CN110229523B - Multiple network liquid silicone rubber and preparation method thereof - Google Patents
Multiple network liquid silicone rubber and preparation method thereof Download PDFInfo
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- CN110229523B CN110229523B CN201910619214.XA CN201910619214A CN110229523B CN 110229523 B CN110229523 B CN 110229523B CN 201910619214 A CN201910619214 A CN 201910619214A CN 110229523 B CN110229523 B CN 110229523B
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/001—Macromolecular compounds containing organic and inorganic sequences, e.g. organic polymers grafted onto silica
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/34—Silicon-containing compounds
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C08L87/00—Compositions of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
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Abstract
The invention belongs to the technical field of nano composite materials, and particularly relates to a multi-network liquid silicone rubber and a preparation method thereof. The preparation method of the silicone rubber comprises the following steps: (1) heating a polysiloxane monomer to 80-100 ℃, adding a catalyst I, mixing, heating to 100-130 ℃ under the condition of stirring, reacting for 50-90 min, and then adding reactive SiO2After the nanometer particles continue to react for 40-80 min, removing the unreacted catalyst I, and concentrating under reduced pressure to obtain a compound A; (2) the compound A and gas phase SiO2And uniformly mixing, sequentially adding a cross-linking agent and a catalyst II, stirring for 10-30min, defoaming in vacuum to obtain a crude product, and curing the crude product at room temperature to obtain the catalyst. Compared with the silicon rubber prepared by the traditional blending method, the multiple-network liquid silicon rubber prepared by the invention has the advantages of obviously improved mechanical property and prominent application prospect, and meanwhile, the method has mild reaction conditions and can be used as a novel high-performance liquid silicon rubber preparation method for large-scale preparation.
Description
Technical Field
The invention belongs to the technical field of nano composite materials, and particularly relates to a multi-network liquid silicone rubber and a preparation method thereof.
Background
Polydimethylsiloxane (PDMS) is often used as a base rubber of liquid silicone rubber, and has excellent high and low temperature resistance, aging resistance, solvent resistance and the like because the dissociation energy of Si-O-Si bonds in a molecular chain is as high as 460 kJ/mol and is far higher than that of C-C bonds, so that the PDMS has very wide application. However, PDMS (polydimethylsiloxane) has weak intermolecular force, and a cross-linked network after cross-linking and curing is very weak, so that the liquid silicone rubber has very poor mechanical properties and cannot meet the use requirements.
At present, the common method is to use silicon dioxide (SiO)2) Inorganic fillers such as calcium carbonate, montmorillonite and carbon nano tube are physically blended with PDMS, so that the strength of a cross-linked network is improved, and the reinforcement of liquid silicone rubber is realized. Wherein SiO is2The reinforcing filler is the most commonly used reinforcing filler due to the characteristics of various structures, easy regulation and control of surface chemical properties, similarity to the structural composition of PDMS and the like. SiO 22The PDMS is an inorganic phase and an organic phase, mainly takes hydrogen bonds and physical adsorption, and cannot form a high-strength crosslinking network.
Therefore, how to improve SiO2The interaction with PDMS, the design and preparation of high-strength cross-linked networks are very important for the reinforcement of liquid silicone rubber.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a multi-network liquid silicone rubber. By adding reactive SiO during the polymerization of polysiloxanes2Nanoparticles of polysiloxane grafted to SiO2Surface, SiO reinforcement2Bonding with polysiloxanes; then using gas phase SiO2The developed network constructs the network structure of polysiloxane through hydrogen bond action, the liquid silicone rubber with multiple cross-linked network structure is prepared, and SiO is obviously improved2Reinforcing effect on liquid silicon rubber.
The invention also provides a preparation method of the multi-network liquid silicone rubber.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of multi-network liquid silicone rubber comprises the following steps:
(1) under the condition of stirring, polysiloxane monomer is addedHeating to 80-100 ℃, adding a catalyst I, mixing, heating to 100-130 ℃, reacting for 50-90 min, and then adding reactive SiO2After the nano particles continue to react for 40-80 min, removing unreacted catalyst I, and obtaining a compound A through decompression and concentration, wherein the compound A is the base adhesive;
(2) the compound A and gas phase SiO2Uniformly mixing (mixing by stirring for 60-120 min), then sequentially adding the cross-linking agent and the catalyst II, continuously stirring for 10-30min, carrying out vacuum defoamation to obtain a crude product, and curing the crude product at room temperature to obtain the catalyst.
