CN104651653B - A kind of preparation method of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density - Google Patents
A kind of preparation method of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density, first nitric acid tungsten, nickel nitrate, copper nitrate, Yttrium trinitrate and water are made into mixed solution by predetermined dose ratio, being configured to alkaline solution with certain density ammonia spirit again, alkaline solution is agitated, crystallization, filter, wash, be dried to obtain precursor powder；Precursor powder is put into reducing atmosphere stove is carried out dissociate, reduction treatment, obtain the tungsten-nickel-copper alloy powder containing yttrium；Alloy powder is polished to be mixed with forming agent and compressing, and gained shaping blank carries out dewaxing, high temperature sintering, final acquisition microalloying of rare earth high density high-strength tungsten-nickel-copper alloy material.The present invention with use the microalloying of rare earth tungsten-nickel-copper alloy powder for preparing of liquid liquid doping method as raw material, the tungsten-nickel-copper alloy prepared by suitable powder metallurgical technique technology, its density >=18.1g/cm3, tensile strength >=850MPa, yield strength >=690MPa.
Description
Technical field
The present invention relates to tungsten alloy material technical field, particularly relate to the preparation method of a kind of high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density.
Background technology
As functional material, tungsten-bast alloy is widely used in the fields such as Aero-Space, electricity power, defence and military and nuclear industry, is used for manufacturing gyro wheel, rocket nozzle, armor-piercing bullet bullet core, high-voltage electrical apparatus switch contact etc..Owing to the elastic modelling quantity of tungsten alloy material is much larger than ferrous materials, therefore may be utilized in fabricating the mill bar of internal thread grinding machine, to reduce mill bar elastic deformation in grinding process, it is ensured that the machining accuracy of female thread and working (machining) efficiency.But common tungsten-bast alloy is compared with structural steel, its intensity is low and fragility is big, it is impossible to meet the requirement of strength of female thread mill pole pair material.How to improve the intensity of tungsten-bast alloy to play the advantage of its high rigidity, just become and manufacture the precondition meeting this kind of structural member performance requirement.
In recent years, many scholars concentrate on material powder preparation and modified aspect to the research of tungsten-nickel-copper alloy tissue, hydrodynamics, and the preparation of tungsten-nickel-copper alloy powder and method of modifying mainly include being atomized water-cooled, high-energy ball milling and oxide reduction, prepared alloy powder still suffer from segregation, be mingled with, the problem such as Task-size Controlling is difficult, greatly govern the further raising of tungsten-nickel-copper alloy microstructure and mechanical property.
Summary of the invention
It is an object of the invention to the deficiency existed for above-mentioned background technology, by using a kind of pre-alloyed powder technology of preparing, and select a kind of microalloy element that tungsten-nickel-copper alloy structure property is greatly improved, realize the Uniform Doped of microalloy element, the final preparation method that a kind of high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density is provided.
For achieving the above object, the technical solution used in the present invention is as follows:
The preparation method of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density of the present invention, specifically comprises the following steps that
(1) it is 52～53.4:1.5～4.8:1.2～2.5:0.11～0.34:2500～3000 to weigh nitric acid tungsten, nickel nitrate, copper nitrate, Yttrium trinitrate and water in molar ratio, is made into mixed solution；
(2) under the conditions of 25～40 DEG C, gained mixed solution is mixed with the ammonia spirit that concentration is 14.56～15.12mol/L, it is made into alkaline solution, ammonia spirit used is 3:1 with the volume ratio of step (1) gained mixed solution, and gained alkaline solution is agitated, crystallization, filter, wash, be dried to obtain precursor powder；
(3) precursor powder is put in reducing atmosphere stove carry out dissociating, reduction treatment, obtain the tungsten-nickel-copper alloy powder containing yttrium；
(4) the tungsten-nickel-copper alloy powder mull containing yttrium is become fine powder, add forming agent mixing, carry out ball milling after mixing, the alloy powder after ball milling is pressed, obtains shaping blank；
(5) shaping blank is heated, slough plasticizer, and by high temperature sintering under argon atmosphere, obtain microalloying of rare earth high density high-strength tungsten-nickel-copper alloy material.
Further, it is to carry out under the conditions of 30 DEG C during step (2) preparation alkaline solution.
