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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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  • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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  • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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  • C04B2235/5208—Fibers
  • C04B2235/5264—Fibers characterised by the diameter of the fibers
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
  • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
  • F16D2200/00—Materials; Production methods therefor
  • F16D2200/006—Materials; Production methods therefor containing fibres or particles
  • F16D2200/0065—Inorganic, e.g. non-asbestos mineral fibres
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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  • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
  • F16D2200/00—Materials; Production methods therefor
  • F16D2200/0082—Production methods therefor
  • F16D2200/0086—Moulding materials together by application of heat and pressure

Definitions

• the present invention relates to an amorphous composite alkali metal titanate composition, which is excellent in chemical stability and thermal stability.
• the present invention relates to a crystalline composite Al-titanium titanate metal composition and a friction material compounded with the composition.
• alkali metal titanates are chemically unstable because they have a large amount of alkali components and a layered crystal structure, and at the time of forming the friction material, the alkali metal ions present in the layers are eluted. Therefore, there is a disadvantage that the resin constituting the matrix of the friction material is deteriorated.
• the crystal structure of the alkali metal titanate becomes a tunnel shape, chemical stability is higher.
• Potassium hexatitanate is produced by the melting method as a typical production method. First, the molten raw material is cooled and solidified to prepare a fibrous mass of potassium dititanate, and then the fibrous mass is swollen and separated by a hydration reaction. Next, the separated fiber is acid-treated, the potassium is leached to a composition of potassium hexatitanate, solid-liquid separation is carried out, and heat treatment is carried out to convert it into a hexatidic acid lithium of tunnel structure. Disclosure of Invention (Japanese Patent No. 2 9 4 6 1 0 7)
• the lithium hexatitanate produced by the above-mentioned melting method requires a conversion step from dititanic acid lithium to hexatitanic acid lithium, and the production process is complicated. In addition, theoretical yield is low due to leaching of potassium.
• the shape obtained by this melting method is a plate-like fiber, and it is difficult to make different shapes other than plate-like according to the required performance.
• the object of the present invention is to eliminate the steps of composition conversion and structure conversion required in the conventional manufacturing methods, and to provide a chemically stable, moisture-resistant and thermally stable base material of a friction material. It is an object of the present invention to provide an amorphous composite titanium titanate metal composition suitable as a material.
• amorphous potassium 1-4 titanate alone is inferior in chemical stability and insufficient in moisture absorption resistance, as in the crystal structure. It has been found that coexistence of a fixed amount of S i ⁇ 2 enables chemical stability and moisture resistance.
• the first amorphous composite alkaline metal titanate metal composition according to the present invention has a formula M 2 0. N T i 0 2 (wherein, M is one or more kinds of alkali metal elements, Alkali metal titanate represented by a number of 4): 60 to 90% by weight, S i ⁇ 2 10 to 40%. / Has a composition of 0, an M 2 OZS i 0 2 ⁇ 2.5 .
• the second amorphous composite aluminum titanate metal composition according to the present invention has the general formula M 2
• Alkali metal titanate represented by nT i 0 2 (wherein, M is at least one alkali metal element and n is a number from 1 to 4): 60% by weight or more and less than 90% by weight, S i O 2 : 10% by weight or more and less than 40% by weight, and an oxide of at least one element selected from the group consisting of B, Mg, Al, P, Ca and Z n: more than 0% by weight
• 10 weight 0/0 has the following composition, an M 2 ⁇ / S i 0 2 ⁇ 2.5.
• Third amorphous composite titanate Al force Li metal composition according to the present invention have the general formula Micromax 2 0
• nT i 0 2 (wherein, Micromax is one or more alkali metal elements, eta is the number of 1 to 4) alkali metal titanate represented by: less than 60 weight 0/0 90% by weight or more, S i 2 2 : 10% by weight or more and less than 40% by weight, and at least one selected from the group consisting of V, Cr, Mn, Fe, Co, Ni, Cu, Y, Zr, Nb, and Ba
• the oxides of the elements of the species having a composition of more than 0% by weight and not more than 10% by weight, and M 20 / S i O 2 ⁇ 2.5.
