CN103233137A - In-situ SiC particle reinforced Ti6Al4V preparation method - Google Patents

In-situ SiC particle reinforced Ti6Al4V preparation method Download PDF

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CN103233137A
CN103233137A CN2013101747224A CN201310174722A CN103233137A CN 103233137 A CN103233137 A CN 103233137A CN 2013101747224 A CN2013101747224 A CN 2013101747224A CN 201310174722 A CN201310174722 A CN 201310174722A CN 103233137 A CN103233137 A CN 103233137A
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powder
total mass
alloy powder
mother alloy
titanium valve
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CN103233137B (en
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张小立
王志新
张瑞杰
刘红燕
刘�英
张照军
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Zhongyuan University of Technology
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Zhongyuan University of Technology
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Abstract

The invention discloses an in-situ SiC particle reinforced Ti6Al4V preparation method. The method comprises the following steps: (1) putting Si powder and C powder into high-energy grinding equipment for mechanical alloying, grinding for 8-48 hours, wherein the mass ratio of the Si powder to the C powder is (2-3):1, then adding SiO2 powder which accounts for 5-20% of the total mass of the Si powder and the C powder, and further grinding for 4-10 hours to obtain a mixed material; (2) uniformly mixing titanium powder, master alloy powder and the mixed material, wherein the addition amount of the titanium powder accounts for 80-95% of the total mass of the titanium powder and the master alloy powder, the addition amount of the master alloy powder accounts for 5-20% of the total mass of the titanium powder and the master alloy powder, the addition amount of the mixed material accounts for 5-40% of the titanium powder and the master alloy powder, and compression molding to produce blanks; and (3) sintering the blanks in a vacuum sintering furnace for two stages at 700-900 DEG C for 0.5-3 hours, then heating to be 1300-1500 DEG C and sintering in an argon atmosphere for 0.5-3 hours. The reinforcement phase of a composite material obtained by the method is produced in situ, interfaces are densely connected together, and the composite material has high strength and is suitable for industrial scale.

