CN105274365A - Titanium alloy preparation technology - Google Patents
Titanium alloy preparation technology Download PDFInfo
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- CN105274365A CN105274365A CN201410336510.6A CN201410336510A CN105274365A CN 105274365 A CN105274365 A CN 105274365A CN 201410336510 A CN201410336510 A CN 201410336510A CN 105274365 A CN105274365 A CN 105274365A
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Abstract
The invention discloses an efficient energy-saving short-process technology for preparing high-quality titanium alloy Ti-Ni-Nb, and provides a titanium alloy preparation technology. The novel technical process is mainly composed of a titanium and titanium alloy crucible-type vacuum induction melting (VIM) technology and a titanium and titanium alloy cold-hearth melting (CHM) technology. The VIM technology is used for primary ingot casting of titanium and titanium alloy preparation, and the electrode preparation of vacuum arc remelting (VAR) electrode arc melting alloy and primary alloy melting of a traditional preparation technology are replaced. The CHM technology is used for secondary refining of the primary titanium and titanium alloy ingot, and then the titanium and titanium alloy ingot in a required shape is prepared. By means of the efficient energy-saving titanium alloy Ti-Ni-Nb preparation technology, the alloy preparation process can be simplified, and high quality alloy ingots in various shapes can be produced.
Description
Technical field
The present invention relates to a kind of preparation technology of titanium alloy, belong to non-ferrous metal titanium materials technology field.
Background technology
Titanium or titanium alloy has that specific tenacity is high, corrosion resistance good and thermotolerance advantages of higher, is widely used in the every field such as Aeronautics and Astronautics.After cold war, titanium or titanium alloy becomes rapidly again army and is required to be civilian, is used for the aspects such as aerospace, ocean exploitation, chemical industry facility and daily light industry.Current titanium alloy is in the stage transformed to " general-purpose warehouses " popular type direction by " strategic materials " color type.Although in world's ore resources, titanium is only second to iron, aluminium, magnesium, be in the 4th be rich in resource, it gets a good chance of the third the practical metal become after iron, aluminium, and exploitation prospect is very wide.
The technology of preparing tempo of titanium alloy quickly, especially in recent years a lot of breakthrough is achieved in this field, and have the trend of constantly speed-raising, but with regard to present circumstances, the principal element of restriction Ti industry development is the expensive price of titanium material, and causes the expensive major cause of titanium material to be titanium complex manufacturing, and the cycle is long, energy consumption is too high, the problems such as rate is low of becoming a useful person.How to reduce titanium material production cost, optimize titanium metallurgical process, become the target of people's effort always.Development research technique is simple, with low cost, and novel technique free from environmental pollution, and preparing high-quality advanced titanium material has been the problem that current people extremely pay close attention to.
Current suitability for industrialized production titanium or titanium alloy is nearly all adopt vacuum self-consumption electrode arc melting technology (VAR), and in electric arc furnace, melting limit in limit crystallizes into ingot in cold-crucible.In vacuum or inert atmosphere, consumable electrode is melted rapidly under the high temperature action of direct current arc, and in water jacketed copper crucible or formed molten bath.When liquid titanium is with the form of molten drop, by nearly 5000K high-temperature electric arc district, transition and when keeping liquid in copper crucible in copper crucible, not only achieve the densification of titanium and its alloys, but also there occurs a series of physical-chemical reaction, play purification effect, make them have better properties.In consumable electrode arc furnace fusion process, fusing and the solidifying of melt of electrode are carried out simultaneously, non-uniform temperature in molten bath, spend huge energy waste and loss of material to be also difficult to obtain a large amount of high temperature titanium liquid; Infusibility be difficult to all even adding with volatile alloying constituent; Crystallization velocity and metallographic structure are also difficult to control; In addition, this technique reclaims waste material difficulty, and the frequency of the ingot casting generation slag inclusion of production is very high, thus limits its application when melting high-quality alloy.
In order to overcome the shortcoming of VAR technology, the eighties in 20th century, cold hearth smelting technique started to rise.Purification and solidifying separates by cold hearth fusion process completely, high-density is mingled with has very large density variation with titanium melt, can sink to be flutterred by scull bottom cold hearth and catch, low density is mingled with makes it melt as far as possible or float by the superheating temperature in molten bath and long-time heat preservation, reach and remove high and low density inclusions, fully realize the object of alloying, obtain the alloy cast ingot of high-quality.Cold hearth melting comprises electron-beam cold bed furnace melting (EBCHM) and plasma cold pool furnace melting (PACHM) two kinds.Method that high-quality titanium alloy usually adopts " cold hearth melting+vacuum consumable smelting (CHM+VAR) ", and become the production method of industrial standards level.
