CN102517464A - Preparation method for in-situ synthesized particle reinforced titanium-based composite material - Google Patents

Preparation method for in-situ synthesized particle reinforced titanium-based composite material Download PDF

Info

Publication number
CN102517464A
CN102517464A CN2011104407757A CN201110440775A CN102517464A CN 102517464 A CN102517464 A CN 102517464A CN 2011104407757 A CN2011104407757 A CN 2011104407757A CN 201110440775 A CN201110440775 A CN 201110440775A CN 102517464 A CN102517464 A CN 102517464A
Authority
CN
China
Prior art keywords
preparation
titanium
smelting furnace
vacuum plasma
arc
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2011104407757A
Other languages
Chinese (zh)
Inventor
赵文天
梁栋
葛文艳
李德林
易更
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
No 52 Institute of China North Industries Group Corp
Original Assignee
No 52 Institute of China North Industries Group Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by No 52 Institute of China North Industries Group Corp filed Critical No 52 Institute of China North Industries Group Corp
Priority to CN2011104407757A priority Critical patent/CN102517464A/en
Publication of CN102517464A publication Critical patent/CN102517464A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a preparation method for an in-situ synthesized particle reinforced titanium-based composite material. The preparation method is characterized by comprising the following steps of: placing a titanium-based material into a water-cooled graphite crucible; vacuumizing a vacuum plasma smelting furnace until the air pressure does not exceed 10 Pa; arcing and smelting; entering a refining period; adding graphite powder which is in a powder feeder and generates reinforced phase through in-situ reaction into the vacuum plasma smelting furnace; performing electromagnetic stirring; stopping arc; and pouring. Compared with the prior art, the preparation method has the advantages of effectively avoiding pollution to alloy melt, obviously increasing the alloying degree of high-melting-point components, reducing aggregation and segregation of the high-melting-point components in cast ingots, guaranteeing alloying uniformity and reasonably controlling the oxygen content of alloy.

