CN105200367B - A kind of vacuum impregnation nano hole sealing agent and its preparation method and application with high osmosis - Google Patents

A kind of vacuum impregnation nano hole sealing agent and its preparation method and application with high osmosis Download PDF

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CN105200367B
CN105200367B CN201410310384.7A CN201410310384A CN105200367B CN 105200367 B CN105200367 B CN 105200367B CN 201410310384 A CN201410310384 A CN 201410310384A CN 105200367 B CN105200367 B CN 105200367B
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sealing agent
hole sealing
vacuum impregnation
nano hole
silica
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CN105200367A (en
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檀四华
向汝明
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Huizhou Huayu Industrial Co Ltd
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Huizhou Huayu Industrial Co Ltd
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Abstract

The present invention discloses a kind of vacuum impregnation nano hole sealing agent with high osmosis, is made of the raw material of following quality proportioning:Silicon carbide:Silica:Auxiliary agent:Solvent=1%~5%:5%~15%:0.1%~3%:65%~95%.The invention also discloses the preparation methods of the vacuum impregnation nano hole sealing agent.The invention also discloses purposes of the vacuum impregnation nano hole sealing agent on iron system, aluminium system, copper system and alloy system precision workpiece.Vacuum impregnation nano hole sealing agent provided by the invention with high osmosis can form chemical crosslinking with metals such as iron, aluminium, zinc, magnesium and generate strong chemical bonded refractory, has the following advantages:(1) compared with general hole sealing agent, there is better permeability, particle<50nm;(2) compared with general hole sealing agent, there is better high-temperature stability;(3) compared with general hole sealing agent, also have the advantages that low viscosity, high-wearing feature.

