CN103752836A - Method for manufacturing spherical niobium and titanium-based alloy powder with small particle size - Google Patents
Method for manufacturing spherical niobium and titanium-based alloy powder with small particle size Download PDFInfo
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Abstract
The invention discloses a method for manufacturing spherical niobium and titanium-based alloy powder with a small particle size. The spherical niobium and titanium-based alloy powder is manufactured by the aid of vacuum induction melting, hydrogen treatment and plasma spheroidization technologies. The method includes firstly, manufacturing niobium and titanium-based spherical alloy ingots by the aid of the vacuum induction melting technology to realize a purification melting effect, reducing the quantity and the size of non-metallic inclusion to the greatest extent and performing homogenization thermal treatment on the niobium and titanium-based spherical alloy ingots to obtain ingots with uniform alloy contents; secondly, performing hydrogen treatment on the ingots to acquire hydrogen absorption niobium and titanium alloy powder; thirdly, sieving the hydrogen absorption niobium and titanium alloy powder, and then performing plasma spheroidization on the hydrogen absorption niobium and titanium alloy powder. The method has the advantages that output power, the powder feeding rate and the airflow rate are optimized in spheroidization procedures, accordingly, hollow powder can be prevented, and the fine powder yield can be increased; the spherical powder obtained by the method is excellent in dispersibility and flowability and uniform in particle size; the niobium and titanium-based alloy powder finally manufactured by the method is small in particle size, uniform in composition, good in flowability, high in spheroidization rate and low in oxygen content and is applicable to the technical field of injection molding, quick molding and thermal spraying.
Description
Technical field
The invention belongs to powder metallurgical technology, a kind of method of preparing the spherical niobium titanium-base alloy of fine grain powder is provided especially.
Background technology
Niobium titanium-base alloy has lower density, higher fusing point and good heat resistance, in Aero-Space and field of thermal spray, has important application prospect.PM technique is to prepare an important method of niobium titanium-base alloy parts, for example, adopt injection moulding, RP technique can prepare the parts of complicated shape.The parameters such as the performance of parts and the shape of material powder, particle diameter and size distribution are closely related.High-quality material powder is the precondition of exploitation powder metallurgy niobium titanium-base alloy.Injection moulding, RP technique material powder used requires that particle diameter is tiny, sphericity is better, oxygen content is low, good fluidity, and the niobium titanium alloy powder of used for hot spraying requires that sphericity is high, narrow particle size distribution, gas and impurity content is low, apparent density is suitable.
The difficult point of the spherical niobium-base alloy powder preparation of low oxygen content fine grain is mainly reflected in: the one, and the refinement of powder (particle diameter <10 μ m) and nodularization; The 2nd, the activity of niobium-base alloy is high, Control for Oxygen Content difficulty.The 3rd, the quantity of nonmetal inclusion and the control of particle diameter, reduce its impact on the mechanical behavior under high temperature of niobium-base alloy.At present, prepare the method that niobium-base alloy powder generally adopts high-energy ball milling, exist to introduce be mingled with, oxygen content is high, powder is reunited and the problem such as particle diameter is thick, out-of-shape, is not suitable for use in the material powder of injection moulding or fast shaping technology.The present invention adopts the quick-fried technique broken and that plasma spheroidization combines of hydrogen to prepare the spherical niobium titanium-base alloy of fine grain powder.The quick-fried broken technique of hydrogen is to utilize the characteristic of the intercrystalline cracking that alloy itself produces in Hydrogen absorption and desorption process of niobium titanium-base alloy and transgranular fracture to cause alloy pulverization, thereby obtains the irregular alloy powder of fine grain.Then, utilize radio frequency plasma spheronization techniques that irregular alloy powder is transformed into spherical niobium titanium alloy powder.The principle of radio frequency plasma nodularization is that powder particle in irregular shape is sprayed in plasma furnace by feeding gun by carrying gas, under radiation, convection current, conduction and four kinds of heat transfer mechanism effects of chemistry, heated rapidly and melted, melt granules forms spherical droplets under surface tension effects, and solidify rapidly, thereby obtain spherical powder under high thermograde.Adopt the feature of the niobium titanium alloy powder that the present invention prepares to be: particle diameter is tiny, composition is even, good fluidity, nodularization rate is high, oxygen content is low, is applicable to injection moulding, Quick-forming and technical field of hot.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing the spherical niobium titanium-base alloy of fine grain powder, be intended to solve a difficult problem for niobium titanium-base alloy powder fining, spheroidization and Control for Oxygen Content, the powder of preparing has advantages of that particle diameter is tiny, good sphericity, oxygen content are lower.