Preferably, the polysiloxane monomer in step (1) is a Dimethylcyclosiloxane Mixture (DMC).
Preferably, the catalyst I in the step (1) is a basic catalyst, the basic catalyst is a metal hydroxide, an alkali metal alkoxide or a quaternary ammonium base, and the amount of the catalyst I is 0.01-0.02% of the mass of the polysiloxane monomer; further preferably, the basic catalyst is tetramethylammonium hydroxide (Me)4NOH）。
Further preferably, the unreacted catalyst I in the step (1) can be removed by heating to 130 ℃ and 150 ℃ to decompose the unreacted catalyst I or neutralizing with acid and alkali.
Preferably, the reactive SiO reacted in step (1)2The reactive group for surface modification of the nanoparticles is epoxy, amino, double bond or mercapto, and more preferably, the reactive group for surface modification is epoxy and the reactive SiO is2The addition amount of the nanometer particles is 0.5-10% of the mass of the basic glue.
Preferably, the gas phase SiO in step (2)2The amount of the adhesive is 1-15% of the mass of the basic adhesive; the gas phase SiO2Specifically, the product is a commercial product H L-200, gas phase SiO2Has developed branched network structure.
Preferably, in the step (2), the cross-linking agent is ketoxime moisture curing type cross-linking agent, the dosage of the ketoxime moisture curing type cross-linking agent is 4-8% of the mass of the base glue, and the catalyst II is organic tin catalyst, and the dosage of the organic tin catalyst is 0.05-0.15% of the mass of the base glue.
Specifically, the curing time in the step (2) is 7 to 15 days.
The multi-network liquid silicone rubber is prepared by the method.
In addition, the reactive SiO2The nanoparticles can be prepared according to patent CN1666954A, or can be purchased from common commercial products.
To distinguish reactive SiO2Nanoparticles and gas phase SiO2m-SiO for the purposes of this application2Denotes reactive SiO2Nanoparticles of n-SiO2Represents gas phase SiO2。
Compared with the prior art, the invention has the beneficial effects that:
1.SiO2enhancement of binding with PDMS: in the invention, m-SiO is added in the polymerization process of PDMS2Using m-SiO2The surface is subjected to condensation reaction with Si-OH at the chain end of PDMS so that the PDMS molecular chain is grafted to SiO through chemical bonds2Surface, effectively strengthen SiO2Bonding with PDMS;
2. construction of a multiple network structure: PDMS molecular chain bonding to m-SiO2Surface to obtain m-SiO of primary structure2PDMS, then using n-SiO2A secondary network structure of PDMS is constructed through hydrogen bond action, and finally micromolecules such as a cross-linking agent and the like are added to carry out chemical cross-linking, so that liquid silicone rubber with a multiple network structure is prepared;
3. the preparation method is simple in preparation process, mild in reaction conditions and beneficial to large-scale production.
Drawings
FIG. 1 is a schematic diagram of the present invention for preparing a multiple network liquid silicone rubber;
FIG. 2 is a diagram showing m-SiO obtained in example 12m-SiO extracted by washing PDMS in toluene2An infrared spectrum of (1);
FIG. 3 is a shear-thinning curve of uncured liquid silicone rubbers prepared in example 1 and comparative example 1;
FIG. 4 is a scanning electron micrograph of a tensile section of the liquid silicone rubbers prepared in examples 1 to 3 and comparative example 1;
FIG. 5 is a scanning electron micrograph of brittle fracture surfaces of liquid silicone rubbers prepared in examples 1 to 3 and comparative example 1 after liquid nitrogen treatment;
fig. 6 is a stress-strain curve of the liquid silicone rubbers prepared in examples 1 to 3 and comparative example 1.