Description

A kind of vacuum impregnation nano hole sealing agent with high osmosis and preparation method thereof and Purposes
Technical field
The present invention relates to vacuum impregnation nano hole sealing agent technical fields more particularly to a kind of vacuum with high osmosis to contain Soak nano hole sealing agent and its preparation method and application.
Background technology
For many hot-spraying coatings, sealing of hole is a necessary last handling process.When coating faces corrosion and oxidation When (sometimes in high temperature) environment, sealing of hole is that coating designs the content necessarily considered.
It is METCO companies of the U.S. (existing SULZER METCO) that first releases seriation hole sealing agent product to market in the world, Its hole sealing agent series has considerable scale, and successfully uses for many years, and important several hole sealing agents have:It is air-dried type glyceride Resin is air-dried type phenolic resin, aluminium vinyl, baking-type phenolic resin and sial resin etc., wherein although first four kinds There is a preferable chemical stability, but its operating temperature is all at 200 DEG C or so, the sealing of hole work that can not be applied under hot environment Skill, and sial resin is although operating temperature can reach 480 DEG C has that abrasion resistance is low, poor permeability.
Other than problem above, general resin can not penetrate into small hole, for some accurate components without Can be power, there is also significant limitations.
Invention content
One kind is provided with high osmosis, height it is an object of the invention to overcome above-mentioned the deficiencies in the prior art place The vacuum impregnation nano hole sealing agent of wearability, high temperature tolerance, low viscosity, solve traditional hole sealing agent poor permeability, wearability it is low, The high problem of non-refractory, viscosity seals to realize for precision components inner void is intact.
To achieve the above object, the technical solution that the present invention takes is:A kind of vacuum impregnation nanometer with high osmosis Hole sealing agent is made of the raw material of following quality proportioning:
Silicon carbide:Silica:Auxiliary agent:Solvent=1%~5%:5%~15%:0.1%~3%:65%~95%.
It is described true as the preferred embodiment of the vacuum impregnation nano hole sealing agent of the present invention with high osmosis Sky impregnation nano hole sealing agent is made of the raw material of following quality proportioning:
Silicon carbide:Silica:Auxiliary agent:Solvent=3.45%:11.25%:0.3%:85%.
As the preferred embodiment of the vacuum impregnation nano hole sealing agent of the present invention with high osmosis, the auxiliary agent Including thickener and coalescents.
As the preferred embodiment of the vacuum impregnation nano hole sealing agent of the present invention with high osmosis, the thickening Agent is polyurethane, and the coalescents are at least one of dipropylene glycol methyl ether, dipropylene, tetrafluoropropanol.
As the preferred embodiment of the vacuum impregnation nano hole sealing agent of the present invention with high osmosis, the solvent For at least one of tetrafluoropropanol or isopropanol.
Secondly, the preparation method for the vacuum impregnation nano hole sealing agent with high osmosis that the present invention also provides a kind of is described Method includes the following steps:
(1) it is silicon carbide according to quality proportioning:Silica:Auxiliary agent:Solvent=1%~5%:5%~15%:0.1% ~3%:65%~95% weighs the quality of each substance respectively;
Or it is silicon carbide that step (1), which is according to quality proportioning,:Silica:Auxiliary agent:Solvent=3.45%:11.25%: 0.3%:85% weighs the quality of each substance respectively;
(2) dispersing speed is adjusted to 300r/m~500r/m, is first slowly added to silicon carbide and silica, added suitable Coalescents, the viscosity feelings of most backsight entire slurry are added to be unlikely to make the excessively high and inconvenient use of slurry viscosity in the solvent of amount Condition adds thickener in right amount, the slurry prepared;
(3) slurry described in step (2) is placed in 200 DEG C~300 DEG C of oven low-temperature bake 10min~30min i.e. Obtain required hole sealing agent.
Finally, the present invention also provides a kind of vacuum impregnation nano hole sealing agent with high osmosis in iron system, aluminium system, copper Purposes in system and alloy system precision workpiece.