Further, in step (2), stir by constant temperature blender with magnetic force during preparation alkaline solution, rotating speed 1000rpm, stirring crystallization temperature 53～65 DEG C, crystallization time 18～23 hours, be dried under the conditions of 150 DEG C with vacuum drying oven.
Further, in step (3), precursor powder is put in carbon atmosphere revolution fluidized furnace, carry out dissociating at 870～910 DEG C, reduction treatment.
Further, in step (4), grinding to form addition forming agent in the alloy powder of fine powder, mix 1.5 hours, then use ball milling 22 hours in planetary ball mill, rotating speed is 350 revs/min；Blank molding uses single shaft die press technology for forming, and mould uses high-strength WC-Co hard alloy to be fabricated by, and briquetting pressure is 240MPa.
Further, in step (5), by sloughing the plasticizer in blank under 170 DEG C of heating conditions.
Further, in step (5), under the conditions of argon shield, the blank sloughing forming agent being carried out high temperature sintering, sintering temperature is 1410 DEG C, temperature retention time 1.4 hours, 6 DEG C/min of heating rate, 15 DEG C/min of rate of temperature fall.
The present invention is to use the microalloying of rare earth tungsten-nickel-copper alloy powder for preparing of liquid liquid doping method as raw material, the tungsten-nickel-copper alloy prepared by suitable powder metallurgical technique technology, its density >=18.1g/cm3, tensile strength >=850MPa, yield strength >=690MPa.
Compared with prior art, the invention have the characteristics that and advantage:
(1) during preparing microalloying of rare earth tungsten-nickel-copper alloy block, the present invention changes rely on merely elemental metals or metal-oxide as raw material to prepare the thinking of tungsten-nickel-copper alloy block in existing method completely, but use liquid liquid doping method, with metal nitrate as raw material, solve rare-earth yttrium occurrence status in tungsten-nickel-copper alloy by solution ratio, optimization of synthesis etc., and obtain microalloying of rare earth tungsten-nickel-copper alloy powder.
(2) this preparation method has prominent specific aim, and Composition Control precision is high, and process stabilizing and repeatability are strong, overcomes the harmful effect because alloying elements distribution is uneven and the mechanical property of prepared tungsten-nickel-copper alloy is brought by coarse grains.
(3) in the preparation process of microalloying of rare earth high density high-strength tungsten-nickel-copper alloy block, use single shaft die forming technique, shaping dies uses high-strength WC-Co hard alloy to be fabricated by, on the one hand the densification of big load cold forming process is conducive to, shaping blank is made to have higher density and structural homogenity, it is ensured that the tungsten-nickel-copper alloy block performance on the whole after sintering is consistent；On the other hand can reduce in cold forming process and bring impurity into because of powder body and the friction of mould, it is ensured that the pure property of entirety of tungsten-nickel-copper alloy body composition of colding pressing.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The preparation method of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density of the embodiment of the present invention, specifically comprises the following steps that
(1) it is 52～53.4:1.5～4.8:1.2～2.5:0.11～0.34:2500～3000 to weigh nitric acid tungsten, nickel nitrate, copper nitrate, Yttrium trinitrate and water in molar ratio, is made into mixed solution；
(2) under the conditions of 25～40 DEG C, gained mixed solution is mixed with the ammonia spirit that concentration is 14.56～15.12mol/L, it is made into alkaline solution, ammonia spirit used is 3:1 with the volume ratio of step (1) gained mixed solution, and gained alkaline solution is agitated, crystallization, filter, wash, be dried to obtain precursor powder；
(3) precursor powder is put in reducing atmosphere stove carry out dissociating, reduction treatment, obtain the tungsten-nickel-copper alloy powder containing yttrium；
(4) the tungsten-nickel-copper alloy powder mull containing yttrium is become fine powder, add forming agent mixing, carry out ball milling after mixing, the alloy powder after ball milling is pressed, obtains shaping blank；
(5) shaping blank is heated, slough plasticizer, and by high temperature sintering under argon atmosphere, obtain microalloying of rare earth high density high-strength tungsten-nickel-copper alloy material.
In embodiments of the present invention, it is to carry out under the conditions of 30 DEG C during step (2) preparation alkaline solution.
