CN102581288B - Method for preparing ultrafine niobium carbide and iron composite powder material - Google Patents
Method for preparing ultrafine niobium carbide and iron composite powder material Download PDFInfo
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- CN102581288B CN102581288B CN2012100810090A CN201210081009A CN102581288B CN 102581288 B CN102581288 B CN 102581288B CN 2012100810090 A CN2012100810090 A CN 2012100810090A CN 201210081009 A CN201210081009 A CN 201210081009A CN 102581288 B CN102581288 B CN 102581288B
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Abstract
The invention discloses an ultrafine niobium carbide and iron composite powder material. Niobium powder, graphite powder and iron powder are used as raw materials, the proportion of the mass of the iron powder in the raw materials is larger than or equal to 15%, and mass ratio of the remaining niobium powder to the remaining graphite powder ranges from 7.65:1 to 7.70:1. The method for preparing the ultrafine niobium carbide and iron composite powder material includes that mixed materials of the niobium powder and the graphite powder are in ball milling to form solid solution containing carbon in niobium, the iron powder is further added into the mixed material to be in ball milling so that niobium particles and iron particles which are dissolved in the carbon form composite bodies, and ultrafine niobium carbide and iron composite powder can be obtained after the composite bodies are annealed. The size of the largest niobium carbide particle in the niobium carbide and iron composite powder is smaller than 500mm. By the aid of the niobium carbide and iron composite powder, excellent wettability of the niobium carbide particles and steel liquid can be realized, problems of gas absorption, poor interface bonding and the like of the niobium carbide particles are solved, and mechanical performances of steel materials are greatly improved.
Description
Technical field
The invention belongs to material science, be specifically related to a kind of niobium carbide-iron composite powder powder material, and the preparation method of this superfine niobium carbide-iron composite powder powder material.
Background technology
Niobium carbide (NbC) is hybrid bonded as ionic bond, covalent bond and the metallic bond of magnesium-yttrium-transition metal and carbon, has high-melting-point (3613 ℃), high rigidity (1800HV), high elastic modulus (580kNmm
-2), the performance such as high abrasion, Thermodynamically stable.And its density (7.78gcm
-3) with ferrous materials density, approach, these characteristics likely make it become optimal hardening constituent in ferrous materials, but due to its fusing point far above the iron fusing point of steel particularly, therefore its very difficult even dispersion is distributed in ferrous materials, its invigoration effect to iron and steel is subject to very large restriction, and therefore the field of NbC institute extensive use now is only generally the technical fields such as carbide alloy, casting are oozed, surface spraying.And in casting, ooze, the field such as surface spraying is while being used niobium carbide, require NbC particle not only tiny (maximum particle size should not be greater than 1 μ m), but also need niobium carbide be combined with the iron and steel interface well or there is good wetability with iron and steel liquid.Therefore how to produce particle more tiny and with the NbC particle that iron and steel can be better fused, be the target that people pursue.
At present, both at home and abroad preparing aspect the superfine niobium carbide particle technique that has possessed comparative maturity, for example: the preparation method's that the preparation method's that denomination of invention is a kind of superfine niobium carbide powder Chinese patent 201110145430.9 and denomination of invention are niobium carbide powder Chinese patent 201110136013.8, and the Cui Zhaowen of Hebei University of Science and Technology utilizes high-energy ball-milling process to prepare the NbC particle of average grain diameter in the 300nm left and right, these all illustrate that it is feasible manufacturing the niobium carbide ultra-fine grain.But this NbC particle is also having great limitation aspect the wetability of improvement and iron and steel liquid.In addition, the Chinese patent 200810147745.5 that denomination of invention is ceramic cladding powder and preparation method thereof, in order to improve the wettability of niobium carbide and ferrous materials, particles of niobium carbide is carried out to metallic cover, but this coating metal used only limits to cobalt and nickel, therefore fundamentally do not solve the wettability problem of niobium carbide and ferrous materials.
