CN104651662B - The vacuum induction melting method of titanium-aluminium alloy target material - Google Patents
The vacuum induction melting method of titanium-aluminium alloy target material Download PDFInfo
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Abstract
The invention discloses a kind of vacuum induction melting method of titanium-aluminium alloy target material.The method carries out vacuum induction melting and prepares titanium-aluminium alloy using CaO crucibles, successively including batching step, baking material step, shove charge step, alloy melting step and casting step.The inventive method has process is simple, with short production cycle, and energy consumption is low, and equipment investment is small, low production cost, alloy composition precise control, and crucible pollution is small, and gas content is low, the advantage without casting flaws such as rimholes.
Description
Technical field
The invention belongs to metallurgical preparation field, the vacuum induction melting method of more particularly to a kind of titanium-aluminium alloy target material.
Background technology
With the arrival in modern mechanical processing industry High-speed machining epoch, the application of coating technology is also focused in countries in the world further
With development.PVD（Physical Vapor Deposition）It is heavy that coating has not been only the performance of raising high-speed alloy cutter
Act on, and it is even more essential for hard alloy cutter, because hard alloy cutter is than high-speed alloy cutter valency
Lattice are more expensive, and utilization rate is higher.In the PVD coatings of cutter, titanium-aluminium alloy is a kind of very important coating materials.For example, Balzers
The two kinds of representational coatings developed are respectively FUTURA NANO and X.CEED, and wherein FUTURA NANO can make cutter in height
Used under conditions of speed processing, and X.CEED can make the cutter have excellent red hardness, inoxidizability, even if in severe processing bar
Under part, its film still has good bond strength with matrix, and the coating materials of both coatings is titanium-aluminium alloy.Titanium-aluminium alloy can
To significantly improve the machining accuracy of cutting-tool's used life and product, but the degree of purity of titanium-aluminium alloy to the use longevity of cutter
Life is played an important role, that is to say, that when carrying out plated film using titanium-aluminium alloy target material, and the degree of purity requirement to target is extremely tight
The content of the impurity such as lattice, particularly carbon, oxygen, nitrogen, the content of impurity is lower, more favourable to cutting-tool's used life.
At present, the method for manufacture titanium-aluminium alloy target material has two kinds, powder sintering and melting and casting method：
（1）Powder sintering：Ti powder and Al powder as used certain particle size in the patent of Publication No. CN101214546A,
Or the alloy powder of atomization, through mixing powder, fill powder, cold isostatic compaction, degassing, high temperature insostatic pressing (HIP) or sintering, then machined be made
Finished product.The advantage of the method can be to make large-sized titanium aluminium target；The shortcoming of the method can not be kept away in manufacturing process
Exempt from that metal impurities, gas can be increased（C、N、O）Content is higher.
（2）Melting and casting method：At present, the method for melting titanium-aluminium alloy has following several：The first is to use vacuum electronic
Beam melting, in the method fusion process, Al volatilizations are big, and composition is difficult to control；Second method is to use vacuum consumable electrode arc furnace
Melting, the titanium-aluminium alloy component segregation of the method melting is big；The third method is using vacuum suspension stove melting, the method melting
Titanium-aluminium alloy, although gas and metals content impurity are than relatively low, but the method needs secondary remelting, and apparatus expensive, energy consumption
Height, causes the high cost of molten alloy.In addition, also have that vacuum induction melting is carried out as crucible material using graphite, but
The alloy pig carbon content for melting out is very high.Carried out very using high-purity CaO crucibles in the patent application of Publication No. CN1420189A
Empty induction melting, the method needs vacuum pumping twice, and feed way is cumbersome, and it adds during calcium deoxidation will make this alloy system
Impurity content increases, and during the calcium oxide that deoxidation is formed is mingled with and remains in alloy solution, substantial amounts of interior life is formed after casting
It is mingled with, it is impossible to remove.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of vacuum induction melting of titanium-aluminium alloy target material
Method.The method process is simple, with short production cycle, low cost, composition precise control, crucible pollution are small, and gas content is low, without gas
The casting flaws such as bubble.
