CN101724762B - Method for preparing nickel-tungsten-yttrium (III) oxide master alloy with uniform tissue for casting - Google Patents
Method for preparing nickel-tungsten-yttrium (III) oxide master alloy with uniform tissue for casting Download PDFInfo
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- CN101724762B CN101724762B CN2008102282238A CN200810228223A CN101724762B CN 101724762 B CN101724762 B CN 101724762B CN 2008102282238 A CN2008102282238 A CN 2008102282238A CN 200810228223 A CN200810228223 A CN 200810228223A CN 101724762 B CN101724762 B CN 101724762B
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Abstract
A method for preparing a nickel-tungsten-yttrium (III) oxide master alloy with uniform tissue for casting is characterized by firstly preparing soluble nickel salt, tungsten salt and yttrium salt into solution (chemical reaction does not happen between the salt solution); preparing the solution into precursor powder; roasting and decomposing the precursor powder into composite oxide powder; finally reducing the composite oxide powder into composite nickel-tungsten-yttrium (III) oxide powder; and forming the composite powder, sintering under the reducing atmosphere and taking out after cooling, thus preparing the nickel-tungsten-yttrium (III) oxide master alloy. The method is characterized by simpler technological process, low cost and good technical effect and has great economic and social value.
Description
Technical field
The present invention relates to the high temperature alloy technology of preparing, a kind of casting homogeneous microstructure (close grain) nickel-tungsten-yttrium oxide master alloy preparation method is provided especially.
Background technology
Superalloy is present dual-use aircraft engine and the irreplaceable key structure material of gas turbine high temperature component, parts such as turbine blade, turning vane, the turbine disk and combustion chamber particularly, it is the basis of a state aviation space industry, the superalloy proportion is up to 60% in advanced person's aircraft engine, and the level of superalloy has reflected the defense force and the industrial level of a country to a certain extent.
Traditional strengthening mechanism of superalloy mainly contains solution strengthening, precipitation strength, grain-boundary strengthening and production technique reinforcement etc.In in reinforcing process, oxide dispersion intensifying is a class and the diverse superalloy of conventional high-temperature alloy, the main production method of this class alloy is to adopt the preparation of mechanical alloying method, by the mechanical alloying method inert oxide compound particle is joined in the powdered alloy, prepare superalloy by the agglomerating mode at last.The creep rupture strength of at present up-to-date oxide-dispersed alloy above thinking classic nickel-base cast superalloy now, can be produced in batches in the U.S., Britain, France, Germany and Japan and other countries.Therefore, this class alloy have an extraordinary development prospect, but also have certain weak point, single etc. as complex technical process, production cost height, apparatus expensive, product.
Comparatively speaking, cast superalloy has the superalloy foundry goods that technology is simple, cost is low, equipment is simple relatively, can produce various complicated shapes.; adopting forging type production dispersed oxide superalloy also to have many difficulties; particularly aspect the oxide compound master alloy, also have many problems to be difficult to solve in casting; casting alloy generally has heredity; homogeneous microstructure nickel-tungsten-yttrium oxide master alloy is the ideal master alloy, and how to prepare is the problem of being badly in need of solution.
Summary of the invention
The purpose of this invention is to provide the preparation method of a kind of casting with homogeneous microstructure (close grain) nickel-tungsten-yttrium oxide master alloy;
The invention provides a kind of preparation method who casts with homogeneous microstructure nickel-tungsten-yttrium oxide master alloy, it is characterized in that:
The first step: the uniform nickel-tungsten of prepared composition-yttrium oxide composite powder is specially:
Nickel salt, tungsten salt, the yttrium salt of solubility are made solution;
Then above-mentioned solution is made precursor powder;
With above-mentioned precursor powder calcination is the oxide composite end;
Again the oxide composite end is reduced into nickel-tungsten-yttrium oxide composite powder;
Second step: nickel-tungsten-yttrium oxide composite powder is carried out moulding, carry out sintering then under protective atmosphere, last cool to room temperature obtains homogeneous microstructure nickel-tungsten-yttrium oxide master alloy.
Among the preparation method of homogeneous microstructure nickel-tungsten of the present invention-yttrium oxide master alloy, employed nickel salt is specially one of nitrate, hydrochloride, this three class of vitriol of solubility or its combination, and yttrium salt is nitrate, and tungsten salt is metatungstic acid ammonia.(any chemical reaction should not take place in the nickel salt of solubility, tungsten salt, yttrium salt in the aqueous solution.)
Comprise following content among the preparation method of homogeneous microstructure nickel-tungsten of the present invention-yttrium oxide master alloy:
The precursor powder calcination that will be made by nickel salt, tungsten salt, the yttrium salts solution of solubility is that the calcination process at oxide composite end specifically is divided into two step calcinations: the first step is slow low temperature calcination, and the calcination temperature is 200 ℃～600 ℃, 2～4 hours calcination time; Second step was the high temperature calcination, 650 ℃～780 ℃ of calcination temperature, 1～2 hour calcination time.
The precursor powder calcination that will be made by nickel salt, tungsten salt, the yttrium salts solution of solubility is that the calcination process at oxide composite end is carried out under air atmosphere, to guarantee thoroughly finishing of oxidizing reaction.