Summary of the invention
The technical issues that need to address of the present invention are to provide a kind of superfine niobium carbide-iron composite powder powder material and preparation method thereof, the NbC ultra-fine grain is generated in the iron powder matrix, make it to become niobium carbide-iron composite powder end, to solve the poor problem of superfine niobium carbide particle and iron and steel liquid wetting.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
A kind of superfine niobium carbide-iron composite powder powder material, to take niobium powder, graphite powder and iron powder as raw material, more than 15% of quality sum that the shared ratio of described iron powder is niobium powder, graphite powder and iron powder, it is quality proportion>=15% in raw material of iron powder, the quality percentage composition of niobium carbide is less than 85%, and the niobium powder in raw material and graphite powder mass ratio are 7.65:1～7.70:1; The mechanical systems such as process ball milling form the complex of the solid solution of carbon in niobium further formation and iron, and, through adding the complex of thermosetting niobium carbide and iron, wherein, the size of niobium carbide the largest particles is less than 500nm
.
The preparation method of superfine niobium carbide-iron composite powder powder material comprises: A, niobium powder, graphite powder and the iron powder of proper proportion of take are raw material; B, ball milling: B1, the mixed material ball milling of niobium powder, graphite powder is become to the solid solution of carbon in niobium; B2, in B1 gained material, add iron powder, further ball milling made solid solution niobium particle and the iron particle of carbon form complex; C, the material of B2 gained is annealed, obtained superfine niobium carbide-iron composite powder end.
Above-mentioned preparation method's of the present invention further improvement is: described mechanical milling process B 1 is with in the ball grinder of packing into after the graphite powder of certain extra proportion mixes by the niobium powder; stainless steel abrading-ball in ball grinder and the mass ratio of material are 35:1～40:1; after ball grinder vacuumizes under argon shield ball milling, make niobium powder and graphite powder form the solid solution of carbon in niobium.
Preparation method's of the present invention further improvement is: the mass ratio of described niobium powder and graphite powder is 7.65:1～7.70:1, and the graphite-phase wherein added is excessive 0.5%～1% for the stoichiometry of NbC, as process control agent.
Preparation method's of the present invention further improvement is: the additional proportion of the iron powder in described mechanical milling process B2 is to be not less than 15% of composite powder gross mass, then under argon shield, continues ball milling, the formed solid solution niobium particle of carbon and the complex of iron particle.
The preparation method's that the present invention is above-mentioned further improvement is: the purity of described niobium powder, graphite powder, iron powder all is greater than 95.0%, also can use purity all to be greater than 97.0% niobium powder, graphite powder, iron powder; The average-size of particle between 300 orders～400 orders, the purity of argon gas>99.99%.
Preparation method's of the present invention further improvement is: described annealing process C is greater than 10 by the powder of B2 gained in vacuum
-3be heated to rapidly 650 ℃～750 ℃ in the vacuum drying oven of Pa, insulation 20min～30min, then be cooled to room temperature, can obtain superfine niobium carbide-iron composite powder end.
Above-mentioned preparation method further improves and is: the speed of described heating is greater than 10 ℃/s, and described cooling speed is greater than 100 ℃/min.
Owing to having adopted technique scheme, the technological progress that the present invention obtains is:
The niobium carbide that method of the present invention is produced-iron composite powder powder material is to make after Nb element and C element solid solution regeneration niobium carbide in the iron powder matrix, therefore niobium carbide and iron can form good complex, and the particle at niobium carbide-iron composite powder end is very tiny; Like this with regard to air-breathing, the interface that solved particles of niobium carbide in conjunction with the problem such as bad, make particles of niobium carbide and iron and steel liquid there is good wetability.Reach these performance needs and strictly control the preparation technology at niobium carbide-iron composite powder end.The present invention, by the accurate control of the technological parameters such as ball milling and vacuum annealing temperature, time, cooling velocity, can be less than the particles of niobium carbide size Control of generation in 500nm.Because the particle of niobium carbide is tiny and good with the wettability of ferrous materials, therefore can make the high degree of dispersion of particles of niobium carbide in iron powder and iron liquid, can not form agglomerate, give full play to its dispersion-strengthened action, greatly improve the mechanical performance of ferrous materials.The required Ball-milling Time of method of the present invention is short in addition, and total Ball-milling Time is only generally 8～13 hours, and the temperature of carbon and niobium generation chemical reaction is low, is only 650 ℃～750 ℃, therefore during method consumption energy consumption of the present invention far below existing method.
