CN105567162A - Preparation method of yttrium aluminum garnet nano fiber/phenolic resin composite friction material - Google Patents
Preparation method of yttrium aluminum garnet nano fiber/phenolic resin composite friction material Download PDFInfo
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- CN105567162A CN105567162A CN201510948276.7A CN201510948276A CN105567162A CN 105567162 A CN105567162 A CN 105567162A CN 201510948276 A CN201510948276 A CN 201510948276A CN 105567162 A CN105567162 A CN 105567162A
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- aluminum garnet
- yttrium aluminum
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
Abstract
The invention relates to a preparation method of an yttrium aluminum garnet nano fiber/phenolic resin composite friction material, belonging to the field of preparation of friction materials. In order to solve the problem that the phenomenon of heat fading, which is generated by the reduction of friction force since the organic constituents in the existing polymer-base friction material are thermally decomposed under high-temperature conditions under which friction braking can be generated, can severely influence the safety and reliability of braking, a nano electrostatic spinning material is utilized to prepare yttrium aluminum garnet nano fibers, and the yttrium aluminum garnet nano fibers are subjected to surface modification and closely combined with the phenolic resin, thereby preparing the yttrium aluminum garnet nano fiber/phenolic resin composite friction material, The yttrium aluminum garnet nano fiber/phenolic resin composite friction material can protect the polymers from decomposition and fading in the friction process. The yttrium aluminum garnet nano fibers are utilized to modify the friction material, so that the friction factor of the modified friction material at 200 DEG C is 0.5, and the wear rate is 0.2-0.3%. The phenolic resin and yttrium aluminum garnet nano fibers are used for the preparation, so the method is environment-friendly and pollution-free.
Description
Technical field
The present invention relates to the preparation method of a kind of yttrium aluminum garnet nano fiber/resol composite friction material, belong to friction materials preparation field.
Background technology
Friction materials is that one is applied on power machine, rubbing effect is relied on to perform the component materials of braking and transmission agency, it is commonly called as brake facing mainly for the manufacture of brake facing and clutch surface is commonly called as clutch disc, and brake facing is used for braking, and clutch coupling is used for transmission.The various vehicles of any mechanical means and motion, all must have drift stop.Friction materials is the key part on this drift stop.It enables mechanical means and the safe and reliable work of various Motor vehicles, is widely used so friction materials is one, material very crucial again.Braking is one of important behavior of vehicle operating, and current great majority take friction catch, and the frictional force namely produced by relative movement between friction plate and brake flange, as damping force, makes mobile safety braking.Therefore breaking system is to the security of vehicle, comfortableness, and energy consumption and pollution etc. have significant impact, and the performance and structure of the friction pair wherein in breaking system is the basic influence factor of riding comfort, weather resistance particularly security.
Current friction materials also exists the heat fading of high temperature friction performance.Thermolysis will be there is under the hot conditions that organic constituent in polymer-based carbon friction materials produces in friction catch, frictional force is caused to reduce, produce heat fading phenomenon, have a strong impact on brake safe and reliable problem, so, need a kind of attrition resistant inorganic material, make it not decompose under friction high temperature, necessary.
Summary of the invention
Technical problem to be solved by this invention: thermolysis will occur under there is for current friction materials the hot conditions that organic constituent in polymer-based carbon friction materials produces in friction catch, frictional force is caused to reduce, produce heat fading phenomenon, have a strong impact on brake safe and reliable problem, provide one and prepare yttrium aluminum garnet nano fiber by nano electrostatic spinning material, subsequently to its surface modification, combine closely with resol, prepare a kind of yttrium aluminum garnet nano fiber/resol composite friction material, can when friction, protection polymkeric substance does not occur to decompose and decline.
