CN112444445A - Method for preparing silicon carbide fiber bundle mechanical sample by using solvent-free glue solution - Google Patents
Method for preparing silicon carbide fiber bundle mechanical sample by using solvent-free glue solution Download PDFInfo
- Publication number
- CN112444445A CN112444445A CN202011126057.8A CN202011126057A CN112444445A CN 112444445 A CN112444445 A CN 112444445A CN 202011126057 A CN202011126057 A CN 202011126057A CN 112444445 A CN112444445 A CN 112444445A
- Authority
- CN
- China
- Prior art keywords
- fiber bundle
- frame
- silicon carbide
- glue solution
- epoxy resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 94
- 239000003292 glue Substances 0.000 title claims abstract description 48
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000003822 epoxy resin Substances 0.000 claims abstract description 27
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 27
- 238000004804 winding Methods 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 238000004321 preservation Methods 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 8
- 239000011324 bead Substances 0.000 claims abstract description 6
- 238000005470 impregnation Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 7
- 239000000123 paper Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 239000004745 nonwoven fabric Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 238000005520 cutting process Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 32
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 229960001124 trientine Drugs 0.000 description 8
- 239000002904 solvent Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 239000002390 adhesive tape Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000004033 plastic Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 206010018338 Glioma Diseases 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 150000001412 amines Chemical group 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
- G01N3/04—Chucks
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0067—Fracture or rupture
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0262—Shape of the specimen
- G01N2203/0278—Thin specimens
- G01N2203/028—One dimensional, e.g. filaments, wires, ropes or cables
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides a method for preparing a silicon carbide fiber bundle mechanical sample by using solvent-free glue solution, which comprises the following steps: continuously winding the silicon carbide fiber bundle wire to be tested on the frame, tightening the fiber bundle wire, and fixing the start end and the stop end; placing the epoxy resin and the frame wound with the fiber bundle yarns in an oven for heat preservation; weighing a curing agent in epoxy resin, and mixing to obtain a uniform glue solution; putting the frame after heat preservation into glue solution for impregnation; taking out the impregnated frame, keeping the frame vertically placed along the extension direction of the fiber, wiping off the rubber beads after the rubber solution completely flows out, and curing; and after the solidified silicon carbide fiber bundle wire is cooled to room temperature, cutting the silicon carbide fiber bundle wire between the winding ends, sticking reinforcing sheets at the two ends, and carrying out mechanical property test. The invention solves the defects existing in the mechanical property test of the silicon carbide fiber bundle by using the glue solution containing the organic solvent at present, and the bundle prepared by using the solvent-free glue solution has small discrete coefficient of tensile strength, high sample preparation efficiency and high detection accuracy.
Description
Technical Field
The invention belongs to the technical field of material testing, and particularly relates to a method for preparing a silicon carbide fiber bundle mechanical sample by using a solvent-free glue solution.
Background
The silicon carbide (SiC) fiber has incomparable excellent performances of other inorganic fibers such as high strength, high modulus, excellent high-temperature oxidation resistance and the like, and has wide application prospect in high-tech fields such as aerospace, weaponry, ship and nuclear industries and the like as an important reinforcement of the ceramic matrix composite, thereby becoming one of key strategic raw materials for developing high-tech weaponry and aerospace industries.
In the aspect of performance evaluation and characterization of the silicon carbide fiber, the strength, modulus and elongation at break of the bundle fiber are one of the basic mechanical performance parameters of the ceramic fiber and are especially important one of a plurality of performance indexes. At present, the sample preparation and the test for tensile property of SiC fiber bundle filaments in China mainly refer to GB/T34520.4-2017 continuous silicon carbide fiber test method part 4 formulated in 2017: drawing performance of the bundle filament, wherein the glue solution for preparing the sample of the SiC fiber bundle filament is composed of epoxy resin, curing agent and a certain amount of acetone as a solvent. The optional epoxy resin provided by the standard has high room-temperature viscosity, cannot be directly used, and a certain amount of solvent is required to be added to improve the resin fluidity, so that the defects that the surface of a prepared fiber sample does not form gliomas or uneven thickness in the length direction after being cured can be overcome.
