CN102191393A - Preparation method of nickel molybdenum boron ternary boride base hard alloy - Google Patents
Preparation method of nickel molybdenum boron ternary boride base hard alloy Download PDFInfo
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- CN102191393A CN102191393A CN 201010127332 CN201010127332A CN102191393A CN 102191393 A CN102191393 A CN 102191393A CN 201010127332 CN201010127332 CN 201010127332 CN 201010127332 A CN201010127332 A CN 201010127332A CN 102191393 A CN102191393 A CN 102191393A
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Abstract
The invention provides a preparation method of nickel molybdenum boron ternary boride base hard alloy. The method comprises the following steps of: sequentially performing ball milling, blending, drying, forming and sintering steps on Mo powder, Ni powder and B powder serving as raw materials to prepare the hard alloy of which Mo2NiB2, namely the boron ternary boride, serves as a hard phase, and Ni base alloy serves as a binding phase. When the method is compared with the currently usually used 'reaction boronizing sintering method', the cost is greatly reduced, required equipment is few, and the preparation process is simple and is easy to realize. The Rockwell hardness (HRA) of the prepared hard alloy can be up to 86, the breaking strength can be up to 1.9GPa, the corrosion loss in 10 weight percent of HNO3 solution at the room temperature is less than 350g.m<2>.h<1>, and the mechanical property and the corrosion resistance can be similar to those of a sample prepared by the 'reaction boronizing sintering' method reported in the document.
Description
Technical field
The present invention relates to a kind of preparation method of molybdenum nickel boron ternary boride base cemented carbide, be mainly used in the wear resistant corrosion resistant field.
Background technology
High firmly, high-abrasive material has broad application prospects in fields such as preparation cutting tool, drill bit, mining machinery, wear-resisting moulds.These materials not only need high-wearing feature, but also will have high strength, high rigidity, high tenacity, a series of premium propertiess such as heat-resisting, anticorrosive.Carbide, nitride, oxide compound, boride can prepare Wimet mutually as hard, yet wherein maximum application of research also is with WC the most widely, carbide such as TiC are as the hard phase, with Co, Fe, metal such as Ni and alloy are as the Wimet of bonding phase.Yet, all belonging to short resource as W, the Co etc. of raw material, a large amount of uses of these elements do not meet the trend of current conservation of resources.
The boride of transition metal has high rigidity, high-melting-point and good electroconductibility and erosion resistance, is the strong candidate of high-abrasive material, existing many at present research reports about boride-based mechanically resistant material.But, also be difficult at short notice accomplish scale production because boride-based mechanically resistant material exists the problem that hard and metal bonding in hard-to-sinter and the sintering process form the fragility third phase mutually easily.
The ternary boride base cemented carbide also has good wear resistance, erosion resistance, resistance to elevated temperatures, and higher hardness, intensity and toughness, is a kind of novel abrasion-proof corrosion-proof corrosion material.From the Mo-Ni-B ternary phase diagrams, can find ternary boride Mo
2NiB
2Can stablize coexistence with metallic matrix Mo or Ni.In recent years, the method that the researchist of Japan's steel metal plate (Toyo Kohan) Co., Ltd. of Japan has proposed a kind of " reaction boronation sintering ", be the boride-based Wimet of feedstock production novel tertiary promptly with binary boride (as MoB, FeB, NiB, VB etc.) and metal, and the formation and the performance of ternary boride explored, different with the production technique of ordinary rigid alloy, the ternary boride as the hard phase forms in sintering process in the method.At present, utilize the method for " reaction boronation sintering " successfully to prepare Mo
2FeB
2-Fe, Mo
2NiB
2-Ni, ternary boride base cemented carbides such as WCoB-Co.Their outstanding advantage has nothing in common with each other, Mo
2FeB
2Base cemented carbide has outstanding wear resistance, Mo
2NiB
2Base cemented carbide has outstanding erosion resistance, and the WCoB base cemented carbide has the good temperature resistance energy.In Japan, these materials as antiwear heat resisting corrosion-resistant member successful Application in fields such as the hot extruding die of injection moulding machine, copper, sea-water pump bearings.