It is deep that hole sealing agent of the present invention can penetrate into inside workpiece after vacuum impregnation working process by capillary theory Layer and achieve the purpose that sealing, improve air-tightness gas-tight leakage leakage, strengthen machine cut processability, increase mechanical compression strength, It improves machining tolerance dimensional accuracy, promote accessory appearance texture and durability.
On the one hand there are organic matters to form chemical bonded refractory for the hole sealing agent, on the other hand there is inorganic matter and generates bond, because This can form chemical crosslinking with metals such as iron, aluminium, zinc, magnesium and generate strong chemical bonded refractory, be that excellent product quality is most important Fundamental requirement.Rather than the resin hole sealing agent of the epoxy resin or worse first-class used in general impregnation sealing of hole factory, this kind of resin are A kind of macromolecule of macromolecule simple surface layer can only form a kind of resin of cladding again for workpiece, can not penetrate into The inside of workpiece, therefore after workpiece sealing of hole, often fraction defective is high when re-plating and uses the operating condition in high temperature height friction Under be easy to make plating film stripping, also tend to that perfect requirement is not achieved under salt spray resistance condition test.
The hole sealing agent be nanoscale molecule (<50nm), there is high osmosis, low-viscosity, even if small hole Hole can also be penetrated into, and drying itself can start to polymerize (polymerization) when evaporating, and finally after liquid evaporation, form ceramics Film and hole and hole interior surface are taken into account and completely sealed.
Application range can be used in powder metallurgy spare part, the airtight component of Pneumatic hand tools, cylinder head, engine spare part, Fuel system, refrigerant condenser, power-operated control system, rack and pinion shell cover, turbine engine spare part, switch valve, menifold, tune Save device, casinghead gas controller, oil pressure side Pu spare part, motor and electronics, military equipment, space flight computer hardware etc..
The reaction mechanism of the hole sealing agent sealing of hole is as follows:
A, it permeates, as shown in Figure 3:
Hole sealing agent, which contains, to be impregnated into the gap of deep layer, hole sealing agent and workpiece internal layer【Iron system, aluminium system, copper system, alloy system】Point Not Cun situation.
B, crosslinking and polymerization, as shown in Figure 4:
Hole sealing agent starts to polymerize (polymerization) and cross-linking reaction (corss-link) ceramics when drying evaporation Body gradually forms.
C, sealing of hole, as shown in Figure 5:
Hole sealing agent and workpiece substrate【Iron system, aluminium system, copper system, alloy system】Strong chemical crosslinking occurs and itself is poly- Close reaction, the ceramic body being formed simultaneously and the efficiency for reaching sealing of hole.
Vacuum impregnation nano hole sealing agent provided by the invention with high osmosis, by change formula rate, have with Lower advantage:(1) compared with general hole sealing agent, there is better permeability, particle<50nm;(2) compared with general hole sealing agent, tool There is a better high-temperature stability, 600 DEG C;(3) compared with general hole sealing agent, also have the advantages that low viscosity, high-wearing feature.
Description of the drawings
Fig. 1 is the SEM that vacuum impregnation nano hole sealing agent of the present invention is applied to before and after micro-arc oxidation workpiece disk sealing of hole Figure.
Fig. 2 is that the SEM of vacuum impregnation nano hole sealing agent embodiment 2 of the present invention schemes.
Fig. 3 is the infiltration mechanism choice of hole sealing agent sealing of hole of the present invention reaction.
Fig. 4 is crosslinking and the polymerization machine drawing of hole sealing agent sealing of hole of the present invention reaction.
Fig. 5 is the sealing of hole mechanism choice of hole sealing agent sealing of hole of the present invention reaction.
Specific implementation mode
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention It is described further.
Embodiment 1
The raw material by following mass ratio of vacuum impregnation nano hole sealing agent with high osmosis described in the present embodiment is made:
Silicon carbide:Silica:Auxiliary agent:Isopropanol=1%:5%:0.1%:65%, wherein the quality proportioning of auxiliary agent is Polyurethane:Tetrafluoropropanol=1:1.
The preparation process of vacuum impregnation nano hole sealing agent, includes the following steps described in the present embodiment:
(1) it is silicon carbide according to quality proportioning:Silica:Polyurethane:Tetrafluoropropanol:Isopropanol=1%:5%: 0.05%:0.05%:65% weighs the quality of each substance respectively;