However, acetone needs to be dried at room temperature for a long time to be fully volatilized, triethylene tetramine is used as a curing agent, moisture is easily absorbed, if the fiber bundle impregnated with glue solution is exposed for too long time under the air condition in the operation process, particularly when the fiber bundle is placed in an environment with high air humidity for a long time, moisture in the air is wrapped among the bundle filaments, the fiber bundle is not easy to discharge during heating and curing, and the defects of formed bubbles, holes and the like cause large dispersion of test results and difficulty in reflecting the intrinsic performance of the material.
Disclosure of Invention
In order to overcome the defects in the prior art, the inventor of the invention carries out intensive research and provides a method for preparing a silicon carbide fiber bundle mechanical sample by using a solvent-free glue solution, the solvent-free glue solution has proper viscosity at room temperature and good wettability with the surface of silicon carbide fiber, the prepared mechanical property sample bundle wire tensile fracture is smooth and cut, the defects are effectively avoided, the dispersion coefficient of the bundle wire strength test result is obviously reduced, the sample preparation time is shortened, and the preparation efficiency is improved, thereby completing the invention.
The technical scheme provided by the invention is as follows:
a method for preparing a silicon carbide fiber bundle silk mechanics sample by using solvent-free glue solution comprises the following steps:
continuously winding a silicon carbide fiber bundle wire to be tested on a frame, applying tension to the fiber bundle wire to tighten the silicon carbide fiber bundle wire to be tested, and fixing the two ends of the start and stop of the fiber bundle wire by using a fixing material;
pouring epoxy resin into a container, putting the frame wound with the fiber bundle yarns in the step (1) into an oven, and keeping the temperature at 30-40 ℃ for 0.5-2 hours;
step (3), weighing a curing agent according to the proportion of 10-18 parts of epoxy resin and 1 part of curing agent, adding the curing agent into the epoxy resin subjected to heat preservation in the step (2), mixing to obtain glue solution, and quickly and uniformly stirring;
step (4), transferring the glue solution in the step (3) into a container, and putting the frame subjected to heat preservation in the step (2) into the container for impregnation;
step (5), taking out the impregnated frame in the step (4), keeping the frame vertically placed along the fiber extension direction, and wiping off the glue beads by using paper, non-woven fabric or fabric with adsorption capacity after the glue solution runs out;
step (6), placing the frame in the step (5) on a tool support to ensure that the tested working section of the fiber bundle is not contacted with other objects, placing the tool support in drying equipment for curing, wherein the curing temperature is 100-150 ℃, and keeping the temperature for 0.5-1 hour;
and (7) after the silicon carbide fiber bundle wires solidified in the step (6) are cooled to room temperature, intercepting the silicon carbide fiber bundle wires between the winding ends, pasting reinforcing sheets at the two ends, and carrying out mechanical property test.
According to the method for preparing the silicon carbide fiber bundle mechanical sample by using the solvent-free glue solution, the method has the following beneficial effects:
(1) according to the invention, through screening the resin for strand impregnation, bisphenol F type or bisphenol A type epoxy resin with viscosity of not more than 4000 mPa.S at room temperature is used, and the composition and curing conditions of the glue solution are optimized, so that a solvent-free glue solution with proper room temperature viscosity is obtained, and the method is suitable for home-made silicon carbide fiber strand impregnation;
(2) according to the invention, the solvent-free glue solution is used for preparing the sample of the mechanical property of the strand, the prepared silicon carbide fiber strand has a smooth and uniform surface, the inside of the fiber strand is fully infiltrated, and the cross section of the tensile fracture position is kept circular and has no defects such as bubbles and nodules;
(3) the discreteness of the tensile strength of the silicon carbide fiber bundle prepared by the invention is less than or equal to 6 percent, and the discreteness coefficient is obviously reduced;
(4) the solvent-free glue solution used in the invention is safe and reliable, does not need to be placed in a room temperature for airing before curing, can be directly placed in an oven for curing, has high curing efficiency, and greatly shortens the sample preparation time;
(5) the solvent-free glue solution used in the invention has no special requirements on the air humidity and temperature of the dipping environment, and is convenient to operate.