Mechanical milling process for the first time of the present invention has been realized the fragmentation, levigate of niobium powder, graphite powder, make graphite powder decrystallized simultaneously, and make in the niobium particle to produce the defects such as a large amount of rooms and dislocation, in the collision process of niobium powder and graphite powder, constantly refinement produces the temperature rise of a large amount of unsalted surfaces and moment and has all significantly reduced the diffusion activation energy of carbon atom in the niobium lattice, thereby carbon is entered in the lattice of niobium, form the solid solution of carbon in niobium, but now do not generate niobium carbide.In niobium carbide, the atomic ratio of carbon and niobium is 1:1, for the first time in mechanical milling process in raw material graphite powder with respect to the stoichiometry of NbC, be excessive adding, excessive graphite powder is as process control agent, can be used for making up the loss of carbon in mechanical milling process, and can reduce the reunion, caking of powder, sticky wall, slimeball and, to the wearing and tearing of abrading-ball and mill tube, can control preferably the powder composition and improve flour extraction.
In mechanical milling process for the second time of the present invention, under the effect of external force collision, extruding, grinding, solid solution the niobium powder of carbon and iron powder broken, overlapping and cold welding repeatedly, form a large amount of lamellar tissues, the further refinement of lamellar tissue and curling overlapping, finally the formed solid solution niobium particle of carbon and the compound system of iron particle.Now through low-temperature heat, carbon and the niobium formation niobium carbide that reacts, thus formed ultrafine niobium carbide and the compound granular pattern material of iron powder.The present invention adopts low-temperature heat, Fast Heating and cooling process fast, guarantee solid solution the niobium of carbon fully to niobium carbide, transform, and form superfines.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in further details:
Superfine niobium carbide of the present invention-iron composite powder powder material is to take niobium powder, graphite powder and iron powder as raw material, the shared ratio of described iron powder is more than 15% of each material quality sum, in niobium carbide-iron composite powder powder material, the quality percentage composition of niobium carbide is less than 85%, and niobium powder and graphite powder mass ratio are 7.65:1～7.70:1; The size of niobium carbide the largest particles is less than 500nm
.
Each embodiment balls grinding machine is the BXQM4L planetary ball mill that Nanjing special wheel new instrument Co., Ltd manufactures, ball grinder is the stainless-steel vacuum tank, volume is 1000ml, abrading-ball is also stainless steel, tri-kinds of φ 20mm, φ 10mm and φ 6mm are arranged, the proportioning of three kinds of balls can be adjusted as required voluntarily, the cumulative volume of abrading-ball account for tank volume 50%.
Embodiment 1
The first step: the mass ratio by niobium powder (granularity is that 325 orders, purity are 99.3%) and graphite powder (purity is 98.0%, granularity be 300 orders) by 7.65:1 mixes, the amount of graphite powder is with respect to the stoichiometry of NbC excessive 0.5%, unnecessary graphite powder is process control agent, form mixed material, in the stainless steel jar mill of packing into, and according to the ratio of grinding media to material (mass ratio of stainless steel abrading-ball and mixed powder) of 38:1 to the stainless steel ball of packing in grinding jar, the diameter of the stainless steel abrading-ball of packing into adds than the ratio of 200 Ф 10mm according to 40 Ф 20mm.Be filled with argon gas (purity > 99.99%) after ball grinder vacuumizes, then ball grinder be installed on planetary ball mill, under the rotating speed of 300r/min, ball milling is 6 hours.
Second step: add again the reduced iron powder identical with graphite powder quality summation with the niobium powder (granularity is that 325 orders, purity are 98.0%) in the ball grinder of the first step, after vacuumizing, be filled with argon gas, under the rotating speed of 300r/min, continue ball milling 5 hours.
The 3rd step: the powder 200g that gets ball milling formation is placed in vacuum and is greater than 10
-3in the vacuum drying oven of Pa, be warming up to 700 ℃ within 1min, insulation 28min then is chilled to room temperature within 7min, can obtain superfine niobium carbide-iron composite powder end.
In the superfine niobium carbide obtained-iron composite powder end, the quality percentage composition of NbC is 50%.
Embodiment 2
The difference of the present embodiment and embodiment 1 is as follows.
The stainless steel abrading-ball that the first step is used and niobium powder (granularity is that 300 orders, purity are 95.0%) and graphite powder (purity is 95.0%, granularity be 300 orders) mixed powder mass ratio is 40:1, the stainless steel abrading-ball used is φ 20mm 40,150 of φ 10mm, 200 of φ 6mm, Ball-milling Time 7 hours.
