled into coating gap and nanometer
Silica forms bridge island bridge connection type.Nano diamond cooperates with mutually with nano silica, increases coating painting jointly
The roughness of layer, increases the contact area of coating and substrate, while enhancing the bonding strength of coating and substrate, such phenomenon
It finds full expression in impact flexibility.Therefore, it is suitably added in range in filler nanometer diamond and nano silica,
The adhesive force of paint coatings is not reduced.
4) measurement of heat dissipation effect
The content of Nano diamond and the content of silica have a certain impact to thermal dispersant coatings heat dissipation performance, according to reality
Conditional consistency principle is tested, the addition of single filler various concentration gradient is measured first.
It is measured using cooling effect of the furnace temperature tester to target paint coatings, model SMT-7-128-500-K,
Match aestheticism High Seience Technology Co., Ltd. in Beijing.Working principle is that temperature signal is changed into thermo-electromotive force by thermocouple, using electrical
Instrument comes out the temperature display that this electromotive force is changed into measured matter.Subjects are LED radiator or CPU radiating fin.Through
The workpiece for crossing different disposal is placed in 145 DEG C of insulating boxs, constant temperature 1h, takes out, its cooling is measured in the case where free convection
Curve, cooling extent of the temperature difference of cooling 15min or so as coating, measurement result are as shown in table 11.
The additional amount of the different fillers of table 11 and the cooling extent of corresponding coating
| Serial number | L | M | N | P |
| Nano diamond (wt%) | 5 | 5 | 10 | 10 |
| Nano silica (wt%) | 4 | 7 | 4 | 7 |
| The temperature difference (DEG C) | 14.1 | 15.6 | 16.9 | 18.5 |
As known from Table 11, when the additive amount of filler nanometer diamond is 5%, and nano silica additive amount is 4%, mesh
The coating cooling extent for marking coating is 14.1 DEG C；When filler nanometer diamond additive amount be 5%, nano silica additive amount
When being 7%, the coating cooling extent of target coating is 15.6 DEG C, and cooling extent improves 10.6%.When filler nanometer diamond
Additive amount be 10%, when nano silica additive amount is 4%, the coating cooling extent of target coating is 16.9 DEG C；When filling out
The additive amount for expecting Nano diamond is 10%, and when nano silica additive amount is 7%, the coating cooling extent of target coating is
18.5 DEG C, cooling extent improves 9.5%.
When the additive amount of filler nanometer silica is 4%, and Nano diamond additive amount is 5%, the painting of target coating
Layer cooling extent is 14.1 DEG C, and when Nano diamond additive amount is 10%, the coating cooling extent of target coating is 16.9 DEG C, drop
Warm amplitude improves 19.8%.When the additive amount of filler-silicon dioxide is 7%, and Nano diamond additive amount is 5%, target is applied
The coating cooling extent of material is 15.6 DEG C, and when Nano diamond additive amount is 10%, the coating cooling extent of target coating is
18.5 DEG C, cooling extent improves 18.6%.
By in above-mentioned conclusion it is found that nano silica is club-like, in coating when a kind of filler additive amount determines
In be in unordered mixed and disorderly distribution, formed it is random netted, Nano diamond is filled in gap, play heat dissipation transmitting function served as bridge.
Nano silica has good thermal coefficient, therefore can play a positive role to the heat dissipation of coating, equally, nanometer Buddha's warrior attendant
Stone is the excellent heat dissipation of one kind, Heat Conduction Material, coefficient of heat transfer with higher and heat-conducting effect.Therefore, by the way that nanogold is added
Hard rock and nano silica have good cooling and heat dissipation effect to target coating.
5) measurement of radiation coefficient
Radiation coefficient (also known as radiance, emissivity, coefficient of blackness, heat emissivity coefficient etc.) is the basic ginseng of the hot physical property of material
One of number, refers to the ratio between actual object and the radiation of black matrix under the same terms (temperature, wavelength and geometrical condition):
In formula: ε (λ, T) is emissivity of the sample in temperature T, and M (λ, T) is that spectral radiance of the sample in temperature T goes out
Degree, M0(λ, T) is spectral radiance out-degree of the black matrix in temperature T.
