Preparation method of carbon-ceramic brake material with strong oxidation resistance

An anti-oxidation, carbon-ceramic technology, applied in mechanical equipment, friction linings, gear transmission mechanisms, etc., can solve the problems of wear and friction interface stability, poor anti-oxidation performance of friction interface, etc., to reduce oxidation wear and improve anti-oxidation. The effect of oxidative power

Inactive Publication Date: 2020-04-24

山东道普安制动材料有限公司

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AI-Extracted Technical Summary

Problems solved by technology

It solves the problems of poor oxidation resistance of the friction interface, severe wear and poor stability of the friction ...

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Method used

(1) the present invention is between pyrolysis carbon substrate layer and pyrolysis carbon substrate layer, introduces boron carbide by chemical vapor deposition, can effectively protect pyrolysis carbon substrate and carbon fiber inside boron carbide layer from being corroded by oxygen, At the same time, it does not affect the pyrolytic carbon layer outside the boron carbide layer to react with molten silicon to form silicon carbide, which protects the integrity of the boron carbide layer itself; improves the uniformity of ceramic phase distribution in each area, and utilizes the high hardness of boron carbide itself. Improves mechanical resistance to wear in carbon/carbon areas.

(2) the present invention controls the introduction amount of boron carbide by the depositio...

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Abstract

The invention relates to a preparation method of a carbon-ceramic brake material with strong oxidation resistance. The method is based on a three-dimensional needled carbon/ceramic brake material. A carbon/carbon-boron carbide composite material is obtained by introducing a CVI deposition B4C process technology between pyrolytic carbon and pyrolytic carbon; a siliconizing treatment is carried outafter a high-temperature treatment; the antioxidant carbon/carbon-boron carbide-silicon carbide composite material with a density of 1.9 g/cm<3> to 3.0 g/cm<3> is obtained; according to the method, the pyrolytic carbon matrix and the carbon fibers in the boron carbide layer can be effectively protected from being eroded by oxygen, meanwhile, the pyrolytic carbon layer outside the boron carbide layer is not influenced and reacts with molten silicon to generate silicon carbide, the integrity of the boron carbide layer is protected; the distribution uniformity of ceramic phases in each area is improved, the mechanical wear resistance of a carbon/carbon area is improved by utilizing the high hardness of boron carbide, the expansion path of cracks in the material failure process is prolonged through the multi-layer structure design, stress release is facilitated, the bearing capacity of the matrix is improved, and the strength and toughness of the brake material become better.

Application Domain

Friction liningActuators

Technology Topic

Molten siliconOxidation resistant +13

Image

Examples

Experimental program(4)

Example Embodiment

[0011] A preparation method of a carbon ceramic brake material with strong oxidation resistance, comprising the following steps:

[0012] 1) After high-temperature heat treatment of the three-dimensional acupuncture preform, pyrolytic carbon was deposited by chemical vapor infiltration CVI to obtain a density of 0.6 g/cm 3 -1.0g/cm 3 of carbon/carbon composites;

[0013] 2) depositing boron carbide on the upper surface of the carbon/carbon composite material by chemical vapor infiltration CVI deposition to obtain a carbon/carbon-boron carbide composite material;

[0014] 3) Pyrolytic carbon was deposited on the surface of the carbon/carbon-boron carbide composite boron carbide by chemical vapor infiltration CVI deposition, resulting in a density of 1.3 g/cm 3 -1.7g/cm 3 Multilayer structure carbon/carbon-boron carbide composite material containing carbon-boron carbide-carbon;

[0015] 4) carrying out high temperature heat treatment on the multi-layer structure carbon/carbon-boron carbide composite material containing carbon-boron carbide-carbon;

[0016] 5) The carbon/carbon-boron carbide composite material processed in step 4) is subjected to siliconizing treatment, and naturally cooled to room temperature to obtain a density of 1.9 g/cm 3 -3.0g/cm 3 Carbon/carbon-boron carbide-silicon carbide composite material with strong oxidation resistance.

[0017] Preferably according to the present invention, the three-dimensional acupuncture preform used in step 1) is an annular preform with an outer diameter of 200-800 mm, an inner diameter of 100-200 mm, and a thickness of 20-100 mm, using two-dimensional plain weave or three-dimensional weaving. made.

[0018] Preferably according to the present invention, step 1) the three-dimensional acupuncture preform carbon fiber adopts a three-dimensional acupuncture preform with a grade of T700.

[0019] Preferably according to the present invention, in step 1), the deposition temperature for depositing pyrolytic carbon is 900°C-1100°C, the deposition time is 50-200h, and the precursor used for deposition is CH 4 and C 3 H 8.

[0020] Preferably according to the present invention, in step 2), the deposition temperature for depositing boron carbide is 800°C-1100°C, the deposition time is 10-200h, the pressure in the furnace is 2kPa, and the precursor used for deposition is BCl 3 -CH 4 and BCl 3 -C 3 H 6 ,

[0021] Preferably according to the present invention, in step 3), the process of depositing pyrolytic carbon is the same as that in step 1).