Description

A kind of original position SiC particle strengthens the preparation method of Ti6Al4V
Technical field
The present invention relates to the new technology of preparing of SiC-Ti6Al4V, improve the technical field of intensity.
Background technology
Ti6Al4V has the specific tenacity height, heat resistance is good, anti-corrosion and advantage such as good biocompatibility, successfully be used for fields such as aerospace, petrochemical complex, biologic medical, but the shortcoming that it wears no resistance and adhesion easily takes place, limited its application, thereby development SiC reinforced composite is necessary selection.
Ti6Al4V alloy components with casting and forging manufacturing technique preparation successfully has been applied in high-tech sector, as military and airframe structure spare business aircraft.But, with forging and castmethod is produced titanium alloy, owing to complex process, lumber recovery is low, product cost is high and following process is difficult, hindered it and used more widely.The research of powder metallurgy titanium alloy starts from the 50's of 20th century.(Pre-alloying PA) prepares titanium alloy, but production cost still shows expensive for civil area, and its application is restricted to adopt the prealloy method the earliest.In the later stage the 80's of 20th century, (Blending elements, BE) the preparation titanium alloy is developed the complex element method faster.
SiC fiber reinforcement titanium matrix composite can keep fatigue and creep property preferably owing to have higher specific tenacity and specific rigidity in the time of 600-1000 ℃ at present, becomes the research focus of aeronautical material.But surface reaction takes place in this matrix material easily between fiber and the matrix in moulding and high temperature use, can cause mechanical property to have a strong impact on.Secondly, the thermal expansivity of titanium alloy substrate and SiC fiber differs greatly, and composite material interface will produce very big residual thermal stress.
Summary of the invention
The objective of the invention is to overcome that phenomenon such as weak connections of crystal boundary, composite material strength reduction appears in existing SiC-Ti6Al4V easily and the original position SiC enhancing Ti6Al4V matrix material that carries out.Use the Si powder of titanium valve, mother alloy powder, an amount of mechanical alloying and C powder, an amount of SiO 2Powder, mold pressing, vacuum sintering obtain original position SiC and strengthen titanium alloy.Can produce continuously, be applicable to technical scale.
A kind of original position SiC particle strengthens the preparation method of Ti6Al4V, and its step is as follows: (1) is put into high energy milling equipment with Si powder and C powder and is carried out mechanical alloying, grinds 8-48 hour, and the mass ratio of Si powder and C powder is 2-3:1, adds SiO then 2Powder, SiO 2The add-on of powder is the 5-20% of Si powder and C powder total mass, continues grinding and obtains compound in 4-10 hour; (2) compound in titanium valve, mother alloy powder 60Al40V and the step (1) is evenly mixed, the add-on of titanium valve is the 80-95% of titanium valve and mother alloy powder total mass, the add-on of mother alloy powder is the 5-20% of titanium valve and mother alloy powder total mass, compound add-on be the 5-40% of titanium valve and mother alloy powder total mass, blank is made in compression molding; (3) blank in the step (2) is carried out two stage sintering in vacuum sintering furnace, at 700-900 ℃ of sintering 0.5-3 hour, be warming up to 1300-1500 ℃ then, in argon atmospher sintering 0.5-3 hour.
Si powder in the described step (1), C powder, SiO 2The order number of powder is the 300-500 order.
Titanium valve in the described step (2), the order number of mother alloy powder are the 300-500 order.
In the described step (2) compound add-on be the 20-30% of titanium valve and mother alloy powder total mass.
The vacuum sintering furnace bottom is covered with the Si powder in the described step (3), and the quality of Si powder is the 3-8 % of blank quality.
Generate SiC particle wild phase by original position in the Ti6Al4V matrix, can eliminate the weak connection at interface fully, eliminate unrelieved stress, obtain ultimate compression strength and reach the 22-35MPa titanium matrix composite.Make C powder and the mechanical alloying of Si powder earlier, add SiO then 2Continue high energy milling, above mixed powder adds titanium valve and the mother alloy powder mixes the back compression molding, obtains the granule intensified titanium alloy of advantages of higher compressive strength performance after the vacuum double sintering.This method gained matrix material wild phase original position generates, and the interface connects closely, intensity improves, be fit to technical scale.
Embodiment
Embodiment 1