Description

The preparation method of in-situ authigenic granule intensified titanium-base compound material
Technical field
The present invention relates to a kind of preparation method of titanium matrix composite.
Background technology
Titanium matrix composite (TMCS) has higher room temperature specific tenacity and compares Young's modulus; Good anti-fatigue performance and high temperature creep-resisting performance and excellent corrosion resisting property; Be widely used in blade of aviation engine, frame, rise and fall set a roof beam in place, on the member such as thrust chamber case, but high raw materials cost and tooling cost have hindered its industrial practicalization.
Titanium matrix composite (TMCS) can be divided into continuous fiber reinforcing titanium matrix composite and granule intensified titanium-base compound material again.The fiber reinforcement titanium matrix composite is owing to exist preparation cost high, complex process, and the difficulty that is shaped, the goods of gained exist significant anisotropism, and the unequal defective of Fiber Distribution makes its development and using all be restricted.By comparison, granule intensified titanium-base compound material has isotropic character, and preparation cost is lower, and method of manufacture is simple, is easy to make complex-shaped part, therefore has bigger development prospect, and gets more and more people's extensive concerning gradually.Simultaneously; Granule intensified titanium-base compound material density is low; Have than aluminium, the better high-temperature behavior of magnesium base composite material; Its tensile strength, fatigue strength, Young's modulus and wearing character are compared all with Ti-6Al-4V wrought alloy of the same race (as-annealed condition) and are improved largely, and can make the further lightweight of structural parts, and the raising of polishing machine can be removed the relatively more expensive surface treatment procedure of cost in the preparation process; This has great significance to reducing the material prepn cost, and these advantages make it aspect military and civilian, all have broad application prospects simultaneously.
Yet; At high temperature reactive behavior is very high owing to titanium, directly in melt, adds wild phase and will cause matrix and wild phase intense reaction, and interface pollution is serious; The strength of materials reduces; Owing to there are problems such as matrix and wild phase wettability, make that the bonding strength of matrix and wild phase is lower simultaneously, cause material property to descend equally.
Addition and in-situ synthesis outside the growth pattern of reinforced particulate in body material comprises, outer addition are exactly directly in melt, to add wild phase, and at high temperature reactive behavior is very high owing to titanium; This method will cause matrix and wild phase intense reaction; Interface pollution is serious, and the strength of materials reduces, simultaneously owing to there are problems such as matrix and wild phase wettability; Make that the bonding strength of matrix and wild phase is lower, cause material property to descend equally.In-situ synthesis then can well be avoided the problems referred to above.
The in-situ authigenic granule intensified titanium-base compound material, isotropy, chemicalstability be good, be easy to moulding, with low cost, can avoid the interface wet ability problem between wild phase and the matrix.At present, the preparation method of in-situ authigenic granule intensified titanium-base compound material mainly contains: powder metallurgy, fusion casting, XD TMTechnology, combustion synthesis method, burning are synthesized---fusion casting, contact reaction method, mechanical alloying method, laser cladding method etc.; In above-mentioned preparation method some that is that all right is ripe; Some operation is loaded down with trivial details, preparation cost is higher; Some is prone to problems such as tissue, component segregation and crystal grain is thick, and some is wayward, the melting environment is relatively poor.
Summary of the invention
Technical problem to be solved by this invention is the preparation method that the good in-situ authigenic granule intensified titanium-base compound material of a kind of alloying homogeneity is provided to the above-mentioned state of the art.
Another technical problem to be solved by this invention provides a kind of preparation method that can control the in-situ authigenic granule intensified titanium-base compound material of oxygen level in the alloy.
It is simple that another technical problem to be solved by this invention provides a kind of technology, the preparation method of the in-situ authigenic granule intensified titanium-base compound material that preparation cost is lower.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of preparation method of in-situ authigenic granule intensified titanium-base compound material is characterized in that comprising the steps:
With the titanium based raw material water-cooled plumbago crucible in the vacuum plasma smelting furnace of packing into, vacuum is extracted into and is no more than 10Pa in the vacuum plasma smelting furnace, charges into mixed gas to 0.8bar~1.1bar to the vacuum plasma smelting furnace; Flow is 10L/min~15L/min, and starting the arc melting gets into refining period; When surpassing 50% molten bath area and form, will add the vacuum plasma smelting furnace from powder feeder in order to the Graphite Powder 99 that reaction in generates wild phase, simultaneously induction stirring 3min~5min; Stop arc, cast, teeming temperature is 1250 ℃~1450 ℃; Comprise hydrogen and argon gas in the aforesaid mixed gas, wherein hydrogen volume accounts for 8%~25% of total mixed gas volume.
