CN111647386B - Preparation method of silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive - Google Patents
Preparation method of silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/16—Adhesives based on 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; Adhesives based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
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- C01B32/00—Carbon; Compounds thereof
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C08K3/38—Boron-containing compounds
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Abstract
A method for preparing a silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive. The method comprises the steps of preparing a rubber-based liquid by utilizing vinyl polycarbosilane, polymethylsiloxane, phenolic resin, ferrocene and isopropanol, taking aluminum powder, nickel powder, silicon powder, boron carbide powder and borate glass powder as a filler mixture, and preparing the high-temperature rubber by mixing the rubber-based liquid and the filler mixture. The invention has the following effects: the high-temperature adhesive can grow silicon carbide nanowires in situ at 1100 ℃ to be toughened, so that the bonding performance of the high-temperature adhesive is greatly improved within the range of 1100-1500 ℃, and particularly after 1300 ℃, the normal-temperature bonding strength of the high-temperature adhesive is improved by 59.2% compared with that of a blank sample without nanowire growth. After the silicon carbide nanowires grow in situ, the high-temperature adhesive shows good toughness at both normal temperature and high temperature, and an obvious approximate yield stage appears on a fracture displacement curve of a bonded bonding piece, so that the high-temperature adhesive is fully shown to have high use safety.
Description
Technical Field
The invention belongs to the technical field of adhesive material preparation, and particularly relates to a preparation method of a silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive.
Background
The adhesive has the characteristics of high connection efficiency, simple operation, low cost and the like, so that the adhesive is widely applied to the production and life of people, wherein the high-temperature adhesive can be directly applied to a high-temperature environment (up to 1500 ℃) after being cured and connected at low temperature, has small stress concentration of a connection interface, has small damage to a base body and the like, and is used for connecting, installing, fixing and repairing certain high-temperature components. These high temperature components typically include components made of high temperature resistant ceramics, ceramic matrix composites, and high temperature alloys. However, the joint strength and toughness of the conventional high-temperature adhesive are still low, and the conventional high-temperature adhesive needs to be toughened and reinforced.
The traditional third-party phase strengthening means limits the application of the method in the preparation of high-temperature glue due to higher cost and difficult solution of agglomeration, and the in-situ grown whisker self-toughening technology is applied to the strengthening of the high-temperature glue due to the characteristics of lower cost, high dispersion of grown whiskers and the like, wherein the in-situ toughening technology for growing mullite whiskers by aluminum fluoride catalysis is most commonly applied. However, the aluminum fluoride catalyst has a severe erosion property to the silicon-containing and aluminum-containing oxides in the glue matrix at high temperature, which easily causes the high-temperature-resistant glue to be porous, and the reduction of compactness causes the attenuation of the bonding effect. Therefore, the method has important significance for preparing the in-situ growth self-toughening type high-temperature adhesive with more prominent strengthening effect by searching for the novel in-situ growth micro-nano phase suitable for the field of adhesive bonding.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method of a silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive.
In order to achieve the aim, the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive provided by the invention comprises the following steps in sequence:
(1) uniformly mixing vinyl polycarbosilane, polymethylsiloxane, phenolic resin, ferrocene and isopropanol according to the mass ratio of 3.5-4.5: 1-2: 0.75-1.25: 0.6-0.9: 1.5-2.5, and then stirring for 5-6 h at 65 ℃ to prepare a gel base solution;
(2) fully and uniformly mixing aluminum powder, nickel powder, silicon powder, boron carbide powder and borate glass powder according to the mass ratio of 1.5-2.5: 1-1.5: 0.35-0.6: 0.15-0.3: 0.1-0.2 to prepare a filler mixture;
(3) and (3) mixing the glue base liquid prepared in the step (1) and the filler mixture prepared in the step (2) in a ball milling tank according to a liquid-solid mass ratio of 5-7: 4-5, and carrying out ball milling for 2-3 h at a rotating speed of 150-200 r/min to obtain the gray black silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature glue with the viscosity of 2500-3000 cps.
In step (1), the vinyl polycarbosilane is in liquid state, and is purchased from chemical research institute of Chinese academy of sciences, with a model number of VHCPS and a viscosity of 650-1000 cps.
In step (1), the polymethylsiloxane is a white powder available from Wacker-Belsil, GermanyTMCompany, chemical formula (CH)3–SiO3/2)x。
In the step (1), the phenolic resin is in a liquid state, is purchased from Jining HuaKai resin Co., Ltd, and has a viscosity of 1000 to 1500 cps.
In the step (1), the ferrocene and the isopropanol are purchased from Aladdin chemical reagent, Inc., and the components are analytically pure.
In the step (2), the aluminum powder is purchased from Beijing Xin Rui technology limited and has a particle size of 3-5 μm.