Drawings
FIG. 1 is a microstructure of a tensile fracture of a silicon carbide fiber bundle prepared in example 1 of the present invention;
FIG. 2 is a microstructure of a tensile fracture of a silicon carbide fiber bundle prepared in example 2 of the present invention;
FIG. 3 is a microstructure of a tensile fracture of a bundle filament prepared in comparative example 1 using a solvent-containing glue solution;
FIG. 4 is a microstructure of a tensile fracture of a bundle filament prepared in comparative example 2 using a solvent-containing glue solution;
fig. 5 is a schematic view of a tool for fixedly winding a silicon carbide fiber frame according to a preferred embodiment of the invention.
Description of the reference numerals
1-a support frame; 2-a groove clamping strip; 3-clamping the silk; 4-frame.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
The invention provides a method for preparing a silicon carbide fiber bundle mechanical sample by using solvent-free glue solution, which comprises the following steps:
continuously winding a silicon carbide fiber bundle wire to be tested on a frame, applying tension to the fiber bundle wire to tighten the silicon carbide fiber bundle wire to be tested, and fixing the two ends of the start and stop of the fiber bundle wire by using a fixing material;
pouring epoxy resin into a container, putting the frame wound with the fiber bundle yarns in the step (1) into an oven, and keeping the temperature at 30-40 ℃ for 0.5-2 hours;
step (3), weighing a curing agent, adding the curing agent into the epoxy resin subjected to heat preservation in the step (2), mixing to obtain a glue solution, and quickly and uniformly stirring;
step (4), transferring the glue solution obtained in the step (3) into a container, and putting the frame subjected to heat preservation in the step (2) into the container to perform normal-temperature normal-pressure impregnation for 5-20 minutes;
step (5), taking out the impregnated frame in the step (4), keeping the frame vertically placed along the fiber extension direction, and wiping off the glue beads by using paper, non-woven fabric or fabric with adsorption capacity after the glue solution runs out;
step (6), placing the frame in the step (5) on a tool support to ensure that the tested working section of the fiber bundle is not contacted with other objects, and placing the tool support in drying equipment for curing;
and (7) after the silicon carbide fiber bundle wires solidified in the step (6) are cooled to room temperature, intercepting the silicon carbide fiber bundle wires between the winding ends, adhering paper, metal or plastic reinforcing sheets at the two ends, and carrying out mechanical property test.
In a preferred embodiment of the present invention, in the step (1), the frame for winding the fiber bundle wire may be a jig having a quadrangular structure made of metal, graphite, ceramic, or the like, in which two opposite sides for winding the fiber bundle wire are parallel, and a portion contacting with the fiber bundle wire is not allowed to have a corner, preferably a rounded corner.
In a preferred embodiment of the present invention, in the step (1), the fixing material for fixing the start and stop ends of the fiber bundle is a common adhesive tape or a high temperature adhesive tape.
In a preferred embodiment of the present invention, in the step (2), the epoxy resin is any one of or a combination of bisphenol a type epoxy resin or bisphenol F type epoxy resin, preferably bisphenol F type epoxy resin, and has a trade mark of 830S, NPEF170, and the like.
Further, the viscosity of the epoxy resin is less than or equal to 4000 mPa.S at room temperature.
And (3) through the heat preservation treatment in the step (2), the fluidity of the resin is ensured, and the fiber is fully soaked.
In a preferred embodiment of the present invention, in the step (3), the curing agent is selected from amine-based curing agents or acid anhydride-based curing agents which are liquid at room temperature, and preferably triethylene tetramine.
In a preferred embodiment of the present invention, in step (4), the container for holding the glue solution includes, but is not limited to, a quadrilateral container, and the material of the quadrilateral container may be glass, metal or plastic, so as to meet the requirement of being able to lay flat the frame for winding the fiber bundle.
In a preferred embodiment of the present invention, in step (6), the material of the tool holder includes, but is not limited to, stainless steel. Preferably, the structure of the tool holder is as shown in fig. 5, and the tool holder includes: the clamping groove strip 2 fixed on the support frame 1 in the hexahedron skeleton form, the clamping groove strip 2 fixed on the support frame 1 in the height direction, the clamping wire 3 at the bottom of the support frame 1 and the frame 4 wound with fiber bundle wires, wherein the clamping groove strips 2 are fixed on the support frame 1 in pairs, a groove used for clamping and fixing the frame 4 is processed on the inner side, and the clamping wire 3 is located below the frame 4 and used for supporting the frame 4 to avoid the frame from touching the bottom.
