CN102041420B - Magnesium-aluminum-titanium-carbon intermediate alloy and preparation method thereof - Google Patents
Magnesium-aluminum-titanium-carbon intermediate alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a magnesium-aluminum-titanium-carbon intermediate alloy which comprises the following chemical components in percentage by weight: 65.00-98.00% of Mg, 1.00-13.00% of Al, 0.40-12.00% of Ti and 0.60-10.00% of C. The preparation course provided by the invention can be finished at quite low temperature, the absorption rate of the carbon is high, and the reaction is complete. Meanwhile, the presence of the titanium carbide can ensure that the main nucleation phase aluminum carbide is formed by being attached on the surface of the titanium carbide, and thus, the intermediate alloy is finer and the distribution is more uniform. The method provided by the invention has the characteristics of high production efficiency, low cost, good refinement effect of the prepared magnesium-aluminum-titanium-carbon intermediate alloy and the like, and is suitable for mass production and application.
Description
Technical field
The present invention relates to a kind of magnesium-aluminium-titanium-carbon master alloy preparation method who is used for refinement magnesium-aluminum alloy crystal grain, belong to technical field of alloy material.
Background technology
Magnesium and alloy thereof have broad application prospects in industrial production owing to have characteristics such as low density, high specific tenacity and specific rigidity, and magnesium-aluminum alloy maximum a kind of magnesiumalloy that is current application.The subject matter that this alloy faces in application process is that its plasticity and toughness are relatively poor, is difficult to forging molding.Address this problem to become and promote one of magnesiumalloy key in application problem; And the crystal grain of refinement magnesiumalloy can effectively improve its plastic deformation ability, also improve performances such as its tensile strength and erosion resistance simultaneously, and therefore the research to the magnesium-aluminum alloy refinement is the important topic that Chinese scholars is extremely paid close attention to always.Current, the thinning method of magnesium-aluminum alloy mainly is to add carbon refinement method, but because the wettability between main source of carbon-graphite and the magnesium is relatively poor, the alloying difficulty, for a long time, with low cost, respond well carbon containing magnesium alloy refiner fails to succeed in developing always.Therefore the insider attempts coming the refinement magnesium-aluminum alloy with the method that adds gaseous carbon sources or carbon containing salt; As add gases such as dry acetylene, carbonic acid gas, Sweet natural gas; Carbonate such as lime carbonate, magnesiumcarbonate, organism such as tetracol phenixin, Sesquichloratum, Perchlorobenzene etc.But the subject matter of these adding methods is that the carbon specific absorption is low, thinning effect is unstable and easy contaminate environment.Document (" Special Processes of Metal Castings and non-ferrous alloy "; 2006; 26 (9): P598-600) reported a kind of method with Sesquichloratum refinement magnesium-aluminum alloy, the shortcoming of this method is to use toxic gases such as can producing chlorinated hydrocarbon in the process, and deterroration is had relatively high expectations.Document (" casting equipment research ", 2003, (4): P16-17 P43) has reported that the characteristics of this method are that the adding of fining agent is more easy to operate with the method for MgCO3 and La2 (CO3) 3 refinement magnesium-aluminum alloys, shortcoming is to be easy to generate the salt slag, pollutes alloy.Document (" Materials Transaction "; 2003,44 (1): P107-110) reported the method that sprays into pure Graphite Powder 99 refinement magnesiumalloy with the argon gas pulse, the shortcoming of this method is that the carbon specific absorption is low; Thinning effect is relatively poor, and aggravates the oxidization burning loss of magnesium easily.
Summary of the invention
The present invention be used to solve the defective of above-mentioned prior art and provide that a kind of cost is low, technology is simple, the effective magnesium-aluminium-titanium-carbon master alloy preparation method of refinement magnesium-aluminum alloy crystal grain.