Further, described powder feeder is serially connected with the plasma gas inlets of vacuum plasma smelting furnace.
As preferably, during starting the arc melting, the electric current 400A~800A of plasma arc, voltage 42V~54V.
As preferably, described Graphite Powder 99 median size is 2 μ m~20 μ m.
As preferably, described titanium based raw material is for referring to Titanium Sponge 40-60 mesh or titanium rod.
Further, described water-cooled plumbago crucible comprises the crucible body and is located at the water jacket of crucible body.
Further, described induction stirring realizes through a plurality of electromagnetic stirrer coils of being located at crucible body bottom.
Compared with prior art, the invention has the advantages that:, adopt vacuum plasma electric arc as thermal source to the titanium matrix composite of the difficult consolute system of low density multicomponent; Utilize water-cooled plumbago crucible and induction stirring; Avoided pollution effectively, significantly improved the alloying level of HMP constituent element, reduced the HMP constituent element in the ingot casting and assembled segregation alloy melt; Guaranteed the homogeneity of alloying; Adopting hydrogen and argon gas simultaneously is the plasma (orifice) gas body source, has improved the reducing atmosphere in the stove, reasonably controls the oxygen level in the alloy.
Description of drawings
Fig. 1 is a vacuum plasma smelting furnace structural representation.
Fig. 2 is the titanium and the matrix material metallographic structure Photomicrograph of gained among the embodiment 3.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment one: with the raw material Titanium Sponge 40-60 mesh water-cooled plumbago crucible of packing into, body of heater is evacuated down to 10Pa, stops vacuum pump, and the mixed gas (wherein the H2 volume content 8%) that charges into hydrogen (H2) and argon gas (Ar) to body of heater is to 1.0bar; Flow is 10L/min, starting the arc melting, starting the arc stage arc-plasma current 400A~470A, voltage 42V~46V; Get into refining period, when molten bath (referring to surpass 50% molten bath area) on a large scale when forming, with median size 20 μ m in order to reaction in generate wild phase Graphite Powder 99 add from powder feeder; Arc-plasma current 600A~650A, voltage 50V~52V, induction stirring 3min simultaneously; Stop arc, cast, teeming temperature is 1350 ℃.Obtain the matrix material of homogeneous microstructure.
As shown in Figure 1; The vacuum plasma smelting furnace comprises body of heater 1, is positioned at the water-cooled plumbago crucible of body of heater 1, electron ion gun electrode 3 and powder feeder 2; Body of heater 1 has plasma gas inlets 11, and electron ion gun electrode 3 is positioned at this ionized gas inlet mouth 11, and powder feeder 2 is series on the admission passage; The water-cooled plumbago crucible comprises crucible body 4 and is positioned at the water jacket 5 of crucible body 4 outer walls that induction stirring realizes through a plurality of electromagnetic stirrer coils 6 of being located at crucible body 4 bottoms.
Embodiment two: with the raw material titanium rod water-cooled plumbago crucible of packing into, body of heater is evacuated down to 1Pa, stops vacuum pump, and the mixed gas (wherein the H2 volume content 25%) that charges into hydrogen (H2) and argon gas (Ar) to body of heater is to 1.1bar; Flow is 15L/min, starting the arc melting, starting the arc stage arc-plasma current 550A~650A, voltage 44V~48V; Get into refining period, when the molten bath forms on a large scale, with median size 10 μ m in order to reaction in generate wild phase Graphite Powder 99 add from powder feeder; Arc-plasma current 700A~800A, voltage 50V~54V, induction stirring 5min simultaneously; Stop arc, cast, teeming temperature is 1350 ℃.Obtain the matrix material of homogeneous microstructure.
Embodiment three: with the raw material Titanium Sponge 40-60 mesh water-cooled plumbago crucible of packing into, body of heater is evacuated down to 0.1Pa, stops vacuum pump, charges into hydrogen (H to body of heater 2) and the mixed gas of argon gas (Ar) (H wherein 2Volume content 20%) to 0.8bar, flow is 12L/min, starting the arc melting, starting the arc stage arc-plasma current 450A~550A; Voltage 44V~48V gets into refining period, when the molten bath forms on a large scale, with median size 2 μ m in order to reaction in generate wild phase Graphite Powder 99 add from powder feeder; Arc-plasma current 650A~750A, voltage 50V~52V, induction stirring 3min simultaneously; Stop arc, cast, teeming temperature is 1350 ℃.Obtain the matrix material of homogeneous microstructure.The titanium matrix composite metallographic structure Photomicrograph of gained shown in Figure 2.
Following table is this titanium matrix composite and the contrast of matrix room-temperature mechanical property parameter:
Figure BDA0000124779010000031
Figure BDA0000124779010000041
Data can be found out from last table; The tensile strength of the TiC/Ti matrix material of vacuum arc melting (VAR) technology preparation can reach more than 120% of titanium of casting; The present invention adopts the tensile strength of the TiC/Ti matrix material of plasma melting (PM) technology preparation then can reach more than 138% of titanium of casting, and the TiC/Ti composite property of plasma melting preparation reaches more than 10% than vacuum arc melting increase rate.Simultaneously chemical analysis shows, it is lower that strengthen body burden in the matrix material this moment, and 1.55wt% is only arranged, and intensity even surpass the arc melting matrix material that strengthens body burden 37wt%.This shows that the plasma melting technology has bigger potentiality in prepared in reaction TiC granule intensified titanium-base compound material aspect in position, and the material mechanical performance of preparation is higher.

