CN103305710B - Titanium-nitrogen alloy and preparation process thereof - Google Patents
Titanium-nitrogen alloy and preparation process thereof Download PDFInfo
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- CN103305710B CN103305710B CN201310216717.5A CN201310216717A CN103305710B CN 103305710 B CN103305710 B CN 103305710B CN 201310216717 A CN201310216717 A CN 201310216717A CN 103305710 B CN103305710 B CN 103305710B
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Abstract
The invention relates to a titanium-nitrogen alloy and a preparation process thereof. The titanium-nitrogen alloy comprises the following chemical components in percentage by weight: greater than or equal to 70% of Ti, 8-16% of N, less than or equal to 8.0% of C, less than or equal to 0.25% of Si, less than or equal to 0.2% of Mn, less than or equal to 0.35% of Cr, less than or equal to 0.6% of V, less than or equal to 0.03% of P and less than or equal to 0.01% of S. The process comprises the following steps: 1) with rutile concentrate fines and carbon black as raw materials, adequately mixing the raw materials by a twin-cone blender and pressing the raw materials into raw material balls; 2) wrapping carbon black powder on the surfaces of the raw material balls obtained in the step 1), wherein the carbon black is 0.5-1.5mm thick; 3) placing the raw material balls of which the surfaces are adhered with carbon black powder in the step 2) into a reaction furnace, controlling temperature and heating in stages under a nitrogen atmosphere and carrying out reductive nitriding treatment; and 4) after the reductive nitriding treatment, blowing by nitrogen, and cooling the product obtained in the step 3) to a temperature below 120 DEG C. The process is simple in course, low in energy consumption and excellent in product quality, and the technical problems that the titanium yield is low and the steel-making process is unstable in smelting microalloyed steel are solved.
Description
Technical field
The present invention relates to a kind of alloy and preparation technology thereof, specifically, relate to a kind of titanium nitrogen alloy and preparation technology thereof.
Background technology
Since 1975, low-carbon microalloyed steel because it is energy-conservation and saving resource, and has the excellent over-all properties such as high strength and high toughness plasticity and obtains develop rapidly.At present, the industry such as oil, chemical industry, automobile, shipbuilding, building materials proposes the requirements such as more harsh intensity, toughness and welding property to material, in addition smelt, process, the further developing of the technique such as thermal treatment, producing microalloying steel becomes inexorable trend.
Micro alloying element conventional in microalloyed steel metallurgy industry has Nb, Ti, V, Si, Mn, Cr, Al etc., to improve comprehensive mechanical performance and the corrosion resistances such as the toughness of steel, ductility, hardness and thermal fatigue resistance.In alloying element, Nb Grain Refinement Effect is remarkable, can depickling deoxygenation, effectively improves the quenching temperature of steel, be therefore widely used, but niobium resource is less, and ferro-niobium is mainly by external import, expensive and under one's control.V improves intensity mainly through the precipitation strength of C compound in ferrite, N compound or carbonitride, but brings the raising of ductile-brittle transition temperature, and the content of general V controls below 0. 10%.
Titanium is the main micro alloying element of early stage micro-alloyed steel, significant be carbon, the effect of nitride in steel-making of titanium.Compared with Nb, V, titanium mainly exists with the form of TiC, TiN or Ti (CN) in steel, has crystal grain thinning and precipitation strength double effects simultaneously.It can make the dense internal organization of steel, crystal grain thinning; Reduce aging sensitivity and cold shortness, strengthen intensity and the toughness of steel, improving welding property.The titanium elements adding trace can improve steel high temperature resistance, high pressure, H
2, N
2, NH
3deng the corrosive power of gas, with other element with the use of improving steel resistant to sea water and H
2the ability of S corrosion.
The sharpest edges of titanium are aboundresources, and at present, commercially the price of ferrotianium is not as good as 1/10 of ferro-niobium and vanadium iron, lower as steel-making additive production cost, most application value economically; But metal titanium is one of element that in rare metal, chemically reactive is the strongest, be the strong reductor in steel, its deoxidizing capacity exceedes silicon, suitable with aluminium.