In the step (2), the silicon powder and the nickel powder are both purchased from Guangzhou Tuoyi trade company Limited and have the particle size of 0.5 μm.
In step (2), the boron carbide powder is obtained from Heilongjiang morning boron carbide Co., Ltd and has a particle size of 6 to 10 μm.
The silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive provided by the invention has the following beneficial effects:
1. compared with a blank control sample without nanowire growth, the bonding strength of the high-temperature adhesive is obviously improved at 1100-1500 ℃, and particularly the bonding strength of the high-temperature adhesive is improved by about 59.2% after treatment at 1300 ℃.
2. After treatment at 1300-1500 ℃, the high-temperature adhesive shows obvious anti-fracture yield effect at both normal temperature and high temperature, which shows that the brittleness is obviously improved;
3. the silicon carbide nanowires grow in the space (cracks, holes and the like) of the high-temperature glue, play a role in repairing the glue internal structure, and are the main reason why the high-temperature glue has an excellent bonding effect.
Drawings
FIG. 1 is a scanning electron microscope image of the surface morphology of the silicon carbide nanowire in-situ growth toughened ceramic precursor type high temperature adhesive prepared in example 1 after being processed at different temperatures; wherein FIG. 1(a) is 1000 ℃, FIG. 1(b) is 1100 ℃, FIG. 1(c) is 1300 ℃, and FIG. 1(d) is 1500 ℃;
FIG. 2 is a TEM photograph of a single SiC nanowire in the SiC nanowire in-situ grown toughened ceramic precursor type high temperature glue prepared in example 1;
FIG. 3 is a comparison of the shear strength of the carbon/carbon composite material bonded part of the silicon carbide nanowire in-situ growth toughened ceramic precursor type high temperature glue prepared in example 1 and a blank sample without nanowire growth after treatment at different temperatures;
FIG. 4 is a comparison of the loading force-displacement curves of the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive prepared in example 1 and the carbon/carbon composite material adhesive bonded by the blank sample without nanowire growth under different conditions;
FIG. 5 is a fracture surface morphology analysis of a carbon-carbon composite material bonded piece bonded with the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive prepared in example 1 after a shear test; in FIG. 5, the wavelength was 500nm in FIG. 5(a), 400nm in FIG. 5(b), and 1 μm in FIG. 5 (c).
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive provided by the embodiment comprises the following steps in sequence:
(1) uniformly mixing vinyl polycarbosilane, polymethylsiloxane, phenolic resin, ferrocene and isopropanol according to the mass ratio of 3.5:1.5:1:0.6:2.5, and stirring for 5 hours at the temperature of 65 ℃ to prepare a gel base solution;
(2) fully and uniformly mixing aluminum powder, nickel powder, silicon powder, boron carbide powder and borate glass powder according to the mass ratio of 1.5:1:0.35:0.2:0.1 to prepare a filler mixture;
(1) and (3) mixing the glue base liquid prepared in the step (1) and the filler mixture prepared in the step (2) in a ball milling tank according to the liquid-solid mass ratio of 5:4, and carrying out ball milling for 2h at the rotating speed of 200r/min to obtain the gray-black silicon carbide nanowire in-situ growth toughened ceramic precursor high-temperature glue with the viscosity of about 2500 cps.
Example 2
(1) Uniformly mixing vinyl polycarbosilane, polymethylsiloxane, phenolic resin, ferrocene and isopropanol according to the mass ratio of 4:2:1.25:0.9:2, and stirring for 6 hours at the temperature of 65 ℃ to prepare the colloidal base solution.
(2) Fully and uniformly mixing aluminum powder, nickel powder, silicon powder, boron carbide powder and trace borate glass powder according to the mass ratio of 2:1.5:0.5:0.15:0.2 to prepare a filler mixture;
(3) and (3) mixing the glue base liquid prepared in the step (1) and the filler mixture prepared in the step (2) in a ball milling tank according to the liquid-solid mass ratio of 6:5, and carrying out ball milling for 3 hours at the rotating speed of 200r/min to obtain the gray-black silicon carbide nanowire in-situ growth toughened ceramic precursor high-temperature glue with the viscosity of about 2500 cps.
Example 3
(1) Uniformly mixing vinyl polycarbosilane, polymethylsiloxane, phenolic resin, ferrocene and isopropanol according to the mass ratio of 4.5:1.5:0.75:0.7:1.5, and stirring for 6 hours at the temperature of 65 ℃ to prepare the colloidal base solution.
(2) Fully and uniformly mixing aluminum powder, nickel powder, silicon powder, boron carbide and trace borate glass powder according to the mass ratio of 2.5:1:0.6:0.3:0.1 to prepare a filler mixture;
(3) and (3) mixing the glue base liquid prepared in the step (1) and the filler mixture prepared in the step (2) in a ball milling tank according to the liquid-solid mass ratio of 7:5, and carrying out ball milling for 3 hours at the rotating speed of 150r/min to obtain the gray-black silicon carbide nanowire in-situ growth toughened ceramic precursor high-temperature glue with the viscosity of about 2500 cps.