To achieve these goals, the present invention uses following technical scheme：
A kind of vacuum induction melting method of titanium-aluminium alloy target material, carries out vacuum induction melting and prepares titanium using CaO crucibles
Aluminium alloy target, successively including batching step, baking material step, shove charge step, alloy melting step and casting step, wherein：
In the baking material step, the feed metal aluminium and titanium sponge that will be prepared are put into vacuum drying oven, and baking temperature is
Less than 150 DEG C, baking time is, no less than 4 hours, to be then cooled to less than 40 DEG C with stove and take out stand-by；
In the shove charge step, toasted feed metal aluminium is put into the bottom of the CaO crucibles of vaccum sensitive stove, then
By top of the titanium sponge pine loaded on metallic aluminium；
In the alloy melting step, the vacuum of the vaccum sensitive stove is set to remain no greater than 0.1Pa first, then with
The electrical power power transmission of no more than 15KW, after the inert gas that 0.2~0.4atm is filled with after 10~15 minutes, then increases power transmission work(
Rate makes raw material rapid melting to more than 35KW, and the maximum temperature of aluminium alloy is controlled at 1580~1610 DEG C after fusing.
The above method is illustrated in order to more detailed, the above method can be illustratively described as：
In the baking material step, the raw material that will be prepared is put into vacuum drying oven, at 80 DEG C, 100 DEG C, 120 DEG C or 140 DEG C
Under conditions of be incubated 4h, 5h or 6h, be then cooled to 15 DEG C, 20 DEG C, 30 DEG C or 40 DEG C taking-ups with stove stand-by；
In the alloy melting step, make first the vaccum sensitive stove vacuum be maintained at 0.01Pa, 0.04Pa,
0.05Pa, 0.06Pa, 0.07Pa, 0.08Pa or 0.1Pa, then with the electrical power power transmission of 10KW, 12KW or 15KW, treat 10min,
The inert gas of 0.2atm, 0.3atm or 0.4atm is filled with after 12min or 15min, power transmission power to 35KW, 40KW is then increased
Or 45KW, making raw material rapid melting, the maximum temperature of aluminium alloy is controlled at 1580 DEG C, 1590 DEG C, 1600 DEG C, 1605 DEG C after fusing
Or 1610 DEG C.
In the above-mentioned methods, the batching step is to weigh titanium sponge and metal respectively by the requirement of titanium-aluminium alloy composition design
Aluminium, used as a kind of preferred embodiment, the batching step is to weigh 0 grade of titanium sponge respectively by the requirement of titanium-aluminium alloy composition design
Metallic aluminium with purity higher than 99.99%, wherein the titanium-aluminium alloy is made up of following element by weight percentage：Ti：60~
70%, Al:30~40%.
In the above-mentioned methods, as a kind of preferred embodiment, in the baking material step, the baking temperature is 100-
140 DEG C, the baking time is 4-5h.The vacuum of the vacuum drying oven is 600-6000Pa.
In the above-mentioned methods, as a kind of preferred embodiment, in the alloy melting step, the vacuum is made first
The vacuum of induction furnace remains 0.01-0.08Pa, then with the electrical power power transmission of 10-15KW, after being filled with 0.2 after 10~15 minutes
The inert gas of~0.4atm, then increases power transmission power to 35-40KW, makes raw material rapid melting, to shorten aluminium alloy and earthenware
The time of contact of crucible, the maximum temperature of aluminium alloy is controlled at 1580~1610 DEG C after fusing, in case aluminium alloy temperature is high and crucible
Reflection accelerates.
In the above-mentioned methods, the inert gas can be argon gas or helium.
