CN103752836B - A kind of method preparing fine grain spherical niobium titanium base alloy powder - Google Patents
A kind of method preparing fine grain spherical niobium titanium base alloy powder Download PDFInfo
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Abstract
The present invention adopts vacuum induction melting+hydrogenation treatment+plasma spheroidization technology to prepare fine grain spherical niobium titanium base alloy powder.First adopt process for vacuum induction smelting to prepare niobium titanium-base alloy ingot casting, solve the problem of sublimate melting, manage the quantity and the size that reduce nonmetal inclusion, and carry out homogenising heat treatment, obtain the uniform ingot casting of alloying component.Then hydrogenation treatment is carried out to ingot casting, obtain and inhale hydrogen niobium titanium alloy powder.Inhale hydrogen niobium titanium alloy powder and carry out plasma spheroidization after screening, in nodularization process, optimize power output, powder feeding rate and airflow rate, avoid hollow powder to be formed, improve fine powder recovery rate.Thus obtain dispersed and good fluidity, even-grained spherical powder.Finally prepare the niobium titanium base alloy powder that particle diameter is tiny, uniform composition, good fluidity, Oxygen potential are high, oxygen content is low.This powder is applicable to injection moulding, Quick-forming and technical field of hot.
Description
Technical field
The invention belongs to powder metallurgical technology, specifically provide a kind of method preparing fine grain spherical niobium titanium base alloy powder.
Background technology
Niobium titanium-base alloy has lower density, higher fusing point and good heat resistance, has important application prospect in Aero-Space and field of thermal spray.PM technique prepares an important method of niobium titanium-base alloy parts, such as, 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 niobium titanium alloy powder used for hot spraying then requires that sphericity is high, narrow particle size distribution, gas and impurity content are low, apparent density is suitable.
Difficult point prepared by low oxygen content fine grain spherical niobium base alloy powder is mainly reflected in: one is refinement (particle diameter <10 μm) and the nodularization of powder; Two is that the activity of niobium-base alloy is high, Control for Oxygen Content difficulty.Three is the quantity of nonmetal inclusion and the control of particle diameter, reduces 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, have that introducing is mingled with, oxygen content is high, powder reunites and the problem such as particle diameter is thick, out-of-shape, be not suitable for use in the material powder of injection moulding or fast shaping technology.The present invention adopts the quick-fried broken technique combined with plasma spheroidization of hydrogen to prepare fine grain spherical niobium titanium base alloy powder.The quick-fried broken technique of hydrogen utilizes 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, thus obtain 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 sprays in plasma furnace by carrying gas by feeding gun by powder particle in irregular shape, be heated rapidly under radiation, convection current, conduction and chemistry four kinds of heat transfer mechanism effects and melt, melt granules forms spherical droplets under surface tension effects, and under high thermograde quick solidification, thus obtain spherical powder.The feature of the niobium titanium alloy powder adopting the present invention to prepare is: particle diameter is tiny, uniform composition, good fluidity, Oxygen potential are 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 preparing fine grain spherical niobium titanium base alloy powder, be intended to solve a difficult problem for the refinement of niobium titanium base alloy powder, spheroidization and Control for Oxygen Content, the powder prepared has the advantage 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 the quantity and the size that reduce nonmetal inclusion, and carries out homogenising heat treatment, obtain the uniform ingot casting of alloying component.Then hydrogenation treatment is carried out to ingot casting, obtain and inhale hydrogen niobium titanium alloy powder.Finally carry out plasma spheroidization, need to optimize power output, powder feeding rate and airflow rate in the process of nodularization, avoid the formation of hollow powders, improve fine powder recovery rate.Finally prepare dispersed 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 block, Nb rod and graphite.Before melting, metal mold is preheating to 350 ~ 400 DEG C, increasing power is stopped after the monitor system of water jacketed copper crucible vacuum induction melting furnace is raised 170 ~ 190kW, 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 mass percentage of various alloying element be 17 ~ 45% Ti, 0 ~ 15% Al, 0 ~ 10% Mo, 0 ~ 5% V, 0 ~ 8% W, Cr, the Zr of 0 ~ 2.5% of 0 ~ 5%, the Nb of the C of 0 ~ 0.05% and surplus.