Crucible type vacuum induction melting method may be solve the high and effective way that material recovery rate is extremely low of current conventional titanium alloy melting technology energy consumption.Therefore, finding novel molten titanium crucible material and technology of preparing thereof, realize the vacuum induction melting of internal heat type, is the key realizing the high-quality and efficient melting of titanium alloy low cost.
Summary of the invention
For the defect that prior art exists, the object of the invention is the preparation technology proposing a kind of titanium alloy, adopt the method can simplify the preparation flow of alloy, the titanium or titanium alloy ingot casting of industrialized mass production high-quality.
For achieving the above object, the present invention adopts following technical scheme:
A preparation technology for titanium alloy, is made up of the cold hearth smelting technique of crucible type process for vacuum induction smelting and titanium or titanium alloy, has following step:
A) starting material are prepared according to the composition of Ti-Ni-Nb alloy, and to pre-treatment of raw material; Residual titanium material: comprise residual titanium scrap stock and titanium bits, need the trade mark identical, the granularity be processed into is substantially identical with titanium sponge size, for subsequent use after oil removing, the process of deoxygenation skin; Titanium sponge and alloying element are dry in vacuum drying box, the moisture of removing surface adsorption, drying condition: temperature about 120 ~ 180 DEG C; Vacuum tightness is about 5Pa; Soaking time 4 ~ 6 hours;
B) pretreated starting material are loaded crucible and carry out melting once by process for vacuum induction smelting, concrete steps are: 1. vacuumize, and vacuum tightness reaches 0.01 ~ 3Pa; 2. heat, heating and temperature control is higher than its fusing point 5 ~ 150 DEG C, and namely 1320 DEG C ~ 1465 DEG C ensure that raw material melts completely; 3. be incubated, raw material melts rear insulation 10 ~ 30 minutes completely, ensures the uniform composition of alloy, reduces segregation; 4. cool, the alloy melt in crucible is casting ingot-forming in water cooled copper mould directly;
C) after an ingot casting physical method and chemical process removing surface, carry out secondary smelting by cold hearth smelting technique, concrete steps are: the 1. control of vacuum tightness, adopt electron beam cold hearth melting, vacuum level requirements 0.015 ~ 3Pa; The melting of using plasma cold hearth, needs the helium vacuumizing rear recoil 30 ~ 100KPa; 2. heating and melting, heating and temperature control is than once casting
Ingot fusing point height 5-100 DEG C, at 1320 DEG C ~ 1415 DEG C, ensures that an ingot casting melts completely; 3. refining, through electron beam or plasma heating once ingot melting after, molten bath is formed in cold bed, control the retention time 30 ~ 60 minutes of solution in molten bath, heavy impurity sinks to the bottom, and the little impurity of proportion floats on the surface, the impurity volatilization of low melting point, oxide dissolution, then cleans out respectively by impurity; 4. cool, through refining, stir after solution flow in water jacketed copper crucible through notch, after the heated and stirred again of the plasma gun on crucible or electron beam gun, solidify rear formation secondary ingot casting;
D) hot-work is subsequently proceeded to after the inspection of secondary ingot quality.
Above-mentioned steps b) in crucible be the one of CaO, ThO2, ZrO2, Y2O3, CaZrO3, BaZrO3.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and significant progress:
The inventive method compares with vacuum self-consumption electrode arc melting (VAR), does not need electrode and the electrode assembly welding technique of suppressing titanium or titanium alloy, shortened process, saves melting equipment.Raw-material particle size can change in a big way, directly can use titanium sponge, almost can absolutely use alloy cycle stock.Titanium alloy T i-Ni-Nb prepared by this method, the low density effectively can eliminating titanium alloy is mingled with (LDI) and high-density is mingled with (HDI), and uniform composition, segregation is considerably less, quality is very high.
Embodiment
The specific embodiment of the preparation technology of titanium alloy of the present invention is described below.