The alleged problem of the present invention solves through following technical scheme:
A kind of magnesium-aluminium-titanium-carbon master alloy, its chemical ingredients (wt%) are by weight percentage counted:
Mg 65.00-98.00，
Al 1.00-13.00，
Ti 0.40-12.00，
C 0.60-10.00。
A kind of method for preparing above-mentioned magnesium-aluminium-titanium-carbon master alloy, it is undertaken by following step:
A. raw material is prepared: prepare raw material according to following mass percent: carbonized titanium powder 0.50%-15.00%, and Graphite Powder 99 0.50%-7.00%, aluminium powder 1.00%-13.00%, surplus are pure magnesium, wherein used titanium carbide granularity is between 5～15 microns;
B. mixing and ball milling: with carbonized titanium powder that takes by weighing and Graphite Powder 99 uniform mixing, mixed powder is placed high energy ball mill ball milling 10-30 hour under the argon shield, to the titanium carbide particle diameter between 300 nanometers to 1.5 micron;
C. prepare the carbon source piece:, subsequent use as the carbon source piece with briquetting behind the aluminium powder uniform mixing of the titanium carbide behind the above-mentioned ball milling and graphite mixed powder and proportional quantity;
D. prepare alloy: the pure magnesium of proportional quantity is placed resistance furnace and under the magnesium alloy covering agent protection, is heated to 700-900 ℃; Pure magnesium is melted fully; The carbon source piece for preparing among the step c is pressed in the magnesium solution kept 1-5 minute; Then liquation is continued insulation 10-20 minute, casting ingot-forming is promptly processed magnesium-aluminium-titanium-carbon master alloy.
The inventive method becomes piece as carbon source with the powder compression of titanium carbide and graphite mixing and ball milling gained, prepares the magnesium-aluminium-titanium-carbon master alloy that is used for the refinement magnesium-aluminum alloy.The advantage of this method is: after titanium carbide and the graphite mixing and ball milling, the titanium carbide ball milling is a fine particle, and graphite evenly is coated on the surface of titanium carbide with the form of decolorizing carbon.Because the powder activity behind the ball milling is higher; After being mixed to join in the low temperature magnesium alloy fused mass with an amount of aluminium powder; The decolorizing carbon that is coated on titanium carbide surface can be rapidly and reactive aluminum generation aluminium carbide, and the aluminium carbide that is generated still can be attached to tiny titanium carbide particle surperficial, and along with the diffusion of titanium carbide in melt; Be distributed in equably in the whole melt, prevented that effectively the gathering of aluminium carbide from growing up.Whole process of preparation can be carried out under lower temperature, and the specific absorption of carbon is high, reacts completely, and the aluminium carbide of generation is tiny and be evenly distributed.The inventive method has characteristics such as production efficiency height, cost magnesium-aluminium-titanium-carbon master alloy refinement magnesium-aluminum alloy crystal grain low, preparation is respond well, is fit to scale operation and application.
Embodiment
Several concrete embodiment below are provided:
Embodiment 1: prepare raw material by following mass percent: 1.00% carbonized titanium powder, 0.50% Graphite Powder 99,3.00% aluminium powder, surplus be pure magnesium, wherein used titanium carbide granularity is 5 microns; Get carbonized titanium powder and Graphite Powder 99 uniform mixing in the raw material, mixed powder placed the high energy ball mill ball milling 10 hours under the argon shield, to the titanium carbide median size be 500 nanometers; With being pressed into 5 centimetres of diameters, high 2 centimetres cylindrical piece behind the titanium carbide behind the ball milling and graphite mixed powder and the proportional quantity aluminium powder uniform mixing, subsequent use as the carbon source piece; The pure magnesium of proportional quantity placed resistance furnace and under magnesium alloy covering agent protection, be heated to 700 ℃ of pure magnesium melt fully; Be pressed into the carbon source piece in the magnesium melt and kept 2 minutes with graphite rod; Then liquation is continued insulation 12 minutes, casting ingot-forming promptly obtains magnesium-aluminium-titanium-carbon master alloy.The composition of prepared magnesium-aluminium-titanium-carbon master alloy is following:
Component content (wt%)
Magnesium (Mg) 95.50,
Aluminium (Al) 3.00,
Titanium (Ti) 0.80,
Carbon (C) 0.70.
Embodiment 2: prepare raw material by following mass percent: 0.50% carbonized titanium powder, 0.50% Graphite Powder 99,1.00% aluminium powder, surplus be pure magnesium, wherein used titanium carbide granularity is 5 microns; Get carbonized titanium powder and Graphite Powder 99 uniform mixing in the raw material, mixed powder placed the high energy ball mill ball milling 15 hours under the argon shield, to the titanium carbide median size be 300 nanometers; With being pressed into 5 centimetres of diameters, high 2 centimetres cylindrical piece behind the titanium carbide behind the ball milling and graphite mixed powder and the proportional quantity aluminium powder uniform mixing, subsequent use as the carbon source piece; The pure magnesium of proportional quantity placed resistance furnace and under insulating covering agent (used insulating covering agent is general magnesium alloy covering agent) protection, be heated to 750 ℃ of pure magnesium melt fully; Be pressed into the carbon source piece in the magnesium melt and kept 1 minute with graphite rod; Then liquation is continued insulation 10 minutes; Casting ingot-forming promptly obtains magnesium-aluminium-titanium-carbon master alloy.The composition of prepared magnesium-aluminium-titanium-carbon master alloy is following:
Component content (wt%)
Magnesium (Mg) 98.00,
Aluminium (Al) 1.00,
Titanium (Ti) 0.40,
Carbon (C) 0.60.