2, homogenising heat treatment: niobium titanium-base alloy ingot casting is in Zhen Kong Du≤10
-2carry out homogenizing annealing process in the vacuum drying oven of Pa, homogenizing annealing treatment temperature is 800 ~ 1100 DEG C, and temperature retention time is 1 ~ 3 hour, obtains alloying component uniform niobium titanium-base alloy ingot casting;
3, hydrogenation treatment: the fritter ingot casting by the method for mechanical crushing, niobium titanium-base alloy ingot casting being broken into 10 ~ 30mm, and be placed in stainless steel pressure tank, pressurized tank is evacuated down to 1.0 × 10
-3pass into high-purity hydrogen after Pa to 0.1 ~ 1.0MPa, 700 ~ 800 DEG C of insulations 1 ~ 2 hour, obtain the suction hydrogen niobium titanium base alloy powder that particle diameter is 50 ~ 300 μm, powder is sieved, obtain the suction hydrogen niobium titanium base alloy powder that particle diameter is less than 120 μm.
4, plasma spheroidization: suction hydrogen niobium titanium base alloy powder average grain diameter being less than 120 μm carries out plasma spheroidization, inhale hydrogen niobium titanium base alloy powder in plasma spheroidization process to absorb heat rapidly the quick-fried broken generation minute spherical niobium titanium base alloy powder of hydrogen, wherein powder feeding rate is 20 ~ 100gmin
-1, plasma power output is 50 ~ 90KW, and vacuum is 1 × 10
-3pa.Finally obtain the fine grain spherical niobium titanium base alloy powder of average grain diameter≤40 μm.
The present invention adopts vacuum induction melting+hydrogenation treatment+plasma spheroidization technology to prepare fine grain spherical powder; Decrease the problem of contaminating impurity and Powder Oxidation in Mechanical Crushing technique, be 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 controlling oxygen content and anti-dirtyization.The niobium titanium alloy powder prepared has the features such as particle diameter is tiny, uniform composition, good fluidity, Oxygen potential are 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, while raising powder flowbility and tap density, improves powder loading, plays important effect to the filling capacity and control sintering warpage improving feeding.During as hot spray powder, effectively can 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
Detailed description of the invention
Embodiment 1: preparation average grain diameter is the minute spherical Nb-45%Ti-3%Mo-0.5%Zr powder of 21 μm
Following raw material is taken: TiNb intermediate alloy, TiMo intermediate alloy, sponge zirconium and Nb rod according to the composition of niobium titanium-base alloy.In niobium titanium-base alloy, the mass percentage of Ti, Mo, Zr and Nb element is Ti, the Mo of 3% of 45%, the Nb of the Zr of 0.5% and surplus.Before melting, metal mold is preheating to 350 DEG C, stop increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system is raised 190kW, 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
-2carry out homogenizing annealing process in the vacuum drying oven of Pa, homogenizing annealing treatment temperature is 800 DEG C, and temperature retention time is 3 hours, obtains alloying component uniform niobium titanium-base alloy ingot casting; By the method for mechanical crushing, niobium titanium-base alloy ingot casting is broken into the fritter ingot casting of 20mm, and is placed in stainless steel pressure tank, pressurized tank is evacuated down to 1.0 × 10
-3pass into high-purity hydrogen after Pa to 0.1MPa, 700 DEG C of insulations 2 hours, obtain the suction hydrogen niobium titanium base alloy powder that particle diameter is less than 110 μm.Suction hydrogen niobium titanium base alloy powder is carried out plasma spheroidization, and inhale hydrogen niobium titanium base alloy powder in plasma spheroidization process and to absorb heat rapidly the quick-fried broken generation minute spherical niobium titanium base alloy powder of hydrogen, wherein powder feeding rate is 80gmin
-1, plasma power output is 50KW, and vacuum is 1 × 10
-3pa.Finally obtain the Nb-45%Ti-3%Mo-0.5%Zr alloy powder that average grain diameter is 21 μm.
