CN102373389A - Preparation method of three-dimensional woven carbon fiber-reinforced magnesium-based composite material - Google Patents
Preparation method of three-dimensional woven carbon fiber-reinforced magnesium-based composite material Download PDFInfo
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- CN102373389A CN102373389A CN2011102919106A CN201110291910A CN102373389A CN 102373389 A CN102373389 A CN 102373389A CN 2011102919106 A CN2011102919106 A CN 2011102919106A CN 201110291910 A CN201110291910 A CN 201110291910A CN 102373389 A CN102373389 A CN 102373389A
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Abstract
The invention relates to a preparation method of a three-dimensional woven carbon fiber-reinforced magnesium-based composite material. The method comprises the following steps of: (1) removing an organic adhesive layer from the surface of three-dimensional woven carbon fiber; (2) coating a layer of silicon dioxide coating on the surface of the three-dimensional woven carbon fiber with a sol-gel method, wherein the thickness of the silicon dioxide coating is greater than 0.2 micro; and (3) preparing the prepared three-dimensional woven carbon fiber coated with the silicon dioxide coating on the surface into the three-dimensional woven carbon fiber-reinforced magnesium-based composite material with a powder metallurgy method. The three-dimensional woven carbon fiber-reinforced magnesium-based composite material prepared with the method has low density, high specific strength, high plasticity, high toughness and high processing performance; and moreover, the preparation method is simple and practical, has low cost, and can be widely applied to the fields of aerospace, nuclear industry, military equipment, various transport facilities, heavy industry, mechanical industry, light industry and the like.
Description
Technical field
The present invention relates to the functional composite material preparing technical field, especially a kind of 3 D weaving carbon fiber strengthens method of preparing magnesium-based composite material.
Background technology
Resources conservation and environmental friendliness have been the main development trend of current industrial society.Research and development lightweight, high-performance, recyclable energy-saving material cause extensive concern just day by day.Magnesium base alloy in lightweight has low density, high specific strength, high specific stiffness, characteristics such as recyclable.It is one of focus of Recent study.Along with to the increasingly high requirement of light metal high-temperature behavior, single alloy material can not satisfy the demands, and the research viewpoint has turned to matrix material gradually.Thomel becomes important enhancing body in the metal-base composites because of it has excellent mechanical property, low density, high heat conductance, low thermal coefficient of expansion.Carbon fiber reinforced magnesium-base composite material not only has the characteristics of magnesiumalloy low density, high specific strength, high specific stiffness; It is not enough effectively to improve the magnesiumalloy high-temperature behavior; Improve material mechanical performance and heat physical properties, therefore have wide practical use at industrial circles such as automobile, space flight, aviations.
Yet, relatively poor wettability between thomel and the magnesium alloy substrate, make its be shaped and vegetation on have certain degree of difficulty.The preparation carbon fiber reinforced magnesium-base composite material matter of utmost importance that need solve is exactly the wettability of improving between thomel and the magnesiumalloy, and the major technique approach is included in and adds alloying element in the magnesium matrix and carbon fiber surface is carried out coating handle.Yet, the alloying element of adding usually can the fiber surface enrichment and with fiber generation surface reaction, reduce the performance of fiber.Solving the most frequently used effective means of wettability problem is exactly that carbon fiber surface coating is handled; And the mode that adopts suitable coating compounds and coating to handle is to solve the wettability key of problem; Once disclose a kind of copper-plated graphite technology in the prior art and strengthened magnesium base composite material; But this technology is complicated, is not suitable for suitability for industrialized production.
Summary of the invention
The present invention will to propose a kind of 3 D weaving carbon fiber in order solving the problems of the technologies described above and to strengthen method of preparing magnesium-based composite material.