No. 201110261893.1, Chinese patent application discloses a kind of preparation method of titanium nitrogen alloy on September 6th, 2011, titanium nitrogen alloy prepared by it, in microalloying steelmaking process, show technology stability difference, the recovery rate of titanium is low, become the technical barrier in the steel-making of long-standing problem titanium microalloying in decades, seriously limit titanium promoting the use of in micro-alloyed steel.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of new titanium nitrogen alloy and preparation technology thereof, uses this titanium nitrogen alloy, can reduce the stability problem of steel production cost and solution titanium nitrogen alloy steel product quality and heat in steelmaking process; Use this preparation technology, the titanium nitrogen alloy constant product quality produced, the recovery rate of titanium is high, and utilization ratio is high.
The technical scheme that the present invention solves the employing of its technical problem is:
The chemical composition of the titanium nitrogen alloy of the present invention, is: Ti >=70%, N:8 ~ 16%, C≤8.0%, Si≤0.25%, Mn≤0.2%, Cr≤0.35%, V≤0.6%, P≤0.03%, S≤0.01% by weight percentage.
The preparation technology of the titanium nitrogen alloy of the present invention, comprises the following steps:
1) with rutile fine ore and carbon black for raw material, adopt bipyramid blender fully mixed by raw material and be pressed into raw material ball;
2) wrap up in one deck carbon powder by sticky for step 1) gained raw material ball surface, the carbon powder thickness that glues be 0.5 ~ 1.5mm;
3) by step 2) surface that the obtains raw material ball that is stained with carbon powder puts into Reaktionsofen, and in a nitrogen atmosphere, temperature control heating stage by stage, carries out reduction Nitrizing Treatment;
4) reduce after Nitrizing Treatment, with nitrogen purging, product temperature step 3) obtained is down to less than 120 DEG C.
Further, described raw material rutile fine ore is a level rutile fine ore, granularity 80 ~ 100 order, and purity is 93.5 ~ 98.5%, and the particle diameter of described raw material carbon black is 100 ~ 200 orders.
Further, the mass ratio of rutile concentrate powder and carbon black is 2.5 ~ 5, and mixing time is 4 ~ 8 hours.
Further, in step 3), described nitrogen is technical pure nitrogen, and nitrogen partial pressure is 0.01 ~ 0.06MPa.
Further, in step 3), the described heating of temperature control stage by stage, is be warming up to 1100 DEG C ~ 1200 DEG C with the speed of 120 ~ 150 DEG C/h, then is warming up to 1700 ~ 1800 DEG C with the speed of 100 ~ 120 DEG C/h, finally, controlling heat-up rate is 40 ~ 50 DEG C/h, processes 2 ~ 5 hours.
Further, the CO (carbon monoxide converter) gas that reduction nitriding process produces is discharged by stove tail, igniting discharge.
Titanium nitrogen alloy of the present invention is mainly used in refining microalloyed steel, it is higher that its titanium and the content of nitrogen compare like product, to the crystal grain thinning of microalloyed steel and precipitation strength effect stronger, make the interior tissue of steel finer and close, effectively reduce aging sensitivity and the cold shortness of product made from steel, strengthen intensity and the toughness of steel, improving welding property.
The preparation method of titanium nitrogen alloy of the present invention; carbon powder is wrapped up in raw material raw material ball surface is sticky; effectively solve the adhesion problem of titanium nitrogen alloy in process of production between product, improve product apparent mass and yield rate, the surface-area 1/8 ~ 1/2 of nitriding reaction time prepared by titanium nitrogen alloy ball can also be increased; and pelletizing surface Graphite Powder 99; the oxygen that part is remaining can be consumed, and protect titanium carbide/titanium nitride in pelletizing, prevent it to be oxidized; improve the nitrogen content in product, improve grade and the qualification rate of product.Secondly, preparation process is by temperature control heating stage by stage, carry out reduction Nitrizing Treatment technique, the titanium in titanium nitrogen alloy is made to be that titanium nitride, titanium carbide or its sosoloid form-titanium carbonitride exists, and improve specific absorption and the stability of titanium, steel strength and performance is improved by crystal grain thinning and precipitation strength in steelmaking process, it also avoid simultaneously and consume metal titanium amount because of problems such as metal titanium deoxidation, removal of impurities, thus the stability problem in solution steelmaking process between steel product quality and heat, and product preparation process process is simple, energy consumption is low, and quality product is excellent.
Embodiment
For a more detailed description to the present invention by the following examples.