In the above-mentioned methods, as a kind of preferred embodiment, in the casting step, when aluminium alloy temperature is higher than conjunction
Cast when more than golden liquid melting temperature 30~50 DEG C.After load melting, pour into a mould as early as possible, can further reduce aluminium alloy with
The time of contact of crucible.
In the method for the invention, raw material through vacuum drying ensuring raw material drying and not oxidized；Using CaO earthenwares
Crucible, aluminium is filled from bottom, and top fills the mode of titanium, and power transmission baking furnace charge, not only improves the volatilization of gas in furnace charge under vacuum, drops
Gas content in low furnace charge, takes full advantage of energy again, is conducive to accelerating speed of melting, it is thus also avoided that plus aluminium alloy during cold burden
Splash；After being filled with inert gas such as argon gas, high power power transmission makes furnace charge and aluminium alloy fully deaerate, and accelerates the molten of furnace charge
Change speed, titanium aluminium ingot inside and epidermis is produced bubble due to being filled with argon gas again；The fusion temperature of aluminium alloy is controlled,
Effectively reduce reaction time of the aluminium alloy with crucible and speed.
The present invention has process is simple compared with prior art, and with short production cycle, energy consumption is low, and equipment investment is small, is produced into
This low, alloy composition precise control, crucible pollution is small, and gas content is low, the advantage without casting flaws such as rimholes.It is above-mentioned excellent
Point is specific as follows：Melting cycle≤30 minute, per the power consumption≤15KWh of stove alloy, Composition Control is accurate, principal component deviation≤
0.5wt%, impurity Ca≤0.015wt% in alloy, Gas content is low（O≤0.12wt%, N≤0.015wt%, C≤0.015wt%）.
Brief description of the drawings
Fig. 1 is the ultrasonic examination figure of alloy cast ingot section obtained in the embodiment of the present invention 1；
Fig. 2 is the ultrasonic examination figure of alloy cast ingot section obtained in the embodiment of the present invention 2；
Fig. 3 is the ultrasonic examination figure of alloy cast ingot section obtained in the embodiment of the present invention 3；
Fig. 4 is the ultrasonic examination figure of alloy cast ingot section obtained in comparative example of the present invention 3；
Fig. 5 is the ultrasonic examination figure of alloy cast ingot section obtained in comparative example of the present invention 4.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail, but the present invention is not limited thereto.
Three below embodiment is according to the manufacture method of titanium-aluminium alloy target material vacuum induction melting of the present invention point
3 stove titanium-aluminium alloy target materials are not prepared for.
Embodiment 1
Titanium-aluminium alloy target material manufactured in the present embodiment is made up of following element by weight percentage：Ti64%, Al36%.
Manufacture method is as follows：
（1）Dispensing：The metallic aluminium of 0 grade of titanium sponge and purity higher than 99.99% is weighed respectively by above-mentioned design of alloy.
（2）Baking material：The raw material titanium and aluminium that will be weighed up are put into vacuum drying oven（Vacuum is 5000Pa）In, in 100 DEG C of bars
5h is incubated under part, it is stand-by to be cooled to 35 DEG C of taking-ups with stove.
（3）Shove charge：By the raw material after baking（That is furnace charge）In metallic aluminium be put into the bottom of 25Kg vaccum sensitive stove CaO crucibles
Portion, then by top of the titanium sponge pine loaded on metallic aluminium.
（4）Alloy melting：The vacuum of vaccum sensitive stove is remained 0.03Pa first, then sent with the electrical power of 15KW
Electricity, after the argon gas that 0.2atm is filled with after 14 minutes, then increases power transmission power to 35KW, makes raw material rapid melting, to shorten conjunction
The time of contact of golden liquid and crucible, after alloy melting after power transmission 11 minutes, the maximum temperature of aluminium alloy is 1585 DEG C after fusing.
（5）Cooling casting：Have a power failure cooling 30s, is cast when aluminium alloy temperature is 1535 DEG C, so as to obtain alloy casting
Ingot.
