CN103143725B - The preparation method of rare earth modified tungsten-base alloy powder - Google Patents
The preparation method of rare earth modified tungsten-base alloy powder Download PDFInfo
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Abstract
The preparation method of rare earth modified tungsten-base alloy powder, comprises the following steps: the salting liquid of tungsten, copper, nickel and rare earth mixes according to the stoichiometric proportion of required tungsten-copper alloy powder by (1), makes reaction stoste; (2) stoste be atomized and spray into reative cell, controlling reaction atmosphere, carry out solution atomization reduction reaction, obtain elementary tungsten-base alloy powder; (3) elementary tungsten-base alloy powder is collected, obtain high performance rare earth modified tungsten-copper alloy powder by high-temperature process.The present invention adopts pyrosol atomization reduction technique to prepare rare earth modified tungsten-base alloy powder, with metal target salting liquid for raw material, by being atomized into aerosol in closed reactor, simultaneously aerosol occurs to decompose and fast reaction obtains target product under the high temperature conditions, it possesses the advantage that vapor phase method and liquid phase method combine, and has that milling efficiency is high, technique is simple, reaction process is controlled, environment amenable advantage.
Description
Technical field
The present invention relates to a kind of preparation method of tungsten-base alloy powder, be specially a kind of method adopting pyrosol atomization reducing process directly to prepare rare earth modified tungsten-base alloy powder.
Background technology
Tungsten-bast alloy is the finely processed product of the second largest eka-tungsten being only second to carbide alloy, is widely used in the fields such as the energy, metallurgy, electronic information, machining, Aero-Space, defence and military and nuclear industry.At present, main tungsten-bast alloy goods have W-Cu, W-Ni-Fe, W-Ni-Cu etc., and its conventional technique of preparation both at home and abroad mainly comprises machine-alloying (MA), sol-gel process (Sol-Gel), condensation seasoning (Freeze Drying), chemical vapor infiltration (Chemical Vapor Deposition), spray drying process (Spray Drying) and solution atomization method (solution Spray) etc.
Comparatively advanced method is that (atomizing and oxidizing solution prepares method that is single or composite metal oxide to pyrosol atomization, national inventing patent, the patent No.: ZL 200920063526.9, authorized announcement date: on October 27th, 2010), the method can be divided into pyrosol atomizing and oxidizing method and pyrosol atomization reducing process.Pyrosol atomizing and oxidizing method is carried out in an oxidizing atmosphere, and the product obtained is metal and alloyed oxide.Pyrosol atomization reducing process is carried out under reducing atmosphere, and the product obtained is metal and alloy powder.
Summary of the invention
Technical problem solved by the invention is: the deficiency existed for prior art, provides that a kind of milling efficiency is high, technique is simple, reaction process is controlled, the preparation method of environment amenable rare earth modified tungsten-base alloy powder.The method for raw material, by adding appropriate rare earth, adopts pyrosol atomization reducing process directly to prepare high-performance rare-earth modification tungsten-base alloy powder with many metal salt solutions such as tungsten and copper nickel.
Technical problem solved by the invention realizes by the following technical solutions:
The preparation method of rare earth modified tungsten-base alloy powder, comprises the following steps:
(1) source liquid prepares: mixed by the salting liquid of tungsten, copper, nickel and rare earth according to the stoichiometric proportion of required tungsten-copper alloy powder, make reaction stoste;
(2) atomization reduction: stoste be atomized and spray into reative cell, controls reaction atmosphere, carries out solution atomization reduction reaction, obtain elementary tungsten-base alloy powder;
(3) sample collection and post processing: collected by elementary tungsten-base alloy powder, obtains high performance rare earth modified tungsten-copper alloy powder by high-temperature process.
Innovative point of the present invention
(1) innovate tungsten-base alloy powder preparation technology, form pyrosol atomization reduction new method
With many metal salt solutions such as tungsten and copper nickel for raw material, pyrosol atomization reducing process is adopted directly to prepare High Performance W base alloy powder.The method is powder body material novel preparation method, possesses that technological process is short, production efficiency is high, the feature such as granularity morphology controllable, process cleans of product.
(2) mixed by metallic element atom level, obtain stoichiometry accurately, the alloy powder of even compact
Mixed with main tungsten solution by the metal such as copper, nickel, the Homogeneous phase mixing in atom level aspect can be realized.In preparation process, each element chemistry metering is than can accurately control, and can prepare the composite powder that multiple constituent element is evenly distributed easily.
