CN105081330A - Large-length-diameter-ratio ultrafine grain hard alloy step-shaped bar and preparation method - Google Patents
Large-length-diameter-ratio ultrafine grain hard alloy step-shaped bar and preparation method Download PDFInfo
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Abstract
The invention belongs to the technical field of powder metallurgy, and in particular, relates to a large-length-diameter-ratio ultrafine grain hard alloy step-shaped bar and a preparation method. The preparation method comprises the following steps: (1) ultrafine tungsten carbide powder and cobalt powder are mixed and grinded to obtain mixed powder; (2) the mixed powder and a multi-component binding agent consisting of paraffin-low molecular coupling agent-high molecular polymer are uniformly mixed to prepare a feedstock; (3) the feedstock is injected on an injection molding machine to form a molded blank; (4) the solvent degreasing and the thermal debinding are performed for the injection-molded blank in sequence; and (5) the ultrafine grain hard alloy step-shaped bar is obtained through sintering. The prepared ultrafine grain hard alloy step-shaped bar is small in alloy porosity and high in hardness and strength; and the diameter and size deviations are +-0.03 mm.
Description
Technical field
The invention belongs to powder metallurgical technology, particularly the step-like bar of a kind of ultra-fine cemented carbide of big L/D ratio and preparation method.
Background technology
Ultra-fine Grained (WC grain degree≤0.5 μm) WC-Co hard alloy has high strength, high rigidity and high-wearing feature, be widely used in machine tool, mould and wear part, comprise the fields such as metal cutting tool, wire drawing and press forming die, sealing ring, nozzle.Along with ultra-fine cemented carbide compressing-sintering technology ripe gradually, its subsequent processing operations is many, difficulty large, high in cost of production problem becomes increasingly conspicuous.
For the manufacture (as carbide drill, slotting cutter, screw tap etc.) of the integral-rotation cutting tool of big L/D ratio, shape and structure complexity, because it has the labyrinth such as screw thread, endoporus, cannot directly be obtained by conventional powder metallurgical method.At present, generally adopt compacting-sintering or extruding-sintering process to obtain ultra-fine cemented carbide bar, main later stage grinding and the attrition process of relying on obtains finished product, and its difficulty of processing is large, manufacturing procedure is many, with high costs.
The major advantage of powder injection forming (PIM) is the low cost precision form that can realize complex shape part, can accurately manufacture the severe service components with complicated shape feature, as various outside grooving, external screw thread, cone-shaped inner surface and outer surface, cross bore and blind hole etc., and the part with above feature all cannot be obtained by conventional powder metallurgical method.
At present, Powder Injection Molding Technology is applied to ultra-fine cemented carbide material to remain at series of problems.First, ultra-fine cemented carbide feeding intensity and density is low, poor fluidity, its injection process is the non-isothermal of a non-newtonian fluid, non-homogeneous, unstable state complex flow process, show poor fluidity, setting rate is fast, mold filling is easily caused to be discontented with, blank easy fracture, easily occur shorting, hole, distortion, fracture, burr, sandwich, density gradient, blemish and the not first-class fault of construction of green compact substance.Secondly, injection base skimming processes is a meticulous and physical and chemical process for complexity, and powder size affects its degreasing mechanism, ensure in skimming processes the size shape of degreasing base and reasonable carbon content very crucial.Finally, ultra-fine cemented carbide sintering is ripe gradually, but the stable acquisition with the ultra-fine crystal WC-Co alloy of efficient shrinkage factor still exists very large challenge.
If realize the PIM near-net-shape of the step-like bar of ultra-fine cemented carbide, by the important economic benefit of generation and environmental benefit.
Summary of the invention
The object of this invention is to provide a kind of step-like bar of ultra-fine cemented carbide and preparation method of big L/D ratio, be achieved through the following technical solutions:
A preparation method for the step-like bar of ultra-fine cemented carbide of big L/D ratio, comprises the following steps:
(1) superfine tungsten carbide powder containing grain growth inhibitor (0.3wt% ~ 1.0wt%) and cobalt powder are added ball grinding cylinder in proportion, wet-milling 24h ~ 100h, the drying of discharging final vacuum or atomization drying, obtain compound powder; Wherein the BET granularity of superfine tungsten carbide powder is 0.15 μm ~ 0.60 μm;
(2) in vacuum kneader, successively add compound powder and wax-based binder that step (1) obtains in proportion, stir, be mixed with the even feeding that powder loading is 45% ~ 57%;
(3) injection moulding: the feeding that step (2) obtains is injected shaping base on injection machine;
(4) solvent degreasing-thermal debinding: the shaping base that step (3) obtains is carried out solvent degreasing-thermal debinding, successively solvent and wax-based binder is removed, obtain degreasing base;
(5) sinter: the degreasing base that step (4) obtains is sintered in vacuum dewaxing-sintering furnace or pressurized sintering furnace, obtains the step-like bar of ultra-fine cemented carbide.