[0022] Preferably according to the present invention, in step 4), the heat treatment temperature is 1800°C-2600°C, and the heat treatment atmosphere is Ar gas.

[0023] According to a preferred embodiment of the present invention, in step 4), the reaction melt of the siliconizing treatment is silicon or silicon alloy, the reaction temperature is 1200°C-1900°C, and the holding time is 0.5h-4h.

[0024] Beneficial effects:

[0025] The present invention is based on the three-dimensional needle punched carbon/ceramic brake material, by introducing CVI between pyrolytic carbon and pyrolytic carbon to deposit B 4 C process technology obtains carbon/carbon-boron carbide composite material, which is siliconized after high temperature treatment to obtain a density of 1.9g/cm 3 -3.0g/cm 3 The oxidation-resistant carbon/carbon-boron carbide-silicon carbide composite material has the following advantages compared with existing materials:

[0026] (1) The present invention introduces boron carbide through chemical vapor deposition between the pyrolytic carbon substrate layer and the pyrolytic carbon substrate layer, which can effectively protect the pyrolytic carbon substrate and carbon fibers inside the boron carbide layer from being eroded by oxygen, and at the same time does not The pyrolytic carbon layer outside the boron carbide layer reacts with molten silicon to form silicon carbide, which protects the integrity of the boron carbide layer itself; improves the uniformity of ceramic phase distribution in each region, and utilizes the high hardness of boron carbide itself to improve carbon/carbon Mechanical wear resistance of the carbon region.

[0027] (2) The present invention controls the introduction amount of boron carbide through the deposition temperature and deposition time of the boron carbide, so that the boron carbide layer not only protects the internal carbon fibers and the matrix, but also does not affect the friction and wear properties of the material.

[0028] (3) The boron trioxide formed by the oxidation of the boron carbide matrix introduced in the present invention has self-healing ability, which can cover the surface of the carbon fiber and the carbon matrix, prevent the further occurrence of the oxidation reaction, reduce the oxidation wear of the brake material, and is more suitable for Application in high-speed and high-energy load conditions;

[0029] (4) The introduction of the silicon carbide substrate of the present invention adopts the liquid silicon infiltration process, the process is simple, the material densification speed is fast, and the process cost is also lower.

[0030] (5) Through the multi-layer structure design of the present invention, the propagation path of cracks during material failure is extended, which is conducive to stress release, can improve the bearing capacity of the substrate, and has better strength and toughness of the brake material, and a higher safety factor.

Example Embodiment

[0032] Example 1:

[0033] A preparation method of a carbon ceramic brake material with strong oxidation resistance, the steps are as follows:

[0034] 1) Preparation of carbon fiber preforms:

[0035] First, the C fiber with the grade of T700 is made into short fiber tire web and non-weft fabric, and then a single layer of 0° non-weft fabric, tire mesh, 90° non-weft fabric, and tire mesh are laid in sequence, and then the edge belt is used. The lower barb barbs are needle punched for lay fabrics and tire nets. The barb thorn brings the fiber of the tire mesh layer to the vertical direction during the needle punching process, so that the non-weft fabric and the tire mesh are integrated into one, and the density of needle punching holes is 8-12 pieces/cm 2. According to the required thickness, the three-dimensional acupuncture carbon fiber preform is obtained after repeated lamination and needle punching. The density of the preform is about 0.55g/cm3, the volume content of carbon fiber is about 40vol.%, and the layer density is about 14 layers/(10mm).

[0036] 2) High temperature heat treatment of fiber preform:

[0037] The carbon fiber preform obtained in step 1 is subjected to high temperature heat treatment, the heat treatment temperature is 1800° C., the holding time is 5h, and the treatment atmosphere is Ar gas.

[0038] 3) Pyrolytic carbon layer deposition

[0039] The carbon fiber preform that has undergone high temperature heat treatment in step 2) is subjected to chemical vapor deposition and pyrolysis of carbon, the deposition temperature is 900 ° C, the deposition time is 60 h, and the precursor is CH 4 and C 3 H 8 , resulting in a density of 0.6 g/cm 3 -1.0g/cm 3 of carbon/carbon composites;

[0040] 4) Boron carbide layer deposition

[0041]The carbon/carbon composite material obtained in step 3) is deposited by chemical vapor infiltration CVI to deposit boron carbide, the deposition temperature is 800 ° C, the deposition time is 15 h, the furnace pressure is 2 kPa, and the precursor is BCl 3 -CH 4 and BCl 3 -C 3 H 6 , the carbon/carbon-boron carbide composites were obtained.

[0042] 5) Pyrolytic carbon layer deposition

[0043] The carbon/carbon-boron carbide composite material obtained in step 4) is deposited pyrolytic carbon by chemical vapor infiltration CVI, and the deposition time is 60 to obtain a density of 1.3g/cm 3 -1.7g/cm 3 Multilayer carbon/carbon-boron carbide composites containing carbon-boron carbide-carbon.

[0044] 6) High temperature heat treatment

[0045] The multi-layer carbon/carbon-boron carbide composite material containing carbon-boron carbide-carbon obtained in step 5) is subjected to high temperature heat treatment, the heat treatment temperature is 1800°C, and the treatment atmosphere is Ar gas.