The performance of alloy cast ingot manufactured in the present embodiment is referring to table 1.
Ultrasonic examination is taken to test obtained ingot blank inside and surface quality, the method for ultrasonic examination is such as
Under：
1）Machining：Ingot blank cuts into size for ￠ 190*15mm through mechanical wires（Ingot blank size is ￠ 190*160mm）'s
Blank, mill processing is carried out to big face of cutting into slices using the alundum wheel of 80 mesh, and surface roughness reaches 3.2 or so after mill processing；
2）Ultrasonic examination：Section is positioned in the tank of ultrasonic test equipment, is visited using 10M focusing probes
Wound, sweep speed is 150mm/s.
3）Preserve C-scan figure：After the completion of flaw detection, related scanned picture is saved in memory, to be analyzed
And judgement.
The ultrasonic examination figure of alloy cast ingot manufactured in the present embodiment section referring to Fig. 1, without rimhole.
Embodiment 2
Titanium-aluminium alloy target material manufactured in the present embodiment is made up of following element by weight percentage：Ti60%, Al40%.
Manufacture method is as follows：
（1）Dispensing：The metallic aluminium of 0 grade of titanium sponge and purity higher than 99.99% is weighed respectively by above-mentioned design of alloy.
（2）Baking material：The raw material titanium and aluminium that will be weighed up are put into vacuum drying oven（Vacuum is 5000Pa）In, in 140 DEG C of bars
4h is incubated under part, it is stand-by to be cooled to 38 DEG C of taking-ups with stove.
（3）Shove charge：By the raw material after baking（That is furnace charge）In metallic aluminium be put into the bottom of 25Kg vaccum sensitive stove CaO crucibles
Portion, then by top of the titanium sponge pine loaded on metallic aluminium.
（4）Alloy melting：The vacuum of vaccum sensitive stove is remained 0.04Pa first, then sent with the electrical power of 13KW
Electricity, after the argon gas that 0.2atm is filled with after 15 minutes, then increases power transmission power to 35KW, makes raw material rapid melting, to shorten conjunction
The time of contact of golden liquid and crucible, after alloy melting after power transmission 10 minutes, the maximum temperature of aluminium alloy is 1580 DEG C after fusing.
（5）Cooling casting：Have a power failure cooling 32s, is cast when aluminium alloy temperature is 1520 DEG C, so as to obtain alloy casting
Ingot.
The performance of alloy cast ingot manufactured in the present embodiment is referring to table 1.
Ingot blank prepared by embodiment 2 is tested using the ultrasonic examination method of inspection in the same manner as in Example 1, is cast
Ingot section ultrasonic examination figure referring to Fig. 2, without rimhole.
Embodiment 3
Titanium-aluminium alloy target material manufactured in the present embodiment is made up of following element by weight percentage：Ti70%, Al30%.
Manufacture method is as follows：
（1）Dispensing：The metallic aluminium of 0 grade of titanium sponge and purity higher than 99.99% is weighed respectively by above-mentioned design of alloy.
（2）Baking material：The raw material titanium and aluminium that will be weighed up are put into vacuum drying oven（Vacuum is 5000Pa）In, in 140 DEG C of bars
4h is incubated under part, it is stand-by to be cooled to 36 DEG C of taking-ups with stove.
（3）Shove charge：By the raw material after baking（That is furnace charge）In metallic aluminium be put into the bottom of 25Kg vaccum sensitive stove CaO crucibles
Portion, then by top of the titanium sponge pine loaded on metallic aluminium.
（4）Alloy melting：The vacuum of vaccum sensitive stove is remained 0.02Pa first, then sent with the electrical power of 15KW
Electricity, after the argon gas that 0.3atm is filled with after 12 minutes, then increases power transmission power to 40KW, makes raw material rapid melting, to shorten conjunction
The time of contact of golden liquid and crucible, after alloy melting after power transmission 12 minutes, the maximum temperature of aluminium alloy is 1605 DEG C after fusing.
