CN100531971C - Method for preparing two-phase titanium alloy powder - Google Patents
Method for preparing two-phase titanium alloy powder Download PDFInfo
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- CN100531971C CN100531971C CNB2007100474991A CN200710047499A CN100531971C CN 100531971 C CN100531971 C CN 100531971C CN B2007100474991 A CNB2007100474991 A CN B2007100474991A CN 200710047499 A CN200710047499 A CN 200710047499A CN 100531971 C CN100531971 C CN 100531971C
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Abstract
The present invention discloses a preparation method of two-phase titanium alloy powder. Said preparation method includes the following steps: A, cutting the ingot casting of titanium alloy into the form of block and placing it into a vacuum sealed quartz glass tube lined with CaO crucible; B, melting mother alloy in the quartz glass tube and quickly cooling to obtain two-phase titanium alloy thin-band; and C, pulverizing the titanium alloy thin-band and placing the pulverized titanium alloy thin-band into a ball grinding mill, ball-grinding to obtain the alloy powder with 18-23 micron, then adopting inert gas or reducing gas to make protection to obtain titanium alloy powder and making dehydrogenization treatment.
Description
Technical field
The present invention relates to a kind of preparation method who prepares two-phase titanium alloy powder.
Background technology
Industrial titanium and titanium alloy powder mainly contain following four kinds of methods: 1. sodium reduction spongy titanium powder.This kind powder output is big, low price, and powder plasticity is good, is suitable for cold forming, is the primary raw material of producing general anti-corrosion goods.But because of it contains higher sodium and chlorion, easy contaminated equipment and material welding performance is degenerated during sintering.2. electrolysis titanium valve.Purity is than the spongy titanium powder height of sodium reduction, but the formability of electrolysis titanium valve is poor than the titanium sponge powder.3. hydrogenation dehydrogenation titanium valve.By the hydrogenation dehydrogenating technology can obtain that quality is good, the titanium valve of fine size and alloy powder thereof; But batch is little, price is more expensive.4. centrifugal atomizing titanium valve.The sixties, U.S.'s nuclear metal company at first adopted the electric arc rotary electrode method to make the pre-alloyed powder of titanium.Powder is spherical in shape.This alloy powder purity height, composition are evenly, good fluidity, loading density be 65% of theoretical value.This kind powder only should adopt hot forming, and the available heat isostatic pressing process is made complex-shaped part.Electric arc rotation electrode flouring technology is a tungsten bar because an electrode is arranged, and the tungstenic amount in the powder reaches 400ppm, so be easy to generate the pollution of tungsten, can reduce the fatigue behaviour of material.For eliminating the pollution of tungsten, having developed again with electron beam or plasma is the rotation electrode and the multiple centrifugal atomizing flouring technologies such as electric arc rotation crucible and electron beam rotating disc of thermal source.This type of powder is a primary raw material of making the metallurgical aviation part of titanium powder.These all are the methods for preparing titanium metal powder, seldom have method directly to produce titanium alloy powder.The present invention intends adopting rapid solidification/mechanical ball milling legal system to be equipped with titanium alloy powder.
Rapid solidification is meant by the quick cooling (〉=10 to alloy melt
4～10
6K/s) or the heterogeneous body forming core contained that make alloy under very big cooling velocity, high growth rates takes place, and (〉=1～100cm/s) solidifies.Since process of setting cold soon, the initial nucleation degree of supercooling is big, how the growth rate height makes solid liquid interface depart from balance, thereby presents the different tissue of a series of and conventional alloy architectural feature.Quicken what caused tissue of freezing rate and architectural feature of cooling velocity.
High-energy ball milling is the solid-state synthetic method commonly used of the various materials of preparation, and the large-scale industrial application of machine-alloying starts from the sixties in 20th century.Machine-alloying obtains alloy powder by mixing simple metal according to certain proportioning and it being carried out ball milling, and its shortcoming is the well living reaction of hybrid concurrency of alloy system that has, and therefore can not prepare with this method.
Summary of the invention
The present invention provides a kind of easy enforcement according to deficiency of the prior art, can prepare particle profile rule, the method for the titanium alloy powder of surfacing.
For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of preparation method of two-phase titanium alloy powder comprises the steps:
A, the ingot casting of titanium alloy is cut into bulk, vacuum seal is in the quartz glass tube that is lined with the CaO crucible;
Foundry alloy in B, the fused silica glass pipe, cooling promptly gets the diphasic titanium alloy strip fast again;
C, the titanium alloy strip after the fragmentation is put into ball mill, ball milling obtains the alloy powder of 18-23 μ m, and adopts inert gas or reducibility gas protection, obtains titanium alloy powder, and carries out dehydrogenation and handle.
