CN103321093A - Preparation method of zirconium boride modified paper base friction material - Google Patents
Preparation method of zirconium boride modified paper base friction material Download PDFInfo
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Abstract
A preparation method of a zirconium boride modified paper base friction material comprises the following steps: dissolving cashew hull modified phenolic resin in absolute ethyl alcohol to obtain a solution A; dispersing multiwalled carbon nanotube in a sodium dodecanesulphonate aqueous solution to obtain a fluid suspension B; dispersing zirconium boride in PMAA to obtain a zirconium diboride dissolving pulp C with good dispersion stability; dispersing short carbon fiber, bamboo fiber and diatomite in water and adding the fluid suspension B and the dissolving pulp to obtain a solution D; pouring the solution D into a fluffer for dispersion, making sheets by a sheet-making machine and drying to obtain a sample wafer E; and uniformly smearing the solution A on the sample wafer E and naturally airing, and carrying out hot briquetting by a vulcanizer so as to obtain the zirconium boride modified paper base friction material with stable friction performance. According to the invention, zirconium boride is used as a raw material to be added in a carbon fiber reinforced resin matrix wet-type friction material, and a single-layer paper base friction material is prepared to endow zirconium boride (ZrB2) with good electroconductibility and thermal conductivity, corrosion resistance, resistance to heat shocks, oxidation resistance at high temperature and wear resistance.
Description
Technical field
The present invention relates to a kind of preparation method of modified paper base frication material, particularly a kind of preparation method of zirconium boride modified paper base frication material.
Background technology
Wet-type friction material refers to work in the friction material in the lubricant medium (mainly being lubricating oil), be mainly used in [P.Marklund in the wet type transmission systems such as automatic transmission, differential mechanism, torque management device and synchronized, R.Larsson.Tribology International, 2008,41:824 – 830.].Because service condition is different, the speed of transmission system, pressure and load difference are very large, single certain material is difficult to satisfy all operating mode instructions for uses, thereby develop multiple Wet-type friction material, mainly comprise cork-rubber base frication material, powder metallurgy friction material, paper friction material and carbon/carbon compound material etc.
Paper friction material mainly is comprised of fiber, binding agent, filler, frictional property regulator etc., usually adopt the mode of papermaking to manufacture, [appoint just Deng Haijin so be called " paper substrate " friction material, Li Ming. automotive engineering, 2004 (11): 1-4.].Owing to it has that coefficient of friction is high, stable friction performance, static and dynamic friction coefficient are widely used in the wet clutch and brake of all kinds of heavy vehicles and engineering machinery than many premium properties such as adjustable, that abrasion resistance properties is good, energy absorption capability is high, particularly as the friction plate material of wet clutch in the automatic gearbox.Along with vehicle to future developments such as high speed, heavy load, light pollutions, development to paper base material is also had higher requirement, researchers have made some effort and effect [Kim S J at paper base material the Nomenclature Composition and Structure of Complexes design aspect, Cho M H, Lim D S, et al.Wear, 2001, (251): 1484～1491].Particularly the in recent years fast development of material with carbon element is so that its application in friction material field has also obtained expansion, teacher Fu Yewei team of Northwestern Polytechnical University is doing aspect the carbon fiber enhancing paper friction material than more comprehensively studying [Fu Yewei, Li Hejun, Li Kezhi etc. tribology journal, 2004 (24): 555-558].ZrB
2Composite material is because the combination property such as non-oxidizability under unique high-strength, high temperature, high conduction, high stability and good ABRASION RESISTANCE, good electrical and thermal conductivity, good corrosion resistance, good resistance to heat shocks, the good high temperature, under the applied at elevated temperature environment, demonstrate powerful vitality, particularly can play in a lot of fields the unique effect [Tian Tingyan that metal and pottery are difficult to be competent at, Zhang Yujun, Zhang Na, Zhang Lan, Zhang Weike. modern technologies pottery, 2005 (04): 21-23].Yet up to the present, also the no one is incorporated into zirconium boride in the friction material (especially paper friction material).Simultaneously, ZrB
2Material melting point is higher, the sintering difficulty, and the intensity of itself is relative with toughness not high, has limited its application under harsh operating environment.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of zirconium boride modified paper base frication material who comes the frictional behaviour of Effective Raise Wet-type friction material by adding the molten slurry of finely dispersed zirconium boride., stable friction performance high by the prepared material friction coefficient of preparation method of the present invention, friction noise is little, ABRASION RESISTANCE is good, heat-conductivity conducting is good, corrosion resistance is good, resistance to heat shocks is good, non-oxidizability is good.
