CN115156541A - Preparation method of high-performance hard alloy with laminated structure - Google Patents
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
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Abstract
A preparation method of high-performance hard alloy with a laminated structure belongs to the technical field of hard alloy preparation. The invention utilizes double powder bins of the selective laser sintering equipment to alternately spread powder, namely, a layer of WC-Co and nylon powder is spread, and then a layer of ZrO powder is spread 2 Co and nylon powders, the powders of the two components being successively and alternately stacked, the nylon in each layer being irradiated by laser light to melt and bond WC-Co or ZrO 2 Co powder to realize layer-by-layer solidification forming and further printingObtaining a hard alloy green compact with a laminated structure, which has a required shape and two components which are continuously and alternately distributed; and then hot-pressing and sintering the green body to remove the nylon serving as a binder, so as to realize complete densification of the alloy, thereby obtaining the hard alloy material with high hardness and high toughness.
Description
Technical Field
The invention relates to a preparation method of laminated structure hard alloy with excellent comprehensive performance, belonging to the technical field of hard alloy preparation.
Background
The WC-Co hard alloy has high hardness and strength, good toughness and excellent wear resistance, and is widely applied to the fields of metal cutting processing, mining, die manufacturing and the like. The hard alloy is mainly prepared by a powder metallurgy method, and comprises three main processes of preparing a mixture, pressing and forming and sintering densification. Specifically, firstly, weighing raw material powder and an organic forming agent according to a ratio, and carrying out wet grinding, spray drying and granulation on the raw material powder and the organic forming agent; pressing the mixture into a green body with a certain shape and structure through a die; and then degreasing and sintering the blank at a certain temperature to obtain the high-strength hard alloy block material. The high hardness and wear resistance of cemented carbides is mainly due to WC, while the toughness is mainly due to the better plastic Co. Since hardness and toughness are inherently contradictory, a homogeneous multiphase material composed of WC and Co uniformly distributed tends to sacrifice some of toughness while achieving high hardness. As the service conditions of cemented carbide tools become more severe, this contradictory property makes it difficult for cemented carbide of uniform composition to meet the rapidly developing modern industrial demands.
To solve this contradiction, it is common in industrial production to coat a certain thickness of Ti (C, N), al with higher hardness on the surface of the cemented carbide by vapor deposition 2 O 3 And the like, are currently in mature use on cutting tools. Or the hard alloy with a double-layer or three-layer structure is constructed by processes of gas phase diffusion, infiltration and the like, wherein the grain size, the Co content and the carbon content are in gradient distribution, for example, the spherical tooth used for mining and rock drilling has a three-layer structure, the outermost layer and the middle layer are both WC + gamma two-phase normal tissues, but the Co content of the outer layer is relatively lower, the inner layer is WC + gamma + eta, and the inner layer contains fine and uniform eta carbon-deficient phases. However, for the cemented carbide product with the two-layer or three-layer structure, when the outermost layer fails due to abrasion or fracture, the alloy as a whole cannot meet the actual use requirements.
Aiming at the technical problems of the background of the field and the existing technology, the invention provides a concept of any multilayer structure hard alloy, and provides a preparation method of a laminated structure hard alloy with excellent comprehensive performance by combining a 3D printing technology.
Disclosure of Invention
The preparation method provided by the invention comprises the following process flows and principles: the powder is alternately spread by using double powder bins of the selective laser sintering equipment, namely, a layer of WC-Co and nylon powder is spread, and then a layer of ZrO is spread 2 Co and nylon powders, the powders of the two components being successively and alternately stacked, the nylon in each layer being irradiated by laser light to melt and bond WC-Co or ZrO 2 Co powder, which is used for realizing layer-by-layer solidification forming and further printing to obtain a hard alloy green body with a required shape and a laminated structure with two components distributed continuously and alternately; and then hot-pressing and sintering the green body to remove the nylon serving as a binder, so as to realize complete densification of the alloy, thereby obtaining the hard alloy material with high hardness and high toughness.