• the fourth amorphous composite alumina titanate metal composition according to the present invention has a general formula M 2 0
• Alkali metal titanate represented by nT i O 2 (wherein, M is at least one alkali metal element and n is a number from 1 to 4): 60% by weight or more and less than 90% by weight, S i O 2: 10 wt% or more and less than 40 weight 0/0, B, Mg, Al, P, ⁇ & ⁇ Pi sigma 11 Tona Ru least one element of the acid I arsenide material is selected from the group: 0 wt% 10% by weight or less and at least one element selected from the group consisting of V, Cr, Mn, Fe, Co, Ni, Cu, Y, Zr, Nb and Ba. oxide: 0 wt% to have a composition of ultra-forte 10 weight 0/0 or less, a M 2 O / S i 0 2 ⁇ 2.5.
• Fig. 1 shows the flat amorphous composite titanium titanate aluminum alloy obtained in Preparation Example 1. It is the microscope picture by the sliding type electron microscope of genus composition powder.
• FIG. 2 is a scanning electron microscopic photomicrograph of the flat amorphous composite composite of aluminum titanate metal titanate composition powder obtained in Preparation Example 1.
• FIG. 3 is a scanning electron microscopic photomicrograph of the fibrous amorphous composite composite metal titanate composition fiber obtained in Preparation Example 2.
• FIG. 4 is a scanning electron micrograph of a spherical amorphous composite composite of an aluminum complex metal titanate composition obtained in Preparation Example 3.
• the amorphous composite alkali metal titanate composition according to the present invention has a general formula M 2 0 ′ nT i 0 2 (wherein, M is one or two or more alkali metal elements, n is and 1-4 number) in alkali metal titanate 6 0 wt% or more, it expressed, comprise S i ⁇ 2 1 0 wt% or more, and M 2 ⁇ _ZS i 0 2 ⁇ 2.
• An oxide of at least one element selected from the group consisting of i, Cu, Y, Zr, Nb and Ba can be included.
• the amorphous composite aluminum titanate metal composition according to the present invention is suitably used as a base material of a friction material, and imparts smooth friction characteristics by blending 3 to 50% by weight as a base material. be able to.
• the alkali metal element is a Group 1 element of the Periodic Table of the Elements, and specifically, it is Li, Na, K, or.
• the amorphous nature of the alkali metal titanate can be obtained by heating and melting the starting material mixture and subjecting the melt to a quenching treatment.
• the quenching process is typically performed by a twin roll method, and while rotating a pair of opposing metal rolls at high speed, Five
• the melt is allowed to flow down the gap, and the melt is quenched in contact with the metal roll, passes through the opening gap, and is discharged downward as a flaky solid. It becomes amorphous due to its quenching effect.
• the amorphous alkali metal titanate thus obtained can be obtained by co-containing S i 2 2 even in the case of a titanic acid in which the number of n is 4 or less in the formula M 2 0 ⁇ n T i O 2. Since the excellent chemical stability and moisture absorption resistance can be ensured, the elution of aluminum ions is prevented during molding of the friction material, and the matrix composition resin of the friction material is not adversely affected. .
• the amorphous alkali metal titanate is stable in the formula M 20 ⁇ n T i 0 2 in the case of a titanic acid in which the number of n is greater than 4 even though it does not contain S i 0 2 S i 0 2 , B, M g, A l, P, C a, Z n, V, C r, M n, F e, C o, N i, C u, Y, Z r, N You may contain oxides, such as b and Ba.
• the amorphous structure of alkali metal titanate causes softening and melting reaction according to the friction conditions (temperature, speed, pressure, etc.), and an appropriate amount of Al- It has been found that the supply of the component and the titanium component has the effect of significantly improving the wear resistance under various conditions. In order to obtain these effects, it is preferable that the content of aluminum titanate in the amorphous composite titanium titanate metal composition be 60% by weight or more.