For achieving the above object, the present invention adopts technical scheme to be:
Step 1: get 0.7g～3.0g cashew nut shell phenol-formaldehyde resin modified, be dissolved in and get phenol resin solution in 50～150ml absolute ethyl alcohol, leave standstill 20h～30h after phenolic resins fully dissolves, sealing is preserved, and obtains A solution;
Step 2: be that to be dispersed in 100～500ml mass concentration be that magnetic agitation configuration Uniform Dispersion obtains carbon nano tube suspension B in 0.1%～0.5% dodecyl sodium sulfate (SDS) aqueous solution for the multi-walled carbon nano-tubes of 30～50nm with 0.5～8g diameter;
Step 3: zirconium boride is dissolved in is mixed with zirconium boride suspension 50～350ml that concentration is 0.12～0.18mol/L in the deionized water, magnetic agitation 10～30min, and then adding the ammonium polymethacrylate (PMAA) of 1～10ml in the suspension, magnetic agitation obtains the molten slurry of zirconium boride C;
Step 4: get chopped carbon fiber that 6～14g diameter is 8～15 μ m, bamboo fibre, 1～5g diatomite that 5～12g beating degree is 75～100 ° of SR and can disperse the water of above-mentioned raw materials fully, it is dispersed in water to get mixed solution, and then the molten slurry C that gets 80～450ml suspended emulsion B and 45～295ml pours in the mixed solution to get D solution into;
Step 5: D solution poured into disperse 800～2000r in the fluffer, take out the D solution after discongesting, handsheet and dry obtains print E on the handsheet machine;
Step 6: with small-bore syringe A solution evenly is coated in print E and upward also naturally dries, hot-forming on vulcanizer, the hot pressing temperature of control vulcanizer is 150～180 ℃, hot pressing time is 10～20min, hot pressing pressure is 3～8MPa, namely obtains the zirconium boride modified paper base frication material of stable friction performance.
The described step 3 magnetic agitation molten slurry C time is 1～4h.
Described step 6 is that positive and negative intersects several times and smears, and carries out the time of penetration of 30～60s after each coating, guarantees that A solution can evenly be impregnated on the print E.
The described step 2 magnetic agitation time is 5～7 hours.
The present invention will be prepared into paper substrate through the technique of the employing papermaking such as homodisperse zirconium boride, homodisperse multi-walled carbon nano-tubes, carbon fiber, bamboo fibre and diatomite, then the phenol resin solution that applies modified rubber is A solution, rear hot-press solidifying to be dried finally is prepared into the friction material print.By controlling the content of various components, can obtain the paper friction material of different coefficients of friction and wear rate.The advantage of this method is that technology controlling and process is simple, and prepared friction material wear rate is low, stable friction performance, material heat conductivity and ABRASION RESISTANCE are good etc.Because these advantages make the method have the potentiality of the large-scale industrial production of developing into.
The invention has the beneficial effects as follows zirconium boride is added in the carbon fiber enhancement resin base Wet-type friction material as raw material, prepare the single-part stationery base frication material.Zirconium boride in the past is used for the thinking of ceramic matric composite modification and the modification that technique refers to paper friction material, thus can be with zirconium boride (ZrB
2) high-melting-point, high strength, high rigidity, non-oxidizability, the good combination properties such as ABRASION RESISTANCE well are dissolved in the paper friction material under good electrical and thermal conductivity, good corrosion resistance, good resistance to heat shocks, the good high temperature.Simultaneously, the working environment of paper friction material has been evaded the shortcoming of zirconium boride composite substantially, utilize the phenolic resins bonding agent zirconium boride and other components well can be combined, acting in conjunction farthest improves the frictional behaviour of paper friction material, effectively reduces wear rate.
Description of drawings
Fig. 1 is the ESEM picture on the embodiment 3 zirconium boride modified paper base frication material surface of preparing.