Detailed Description
The present invention will be further described with reference to the following drawings and examples, but the technical solution of the present invention is not limited thereto. In the following examples, reactive SiO was used2All the reactive groups modified on the surface of the nano particles are epoxy groups; the dimethylcyclosiloxane mixture comprises hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6), D4>95 percent, and the manufacturer is Shenzhen Jipeng silicon fluoride materials Limited.
Example 1
Under the condition of stirring (stirring is carried out throughout the whole reaction process), 100 g of DMC is heated to 90 ℃ and then 0.02 g of Me is added4NOH, and gradually heating to 110 ℃, reacting for 50 min (calculating time from heating to 90 ℃ and keeping the final temperature at 110 ℃), and then adding 1 g of reactive SiO2Nanoparticles (m-SiO)2) After the reaction is continued for 60min, the temperature is raised to 130 ℃ to remove the unreacted catalyst Me4NOH, reduced pressure distillation until no fraction is removed, and room temperature cooling to obtain compound A (m-SiO)2PDMS); then the prepared m-SiO2PDMS with 9 g of gas phase SiO2（n-SiO2) Mixing and stirring for 60min, adding 6 g of methyl tributyl ketoxime silane and 1.5 g of vinyl tributyl ketoxime silane, stirring for 10 min, adding 0.05 g of dibutyltin dilaurate, stirring for 10 min, defoaming in vacuum to obtain a crude product, and curing the crude product at room temperature for 10 days to obtain the multi-network liquid silicone rubber.
Example 2
100 g of DMC is heated to 90 ℃ under the condition of stirring, and then 0.02 g of Me is added4NOH, and gradually heating to 110 ℃, reacting for 50 min (calculating time from heating to 90 ℃, and finally keeping the temperature at 110 ℃), and then adding 0.5 gm-SiO2Continuing the reactionAfter 60min, the temperature is raised to 130 ℃ to remove the unreacted catalyst Me4NOH, reduced pressure distillation is carried out until no fraction is removed, and m-SiO is obtained after room temperature cooling2(ii)/PDMS; then the prepared m-SiO2PDMS and 9.5 g n-SiO2Mixing and stirring for 60min, adding 6 g of methyl tributyl ketoxime silane and 1.5 g of vinyl tributyl ketoxime silane, stirring for 10 min, adding 0.05 g of dibutyltin dilaurate, stirring for 10 min, defoaming in vacuum to obtain a crude product, and curing the crude product at room temperature for 10 days to obtain the multi-network liquid silicone rubber.
Example 3
100 g of DMC is heated to 90 ℃ under the condition of stirring, and then 0.02 g of Me is added4NOH, gradually heating to 110 ℃, reacting for 50 min (calculating time from heating to 90 ℃ and keeping the final temperature at 110 ℃), and then adding 2 g m-SiO2After the reaction is continued for 60min, the temperature is raised to 130 ℃ to remove the unreacted catalyst Me4NOH, reduced pressure distillation is carried out until no fraction is removed, and m-SiO is obtained after room temperature cooling2(ii)/PDMS; then the prepared m-SiO2PDMS and 8 g n-SiO2Mixing and stirring for 60min, adding 6 g of methyl tributyl ketoxime silane and 1.5 g of vinyl tributyl ketoxime silane, stirring for 10 min, adding 0.05 g of dibutyltin dilaurate, stirring for 10 min, defoaming in vacuum to obtain a crude product, and curing the crude product at room temperature for 10 days to obtain the multi-network liquid silicone rubber.
Example 4
100 g of DMC is heated to 90 ℃ under the condition of stirring, and then 0.02 g of Me is added4NOH, gradually increasing the temperature to 110 ℃, reacting for 90 min (calculating time from heating to 90 ℃ and keeping the final temperature at 110 ℃), and then adding 2 g m-SiO2After the reaction is continued for 60min, the temperature is raised to 130 ℃ to remove the unreacted catalyst Me4NOH, reduced pressure distillation is carried out until no fraction is removed, and m-SiO is obtained after room temperature cooling2(ii)/PDMS; then the prepared m-SiO2PDMS and 8 g n-SiO2Mixing and stirring for 60min, adding 6 g methyl tributyl ketoxime silane and 1.5 g vinyl tributyl ketoxime silane, stirring for 10 min, adding 0.05 g dibutyltin dilaurate, stirring for 10 min, and vacuum defoamingAnd then obtaining a crude product, and curing the crude product at room temperature for 10 days to obtain the multi-network liquid silicone rubber.