In embodiments of the present invention, in step (2), stir by constant temperature blender with magnetic force during preparation alkaline solution, rotating speed 1000rpm, stirring crystallization temperature 53～65 DEG C, crystallization time 18～23 hours, be dried under the conditions of 150 DEG C with vacuum drying oven.
In embodiments of the present invention, in step (3), precursor powder is put in carbon atmosphere revolution fluidized furnace, carry out dissociating at 870～910 DEG C, reduction treatment.
In embodiments of the present invention, in step (4), grinding to form addition forming agent in the alloy powder of fine powder, mix 1.5 hours, then use ball milling 22 hours in planetary ball mill, rotating speed is 350 revs/min；Blank molding uses single shaft die press technology for forming, and mould uses high-strength WC-Co hard alloy to be fabricated by, and briquetting pressure is 240MPa.
In embodiments of the present invention, in step (5), by sloughing the plasticizer in blank under 170 DEG C of heating conditions.
In embodiments of the present invention, in step (5), under the conditions of argon shield, the blank sloughing forming agent being carried out high temperature sintering, sintering temperature is 1410 DEG C, temperature retention time 1.4 hours, 6 DEG C/min of heating rate, 15 DEG C/min of rate of temperature fall.
Below in conjunction with specific embodiment, the application principle of the present invention is further described.In following example, the hard alloy block tensile strength of material test condition of preparation meets " GB/T228.1-2010 " standard, and density measurement condition meets " GB/T5163-2006 " standard.
Embodiment 1
52:4.4:2.5:0.11 weighs nitric acid tungsten (WNO respectively the most in molar ratio3·2H2O), nickel nitrate (Ni (NO3)2·6H2O), copper nitrate (Cu (NO3)2·6H2And Yttrium trinitrate (Y (NO O)3)3·6H2O), the concrete consumption of raw material weighed is: nitric acid tungsten (WNO3·2H2O) it is 146.5g, nickel nitrate (Ni (NO3)2Be 6H2O) 12.8g, copper nitrate (Cu (NO3) 2 6H2O) be 7.4g, Yttrium trinitrate (Y (NO3)3·6H2O) it is 0.42g, measures distilled water 450ml with graduated cylinder, the raw material weighed is joined stirring and dissolving in beaker with the distilled water measured, it is thus achieved that mixed solution.Under the conditions of 30 DEG C, being to join mixed solution in dropping mode in 14.56mol/L ammonia spirit by concentration, ammonia/mixed liquor volume ratio is for 3:1, and be stirred at 59 DEG C, crystallization 18 hours, through filtering, 150 DEG C of vacuum drying obtain precursor powder；
Take out precursor powder, 890 DEG C with carbon atmosphere revolution fluidized furnace carry out dissociating, reduction treatment, obtain containing yttrium tungsten-nickel-copper alloy powder；
Yttrium tungsten-nickel-copper alloy powder will be contained, grind to form fine powder, and add forming agent and mix 1.5 hours, ball milling 22 hours after mixed, and the powder body loading cold stamping die after ball milling is pressed into green compact in single shaft moulding press, mould uses high-strength WC-Co hard alloy to be fabricated by, briquetting pressure 240MPa；
With air dry oven, green compact are dewaxed at 170 DEG C, and carry out high temperature sintering, sintering temperature 1410 DEG C, temperature retention time 1.4 hours, 6 DEG C/min of heating rate, 15 DEG C/min of rate of temperature fall, argon shield.