Fig. 2 is the partial enlarged drawing of Fig. 1.
The specific embodiment
Embodiment 1:
Step 1: get 1.2g cashew nut shell phenol-formaldehyde resin modified, be dissolved in and get phenol resin solution in the 150ml absolute ethyl alcohol, leave standstill 20h～30h after phenolic resins fully dissolves, sealing is preserved, and obtains A solution;
Step 2: be that to be dispersed in the 200ml mass concentration be that magnetic agitation 5～7h configuration Uniform Dispersion obtains carbon nano tube suspension B in 0.25% dodecyl sodium sulfate (SDS) aqueous solution for the multi-walled carbon nano-tubes of 30～50nm with the 0.5g diameter;
Step 3: zirconium boride is dissolved in is mixed with the zirconium boride suspension 50ml that concentration is 0.12mol/L in the deionized water, magnetic agitation 10～30min, and then adding the ammonium polymethacrylate (PMAA) of 1ml in the suspension, magnetic agitation 1～4h obtains the molten slurry of zirconium boride C;
Step 4: get chopped carbon fiber that the 10g diameter is 8～15 μ m, bamboo fibre, 3g diatomite that the 8g beating degree is 85 ° of SR and can disperse the water of above-mentioned raw materials fully, it is dispersed in water to get mixed solution, and then the molten slurry C that gets 100ml suspended emulsion B and 45ml pours in the mixed solution to get D solution into;
Step 5: D solution poured into disperse 900r in the fluffer, take out the D solution after discongesting, handsheet and dry obtains print E on the handsheet machine;
Step 6: with small-bore syringe A solution evenly is coated in print E and upward also naturally dries, described coating is that the positive and negative at print E intersects several times and smears, and carry out the time of penetration of 30～60s after each coating, guarantee that A solution can evenly be impregnated on the print E, it is hot-forming on vulcanizer after coating is finished, the hot pressing temperature of control vulcanizer is 150 ℃, hot pressing time is 10min, hot pressing pressure is 3MPa, namely obtains the zirconium boride modified paper base frication material of stable friction performance.
Embodiment 2:
Step 1: get 1.3g cashew nut shell phenol-formaldehyde resin modified, be dissolved in and get phenol resin solution in the 145ml absolute ethyl alcohol, leave standstill 20h～30h after phenolic resins fully dissolves, sealing is preserved, and obtains A solution;
Step 2: be that to be dispersed in the 250ml mass concentration be that magnetic agitation 5～7h configuration Uniform Dispersion obtains carbon nano tube suspension B in 0.2% dodecyl sodium sulfate (SDS) aqueous solution for the multi-walled carbon nano-tubes of 30～50nm with the 1g diameter;
Step 3: zirconium boride is dissolved in is mixed with the zirconium boride suspension 150ml that concentration is 0.13mol/L in the deionized water, magnetic agitation 10～30min, and then adding the ammonium polymethacrylate (PMAA) of 3.5ml in the suspension, magnetic agitation 1～4h obtains the molten slurry of zirconium boride C;
Step 4: get chopped carbon fiber that the 8g diameter is 8～15 μ m, bamboo fibre, 4g diatomite that the 7g beating degree is 80 ° of SR and can disperse the water of above-mentioned raw materials fully, it is dispersed in water to get mixed solution, and then the molten slurry C that gets 150ml suspended emulsion B and 90ml pours in the mixed solution to get D solution into;
Step 5: D solution poured into disperse 1000r in the fluffer, take out the D solution after discongesting, handsheet and dry obtains print E on the handsheet machine;
Step 6: with small-bore syringe A solution evenly is coated in print E and upward also naturally dries, described coating is that the positive and negative at print E intersects several times and smears, and carry out the time of penetration of 30～60s after each coating, guarantee that A solution can evenly be impregnated on the print E, it is hot-forming on vulcanizer after coating is finished, the hot pressing temperature of control vulcanizer is 155 ℃, hot pressing time is 12min, hot pressing pressure is 4MPa, namely obtains the zirconium boride modified paper base frication material of stable friction performance.