• the amorphous composite alkali metal titanate composition contains not less than 10% by weight of S i O 2 and the ratio of M 20 to S i O 2 of alkali metal titanate. That is, M 2 Z S i 2 is specified to 2.5 or less.
• the content of SiO 2 contained in the amorphous composite aluminum titanate metal composition is 10% by weight or more, the content of the alkali metal titanate is 90% by weight or less.
• the alkali metal titanate is 60% by weight or more, SiO 2 is 40% by weight or less.
• the oxides of B, Mg, Al, P, and & and 2! 1 have the effect of improving the chemical stability'stability, and also have the function of improving the thermal stability. Therefore, it is desirable to include an oxide of at least one element selected from the group consisting of B, Mg, Al, P, Ca and Z n. If the content is too high, the compounding balance between aluminum titanate and Si iO 2 will be lost, so the upper limit is made 10% by weight.
• the content of aluminum titanate is less than 90% by weight, S i ⁇ 2 is less than 40% by weight.
• the oxide of at least one element selected from the group is included, the amount of titanium titanate is less than 90% by weight, and SiO 2 is less than 40% by weight.
• an oxide of at least one element selected from the group consisting of B, M g, Al, P, C a and Z n is further contained in addition to the oxides of these elements, The same is true.
• the amorphous composite alkali metal titanate composition of the present invention is a friction material, and more specifically, a brake lining for a braking device of an automobile, a railway vehicle, an aircraft, an industrial machine, etc., a disc pad, a clutch facing, etc. It is suitably applied as a base material of a friction material that constitutes a sliding surface.
• non-crystalline composite alkali metal titanate composition applied as a base material of a friction material is 3 to 50 weight%.
• the friction material together with the amorphous composite aluminum titanate metal composition, if desired, other known types of other materials (for example, polyamide fiber, ferrite fiber, steel fiber, copper fiber, Glass fiber, ceramic fiber, crystalline titanic acid compound fiber, etc. can be compounded in a composite manner.
• the base material is usually treated with a silane coupling agent or a titanate coupling agent for the purpose of improving the dispersibility and binding to the binder resin. It is applied and used according to the law.
• the friction material may, if desired, be a known friction and wear modifier (for example, natural or synthetic rubber powder, Kash-1 resin powder, organic powder, graphite, molybdenum disulfide, inorganic powder, metal powder, oxide powder, etc.
• a known friction and wear modifier for example, natural or synthetic rubber powder, Kash-1 resin powder, organic powder, graphite, molybdenum disulfide, inorganic powder, metal powder, oxide powder, etc.
• various additives eg, fungicides, lubricants, grinding agents, etc.
• a base material is dispersed in a binder resin, and if necessary, a friction and wear modifier and additives are added and uniformly mixed to prepare a raw material composition.
• mold molding is performed, and heating under pressure (approx. Binder molding is carried out at 10 to 40 MP a, temperature about 150 to 200 ° C.), and after removal from the mold, heat treatment is optionally carried out in a heating furnace (1 500 to 200 ° C.). And holding for about 1 to 12 hours), and then subjecting the molded body to machining and polishing to finish it as a friction material having a predetermined shape.
• Preparation Example 1 Flat amorphous composite titanium oxide metal complex metal composition
• the mixture is weighed so that the molar ratio is 2 and the homogeneous mixture is heated at 800 for 2 hours to obtain a powder of potassium titanate (KsO ⁇ 2T i 0 2 ).
• Silica (S i O 2) and magnesium hydroxide (Mg (OH) 2 ) were added to the obtained titanium titanate (K 2 0 2 T i 0 2 ), KsO ⁇ 2 T i Os / S i 0
• the obtained melt is poured between metal twin rolls rotating at a circumferential speed of 3.6 m / s, and after quenching, the resulting quenched solidified product is crushed by a hammer mill to obtain a powder.