Radiance measurement is carried out to coating sample using IR-2 type two waveband emissivity measurement instrument, measurement wave band is 1~22 μ
M, blackbody temperature are set as 145 DEG C, after black matrix is stablized, and wave band is different, need to use optical filter, and using the reference sample of known radiance
Plate is corrected at the corresponding temperature.Test results are shown in figure 6.
As can be known from Fig. 6, when filler nanometer diamond and nano silica additive amount are 0%, the painting of target coating
Layer radiation coefficient is 0.67, when the additive amount of filler nanometer diamond is 5%, and nano silica additive amount is 4%, target
The coating radiation coefficient of coating is 0.87, and radiation coefficient improves 29.8%；When filler nanometer diamond additive amount be 5%,
When nano silica additive amount is 7%, the coating radiation coefficient of target coating is 0.89, and radiation coefficient improves 32.8%；
When the additive amount of filler nanometer diamond is 10%, and nano silica additive amount is 4%, the coating radiative chain of target coating
Number is 0.88, and radiation coefficient improves 31.3%；When the additive amount of filler nanometer diamond is 10%, nano silica is added
When amount is 7%, the coating radiation coefficient of target coating is 0.90, and radiation coefficient improves 34.3%.
In from the above, it can be clearly seen that, pass through the Nano diamond of high thermal conductivity and high wave transparent, low-k
Nano silica is added, and is evenly distributed on it in polyacrylic resin, can play the effect of good heat loss through radiation.Cause
This, the selected range of Nano diamond is 5~10% and nano silica selectes range 4~7%, can be played to coating good
Good heat spreading function.
6) neutral salt spray performance measurement
Testing liquid is met in GB6682 tertiary effluent using meeting the analytically pure sodium chloride solution of GB1266 and be dissolved in, concentration
For 50 ± 1g/L；Solution ph is 6.5~7.2.Temperature in the performance test space of equipment is 35 ± 2 DEG C；In working space
Interior any position, area 80cm2Collection funnel be continuously atomized the salt fog settling amount of 16h, it is average be collected into 1.0 per hour~
The solution of 2.0mL；Scratch, scratch stroke antireflective coating layer to ground are drawn in specimen surface, and scratch isolated edge is made to be greater than 20mm.
It is filtered before the basin of solution injection devices, prevents solid matter plug nozzle.Spray chamber is by resistance in salt spray test chamber
The material of saline solution corrosion is made or lining, top cover or lid should tilt upwards, is greater than 25 ° with the angle of horizontal plane, makes to coagulate
The drop collected on lid is not dropped on test plate (panel).The sample of tetra- kinds of A, L, M, N, P different compositions is put into spray chamber, closes spray
Fog chamber's top cover opens testing liquid basin valve, so that solution is flowed to storage tank, tested, is measured in parallel twice.The test plate (panel) period
Property visually inspected, but do not allow destroy test plate (panel) surface.60min is not to be exceeded in the review time in any one period for 24 hours, and
It is checked in the daily same time.At the end of test period, test plate (panel) is taken out from case, is rinsed test plate (panel) with clean water and is removed table
Remaining testing liquid on face checks the breakoff phenomenon on test plate (panel) surface.
The sample test plate (panel)s for checking the different compositions of tetra- kinds of A, L, M, N, P, it is existing there is no blistering, getting rusty etc. on test plate (panel) surface
As, but can clearly be seen that serious corrosion phenomenon at scratch, to the template of tetra- different formulations of A, L, M, N, P composition into
The test of row adhesive force, test result is as follows shown in table 12.