Wherein, described titanium alloy is the TC6 alloy, is Ti
6Al
2.5Mo
2Cr
0.3Si
0.5The Fe diphasic titanium alloy.
Wherein: in the described steps A, use wire cutting machine that foundry alloy is cut into the bulk of 8～10mm * 3～5mm * 2～4mm, and utilize polishing machine to polish off the oxide layer of block surface.
Wherein: in the described steps A, quartz glass tube vacuum is 10
-3～10
-4Pa.
Wherein: among the described step B, adopt heating in medium frequency equipment fusion foundry alloy.
Wherein: among the described step B, adopt the output oscillating current of 600～900A, the melting time is 20～60s, is heated to 1800 ℃～2000 ℃.
Wherein, among the described step B, alloy molten fully after, in quartz ampoule, feed argon gas, utilize argon pressure the titanium alloy of fusion to be ejected into cooling fast on the water-cooled copper roller of rotation.During cooling, titanium alloy is ejected on the copper roller with extremely thin one deck, can moment from the molten condition cool to room temperature, generally being no more than 1 second can cool off.
Wherein, among the described step B, feed argon gas, making the pressure in the quartz ampoule is 10～20kPa.
Wherein, described copper roller rotating speed is 600r/min～1000r/min.
Wherein, behind the preparation titanium alloy strip, the titanium alloy strip is carried out annealing in process in described step B, annealing temperature is 250～350 ℃, and temperature retention time is 0.5～1 hour, cool to 100～150 ℃ then with the furnace after air cooling to room temperature.
Wherein: among the described step C, select the ball mill of agate jar and abrading-ball for use, material ball ratio is 15～20:1, ball milling time 3h～5h.
Wherein: among the described step C, the dehydrogenation treatment temperature is 400 ℃～500 ℃.
The preparation method that the present invention adopts is the preparation technology that single roller rapid quenching combines with mechanical ball milling.Obtain the titanium alloy strip by the single roller rapid quenching rapid solidification earlier, again strip is carried out high-energy ball milling, move back hydrogen and handle acquisition Ti alloy with high performance powder.
In the above-mentioned steps A, liner CaO crucible is for preventing molten titanium alloy and quartz glass tube reaction, avoid introducing Si impurity in the quartz glass tube, and avoids that the too high glass tube that makes of temperature breaks in the fusion process.There is a piston that has a conduit quartz glass tube upper end, can vacuumize to handle and add protective atmosphere to quartz glass tube by conduit and handle.Before foundry alloy is heated quartz ampoule is vacuumized processing, prevent that impurity from sneaking in the alloy, vacuum is about 10
-3～10
-4Pa.
In the above-mentioned steps A, it is long-pending in order to increase alloy surface that foundry alloy is cut into small pieces, and is beneficial to Fast Heating and dissolves.
Among the above-mentioned step B, utilize the Frequency Induction Heating mode, control heating power by the current/voltage of regulating in the induction coil, initial heating power is 5kW, treats that alloy progressively is increased to about 20kW after rubescent, melts fully until alloy.After melting fully, alloy to continue to heat 3～5 minutes, melt is stirred under faradic effect, in quartz glass tube, feed argon gas then, when air pressure reaches 10～20kPa, melt is overcoming the water-cooled copper roller surface that surface tension is rotated at a high speed below the nozzle ejection of quartz ampoule lower end arrives under the gas pressure effect, the moment that melt and copper roller surface contact solidifies rapidly and throws forward with the form of strip under the centrifugal action that the copper roller rotates and shoots out, thus acquisition Ti-Al-Mo-Cr-Si-Fe strip.
Among the above-mentioned step B, because the formation of strip is cooled off realization rapidly by alloy material under the condition of high temperature, the caused matrix distortion of lattice of distortion of lattice and impurity element meeting causes material internal to produce internal stress, thereby can handle by subsequent annealing and eliminate internal stress, annealing temperature is below crystallization temperature.According to the thermodynamic property of material composition, annealing process is decided to be 200～350 ℃ of insulations 0.5～1 hour down among the present invention, cool to 100～150 ℃ with the furnace after air cooling to room temperature.