Embodiment 2
Nitric acid tungsten (WNO is weighed the most in molar ratio for 52.8:2.7:1.7:0.223·2H2O), nickel nitrate (Ni (NO3)2·6H2O), copper nitrate (Cu (NO3)2·6H2And Yttrium trinitrate (Y (NO O)3)3·6H2O), the concrete consumption of raw material weighed is: nitric acid tungsten (WNO3·2H2O) it is 148.8g, nickel nitrate (Ni (NO3)2·6H2O) be 7.86g, copper nitrate (Cu (NO3)2·6H2O) it is 5.03g, Yttrium trinitrate (Y (NO3)3·6H2O) it is 0.84g, measures distilled water 500ml with graduated cylinder, the raw material weighed is joined stirring and dissolving in beaker with the distilled water measured, it is thus achieved that mixed solution.Under the conditions of 34 DEG C, being to join mixed solution in dropping mode in 14.88mol/L ammonia spirit by concentration, ammonia/mixed liquor volume ratio is for 3:1, and be stirred at 62 DEG C, crystallization 21 hours, through filtering, 150 DEG C of vacuum drying obtain precursor powder；
Take out precursor powder, 890 DEG C with carbon atmosphere revolution fluidized furnace carry out dissociating, reduction treatment, obtain containing yttrium tungsten-nickel-copper alloy powder；
Yttrium tungsten-nickel-copper alloy powder will be contained, grind to form fine powder, and add forming agent and mix 1.5 hours, ball milling 22 hours after mixed, and ball-milled powder is loaded cold stamping die in single shaft moulding press, be pressed into green compact, mould uses high-strength WC-Co hard alloy to be fabricated by, pressure 240MPa；
With air dry oven, green compact are dewaxed at 170 DEG C, and carry out high temperature sintering, sintering temperature 1410 DEG C, temperature retention time 1.4 hours, 6 DEG C/min of heating rate, 15 DEG C/min of rate of temperature fall, argon shield.
Embodiment 3
Nitric acid tungsten (WNO is weighed the most in molar ratio for 53.4:1.5:1.2:0.343·2H2O), nickel nitrate (Ni (NO3)2·6H2O), copper nitrate (Cu (NO3)2·6H2O), Yttrium trinitrate (Y (NO3)3·6H2O), the concrete consumption of raw material weighed is: nitric acid tungsten (WNO3·2H2O) it is 150.5g, nickel nitrate (Ni (NO3)2·6H2O) be 4.37g, copper nitrate (Cu (NO3)2·6H2O) it is 3.55g, Yttrium trinitrate (Y (NO3)3·6H2O) it is 1.3g, measures distilled water 540ml with graduated cylinder, the raw material weighed is joined stirring and dissolving in beaker with the distilled water measured, it is thus achieved that mixed solution.Under the conditions of 38 DEG C, it is that 15.12mol/L ammonia spirit joins mixed solution in dropping mode by 1200ml concentration, ammonia/mixed liquor volume ratio is for 3:1, and be stirred at 65 DEG C, crystallization 23 hours, through filtering, 150 DEG C of vacuum drying obtain precursor powder；
Take out precursor powder, 910 DEG C with carbon atmosphere revolution fluidized furnace carry out dissociating, reduction treatment, obtain containing yttrium tungsten-nickel-copper alloy powder；
Yttrium tungsten-nickel-copper alloy powder will be contained, grind to form fine powder, and add forming agent and mix 1.5 hours, ball milling 22 hours after mixed, and ball-milled powder is loaded cold stamping die in single shaft moulding press, be pressed into green compact, mould uses high-strength WC-Co hard alloy to be fabricated by, pressure 240MPa；
With air dry oven, green compact are dewaxed at 170 DEG C, and carry out high temperature sintering, sintering temperature 1410 DEG C, temperature retention time 1.4 hours, 6 DEG C/min of heating rate, 15 DEG C/min of rate of temperature fall, argon shield.
Embodiment 4
52:3.2:2:0.28 weighs nitric acid tungsten (WNO respectively the most in molar ratio3·2H2O), nickel nitrate (Ni (NO3)2·6H2O), copper nitrate (Cu (NO3)2·6H2And Yttrium trinitrate (Y (NO O)3)3·6H2O), the concrete consumption of raw material weighed is: nitric acid tungsten (WNO3·2H2O) it is 146.5g, nickel nitrate (Ni (NO3)2Be 6H2O) 9.31g, copper nitrate (Cu (NO3) 2 6H2O) be 5.92g, Yttrium trinitrate (Y (NO3)3·6H2O) it is 1.07g, measures distilled water 530ml with graduated cylinder, the raw material weighed is joined stirring and dissolving in beaker with the distilled water measured, it is thus achieved that mixed solution.Under the conditions of 30 DEG C, being to join mixed solution in dropping mode in 14.56mol/L ammonia spirit by concentration, ammonia/mixed liquor volume ratio is for 3:1, and be stirred at 55 DEG C, crystallization 21 hours, through filtering, 150 DEG C of vacuum drying obtain precursor powder；
Take out precursor powder, 890 DEG C with carbon atmosphere revolution fluidized furnace carry out dissociating, reduction treatment, obtain containing yttrium tungsten-nickel-copper alloy powder；
Yttrium tungsten-nickel-copper alloy powder will be contained, grind to form fine powder, and add forming agent and mix 1.5 hours, ball milling 22 hours after mixed, and ball-milled powder is loaded cold stamping die in single shaft moulding press, be pressed into green compact, mould uses high-strength WC-Co hard alloy to be fabricated by, pressure 240MPa；
With air dry oven, green compact are dewaxed at 170 DEG C, and carry out high temperature sintering, sintering temperature 1410 DEG C, temperature retention time 1.4 hours, 6 DEG C/min of heating rate, 15 DEG C/min of rate of temperature fall, argon shield.