Example 5
100 g of DMC is heated to 90 ℃ under the condition of stirring, and then 0.02 g of Me is added4NOH, gradually increasing the temperature to 110 ℃, reacting for 50 min (calculating time from heating to 90 ℃ and keeping the final temperature at 110 ℃), and then adding 6 g m-SiO2After the reaction is continued for 60min, the temperature is raised to 130 ℃ to remove the unreacted catalyst Me4NOH, reduced pressure distillation is carried out until no fraction is removed, and m-SiO is obtained after room temperature cooling2(ii)/PDMS; then the prepared m-SiO2PDMS and 8 g n-SiO2Mixing and stirring for 60min, adding 6 g of methyl tributyl ketoxime silane and 1.5 g of vinyl tributyl ketoxime silane, stirring for 10 min, adding 0.05 g of dibutyltin dilaurate, stirring for 10 min, defoaming in vacuum to obtain a crude product, and curing the crude product at room temperature for 10 days to obtain the multi-network liquid silicone rubber.
Comparative example 1
100 g of PDMS with a viscosity of 50000 mPa ∙ s was mixed with 10 g of highly branched n-SiO2And (3) mechanically stirring for 60min, sequentially adding 6 g of methyl tributyl ketoxime silane and 1.5 g of vinyl tributyl ketoxime silane, continuously stirring for 10 min, then adding 0.05 g of dibutyltin dilaurate, stirring for 10 min, and vacuumizing and defoaming to obtain the blending-method liquid silicone rubber.
Comparative example 2
100 g of DMC is heated to 90 ℃ under the condition of stirring, and then 0.02 g of Me is added4NOH, and gradually heating to 110 ℃, reacting for 50 min (calculating time from heating to 90 ℃ and keeping the final temperature at 110 ℃), and then adding 10 g of reactive SiO2Nanoparticles (m-SiO)2) After the reaction is continued for 60min, the temperature is raised to 130 ℃ to remove the unreacted catalyst Me4And (3) distilling NOH under reduced pressure until no fraction is removed, and cooling at room temperature to obtain the liquid silicone rubber.
The mechanical properties of the liquid silicone rubbers prepared using examples 1-3 and comparative examples 1-2 are shown in Table 1.
TABLE 1 mechanical Properties of liquid Silicone rubbers prepared in examples 1-3 and comparative examples 1-2
It can be seen from table 1 that examples 1-3 obtained by the process of the present invention are superior in mechanical properties, much higher than those obtained by physical mixing (comparative example 1) or polymeric grafting (comparative example 2), especially in elongation at break, wherein example 2 is improved by 99.4% compared to comparative example 1 and 52.7% compared to comparative example 2, showing a significant synergistic effect. While the tensile strength of examples 1-3 can be determined by polymerizing SiO during the grafting process2The increase in the amount added indicates that the two SiO types can be adjusted2The proportion of the silicone rubber meets different use requirements.
Examples 1 to 3 differ by the addition of two SiO2In the step (2), reactive SiO2Nanoparticles and gas phase SiO2The addition ratio of (A) is different, and the aim is to explore two kinds of SiO2The proportion of the addition of (b) has an influence on the reinforcing effect, the reactive SiO used2The nanometer particles are pilot-plant product RNS-E type silicon dioxide produced by national local combined engineering research center of application technology of nanometer hybrid materials, the surface of the pilot-plant product RNS-E type silicon dioxide is modified with epoxy groups, and reactive SiO used in the application is2The primary particle diameter of the nano-particles is 5-60nm, and the size of the aggregation structure is 1-10 μm.
Comparative example 1 is a liquid silicone rubber prepared by a conventional blending method using a commercially available hydroxyl terminated PDMS with a viscosity of 50000 mPa ∙ s and a gas phase SiO2Is H L-200.
Comparative example 2 differs from example 1 in that comparative example 2 only employs SiO reactive with the polymerization of PDMS2The nanoparticles were grafted, i.e., the process of comparative example 2 used only the first step of example 1 and did not involve the second step of blending.