The technical scheme that the present invention adopted is: a kind of 3 D weaving carbon fiber strengthens method of preparing magnesium-based composite material, and its preparation process is:
(1) at first removes the surperficial organic glue-line of 3 D weaving carbon fiber;
(2) adopt sol-gel method at 3 D weaving carbon fiber surface-coated last layer silica dioxide coating, silica dioxide coating thickness is greater than 0.2 micron;
(3) there is 3 D weaving carbon fiber and magnesium alloy substrate compound of silica dioxide coating on the surface: behind the 3 D weaving carbon fiber for preparing the surface-coated silica dioxide coating, adopt powder metallurgic method can prepare 3 D weaving carbon fiber and strengthen magnesium base composite material.
In preferred embodiment of the present invention, the method for organic glue-line on the described removal 3 D weaving carbon fiber of step (1) surface is: 3 D weaving carbon fiber is soaked in the acetone removed photoresist in 5-10 hour.
In preferred embodiment of the present invention; The described sol-gel method of step (2) in the method for 3 D weaving carbon fiber surface-coated last layer silica dioxide coating is: the nitric acid alligatoring carbon fiber surface with 50%; Subsequently fibrage body impregnated in the silicon dioxide gel that configures, dipping 1-2h under vacuum condition takes out dry, sintering then; Sintering temperature is 600-700 ℃, sintering time 1-2 hour.
In preferred embodiment of the present invention, being prepared as of described silicon dioxide gel adopts tetraethoxy to be dissolved in the ethanol, slowly adds deionized water in proportion; Adding hydrolyst concentrated hydrochloric acid accent PH2-3; Add an amount of USP Kosher simultaneously and make dry control chemicaladditives, keep 60 ℃ of constant temperature, through violent stirring 0.5-1h; Make tetraethoxy hydrolysis under acidic conditions; Get silicon dioxide gel, wherein, the mol ratio of tetraethoxy, hydrochloric acid, ethanol, USP Kosher is 1:0.5:1.5:0.8.
In preferred embodiment of the present invention, the 3 D weaving carbon fiber of said step (3) powder metallurgic method compound surface coating silicon dioxide coating and the concrete steps of magnesium alloy substrate are:
(3-1) by volume per-cent coating 3 D weaving carbon fiber 10-30%, magnesium powder 70-90% get the raw materials ready, and magnesium powder for preparing and coating 3 D weaving carbon fiber are put into mixed powder on the ball mill, and ball-to-powder weight ratio is 3-4:1, and rotating speed is 200-300 rev/min, mixes powder 3-6 hour;
The powder that (3-2) step (3-1) is mixed is put into the coldmoulding of stainless steel grinding tool, adopts Triple Pressed Stearic Acid to do lubricant, and pressing pressure is greater than 600MPa, the demoulding after pressurize 1-5 minute;
The compacting sun-dried mud brick that (3-3) step (3-2) is obtained is put into the sintering mold sintering; Adopt graphite as lubricant, sintering temperature is 600-700 ℃, sintering time 1-3 hour; Argon shield cools to the greenhouse with the furnace and promptly prepares 3 D weaving carbon fiber enhancing magnesium base composite material.
In preferred embodiment of the present invention; It is hot-pressed that step (3-3) sintering is obtained 3 D weaving carbon fiber enhancing magnesium base composite material; Extrusion ratio is 10-12:1; Extrusion temperature is 300-400 ℃, and soaking time is 10-20 minute, can prepare the higher 3 D weaving carbon fiber of density and strengthen magnesium base composite material.
Beneficial effect of the present invention is: the present invention will be coated with between 3 D weaving carbon fiber and the magnesium-base alloy material of silica dioxide coating through slight surface reaction; Improved the wettability between the two; Effectively promoted the infiltration process of magnesiumalloy solution in 3 D weaving carbon fiber; Make 3 D weaving carbon fiber enhancing magnesium base composite material and have low density, high specific strength and good plasticity, toughness and processing characteristics; And the preparation method is simple, and is with low cost, can be widely used in fields such as aerospace, nuclear industry and military equipment and various transport facility, heavy industry, mechanical industry, light industry.