The specific requirement that described all kinds of oxide composites end is reduced to nickel-tungsten-yttrium oxide composite powder is: carry out under reducing atmosphere; The two step reduction modes that the concrete employing of described reduction process is carried out successively: the first step, reduction temperature are 600 ℃～630 ℃, soaking time 1～3 hour; In second step, reduction temperature is 700 ℃～750 ℃, soaking time 1～3 hour.
It is also should satisfy following specific requirement that described all kinds of oxide composites end is reduced to nickel-tungsten-yttrium oxide composite powder: reducing gas is high-purity hydrogen or the mixed gas that decomposes ammonia or high-purity hydrogen and nitrogen; The flow control of reducing gas is at 5～50ml/min.cm
2
It is also should satisfy following specific requirement that described all kinds of oxide composites end is reduced to nickel-tungsten-yttrium oxide composite powder: the reduction of oxide powder can be adopted high-purity hydrogen; Perhaps adopt the mixed gas of high-purity hydrogen and high-purity nitrogen, wherein, the ratio of hydrogen and nitrogen is between 1:1～1:5.
When described all kinds of oxide composites end is reduced to nickel-tungsten-yttrium oxide composite powder, specifically adopt continous way atmosphere protection tube furnace or intermittent type atmosphere protection tube furnace.
Among the present invention, the preparation method of described homogeneous microstructure nickel-tungsten-yttrium oxide master alloy also comprises following content: nickel-tungsten-yttrium oxide composite powder is carried out moulding, under reducing atmosphere, carry out isothermal sintering then, take out behind the cool to room temperature, make uniform nickel tungsten base yttrium oxide master alloy.
Among the present invention, the preparation method of described homogeneous microstructure nickel-tungsten-yttrium oxide master alloy should satisfy following requirement:
1) will carry out molding mode through the nickel-tungsten-yttrium oxide composite powder that obtains after the reduction reaction is: mold pressing or cold isostatic compaction;
2) biscuit carries out the requirement of isothermal sintering and is under reducing atmosphere: 1480 ℃～1600 ℃ isothermal sinterings;
3) soaking time is 1～3 hour;
4) after heat preservation sintering finished, with stove insulation cool to room temperature, taking-up got final product;
5) alloy sintering adopts continous way atmosphere protection tube furnace, also can adopt intermittent type atmosphere protection tube furnace;
6) the sintering and reducing protective atmosphere is specially high-purity hydrogen, or the mixed gas of high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is between 1:1～1:5;
7) traffic requirement of reducing gas is controlled at 5～50ml/min.cm
2
The present invention can be used for the preparation of oxide dispersion intensifying nickel-base alloy, specifically can adopt castmethod: at first with required other raw material fusing of nickel-base alloy, in liquid alloy, add the relatively large nickel-tungsten-yttrium oxide master alloy of mean density then, thereby make the nickel-base alloy of oxide dispersion intensifying.
The preparation-obtained homogeneous microstructure nickel-tungsten of the present invention-yttrium oxide master alloy has uniform close grain, and crystal grain is tiny, and technique effect is much better than prior art.The present invention has foreseeable huge economic and social value.
Description of drawings
The present invention is further detailed explanation below in conjunction with drawings and the embodiments:
Fig. 1 is 10%Y
2O
3The master alloy microtexture;
Fig. 2 is 5%Y
2O
3The master alloy microtexture.
Embodiment
Embodiment 1
Nickel salt, tungsten salt, the yttrium salt of solubility are made solution, and any chemical reaction should not take place in the aqueous solution of the nickel salt of solubility, tungsten salt, yttrium salt each other, is specially nickelous nitrate, Yttrium trinitrate and metatungstic acid ammonia, and composition proportion is Ni:W:Y
2O
3=9:81:10 (mass ratio) makes the precursor powder of nickel tungsten yttrium salt with above-mentioned solution with high temperature atomization drying method, and atomization drying adopts the centrifugal atomizing dried forms, is nickel tungsten yttrium oxide composite powder with above-mentioned nickel tungsten yttrium salt precursor body powder calcination then; The calcination process is divided into two step calcinations: the first step is slow low temperature calcination, and the calcination temperature is 350 ℃, 3 hours calcination time, second step was the high temperature calcination, 750 ℃ of calcination temperature, 2 hours calcination time, the precursor powder calcination carries out under air atmosphere, guarantees thoroughly finishing of oxidizing reaction; Above-mentioned nickel tungsten yttrium oxide composite powder is reduced to nickel tungsten yttrium oxide composite powder under hydrogen atmosphere; Described reduction process can be adopted as the reduction of two steps, and the first step reduction temperature is 630 ℃, soaking time 3 hours, and the second step reduction temperature is 750 ℃, soaking time 3 hours, reducing gas is a high-purity hydrogen; The flow of reducing gas can be controlled in 20ml/min.cm
2The reduction-oxidation composite powder adopts continous way atmosphere protection tube furnace.