• the composition substantially agrees with the raw material composition, and the average passing diameter is about 300 m and the average thickness is about It was confirmed that the composition was a flat amorphous composite amorphous titanium titanate metal composition of 80 m.
• test composition according to Preparation Example 1 is shown as No. 2 in Table 1.
• T i OsZKzO 2 ⁇ , 2 ⁇ i 0 2 / / S i 0 2 / F e 2
• T i OzZKzO 2 K 2 0 ⁇ 2 T i O 2 / S i O 2 / M g O / Z
• T i Z 2 ZK 2 0 1.7, ⁇ 2 0 ⁇ 1.
• T i 0 2 ZK 2 0 3 K 2 0 ⁇ ⁇ 3 T i O 2 / S i O 2 /
• Preparation Example 2 Amorphous Composite Alkali Metal Titanate Titanate in Fiber Form
• the molar ratio of lithium carbonate (K 2 C 3 O 3 ) to titanium dioxide (T i O 2 ) is changed as in Preparation Example 1 the titanate force Li um obtained by the method ( ⁇ 2 0 ⁇ 1.
• Add 7 T i ⁇ 2 / S i O 2 / A 1 2 Q 3 78/1 8 4 weight ratio, The mixture is put in a platinum crucible and melted at 115.degree. C. for 2 hours.
• the obtained melt was transferred to a heating crucible having a nozzle hole at the bottom, and a trickle flow from the tip of the nozzle was made, and compressed air was blown away to obtain a fiber.
• the resulting fibers were observed with a scanning electron microscope, and the photomicrograph is shown in FIG.
• the composition was determined by X-ray diffraction to determine the presence or absence of the crystal phase, and fluorescent X-ray analysis was performed. It was confirmed that the composite was a fibrous amorphous composite alumina titanate metal composition having an average aspect ratio (length ⁇ diameter) of 0 ⁇ m and 50.
• test composition according to Preparation Example 2 is shown as No. 3 in Table 1.
• Lithium titanate (K 2 O 2 2. 2.8) obtained by the same method as in Production Example 1 by changing the molar ratio of carbonated lithium (K 2 C 0 3 ) and titanium dioxide (T i O 2 ).
• T i O 2), silica (S i 0 2) and calcium carbonate (C a C_ ⁇ 3), kappa 2 ⁇ ⁇ 2.8 T i ⁇ 2 / S i O 2 / C a 0 8 2/1 0
• the mixture was sprayed to a weight ratio of / 6, and the mixture was sprayed by a spraying apparatus (CASTON DYN DS 8000, manufactured by Nippon Tek Co., Ltd.), and quenched in water to obtain a powder.
• the obtained powder was observed with a scanning electron microscope, and its photomicrograph is shown in FIG.
• a spherical amorphous composite titanic acid having an average particle diameter of about 30 m with a composition substantially identical to the raw material composition. It was confirmed that it was an aluminum metal composition.
• test composition according to Preparation Example 3 is shown as No. 4 in Table 1.
• No. 14 is an example of known crystalline potassium hexatitanate.
• Mixtures formulated to give a Ti Os / KsO molar ratio of 2 at 1 200 ° C 1 The solution is heated and melted, and the resulting melt is solidified by cooling to form a fiber mass of potassium dititanate, and the fiber mass is swollen and separated by a hydration reaction, subjected to acid treatment and force dissolution treatment. Thereafter, it was manufactured by performing solid-liquid separation and heat treatment.
• the average fiber length is about 150 ⁇ m, and the average fiber width is about 30 ⁇ m.
• Nos. 1 to 6 are examples of the present invention
• Nos. 1 to 13 are comparative examples
• No. 14 is a conventional example of a crystal structure.