In China, the research of relevant ternary boride mainly concentrates on it is covered the steel matrix aspect as hard coat, and material also only is confined to Mo
2FeB
2, and the research of ternary boride base cemented carbide seldom has bibliographical information, still need aspect application exploitation and expansion.Why the ternary boride base cemented carbide does not cause enough attention in China, it is main because China's tungsten ore resource is abundant relatively, the research WC base cemented carbide is relative with application ripe, in addition, to cost an arm and a leg also be a major reason to preparation ternary boride required binary boride.Yet WC is the important strategic goods and materials, and along with the exploitation of tungsten ore resource totally, the hard wear-resistant material of seeking novel not tungstenic is extremely urgent.Mo
2NiB
2The ternary boride base cemented carbide is exactly most suitable equivalent material, it not only has high strength, high rigidity, high tenacity, and has a very outstanding erosion resistance, but want the scope of further its application of develop and spread, also need under the prerequisite that does not reduce its various aspects of performance, reduce its preparation cost.
Summary of the invention
The object of the present invention is to provide a kind of preparation were established of new molybdenum nickel boron ternary boride base cemented carbide, to reduce Mo
2NiB
2The preparation cost of ternary boride, replacing the WC Wimet to a certain extent, thus the protection strategic resource.
The present invention solves above-mentioned technical problem by the following technical solutions:
A kind of preparation method of molybdenum nickel boron ternary boride base cemented carbide, may further comprise the steps: with Mo powder, Ni powder and B powder is raw material, makes with Mo through ball milling mixing, drying, moulding and sintering step successively
2NiB
2Ternary boride is the hard phase, serves as the Wimet of bonding phase with Ni base alloy.
Preferably, the purity of described Mo powder＞95% is crossed 200 mesh sieves; The purity of described Ni powder＞95% is crossed 325 mesh sieves; The purity of described B powder＞95% is crossed 325 mesh sieves.
Preferably, in the described raw material, according to Mo
2NiB
2In the Mol ratio of each element, be benchmark in B, Mo is excessive 2～22%, Ni excessive 54～154% carries out proportioning; Be Mo: Ni: the mol ratio of B is (1.02～1.22): (0.77～1.27): 1.
Preferably, in the described ball milling mixing process, be dispersion medium with dehydrated alcohol or acetone, with Stainless Steel Ball or Si
3N
4Ball is a ball-milling medium, and ball material weight ratio is (2～4): 1, and the ball mill mixing time is 8～16 hours.
Preferably, described drying process is at 55～85 ℃ of oven dry, the powder that obtains mixing with gained slurry in the described ball milling mixing process.
Preferably, described moulding process is at 5～50kgf/cm
2Pressure under with the powder compacting of described drying process gained, preferably at 10～40kgf/cm
2Pressure under with the powder compacting of described drying process gained.
Preferably, described sintering process is a sintering under vacuum or inert atmosphere (as Ar gas shiled atmosphere), and heat-up rate is 3～20 ℃/min, and sintering temperature is 1150～1600 ℃, and is incubated 20～120min under this sintering temperature, then with the stove naturally cooling.
To adopting the prepared molybdenum nickel boron ternary boride base cemented carbide of aforesaid method to carry out mechanical property and erosion resistance test, Rockwell hardness HRA reaches as high as 86, and cross-breaking strength can reach 1.9GPa, under the room temperature at the HNO of 10wt.%
3Corrosion loss amount in the solution is at 300gm
-2H
-1About, these characteristics all this system Wimet with " reaction boronation sintering " method preparation are close.
Polished surface and the surface of fracture that adopts the prepared molybdenum nickel boron ternary boride base cemented carbide of aforesaid method carried out microscopic examination, find even particle distribution, size is at 2～6 μ m, and fracture mode mainly is a transgranular fracture.