A preparation technology for titanium alloy, is made up of the cold hearth smelting technique of crucible type process for vacuum induction smelting and titanium or titanium alloy, has following step:
A) starting material are prepared according to the composition of Ti-Ni-Nb alloy, and to pre-treatment of raw material; Residual titanium material: comprise residual titanium scrap stock and titanium bits, need the trade mark identical, the granularity be processed into is substantially identical with titanium sponge size, for subsequent use after oil removing, the process of deoxygenation skin; Titanium sponge and alloying element are dry in vacuum drying box, the moisture of removing surface adsorption, drying condition: temperature about 120 ~ 180 DEG C; Vacuum tightness is about 5Pa; Soaking time 4 ~ 6 hours;
B) pretreated starting material are loaded CaO crucible and carry out melting once by process for vacuum induction smelting, concrete steps are: 1. vacuumize, and vacuum tightness reaches 0.01 ~ 3Pa; 2. heat, heating and temperature control is higher than its fusing point 5 ~ 150 DEG C, and namely 1320 DEG C ~ 1465 DEG C ensure that raw material melts completely; 3. be incubated, raw material melts rear insulation 10 ~ 30 minutes completely, ensures the uniform composition of alloy, reduces segregation; 4. cool, the alloy melt in crucible is casting ingot-forming in water cooled copper mould directly;
C) after an ingot casting physical method and chemical process removing surface, carry out secondary smelting by cold hearth smelting technique, concrete steps are: the 1. control of vacuum tightness, adopt electron beam cold hearth melting, vacuum level requirements 0.015 ~ 3Pa; The melting of using plasma cold hearth, needs the helium vacuumizing rear recoil 30 ~ 100KPa; 2. heating and melting, heating and temperature control, than an ingot casting fusing point height 5-100 DEG C, at 1320 DEG C ~ 1415 DEG C, ensures that an ingot casting melts completely; 3. refining, through electron beam or plasma heating once ingot melting after, molten bath is formed in cold bed, control the retention time 30 ~ 60 minutes of solution in molten bath, heavy impurity sinks to the bottom, and the little impurity of proportion floats on the surface, the impurity volatilization of low melting point, oxide dissolution, then cleans out respectively by impurity; 4. cool, through refining, stir after solution flow in water jacketed copper crucible through notch, after the heated and stirred again of the plasma gun on crucible or electron beam gun, solidify rear formation secondary ingot casting;
D) hot-work is subsequently proceeded to after the inspection of secondary ingot quality.More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.
The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and application claims protection domain is defined by appending claims and equivalent thereof.
Claims (2)
1. a preparation technology for titanium alloy, is made up of the cold hearth smelting technique of crucible type process for vacuum induction smelting and titanium or titanium alloy, it is characterized in that, have following step:
A) starting material are prepared according to the composition of Ti-Ni-Nb alloy, and to pre-treatment of raw material; Residual titanium material: comprise residual titanium scrap stock and titanium bits, need the trade mark identical, the granularity be processed into is substantially identical with titanium sponge size, for subsequent use after oil removing, the process of deoxygenation skin; Titanium sponge and alloying element are dry in vacuum drying box, the moisture of removing surface adsorption, drying condition: temperature 120 ~ 180 DEG C; Vacuum tightness 5Pa; Soaking time 4 ~ 6 hours;
B) pretreated starting material are loaded crucible and carry out melting once by process for vacuum induction smelting, concrete steps are: 1. vacuumize, and vacuum tightness reaches 0.01 ~ 3Pa; 2. heat, heating and temperature control is higher than its fusing point 5 ~ 150 DEG C, and namely 1320 DEG C ~ 1465 DEG C ensure that raw material melts completely; 3. be incubated, raw material melts rear insulation 10 ~ 30 minutes completely, ensures the uniform composition of alloy, reduces segregation; 4. cool, the alloy melt in crucible is casting ingot-forming in water cooled copper mould directly;
C) after an ingot casting physical method and chemical process removing surface, carry out secondary smelting by cold hearth smelting technique, concrete steps are: the 1. control of vacuum tightness, adopt electron beam cold hearth melting, vacuum level requirements 0.015 ~ 3Pa; The melting of using plasma cold hearth, needs the helium vacuumizing rear recoil 30 ~ 100KPa; 2. heating and melting, heating and temperature control is than once casting
Ingot fusing point height 5-100 DEG C, at 1320 DEG C ~ 1415 DEG C, ensures that an ingot casting melts completely; 3. refining, through electron beam or plasma heating once ingot melting after, molten bath is formed in cold bed, control the retention time 30 ~ 60 minutes of solution in molten bath, heavy impurity sinks to the bottom, and the little impurity of proportion floats on the surface, the impurity volatilization of low melting point, oxide dissolution, then cleans out respectively by impurity; 4. cool, through refining, stir after solution flow in water jacketed copper crucible through notch, after the heated and stirred again of the plasma gun on crucible or electron beam gun, solidify rear formation secondary ingot casting;
D) hot-work is subsequently proceeded to after the inspection of secondary ingot quality.