Embodiment 3:
Step 1: get 1.4g cashew nut shell phenol-formaldehyde resin modified, be dissolved in and get phenol resin solution in the 140ml absolute ethyl alcohol, leave standstill 20h～30h after phenolic resins fully dissolves, sealing is preserved, and obtains A solution;
Step 2: be that to be dispersed in the 300ml mass concentration be that magnetic agitation 5～7h configuration Uniform Dispersion obtains carbon nano tube suspension B in 0.15% dodecyl sodium sulfate (SDS) aqueous solution for the multi-walled carbon nano-tubes of 30～50nm with the 1.5g diameter;
Step 3: zirconium boride is dissolved in is mixed with the zirconium boride suspension 200ml that concentration is 0.14mol/L in the deionized water, magnetic agitation 10～30min, and then adding the ammonium polymethacrylate (PMAA) of 4.5ml in the suspension, magnetic agitation 1～4h obtains the molten slurry of zirconium boride C;
Step 4: get chopped carbon fiber that the 9g diameter is 8～15 μ m, bamboo fibre, 5g diatomite that the 6g beating degree is 75 ° of SR and can disperse the water of above-mentioned raw materials fully, it is dispersed in water to get mixed solution, and then the molten slurry C that gets 200ml suspended emulsion B and 135ml pours in the mixed solution to get D solution into;
Step 5: D solution poured into disperse 1100r in the fluffer, take out the D solution after discongesting, handsheet and dry obtains print E on the handsheet machine;
Step 6: with small-bore syringe A solution evenly is coated in print E and upward also naturally dries, described coating is that the positive and negative at print E intersects several times and smears, and carry out the time of penetration of 30～60s after each coating, guarantee that A solution can evenly be impregnated on the print E, it is hot-forming on vulcanizer after coating is finished, the hot pressing temperature of control vulcanizer is 160 ℃, hot pressing time is 14min, hot pressing pressure is 5MPa, namely obtains the zirconium boride modified paper base frication material of stable friction performance.
Fig. 1 is the ESEM picture on the embodiment 3 zirconium boride modified paper base frication material surface of preparing.Fig. 2 is the partial enlarged drawing of Fig. 1, can be clear that on zirconium boride modified paper base frication material surface uniform ground by Fig. 2 and adhere to zirconium boride.
Embodiment 4:
Step 1: get 0.7g cashew nut shell phenol-formaldehyde resin modified, be dissolved in and get phenol resin solution in the 50ml absolute ethyl alcohol, leave standstill 20h～30h after phenolic resins fully dissolves, sealing is preserved, and obtains A solution;
Step 2: be that to be dispersed in the 100ml mass concentration be that magnetic agitation 5～7h configuration Uniform Dispersion obtains carbon nano tube suspension B in 0.1% dodecyl sodium sulfate (SDS) aqueous solution for the multi-walled carbon nano-tubes of 30～50nm with the 3g diameter;
Step 3: zirconium boride is dissolved in is mixed with the zirconium boride suspension 300ml that concentration is 0.16mol/L in the deionized water, magnetic agitation 10～30min, and then adding the ammonium polymethacrylate (PMAA) of 6ml in the suspension, magnetic agitation 1～4h obtains the molten slurry of zirconium boride C;
Step 4: get chopped carbon fiber that the 12g diameter is 8～15 μ m, bamboo fibre, 2g diatomite that the 10g beating degree is 90 ° of SR and can disperse the water of above-mentioned raw materials fully, it is dispersed in water to get mixed solution, and then the molten slurry C that gets 80ml suspended emulsion B and 160ml pours in the mixed solution to get D solution into;
Step 5: D solution poured into disperse 1500r in the fluffer, take out the D solution after discongesting, handsheet and dry obtains print E on the handsheet machine;
Step 6: with small-bore syringe A solution evenly is coated in print E and upward also naturally dries, described coating is that the positive and negative at print E intersects several times and smears, and carry out the time of penetration of 30～60s after each coating, guarantee that A solution can evenly be impregnated on the print E, it is hot-forming on vulcanizer after coating is finished, the hot pressing temperature of control vulcanizer is 180 ℃, hot pressing time is 16min, hot pressing pressure is 6MPa, namely obtains the zirconium boride modified paper base frication material of stable friction performance.