In the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive prepared by the method, the main binding phase is a copolymer of polycarbosilane, polysiloxane and resin; ferrocene is a growth catalyst of the silicon carbide nanowire; the silicon powder, the aluminum powder and the nickel powder are used as the most main additives, and are used for generating a high-temperature ceramic phase on one hand and a temperature-resistant intermetallic compound on the other hand; boron carbide and glass powder are mainly melted at high temperature to improve the structure of the high-temperature glue; meanwhile, the oxidation of boron carbide can effectively compensate the volume shrinkage of the high-temperature agent in the heat treatment process.
In order to verify the toughening and reinforcing effects of the high temperature adhesive provided in the above embodiment, the inventor uses the high temperature adhesive without nanowire growth (without ferrocene) as a blank control sample, and the preparation method of the blank control sample is as follows:
(1) uniformly mixing vinyl polycarbosilane, polymethylsiloxane, phenolic resin and isopropanol according to the mass ratio of 3.5:1.5:1:2.5, and stirring for 5 hours at 65 ℃ to prepare the rubber base liquid.
(2) Fully and uniformly mixing aluminum powder, nickel powder, silicon powder, boron carbide and trace borate glass powder according to the mass ratio of 1.5:1:0.35:0.2:0.1 to prepare a filler mixture;
(3) and (3) mixing the glue base liquid prepared in the step (1) and the mixed filler prepared in the step (2) in a ball milling tank according to the liquid-solid mass ratio of 5:4, and carrying out ball milling for 2 hours at the rotating speed of 200r/min to obtain the gray-black high-temperature glue with the viscosity of about 2500 cps.
The experimental procedure was as follows:
1) the carbon/carbon composite material plate (30 multiplied by 10 multiplied by 3mm) which is polished, cleaned and dried is laid on a smooth and flawless glass plate, and the bonding surface is placed upwards;
2) the high-temperature glue and the blank control sample prepared in the above example were respectively spread on the entire one surface of each adherend using a spatula, and then the thickness of the high-temperature glue was controlled to 200 μm using an applicator;
3) bonding two carbon/carbon composite material plates together in a mode that bonding surfaces are opposite, pressing the plates into a bonding piece, curing the bonding piece at 200 ℃ for 2 hours, and then cutting the bonding piece into a double-notch test piece, wherein the area of the bonding surface is 12 multiplied by 10mm2；
4) Calcining the test piece in a high temperature furnace at different temperatures (300 deg.C, 400 deg.C, 500 deg.C, 600 deg.C, 700 deg.C, 800 deg.C, 900 deg.C, 1000 deg.C, 1100 deg.C, 1200 deg.C, 1300 deg.C, 1400 deg.C, 1500 deg.C) for 1 h;
5) and (3) observing the microstructure of the high-temperature adhesive: the bonded parts treated at different temperatures were prepared into SEM test samples, and the morphology of the high temperature glue in the bonded area was observed with a scanning electron microscope analyzer (Nanosem430, FEI), as shown in fig. 1.
As can be seen from FIG. 1, after the treatment at 1000 ℃, no nanowire is generated in the high-temperature glue; after the treatment at 1100 ℃, a small amount of short and thick linear bodies begin to be generated; after 1300 ℃, the slender nanowires are fully distributed with the glue matrix, the length-diameter ratio of the nanowires is about 30-40, and the high-temperature glue structure is still compact; after 1500 ℃, the length-diameter ratio of the nanowire is continuously increased to be more than 50.
6) Transmission analysis of nanowires: transmission scanning electron microscopy (Tecnai G2F 20, FEI) was used to demonstrate that the in-situ grown nanowire composition is silicon carbide, and a high-low power transmission photograph thereof is shown in FIG. 2. As can be seen from fig. 2: single crystal electron diffraction showed (111), (210) and
three facets, with a interplanar spacing along the growth direction of 0.25nm, is sufficient to demonstrate that the in situ grown nanowire component is beta-silicon carbide.
6) And (3) shear testing: the ordinary temperature bonding strength of the bonding piece treated at different temperatures is tested by using a CSS-44001 universal testing machine, the high temperature shearing strength of the bonding piece at high temperature is tested by using an RDL-15 high temperature universal testing machine, the bonding performance and the fracture toughness of the high temperature adhesive prepared in the comparative example and the blank control sample without nanowire growth are evaluated, and the ordinary temperature bonding strength of the two high temperature adhesives treated at different temperatures and the loading force-displacement curve under different conditions are respectively shown in fig. 3 and fig. 4;
as can be seen from FIG. 3, the bonding strength of the high temperature adhesive prepared in the example is improved from 1000 ℃, and the bonding strength at normal temperature is much higher than that of the blank control sample in the temperature range of 1100-1500 ℃; the bonding strength of the high temperature glue prepared in the above example after treatment at 1100 ℃, 1200 ℃, 1300 ℃, 1400 ℃ and 1500 ℃ was improved by 24.8%, 41.7%, 59.2%, 55.4% and 51.0%, respectively, compared to a blank control sample without nanowire growth.