（5）Cooling casting：Have a power failure cooling 40s, is cast when aluminium alloy temperature is 1550 DEG C, so as to obtain alloy casting
Ingot.
The performance of alloy cast ingot manufactured in the present embodiment is referring to table 1.
Ingot blank prepared by embodiment 3 is tested using the ultrasonic examination method of inspection in the same manner as in Example 1, is cast
Ingot section ultrasonic examination figure referring to Fig. 3, without rimhole.
In order to further illustrate advantages of the present invention, four comparative examples are as follows.
Comparative example 1
Titanium-aluminium alloy target material manufactured in the present embodiment is made up of following element by weight percentage：Ti64%, Al36%.
Manufacture method is powder sintering, specific as follows：
（1）It is prepared by powder：The titanium-aluminium alloy powder for meeting mentioned component ratio requirement is obtained using atomization drying method, puts down
Equal particle diameter is 130 μm.
（2）Isostatic cool pressing：The powder that will be mixed is fitted into cold isostatic mould, and 30min is suppressed under 2 tons of pressure.
（3）Degassing：Isostatic cool pressing base is put into the iron jacket being made ready beforehand for, is placed in degasification furnace and is de-gassed treatment,
Degassing temperature is 400 DEG C, and degassing time is 20h.
（4）HIP sintering：The jacket that finishes of deaerating is put into compacting sintering in hot isostatic apparatus, and temperature is 1200
DEG C, time 3h, pressure is 120MPa.
The performance of alloy target material prepared by this comparative example is referring to table 1.
Comparative example 2
Titanium-aluminium alloy target material manufactured in the present embodiment is made up of following element by weight percentage：Ti64%, Al36%.
Manufacture method be cold crucible, vacuum suspension stove melting and casting method, it is specific as follows：
（1）Dispensing：The metallic aluminium of 0 grade of titanium sponge and purity higher than 99.99% is weighed respectively by above-mentioned design of alloy.
（2）Piezoelectricity pole：Titanium sponge and metal aluminum blocks are pressed into the electrode block being adapted with water jacketed copper crucible size.
（3）Shove charge：Electrode block is put into the water jacketed copper crucible of vacuum suspension stove.
（4）Alloy melting：The vacuum of vacuum suspension stove is remained 0.03Pa first, be powered and heat up, output current is
150A, power output is 45~55kW, electrode block is melted rapidly, 7~10min of smelting time.
（5）Cooling casting：Have a power failure cooling 60s, automatic casting is carried out when aluminium alloy temperature is 1650 DEG C, so as to be closed
Golden ingot casting.
The performance of alloy cast ingot prepared by this comparative example is referring to table 1.
Comparative example 3
The comparative example eliminates the baking material step in embodiment 1, and other are same as Example 1.
The performance of alloy cast ingot prepared by this comparative example is referring to table 1.
Ingot blank prepared by comparative example 3 is tested using the ultrasonic examination method of inspection in the same manner as in Example 1, is cast
The ultrasonic examination figure of ingot section participates in Fig. 4, and the white portion irised out in figure is internal porosity accumulation regions, and size is 3~5mm.
Comparative example 4
Alloy melting step in embodiment 1 is changed into：The vacuum of vaccum sensitive stove is set to remain 0.03Pa first, then
So that the argon gas of 0.2atm can be filled with after the electrical power power transmission of 15KW, 25min melting sources are treated；Other are same as Example 1.
The performance of alloy cast ingot prepared by this comparative example is referring to table 1.
Ingot blank prepared by comparative example 4 is tested using the ultrasonic examination method of inspection in the same manner as in Example 1, is cast
The ultrasonic examination figure of ingot section is referring to Fig. 5.The white portion irised out in figure is internal porosity accumulation regions, and size is 1~2mm.