For the purpose of comparative analysis, SiO in examples 1-3 and comparative examples 1-22The total content is 10%.
FIG. 2 shows the m-SiO obtained in example 12Dissolving PDMS in toluene solvent, washing and extracting for multiple times to obtain m-SiO2(RNS-E) infrared spectrum. Toluene is a good solvent for polysiloxanes, and can dissolve polysiloxanes, but cannot dissolve SiO2. After repeated elution with toluene solvent, the free or adsorbed SiO2The polysiloxane on the surface is washed off but can not be combined on SiO through chemical bonding2The surface polysiloxane washed away. 3433 cm can be seen on the infrared spectrum-1And 1629cm-1The positions of the two parts respectively correspond to a stretching vibration peak and a bending vibration peak of Si-OH, and are 1092 cm-1And 803 cm-1The positions of the two vibration peaks respectively correspond to an asymmetric stretching vibration peak and a symmetric stretching vibration peak of Si-O-Si, and are 2965 cm-1And 1261 cm-1Respectively corresponding to the asymmetric stretching vibration peak and Si-CH of C-H3Symmetric stretching vibration peak of 847 cm-1The position corresponds to the peak of the asymmetric stretching vibration of the epoxy group. By comparing the RNS-E with the extracted RNS-E infrared spectrum, the Si-OH characteristic peak intensity is weakened, and the peak intensity of the C-H bond is increased, which indicates that the PDMS chain segment is grafted to the SiO through the chemical bond2A surface; in addition, the characteristic peak of the epoxy group is weakened, which is probably because in the reaction process, part of the epoxy group generates ring-opening reaction, and SiO is improved2The reactivity of (a).
Fig. 3 is a rheological curve before the liquid silicone rubber prepared in example 1 and comparative example 1 is cured, and it can be seen from fig. 3 that the shear thinning phenomenon of the two samples is very obvious, the viscosity is very obviously reduced under the action of lower shear force, but the viscosity of example 1 is always higher than that of comparative example 1. It is shown that the transient network structure strength of example 1 is higher than that of comparative example 1, and SiO contained in example 1 and comparative example 12The total amount of (A) is 10%, except that the preparation method is different, in example 1, the surface modified SiO2The bonding effect between the filler and PDMS is a strong chemical bond effect, H L-200 with a developed network is added in a blending mode on the basis, a secondary network structure is constructed through a hydrogen bond effect, and the comparative example 1 is only a single network structure mainly based on the filler-filler effect, and the interaction is weak, so that the viscosity is always low.
FIG. 4 is a scanning electron micrograph of a tensile cross section of the liquid silicone rubbers prepared in examples 1 to 3 and comparative example 1, and it can be seen from FIG. 4 that the cross section morphologies of examples 1 to 3 are significantly different from those of comparative example 1, the cross section of the sample in comparative example 1 is more flat, and the cross section morphologies of examples 1 to 3 exhibit a significant tearing phenomenon, which is closely related to the internal structure thereof, to further illustrate the formation of a multiple cross-linked network structure of the silicone rubber of the present invention.
FIG. 5 is a scanning electron micrograph of brittle fracture surface of liquid silicone rubber treated with liquid nitrogen prepared in examples 1-3 and comparative example 1, and it is apparent that SiO in the samples of examples 1-32The dispersion is more uniform, which shows that the invention is beneficial to improving SiO2Dispersion of (2).
FIG. 6 is a stress-strain curve of the liquid silicone rubbers prepared in examples 1-3 and comparative example 1, from which it can be seen that the elongation at break of the silicone rubbers obtained in examples 1-3 is significantly improved by nearly 1-fold or more, and by adjusting m-SiO2And n-SiO2The addition proportion of (A) can further regulate and control the performance of the liquid silicone rubber. The great improvement of the mechanical property is benefited by the construction of a liquid silicon rubber multi-network structure.