For solving the problems of the technologies described above, the present invention adopts technical scheme as described below to be:
(1) by solid-liquid mass ratio 1:5, by Y
2o
3being added into massfraction is in the concentrated nitric acid solution of 65%, is uniformly mixed and is heated to 60 ~ 65 DEG C to its intensification, after 25 ~ 30min to be heated, by Y
3+and Al
3+mol ratio is 3:5, by Al(NO
3)
39H
2o is added in above-mentioned solution, continues insulation reaction 2 ~ 3h, is prepared into intermediate liquid;
(2) after insulation reaction completes, count by weight, choose the polyvinylpyrrolidone of the intermediate liquid of the above-mentioned preparation of 35 ~ 65 parts, the deionized water of 25 ~ 30 parts and 10 ~ 35 parts, under 600 ~ 800r/min, magnetic agitation 3 ~ 5h, stop heating subsequently and encapsulation process, make its standing and defoaming 6 ~ 8h, be prepared into precursor solution;
(3) after deaeration completes, the precursor solution of above-mentioned preparation is injected the syringe that nozzle is housed, jet hole diameter is 1mm, adjustment nozzle and horizontal plane angle are 10 ~ 15 °, arranging voltage is 20kV, and solidification distance is 13 ~ 15cm, at 18 ~ 20 DEG C, carry out spinning when relative humidity is 50% ~ 60%, collect and be prepared into dispersion of nanofibers;
(4) calcined in retort furnace by the dispersion of nanofibers of above-mentioned preparation, controlling calcining temperature is 600 DEG C, and temperature rise rate is 2 DEG C/min, treats that muffle furnace reaches 900 DEG C, insulation calcining 1 ~ 2h, stops heating making its naturally cooling be prepared into Y subsequently
3al
5o
12nanofiber, presses solid-liquid mass ratio 1:5, subsequently by Y
3al
5o
12nanofiber and γ-aminopropyl triethoxysilane are uniformly mixed and are prepared into nanometer slurries, are placed on dry 6 ~ 8h in 60 ~ 80 DEG C of baking ovens subsequently, are prepared into coupling modifier yttrium aluminum garnet nano fiber;
(5) 1:10 in molar ratio, tung oil and phenolic aldehyde are uniformly mixed, and heating makes its back flow reaction 1 ~ 2h at being placed in 100 ~ 110 DEG C, be prepared into prepolymer, press solid-liquid mass ratio 1:10 subsequently, the coupling modifier yttrium aluminum garnet nano fiber of above-mentioned preparation and performed polymer are uniformly mixed, and are placed in 200 ~ 300W sonic oscillation process, 40 ~ 50min, make it fully disperse and with its combination;
(6) after dispersion completes, frozen water is cooled to 60 DEG C, under 200 ~ 300r/min speed, slowly adding with phenol mol ratio in performed polymer is paraformaldehyde and the epoxy soybean oil of 3:2, to be added complete after, continue to be heated to 100 ~ 110 DEG C, it is made to be incubated back flow reaction 2 ~ 3h, subsequently imurity-removal is vacuumized to it, and continue to be warming up to 120 ~ 125 DEG C of reaction 2 ~ 3h, leave standstill and be cooled to 20 ~ 30 DEG C, a kind of yttrium aluminum garnet nano fiber/resol composite friction material can be prepared into.
Application method of the present invention is: the yttrium aluminum garnet nano of above-mentioned preparation fiber/resol composite friction material is placed in injection moulding machine, injection moulding is carried out at 160 ~ 165 DEG C, take out from cast iron die subsequently, can clutch friction material be prepared into, subsequently it be assembled.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the present invention passes through yttrium aluminum garnet nano fibre modification friction materials, and the frictional coefficient at 200 DEG C is 0.5, and wear rate is 0.2 ~ 0.3%;
(2) be prepared by resol and yttrium aluminum garnet nano fiber, cost is low, easy to operate.