Embodiment
A kind of 3 D weaving carbon fiber strengthens method of preparing magnesium-based composite material, and its preparation process is:
(1) at first removes the surperficial organic glue-line of 3 D weaving carbon fiber;
(2) adopt sol-gel method at 3 D weaving carbon fiber surface-coated last layer silica dioxide coating, silica dioxide coating thickness is greater than 0.2 micron;
(3) there is 3 D weaving carbon fiber and magnesium alloy substrate compound of silica dioxide coating on the surface: behind the 3 D weaving carbon fiber for preparing the surface-coated silica dioxide coating, adopt powder metallurgic method can prepare 3 D weaving carbon fiber and strengthen magnesium base composite material.
Wherein, the method for organic glue-line on the described removal 3 D weaving carbon fiber of step (1) surface is: 3 D weaving carbon fiber is soaked in the acetone removed photoresist in 5-10 hour; The described sol-gel method of step (2) in the method for 3 D weaving carbon fiber surface-coated last layer silica dioxide coating is: the nitric acid alligatoring carbon fiber surface with 50% impregnated in fibrage body in the silicon dioxide gel that configures dipping 1-2h under vacuum condition subsequently; Take out dry, sintering then, sintering temperature is 600-700 ℃, sintering time 1-2 hour; Being prepared as of silicon dioxide gel adopts tetraethoxy to be dissolved in the ethanol; Slowly add deionized water in proportion, adding hydrolyst concentrated hydrochloric acid accent PH2-3, add an amount of USP Kosher simultaneously and make dry control chemicaladditives; Keep 60 ℃ of constant temperature; Through violent stirring 0.5-1h, make tetraethoxy hydrolysis under acidic conditions, get silicon dioxide gel; Wherein, the mol ratio of tetraethoxy, hydrochloric acid, ethanol, USP Kosher is 1:0.5:1.5:0.8.
The 3 D weaving carbon fiber of the described powder metallurgic method compound surface of step (3) coating silicon dioxide coating and the concrete steps of magnesium alloy substrate are:
(3-1) by volume per-cent coating 3 D weaving carbon fiber 10-30%, magnesium powder 70-90% get the raw materials ready, and magnesium powder for preparing and coating 3 D weaving carbon fiber are put into mixed powder on the ball mill, and ball-to-powder weight ratio is 3-4:1, and rotating speed is 200-300 rev/min, mixes powder 3-6 hour;
The powder that (3-2) step (3-1) is mixed is put into the coldmoulding of stainless steel grinding tool, adopts Triple Pressed Stearic Acid to do lubricant, and pressing pressure is greater than 600MPa, the demoulding after pressurize 1-5 minute;
The compacting sun-dried mud brick that (3-3) step (3-2) is obtained is put into the sintering mold sintering; Adopt graphite as lubricant, sintering temperature is 600-700 ℃, sintering time 1-3 hour; Argon shield cools to the greenhouse with the furnace and promptly prepares 3 D weaving carbon fiber enhancing magnesium base composite material.
It is hot-pressed step (3-3) sintering to be obtained 3 D weaving carbon fiber enhancing magnesium base composite material; Extrusion ratio is 10-12:1; Extrusion temperature is 300-400 ℃, and soaking time is 10-20 minute, can prepare the higher 3 D weaving carbon fiber of density and strengthen magnesium base composite material.
Introduce the present invention in detail below in conjunction with embodiment.