Claims (7)

1. the preparation method of an in-situ authigenic granule intensified titanium-base compound material is characterized in that comprising the steps:
With the titanium based raw material water-cooled plumbago crucible in the vacuum plasma smelting furnace of packing into, vacuum is extracted into and is no more than 10Pa in the vacuum plasma smelting furnace, charges into mixed gas to 0.8bar~1.1bar to the vacuum plasma smelting furnace; Flow is 10L/min~15L/min, and starting the arc melting gets into refining period; When surpassing 50% molten bath area and form, will add the vacuum plasma smelting furnace from powder feeder in order to the Graphite Powder 99 that reaction in generates wild phase, simultaneously induction stirring 3min~5min; Stop arc, cast, teeming temperature is 1250 ℃~1450 ℃; Comprise hydrogen and argon gas in the aforesaid mixed gas, wherein hydrogen volume accounts for 8%~25% of total mixed gas volume.
2. preparation method according to claim 1 is characterized in that described powder feeder is serially connected with the plasma gas inlets of vacuum plasma smelting furnace.
3. preparation method according to claim 1, when it is characterized in that starting the arc melting, the electric current 400A~800A of plasma arc, voltage 42V~54V.
4. preparation method according to claim 1 is characterized in that described Graphite Powder 99 median size is 2 μ m~20 μ m.
5. preparation method according to claim 1 is characterized in that described titanium based raw material is for referring to Titanium Sponge 40-60 mesh or titanium rod.
6. preparation method according to claim 1 is characterized in that described water-cooled plumbago crucible comprises the crucible body and is located at the water jacket of crucible body.
7. preparation method according to claim 6 is characterized in that described induction stirring realizes through a plurality of electromagnetic stirrer coils of being located at crucible body bottom.
CN2011104407757A 2011-12-26 2011-12-26 Preparation method for in-situ synthesized particle reinforced titanium-based composite material Pending CN102517464A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2011104407757A CN102517464A (en) 2011-12-26 2011-12-26 Preparation method for in-situ synthesized particle reinforced titanium-based composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2011104407757A CN102517464A (en) 2011-12-26 2011-12-26 Preparation method for in-situ synthesized particle reinforced titanium-based composite material

Publications (1)

Publication Number Publication Date
CN102517464A true CN102517464A (en) 2012-06-27

Family

ID=46288526

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2011104407757A Pending CN102517464A (en) 2011-12-26 2011-12-26 Preparation method for in-situ synthesized particle reinforced titanium-based composite material

Country Status (1)

Country Link
CN (1) CN102517464A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103673596A (en) * 2013-11-22 2014-03-26 江苏博迁新材料有限公司 Semi-fusion type crucible heating device
US20160177418A1 (en) * 2013-03-18 2016-06-23 Korea Institute Of Industrial Technology Refining device and refining method for titanium scraps and sponge titanium using deoxidising gas
CN108396172A (en) * 2018-02-23 2018-08-14 深圳万佳互动科技有限公司 A kind of granule intensified titanium-base compound material and preparation method thereof
WO2019088007A1 (en) * 2017-10-31 2019-05-09 株式会社神戸製鋼所 Method for purifying titanium material
CN110592416A (en) * 2019-10-24 2019-12-20 沈阳工业大学 Plasma-assisted gas alloying method
CN113981263A (en) * 2021-10-26 2022-01-28 北京科技大学 Method for preparing copper-based titanium carbide composite material through in-situ reaction