Embodiment 2: preparation average grain diameter is the minute spherical Nb-40%Ti-6%Mo-1.5%Zr powder of 32 μm
Following raw material is taken: TiNb intermediate alloy, TiMo intermediate alloy, sponge zirconium and Nb rod according to the composition of niobium titanium-base alloy.In niobium titanium-base alloy, the mass percentage of Ti, Mo, Zr and Nb is Ti, the Mo of 6% of 40%, the Nb of the Zr of 1.5% and surplus.Before melting, metal mold is preheating to 400 DEG C, stop increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system is raised 180kW, 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
-2carry out homogenizing annealing process in the vacuum drying oven of Pa, homogenizing annealing treatment temperature is 900 DEG C, and temperature retention time is 2 hours, obtains alloying component uniform niobium titanium-base alloy ingot casting; By the method for mechanical crushing, niobium titanium-base alloy ingot casting is broken into the fritter ingot casting of 30mm, and is placed in stainless steel pressure tank, pressurized tank is evacuated down to 1.0 × 10
-3pass into high-purity hydrogen after Pa to 0.3MPa, 750 DEG C of insulations 1 hour, obtain the suction hydrogen niobium titanium base alloy powder that particle diameter is less than 80 μm.Suction hydrogen niobium titanium base alloy powder is carried out plasma spheroidization, and inhale hydrogen niobium titanium base alloy powder in plasma spheroidization process and to absorb heat rapidly the quick-fried broken generation minute spherical niobium titanium base alloy powder of hydrogen, wherein powder feeding rate is 100gmin
-1, plasma power output is 60KW, and vacuum is 1 × 10
-3pa.Finally obtain the Nb-40%Ti-6%Mo-1.5%Zr alloy powder that average grain diameter is 32 μm.
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 μm
Following raw material is taken: TiNb intermediate alloy, TiAl intermediate alloy, TiCr intermediate alloy, TiW intermediate alloy, V block and Nb rod according to the composition of niobium titanium-base alloy.In niobium titanium-base alloy, the content of various alloying element is: the Ti of 20%, the Al of 4%, 3% Cr, V, the W of 4.5% of 5%, the Nb of the graphite of 0.03% and surplus.Before melting, metal mold is preheating to 380 DEG C, stop increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system is raised 170kW, 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
-2carry out homogenizing annealing process in the vacuum drying oven of Pa, homogenizing annealing treatment temperature is 1000 DEG C, and temperature retention time is 1 hour, obtains alloying component uniform niobium titanium-base alloy ingot casting; By the method for mechanical crushing, niobium titanium-base alloy ingot casting is broken into the fritter ingot casting of 10mm, and is placed in stainless steel pressure tank, pressurized tank is evacuated down to 1.0 × 10
-3pass into high-purity hydrogen after Pa to 1.0MPa, 800 DEG C of insulations 1.5 hours, obtain the suction hydrogen niobium titanium base alloy powder that particle diameter is less than 72 μm.Suction hydrogen niobium titanium base alloy powder is carried out plasma spheroidization, and inhale hydrogen niobium titanium base alloy powder in plasma spheroidization process and to absorb heat rapidly the quick-fried broken generation minute spherical niobium titanium base alloy powder of hydrogen, wherein powder feeding rate is 20gmin
-1, plasma power output is 70KW, and vacuum is 1 × 10
-3pa.Obtain the Nb-20%Ti-4%Al-3%Cr-5%V-4.5%W-0.03%C alloy powder that average grain diameter is 15 μm.