Further, described grain growth inhibitor is vanadium carbide (VC), chromium carbide (Cr
3c
2), one or more in ramet (TaC) and niobium carbide (NbC).
Further, the mass percent of described superfine tungsten carbide powder and cobalt powder is (96:4) ~ (85:15).
Further, described wax-based binder is made up of paraffin, high molecular polymer and low molecule couplant; The formation of each component and mass percentage are: paraffin is Tai Er carbide alloy height paraffin refined wax, accounts for 60% ~ 70%; High molecular polymer is one or more in high density polyethylene (HDPE), polypropylene, low density polyethylene (LDPE) and ethylene-vinyl acetate copolymer, accounts for 20% ~ 40% altogether; Low molecule couplant is one or more in stearic acid, o-phthalic acid dibutyl ester and dibutyl phthalate, accounts for 5% ~ 15% altogether.
Further, the concrete operations of step (2) are: a. adds high molecular polymer in vacuum kneader, add compound powder every 5min is secondary in three batches; B. secondaryly in two batches Tai Er carbide alloy height paraffin refined wax is added; C. low molecule couplant is added; Melting temperature is 120 ~ 150 DEG C, and mixing time is 2 ~ 4h.
Further, in step (3), during injection moulding, injection temperature is 120 DEG C ~ 165 DEG C, and injection pressure is 20MPa ~ 120Mpa; Described shaping base is of a size of φ 2.8mm × (4 ~ 10mm)/φ 2.2mm × (10 ~ 26mm).
Further, in step (4), during solvent degreasing, solvent is gasoline or normal heptane, and solvent temperature is 30 DEG C ~ 45 DEG C, and degreasing rate is 50% ~ 68%; During thermal debinding, maximum temperature and temperature retention time are respectively 500 DEG C ~ 650 DEG C, 30min ~ 120min, and protective atmosphere is H
2, N
2, one or more in Ar.
According to the step-like bar of ultra-fine cemented carbide of a kind of big L/D ratio that above-mentioned preparation method obtains, the alloy porosity A02B00C00 of the step-like bar of ultra-fine cemented carbide of described big L/D ratio, WC grain degree is 0.20 μm ~ 0.40 μm, and diameter and length dimension deviation are ± 0.03mm.
Beneficial effect of the present invention is: the deficiency that instant invention overcomes prior powder metallurgy die forming and existing powder injection forming, the water cutter blast tube, screw tap, milling cutter etc. that not only can be used for preparing big L/D ratio have the carbide alloy near-net-shape product of complicated shape, and efficiently solve the key technologies such as feeding skewness of the prior art and size Control; The present invention has not only saved valuable mineral resources, and greatly reduces difficulty of processing, has good economic benefit and environmental benefit.
Accompanying drawing explanation
Fig. 1: a kind of ultra-fine cemented carbide injection base schematic shapes in the present invention, numerical value shown in Fig. 1 is actual mould size;
Fig. 2: the microstructure figure of Ultra-fine Grained WC-10Co hard alloy bar in the embodiment of the present invention 1;
Fig. 3: the microstructure figure of Ultra-fine Grained WC-12Co hard alloy bar in the embodiment of the present invention 2.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme of the present invention is described further.
Embodiment 1
A kind of preparation method of Ultra-fine Grained WC-10Co Carbide Step shape bar of big L/D ratio:
(1) will containing vanadium carbide (VC, 0.35wt%), chromium carbide (Cr
3c
2, 0.45wt%) superfine tungsten carbide powder and cobalt powder add ball milling in proportion and fill with, wet-milling 30h, discharging final vacuum is dry, and sieve 320 orders, obtains compound powder; Wherein superfine tungsten carbide powder BET granularity is 0.60 μm, and Co content is 10%;
(2) mass percentage of each component formation and each component of choosing wax-based binder is: wax is Tai Er carbide alloy height paraffin refined wax, accounts for 63% altogether; Polyphosphazene polymer is combined into high density polyethylene (HDPE), polypropylene, ethylene-vinyl acetate copolymer, accounts for 30% altogether; Low molecule couplant is stearic acid, o-phthalic acid dibutyl ester, accounts for 7% altogether.