• No. 1 1 is an example not containing S i 2 2
• Example No. 1 2 is an example where the value of M 2 O Z S i O 2 is larger than the value 2.5 of the present invention
• No. 1 3 is S i O This is an example in which the content of 2 is small, and the value of MzO / S i 2 2 is larger than the value 2.5 of the present invention.
• Examples No. 1 to No. 6 of the present invention have a smaller weight increase rate due to water absorption compared to Comparative Examples No. 1 to No. 13 and have excellent moisture absorption resistance. It is shown that.
• No. 14 has a smaller weight increase rate due to water absorption than the example of the present invention, it is crystalline, and as described above, it is converted from potassium dititanate to potassium hexatitanate. Since the process is required, the manufacturing process is complicated, and potassium leaching occurs, so that the theoretical yield is low.
• the raw material for the friction material is, by weight, 20% base component, 4% Kepler pulp, 17% copper fiber, 4% ceramic fiber, 10% abrasive material, 5% strength, 4% organic powder Lubricant 6%, barium sulfate 20%, fuyol resin 1 8066941
• test friction materials using the respective compositions No. 1 to No. 6 and No. 11 to No. 14 as base materials in Table 2 were each 0% and No. 1 a ⁇ It represents as No. 6 a and No. 1 1 a to No. 1 4 a.
• test friction material was subjected to a wear test according to J AS OC 4 2 7 “Brake lining, pad wear dynamometer test method”, friction coefficient), pad wear (mm) and disk wear (; For um), the results shown in Table 2 were obtained.
• the coefficient of friction is the average coefficient of friction during steady state at each temperature, and the amount of pad wear and the amount of disc wear are the average amount of wear per 100 cycles of braking.
• the embodiments No. 1a to No. 6a of the present invention correspond to the low temperature region corresponding to the relatively low initial braking speed as compared with the comparative examples No. 1 1a and No. 1 2a.
• Pads and discs have high friction coefficient from (100 ° C) to high temperature range (400 ° C) corresponding to high braking initial velocity accompanied by temperature rise of the friction surface. Low amount, excellent in wear resistance. This is considered in the embodiment of the present invention to form a stable fluidized bed at the friction interface from the low temperature zone to the high temperature zone and to form a uniform transfer layer on the mating disk surface. .
• No. 13 a has a high coefficient of friction substantially equivalent to that of the embodiment of the present invention
• the pad wear amount is larger and the disk wear amount is larger than the embodiment of the present invention. This is considered to be because the transfer layer formed on the disk surface is more fragile than the embodiment of the present invention.
• No. 14 a is equal to or more than the embodiment of the present invention in terms of the coefficient of friction, but the amount of pad wear and disk wear is larger than that of the embodiment of the present invention. This is considered to be due to the fact that No. 14 a is crystalline and has a high melting point and does not cause a softening phenomenon, so it is somewhat inferior to the stable formation of the fluidized bed at the friction interface as compared with the example of the present invention.
• the amorphous composite alkali metal titanate composition of the present invention is chemically stable and excellent in moisture absorption resistance, and when applied to a friction material such as a disk pad of a car, it can be used as a conventional crystal. Compared to the quality alkali metal hexatitanate, it is possible to obtain the friction and wear characteristics with improved wear resistance and facing damage while having almost the same stability of friction coefficient under high temperature and high load.
• the amorphous composite aluminum titanate metal composition of the present invention has an advantage of being able to optionally produce a flat, fibrous or spherical composition by selecting an appropriate production method. .
• the flat shape is suitably selected in terms of pore formation and strength improvement, and a typical size is an average diameter of 10 to 600 jum and an average thickness of 3 to 200 ⁇ m.
• the fiber shape is suitably selected in view of the further improvement of pore formation and strength, and the typical size has an average diameter of 5 to 100 ⁇ and an aspect ratio (diameter to diameter) of 10 or more.
• the spherical shape is suitably selected in terms of flowability and dispersibility, and the typical size is an average particle size of 5 to 5: L O O ni.

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