Adding the quality of iron powder (granularity is that 400 orders, purity are 95.0%) in second step is 80% of niobium powder and graphite powder quality summation, and Ball-milling Time is 4 hours.
The 3rd step programming rate is to be warming up within 1min, and, 650 ℃ of insulations 30 minutes, then within 6min, is chilled to room temperature.
In the superfine niobium carbide obtained-iron composite powder end, the quality percentage composition of NbC is 55.5%.
Embodiment 3
The difference of the present embodiment and embodiment 1 is as follows.
The ratio of first step niobium powder (granularity is that 400 orders, purity are 97.0%) and graphite powder (purity is 95.0%, granularity be 400 orders) is 7.68:1, the stainless steel abrading-ball used and niobium powder and graphite powder mixed powder mass ratio are 35:1, the stainless steel abrading-ball used is φ 20mm 40,200 of φ 10mm, Ball-milling Time 8 hours; The Ball-milling Time of second step is 4 hours, and the granularity of the iron powder used is 300 orders, and purity is 97%.
In the superfine niobium carbide obtained-iron composite powder end, the quality percentage composition of NbC is 50%.
Embodiment 4
The difference of the present embodiment and embodiment 1 is as follows.
The ratio of first step niobium powder and graphite powder is 7.70:1, and the stainless steel abrading-ball used and niobium powder and graphite powder mixed powder mass ratio are 35:1, the stainless steel abrading-ball used is φ 20mm 40,200 of φ 10mm, Ball-milling Time 5 hours; The quality that adds iron powder of second step is 30% of niobium powder and graphite powder quality summation, and Ball-milling Time is 5 hours.
In the superfine niobium carbide obtained-iron composite powder end, the quality percentage composition of NbC is 76.9%.
Embodiment 5
The difference of the present embodiment and embodiment 1 is as follows.
The quality that adds iron powder of second step is 17.6% of niobium powder and graphite powder quality summation.
In the superfine niobium carbide obtained-iron composite powder end, the quality percentage composition of NbC is 85%.
The result that above four embodiment gained samples are detected is as follows.
At first after second step being finished, resulting powder carries out X-ray diffraction (XRD) analysis, and phase is Nb and Fe.To vacuum annealing, later powder carries out XRD analysis again, and phase is NbC and Fe.Proof NbC generates in vacuum annealing process.The powder later to vacuum annealing carries out the magnetic test, and powder all has ferromagnetism, illustrates that niobium carbide and iron powder are compound systems.Watery hydrochloric acid with 10% dissolves the iron powder in composite powder, remaining particles of niobium carbide is utilized to AFM and its pattern of sem observation measurement size, embodiment 1 gained niobium carbide maximum particle size is 470nm, embodiment 2 gained niobium carbide maximum particle sizes are 400nm, embodiment 3 gained niobium carbide maximum particle sizes are 450nm, and the niobium carbide maximum particle size of embodiment 4 gained is 480nm; The niobium carbide maximum particle size of embodiment 5 gained is 480 nm.
The ratio of the total raw material that the iron powder described in the present invention is shared can also be to be greater than 15% arbitrary proportion; Certainly, when ratio is less than 15%, also can form superfine niobium carbide-iron composite powder powder material, but the wettability of itself and iron and steel liquid is poor.
Embodiment 6
Prepared superfine niobium carbide-iron composite powder powder material is applied to casting to be oozed part and compares with the niobium carbide of not compound identical particle size.The specific embodiment is as follows:
Casting infiltration layer material: A, B, C, D, E are respectively the composite powders that above-described embodiment 1 to embodiment 5 obtains, and F is the average particle size particle size niobium carbide powder that is 350nm and the mixed-powder of equal in quality iron powder.
Get above-mentioned casting infiltration layer materials A, B, C, D, E, each 180 grams of F, the organic binder bond and the inorganic binder that add respectively a certain amount of autogamy, organic stick plays cementation in powder forming, and inorganic binder plays bonding and flux in casting, through fully stirring and make paste, be coated on respectively same casting mold die cavity bottom surface symmetric position everywhere, coating layer thickness is 25mm, for casting, oozes test.With the intermediate frequency furnace melting ZG45 cast steel of 20 kg, pouring temperature is 1650 ℃ of left and right, and running gate system is the open cast gate of rising pouring, casting mold is baked to 300 ℃ of left and right before cast.