Embodiment
First by solid-liquid mass ratio 1:5, by Y
2o
3being added into massfraction is in the concentrated nitric acid solution of 65%, is uniformly mixed and is heated to 60 ~ 65 DEG C to its intensification, after 25 ~ 30min to be heated, by Y
3+and Al
3+mol ratio is 3:5, by Al(NO
3)
39H
2o is added in above-mentioned solution, continues insulation reaction 2 ~ 3h, is prepared into intermediate liquid; After insulation reaction completes, count by weight, choose the polyvinylpyrrolidone of the intermediate liquid of the above-mentioned preparation of 35 ~ 65 parts, the deionized water of 25 ~ 30 parts and 10 ~ 35 parts, under 600 ~ 800r/min, magnetic agitation 3 ~ 5h, stop heating subsequently and encapsulation process, make its standing and defoaming 6 ~ 8h, be prepared into precursor solution; After deaeration completes, the precursor solution of above-mentioned preparation is injected the syringe that nozzle is housed, jet hole diameter is 1mm, adjustment nozzle and horizontal plane angle are 10 ~ 15 °, arranging voltage is 20kV, and solidification distance is 13 ~ 15cm, at 18 ~ 20 DEG C, carry out spinning when relative humidity is 50% ~ 60%, collect and be prepared into dispersion of nanofibers; Calcined in retort furnace by the dispersion of nanofibers of above-mentioned preparation, controlling calcining temperature is 600 DEG C, and temperature rise rate is 2 DEG C/min, treats that muffle furnace reaches 900 DEG C, insulation calcining 1 ~ 2h, stops heating making its naturally cooling be prepared into Y subsequently
3al
5o
12nanofiber, presses solid-liquid mass ratio 1:5, subsequently by Y
3al
5o
12nanofiber and γ-aminopropyl triethoxysilane are uniformly mixed and are prepared into nanometer slurries, are placed on dry 6 ~ 8h in 60 ~ 80 DEG C of baking ovens subsequently, are prepared into coupling modifier yttrium aluminum garnet nano fiber; 1:10 in molar ratio, tung oil and phenolic aldehyde are uniformly mixed, and heating makes its back flow reaction 1 ~ 2h at being placed in 100 ~ 110 DEG C, be prepared into prepolymer, press solid-liquid mass ratio 1:10 subsequently, the coupling modifier yttrium aluminum garnet nano fiber of above-mentioned preparation and performed polymer are uniformly mixed, and are placed in 200 ~ 300W sonic oscillation process, 40 ~ 50min, make it fully disperse and with its combination; After dispersion completes, frozen water is cooled to 60 DEG C, under 200 ~ 300r/min speed, slowly adding with phenol mol ratio in performed polymer is paraformaldehyde and the epoxy soybean oil of 3:2, to be added complete after, continue to be heated to 100 ~ 110 DEG C, make it be incubated back flow reaction 2 ~ 3h, subsequently imurity-removal is vacuumized to it, and continue to be warming up to 120 ~ 125 DEG C of reaction 2 ~ 3h, leave standstill and be cooled to 20 ~ 30 DEG C, a kind of yttrium aluminum garnet nano fiber/resol composite friction material can be prepared into.
Example 1
First by solid-liquid mass ratio 1:5, by Y
2o
3being added into massfraction is in the concentrated nitric acid solution of 65%, is uniformly mixed and is heated to 60 DEG C to its intensification, after 25min to be heated, by Y
3+and Al
3+mol ratio is 3:5, by Al(NO
3)
39H
2o is added in above-mentioned solution, continues insulation reaction 2h, is prepared into intermediate liquid; After insulation reaction completes, count by weight, choose the polyvinylpyrrolidone of the intermediate liquid of the above-mentioned preparation of 35 parts, the deionized water of 30 parts and 35 parts, under 600r/min, magnetic agitation 3h, stops heating and encapsulation process subsequently, make its standing and defoaming 6h, be prepared into precursor solution; After deaeration completes, the precursor solution of above-mentioned preparation is injected the syringe that nozzle is housed, jet hole diameter is 1mm, adjustment nozzle and horizontal plane angle are 10 °, arranging voltage is 20kV, and solidification distance is 13cm, at 18 DEG C, carry out spinning when relative humidity is 50%, collect and be prepared into dispersion of nanofibers; Calcined in retort furnace by the dispersion of nanofibers of above-mentioned preparation, controlling calcining temperature is 600 DEG C, and temperature rise rate is 2 DEG C/min, treats that muffle furnace reaches 900 DEG C, insulation calcining 1h, stops heating making its naturally cooling be prepared into Y subsequently
3al
5o