In a preferred embodiment of the present invention, in the step (7), the thickness of the reinforcing sheet is 0.4 to 1.2 mm.
Examples
Example 1
Domestic 0.5K silicon carbide fiber bundle wires are continuously wound on a stainless steel frame, the size of the stainless steel frame is 480mm multiplied by 300mm, and the interval between the fiber bundles is kept to be 15 mm. And applying certain tension to the fiber bundle wires in the winding process to ensure that the silicon carbide fiber bundle wires to be tested are tight, fixing the two ends of the fiber winding by using a medical adhesive tape, and placing the stainless steel frame on the tool support. 800g of 830S epoxy resin is poured into a beaker, and the beaker and a frame wound with the strand are put into an oven and are kept at 40 ℃ for 1 hour. And weighing 50g of triethylene tetramine, adding the triethylene tetramine into the resin after heat preservation, and quickly and uniformly stirring. Transferring the mixed glue solution into a rectangular metal container, putting the frame after heat preservation into the container, timing after the glue solution submerges the frame, standing for 10 minutes, taking out the impregnated frame, keeping the frame vertically placed along the fiber extension direction, and wiping off redundant glue beads by newspaper after the glue solution runs out. And placing the frame on a tool support to ensure that the tested working section of the fiber bundle is not contacted with other hard objects, and placing the tool support in an oven for curing, wherein the curing system is to heat the fiber bundle to 130 ℃ from room temperature at 8 ℃/min and keep the temperature at 130 ℃ for 40 minutes. After the solidified silicon carbide fiber bundle is cooled to room temperature, 300mm of the silicon carbide fiber bundle between the winding ends is cut, 10 samples are obtained, paper reinforcing sheets are adhered to the two ends of the fiber by 50mm AB glue, mechanical property tests are carried out after firm adhesion, the results are shown in table 1, and the microstructure diagrams of the stretching fracture of the bundle are respectively shown in fig. 1 and fig. 3. Of these, comparative example 1 is identical to example 1, differing only in that: the sample was prepared by using an organic solvent-containing aqueous solution, and 800g of 6101 epoxy resin was added with 200g of acetone solvent in addition to 50g of triethylenetetramine.
Example 2
The domestic 1K silicon carbide fiber bundle is continuously wound on a graphite frame, the size of the graphite frame is 180mm multiplied by 300mm, and the interval between the fiber bundles is kept to be 10 mm. And applying certain tension to the fiber bundle wires in the winding process to ensure that the silicon carbide fiber bundle wires to be tested are tight, fixing the two ends of the fiber winding by using a medical adhesive tape, and placing the graphite frame on a tool support. 500g of 830S epoxy resin was poured into a beaker, and the beaker and the frame with the bundled yarn wound thereon were placed in an oven and kept at 40 ℃ for 40 minutes. And weighing 40g of triethylene tetramine, adding the triethylene tetramine into the resin after heat preservation, and quickly and uniformly stirring. Transferring the mixed glue solution into a rectangular plastic container, putting the frame after heat preservation into the container, timing after the glue solution submerges the frame, standing for 5 minutes, taking out the impregnated frame, keeping the frame vertically placed along the fiber extension direction, and wiping off redundant glue beads by newspaper after the glue solution runs out. And placing the frame on a special tool support to ensure that the tested working section of the fiber bundle is not contacted with other hard objects, and placing the tool support in an oven for curing, wherein the curing system is to heat the fiber bundle to 120 ℃ from room temperature at 8 ℃/min, and the temperature of 120 ℃ is kept for 20 minutes. After the solidified silicon carbide fiber bundle is cooled to room temperature, 300mm of the silicon carbide fiber bundle between the winding ends is cut, 10 samples are obtained, paper reinforcing sheets are adhered to the two ends of the fiber by 50mm AB glue, mechanical property tests are carried out after the two ends are firmly adhered, the results are shown in table 1, and the microstructure diagrams of the stretching fracture of the bundle are respectively shown in fig. 2 and 4. Of these, comparative example 2 is identical to example 2, differing only in that: the sample was prepared by using an organic solvent-containing glue solution, and 125g of an acetone solvent was added to 500g of 6101 epoxy resin in addition to 40g of triethylenetetramine.