Adopt line to cut sample, measure by casting casting that infiltration layer materials A, B, C, D, E, F form and ooze composite bed thickness and be listed in the table below
As can be seen here, niobium carbide-iron composite powder end is significant in effect aspect the wetability of improving between niobium carbide and iron and steel liquid.
Adopt MLD-10 impact abrasive wear testing machine to detect the impact abrasion performance of composite bed, do not add abrasive material during impact, requirement according to testing machine, the impact wear sample is divided into sample and lower sample, upper sample is of a size of l0mm * l0mm * 30mm, and shock surface is the face with the l0mm * l0mm of composite bed, with it to the mill lower sample be the ring sample that ZG45 makes, its internal diameter is that 30mm, external diameter are 50mm, and width is 20mm.The electronic balance that is 0.1mg with sensibility reciprocal in wear test is weighed to the sample before and after wearing and tearing, and the front sample of weighing all cleans up through alcohol, and electricity consumption dries up.Above-mentioned casting is oozed to four samples that obtain and distinguish pre-grinding 40 minutes, weighing, be designated as m by this quality
0.Continue again wearing and tearing 2 hours, weighing, quality is designated as m
l, wear weight loss is Δ m=m
0-m
l.Weigh with Δ m the binding ability that particles of niobium carbide and ZG45 matrix in composite bed are oozed in casting.Following table is the impact wear numerical value of various sample
Wear weight loss contrast by upper sample 1～5 in above experiment with upper sample 6, illustrate that niobium carbide-iron composite powder end is significant in effect aspect the binding ability of improving between particles of niobium carbide and steel substrate.By the abrasion condition contrast of the ZG45 with without the casting infiltration layer, prove employing method manufacture of the present invention niobium carbide-the iron composite powder end can be improved the mechanical performances such as wearability of material greatly.
Claims (5)
1. the preparation method of superfine niobium carbide-iron composite powder powder material is characterized in that:
A, niobium powder, graphite powder and the iron powder of proper proportion of take are raw material;
B, ball milling;
B1, the mixed material ball milling of niobium powder, graphite powder is become to the solid solution of carbon in niobium;
B2, in B1 gained material, add iron powder, further ball milling made solid solution niobium particle and the iron particle of carbon form complex;
C, the material of B2 gained is annealed, obtained superfine niobium carbide-iron composite powder end;
The mass ratio of described niobium powder and graphite powder is 7.65:1～7.70:1, and the graphite-phase wherein added is excessive 0.5%～1% for the stoichiometry of NbC, as process control agent;
The additional proportion of the iron powder in described mechanical milling process B2 is to be not less than 15% of composite powder gross mass, then under argon shield, continues ball milling, the formed solid solution niobium particle of carbon and the complex of iron particle.
2. the preparation method of superfine niobium carbide-iron composite powder powder material according to claim 1; it is characterized in that: described mechanical milling process B1 is with in the ball grinder of packing into after graphite powder mixes by the niobium powder; stainless steel abrading-ball in ball grinder and the mass ratio of material are 35:1～40:1; after ball grinder vacuumizes under argon shield ball milling, make niobium powder and graphite powder form the solid solution of carbon in niobium.
3. according to the preparation method of the described superfine niobium carbide of claim 1～2 any one-iron composite powder powder material, it is characterized in that: the purity of described niobium powder, graphite powder, iron powder all is not less than 95.0%, the average-size of particle between 300 orders～400 orders, the purity of argon gas>99.99%.
4. the preparation method of superfine niobium carbide-iron composite powder powder material according to claim 1, it is characterized in that: described annealing process C is greater than 10 by the powder of B2 gained in vacuum
-3be heated to rapidly 650 ℃～750 ℃ in the vacuum drying oven of Pa, insulation 20min～30min, then be cooled to room temperature, can obtain superfine niobium carbide-iron composite powder end.
5. the preparation method of superfine niobium carbide-iron composite powder powder material according to claim 4, it is characterized in that: the speed of described heating is greater than 10 ℃/s, and cooling velocity should be greater than 100 ℃/min.
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| CN107338435B (en) * | 2017-06-26 | 2022-02-18 | 华东交通大学 | Mixed powder for synchronously feeding pure copper and preparation method thereof |
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| US4886638A (en) * | 1989-07-24 | 1989-12-12 | Gte Products Corporation | Method for producing metal carbide grade powders |
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