Embodiment 5:
Step 1: get 2.0g cashew nut shell phenol-formaldehyde resin modified, be dissolved in and get phenol resin solution in the 100ml absolute ethyl alcohol, leave standstill 20h～30h after phenolic resins fully dissolves, sealing is preserved, and obtains A solution;
Step 2: be that to be dispersed in the 400ml mass concentration be that magnetic agitation 5～7h configuration Uniform Dispersion obtains carbon nano tube suspension B in 0.3% dodecyl sodium sulfate (SDS) aqueous solution for the multi-walled carbon nano-tubes of 30～50nm with the 5g diameter;
Step 3: zirconium boride is dissolved in is mixed with the zirconium boride suspension 100ml that concentration is 0.18mol/L in the deionized water, magnetic agitation 10～30min, and then adding the ammonium polymethacrylate (PMAA) of 8ml in the suspension, magnetic agitation 1～4h obtains the molten slurry of zirconium boride C;
Step 4: get chopped carbon fiber that the 6g diameter is 8～15 μ m, bamboo fibre, 1g diatomite that the 5g beating degree is 100 ° of SR and can disperse the water of above-mentioned raw materials fully, it is dispersed in water to get mixed solution, and then the molten slurry C that gets 300ml suspended emulsion B and 80ml pours in the mixed solution to get D solution into;
Step 5: D solution poured into disperse 2000r in the fluffer, take out the D solution after discongesting, handsheet and dry obtains print E on the handsheet machine;
Step 6: with small-bore syringe A solution evenly is coated in print E and upward also naturally dries, described coating is that the positive and negative at print E intersects several times and smears, and carry out the time of penetration of 30～60s after each coating, guarantee that A solution can evenly be impregnated on the print E, it is hot-forming on vulcanizer after coating is finished, the hot pressing temperature of control vulcanizer is 170 ℃, hot pressing time is 18min, hot pressing pressure is 7MPa, namely obtains the zirconium boride modified paper base frication material of stable friction performance.
Embodiment 6:
Step 1: get 2.6g cashew nut shell phenol-formaldehyde resin modified, be dissolved in and get phenol resin solution in the 80ml absolute ethyl alcohol, leave standstill 20h～30h after phenolic resins fully dissolves, sealing is preserved, and obtains A solution;
Step 2: be that to be dispersed in the 500ml mass concentration be that magnetic agitation 5～7h configuration Uniform Dispersion obtains carbon nano tube suspension B in 0.4% dodecyl sodium sulfate (SDS) aqueous solution for the multi-walled carbon nano-tubes of 30～50nm with the 6g diameter;
Step 3: zirconium boride is dissolved in is mixed with the zirconium boride suspension 350ml that concentration is 0.15mol/L in the deionized water, magnetic agitation 10～30min, and then adding the ammonium polymethacrylate (PMAA) of 10ml in the suspension, magnetic agitation 1～4h obtains the molten slurry of zirconium boride C;
Step 4: get chopped carbon fiber that the 14g diameter is 8～15 μ m, bamboo fibre, 2.5g diatomite that the 9g beating degree is 95 ° of SR and can disperse the water of above-mentioned raw materials fully, it is dispersed in water to get mixed solution, and then the molten slurry C that gets 450ml suspended emulsion B and 295ml pours in the mixed solution to get D solution into;
Step 5: D solution poured into disperse 800r in the fluffer, take out the D solution after discongesting, handsheet and dry obtains print E on the handsheet machine;
Step 6: with small-bore syringe A solution evenly is coated in print E and upward also naturally dries, described coating is that the positive and negative at print E intersects several times and smears, and carry out the time of penetration of 30～60s after each coating, guarantee that A solution can evenly be impregnated on the print E, it is hot-forming on vulcanizer after coating is finished, the hot pressing temperature of control vulcanizer is 165 ℃, hot pressing time is 20min, hot pressing pressure is 8MPa, namely obtains the zirconium boride modified paper base frication material of stable friction performance.