TABLE 1 comparison table of tensile property results of bundle filaments tested by using solvent-free glue solution
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (8)
1. A method for preparing a silicon carbide fiber bundle mechanical sample by using solvent-free glue solution is characterized by comprising the following steps:
continuously winding a silicon carbide fiber bundle wire to be tested on a frame, applying tension to the fiber bundle wire to tighten the silicon carbide fiber bundle wire to be tested, and fixing the two ends of the start and stop of the fiber bundle wire by using a fixing material;
pouring epoxy resin into a container, putting the frame wound with the fiber bundle yarns in the step (1) into an oven, and keeping the temperature at 30-40 ℃ for 0.5-2 hours;
step (3), weighing a curing agent, adding the curing agent into the epoxy resin subjected to heat preservation in the step (2), mixing to obtain a glue solution, and quickly and uniformly stirring;
step (4), transferring the glue solution in the step (3) into a container, and putting the frame subjected to heat preservation in the step (2) into the container for impregnation;
step (5), taking out the impregnated frame in the step (4), keeping the frame vertically placed along the fiber extension direction, and wiping off the glue beads by using paper, non-woven fabric or fabric with adsorption capacity after the glue solution runs out;
step (6), placing the frame in the step (5) on a tool support to ensure that the tested working section of the fiber bundle is not contacted with other objects, and placing the tool support in drying equipment for curing;
and (7) after the silicon carbide fiber bundle wires solidified in the step (6) are cooled to room temperature, intercepting the silicon carbide fiber bundle wires between the winding ends, pasting reinforcing sheets at the two ends, and carrying out mechanical property test.
2. The method according to claim 1, wherein in the step (1), the frame for winding the fiber bundle wire is a quadrilateral tool made of metal, graphite or ceramic, and two opposite sides of the frame for winding the fiber bundle wire are parallel, and the part contacted with the fiber bundle wire is not allowed to have an edge.
3. The method according to claim 1, wherein in the step (2), the epoxy resin is any one of or a combination of bisphenol A type epoxy resin and bisphenol F type epoxy resin, preferably bisphenol F type epoxy resin.
4. The method according to claim 3, wherein the epoxy resin has a viscosity of 4000 mPa-S or less at 25 ℃.
5. The method according to claim 1, wherein in the step (3), when the curing agent is weighed, the curing agent is weighed according to a ratio of 10-18 parts of the epoxy resin to 1 part of the curing agent.
6. The method according to claim 1, wherein the step (4) comprises immersing the substrate at room temperature and pressure for 5 to 20 minutes.
7. The method according to claim 1, wherein in the step (6), the curing temperature is 100 to 150 ℃ and the curing time is 0.5 to 1 hour.