The invention provides a preparation method of a high-performance hard alloy with a laminated structure, which is characterized by comprising the following steps of:
(1) ZrO 2 is mixed with 2 Mixing the powder, co powder, polyethylene glycol and deionized water in proportion to prepare slurry, then spray-drying to obtain spherical powder, carrying out heat treatment on the spray-dried powder, and screening to obtain ZrO with particle size distribution of 10-40 microns 2 -Co feed powder of ZrO 2 The average particle size of the powder was 0.2 μm, the average particle size of Co powder was 0.6 μm, co was in ZrO 2 10-14% of-Co powder, 2-4% of polyethylene glycol and ZrO 2 And Co powder accounts for 55-65% of the mass ratio of the slurry, the heat treatment temperature of the spray granulation powder is 950-1050 ℃, and the heat preservation time is 1h;
(2) Carrying out agglomeration granulation on WC-Co powder according to the process of the step (1), and screening to obtain WC-Co feed powder with the particle size distribution of 5-20 micrometers, wherein the average particle size of the WC powder is 0.8 mu m, and Co accounts for 10-14% of the mass fraction of the WC-Co powder;
(3) ZrO obtained in the step (1) and the step (2) 2 Respectively and independently mixing the feed powder of-Co and WC-Co with nylon powder uniformly, and mixing the twoRespectively placing the seed powder in two powder storage bins of a selective laser sintering printer, heating a powder laying platform to 170 ℃, continuously and alternately laying the powder in the two powder bins, melting nylon in each layer of powder through laser irradiation, and correspondingly ZrO in each layer 2 the-Co or WC-Co powder is bonded and formed, and the hard alloy green body with the required shape and the double-component continuous and alternate distribution and the laminated structure can be obtained after stacking layer by layer, wherein the mass percentage of the nylon powder in each layer of powder is 4-6%, the powder spreading thickness of each layer is 140-160 mu m, the particle size distribution of the nylon powder is 20-80 mu m, and the heating rate of a powder spreading platform is 1.5 ℃/min;
(4) And (4) carrying out rapid hot-pressing sintering on the hard alloy green compact with the laminated structure printed in the step (3), wherein the final state sintering temperature is 1170-1230 ℃, the heat preservation time is 2-4min, the applied pressure is 35-45MPa, and the hard alloy with the laminated structure and the excellent comprehensive performance and the two components are continuously and alternately distributed after cooling.
The method of the invention has the following technical characteristics and advantages:
(1) The innovative method for constructing the hard alloy with any multilayer structure based on the 3D printing technology is provided, the component structure and the layer number of each layer can be adjusted at will, and the method has universality on the design and preparation of metal/ceramic materials with special structure and function requirements; (2) Incorporated ZrO 2 The components can generate martensite phase transformation (from a tetragonal crystal structure to a monoclinic structure) under the condition of room temperature due to stress induction, and the volume expansion generated by the phase transformation can effectively inhibit or hinder the crack propagation in the alloy, so that the ZrO distributed at intervals 2 The Co layer may improve the overall toughness of the alloy; (3) Because the hard alloy has the structural characteristic of 'double-component continuous and alternate distribution' and the thickness of each layer is only 140-160 microns, when the WC-Co layer with high wear resistance at the outer layer is completely worn and falls off, the new WC-Co layer can be quickly used as a bearing surface to resist the external friction action, so that the hard alloy product with the structure is not scrapped in a short time; (4) Because the 3D printing technology is used for printing layer by layer, the shape of the product is not limited, and the hard alloy part with a complex structure which is difficult to form by the conventional powder metallurgy process can be prepared. (5) The invention solves the problem of the traditional powder metallurgy method for preparationThe homogeneous structure hard alloy can not meet the problems of some special use requirements, and the hard alloy material with high hardness and high toughness is developed through the innovative design of the organization structure, so that the homogeneous structure hard alloy has outstanding popularization and application values.
Drawings
Morphology (a) and ZrO of WC-Co feed powder obtained by spray drying in FIG. 1, example 1 2 Morphology of Co feed powder (b).
FIG. 2, WC-Co and ZrO prepared 2 -microstructure of a laminated cemented carbide with alternating Co distribution, wherein (a) is the microstructure of the laminated cemented carbide prepared in example 1; (b) The microstructure of the laminated-structure cemented carbide prepared in example 2; (c) The microstructure of the laminated cemented carbide prepared in example 3 was used.