Compared with prior art, beneficial effect of the present invention is:
1) cost of material is relatively cheap, and preparation cost is lower;
2) required equipment is few, and preparation technology is simple, realizes easily;
3) prepared molybdenum nickel boron ternary boride base cemented carbide even structure has higher hardness and intensity, and mechanical property can compare favourably with existing reported values.
Description of drawings
Fig. 1. the XRD figure spectrum of embodiment 1-3 gained alloy;
Fig. 2. the typical mechanical property of embodiment 1-3 gained alloy compares with the performance of existing " reaction boronation sintering " method gained alloy;
Fig. 3. (a:1150 ℃ in the SEM photo of the surface of fracture of embodiment 1-3 gained alloy; B:1350 ℃; C:1550 ℃).
Fig. 4. embodiment 4 gained alloys are at the HNO of 10wt.%
3The SEM photo of corrosion after 1 hour in the solution.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in restriction protection scope of the present invention.
Embodiment 1
Take by weighing Mo:16.13g respectively, Ni:12.09g, B:1.78g (prescription 1), with acetone is dispersion medium, and Stainless Steel Ball is abrading-ball (ratio of grinding media to material is 4: 1), batch mixing 12h, the slurry of gained sieves by rotary evaporation and oven dry and obtains the mixed powder of good fluidity, at 40kgf/cm
2Forming under the pressure, sintering in vacuum oven then, heat-up rate is 5 ℃/min, at 1150 ℃ of insulation 120min.Interpretation of result shows that gained sample main component is hard phase Mo
2NiB
2With the Ni mutually that bonds, as shown in Figure 1.Rockwell hardness HRA can reach 81.3, and cross-breaking strength can reach 1.58GPa, and fracture mode is mainly along brilliant fracture, as shown in Figure 3.HNO at 10wt.%
3Corrosion loss amount in the solution is 259gm
-2H
-1
Embodiment 2
Obtain the mixed powder of good fluidity by embodiment 1, at 10kgf/cm
2Forming under the pressure, sintering in vacuum oven then, heat-up rate is 20 ℃/min, at 1350 ℃ of insulation 60min.Rockwell hardness HRA can reach 84.8, and cross-breaking strength can reach 1.79GPa, and fracture mode is mainly transgranular fracture.HNO at 10wt.%
3Corrosion loss amount in the solution is 242gm
-2H
-1
Embodiment 3
Obtain the mixed powder of good fluidity by embodiment 1, at 10kgf/cm
2Forming under the pressure, sintering in vacuum oven then, heat-up rate is 10 ℃/min, at 1550 ℃ of insulation 20min.Rockwell hardness HRA can reach 83.2, and cross-breaking strength can reach 1.71GPa.HNO at 10wt.%
3Corrosion loss amount in the solution is 285gm
-2H
-1
Embodiment 4
Take by weighing Mo:19.98g respectively, Ni:8.15g, B:1.87g (prescription 2) is a ball-milling medium with the dehydrated alcohol, Si
3N
4Ball is an abrading-ball, and ratio of grinding media to material is 2: 1, and batch mixing 16h, gained slurry sieve by rotary evaporation and oven dry and obtain the mixed powder of good fluidity, at 40kgf/cm
2Forming under the pressure, sintering in vacuum oven then, heat-up rate is 5 ℃/min, at 1150 ℃ of insulation 120min.Interpretation of result shows that gained sample main component is hard phase Mo
2NiB
2With the Ni mutually that bonds.Rockwell hardness HRA can reach 82.9, and cross-breaking strength can reach 1.38GPa.HNO at 10wt.%
3Corrosion loss amount in the solution is 334gm
-2H
-1, the SEM photo after the corrosion as shown in Figure 4.