(2) dispersing speed is adjusted to 300r/m, is first slowly added to silicon carbide and silica, add suitable isopropyl Tetrafluoropropanol is added to be unlikely to make the excessively high and inconvenient use of slurry viscosity in alcohol, and the viscosity situation of most backsight entire slurry is appropriate Add polyurethane, the slurry prepared;
(3) slurry described in step (2) is placed in low-temperature bake 10min in 200 DEG C of oven and obtains required sealing of hole Agent.
Embodiment 2
The raw material by following mass ratio of vacuum impregnation nano hole sealing agent with high osmosis described in the present embodiment is made:
Silicon carbide:Silica:Auxiliary agent:Isopropanol=3.45%:11.25%:0.3%:85%, wherein the matter of auxiliary agent Amount proportioning is polyurethane:Dipropylene=1:1.
The preparation process of vacuum impregnation nano hole sealing agent, includes the following steps described in the present embodiment:
(1) it is silicon carbide according to quality proportioning:Silica:Polyurethane:Dipropylene:Isopropanol=3.45%: 11.25%:0.15%:0.15%:85% weighs the quality of each substance respectively;
(2) dispersing speed is adjusted to 400r/m, is first slowly added to silicon carbide and silica, add suitable isopropyl Dipropylene, the viscosity situation of most backsight entire slurry is added to be unlikely to make the excessively high and inconvenient use of slurry viscosity in alcohol Appropriate addition polyurethane, the slurry prepared;
(3) slurry described in step (2) is placed in low-temperature bake 20min in 250 DEG C of oven and obtains required sealing of hole Agent.
Fig. 2 is the SEM figures of the present embodiment, there it can be seen that nanometer particle size<50nm, even if facing small hole, this Inventing the vacuum impregnation nano hole sealing agent can also penetrate into, and achieve the effect that seal hole completely.
Embodiment 3
The raw material by following mass ratio of vacuum impregnation nano hole sealing agent with high osmosis described in the present embodiment is made:
Silicon carbide:Silica:Auxiliary agent:Tetrafluoropropanol=5%:15%:3%:95%, wherein the quality proportioning of auxiliary agent For polyurethane:Dipropylene glycol methyl ether=1:1.
The preparation process of vacuum impregnation nano hole sealing agent, includes the following steps described in the present embodiment:
(1) it is silicon carbide according to quality proportioning:Silica:Polyurethane:Dipropylene glycol methyl ether:Tetrafluoropropanol=5%: 15%:1.5%:1.5%:95% weighs the quality of each substance respectively;
(2) dispersing speed is adjusted to 500r/m, is first slowly added to silicon carbide and silica, add suitable tetrafluoro Dipropylene glycol methyl ether, the viscosity feelings of most backsight entire slurry are added to be unlikely to make the excessively high and inconvenient use of slurry viscosity in propyl alcohol Condition adds polyurethane in right amount, the slurry prepared;
(3) slurry described in step (2) is placed in low-temperature bake 30min in 300 DEG C of oven and obtains required sealing of hole Agent.
Comparative example 1
This comparative example is to carry out the performance of vacuum impregnation nano hole sealing agent in embodiment 1-3 and general hole sealing agent, comparison As a result shown in following table.Wherein, the raw material group of general hole sealing agent becomes:Nickel acetate:Benzoic acid:Sodium benzoate:How to be sulfonate:Have Machine silicon defoaming agent=75%:1%:1%:15%:0.5%.
Experimental example 2
Hole sealing agent in the present embodiment 2 is applied to micro-arc oxidation workpiece disk, as shown in Figure 1, upper left and upper right quarter Before being divided into sealing of hole, the pattern of micro-arc oxidation workpiece disk, it is clear that there are many holes for workpiece disk, aperture is most It is big up to 4 μm or so, it is minimum up to Nano grade, in embodiment 2 hole sealing agent by vacuum impregnation process in differential arc oxidation After on workpiece disk, as shown in Figure 1, bottom left section and lower right-most portion are the patterns after sealing of hole, it is evident that see, workpiece disk Hole sealed by intact.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is protected to the present invention The limitation of range is protected, although being explained in detail to the present invention with reference to preferred embodiment, those skilled in the art should Understand, technical scheme of the present invention can be modified or replaced equivalently, without departing from the essence of technical solution of the present invention And range.