The performance table of the embodiment of the present invention of table 1 and comparative example product
Note：Because comparative example 3 eliminates baking material step, so the alloy melting step of comparative example 3 will reach and embodiment 1
Identical vacuum needs consumption longer pumpdown time, thus fusion process compared to embodiment 1 will 10min long, be
35min。
Claims (3)
1. a kind of vacuum induction melting method of titanium-aluminium alloy target material, it is characterised in that vacuum induction is carried out using CaO crucibles and is melted
The standby titanium-aluminium alloy target material of refining, successively including batching step, baking material step, shove charge step, alloy melting step and casting step
Suddenly, wherein：
In the baking material step, the feed metal aluminium and titanium sponge that will be prepared are put into vacuum drying oven, baking temperature be less than
150 DEG C, baking time is, no less than 4 hours, to be then cooled to less than 40 DEG C with stove and take out stand-by；
In the shove charge step, toasted feed metal aluminium is put into the bottom of the CaO crucibles of vaccum sensitive stove, then by sea
Continuous top of the titanium pine loaded on metallic aluminium；
In the alloy melting step, the vacuum of the vaccum sensitive stove is set to remain 0.01-0.08Pa first, then with
The electrical power power transmission of 10-15kW, after the inert gas that 0.2~0.4atm is filled with after 10~15 minutes, then increases power transmission power
To 35-40kW, make raw material rapid melting, the maximum temperature of aluminium alloy is controlled at 1580~1610 DEG C after fusing,
In the casting step, cast when aluminium alloy temperature is higher than more than aluminium alloy melting temperature 30~50 DEG C.
2. the vacuum induction melting method of titanium-aluminium alloy target material according to claim 1, it is characterised in that the dispensing step
Suddenly it is to weigh the metallic aluminium of 0 grade of titanium sponge and purity higher than 99.99% respectively by the requirement of titanium-aluminium alloy composition design, wherein described
Titanium-aluminium alloy constitutes Ti by following element by weight percentage：60~70%, Al：30~40%.
3. the vacuum induction melting method of titanium-aluminium alloy target material according to claim 1, it is characterised in that in the baking material
In step, the baking temperature is 100-140 DEG C, and the baking time is 4-5h, and the vacuum of the vacuum drying oven is 600-
6000Pa。
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| CN109402426A (en) * | 2018-12-29 | 2019-03-01 | 宝鸡长征金属材料有限公司 | A kind of preparation method of fine grain three-element catalytic vacuum melting TiAl target |
| CN112725658B (en) * | 2020-12-10 | 2022-01-18 | 先导薄膜材料（广东）有限公司 | Preparation method of titanium-aluminum alloy target |
| CN113293311B (en) * | 2021-05-28 | 2022-12-09 | 金川集团股份有限公司 | Method for preparing high-purity nickel ingot by vacuum induction cold crucible smelting |
| CN113529027A (en) * | 2021-05-31 | 2021-10-22 | 洛阳科威钨钼有限公司 | Preparation method of high-purity oxygen-free copper sputtering coating target material |
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| JPS61223172A (en) * | 1985-03-29 | 1986-10-03 | Natl Res Inst For Metals | Manufacture of intermetallic compound tial base alloy |
| JP3694341B2 (en) * | 1994-03-10 | 2005-09-14 | 新日本製鐵株式会社 | TiAl intermetallic compound based alloy material with excellent high temperature characteristics and method for producing the same |
| CN1164780C (en) * | 2001-12-25 | 2004-09-01 | 中国科学院金属研究所 | Process for vacuum induction smelting of Ti-Al-Nb-B alloy |
| CN101994017A (en) * | 2009-08-25 | 2011-03-30 | 周晓君 | Process for melting silver palladium aluminum and zinc alloy through vacuum induction |
| CN103074520A (en) * | 2013-01-14 | 2013-05-01 | 北京工业大学 | Er-containing high-niobium Ti-Al intermetallic compound material and preparation method thereof |
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