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 μm
Following raw material is taken: TiAl intermediate alloy, sponge Zr, V block, Nb rod and graphite according to the composition of niobium titanium-base alloy.In niobium titanium-base alloy, the content of various alloying element is: the Ti of 38%, the Al of 5%, V, the Zr of 0.5% of 4.5%, the Nb of the C of 0.05% and surplus.Before melting, metal mold is preheating to 360 DEG C, stop increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system is raised 180kW, 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
-2carry out homogenizing annealing process in the vacuum drying oven of Pa, homogenizing annealing treatment temperature is 1100 DEG C, and temperature retention time is 2 hours, obtains alloying component uniform niobium titanium-base alloy ingot casting; By the method for mechanical crushing, niobium titanium-base alloy ingot casting is broken into the fritter ingot casting of 25mm, and is placed in stainless steel pressure tank, pressurized tank is evacuated down to 1.0 × 10
-3pass into high-purity hydrogen after Pa to 0.6MPa, 750 DEG C of insulations 1 hour, obtain the suction hydrogen niobium titanium base alloy powder that particle diameter is less than 61 μm.Suction hydrogen niobium titanium base alloy powder is carried out plasma spheroidization, and inhale hydrogen niobium titanium base alloy powder in plasma spheroidization process and to absorb heat rapidly the quick-fried broken generation minute spherical niobium titanium base alloy powder of hydrogen, wherein powder feeding rate is 50gmin
-1, plasma power output is 80KW, and vacuum is 1 × 10
-3pa.Obtain the Nb-38%Ti-5%Al-4.5%V-0.5%Zr-0.05%C alloy powder that average grain diameter is 30 μm.
Claims (3)
1. prepare a method for fine grain spherical niobium titanium base alloy powder, it is characterized in that:
Step one, 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 block, Nb rod and graphite; Before melting, metal mold is preheating to 350 ~ 400 DEG C, increasing power is stopped after water jacketed copper crucible vacuum induction melting furnace monitor system is brought up to 170 ~ 190kW, 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 by mass percentage: the Ti of 17 ~ 45%, the Al of 0 ~ 15%, 0 ~ 10% Mo, 0 ~ 5% V, 0 ~ 8% W, Cr, the Zr of 0 ~ 2.5% of 0 ~ 5%, the Nb of the C of 0 ~ 0.05% and surplus;
Step 2, niobium titanium-base alloy ingot casting are in Zhen Kong Du≤10
-2carry out homogenizing annealing process in the vacuum drying oven of Pa, homogenizing annealing treatment temperature is 800 ~ 1100 DEG C, and temperature retention time is 1 ~ 3 hour, obtains alloying component uniform niobium titanium-base alloy ingot casting;
Step 3, by the method for mechanical crushing, niobium titanium-base alloy ingot casting is broken into the fritter ingot casting of 10 ~ 30mm, and is placed in stainless steel pressure tank, pressurized tank is evacuated down to 1.0 × 10
-3pass into high-purity hydrogen after Pa to 0.1 ~ 1.0MPa, 700 ~ 800 DEG C of insulations 1 ~ 2 hour, obtain the suction hydrogen niobium titanium base alloy powder that particle diameter is 50 ~ 300 μm, powder is sieved, obtain the fine grained suction hydrogen niobium titanium base alloy powder that particle diameter is less than 120 μm;
Step 4, fine grained is inhaled hydrogen niobium titanium base alloy powder carry out plasma spheroidization, in plasma spheroidization process, fine grained is inhaled hydrogen niobium titanium base alloy powder and to be absorbed heat rapidly the quick-fried broken generation minute spherical niobium titanium base alloy powder of hydrogen, and wherein powder feeding rate is 20 ~ 100gmin
-1, plasma power output is 50 ~ 90KW, and vacuum is 1 × 10
-3pa, finally obtains fine grain spherical niobium titanium base alloy powder.
2. a kind of method preparing fine grain spherical niobium titanium base alloy powder according to claim 1, is characterized in that: the particle diameter inhaling hydrogen niobium titanium base alloy powder is 50 μm ~ 100 μm.
3. a kind of method preparing fine grain spherical niobium titanium base alloy powder according to claim 1, is characterized in that: average grain diameter≤40 μm of fine grain spherical niobium titanium base alloy powder.
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