Among the above-mentioned step C, the range of choice of material ball ratio is that 15-20:1 is for strip powder and steel ball are fully ground, and the ball milling time is that 3h-5h is in order to prevent that the powder internal stress from increasing.
Among the above-mentioned step C, the dehydrogenation treatment temperature is 400 ℃～500 ℃.
The single roller fast rotational of the simple Frequency Induction Heating of use of the present invention rapid cooling method prepares the titanium alloy strip.Because titanium alloy is active big, therefore the fusing point height prolongation heat time heating time that should be suitable in the process that adopts eddy-current heating, thoroughly melts titanium alloy, to guarantee that the alloy thing is consistent with parent phase in the final strip that obtains.
Beneficial effect of the present invention: Technical Board is limited to the production of Titanium (powder), the preparation of little titanium alloy powder at present.In the scope that impurity content allows, the present invention adopts comparatively direct mode successfully to prepare the alloy powder of titanium, and preparation technology is simple, easy operating.
Description of drawings
The Ti of Fig. 1 embodiment 1 preparation
6-Al
2.5-Mo
2-Cr
0.3-Si
0.5The XRD diffraction spectrogram of-Fe two-phase titanium alloy powder and foundry alloy
The Ti of embodiment 1 preparation as shown in Figure 1
6-Al
2.5-Mo
2-Cr
0.3-Si
0.5In the XRD diffraction spectra of-Fe two-phase titanium alloy powder, as can be seen, powder spectral line and foundry alloy spectral line are identical substantially, illustrate that gained alloy powder basis does not change.
The Ti of Fig. 2 embodiment 1 preparation
6-Al
2.5-Mo
2-Cr
0.3-Si
0.5The SEM photo of-Fe two-phase titanium alloy powder
The Ti of embodiment 1 preparation as shown in Figure 2
6-Al
2.5-Mo
2-Cr
0.3-Si
0.5Among the SEM figure of-Fe powder, as can be seen, being characterized as of the alloy powder after low temperature and middle temperature dehydrogenation is polygonal granular or packaged, particle profile rule, and surfacing, corner angle are clearly demarcated.This explanation when dehydrogenation between powder particle agglomeration very little.In addition, as can be seen, powder diameter is 19 μ m from SEM figure.
The specific embodiment
Embodiment 1
With foundry alloy for the TC6 titanium alloy cuts into the cubed pieces of size about 8～10mm * 3～5mm * 2～4mm, polish wait the cleaning surfaces processing after, be encapsulated in the quartz glass tube that has zirconia crucible and nozzle, be evacuated to 10
-4Pa.With Intermediate Frequency Induction Heating Equipment quartz ampoule is heated, the output oscillating current of Intermediate Frequency Induction Heating Equipment is 600A, initial heating power is 5kW, treat that alloy progressively is increased to 15kW after rubescent, melting time is 20s, be heated to 1800 ℃, alloy melts the back fully and continues heating 5 minutes, alloy is stirred, feed argon gas then in quartz ampoule, ar pressure is 15kPa, and melt is ejected on the high speed copper roller rotating from the nozzle of quartz ampoule lower end fast under the argon pressure effect, copper roller rotating speed 800r/min, rapid solidification obtains the strip that wide 15mm thickness is about 100 μ m.Strip is carried out the vacuum stress relief annealing handles, 300 ℃ of insulations one hour down, cool to the furnace 100 ℃ then air cooling to room temperature.Again the titanium alloy strip is put into ball mill, adopt argon shield to carry out ball milling, ratio of grinding media to material 20:1, ball milling time 3h carries out dehydrogenation to powder subsequently and handles under 400 ℃, obtain titanium alloy powder.
Embodiment 2
With foundry alloy for the TC6 titanium alloy cuts into the cubed pieces of size about 8～10mm * 3～5mm * 2～4mm, polish wait the cleaning surfaces processing after, be encapsulated in the quartz glass tube that has zirconia crucible and nozzle, be evacuated to 10
-4Pa.With Intermediate Frequency Induction Heating Equipment quartz ampoule is heated, the output oscillating current of Intermediate Frequency Induction Heating Equipment is 800A, initial heating power is 5kW, treat that alloy progressively is increased to 15kW after rubescent, melting time is 40S, be heated to 1900 ℃, alloy melts the back fully and continues heating 5 minutes, alloy is stirred, feed argon gas then in quartz ampoule, ar pressure is 20kPa, and melt is ejected on the high speed copper roller rotating from the nozzle of quartz ampoule lower end fast under the argon pressure effect, copper roller rotating speed 1000r/min, rapid solidification obtains the strip that wide 15mm thickness is about 80 μ m.Strip is carried out the vacuum stress relief annealing handles, at 250 ℃ down after insulation half an hour, cool to the furnace 100 ℃ then air cooling to room temperature.Again the titanium alloy strip is put into ball mill, adopt argon shield to carry out ball milling, ratio of grinding media to material 20:1, ball milling time 3h carries out dehydrogenation to powder subsequently and handles under 450 ℃, obtain titanium alloy powder.