(3) in vacuum kneader, the compound powder that the wax-based binder of step (2) and step (1) obtain is carried out mixing: first add high molecular polymer, every the 5min secondary compound powder adding step (1) and obtain in three batches, secondly, secondaryly in two batches add the Tai Er carbide alloy height paraffin refined wax described in (2), finally add low molecule couplant, melting temperature is 150 DEG C, mixing time is 3h, obtains the even feeding that compound powder useful load is 49%;
(4) feeding that step (3) obtains is injected shaping base on injection machine, base injection temperature is 145 DEG C, and injection pressure is 100MPa, and shaping base is of a size of φ 2.8mm × 10mm/ φ 2.2mm × 26mm;
(5) degreasing base is obtained after the injection base that step (4) obtains being carried out solvent degreasing-thermal debinding.In solvent degreasing process, solvent is normal heptane; Solvent temperature is 40 DEG C, and its degreasing rate is about 65%; In thermal debinding process, maximum temperature and its temperature retention time are respectively 550 DEG C, 60min, and protective atmosphere is H
2;
(6) the degreasing base that step (5) obtains is sintered in vacuum atmosphere sintering integrated furnace, obtain Ultra-fine Grained WC-10Co Carbide Step shape bar.
As shown in Figure 2, the grain size of WC is 0.29 μm to the microstructure of the Ultra-fine Grained WC-10Co Carbide Step shape bar in the present embodiment 1, alloy porosity A02B00C00, HV
10hardness is 1728, and bending strength intensity is 1810MPa, and diameter and length dimension deviation are ± 0.03mm.
Embodiment 2
A kind of preparation method of Ultra-fine Grained WC-12Co Carbide Step shape bar of big L/D ratio:
(1) will containing chromium carbide (Cr
3c
2, 0.35wt%) superfine tungsten carbide powder and cobalt powder add ball milling in proportion and fill with, wet-milling 48h, discharging final vacuum is dry, and sieve 320 orders, obtains compound powder; Wherein superfine tungsten carbide powder BET granularity is 0.32 μm, and Co content is 12%;
(2) mass percentage of each component formation and each component of choosing wax-based binder is: wax is Tai Er carbide alloy height paraffin refined wax, accounts for 63% altogether; Polyphosphazene polymer is combined into high density polyethylene (HDPE), polypropylene, accounts for 30% altogether; Low molecule couplant is stearic acid, o-phthalic acid dibutyl ester, accounts for 7% altogether.
(3) in vacuum kneader, the compound powder that the wax-based binder of step (2) and step (1) obtain is carried out mixing: first add high molecular polymer, every the 5min secondary compound powder adding step (1) and obtain in three batches, secondly, secondaryly in two batches add the Tai Er carbide alloy height paraffin refined wax described in (2), finally add low molecule couplant, melting temperature is 150 DEG C, mixing time is 3h, obtains the even feeding that compound powder useful load is 49%;
(4) feeding that step (3) obtains is injected shaping base on injection machine, base injection temperature is 140 DEG C, and injection pressure is 80MPa, and shaping base is of a size of φ 2.8mm × 10mm/ φ 2.2mm × 26mm;
(5) degreasing base is obtained after the injection base that step (4) obtains being carried out solvent degreasing-thermal debinding.In solvent degreasing process, solvent is normal heptane; Solvent temperature is 35 DEG C, and its degreasing rate is about 65%; In thermal debinding process, maximum temperature and its temperature retention time are respectively 500 DEG C, 90min, and protective atmosphere is N
2and H
2;
(6) the degreasing base that step (5) obtains is sintered in vacuum atmosphere sintering integrated furnace, obtain Ultra-fine Grained WC-12Co Carbide Step shape bar.
As shown in Figure 3, the grain size of WC is 0.28 μm to the microstructure of the Ultra-fine Grained WC-12Co Carbide Step shape bar of a kind of big L/D ratio in the present embodiment 2, alloy porosity A02B00C00, HV
10hardness is 1591, and bending strength intensity is 1449MPa, and diameter and length dimension deviation are ± 0.03mm.