Embodiment 7:
Step 1: get 3.0g cashew nut shell phenol-formaldehyde resin modified, be dissolved in and get phenol resin solution in the 120ml absolute ethyl alcohol, leave standstill 20h～30h after phenolic resins fully dissolves, sealing is preserved, and obtains A solution;
Step 2: be that to be dispersed in the 450ml mass concentration be that magnetic agitation 5～7h configuration Uniform Dispersion obtains carbon nano tube suspension B in 0.5% dodecyl sodium sulfate (SDS) aqueous solution for the multi-walled carbon nano-tubes of 30～50nm with the 8g diameter;
Step 3: zirconium boride is dissolved in is mixed with the zirconium boride suspension 250ml that concentration is 0.17mol/L in the deionized water, magnetic agitation 10～30min, and then adding the ammonium polymethacrylate (PMAA) of 5ml in the suspension, magnetic agitation 1～4h obtains the molten slurry of zirconium boride C;
Step 4: get chopped carbon fiber that the 7g diameter is 8～15 μ m, bamboo fibre, 3.5g diatomite that the 12g beating degree is 80 ° of SR and can disperse the water of above-mentioned raw materials fully, it is dispersed in water to get mixed solution, and then the molten slurry C that gets 350ml suspended emulsion B and 200ml pours in the mixed solution to get D solution into;
Step 5: D solution poured into disperse 1800r in the fluffer, take out the D solution after discongesting, handsheet and dry obtains print E on the handsheet machine;
Step 6: with small-bore syringe A solution evenly is coated in print E and upward also naturally dries, described coating is that the positive and negative at print E intersects several times and smears, and carry out the time of penetration of 30～60s after each coating, guarantee that A solution can evenly be impregnated on the print E, it is hot-forming on vulcanizer after coating is finished, the hot pressing temperature of control vulcanizer is 175 ℃, hot pressing time is 15min, hot pressing pressure is 5MPa, namely obtains the zirconium boride modified paper base frication material of stable friction performance.
Claims (4)
1. the preparation method of a zirconium boride modified paper base frication material is characterized in that:
Step 1: get 0.7g～3.0g cashew nut shell phenol-formaldehyde resin modified, be dissolved in and get phenol resin solution in 50～150ml absolute ethyl alcohol, leave standstill 20h～30h after phenolic resins fully dissolves, sealing is preserved, and obtains A solution;
Step 2: be that to be dispersed in 100～500ml mass concentration be that magnetic agitation configuration Uniform Dispersion obtains carbon nano tube suspension B in 0.1%～0.5% dodecyl sodium sulfate (SDS) aqueous solution for the multi-walled carbon nano-tubes of 30～50nm with 0.5～8g diameter;
Step 3: zirconium boride is dissolved in is mixed with zirconium boride suspension 50～350ml that concentration is 0.12～0.18mol/L in the deionized water, magnetic agitation 10～30min, and then adding the ammonium polymethacrylate (PMAA) of 1～10ml in the suspension, magnetic agitation obtains the molten slurry of zirconium boride C;
Step 4: getting chopped carbon fiber, the 5～12g beating degree that 6～14g diameter is 8～15 μ m is 75～100.The bamboo fibre of SR, 1～5g diatomite and can disperse the water of above-mentioned raw materials fully are dispersed in water to get mixed solution with it, and then the molten slurry C that gets 80～450ml suspended emulsion B and 45～295ml pours in the mixed solution to get D solution into;
Step 5: D solution poured into disperse 800～2000r in the fluffer, take out the D solution after discongesting, handsheet and dry obtains print E on the handsheet machine;
Step 6: with small-bore syringe A solution evenly is coated in print E and upward also naturally dries, hot-forming on vulcanizer, the hot pressing temperature of control vulcanizer is 150～180 ℃, hot pressing time is 10～20min, hot pressing pressure is 3～8MPa, namely obtains the zirconium boride modified paper base frication material of stable friction performance.
2. the preparation method of zirconium boride modified paper base frication material according to claim 1, it is characterized in that: the described step 3 magnetic agitation molten slurry C time is 1～4h.
3. the preparation method of zirconium boride modified paper base frication material according to claim 1, it is characterized in that: described step 6 is that positive and negative intersects several times and smears, and carry out the time of penetration of 30～60s after each coating, guarantee that A solution can evenly be impregnated on the print E.
4. the preparation method of zirconium boride modified paper base frication material according to claim 1, it is characterized in that: the described step 2 magnetic agitation time is 5～7 hours.
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