As shown in FIG. 1, the present invention prepares a multiple network liquid silicone rubber by two steps, the first step is to use SiO with surface modified with reactive groups2Polymerizing with PDMS to graft PDMS to SiO2Surface, SiO reinforcement2The bonding effect between the primary structure and PDMS is obtained2(ii)/PDMS; the second step is blending, using highly branched gas phase SiO2The liquid silicone rubber with the multiple cross-linked network structure is prepared by constructing the secondary network structure of PDMS through hydrogen bond action in a developed network.
It should be noted that the curing time used in the examples of the present invention is 10 days, which is not a limitation of the present invention, as long as the crude product is cured.
Claims (5)
1. The preparation method of the multi-network liquid silicone rubber is characterized by comprising the following steps:
(1) heating the polysiloxane monomer to 80-100 deg.CAdding a catalyst I after the reaction is finished, mixing, heating to 100 ℃ and 130 ℃ under the stirring condition, reacting for 50-90 min, and then adding reactive SiO2After the nano particles continue to react for 40-80 min, removing the unreacted catalyst I, and concentrating under reduced pressure to obtain a compound A, wherein the compound A is the base adhesive;
(2) the compound A and gas phase SiO2Uniformly mixing, sequentially adding a cross-linking agent and a catalyst II, stirring for 10-30min to obtain a crude product, and curing the crude product at room temperature to obtain the catalyst;
the polysiloxane monomer in the step (1) is a dimethyl cyclosiloxane mixture;
the catalyst I in the step (1) is an alkaline catalyst which is metal hydroxide, alkali metal alkoxide or quaternary ammonium base, and the using amount of the catalyst I is 0.01-0.02% of the mass of the polysiloxane monomer;
reactive SiO in step (1)2The reactive group modified on the surface of the nanometer particles is one of epoxy group, amino group or sulfydryl, and the reactive SiO is2The addition amount of the nano particles is 0.5-10% of the mass of the basic glue;
the gas phase SiO in the step (2)2The amount of the adhesive is 1-15% of the mass of the basic adhesive;
in the step (2), the catalyst II is an organic tin catalyst, and the dosage of the catalyst II is 0.05-0.15% of the mass of the basic adhesive.
2. The method for preparing multi-network liquid silicone rubber according to claim 1, wherein the unreacted catalyst I in step (1) can be removed by heating to 130 ℃ and 150 ℃ to decompose the unreacted catalyst I or neutralizing with acid and alkali.
3. The method for preparing a multiple network liquid silicone rubber according to claim 1, wherein the crosslinking agent in step (2) is a ketoxime moisture-curable crosslinking agent in an amount of 4 to 8% by mass based on the mass of the base rubber.
4. The method for preparing a multiple network liquid silicone rubber according to claim 1, wherein catalyst i is tetramethylammonium hydroxide and catalyst ii is dibutyltin dilaurate.
5. The multi-network liquid silicone rubber prepared by the method of any one of claims 1 to 4.
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|---|---|---|---|---|
| EP1627895A1 (en) * | 2004-08-19 | 2006-02-22 | Wacker Chemie AG | Silicon rubber composition comprising mineral fibers |
| CN103937257A (en) * | 2014-03-24 | 2014-07-23 | 惠州市安品新材料有限公司 | Organic silicone thixotropic agent and thixotropy addition type liquid silicone rubber |
| CN106832319A (en) * | 2017-01-22 | 2017-06-13 | 河南大学 | A kind of method that original position prepares nano silicon/hydroxyl-terminated injecting two methyl siloxane hybrid material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1627895A1 (en) * | 2004-08-19 | 2006-02-22 | Wacker Chemie AG | Silicon rubber composition comprising mineral fibers |
| CN103937257A (en) * | 2014-03-24 | 2014-07-23 | 惠州市安品新材料有限公司 | Organic silicone thixotropic agent and thixotropy addition type liquid silicone rubber |
| CN106832319A (en) * | 2017-01-22 | 2017-06-13 | 河南大学 | A kind of method that original position prepares nano silicon/hydroxyl-terminated injecting two methyl siloxane hybrid material |
Non-Patent Citations (1)
| Title |
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| "Effect of nano-silica filler on-microstructure and mechanical properties of polydimethylsiloxane-based nanocomposites prepared by "inhibition-grafting"method";jian liu etal;《Composites Science and Technology》;20181020;第167卷;第355-363页 * |
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