(3) by rare earth modified, tungsten-base alloy powder performance is effectively improved
In metal salt solution proportioning process, add appropriate rare earth element, obtain High Performance W base alloy powder by pyrosol atomization reduction.The interpolation of rare earth element can promote tungsten base powder alloy, and crystal grain thinning tissue effectively improves tungsten-base alloy powder performance.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention adopts pyrosol atomization reduction technique to prepare rare earth modified tungsten-base alloy powder, with metal target salting liquid for raw material, by being atomized into aerosol in closed reactor, simultaneously aerosol occurs to decompose and fast reaction obtains target product under the high temperature conditions, it possesses the advantage that vapor phase method and liquid phase method combine, there is milling efficiency high, technique is simple, reaction process is controlled, environment amenable advantage, compare liquid phase wet-chemical milling method, the cumbersome procedure that it can avoid liquid-solid two-phase to be separated, can save in liquid phase method pulverizing process and filter, washing, dry, the steps such as pulverizing and calcining.The method breaches tungsten-base alloy powder traditional production technique bottleneck, opens efficient, clean, short route powder body material and prepares new way.
Detailed description of the invention
Reaching object to make technological means of the present invention, creation characteristic, workflow, using method and effect is easy to understand, setting forth the present invention further below.
For tungsten-copper alloy powder: with ammonium metatungstate and copper nitrate for raw material, accurately ammonium metatungstate is taken and copper nitrate is mixed with precursor solution according to the stoichiometric proportion of required tungsten-copper alloy powder, add a certain amount of rare earth element and additive, by pressure or siphon, precursor solution is transported to atomizer, precursor solution and atomization gas are in nozzle exterior or internal mix, and precursor solution atomization is fine liquid.Be injected in high temperature reaction stove after dripping; After drop enters reacting furnace, under reducing atmosphere condition, through a series of physical and chemical processes such as solvent evaporation, solute crystallization, particle drying, decomposition reaction, sinter moldings within the extremely short time, finally form required tungsten-copper alloy powder particle; Tungsten-copper alloy powder enters dust-precipitator with reaction end gas from the exhaust opening of reacting furnace and is collected; Reaction end gas enters in eluting column, the tail gas after process through blower fan and blast pipe emptying; Being arranged at the blower fan after eluting column keeps whole system to run under negative pressure.
High-temperature post-treatment is carried out to tungsten-copper alloy powder, by factors such as programming rate, temperature retention time, post-processing temperature and the furnace atmospheres in control last handling process, obtains high performance rare earth modified tungsten-copper alloy powder.
More than show and describe general principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (1)
1. the preparation method of rare earth modified tungsten-base alloy powder, is characterized in that: comprise the following steps:
(1) source liquid prepares: mixed by the salting liquid of tungsten, copper, nickel and rare earth according to the stoichiometric proportion of required tungsten-copper alloy powder, make reaction source liquid;
(2) atomization reduction: be atomized by source liquid and spray into reative cell, controls reaction atmosphere, carries out solution atomization reduction reaction, obtain elementary tungsten-base alloy powder;
(3) sample collection and post processing: collected by elementary tungsten-base alloy powder, obtains high performance rare earth modified tungsten-copper alloy powder by high-temperature process.
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| CN103143725B true CN103143725B (en) | 2015-08-12 |
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| CN104128605B (en) * | 2014-07-24 | 2016-06-08 | 华侨大学 | Rare earth modified tungstenio binder diamond saw blade and manufacture method thereof |
| CN104259465B (en) * | 2014-07-24 | 2016-08-17 | 华侨大学 | A kind of rare earth modified tungstenio binder diamond drill bit and manufacture method thereof |
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| CN102114546A (en) * | 2011-03-29 | 2011-07-06 | 兰州金川新材料科技股份有限公司 | Method for preparing spherical silver powder |
| CN102383016A (en) * | 2011-11-02 | 2012-03-21 | 中南大学 | Microwave sintering and heat treatment method for preparing high-performance tungsten-based high-density alloy |
| CN102732743A (en) * | 2012-07-11 | 2012-10-17 | 中国兵器工业第五九研究所 | W-Cu composite material with high Cu content and preparation method of W-Cu composite material |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS57143401A (en) * | 1981-02-28 | 1982-09-04 | Sumitomo Metal Ind Ltd | Treatment of metallic powder |
| CN1393310A (en) * | 2001-06-22 | 2003-01-29 | 中国科学院金属研究所 | Process for preparing nano-class composite W-Cu powder |
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