A kind of original position SiC particle strengthens the preparation method of Ti6Al4V, and its step is as follows: (1) is put into high energy milling equipment with Si powder and C powder and is carried out mechanical alloying, grinds 48 hours, and the mass ratio of Si powder and C powder is 2:1, adds SiO then 2Powder, SiO 2The add-on of powder is 20% of Si powder and C powder total mass, continues grinding and obtains compound in 10 hours; (2) compound in titanium valve, mother alloy powder and the step (1) is evenly mixed, the add-on of titanium valve is 95% of titanium valve and mother alloy powder total mass, the add-on of mother alloy powder is 5% of titanium valve and mother alloy powder total mass, compound add-on be 5% of titanium valve and mother alloy powder total mass, blank is made in compression molding; (3) blank in the step (2) is carried out two stage sintering in vacuum sintering furnace, 700 ℃ of sintering 0.5 hour, be warming up to 1300 ℃ then, sintering is 0.5 hour in argon atmospher.Test sample ultimate compression strength reaches 23MPa.
Embodiment 2
A kind of original position SiC particle strengthens the preparation method of Ti6Al4V, and its step is as follows: (1) is put into high energy milling equipment with Si powder and C powder and is carried out mechanical alloying, grinds 8 hours, and the mass ratio of Si powder and C powder is 3:1, adds SiO then 2Powder, SiO 2The add-on of powder is 5% of Si powder and C powder total mass, continues grinding and obtains compound in 10 hours; (2) compound in titanium valve, mother alloy powder and the step (1) is evenly mixed, the add-on of titanium valve is 80% of titanium valve and mother alloy powder total mass, the add-on of mother alloy powder is 15% of titanium valve and mother alloy powder total mass, compound add-on be 20% of titanium valve and mother alloy powder total mass, blank is made in compression molding; (3) blank in the step (2) is carried out two stage sintering in vacuum sintering furnace, at 800 ℃ of sintering 0.5-3 hours, be warming up to 1400 ℃ then, sintering is 2 hours in argon atmospher.Test sample ultimate compression strength reaches 25MPa.
Embodiment 3
A kind of original position SiC particle strengthens the preparation method of Ti6Al4V, and its step is as follows: (1) is put into high energy milling equipment with Si powder and C powder and is carried out mechanical alloying, grinds 30 hours, and the mass ratio of Si powder and C powder is 2.5:1, adds SiO then 2Powder, SiO 2The add-on of powder is 15% of Si powder and C powder total mass, continues grinding and obtains compound in 8 hours; (2) compound in titanium valve, mother alloy powder and the step (1) is evenly mixed, the add-on of titanium valve is 90% of titanium valve and mother alloy powder total mass, the add-on of mother alloy powder is 10% of titanium valve and mother alloy powder total mass, compound add-on be 30% of titanium valve and mother alloy powder total mass, blank is made in compression molding; (3) blank in the step (2) is carried out two stage sintering in vacuum sintering furnace, 800 ℃ of sintering 2 hours, be warming up to 1400 ℃ then, sintering is 2 hours in argon atmospher.Test sample ultimate compression strength reaches 24MPa.
Embodiment 4
A kind of original position SiC particle strengthens the preparation method of Ti6Al4V, and its step is as follows: (1) is put into high energy milling equipment with Si powder and C powder and is carried out mechanical alloying, grinds 35 hours, and the mass ratio of Si powder and C powder is 3:1, adds SiO then 2Powder, SiO 2The add-on of powder is 15% of Si powder and C powder total mass, continues grinding and obtains compound in 6 hours; (2) compound in titanium valve, mother alloy powder and the step (1) is evenly mixed, the add-on of titanium valve is 85% of titanium valve and mother alloy powder total mass, the add-on of mother alloy powder is 20% of titanium valve and mother alloy powder total mass, compound add-on be 20% of titanium valve and mother alloy powder total mass, blank is made in compression molding; (3) blank in the step (2) is carried out two stage sintering in vacuum sintering furnace, 900 ℃ of sintering 2 hours, be warming up to 1500 ℃ then, sintering is 1 hour in argon atmospher.
Embodiment 5
5g titanium valve, 1g mother alloy powder are evenly mixed; Si powder and C powder high energy milling 40 hours add SiO 2 powder and continue to grind 4 hours, take out and take by weighing 1.6g, and evenly mix with the titanium alloy powder.Above compound is pressed into the blank of 5 * 5 * 40mm, moves in the vacuum sintering furnace that is covered with a small amount of silica flour in 900 ℃ of insulations 1 hour, is warming up to 1350 ℃ then and feeds argon gas insulation 1.5 hours.Test sample ultimate compression strength reaches 22MPa.
Embodiment 6
5g titanium valve, 1g mother alloy powder are evenly mixed; Si powder and C powder high energy milling 40 hours add SiO 2 powder and continue to grind 4 hours, take out and take by weighing 2g, and evenly mix with the titanium alloy powder.Above compound is pressed into the blank of 5 * 5 * 40mm, moves in the vacuum sintering furnace that is covered with a small amount of silica flour in 800 ℃ of insulations 1 hour, is warming up to 1400 ℃ then and feeds argon gas insulation 1.0 hours.Test sample ultimate compression strength reaches 25MPa.
In above-described embodiment, the Si powder in the step (1), C powder, SiO 2The order number of powder is the 300-500 order, titanium valve in the step (2), the order number of mother alloy powder are the 300-500 order, in the step (2) compound add-on be the 20-30% of titanium valve and mother alloy powder total mass, the vacuum sintering furnace bottom is covered with the Si powder in the step (3), and the quality of Si powder is the 3-8 % of blank quality.