Claims (9)
1. a preparation method for the step-like bar of the ultra-fine cemented carbide of big L/D ratio, is characterized in that, comprise the following steps:
(1) superfine tungsten carbide powder containing grain growth inhibitor 0.3wt% ~ 1.0wt% and cobalt powder are added ball grinding cylinder in proportion, wet-milling 24h ~ 100h, the drying of discharging final vacuum or atomization drying, obtain compound powder; Wherein, the BET granularity of superfine tungsten carbide powder is 0.15 μm ~ 0.60 μm;
(2) in vacuum kneader, successively add compound powder and wax-based binder that step (1) obtains in proportion, stir, carry out mixing, be mixed with the even feeding that powder loading is 45% ~ 57%;
(3) injection moulding: the feeding that step (2) obtains is injected shaping base on injection machine;
(4) solvent degreasing-thermal debinding: the injection base that step (3) obtains is carried out solvent degreasing-thermal debinding, successively solvent and wax-based binder is removed, obtain degreasing base;
(5) sinter: the degreasing base that step (4) obtains is sintered in vacuum dewaxing-sintering furnace or pressurized sintering furnace, obtains the step-like bar of ultra-fine cemented carbide.
2. preparation method according to claim 1, is characterized in that, described grain growth inhibitor is one or more in vanadium carbide, chromium carbide, ramet and niobium carbide.
3. preparation method according to claim 1, is characterized in that, the mass percent of described superfine tungsten carbide powder and cobalt powder is (96:4) ~ (85:15).
4. preparation method according to claim 1, is characterized in that, described wax-based binder is made up of paraffin, high molecular polymer and low molecule couplant.
5. preparation method according to claim 4, is characterized in that, described paraffin is Tai Er carbide alloy height paraffin refined wax, accounts for 60% ~ 70% of wax-based binder gross mass; Described high molecular polymer is one or more in high density polyethylene (HDPE), polypropylene, low density polyethylene (LDPE) and ethylene-vinyl acetate copolymer, accounts for 20% ~ 40% of wax-based binder gross mass altogether; Described low molecule couplant is one or more in stearic acid, o-phthalic acid dibutyl ester and dibutyl phthalate, accounts for 5% ~ 15% of wax-based binder gross mass altogether.
6. preparation method according to claim 4, is characterized in that, the concrete operations of step (2) are: a. adds high molecular polymer in vacuum kneader, adds compound powder every 5min is secondary in three batches; B. secondaryly in two batches Tai Er carbide alloy height paraffin refined wax is added; C. low molecule couplant is added; Melting temperature is 120 ~ 150 DEG C, and mixing time is 2 ~ 4h.
7. preparation method according to claim 1, is characterized in that, in step (3), during injection moulding, injection temperature is 120 DEG C ~ 165 DEG C, and injection pressure is 20MPa ~ 120Mpa; Described shaping base is of a size of φ 2.8mm × (4 ~ 10mm)/φ 2.2mm × (10 ~ 26mm).
8. preparation method according to claim 1, is characterized in that, in step (4), during solvent degreasing, solvent is gasoline or normal heptane, and solvent temperature is 30 DEG C ~ 45 DEG C, and degreasing rate is 50% ~ 68%; During thermal debinding, maximum temperature and temperature retention time are respectively 500 DEG C ~ 650 DEG C, 30min ~ 120min, and protective atmosphere is H
2, N
2, one or more in Ar.
9. a kind of step-like bar of ultra-fine cemented carbide of big L/D ratio that obtains of preparation method according to claim 1, it is characterized in that, the alloy porosity A02B00C00 of the step-like bar of ultra-fine cemented carbide of described big L/D ratio, WC grain degree is 0.20 μm ~ 0.40 μm, and diameter and length dimension deviation are ± 0.03mm.
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| CN106282625A (en) * | 2016-08-02 | 2017-01-04 | 江苏省海洋资源开发研究院(连云港) | A kind of near-net-shape method of ultra-fine cemented carbide |
| CN107052346A (en) * | 2016-12-28 | 2017-08-18 | 江苏精研科技股份有限公司 | The preparation technology of powder injection forming tungsten-nickel hard alloy |
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| CN108034847A (en) * | 2017-10-20 | 2018-05-15 | 苏州欧美克合金工具有限公司 | A kind of hard alloy degreasing of graphene modification, sintering process |
| CN108057894A (en) * | 2017-12-12 | 2018-05-22 | 鑫京瑞钨钢（厦门）有限公司 | A kind of gradient hard alloy pole |
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| CN117020198B (en) * | 2023-10-08 | 2023-12-08 | 华南理工大学 | Metal injection molding feed of kovar alloy |
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