12nanofiber, presses solid-liquid mass ratio 1:5, subsequently by Y
3al
5o
12nanofiber and γ-aminopropyl triethoxysilane are uniformly mixed and are prepared into nanometer slurries, are placed on dry 6h in 60 DEG C of baking ovens subsequently, are prepared into coupling modifier yttrium aluminum garnet nano fiber; 1:10 in molar ratio, tung oil and phenolic aldehyde are uniformly mixed, and heating makes its back flow reaction 1h at being placed in 100 DEG C, be prepared into prepolymer, press solid-liquid mass ratio 1:10 subsequently, the coupling modifier yttrium aluminum garnet nano fiber of above-mentioned preparation and performed polymer are uniformly mixed, and are placed in 200 ~ 300W sonic oscillation process 40min, make it fully disperse and with its combination; After dispersion completes, frozen water is cooled to 60 DEG C, under 200r/min speed, slowly adding with phenol mol ratio in performed polymer is paraformaldehyde and the epoxy soybean oil of 3:2, to be added complete after, continue to be heated to 100 DEG C, make it be incubated back flow reaction 2h, subsequently imurity-removal is vacuumized to it, and continue to be warming up to 120 DEG C of reaction 2h, leave standstill and be cooled to 20 DEG C, a kind of yttrium aluminum garnet nano fiber/resol composite friction material can be prepared into.
The yttrium aluminum garnet nano of above-mentioned preparation fiber/resol composite friction material is placed in injection moulding machine, at 160 DEG C, carries out injection moulding, take out from cast iron die subsequently, can clutch friction material be prepared into, subsequently it be assembled.
Example 2
First by solid-liquid mass ratio 1:5, by Y
2o
3being added into massfraction is in the concentrated nitric acid solution of 65%, is uniformly mixed and is heated to 62 DEG C to its intensification, after 27min to be heated, by Y
3+and Al
3+mol ratio is 3:5, by Al(NO
3)
39H
2o is added in above-mentioned solution, continues insulation reaction 2.5h, is prepared into intermediate liquid; After insulation reaction completes, count by weight, choose the polyvinylpyrrolidone of the intermediate liquid of the above-mentioned preparation of 40 parts, the deionized water of 25 parts and 35 parts, under 700r/min, magnetic agitation 4h, stops heating and encapsulation process subsequently, make its standing and defoaming 7h, be prepared into precursor solution; After deaeration completes, the precursor solution of above-mentioned preparation is injected the syringe that nozzle is housed, jet hole diameter is 1mm, adjustment nozzle and horizontal plane angle are 12 °, arranging voltage is 20kV, and solidification distance is 14cm, at 19 DEG C, carry out spinning when relative humidity is 55%, collect and be prepared into dispersion of nanofibers; Calcined in retort furnace by the dispersion of nanofibers of above-mentioned preparation, controlling calcining temperature is 600 DEG C, and temperature rise rate is 2 DEG C/min, treats that muffle furnace reaches 900 DEG C, insulation calcining 1.5h, stops heating making its naturally cooling be prepared into Y subsequently
3al
5o
12nanofiber, presses solid-liquid mass ratio 1:5, subsequently by Y
3al
5o12 nanofiber and γ-aminopropyl triethoxysilane are uniformly mixed and are prepared into nanometer slurries, are placed on dry 7h in 70 DEG C of baking ovens subsequently, are prepared into coupling modifier yttrium aluminum garnet nano fiber; 1:10 in molar ratio, tung oil and phenolic aldehyde are uniformly mixed, and heating makes its back flow reaction 1.5h at being placed in 105 DEG C, be prepared into prepolymer, press solid-liquid mass ratio 1:10 subsequently, the coupling modifier yttrium aluminum garnet nano fiber of above-mentioned preparation and performed polymer are uniformly mixed, and are placed in 250W sonic oscillation process 45min, make it fully disperse and with its combination; After dispersion completes, frozen water is cooled to 60 DEG C, under 250r/min speed, slowly adding with phenol mol ratio in performed polymer is paraformaldehyde and the epoxy soybean oil of 3:2, to be added complete after, continue to be heated to 105 DEG C, make it be incubated back flow reaction 2.5h, subsequently imurity-removal is vacuumized to it, and continue to be warming up to 122 DEG C of reaction 2.5h, leave standstill and be cooled to 25 DEG C, a kind of yttrium aluminum garnet nano fiber/resol composite friction material can be prepared into.