With foundry alloy for the TC6 titanium alloy cuts into the cubed pieces of size about 8～10mm * 3～5mm * 2～4mm, polish wait the cleaning surfaces processing after, be encapsulated in the quartz glass tube that has zirconia crucible and nozzle, be evacuated to 10
-4Pa.With Intermediate Frequency Induction Heating Equipment quartz ampoule is heated, the output oscillating current of Intermediate Frequency Induction Heating Equipment is 900A, initial heating power is 5kW, treat that alloy progressively is increased to 15kW after rubescent, melting time is 50S, be heated to 2000 ℃, alloy melts the back fully and continues heating 5 minutes, alloy is stirred, feed argon gas then in quartz ampoule, ar pressure is 16kPa, and melt is ejected on the high speed copper roller rotating from the nozzle of quartz ampoule lower end fast under the argon pressure effect, copper roller rotating speed 800r/min, rapid solidification obtains the strip that wide 15mm thickness is about 100 μ m.Strip is carried out the vacuum stress relief annealing handles, 200 ℃ of insulations after a hour down, cool to the furnace 150 ℃ then air cooling to room temperature.Again the titanium alloy strip is put into ball mill, adopt argon shield to carry out ball milling, ratio of grinding media to material 18:1, ball milling time 5h carries out dehydrogenation to powder subsequently and handles, and dehydrogenation is handled 450 ℃, obtains titanium alloy powder.
Embodiment 4
With foundry alloy for the TC6 titanium alloy cuts into the cubed pieces of size about 8～10mm * 3～5mm * 2～4mm, polish wait the cleaning surfaces processing after, be encapsulated in the quartz glass tube that has zirconia crucible and nozzle, be evacuated to 10
-4Pa.With Intermediate Frequency Induction Heating Equipment quartz ampoule is heated, the output oscillating current of Intermediate Frequency Induction Heating Equipment is 850A, initial heating power is 5kW, treat that alloy progressively is increased to 15kW after rubescent, melting time is 60S, be heated to 1850 ℃, alloy melts the back fully and continues heating 5 minutes, alloy is stirred, feed argon gas then in quartz ampoule, ar pressure is 17kPa, and melt is ejected on the high speed copper roller rotating from the nozzle of quartz ampoule lower end fast under the argon pressure effect, copper roller rotating speed 800r/min, rapid solidification obtains the strip that wide 15mm thickness is about 100 μ m.Strip is carried out the vacuum stress relief annealing handles, 300 ℃ of insulations after a hour down, cool to the furnace 130 ℃ then air cooling to room temperature.Again the titanium alloy strip is put into ball mill, adopt argon shield to carry out ball milling, ratio of grinding media to material 17:1, ball milling time 3h carries out dehydrogenation to powder subsequently and handles under 430 ℃, obtain titanium alloy powder.
Embodiment 5
With foundry alloy for the TC6 titanium alloy cuts into the cubed pieces of size about 8～10mm * 3～5mm * 2～4mm, polish wait the cleaning surfaces processing after, be encapsulated in the quartz glass tube that has zirconia crucible and nozzle, be evacuated to 10
-4Pa.With Intermediate Frequency Induction Heating Equipment quartz ampoule is heated, the output oscillating current of Intermediate Frequency Induction Heating Equipment is 750A, initial heating power is 5kW, treat that alloy progressively is increased to 15kW after rubescent, melting time is 30S, be heated to 1950 ℃, alloy melts the back fully and continues heating 5 minutes, alloy is stirred, feed argon gas then in quartz ampoule, ar pressure is 18kPa, and melt is ejected on the high speed copper roller rotating from the nozzle of quartz ampoule lower end fast under the argon pressure effect, copper roller rotating speed 800r/min, rapid solidification obtains the strip that wide 15mm thickness is about 100 μ m.Strip is carried out the vacuum stress relief annealing handles, 350 ℃ of insulations after a hour down, cool to the furnace 120 ℃ then air cooling to room temperature.Again the titanium alloy strip is put into ball mill, adopt argon shield to carry out ball milling, ratio of grinding media to material 20:1, ball milling time 4h carries out dehydrogenation to powder subsequently and handles under 470 ℃, obtain titanium alloy powder.