Embodiment 1
For refining a preparation technology for the titanium nitrogen alloy of microalloyed steel, specific embodiments:
1) by 80 orders, 93.5% rutile fine ore 150 kilograms and 100 object carbon blacks 40 kilograms, adopt bipyramid blender raw material is fully mixed 4 hours and is pressed into raw material ball;
2) wrap up in one deck carbon powder by sticky for step 1) gained raw material ball surface, the carbon powder thickness that glues be 0.5 mm;
3) by step 2) surface that the obtains raw material ball that is stained with carbon powder puts into Reaktionsofen, under the nitrogen atmosphere of 0.01Mpa, temperature control heating stage by stage, carry out reduction Nitrizing Treatment, temperature control heat-processed is stage by stage: product temperature is risen to 1100 DEG C by the heat-up rate of 120 DEG C/h, with the speed of 100 DEG C, temperature is risen to 1700 DEG C again, finally control heat-up rate and be about 50 DEG C/h process 3 hours; The CO (carbon monoxide converter) gas that reduction nitriding process produces is discharged by stove tail, igniting discharge;
4) with nitrogen purging, the product temperature after process is down to less than 120 DEG C, obtain titanium nitrogen alloy product, the composition of this titanium nitrogen alloy product is: Ti:78.5%, N:8.5%, C:7.0%, Si≤0.25%, Mn:0.15%, Cr:0.30%, V:0.55%, P:0.03%, S:0.01%.
Embodiment 2
For refining a preparation technology for the titanium nitrogen alloy of microalloyed steel, specific embodiments:
1) by 100 orders, 98% rutile fine ore 155 kilograms and 200 object carbon blacks 45 kilograms, adopt bipyramid blender raw material is fully mixed 6 hours and is pressed into raw material ball;
2) wrap up in one deck carbon powder by sticky for step 1) gained raw material ball surface, the carbon powder thickness that glues be 1.0 mm;
3) by step 2) surface that the obtains raw material ball that is stained with carbon powder puts into Reaktionsofen, under the nitrogen atmosphere of 0.03Mpa, temperature control heating stage by stage, carry out reduction Nitrizing Treatment, temperature control heat-processed is stage by stage: product temperature is risen to 1200 DEG C by the heat-up rate of 130 DEG C/h, with the speed of 100 DEG C, temperature is risen to 1800 DEG C again, finally control heat-up rate and be about 50 DEG C/h process 4 hours; The CO (carbon monoxide converter) gas that reduction nitriding process produces is discharged by stove tail, igniting discharge;
4) with nitrogen purging, the product temperature after process is down to less than 120 DEG C, obtain titanium nitrogen alloy product, the composition of this titanium nitrogen alloy product is: Ti:75%, N:15.5%, C:6.0%, Si≤0.22%, Mn:0.13%, Cr:0.25%, V:0.48%, P:0.02%, S:0.008%.
Embodiment 3
For refining a preparation technology for the titanium nitrogen alloy of microalloyed steel, specific embodiments:
1) by 100 orders, 95% rutile fine ore 130 kilograms and 200 object carbon blacks 35 kilograms, adopt bipyramid blender raw material is fully mixed 5 hours and is pressed into raw material ball;
2) wrap up in one deck carbon powder by sticky for step 1) gained raw material ball surface, the carbon powder thickness that glues be 1.20mm;
3) by step 2) surface that the obtains raw material ball that is stained with carbon powder puts into Reaktionsofen, under the nitrogen atmosphere of 0.06Mpa, temperature control heating stage by stage, carry out reduction Nitrizing Treatment, temperature control heat-processed is stage by stage: product temperature is risen to 1100 DEG C by the heat-up rate of 150 DEG C/h, with the speed of 120 DEG C, temperature is risen to 1700 DEG C again, finally control heat-up rate and be about 40 DEG C/h process 5 hours; The CO (carbon monoxide converter) gas that reduction nitriding process produces is discharged by stove tail, igniting discharge;
4) with nitrogen purging, the product temperature after process is down to less than 120 DEG C, obtain titanium nitrogen alloy product, the composition of this titanium nitrogen alloy product is: Ti:80.5%, N:14%, C:6.40%, Si≤0.23%, Mn:0.14%, Cr:0.23%, V:0.50%, P:0.025%, S:0.006%.