The test result of the template adhesive force of 12 different formulations of table composition
| Serial number | L | M | N | P |
| Adhesive force (grade) before salt fog | 0 | 0 | 0 | 0 |
| Adhesive force (grade) after salt fog | 0 | 0 | 0 | 0 |
By upper table it is found that the coating of target coating passes through after salt fog destructive testing, the additive amount 5 of Nano diamond
~10% and nano silica additive amount 4~7% as filler be added coating in, the adhesive force of target paint coatings does not have
It changes.After salt mist experiment, entire test plate (panel) surface is made a general survey of, does not find any bubble impression；It is cut in coating cross
There is the trace of corrosion in oral area position due to exposing the substrate of the inside above substrate.
Claims (4)
1. a kind of anti-corrosion heat radiation coating, which is characterized in that be made of the raw material of following weight percent: polyacrylic resin 74.9
~82.9%, Nano diamond 5~10%, nano silica 4~7%, polyacrylic acid 0.7%, polyacrylamide 2.3%, coupling agent
A-1100 2%, defoaming agent AFE-7500 0.1%, dimethlbenzene 3%.
2. anti-corrosion heat radiation coating as described in claim 1, which is characterized in that the Nano diamond particle size distribution range is 5
~20nm, the nano silica are club-like fiber, and diameter range is 5~20nm, and length range is 50~100nm.
3. the preparation method of anti-corrosion heat radiation coating of any of claims 1 or 2, which comprises the following steps:
1) 70~80 DEG C of water of 3 times of quality of coupling agent is first added into coupling agent A-1100 and stirs evenly, standing 30min makes
Coupling agent is fully hydrolyzed, and is added after Nano diamond and nano silica stir 30~35min under 1000rpm, in 105
DEG C it is dried to obtain the Nano diamond and nano silica that coupling agent is contained on surface；
2) acrylic resin, polyacrylamide, polyacrylic acid are mixed and stirs 20~30min under 800rpm revolving speed, be added
The Nano diamond and nano silica of coupling agent are contained in the surface of step 1), and side edged is stirred with the revolving speed of 500~600rpm
It mixes, after being added to coupling agent mixed solution, continues to keep revolving speed stirring 1h, while defoaming agent 7500 is added, add after stirring
Enter dimethlbenzene to continue to stir 6h, makes material dispersion uniformly up to anti-corrosion heat radiation coating.
4. the preparation method of the anti-corrosion heat radiation coating as claimed in claim 3, which is characterized in that described in step 1)
Nano diamond and nano silica must pass through following surface treatment:
A) silica is put into crucible, covers crucible cover, be put into Muffle furnace, heated up according to staged: room temperature to 120
DEG C, heating rate is 1 DEG C/min, keeps the temperature 30min, then be warming up to 400 DEG C by 120 DEG C, keeps the temperature 30min, then be warming up to by 400 DEG C
750 DEG C, 1h is kept the temperature, naturally cools to room temperature after heat preservation；
B) concentrated sulfuric acid that concentration is 98% is added in cast iron autoclave, reaction kettle surface is passivated, is then spent
Ionized water cleans reaction kettle, until the pH value of aqueous solution is about 6.50~7.00 in reaction kettle；
C) be 5~10nm by particle size range, the Nano diamond of 100~150ct is put into above-mentioned autoclave, is about reacted
/ 10th of autoclave body product, are added the deionized water of 8~10 times of Nano diamond quality, reaction kettle are carried out closed, be put into perseverance
It is heated in warm drying box, using slow heating mode, 1 DEG C/min, is warming up to 120 DEG C, constant temperature 30min, natural cooling is received
Rice diamond turbid；
D) Nano diamond turbid is centrifuged 10min in the case where revolving speed is 8000~10000rpm, outwells supernatant liquor；
E) 600~6000g Nano diamond and nano silica gradually plasma modification: are put into plasma handling system
In, handle 30min under the conditions of pure hydrogen, 200 DEG C for the treatment of temperature, hydrogen flowing quantity 60cm3/ min obtains the modified nanometer in surface
Diamond or nano silica.
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