2. the preparation technology of a kind of titanium alloy according to claim 1, is characterized in that, the crucible in described step b) is the one of CaO, ThO2, ZrO2, Y2O3, CaZrO3, BaZrO3.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951016A (en) * | 2016-06-01 | 2016-09-21 | 洛阳双瑞精铸钛业有限公司 | Short-flow preparation method of TA5 titanium alloy medium-thickness plate for ship |
| CN109574661A (en) * | 2018-12-13 | 2019-04-05 | 沃尔曼科技张家港有限公司 | A kind of preparation method and application of barium zirconate ceramic core |
| CN110578061A (en) * | 2018-06-07 | 2019-12-17 | 湖南稀土金属材料研究院 | Electron beam melting continuous ingot casting method for high-purity rare earth metal |
| CN111254318A (en) * | 2020-03-12 | 2020-06-09 | 西安华创新材料有限公司 | Fine smelting and purifying method for large-size nickel-titanium shape memory alloy cast ingot |
| CN111334674A (en) * | 2020-03-13 | 2020-06-26 | 王书杰 | Device for preparing titanium rod, titanium alloy and titanium alloy device |
| CN111945023A (en) * | 2020-07-29 | 2020-11-17 | 中国船舶重工集团公司第七二五研究所 | Vacuum induction melting method of titanium and titanium alloy ingots |
| CN112095019A (en) * | 2020-08-11 | 2020-12-18 | 大连理工大学 | Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution |
| CN112813300A (en) * | 2019-11-12 | 2021-05-18 | 新疆大学 | Low-cost titanium alloy preparation method |
| CN113881854A (en) * | 2021-10-28 | 2022-01-04 | 西部钛业有限责任公司 | Method for eliminating low-density inclusion defect source of titanium alloy ingot |
| CN113881859A (en) * | 2020-06-19 | 2022-01-04 | 新疆大学 | Preparation method of middle and small-sized titanium and titanium alloy thin-walled tube |
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2014
- 2014-07-16 CN CN201410336510.6A patent/CN105274365A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951016B (en) * | 2016-06-01 | 2017-07-28 | 洛阳双瑞精铸钛业有限公司 | A kind of short process making method of naval vessel TA5 titanium alloy medium-thick plates |
| CN105951016A (en) * | 2016-06-01 | 2016-09-21 | 洛阳双瑞精铸钛业有限公司 | Short-flow preparation method of TA5 titanium alloy medium-thickness plate for ship |
| CN110578061A (en) * | 2018-06-07 | 2019-12-17 | 湖南稀土金属材料研究院 | Electron beam melting continuous ingot casting method for high-purity rare earth metal |
| CN109574661A (en) * | 2018-12-13 | 2019-04-05 | 沃尔曼科技张家港有限公司 | A kind of preparation method and application of barium zirconate ceramic core |
| CN112813300A (en) * | 2019-11-12 | 2021-05-18 | 新疆大学 | Low-cost titanium alloy preparation method |
| CN111254318A (en) * | 2020-03-12 | 2020-06-09 | 西安华创新材料有限公司 | Fine smelting and purifying method for large-size nickel-titanium shape memory alloy cast ingot |
| CN111334674A (en) * | 2020-03-13 | 2020-06-26 | 王书杰 | Device for preparing titanium rod, titanium alloy and titanium alloy device |
| CN113881859A (en) * | 2020-06-19 | 2022-01-04 | 新疆大学 | Preparation method of middle and small-sized titanium and titanium alloy thin-walled tube |
| CN113881859B (en) * | 2020-06-19 | 2022-11-11 | 新疆大学 | Preparation method of middle and small-sized titanium and titanium alloy thin-walled tube |
| CN111945023A (en) * | 2020-07-29 | 2020-11-17 | 中国船舶重工集团公司第七二五研究所 | Vacuum induction melting method of titanium and titanium alloy ingots |
| CN112095019A (en) * | 2020-08-11 | 2020-12-18 | 大连理工大学 | Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution |
| CN113881854A (en) * | 2021-10-28 | 2022-01-04 | 西部钛业有限责任公司 | Method for eliminating low-density inclusion defect source of titanium alloy ingot |
| CN113881854B (en) * | 2021-10-28 | 2023-08-15 | 西部钛业有限责任公司 | Method for eliminating sources of low-density inclusion defects of titanium alloy cast ingot |
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