First the present invention adopts process for vacuum induction smelting to prepare niobium titanium-base alloy ingot casting, solves the problem of sublimate melting, manages to reduce quantity and the size of nonmetal inclusion, and carries out homogenising heat treatment, obtains the uniform ingot casting of alloying component.Then ingot casting is carried out to hydrogenation treatment, obtain and inhale hydrogen niobium titanium alloy powder.Finally carry out plasma spheroidization, in the process of nodularization, need to optimize power output, powder feeding rate and airflow rate, avoid the formation of hollow powder, improve fine powder recovery rate.Finally prepare dispersiveness and good fluidity, even-grained spherical niobium titanium-base alloy powder, preparation technology as shown in Figure 1.Concrete technology step has:
1, vacuum induction melting: take following raw material according to the composition of niobium titanium-base alloy: TiNb intermediate alloy, TiAl intermediate alloy, TiMo intermediate alloy, TiCr intermediate alloy, TiW intermediate alloy, sponge Zr, V piece, Nb rod and graphite.Before melting, metal mold is preheating to 350～400 ℃, to after the monitor system rising 170～190kW of water jacketed copper crucible vacuum induction melting furnace, stop increasing power, then under firm power, melting 1～3min obtains melt, obtains niobium titanium-base alloy ingot casting after cooling;
The composition of described niobium titanium-base alloy is: the Ti that the quality percentage composition of various alloying elements is 17～45%, 0～15% Al, 0～10% Mo, 0～5% V, 0～8% W, 0～5% Cr, 0～2.5% Zr, 0～0.05% C and the Nb of surplus.
2, homogenising heat treatment: niobium titanium-base alloy ingot casting is in Zhen Kong Du≤10
-2in the vacuum drying oven of Pa, carry out homogenizing annealing processing, homogenizing annealing treatment temperature is 800～1100 ℃, and temperature retention time is 1～3 hour, obtains the uniform niobium titanium-base alloy of alloying component ingot casting;
3, hydrogenation treatment: the method by mechanical disintegration is broken into niobium titanium-base alloy ingot casting on the fritter ingot casting of 10～30mm, and is placed in stainless steel pressure tank, and pressurized tank is evacuated down to 1.0 * 10
-3after Pa, pass into high-purity hydrogen to 0.1～1.0MPa, 700～800 ℃ of insulations 1～2 hour, obtaining particle diameter was the suction hydrogen niobium titanium-base alloy powder of 50～300 μ m, and powder is sieved, and obtains the suction hydrogen niobium titanium-base alloy powder that particle diameter is less than 120 μ m.
4, plasma nodularization: the suction hydrogen niobium titanium-base alloy powder that average grain diameter is less than to 120 μ m carries out plasma spheroidization, in plasma spheroidization process, inhale the hydrogen niobium titanium-base alloy powder quick-fried broken generation minute spherical niobium titanium-base alloy powder of hydrogen that absorbs heat rapidly, wherein powder feeding rate is 20～100gmin
-1, plasma power output is 50～90KW, vacuum is 1 * 10
-3pa.Finally obtain the spherical niobium titanium-base alloy of the fine grain powder of average grain diameter≤40 μ m.