Embodiment 1
(1) 3 D weaving carbon fiber is soaked in the acetone removed photoresist in 5 hours;
(2) prepare silicon dioxide gel then: adopt tetraethoxy to be dissolved in the ethanol, slowly add deionized water in proportion, adding hydrolyst concentrated hydrochloric acid accent PH2-3; Add an amount of USP Kosher simultaneously and make dry control chemicaladditives, keep 60 ℃ of constant temperature, through violent stirring 0.5h; Make tetraethoxy hydrolysis under acidic conditions; Get silicon dioxide gel, wherein, the mol ratio of tetraethoxy, hydrochloric acid, ethanol, USP Kosher is 1:0.5:1.5:0.8; Adopt sol-gel method at 3 D weaving carbon fiber surface-coated last layer silica dioxide coating again; Silica dioxide coating thickness is 0.3 micron: the nitric acid alligatoring carbon fiber surface with 50%; Subsequently fibrage body impregnated in the silicon dioxide gel that configures, dipping 1h under vacuum condition takes out dry, sintering then; Sintering temperature is 600 ℃, sintering time 2 hours;
(3) 3 D weaving carbon fiber and the magnesium alloy substrate of powder metallurgic method compound surface coating silicon dioxide coating: by volume per-cent coating 3 D weaving carbon fiber 10%, magnesium powder 90% are got the raw materials ready earlier; Magnesium powder for preparing and coating 3 D weaving carbon fiber are put into mixed powder on the ball mill; Ball-to-powder weight ratio is 3:1; Rotating speed is 200 rev/mins, mixes powder 6 hours; Then the powder that mixes is put into the coldmoulding of stainless steel grinding tool, adopt Triple Pressed Stearic Acid to do lubricant, pressing pressure 650MPa, pressurize demoulding after 1 minute; The compacting sun-dried mud brick that will obtain is at last put into the sintering mold sintering, adopts graphite as lubricant, and sintering temperature is 700 ℃, sintering time 1 hour, and argon shield cools to the greenhouse with the furnace and promptly prepares 3 D weaving carbon fiber enhancing magnesium base composite material; It is hot-pressed sintering to be obtained 3 D weaving carbon fiber enhancing magnesium base composite material, and extrusion ratio is 10:1, and extrusion temperature is 300 ℃, and soaking time is 20 minutes, prepares the higher 3 D weaving carbon fiber of density and strengthens magnesium base composite material.
Embodiment 2
(1) 3 D weaving carbon fiber is soaked in the acetone removed photoresist in 10 hours;
(2) prepare silicon dioxide gel then: adopt tetraethoxy to be dissolved in the ethanol, slowly add deionized water in proportion, adding hydrolyst concentrated hydrochloric acid accent PH2-3; Add an amount of USP Kosher simultaneously and make dry control chemicaladditives, keep 60 ℃ of constant temperature, through violent stirring 1h; Make tetraethoxy hydrolysis under acidic conditions; Get silicon dioxide gel, wherein, the mol ratio of tetraethoxy, hydrochloric acid, ethanol, USP Kosher is 1:0.5:1.5:0.8; Adopt sol-gel method at 3 D weaving carbon fiber surface-coated last layer silica dioxide coating again; 0.4 micron of silica dioxide coating thickness: nitric acid alligatoring carbon fiber surface with 50%; Subsequently fibrage body impregnated in the silicon dioxide gel that configures, dipping 2h under vacuum condition takes out dry, sintering then; Sintering temperature is 700 ℃, sintering time 1 hour;
(3) 3 D weaving carbon fiber and the magnesium alloy substrate of powder metallurgic method compound surface coating silicon dioxide coating: by volume per-cent coating 3 D weaving carbon fiber 30%, magnesium powder 70 are got the raw materials ready earlier; Magnesium powder for preparing and coating 3 D weaving carbon fiber are put into mixed powder on the ball mill; Ball-to-powder weight ratio is 4:1; Rotating speed is 200 rev/mins, mixes powder 3 hours; Then the powder that mixes is put into the coldmoulding of stainless steel grinding tool, adopt Triple Pressed Stearic Acid to do lubricant, pressing pressure 700MPa, pressurize demoulding after 3 minutes; The compacting sun-dried mud brick that will obtain is at last put into the sintering mold sintering, adopts graphite as lubricant, and sintering temperature is 600 ℃, sintering time 3 hours, and argon shield cools to the greenhouse with the furnace and promptly prepares 3 D weaving carbon fiber enhancing magnesium base composite material; It is hot-pressed sintering to be obtained 3 D weaving carbon fiber enhancing magnesium base composite material, and extrusion ratio is 12:1, and extrusion temperature is 400 ℃, and soaking time is 10 minutes, can prepare the higher 3 D weaving carbon fiber of density and strengthen magnesium base composite material.