Embodiment 3: prepare raw material by following mass percent: 15.00% carbonized titanium powder, 7% Graphite Powder 99,13.00% aluminium powder, surplus be pure magnesium, wherein used titanium carbide granularity is 15 microns; Get carbonized titanium powder and Graphite Powder 99 uniform mixing in the raw material, mixed powder placed the high energy ball mill ball milling 30 hours under the argon shield, to the titanium carbide median size be 1.5 microns; With being pressed into 5 centimetres of diameters, high 4 centimetres cylindrical piece behind the titanium carbide behind the ball milling and graphite mixed powder and the proportional quantity aluminium powder uniform mixing, subsequent use as the carbon source piece; The pure magnesium of proportional quantity placed resistance furnace and under magnesium alloy covering agent protection, be heated to 900 ℃ of pure magnesium melt fully; Be pressed into the carbon source piece in the magnesium melt and kept 5 minutes with graphite rod; Then liquation is continued insulation 20 minutes, casting ingot-forming promptly obtains magnesium-aluminium-titanium-carbon master alloy.The composition of prepared magnesium-aluminium-titanium-carbon master alloy is following:
Component content (wt%)
Magnesium (Mg) 65.00,
Aluminium (Al) 13.00,
Titanium (Ti) 12.00,
Carbon (C) 10.00.
Embodiment 4: prepare raw material by following mass percent: 5.00% carbonized titanium powder, 1.00% Graphite Powder 99,6.00% aluminium powder, surplus be pure magnesium, wherein used titanium carbide granularity is 7 microns; Get carbonized titanium powder and Graphite Powder 99 uniform mixing in the raw material, mixed powder placed the high energy ball mill ball milling 20 hours under the argon shield, to the titanium carbide median size be 1 micron; With being pressed into 5 centimetres of diameters, high 3 centimetres cylindrical piece behind the titanium carbide behind the ball milling and graphite mixed powder and the proportional quantity aluminium powder uniform mixing, subsequent use as the carbon source piece; The pure magnesium of proportional quantity placed resistance furnace and under magnesium alloy covering agent protection, be heated to 800 ℃ of pure magnesium melt fully; Be pressed into the carbon source piece in the magnesium melt and kept 4 minutes with graphite rod; Then liquation is continued insulation 17 minutes, casting ingot-forming promptly obtains magnesium-aluminium-titanium-carbon master alloy.The composition of prepared magnesium-aluminium-titanium-carbon master alloy is following:
Component content (wt%)
Magnesium (Mg) 88.00,
Aluminium (Al) 6.00,
Titanium (Ti) 4.00,
Carbon (C) 2.00.
Embodiment 5: prepare raw material by following mass percent: 10.00% carbonized titanium powder, 4.00% Graphite Powder 99,12.00% aluminium powder, surplus be pure magnesium, wherein used titanium carbide granularity is 10 microns; Get carbonized titanium powder and Graphite Powder 99 uniform mixing in the raw material, mixed powder placed the high energy ball mill ball milling 25 hours under the argon shield, to the titanium carbide median size be 1 micron; With being pressed into 5 centimetres of diameters, high 4 centimetres cylindrical piece behind the titanium carbide behind the ball milling and graphite mixed powder and the proportional quantity aluminium powder uniform mixing, subsequent use as the carbon source piece; The pure magnesium of proportional quantity placed resistance furnace and under magnesium alloy covering agent protection, be heated to 850 ℃ of pure magnesium melt fully; Be pressed into the carbon source piece in the magnesium melt and kept 5 minutes with graphite rod; Then liquation is continued insulation 20 minutes, casting ingot-forming promptly obtains magnesium-aluminium-titanium-carbon master alloy.The composition of prepared magnesium-aluminium-titanium-carbon master alloy is following:
Component content (wt%)
Magnesium (Mg) 74.00,
Aluminium (Al) 12.00,
Titanium (Ti) 8.00,
Carbon (C) 6.00.