8. The method according to claim 1, wherein in the step (7), the thickness of the reinforcing sheet is 0.4 to 1.2 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011126057.8A CN112444445A (en) | 2020-10-20 | 2020-10-20 | Method for preparing silicon carbide fiber bundle mechanical sample by using solvent-free glue solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011126057.8A CN112444445A (en) | 2020-10-20 | 2020-10-20 | Method for preparing silicon carbide fiber bundle mechanical sample by using solvent-free glue solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112444445A true CN112444445A (en) | 2021-03-05 |
Family
ID=74735584
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011126057.8A Pending CN112444445A (en) | 2020-10-20 | 2020-10-20 | Method for preparing silicon carbide fiber bundle mechanical sample by using solvent-free glue solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112444445A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977557A (en) * | 2012-12-11 | 2013-03-20 | 蓝星(北京)化工机械有限公司 | Room temperature curing epoxy resin composition and preparation method thereof |
| CN103981715A (en) * | 2014-05-28 | 2014-08-13 | 航天材料及工艺研究所 | No-solvent type glue solution for testing tensile property of carbon fiber multifilament and application method of no-solvent type glue solution |
| CN104448242A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Epoxy resin composition |
| JP2016204540A (en) * | 2015-04-24 | 2016-12-08 | 三菱レイヨン株式会社 | Tow prepreg and composite material reinforcement pressure container |
| CN108318302A (en) * | 2018-01-18 | 2018-07-24 | 航天材料及工艺研究所 | A kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament |
-
2020
- 2020-10-20 CN CN202011126057.8A patent/CN112444445A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977557A (en) * | 2012-12-11 | 2013-03-20 | 蓝星(北京)化工机械有限公司 | Room temperature curing epoxy resin composition and preparation method thereof |
| CN104448242A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Epoxy resin composition |
| CN103981715A (en) * | 2014-05-28 | 2014-08-13 | 航天材料及工艺研究所 | No-solvent type glue solution for testing tensile property of carbon fiber multifilament and application method of no-solvent type glue solution |
| JP2016204540A (en) * | 2015-04-24 | 2016-12-08 | 三菱レイヨン株式会社 | Tow prepreg and composite material reinforcement pressure container |
| CN108318302A (en) * | 2018-01-18 | 2018-07-24 | 航天材料及工艺研究所 | A kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament |
Non-Patent Citations (2)
| Title |
|---|
| 王军 等: "《连续碳化硅纤维测试方法 第4部分：束丝拉伸性能》", 《中华人民共和国国家标准 GB/T 34520.4-2017》, 1 November 2017 (2017-11-01) * |
| 王玲 等: "《碳纤维复丝拉伸性能试验方法》", 《中华人民共和国国家标准 GB/T 3362-2017》, 14 October 2017 (2017-10-14), pages 2 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108469366B (en) | Large-tow carbon fiber multifilament tensile property test sample and sample preparation method thereof | |
| CN108318302B (en) | Sample preparation method for tensile property test of asphalt-based carbon fiber multifilament | |
| CN112730064B (en) | Method for testing tensile breaking strength of carbon fiber fabric | |
| CN108303296B (en) | Sample preparation method for tensile property test of high-model carbon fiber multifilament | |
| CN100500984C (en) | Temperature tolerance type carbon fibre emulsion sizing agent and its preparation process and application | |
| CN102809499B (en) | Sample preparation method for carbon fiber tensile property test | |
| US10023979B2 (en) | Bundle of carbon fibers and method of manufacturing the same | |
| CN109596464B (en) | Method for testing interface performance of carbon nanotube surface modified fiber | |
| CN109406234B (en) | Large-tow carbon fiber multifilament tensile sample and preparation device and method thereof | |
| CN108660764B (en) | Modification processing method of F-12 aramid fiber fabric of conveyor belt framework material | |
| CN105352773A (en) | Method for testing breaking strength of glass fiber product | |
| CN107541018B (en) | Impregnating resin for reinforcing aramid fiber honeycomb composite material and application thereof | |
| CN103645082B (en) | For gumming device and the dipping method of the test of carbon fiber tensile property of multi-filament | |
| CN112444445A (en) | Method for preparing silicon carbide fiber bundle mechanical sample by using solvent-free glue solution | |
| CN205374133U (en) | A carbon fiber multifilament for tensile test | |
| JP2011207930A (en) | Prepreg and method for producing the same, and fiber-reinforced resin molding | |
| CN111562175A (en) | Method for testing strength of ceramic fiber after high-temperature treatment | |
| CN115322717A (en) | Fiber-reinforced resin-based adhesive capable of being used for underwater construction and repairing underwater vehicle shell, and preparation method and construction method thereof | |
| CN111678788B (en) | Mechanical property testing method of high-strength high-modulus carbon fiber filament | |
| CN109323904B (en) | Sample preparation method and device for testing retention rate of high-temperature strength of fiber bundle filaments | |
| CN206177789U (en) | A testing arrangement that is used for gluing agent and material cohesion | |
| CN203688322U (en) | Gum dipping device for tensile property test of carbon fiber multifilament | |
| Chiao et al. | A tensile test method for fibers | |
| CN113740135A (en) | Carbon fiber multifilament sample strip reinforcing method and device | |
| JP2004244258A (en) | Carbon fiber for carbon fiber reinforced carbon composite materials and method of manufacturing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210305 |