Claims (5)

1. an original position SiC particle strengthens the preparation method of Ti6Al4V, it is characterized in that its step is as follows: (1) is put into high energy milling equipment with Si powder and C powder and is carried out mechanical alloying, grinds 8-48 hour, the mass ratio of Si powder and C powder is 2-3:1, adds SiO then 2Powder, SiO 2The add-on of powder is the 5-20% of Si powder and C powder total mass, continues grinding and obtains compound in 4-10 hour;
(2) compound in titanium valve, mother alloy powder and the step (1) is evenly mixed, the add-on of titanium valve is the 80-95% of titanium valve and mother alloy powder total mass, the add-on of mother alloy powder is the 5-20% of titanium valve and mother alloy powder total mass, compound add-on be the 5-40% of titanium valve and mother alloy powder total mass, blank is made in compression molding;
(3) blank in the step (2) is carried out two stage sintering in vacuum sintering furnace, at 700-900 ℃ of sintering 0.5-3 hour, be warming up to 1300-1500 ℃ then, in argon atmospher sintering 0.5-3 hour.
2. original position SiC particle according to claim 1 strengthens the preparation method of Ti6Al4V, it is characterized in that: the Si powder in the described step (1), C powder, SiO 2The order number of powder is the 300-500 order.
3. original position SiC particle according to claim 1 strengthens the preparation method of Ti6Al4V, and it is characterized in that: the titanium valve in the described step (2), the order number of mother alloy powder are the 300-500 order.
4. original position SiC particle according to claim 1 strengthens the preparation method of Ti6Al4V, it is characterized in that: in the described step (2) compound add-on be the 20-30% of titanium valve and mother alloy powder total mass.
5. original position SiC particle according to claim 1 strengthens the preparation method of Ti6Al4V, it is characterized in that: the vacuum sintering furnace bottom is covered with the Si powder in the described step (3), and the quality of Si powder is the 3-8 % of blank quality.
CN201310174722.4A 2013-05-13 2013-05-13 In-situ SiC particle reinforced Ti6Al4V preparation method Expired - Fee Related CN103233137B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107904439A (en) * 2017-11-16 2018-04-13 淮阴工学院 A kind of in-situ nano multiphase composite toughening titanium matrix composite and preparation method thereof
CN111485141A (en) * 2020-06-05 2020-08-04 天钛隆(天津)金属材料有限公司 SiC particle reinforced aluminum titanium matrix composite material and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01282164A (en) * 1988-05-07 1989-11-14 Kobe Steel Ltd Joined body of ceramics and metal
JP2005089807A (en) * 2003-09-16 2005-04-07 Univ Nihon Fiber reinforced composite material comprising metal reinforced fiber and titanium or titanium alloy, and its manufacturing method by spark plasma sintering (sps) method
CN1900333A (en) * 2006-07-25 2007-01-24 霍宏伟 Method for in-situ synthesizing metal base composite material
CN101306501A (en) * 2008-07-07 2008-11-19 盐城市鑫洋电热合金厂 Preparation method of high intensity Ti6Al4V diphase reinforced composite material
CN102864336A (en) * 2012-09-27 2013-01-09 苏州东海玻璃模具有限公司 In situ synthesis TiC particle reinforced titanium-aluminum-vanadium alloy material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01282164A (en) * 1988-05-07 1989-11-14 Kobe Steel Ltd Joined body of ceramics and metal
JP2005089807A (en) * 2003-09-16 2005-04-07 Univ Nihon Fiber reinforced composite material comprising metal reinforced fiber and titanium or titanium alloy, and its manufacturing method by spark plasma sintering (sps) method
CN1900333A (en) * 2006-07-25 2007-01-24 霍宏伟 Method for in-situ synthesizing metal base composite material
CN101306501A (en) * 2008-07-07 2008-11-19 盐城市鑫洋电热合金厂 Preparation method of high intensity Ti6Al4V diphase reinforced composite material
CN102864336A (en) * 2012-09-27 2013-01-09 苏州东海玻璃模具有限公司 In situ synthesis TiC particle reinforced titanium-aluminum-vanadium alloy material and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107904439A (en) * 2017-11-16 2018-04-13 淮阴工学院 A kind of in-situ nano multiphase composite toughening titanium matrix composite and preparation method thereof
CN107904439B (en) * 2017-11-16 2020-01-07 淮阴工学院 In-situ nano multiphase composite strengthening and toughening titanium-based composite material and preparation method thereof
CN111485141A (en) * 2020-06-05 2020-08-04 天钛隆(天津)金属材料有限公司 SiC particle reinforced aluminum titanium matrix composite material and preparation method thereof
CN111485141B (en) * 2020-06-05 2021-12-14 天钛隆(天津)金属材料有限公司 SiC particle reinforced aluminum titanium matrix composite material and preparation method thereof

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