Fig. 3 shows the results of elemental analysis of each layer in the cemented carbide having a stacked structure prepared in example 2.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1 ZrO 2 having an average particle size of 0.2. Mu.m 2 Mixing powder, co powder with average particle size of 0.6 μm, polyethylene glycol and deionized water at a certain proportion to obtain slurry, spray drying to obtain spherical powder, heat treating the spray dried powder, and sieving to obtain ZrO powder with particle size distribution of 10-40 μm 2 -Co feed powder, where Co is ZrO 2 10% of-Co powder, 2% of polyethylene glycol and ZrO 2 The mass ratio of the-Co powder to the slurry is 65%, the heat treatment temperature of the spray granulation powder is 950 ℃, and the temperature is kept for 1h. And (3) agglomerating and granulating the WC-Co powder according to the same process, and screening to obtain WC-Co feed powder with the particle size distribution of 5-20 microns, wherein the average particle size of the initial WC powder is 0.8 mu m, and the mass percentage of Co in the WC-Co powder is 14%. WC-Co, zrO obtained by spray drying 2 The morphology of the-Co feed powder is shown in fig. 1 (a) and (b), respectively. ZrO to be obtained 2 Respectively and independently mixing the-Co feeding powder and the WC-Co feeding powder with the nylon powder uniformly, and respectively mixing the two mixed powdersPlacing the powder in two powder storage bins of a selective laser sintering printer, heating a powder laying platform to 170 ℃, continuously and alternately laying the powder in the two powder bins, melting nylon in each layer of powder through laser irradiation, and melting ZrO in each layer 2 And (2) bonding and forming Co or WC-Co powder, and stacking layer by layer to obtain the hard alloy green body with a laminated structure, wherein the hard alloy green body is in a required shape and has two components distributed continuously and alternately, the mass ratio of the nylon powder in each layer of powder is 4%, the powder spreading thickness of each layer is 140 mu m, the particle size distribution of the nylon powder is 20-80 mu m, and the heating rate of a powder spreading platform is 1.5 ℃/min. And (3) carrying out rapid hot-pressing sintering on the printed hard alloy green compact with the laminated structure, wherein the final state sintering temperature is 1170 ℃, the heat preservation time is 4min, the applied pressure is 45MPa, and cooling is carried out to obtain the hard alloy with the laminated structure and excellent comprehensive performance, wherein the microstructure of the hard alloy is shown in (a) in figure 2, and the test results of surface hardness, toughness and wear resistance are shown in table 1.
Example 2 ZrO 2 having an average particle size of 0.2 μm 2 Mixing powder, co powder with average particle size of 0.6 μm, polyethylene glycol and deionized water at a certain proportion to obtain slurry, spray drying to obtain spherical powder, heat treating the spray dried powder, and sieving to obtain ZrO powder with particle size distribution of 10-40 μm 2 -Co feed powder, where Co is ZrO 2 12% of-Co powder, 3% of polyethylene glycol and ZrO 2 The mass ratio of the-Co powder to the slurry is 60%, the heat treatment temperature of the spray granulation powder is 1000 ℃, and the heat preservation time is 1h. ) And (3) agglomerating and granulating the WC-Co powder according to the same process, and screening to obtain WC-Co feed powder with the particle size distribution of 5-20 microns, wherein the average particle size of the initial WC powder is 0.8 mu m, and the mass percentage of Co in the WC-Co powder is 12%. ZrO to be obtained 2 Respectively and uniformly mixing the-Co feeding powder and the WC-Co feeding powder with nylon powder, respectively placing the two mixed powders into two powder storage bins of a selective laser sintering printer, heating a powder laying platform to 170 ℃, continuously and alternately laying the powder in the two powder bins, melting the nylon in each layer of powder through laser irradiation, and melting ZrO in each layer of powder 2 Bonding and forming-Co or WC-Co powder, and stacking layer by layerPrinting to obtain the hard alloy green compact with the required shape and the double-component continuous and alternate distribution laminated structure, wherein the mass percentage of the nylon powder in each layer of powder is 5%, the powder spreading thickness of each layer is 150 mu m, the particle size distribution of the nylon powder is 20-80 mu m, and the heating rate of the powder spreading platform is 1.5 ℃/min. And (3) carrying out rapid hot-pressing sintering on the printed hard alloy green body with the laminated structure, wherein the final state sintering temperature is 1200 ℃, the heat preservation time is 3min, the applied pressure is 40MPa, and cooling is carried out to obtain the hard alloy with the laminated structure and excellent comprehensive performance, wherein the microstructure of the hard alloy is shown in (b) in figure 2, the element analysis result in each layer is shown in figure 3, and the surface hardness, toughness and wear resistance test result is shown in table 1.