The yttrium aluminum garnet nano of above-mentioned preparation fiber/resol composite friction material is placed in injection moulding machine, at 162 DEG C, carries out injection moulding, take out from cast iron die subsequently, can clutch friction material be prepared into, subsequently it be assembled.
Example 3
First by solid-liquid mass ratio 1:5, by Y
2o
3being added into massfraction is in the concentrated nitric acid solution of 65%, is uniformly mixed and is heated to 65 DEG C to its intensification, after 30min to be heated, by Y
3+and Al
3+mol ratio is 3:5, by Al(NO
3)
39H
2o is added in above-mentioned solution, continues insulation reaction 3h, is prepared into intermediate liquid; After insulation reaction completes, count by weight, choose the polyvinylpyrrolidone of the intermediate liquid of the above-mentioned preparation of 65 parts, the deionized water of 25 parts and 10 parts, under 800r/min, magnetic agitation 5h, stops heating and encapsulation process subsequently, make its standing and defoaming 8h, be prepared into precursor solution; After deaeration completes, the precursor solution of above-mentioned preparation is injected the syringe that nozzle is housed, jet hole diameter is 1mm, adjustment nozzle and horizontal plane angle are 15 °, arranging voltage is 20kV, and solidification distance is 15cm, at 20 DEG C, carry out spinning when relative humidity is 60%, collect and be prepared into dispersion of nanofibers; Calcined in retort furnace by the dispersion of nanofibers of above-mentioned preparation, controlling calcining temperature is 600 DEG C, and temperature rise rate is 2 DEG C/min, treats that muffle furnace reaches 900 DEG C, insulation calcining 2h, stops heating making its naturally cooling be prepared into Y subsequently
3al
5o
12nanofiber, presses solid-liquid mass ratio 1:5, subsequently by Y
3al
5o
12nanofiber and γ-aminopropyl triethoxysilane are uniformly mixed and are prepared into nanometer slurries, are placed on dry 8h in 80 DEG C of baking ovens subsequently, are prepared into coupling modifier yttrium aluminum garnet nano fiber; 1:10 in molar ratio, tung oil and phenolic aldehyde are uniformly mixed, and heating makes its back flow reaction 2h at being placed in 110 DEG C, be prepared into prepolymer, press solid-liquid mass ratio 1:10 subsequently, the coupling modifier yttrium aluminum garnet nano fiber of above-mentioned preparation and performed polymer are uniformly mixed, and are placed in 300W sonic oscillation process 50min, make it fully disperse and with its combination; After dispersion completes, frozen water is cooled to 60 DEG C, under 300r/min speed, slowly adding with phenol mol ratio in performed polymer is paraformaldehyde and the epoxy soybean oil of 3:2, to be added complete after, continue to be heated to 110 DEG C, make it be incubated back flow reaction 3h, subsequently imurity-removal is vacuumized to it, and continue to be warming up to 125 DEG C of reaction 3h, leave standstill and be cooled to 30 DEG C, a kind of yttrium aluminum garnet nano fiber/resol composite friction material can be prepared into.
The yttrium aluminum garnet nano of above-mentioned preparation fiber/resol composite friction material is placed in injection moulding machine, at 165 DEG C, carries out injection moulding, take out from cast iron die subsequently, can clutch friction material be prepared into, subsequently it be assembled.