The foregoing description only is used for that the present invention will be described, does not constitute the restriction to the claim scope, and other substantial equivalence means that it may occur to persons skilled in the art that are all in claim scope of the present invention.
Claims (9)
1, a kind of preparation method of two-phase titanium alloy powder comprises the steps:
A, the ingot casting of titanium alloy is cut into bulk, vacuum seal is in the quartz glass tube that is lined with the CaO crucible;
Foundry alloy in B, the fused silica glass pipe, alloy molten fully after, in quartz ampoule, feed argon gas, cooling obtains the diphasic titanium alloy strip thereby utilize argon pressure the titanium alloy of fusion to be ejected on the water-cooled copper roller of rotation fast;
C, the titanium alloy strip after the fragmentation is put into ball mill, ball milling obtains the alloy powder of 18-23 μ m, and adopts inert gas or reducibility gas protection, and obtain titanium alloy powder, and carry out dehydrogenation and handle,
Wherein, described titanium alloy is the TC6 alloy.
2, the preparation method of two-phase titanium alloy powder according to claim 1, it is characterized in that: in the described steps A, use wire cutting machine that the ingot casting of titanium alloy is cut into the bulk of 8～10mm * 3～5mm * 2～4mm, and utilize polishing machine to polish off the oxide layer of block surface.
3, the preparation method of two-phase titanium alloy powder according to claim 1 is characterized in that: in the described steps A, quartz glass tube vacuum is 10-3～10
-4Pa.
4, the preparation method of two-phase titanium alloy powder according to claim 1 is characterized in that: among the described step B, adopt heating in medium frequency equipment fusion foundry alloy.
5, the preparation method of two-phase titanium alloy powder according to claim 4 is characterized in that: among the described step B, adopt the output oscillating current of 600～900A, the melting time is 20～60s, is heated to 1800 ℃～2000 ℃.
6, the preparation method of two-phase titanium alloy powder according to claim 1 is characterized in that, among the described step B, feeds argon gas, and making the pressure in the quartz ampoule is 10～20kPa.
7, the preparation method of two-phase titanium alloy powder according to claim 1 is characterized in that, described copper roller rotating speed is 600r/min～1000r/min.
8, the preparation method of two-phase titanium alloy powder according to claim 1, it is characterized in that, after in described step B, preparing the titanium alloy strip, the titanium alloy strip is carried out annealing in process, annealing temperature is 200～350 ℃, temperature retention time is 0.5～1 hour, cool to 100～150 ℃ then with the furnace after air cooling to room temperature.
9, the preparation method of two-phase titanium alloy powder according to claim 1 is characterized in that: among the described step C, the dehydrogenation treatment temperature is 400 ℃～500 ℃.
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|---|---|---|---|
| CNB2007100474991A CN100531971C (en) | 2007-10-26 | 2007-10-26 | Method for preparing two-phase titanium alloy powder |
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|---|---|---|---|
| CNB2007100474991A CN100531971C (en) | 2007-10-26 | 2007-10-26 | Method for preparing two-phase titanium alloy powder |
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| CN100531971C true CN100531971C (en) | 2009-08-26 |
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| CN102756130A (en) * | 2012-07-11 | 2012-10-31 | 沈阳理工大学 | Preparation method of metal powder |
| CN103846447B (en) * | 2012-12-06 | 2016-04-27 | 北京有色金属研究总院 | The aerosolization preparation method of a kind of superfine spherical titanium or titanium alloy powder |
| CN111763847B (en) * | 2020-06-29 | 2021-07-06 | 西安斯瑞先进铜合金科技有限公司 | Method for preparing copper-titanium 50 intermediate alloy by using magnetic suspension smelting process |
| CN111647767B (en) * | 2020-06-29 | 2021-07-20 | 西安斯瑞先进铜合金科技有限公司 | Method for preparing CuTi25 intermediate alloy by using magnetic suspension smelting process |
| CN114160786B (en) * | 2021-11-25 | 2022-07-26 | 有研工程技术研究院有限公司 | Mixed powder type getter and preparation method thereof |
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