With above-mentioned foundation desirable embodiment of the present invention is enlightenment, and through above-mentioned description, the related work personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the specification sheets, must confirm its technical scope according to the claim scope.
Claims (6)
1. a 3 D weaving carbon fiber strengthens method of preparing magnesium-based composite material, it is characterized in that its preparation process is:
(1) at first removes the surperficial organic glue-line of 3 D weaving carbon fiber;
(2) adopt sol-gel method at 3 D weaving carbon fiber surface-coated last layer silica dioxide coating, silica dioxide coating thickness is greater than 0.2 micron;
(3) there is 3 D weaving carbon fiber and magnesium alloy substrate compound of silica dioxide coating on the surface: behind the 3 D weaving carbon fiber for preparing the surface-coated silica dioxide coating, adopt powder metallurgic method can prepare 3 D weaving carbon fiber and strengthen magnesium base composite material.
2. 3 D weaving carbon fiber according to claim 1 strengthens method of preparing magnesium-based composite material; It is characterized in that the method for organic glue-line on the described removal 3 D weaving carbon fiber of step (1) surface is: 3 D weaving carbon fiber is soaked in the acetone removed photoresist in 5-10 hour.
3. 3 D weaving carbon fiber according to claim 1 strengthens method of preparing magnesium-based composite material; It is characterized in that the described sol-gel method of step (2) in the method for 3 D weaving carbon fiber surface-coated last layer silica dioxide coating is: the nitric acid alligatoring carbon fiber surface with 50% impregnated in fibrage body in the silicon dioxide gel that configures subsequently; Dipping 1-2h under vacuum condition; Take out dry, sintering then, sintering temperature is 600-700 ℃, sintering time 1-2 hour.
4. 3 D weaving carbon fiber according to claim 3 strengthens method of preparing magnesium-based composite material, it is characterized in that, being prepared as of described silicon dioxide gel adopts tetraethoxy to be dissolved in the ethanol; Slowly add deionized water in proportion, adding hydrolyst concentrated hydrochloric acid accent PH2-3, add an amount of USP Kosher simultaneously and make dry control chemicaladditives; Keep 60 ℃ of constant temperature; Through violent stirring 0.5-1h, make tetraethoxy hydrolysis under acidic conditions, get silicon dioxide gel; Wherein, the mol ratio of tetraethoxy, hydrochloric acid, ethanol, USP Kosher is 1:0.5:1.5:0.8.
5. 3 D weaving carbon fiber according to claim 1 strengthens method of preparing magnesium-based composite material; It is characterized in that the 3 D weaving carbon fiber of said step (3) powder metallurgic method compound surface coating silicon dioxide coating and the concrete steps of magnesium alloy substrate are:
(3-1) by volume per-cent coating 3 D weaving carbon fiber 10-30%, magnesium powder 70-90% get the raw materials ready, and magnesium powder for preparing and coating 3 D weaving carbon fiber are put into mixed powder on the ball mill, and ball-to-powder weight ratio is 3-4:1, and rotating speed is 200-300 rev/min, mixes powder 3-6 hour;
The powder that (3-2) step (3-1) is mixed is put into the coldmoulding of stainless steel grinding tool, adopts Triple Pressed Stearic Acid to do lubricant, and pressing pressure is greater than 600MPa, the demoulding after pressurize 1-5 minute;
The compacting sun-dried mud brick that (3-3) step (3-2) is obtained is put into the sintering mold sintering; Adopt graphite as lubricant, sintering temperature is 600-700 ℃, sintering time 1-3 hour; Argon shield cools to the greenhouse with the furnace and promptly prepares 3 D weaving carbon fiber enhancing magnesium base composite material.