As can be seen from fig. 4, compared with the blank control sample without nanowire growth, the fracture toughness of the high-temperature adhesive bonding piece prepared in the above embodiment is obviously improved after being treated at 1300 ℃ and tested at normal temperature, and an obvious approximate yield stage appears on the loading displacement curve, which proves that the growth of the nanowire effectively obtains the toughening effect. Meanwhile, the fracture displacement of the bonded part bonded by the high-temperature adhesive is higher than the test result of the normal temperature even at 1300 ℃, which is enough to show that the high-temperature adhesive prepared in the embodiment has higher damage resistance at high temperature.
7) And (3) observing a fracture surface: the morphology of the bonded surface after fracture by shear test was observed using a scanning electron microscope, as shown in fig. 5. The silicon carbide nanowires mainly grow in existing defect cracks of the high-temperature-resistant adhesive, and the cracks are effectively repaired in a bridging or overlapping mode, namely the structure of the high-temperature-resistant adhesive is improved; furthermore, as can be seen from fig. 5c, the growth of the nanowires also effectively hinders the propagation of cracks, which is another important reason for the toughening enhancement.
Those skilled in the art, having the benefit of this disclosure, will appreciate numerous modifications and variations there from, and fall within the scope of the invention.
Claims (8)
1. A preparation method of a silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive is characterized by comprising the following steps: the preparation method comprises the following steps which are carried out in sequence:
(1) uniformly mixing vinyl polycarbosilane, polymethylsiloxane, phenolic resin, ferrocene and isopropanol according to the mass ratio of 3.5-4.5: 1-2: 0.75-1.25: 0.6-0.9: 1.5-2.5, and then stirring for 5-6 h at 65 ℃ to prepare a gel base solution;
(2) fully and uniformly mixing aluminum powder, nickel powder, silicon powder, boron carbide powder and borate glass powder according to the mass ratio of 1.5-2.5: 1-1.5: 0.35-0.6: 0.15-0.3: 0.1-0.2 to prepare a filler mixture;
(3) and (3) mixing the glue base liquid prepared in the step (1) and the filler mixture prepared in the step (2) in a ball milling tank according to a liquid-solid mass ratio of 5-7: 4-5, and carrying out ball milling for 2-3 h at a rotating speed of 150-200 r/min to obtain the gray black silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature glue with the viscosity of 2500-3000 cps.
2. The method for preparing the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive according to claim 1, which is characterized by comprising the following steps: in the step (1), the vinyl polycarbosilane is in a liquid state, the model is VHCPS, and the viscosity is 650-1000 cps.
3. The method for preparing the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive according to claim 1, which is characterized by comprising the following steps: in the step (1), the polymethylsiloxane is white powder.
4. The method for preparing the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive according to claim 1, which is characterized by comprising the following steps: in the step (1), the phenolic resin is in a liquid state, and the viscosity is 1000-1500 cps.
5. The method for preparing the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive according to claim 1, which is characterized by comprising the following steps: in step (1), the ferrocene and isopropanol components are analytically pure.
6. The method for preparing the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive according to claim 1, which is characterized by comprising the following steps: in the step (2), the particle size of the aluminum powder is 3-5 μm.
7. The method for preparing the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive according to claim 1, which is characterized by comprising the following steps: in the step (2), the particle size of the silicon powder and the nickel powder is 0.5 μm.
8. The method for preparing the silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive according to claim 1, which is characterized by comprising the following steps: in the step (2), the particle size of the boron carbide powder is 6-10 μm.
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| US7378362B2 (en) * | 2000-09-29 | 2008-05-27 | Goodrich Corporation | Boron carbide based ceramic matrix composites |
| CN107903067A (en) * | 2017-12-01 | 2018-04-13 | 苏州宏久航空防热材料科技有限公司 | A kind of growth in situ SiC nanowire enhancing SiC ceramic based composites and preparation method thereof |
| CN109516828B (en) * | 2018-10-15 | 2021-03-30 | 广东工业大学 | Novel connection method of silicon carbide ceramic for core, silicon carbide ceramic prepared by connection method and application of silicon carbide ceramic |
| CN111187092B (en) * | 2019-05-20 | 2021-10-01 | 中国科学院上海硅酸盐研究所 | Suspension slurry and method for reactive joining of silicon carbide ceramics |
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