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101130840A (en) * 2007-09-27 2008-02-27 上海交通大学 Hydrogen permeating superplasticity processing method for in-situ synthesized titanium-based composite material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101130840A (en) * 2007-09-27 2008-02-27 上海交通大学 Hydrogen permeating superplasticity processing method for in-situ synthesized titanium-based composite material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
赵文天等: "等离子熔铸法制备原位TiCp/Ti复合材料的金相组织", 《兵器材料科学与工程》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160177418A1 (en) * 2013-03-18 2016-06-23 Korea Institute Of Industrial Technology Refining device and refining method for titanium scraps and sponge titanium using deoxidising gas
US9840755B2 (en) * 2013-03-18 2017-12-12 Korea Institute Of Industrial Technology Refining device and refining method for titanium scraps and sponge titanium using deoxidising gas
CN103673596A (en) * 2013-11-22 2014-03-26 江苏博迁新材料有限公司 Semi-fusion type crucible heating device
WO2019088007A1 (en) * 2017-10-31 2019-05-09 株式会社神戸製鋼所 Method for purifying titanium material
RU2738280C1 (en) * 2017-10-31 2020-12-11 Кабусики Кайся Кобе Сейко Се (Кобе Стил, Лтд.) Method of cleaning titanium material
CN108396172A (en) * 2018-02-23 2018-08-14 深圳万佳互动科技有限公司 A kind of granule intensified titanium-base compound material and preparation method thereof
CN108396172B (en) * 2018-02-23 2019-06-21 温州海诚光学有限公司 A kind of granule intensified titanium-base compound material and preparation method thereof
CN110592416A (en) * 2019-10-24 2019-12-20 沈阳工业大学 Plasma-assisted gas alloying method
CN113981263A (en) * 2021-10-26 2022-01-28 北京科技大学 Method for preparing copper-based titanium carbide composite material through in-situ reaction

Similar Documents

Publication Publication Date Title
CN102517464A (en) Preparation method for in-situ synthesized particle reinforced titanium-based composite material
CN112391556B (en) High-strength high-conductivity Cu-Cr-Nb alloy reinforced by double-peak grain size and double-scale nanophase
RU2329122C2 (en) Method of items production from metal alloys without melting
Gao et al. Electron beam melted TiC/high Nb–TiAl nanocomposite: Microstructure and mechanical property
CN105537603A (en) Preparing method for ultra-fine high-purity Ti2AlNb alloy powder
CN109161735B (en) Graphene rare earth cerium reinforced Al-Si-Mg cast aluminum alloy and preparation method thereof
CN104674103A (en) CrFeCoNiNbx high-entropy alloy and preparation method thereof
CN103757514A (en) High-entropy AlCoCrFeNiCuC alloy and preparation method thereof
CN203390198U (en) Titanium-based powder preparation device
CN106756266A (en) A kind of aluminium molybdenum chromium tin niobium intermediate alloy and preparation method thereof
CN102418025A (en) Structure controlled preparation method for Nb-Si-based complex alloy
RU2607857C1 (en) Method of producing electrodes from nickel aluminide-based alloys
CN106636933A (en) Method for preparing multi-phase reinforced ferrite alloy
CN111041287A (en) Graphene-reinforced Al-Si cast aluminum alloy and preparation method thereof
RU2618038C2 (en) Method for obtaining a heat-resistant alloy based on niobium
CN109112347A (en) A kind of high-strength high-conductivity copper-chromium-zirconium and preparation method thereof
CN115044794A (en) Cu- (Y) with excellent performance 2 O 3 -HfO 2 ) Alloy and preparation method thereof
CN107952966A (en) The preparation method at spherical titanium aluminium-based alloyed powder end
CN101876043A (en) Homogenization heat treatment method suitable for spray forming of 7000 series aluminum alloys
CN116607028B (en) Smelting method of refractory high-entropy alloy
Li et al. Microstructural evolution and mechanical properties of eutectoid Ti–7Ni alloy produced by electron beam powder bed fusion
CN112831708A (en) Titanium-aluminum-based polycrystalline heat-resistant titanium alloy and preparation method thereof
CN116287953A (en) Nuclear grade ferritic stainless steel with high-density nano-dispersed particles and preparation method thereof
RU2630157C2 (en) Method to produce electrodes of alloys based on titanium aluminide
CN103589912A (en) Melting method of powder superalloy

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20120627