Claims (1)
1. a preparation method for yttrium aluminum garnet nano fiber/resol composite friction material, is characterized in that concrete preparation process is:
(1) by solid-liquid mass ratio 1:5, by Y
2o
3being added into massfraction is in the concentrated nitric acid solution of 65%, is uniformly mixed and is heated to 60 ~ 65 DEG C, after 25 ~ 30min to be heated, by Y to its intensification
3+and Al
3+mol ratio is 3:5, by Al(NO
3)
39H
2o is added in above-mentioned solution, continues insulation reaction 2 ~ 3h, is prepared into intermediate liquid;
(2) after insulation reaction completes, count by weight, choose the polyvinylpyrrolidone of the intermediate liquid of the above-mentioned preparation of 35 ~ 65 parts, the deionized water of 25 ~ 30 parts and 10 ~ 35 parts, under 600 ~ 800r/min, magnetic agitation 3 ~ 5h, stop heating subsequently and encapsulation process, make its standing and defoaming 6 ~ 8h, be prepared into precursor solution;
(3) after deaeration completes, the precursor solution of above-mentioned preparation is injected the syringe that nozzle is housed, jet hole diameter is 1mm, adjustment nozzle and horizontal plane angle are 10 ~ 15 °, arranging voltage is 20kV, and solidification distance is 13 ~ 15cm, at 18 ~ 20 DEG C, carry out spinning when relative humidity is 50% ~ 60%, collect and be prepared into dispersion of nanofibers;
(4) calcined in retort furnace by the dispersion of nanofibers of above-mentioned preparation, controlling calcining temperature is 600 DEG C, and temperature rise rate is 2 DEG C/min, treats that muffle furnace reaches 900 DEG C, insulation calcining 1 ~ 2h, stops heating making its naturally cooling be prepared into Y subsequently
3al
5o
12nanofiber, presses solid-liquid mass ratio 1:5, subsequently by Y
3al
5o
12nanofiber and γ-aminopropyl triethoxysilane are uniformly mixed and are prepared into nanometer slurries, are placed on dry 6 ~ 8h in 60 ~ 80 DEG C of baking ovens subsequently, are prepared into coupling modifier yttrium aluminum garnet nano fiber;
(5) 1:10 in molar ratio, tung oil and phenolic aldehyde are uniformly mixed, and heating makes its back flow reaction 1 ~ 2h at being placed in 100 ~ 110 DEG C, be prepared into prepolymer, press solid-liquid mass ratio 1:10 subsequently, the coupling modifier yttrium aluminum garnet nano fiber of above-mentioned preparation and performed polymer are uniformly mixed, and are placed in 200 ~ 300W sonic oscillation process, 40 ~ 50min, make it fully disperse and with its combination;
(6) after dispersion completes, frozen water is cooled to 60 DEG C, under 200 ~ 300r/min speed, slowly adding with phenol mol ratio in performed polymer is paraformaldehyde and the epoxy soybean oil of 3:2, to be added complete after, continue to be heated to 100 ~ 110 DEG C, it is made to be incubated back flow reaction 2 ~ 3h, subsequently imurity-removal is vacuumized to it, and continue to be warming up to 120 ~ 125 DEG C of reaction 2 ~ 3h, leave standstill and be cooled to 20 ~ 30 DEG C, a kind of yttrium aluminum garnet nano fiber/resol composite friction material can be prepared into.
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| CN102850561A (en) * | 2012-10-09 | 2013-01-02 | 桂林理工大学 | Preparation method of mesoporous molecular sieve in-situ reinforcing phenolic resin based friction material |
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2015
- 2015-12-17 CN CN201510948276.7A patent/CN105567162A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148330A (en) * | 2007-09-06 | 2008-03-26 | 贵州大学 | Modified method for fibriform paligorskite and its product and application |
| CN101235557A (en) * | 2008-03-12 | 2008-08-06 | 长春理工大学 | Method for preparing rare earth garnet type compound nano fiber |
| CN102850561A (en) * | 2012-10-09 | 2013-01-02 | 桂林理工大学 | Preparation method of mesoporous molecular sieve in-situ reinforcing phenolic resin based friction material |
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Application publication date: 20160511 |
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