The different embodiment of table 1 prepares the performance parameter of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density
As can be seen from Table 1, the microalloying of rare earth tungsten-nickel-copper alloy prepared by embodiment 1-4 method has the features such as density is high, crystal grain is tiny, fine and close, high-strength.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (4)
1. the preparation method of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density, it is characterised in that: described preparation method
Specifically comprise the following steps that
(1) be in molar ratio 52～53.4:1.5～4.8:1.2～2.5:0.11～0.34:2500～3000 weigh nitric acid tungsten,
Nickel nitrate, copper nitrate, Yttrium trinitrate and water, be made into mixed solution；
(2) under the conditions of 25～40 DEG C, gained mixed solution is mixed with the ammonia spirit that concentration is 14.56～15.12mol/L,
Being made into alkaline solution, ammonia spirit used is 3:1 with the volume ratio of step (1) gained mixed solution, gained alkaline solution warp
Stirring, crystallization, filter, wash, be dried to obtain precursor powder；
(3) precursor powder is put in reducing atmosphere stove carry out dissociating, reduction treatment, obtain the tungsten ambrose alloy containing yttrium and close
Bronze end；
(4) the tungsten-nickel-copper alloy powder mull containing yttrium is become fine powder, adds forming agent mixing, after mixing, carry out ball milling,
Alloy powder after ball milling is pressed, obtains shaping blank；
(5) shaping blank is heated, slough forming agent, and by high temperature sintering under argon atmosphere, obtain rare earth micro-
Alloying high density high-strength tungsten-nickel-copper alloy material；
In described step (2), stir by constant temperature blender with magnetic force during preparation alkaline solution, rotating speed 1000rpm, stir crystallization temperature
Spend 53～65 DEG C, crystallization time 18～23 hours, it is dried under the conditions of 150 DEG C with vacuum drying oven；
In described step (4), grind to form addition forming agent in the alloy powder of fine powder, mix 1.5 hours, then use planet
Ball milling 22 hours in ball mill, rotating speed is 350 revs/min；Blank molding uses single shaft die press technology for forming, mould
Using high-strength WC-Co hard alloy to be fabricated by, typed pressure is 240MPa；
In described step (5), under the conditions of argon shield, the blank sloughing forming agent is carried out high temperature sintering, sintering temperature
Degree is 1410 DEG C, temperature retention time 1.4 hours, 6 DEG C/min of heating rate, 15 DEG C/min of rate of temperature fall.
2. the preparation method of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density as claimed in claim 1, it is characterised in that:
It is to carry out under the conditions of 30 DEG C during step (2) preparation alkaline solution.
3. the preparation method of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density as claimed in claim 1, it is characterised in that:
In step (3), precursor powder is put in carbon atmosphere revolution fluidized furnace, carry out dissociating, going back original place at 870～910 DEG C
Reason.
4. the preparation method of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density as claimed in claim 1, it is characterised in that:
In step (5), by sloughing the forming agent in blank under 170 DEG C of heating conditions.
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| CN105349814B (en) * | 2015-10-21 | 2017-06-30 | 陕西理工学院 | The preparation method of Co base high temperature adhesive hard alloy |
| CN105268983B (en) * | 2015-10-21 | 2017-09-22 | 陕西理工学院 | The preparation method of W Ni Cu pre-alloyed powders |
| CN105921762B (en) * | 2016-06-17 | 2017-11-03 | 陕西理工学院 | The Co-based alloy powder preparation method of shaping can be densified |
| CN110885957A (en) * | 2019-12-20 | 2020-03-17 | 西安华山钨制品有限公司 | Process for improving density of tungsten-nickel-copper alloy |
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