[0046] 7) Silicon infiltration treatment

[0047] The carbon/carbon-boron carbide composite material processed in step 6) is subjected to siliconizing treatment, the reaction melt is silicon, the reaction temperature is 1500 ° C, the holding time is 1, and it is naturally cooled to room temperature with the furnace to obtain a density of 1.9g. /cm 3 -3.0g/cm 3 Antioxidant properties of carbon/carbon-boron carbide-silicon carbide composites.

[0048] Antioxidant ability comparison

[0049] The carbon/carbon-boron carbide-silicon carbide composite material of Example 1 and the existing material were placed in static air for 12 hours, and the weight loss rate of static air oxidation for 12 hours was measured. Boron-carbon-silicon carbide composites.

[0050] Table 1 Oxidation weight loss rate of carbon ceramic material after static air oxidation for 12h

[0051]

[0052] It can be seen from Table 1 that the carbon/carbon-boron carbide-silicon carbide composite material of the present embodiment 1, whether it is a semi-finished product or a finished product, the weight loss rate after being placed in static air for 12h is much smaller than the prior art, indicating that the carbon/carbon/carbon/boron carbide-silicon carbide composite material of the present invention is much smaller than the prior art. Carbon-boron carbide-silicon carbide composites have strong oxidation resistance.

Example Embodiment

[0053] Example 2:

[0054] A preparation method of a carbon ceramic brake material with strong oxidation resistance, the steps are as follows:

[0055] 1) Preparation of carbon fiber preforms:

[0056] First, the C fiber with the grade of T700 is made into short fiber tire net and non-weft fabric, and then a single layer of 0° non-weft fabric, tire net, 90° non-weft fabric, and tire net are successively layered in turn, and then the edge belt is used. The lower barb barbs are needle punched for lay fabrics and tire nets. The barb thorns bring the fibers of the tire mesh layer to the vertical direction during the needle punching process, so that the non-weft fabric and the tire mesh are integrated into one, and the density of needle punching holes is 8 to 12/cm2. According to the required thickness, the three-dimensional acupuncture carbon fiber preform is obtained after repeated lamination and needle punching. The density of the preform is about 0.55g/cm3, the volume content of carbon fiber is about 40vol.%, and the layer density is about 14 layers/(10mm).

[0057] 2) High temperature heat treatment of fiber preform:

[0058] The carbon fiber preform obtained in step 1 is subjected to high temperature heat treatment, the heat treatment temperature is 1900° C., the holding time is 3 hours, and the treatment atmosphere is Ar gas.

[0059] 3) Pyrolytic carbon layer deposition

[0060] The carbon fiber preform that has undergone high temperature heat treatment in step 2) is subjected to chemical vapor deposition and pyrolysis of carbon, the deposition temperature is 1000 ° C, the deposition time is 80 h, and the precursor is CH 4 and C 3 H 8 , resulting in a density of 0.6 g/cm 3 -1.0g/cm 3 of carbon/carbon composites.

[0061] 4) Boron carbide layer deposition

[0062] The carbon/carbon composite material obtained in step 3) is deposited by chemical vapor infiltration CVI to deposit boron carbide, the deposition temperature is 1000 ° C, the deposition time is 20 h, the furnace pressure is 2 kPa, and the precursor is BCl 3 -CH 4 and BCl 3 -C 3 H 6 , the carbon/carbon-boron carbide composites were obtained.

[0063] 5) Pyrolytic carbon layer deposition

[0064] The carbon/carbon-boron carbide composite obtained in step 4 was deposited by chemical vapor infiltration CVI to deposit pyrolytic carbon, and the deposition time was 80h to obtain a density of 1.3g/cm 3 -1.7g/cm 3 Multilayer carbon/carbon-boron carbide composites containing carbon-boron carbide-carbon.

[0065] 6) High temperature heat treatment

[0066] The multi-layer carbon/carbon-boron carbide composite material containing carbon-boron carbide-carbon obtained in step 5) is subjected to high temperature heat treatment, the heat treatment temperature is 2000°C, and the treatment atmosphere is Ar gas.

[0067] 7) Silicon infiltration treatment

[0068] The carbon/carbon-boron carbide composite material processed in step 6 is subjected to siliconizing treatment, and the reaction melt is silicon alloy (Cu-Si, Fe-Si, Al-Si, Zr-Si, Hf-Si), and the reaction temperature is is 1600 ° C, the holding time is 2 hours, and it is naturally cooled to room temperature with the furnace to obtain a density of 1.9 g/cm. 3 -3.0g/cm 3 Self-healing antioxidant capacity of carbon/carbon-boron carbide-silicon alloy composites.

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PUM

Property	Measurement	Unit
Density	0.6 ~ 1.0	g/cm³
Density	1.3 ~ 1.7	g/cm³
Density	1.9 ~ 3.0	g/cm³
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Improve antioxidant capacity

Preparation method of carbon-ceramic brake material with strong oxidation resistance

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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