Embodiment 4
For refining a preparation technology for the titanium nitrogen alloy of microalloyed steel, specific embodiments:
1) by 100 orders, 95% rutile fine ore 160 kilograms and 100 object carbon blacks 60 kilograms, adopt bipyramid blender raw material is fully mixed 8 hours and is pressed into raw material ball;
2) wrap up in one deck carbon powder by sticky for step 1) gained raw material ball surface, the carbon powder thickness that glues be 1.5mm;
3) by step 2) surface that the obtains raw material ball that is stained with carbon powder puts into Reaktionsofen, under the nitrogen atmosphere of 0.04Mpa, temperature control heating stage by stage, carry out reduction Nitrizing Treatment, temperature control heat-processed is stage by stage: product temperature is risen to 1150 DEG C by the heat-up rate of 140 DEG C/h, with the speed of 110 DEG C, temperature is risen to 1800 DEG C again, finally control heat-up rate and be about 45 DEG C/h process 2 hours; The CO (carbon monoxide converter) gas that reduction nitriding process produces is discharged by stove tail, igniting discharge;
4) with nitrogen purging, the product temperature after process is down to less than 120 DEG C, obtain titanium nitrogen alloy product, the composition of this titanium nitrogen alloy product is: Ti:82.5%, N:9.8%, C:5.35%, Si≤0.24%, Mn:0.19%, Cr:0.31%, V:0.55%, P:0.025%, S:0.01%.
Claims (1)
1. a preparation technology for titanium nitrogen alloy, is characterized in that, the chemical composition of described titanium nitrogen alloy is by weight percentage: Ti >=70%, N:8 ~ 16%, C≤8.0%, Si≤0.25%, Mn≤0.2%, Cr≤0.35%, V≤0.6%, P≤0.03%, S≤0.01%;
The preparation technology of described titanium nitrogen alloy, comprises the following steps:
1) with rutile fine ore and carbon black for raw material, adopt bipyramid blender fully mixed by raw material and be pressed into raw material ball;
2) wrap up in one deck carbon powder by sticky for step 1) gained raw material ball surface, the carbon powder thickness that glues be 0.5 ~ 1.5mm;
3) by step 2) surface that the obtains raw material ball that is stained with carbon powder puts into Reaktionsofen, and in a nitrogen atmosphere, temperature control heating stage by stage, carries out reduction Nitrizing Treatment;
4) reduce after Nitrizing Treatment, with nitrogen purging, product temperature step 3) obtained is down to less than 120 DEG C;
In step 3), the described heating of temperature control stage by stage, is be warming up to 1100 DEG C ~ 1200 DEG C with the speed of 120 ~ 150 DEG C/h, then is warming up to 1700 ~ 1800 DEG C with the speed of 100 ~ 120 DEG C/h, finally, controlling heat-up rate is 40 ~ 50 DEG C/h, processes 2 ~ 5 hours.
2. the preparation technology of titanium nitrogen alloy as claimed in claim 1, it is characterized in that, described raw material rutile fine ore is a level rutile fine ore, granularity 80 ~ 100 order, and purity is 93.5 ~ 98.5%, and the particle diameter of described raw material carbon black is 100 ~ 200 orders.
3. the preparation technology of titanium nitrogen alloy as claimed in claim 1 or 2, it is characterized in that, the mass ratio of rutile concentrate powder and carbon black is 2.5 ~ 5, and mixing time is 4 ~ 8 hours.
4. the preparation technology of titanium nitrogen alloy as claimed in claim 1 or 2, it is characterized in that, in step 3), described nitrogen is technical pure nitrogen, and nitrogen partial pressure is 0.01 ~ 0.06MPa.
5. the preparation technology of titanium nitrogen alloy as claimed in claim 3, it is characterized in that, in step 3), described nitrogen is technical pure nitrogen, and nitrogen partial pressure is 0.01 ~ 0.06MPa.
6. the preparation technology of titanium nitrogen alloy as claimed in claim 1 or 2, is characterized in that, the CO (carbon monoxide converter) gas that reduction nitriding process produces is discharged by stove tail, igniting discharge.
7. the preparation technology of titanium nitrogen alloy as claimed in claim 3, is characterized in that, the CO (carbon monoxide converter) gas that reduction nitriding process produces is discharged by stove tail, igniting discharge.
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