Embodiment 5
Obtain the mixed powder of good fluidity by embodiment 4, at 10kgf/cm
2Forming under the pressure, sintering in vacuum oven then, heat-up rate is 15 ℃/min, at 1200 ℃ of insulation 120min.Rockwell hardness HRA can reach 85.7, and cross-breaking strength can reach 1.53GPa.HNO at 10wt.%
3Corrosion loss amount in the solution is 272gm
-2H
-1
Embodiment 6
Take by weighing Mo:19.98g respectively, Ni:9.54g, B:1.87g (prescription 3) is a ball-milling medium with the dehydrated alcohol, Si
3N
4Ball is an abrading-ball, and ratio of grinding media to material is 2: 1, and batch mixing 8h, gained slurry sieve and obtain the mixed powder of good fluidity by rotary evaporation and oven dry under 55～85 ℃, at 40kgf/cm
2Forming under the pressure, sintering under Ar gas atmosphere protection then, heat-up rate is 3 ℃/min, at 1600 ℃ of insulation 40min.Interpretation of result shows that gained sample main component is hard phase Mo
2NiB
2With the Ni mutually that bonds.Rockwell hardness HRA can reach 81.3, and cross-breaking strength can reach 1.58GPa.HNO at 10wt.%
3Corrosion loss amount in the solution is 259gm
-2H
-1
Raw material used in the foregoing description all satisfies: the purity of Mo powder＞95%, cross 200 mesh sieves; The purity of Ni powder＞95% is crossed 325 mesh sieves; The purity of B powder＞95% is crossed 325 mesh sieves.
Claims (7)
1. the preparation method of a molybdenum nickel boron ternary boride base cemented carbide, may further comprise the steps: with Mo powder, Ni powder and B powder is raw material, successively through ball milling mix, dry, moulding and sintering step make with Mo
2NiB
2Ternary boride is the hard phase, serves as the Wimet of bonding phase with Ni base alloy.
2. the preparation method of molybdenum nickel boron ternary boride base cemented carbide as claimed in claim 1 is characterized in that, the purity of described Mo powder＞95% is crossed 200 mesh sieves; The purity of described Ni powder＞95% is crossed 325 mesh sieves; The purity of described B powder＞95% is crossed 325 mesh sieves.
3. the preparation method of molybdenum nickel boron ternary boride base cemented carbide as claimed in claim 1 is characterized in that in the described raw material, the mol ratio of Mo: Ni: B is (1.02～1.22): (0.77～1.27): 1.
4. the preparation method of molybdenum nickel boron ternary boride base cemented carbide as claimed in claim 1 is characterized in that, in the described ball milling mixing process, is dispersion medium with dehydrated alcohol or acetone, with Stainless Steel Ball or Si
3N
4Ball is a ball-milling medium, and ball material weight ratio is (2～4): 1, and the ball mill mixing time is 8～16 hours.
5. the preparation method of molybdenum nickel boron ternary boride base cemented carbide as claimed in claim 1 is characterized in that, described drying process is 55～85 ℃ of oven dry with gained slurry in the described ball milling mixing process.
6. the preparation method of molybdenum nickel boron ternary boride base cemented carbide as claimed in claim 1 is characterized in that described moulding process is at 5～50kgf/cm
2Pressure under with the powder compacting of described drying process gained.
7. as the preparation method of the described molybdenum nickel of arbitrary claim boron ternary boride base cemented carbide among the claim 1-6, it is characterized in that, described sintering process is a sintering under vacuum or inert atmosphere, and heat-up rate is 3～20 ℃/min, and sintering temperature is 1150～1600 ℃.
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| CN112111684B (en) * | 2020-10-10 | 2021-11-30 | 广东博杰特新材料科技有限公司 | 3D prints ternary boride Mo2NiB2Alloy powder and production process thereof |
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| CN116121616A (en) * | 2022-11-25 | 2023-05-16 | 西安近代化学研究所 | TiN modified Mo 2 NiB 2 Method for producing a base composite material |
| CN116621586A (en) * | 2023-05-29 | 2023-08-22 | 西安热工研究院有限公司 | WNiB ceramic and preparation method thereof |
| CN117819982B (en) * | 2023-12-01 | 2024-06-11 | 西南大学 | High-entropy boride ceramic and preparation method thereof |
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Application publication date: 20110921 |