Claims (5)

1. a kind of vacuum impregnation nano hole sealing agent with high osmosis, is made of the raw material of following quality proportioning:
Silicon carbide:Silica:Auxiliary agent:Solvent=1%~5%:5%~15%:0.1%~3%:65%~95%;
The auxiliary agent includes thickener and coalescents;The thickener is polyurethane, and the coalescents are dipropylene glycol first At least one of ether, dipropylene, tetrafluoropropanol;
The solvent is at least one of tetrafluoropropanol or isopropanol;
The preparation method of the vacuum impregnation nano hole sealing agent with high osmosis includes the following steps:
(1) it is silicon carbide according to quality proportioning:Silica:Auxiliary agent:Solvent=1%~5%:5%~15%:0.1%~ 3%:65%~95% weighs the quality of each substance respectively;
(2) dispersing speed is adjusted to 300r/m~500r/m, is first slowly added to silicon carbide and silica, added suitable Coalescents are added to be unlikely to make the excessively high and inconvenient use of slurry viscosity in solvent, and the viscosity situation of most backsight entire slurry is suitable Amount addition thickener, the slurry prepared;
(3) slurry described in step (2) low-temperature bake 10min~30min in 200 DEG C~300 DEG C of oven is placed in obtain Required hole sealing agent.
2. the vacuum impregnation nano hole sealing agent with high osmosis according to claim 1, which is characterized in that the vacuum contains Leaching nano hole sealing agent is made of the raw material of following quality proportioning:
Silicon carbide:Silica:Auxiliary agent:Solvent=3.45%:11.25%:0.3%:85%.
3. a kind of preparation method of the vacuum impregnation nano hole sealing agent with high osmosis as described in claim 1-2 is any, It is characterized in that, the described method comprises the following steps:
(1) it is silicon carbide according to quality proportioning:Silica:Auxiliary agent:Solvent=1%~5%:5%~15%:0.1%~ 3%:65%~95% weighs the quality of each substance respectively;
Or it is silicon carbide that step (1), which is according to quality proportioning,:Silica:Auxiliary agent:Solvent=3.45%:11.25%:0.3%: 85% weighs the quality of each substance respectively;
(2) dispersing speed is adjusted to 300r/m~500r/m, is first slowly added to silicon carbide and silica, added suitable Coalescents are added to be unlikely to make the excessively high and inconvenient use of slurry viscosity in solvent, and the viscosity situation of most backsight entire slurry is suitable Amount addition thickener, the slurry prepared;
(3) slurry described in step (2) low-temperature bake 10min~30min in 200 DEG C~300 DEG C of oven is placed in obtain Required hole sealing agent.
4. a kind of vacuum impregnation nano hole sealing agent with high osmosis as described in claim 1-2 is any is in iron system, aluminium system, copper It is the purposes on precision workpiece.
5. the purposes of the vacuum impregnation nano hole sealing agent with high osmosis as claimed in claim 4, which is characterized in that the essence Close workpiece is alloy system precision workpiece.
CN201410310384.7A 2014-06-30 2014-06-30 A kind of vacuum impregnation nano hole sealing agent and its preparation method and application with high osmosis Active CN105200367B (en)

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CN114315246B (en) * 2021-12-29 2022-11-25 西南科技大学 Hole sealing agent with repairing function and application thereof

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CN101949481A (en) * 2010-09-17 2011-01-19 西安超码科技有限公司 Method for preparing wound heat-insulating drum
CN102732131A (en) * 2012-07-23 2012-10-17 河北晨阳工贸集团有限公司 Paint in aqueous epoxy thick paste and preparation method thereof
CN103058712A (en) * 2013-01-10 2013-04-24 湖南南方搏云新材料有限责任公司 C/SiC composite coating applied to surface of low-density carbon/carbon composite material and preparation process thereof
CN103498179A (en) * 2013-10-22 2014-01-08 哈尔滨三泳金属表面技术有限公司 Aluminum or aluminum alloy surface oxide film and method for preparing same
CN103881496A (en) * 2014-03-18 2014-06-25 中国兵器工业集团第五三研究所 Transparent protective coat for concrete

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1878668A (en) * 2004-11-04 2006-12-13 Lg化学株式会社 Ultralight ceramic plate and method for manufacturing same
CN101949481A (en) * 2010-09-17 2011-01-19 西安超码科技有限公司 Method for preparing wound heat-insulating drum
CN102732131A (en) * 2012-07-23 2012-10-17 河北晨阳工贸集团有限公司 Paint in aqueous epoxy thick paste and preparation method thereof
CN103058712A (en) * 2013-01-10 2013-04-24 湖南南方搏云新材料有限责任公司 C/SiC composite coating applied to surface of low-density carbon/carbon composite material and preparation process thereof
CN103498179A (en) * 2013-10-22 2014-01-08 哈尔滨三泳金属表面技术有限公司 Aluminum or aluminum alloy surface oxide film and method for preparing same
CN103881496A (en) * 2014-03-18 2014-06-25 中国兵器工业集团第五三研究所 Transparent protective coat for concrete

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