Example 3 ZrO 2 having an average particle size of 0.2. Mu.m 2 Mixing powder, co powder with average particle size of 0.6 μm, polyethylene glycol and deionized water at a certain proportion to obtain slurry, spray drying to obtain spherical powder, heat treating the spray dried powder, and sieving to obtain ZrO with particle size distribution of 10-40 μm 2 -Co feed powder, where Co is ZrO 2 14% of-Co powder, 4% of polyethylene glycol and ZrO 2 The mass ratio of-Co powder to the slurry is 55%, the heat treatment temperature of the spray granulation powder is 1050 ℃, and the temperature is kept for 1h. ) And (3) agglomerating and granulating the WC-Co powder according to the same process, and screening to obtain WC-Co feed powder with the particle size distribution of 5-20 microns, wherein the average particle size of the initial WC powder is 0.8 mu m, and the mass percentage of Co in the WC-Co powder is 10%. ZrO to be obtained 2 Respectively and uniformly mixing the-Co feeding powder and the WC-Co feeding powder with nylon powder, respectively placing the two mixed powders into two powder storage bins of a selective laser sintering printer, heating a powder laying platform to 170 ℃, continuously and alternately laying the powder in the two powder bins, melting the nylon in each layer of powder through laser irradiation, and melting ZrO in each layer of powder 2 -Co or WC-Co powder is bonded and formed, and the cemented carbide green body with a laminated structure, which has a required shape and two components continuously and alternately distributed, can be printed after being stacked layer by layer, wherein the mass percentage of the nylon powder in each layer of powder is 6 percent, the powder spreading thickness of each layer is 160 mu m, the particle size distribution of the nylon powder is 20-80 mu m,the heating rate of the powder spreading platform is 1.5 ℃/min. And (3) carrying out rapid hot-pressing sintering on the printed hard alloy green body with the laminated structure, wherein the final state sintering temperature is 1230 ℃, the heat preservation time is 2min, the applied pressure is 35MPa, and cooling is carried out to obtain the hard alloy with the laminated structure and excellent comprehensive performance, wherein the microstructure of the hard alloy is shown as (c) in figure 2, and the test results of surface hardness, toughness and wear resistance are shown as table 1.
TABLE 1 hardness, toughness and wear resistance of cemented carbide with a laminated structure sintered at different temperatures
Claims (1)
1. The preparation method of the high-performance hard alloy with the laminated structure is characterized by comprising the following steps of:
(1) ZrO 2 is mixed with 2 Mixing the powder, co powder, polyethylene glycol and deionized water in proportion to prepare slurry, then spray-drying to obtain spherical powder, carrying out heat treatment on the spray-dried powder, and screening to obtain ZrO with particle size distribution of 10-40 microns 2 -Co feed powder of ZrO 2 The average particle size of the powder was 0.2 μm, the average particle size of Co powder was 0.6 μm, co was in ZrO 2 10-14% of-Co powder, 2-4% of polyethylene glycol and ZrO 2 The Co powder accounts for 55-65% of the mass ratio of the slurry, the heat treatment temperature of the spray granulation powder is 950-1050 ℃, and the heat preservation is carried out for 1h;
(2) Carrying out agglomeration granulation on WC-Co powder according to the process of the step (1), and screening to obtain WC-Co feed powder with the particle size distribution of 5-20 micrometers, wherein the average particle size of the WC powder is 0.8 mu m, and Co accounts for 10-14% of the mass fraction of the WC-Co powder;
(3) ZrO obtained in the step (1) and the step (2) 2 Respectively and independently mixing Co feeding powder and WC-Co feeding powder with nylon powder uniformly, respectively placing the two mixed powders into two powder storage bins of a selective laser sintering printer, heating a powder laying platform to 170 ℃, and then continuously and alternately laying powder in the two powder bins,melting nylon in each layer of powder by laser irradiation to obtain corresponding ZrO in each layer 2 the-Co or WC-Co powder is bonded and formed, and the hard alloy green body with the required shape and the double-component continuous and alternate distribution and the laminated structure can be obtained after stacking layer by layer, wherein the mass percentage of the nylon powder in each layer of powder is 4-6%, the powder spreading thickness of each layer is 140-160 mu m, the particle size distribution of the nylon powder is 20-80 mu m, and the heating rate of a powder spreading platform is 1.5 ℃/min;
(4) And (4) carrying out rapid hot-pressing sintering on the hard alloy green compact with the laminated structure printed in the step (3), wherein the final state sintering temperature is 1170-1230 ℃, the heat preservation time is 2-4min, the applied pressure is 35-45MPa, and the hard alloy with the laminated structure and the excellent comprehensive performance and the two components are continuously and alternately distributed after cooling.
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