Claims (1)
1. method for preparing magnesium-aluminium-titanium-carbon master alloy is characterized in that it carries out as follows:
A. raw material is prepared: prepare raw material according to following mass percent: carbonized titanium powder 0.50%-15.00%, and Graphite Powder 99 0.5%-7.00%, aluminium powder 1.00%-13.00%, surplus are pure magnesium, wherein used titanium carbide granularity is between 5 microns to 15 microns;
B. mixing and ball milling: with carbonized titanium powder that takes by weighing and Graphite Powder 99 uniform mixing, mixed powder is placed high energy ball mill ball milling 10-30 hour under the argon shield, be 300 nanometers to 1.5 micron to the titanium carbide median size between;
C. prepare the carbon source piece:, subsequent use as the carbon source piece with briquetting behind the aluminium powder uniform mixing of the titanium carbide behind the above-mentioned ball milling and graphite mixed powder and proportional quantity;
D. prepare alloy: the pure magnesium of proportional quantity is placed resistance furnace and under the magnesium alloy covering agent protection, is heated to 700-900 ℃; Pure magnesium is melted fully; The carbon source piece for preparing among the step c is pressed in the magnesium solution kept 1-5 minute; Then liquation is continued insulation 10-20 minute, casting ingot-forming is promptly processed magnesium-aluminium-titanium-carbon master alloy;
The chemical ingredients of the said magnesium of processing-aluminium-titanium-carbon master alloy (wt%) is by weight percentage counted:
Mg 65.00-98.00，
Al 1.00-13.00，
Ti 0.40-12.00，
C 0.60-10.00。
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| CN105369095A (en) * | 2015-10-09 | 2016-03-02 | 天长市兴宇铸造有限公司 | Nano titanium carbide modified Mg-Al-Ca series magnesium alloy material for casting of automobile part and preparation method of nano titanium carbide modified Mg-Al-Ca series magnesium alloy material |
| CN106148787B (en) * | 2016-08-22 | 2019-06-21 | 上海交通大学 | Magnesium lithium alloy and preparation method thereof suitable for sand casting |
| CN108048677A (en) * | 2017-11-28 | 2018-05-18 | 仝仲盛 | The production method of the magnesium alloy of crystal grain refinement |
| CN109518027B (en) * | 2018-12-03 | 2020-10-09 | 河北工业大学 | Preparation method and application of fine-grain Mg-Al-Ti-C intermediate alloy |
| CN111155010A (en) * | 2020-01-16 | 2020-05-15 | 深圳市新星轻合金材料股份有限公司 | Preparation method of magnesium-aluminum-titanium alloy |
| CN111118362A (en) * | 2020-01-16 | 2020-05-08 | 深圳市新星轻合金材料股份有限公司 | Preparation method of magnesium-aluminum-titanium-niobium alloy |
| CN111155009A (en) * | 2020-01-16 | 2020-05-15 | 深圳市新星轻合金材料股份有限公司 | Preparation method of magnesium-aluminum-titanium-chromium alloy |
| CN111235415A (en) * | 2020-01-16 | 2020-06-05 | 深圳市新星轻合金材料股份有限公司 | Preparation method of magnesium-aluminum-titanium-vanadium alloy |
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| CN1290760A (en) * | 2000-10-20 | 2001-04-11 | 山东大学 | Method for preparing aluminium-titanium-carbon intermediate alloy |
| CN1865473A (en) * | 2006-06-22 | 2006-11-22 | 山东大学 | Nickel-silicon-boron intermediate alloy and process for preparing same |
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| JP5089945B2 (en) * | 2006-09-14 | 2012-12-05 | 国立大学法人 熊本大学 | High strength magnesium alloy with high corrosion resistance |
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| CN1290760A (en) * | 2000-10-20 | 2001-04-11 | 山东大学 | Method for preparing aluminium-titanium-carbon intermediate alloy |
| CN1865473A (en) * | 2006-06-22 | 2006-11-22 | 山东大学 | Nickel-silicon-boron intermediate alloy and process for preparing same |
Non-Patent Citations (2)
| Title |
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| JP特开2008-69418A 2008.03.27 |
| 柳延辉等.Al-Ti-C中间合金对Mg-Al合金的晶粒细化作用.《中国有色金属学报》.2003,第13卷(第3期),第622-625页. * |
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