The present invention adopts vacuum induction melting+hydrogenation treatment+plasma spheroidization technology to prepare fine grain spherical powder; The problem that has reduced contaminating impurity and Powder Oxidation in Mechanical Crushing technique, is conducive to the control of oxygen content.Employing radio frequency plasma is thermal source, and vacuum is plasma work atmosphere, reduces the oxidation of niobium titanium alloy powder in nodularization process, is conducive to control oxygen content and anti-dirtyization.The niobium titanium alloy powder of preparing has the features such as particle diameter is tiny, composition even, good fluidity, nodularization rate is high, oxygen content is low, is applicable to injection moulding, Quick-forming and technical field of hot.When this powder is used as the material powder of injection moulding, fine grain spherical powder, when improving powder flowbility and tap density, has improved powder loading, to improving the filling capacity of feeding and controlling sintering warpage and play important effect.During as hot spray powder, can effectively improve the mobility of powder, improve the bulk density of powder in coating.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention
The specific embodiment
Embodiment 1: preparation average grain diameter is the minute spherical Nb-45%Ti-3%Mo-0.5%Zr powder of 21 μ m
According to the composition of niobium titanium-base alloy, take following raw material: TiNb intermediate alloy, TiMo intermediate alloy, sponge zirconium and Nb rod.The Ti that in niobium titanium-base alloy, the quality percentage composition of Ti, Mo, Zr and Nb element is 45%, 3% Mo, 0.5% Zr and the Nb of surplus.Metal mold is preheating to 350 ℃ before melting, will after water jacketed copper crucible vacuum induction melting furnace monitor system rising 190kW, stops increasing power, then under firm power, melting 1min obtains melt, obtains niobium titanium-base alloy ingot casting after cooling; Niobium titanium-base alloy ingot casting is in Zhen Kong Du≤10
-2in the vacuum drying oven of Pa, carry out homogenizing annealing processing, homogenizing annealing treatment temperature is 800 ℃, and temperature retention time is 3 hours, obtains the uniform niobium titanium-base alloy of alloying component ingot casting; Method by mechanical disintegration is broken into niobium titanium-base alloy ingot casting on the fritter ingot casting of 20mm, and is placed in stainless steel pressure tank, and pressurized tank is evacuated down to 1.0 * 10
-3after Pa, pass into high-purity hydrogen to 0.1MPa, 700 ℃ of insulations 2 hours, obtain the suction hydrogen niobium titanium-base alloy powder that particle diameter is less than 110 μ m.Suction hydrogen niobium titanium-base alloy powder is carried out to plasma spheroidization, inhale the hydrogen niobium titanium-base alloy powder quick-fried broken generation minute spherical niobium titanium-base alloy powder of hydrogen that absorbs heat rapidly in plasma spheroidization process, wherein powder feeding rate is 80gmin
-1, plasma power output is 50KW, vacuum is 1 * 10
-3pa.Finally obtaining average grain diameter is the Nb-45%Ti-3%Mo-0.5%Zr alloy powder of 21 μ m.
Embodiment 2: preparation average grain diameter is the minute spherical Nb-40%Ti-6%Mo-1.5%Zr powder of 32 μ m
According to the composition of niobium titanium-base alloy, take following raw material: TiNb intermediate alloy, TiMo intermediate alloy, sponge zirconium and Nb rod.The Ti that in niobium titanium-base alloy, the quality percentage composition of Ti, Mo, Zr and Nb is 40%, 6% Mo, 1.5% Zr and the Nb of surplus.Metal mold is preheating to 400 ℃ before melting, will after water jacketed copper crucible vacuum induction melting furnace monitor system rising 180kW, stops increasing power, then under firm power, melting 2min obtains melt, obtains niobium titanium-base alloy ingot casting after cooling; Niobium titanium-base alloy ingot casting is in Zhen Kong Du≤10
-2in the vacuum drying oven of Pa, carry out homogenizing annealing processing, homogenizing annealing treatment temperature is 900 ℃, and temperature retention time is 2 hours, obtains the uniform niobium titanium-base alloy of alloying component ingot casting; Method by mechanical disintegration is broken into niobium titanium-base alloy ingot casting on the fritter ingot casting of 30mm, and is placed in stainless steel pressure tank, and pressurized tank is evacuated down to 1.0 * 10
-3after Pa, pass into high-purity hydrogen to 0.3MPa, 750 ℃ of insulations 1 hour, obtain the suction hydrogen niobium titanium-base alloy powder that particle diameter is less than 80 μ m.Suction hydrogen niobium titanium-base alloy powder is carried out to plasma spheroidization, inhale the hydrogen niobium titanium-base alloy powder quick-fried broken generation minute spherical niobium titanium-base alloy powder of hydrogen that absorbs heat rapidly in plasma spheroidization process, wherein powder feeding rate is 100gmin
-1, plasma power output is 60KW, vacuum is 1 * 10
-3pa.Finally obtaining average grain diameter is the Nb-40%Ti-6%Mo-1.5%Zr alloy powder of 32 μ m.