6. 3 D weaving carbon fiber according to claim 5 strengthens method of preparing magnesium-based composite material; It is characterized in that; It is hot-pressed that step (3-3) sintering is obtained 3 D weaving carbon fiber enhancing magnesium base composite material, and extrusion ratio is 10-12:1, and extrusion temperature is 300-400 ℃; Soaking time is 10-20 minute, can prepare the higher 3 D weaving carbon fiber of density and strengthen magnesium base composite material.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103272365A (en) * | 2013-06-24 | 2013-09-04 | 北京联合大学 | Prone type mechanical body building device, material adopted for same and preparation method for material |
| CN105478683A (en) * | 2015-12-08 | 2016-04-13 | 天津航天机电设备研究所 | Carbon fiber reinforced Mg-base composite hollow pipe and preparation method thereof |
| CN107245678A (en) * | 2017-04-12 | 2017-10-13 | 芜湖扬展新材料科技服务有限公司 | A kind of magnesium alloy |
| CN108853587A (en) * | 2017-05-10 | 2018-11-23 | 上海交通大学 | Magnesium alloy and macromolecule silk material shuffling composite patch and application thereof |
| CN108853608A (en) * | 2017-05-10 | 2018-11-23 | 上海交通大学 | A kind of biodegradable medical magnesium alloy sticking patch and its preparation method and application |
| CN110172652A (en) * | 2019-06-17 | 2019-08-27 | 江仁燕 | A kind of chopped carbon fiber enhancing Mg-Al-Li system alloy-base composite material |
| CN111013248A (en) * | 2019-12-26 | 2020-04-17 | 山东国大黄金股份有限公司 | Preparation method of carbon fiber filter plate |
| CN111155038A (en) * | 2020-02-13 | 2020-05-15 | 上海交通大学 | Preparation method of chopped carbon fiber reinforced magnesium-based composite material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103272365A (en) * | 2013-06-24 | 2013-09-04 | 北京联合大学 | Prone type mechanical body building device, material adopted for same and preparation method for material |
| CN105478683A (en) * | 2015-12-08 | 2016-04-13 | 天津航天机电设备研究所 | Carbon fiber reinforced Mg-base composite hollow pipe and preparation method thereof |
| CN105478683B (en) * | 2015-12-08 | 2018-04-20 | 天津航天机电设备研究所 | A kind of carbon fiber reinforced magnesium-base composite material hollow pipe and preparation method thereof |
| CN107245678A (en) * | 2017-04-12 | 2017-10-13 | 芜湖扬展新材料科技服务有限公司 | A kind of magnesium alloy |
| CN108853587A (en) * | 2017-05-10 | 2018-11-23 | 上海交通大学 | Magnesium alloy and macromolecule silk material shuffling composite patch and application thereof |
| CN108853608A (en) * | 2017-05-10 | 2018-11-23 | 上海交通大学 | A kind of biodegradable medical magnesium alloy sticking patch and its preparation method and application |
| CN110172652A (en) * | 2019-06-17 | 2019-08-27 | 江仁燕 | A kind of chopped carbon fiber enhancing Mg-Al-Li system alloy-base composite material |
| CN111013248A (en) * | 2019-12-26 | 2020-04-17 | 山东国大黄金股份有限公司 | Preparation method of carbon fiber filter plate |
| CN111013248B (en) * | 2019-12-26 | 2021-10-26 | 山东国大黄金股份有限公司 | Preparation method of carbon fiber filter plate |
| CN111155038A (en) * | 2020-02-13 | 2020-05-15 | 上海交通大学 | Preparation method of chopped carbon fiber reinforced magnesium-based composite material |
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Application publication date: 20120314 |