Embodiment 3: preparation average grain diameter is the minute spherical Nb-20%Ti-4%Al-3%Cr-5%V-4.5%W-0.03%C powder of 15 μ m
According to the composition of niobium titanium-base alloy, take following raw material: TiNb intermediate alloy, TiAl intermediate alloy, TiCr intermediate alloy, TiW intermediate alloy, V piece and Nb rod.In niobium titanium-base alloy, the content of various alloying elements is: 20% Ti, 4% Al, 3% Cr, 5% V, 4.5% W, 0.03% graphite and the Nb of surplus.Metal mold is preheating to 380 ℃ before melting, will after water jacketed copper crucible vacuum induction melting furnace monitor system rising 170kW, stops increasing power, then under firm power, melting 3min obtains melt, obtains niobium titanium-base alloy ingot casting after cooling; Niobium titanium-base alloy ingot casting is in Zhen Kong Du≤10
-2in the vacuum drying oven of Pa, carry out homogenizing annealing processing, homogenizing annealing treatment temperature is 1000 ℃, and temperature retention time is 1 hour, obtains the uniform niobium titanium-base alloy of alloying component ingot casting; Method by mechanical disintegration is broken into niobium titanium-base alloy ingot casting on the fritter ingot casting of 10mm, and is placed in stainless steel pressure tank, and pressurized tank is evacuated down to 1.0 * 10
-3after Pa, pass into high-purity hydrogen to 1.0MPa, 800 ℃ of insulations 1.5 hours, obtain the suction hydrogen niobium titanium-base alloy powder that particle diameter is less than 72 μ m.Suction hydrogen niobium titanium-base alloy powder is carried out to plasma spheroidization, inhale the hydrogen niobium titanium-base alloy powder quick-fried broken generation minute spherical niobium titanium-base alloy powder of hydrogen that absorbs heat rapidly in plasma spheroidization process, wherein powder feeding rate is 20gmin
-1, plasma power output is 70KW, vacuum is 1 * 10
-3pa.Obtaining average grain diameter is the Nb-20%Ti-4%Al-3%Cr-5%V-4.5%W-0.03%C alloy powder of 15 μ m.
Embodiment 4: preparation average grain diameter is the thin spherical Nb-38%Ti-5%Al-4.5%V-0.5%Zr-0.05%C powder of 30 μ m
According to the composition of niobium titanium-base alloy, take following raw material: TiAl intermediate alloy, sponge Zr, V piece, Nb rod and graphite.In niobium titanium-base alloy, the content of various alloying elements is: 38% Ti, 5% Al, 4.5% V, 0.5% Zr, 0.05% C and the Nb of surplus.Metal mold is preheating to 360 ℃ before melting, will after water jacketed copper crucible vacuum induction melting furnace monitor system rising 180kW, stops increasing power, then under firm power, melting 2min obtains melt, obtains niobium titanium-base alloy ingot casting after cooling; Niobium titanium-base alloy ingot casting is in Zhen Kong Du≤10
-2in the vacuum drying oven of Pa, carry out homogenizing annealing processing, homogenizing annealing treatment temperature is 1100 ℃, and temperature retention time is 2 hours, obtains the uniform niobium titanium-base alloy of alloying component ingot casting; Method by mechanical disintegration is broken into niobium titanium-base alloy ingot casting on the fritter ingot casting of 25mm, and is placed in stainless steel pressure tank, and pressurized tank is evacuated down to 1.0 * 10
-3after Pa, pass into high-purity hydrogen to 0.6MPa, 750 ℃ of insulations 1 hour, obtain the suction hydrogen niobium titanium-base alloy powder that particle diameter is less than 61 μ m.Suction hydrogen niobium titanium-base alloy powder is carried out to plasma spheroidization, inhale the hydrogen niobium titanium-base alloy powder quick-fried broken generation minute spherical niobium titanium-base alloy powder of hydrogen that absorbs heat rapidly in plasma spheroidization process, wherein powder feeding rate is 50gmin
-1, plasma power output is 80KW, vacuum is 1 * 10
-3pa.Obtaining average grain diameter is the Nb-38%Ti-5%Al-4.5%V-0.5%Zr-0.05%C alloy powder of 30 μ m.
Claims (4)
1. a method of preparing the spherical niobium titanium-base alloy of fine grain powder, is characterized in that:
Step 1, according to the composition of niobium titanium-base alloy, take following raw material: TiNb intermediate alloy, TiAl intermediate alloy, TiMo intermediate alloy, TiCr intermediate alloy, TiW intermediate alloy, sponge Zr, V piece, Nb rod and graphite; Before melting, metal mold is preheating to 350～400 ℃, after being brought up to 170～190kW, water jacketed copper crucible vacuum induction melting furnace monitor system stops increasing power, then under firm power, melting 1～3min obtains melt, obtains niobium titanium-base alloy ingot casting after cooling;
Step 2, niobium titanium-base alloy ingot casting are in Zhen Kong Du≤10
-2in the vacuum drying oven of Pa, carry out homogenizing annealing processing, homogenizing annealing treatment temperature is 800～1100 ℃, and temperature retention time is 1～3 hour, obtains the uniform niobium titanium-base alloy of alloying component ingot casting;
Step 3, the method by mechanical disintegration are broken into niobium titanium-base alloy ingot casting on the fritter ingot casting of 10～30mm, and are placed in stainless steel pressure tank, and pressurized tank is evacuated down to 1.0 * 10
-3after Pa, pass into high-purity hydrogen to 0.1～1.0MPa, 700～800 ℃ of insulations 1～2 hour, obtaining particle diameter was the suction hydrogen niobium titanium-base alloy powder of 50～300 μ m, and powder is sieved, and obtained the fine grained suction hydrogen niobium titanium-base alloy powder that particle diameter is less than 120 μ m;
Step 4, fine grained is inhaled to hydrogen niobium titanium-base alloy powder carry out plasma spheroidization, inhale the hydrogen niobium titanium-base alloy powder quick-fried broken generation minute spherical niobium titanium-base alloy powder of hydrogen that absorbs heat rapidly in plasma spheroidization process, wherein powder feeding rate is 20～100gmin
-1, plasma power output is 50～90KW, vacuum is 1 * 10
-3pa, finally obtains the spherical niobium titanium-base alloy of fine grain powder.
2. a kind of method of preparing the spherical niobium titanium-base alloy of fine grain powder according to claim 1, is characterized in that: the composition of niobium titanium-base alloy is: 17～45% Ti, 0～15% Al, 0～10% Mo, 0～5% V, 0～8% W, 0～5% Cr, 0～2.5% Zr, 0～0.05% C and the Nb of surplus.
3. a kind of method of preparing the spherical niobium titanium-base alloy of fine grain powder according to claim 1, is characterized in that: the particle diameter of inhaling hydrogen niobium titanium-base alloy powder is less than 100 μ m.
4. a kind of method of preparing the spherical niobium titanium-base alloy of fine grain powder according to claim 1, is characterized in that: the average grain diameter≤40 μ m of the spherical niobium titanium-base alloy of fine grain powder.
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