The technological process for preparing Ni-based yttrium oxide master alloy is as follows: the composite powder that at first the atomization drying method is added the reduction method preparation carries out moulding with the compression molding mode, under reducing atmosphere, carry out isothermal sintering, sintering temperature is 1500 ℃, and soaking time is 1 hour; The sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen and high-purity nitrogen, and the ratio of hydrogen and nitrogen is 1:2, and the flow of reducing gas is 20ml/min.cm
2Alloy sintering adopts continous way atmosphere protection tube furnace, after heat preservation sintering finishes, with stove insulation cool to room temperature, prepares uniform Ni-based yttrium oxide master alloy at last, and the alloy microtexture is seen Fig. 1.
Embodiment 2
Nickel salt, tungsten salt, the yttrium salt of solubility are made solution, be specially nickelous nitrate, Yttrium trinitrate and metatungstic acid ammonia, composition proportion is Ni:W:Y
2O
3=9.5:85.5:5 (mass ratio), above-mentioned solution is made the precursor powder of nickel tungsten yttrium salt with high temperature atomization drying method, atomization drying adopts the centrifugal atomizing dried forms, is nickel tungsten yttrium oxide composite powder with above-mentioned nickel tungsten yttrium salt precursor body powder calcination then; The calcination process is divided into two step calcinations: the first step is slow low temperature calcination, and the calcination temperature is 450 ℃, 3 hours calcination time, second step was the high temperature calcination, 750 ℃ of calcination temperature, 2 hours calcination time, the precursor powder calcination carries out under air atmosphere, guarantees thoroughly finishing of oxidizing reaction; Above-mentioned nickel tungsten yttrium oxide composite powder is reduced to nickel tungsten yttrium oxide composite powder under hydrogen atmosphere; Described reduction process can be adopted as the reduction of two steps, and the first step reduction temperature is 630 ℃, soaking time 2 hours, and the second step reduction temperature is 750 ℃, soaking time 2 hours, reducing gas is a high-purity hydrogen; The flow of reducing gas can be controlled in 15ml/min.cm
2The reduction-oxidation composite powder adopts continous way atmosphere protection tube furnace.
The technological process for preparing Ni-based yttrium oxide master alloy is as follows: the composite powder that at first the atomization drying method is added the reduction method preparation carries out moulding with the compression molding mode, under reducing atmosphere, carry out isothermal sintering, sintering temperature is 1550 ℃, and soaking time is 1 hour; The sintering and reducing protective atmosphere adopts high-purity hydrogen, and flow is 15ml/min.cm
2, alloy sintering adopts continous way atmosphere protection tube furnace; After heat preservation sintering finishes, with stove insulation cool to room temperature, obtain nickel tungsten base yttrium oxide master alloy at last, the alloy microtexture is seen Fig. 2.
Embodiment 3
Nickel salt, tungsten salt, the yttrium salt of solubility are made solution, and any chemical reaction should not take place in the aqueous solution of the nickel salt of solubility, tungsten salt, yttrium salt each other.Be specially nickelous nitrate, Yttrium trinitrate and metatungstic acid ammonia, composition proportion is Ni:W:Y
2O
3=9.2:82.8:8 (mass ratio) makes the precursor powder of nickel tungsten yttrium salt with above-mentioned solution with the centrifugal atomizing drying means, is nickel tungsten yttrium oxide composite powder with above-mentioned nickel tungsten yttrium salt precursor body powder calcination then; The calcination process is divided into two step calcinations: the first step is slow low temperature calcination, and the calcination temperature is 400 ℃, 3 hours calcination time, second step was the high temperature calcination, 750 ℃ of calcination temperature, 2 hours calcination time, the precursor powder calcination carries out under air atmosphere, guarantees thoroughly finishing of oxidizing reaction; Above-mentioned nickel tungsten yttrium oxide composite powder is reduced to nickel tungsten yttrium oxide composite powder under hydrogen atmosphere; Described reduction process can be adopted as the reduction of two steps, and the first step reduction temperature is 630 ℃, soaking time 2 hours, and the second step reduction temperature is 750 ℃, soaking time 2 hours, reducing gas is a high-purity hydrogen; The flow of reducing gas can be controlled in 30ml/min.cm
2The reduction-oxidation composite powder adopts continous way atmosphere protection tube furnace.
The technological process for preparing Ni-based yttrium oxide master alloy is as follows: the composite powder that at first the atomization drying method is added the reduction method preparation carries out moulding with the compression molding mode, under reducing atmosphere, carry out isothermal sintering, sintering temperature is 1520 ℃, and soaking time is 1 hour; The sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen and high-purity nitrogen, and the ratio of hydrogen and nitrogen is 1:1, and the flow of reducing gas is 15ml/min.cm
2Alloy sintering adopts continous way atmosphere protection tube furnace, after heat preservation sintering finishes, with stove insulation cool to room temperature, prepares uniform nickel tungsten base yttrium oxide master alloy at last.
Claims (6)
1. cast preparation method, it is characterized in that with homogeneous microstructure nickel-tungsten-yttrium oxide master alloy:
The preparation method of described homogeneous microstructure nickel-tungsten-yttrium oxide master alloy:
The first step: the uniform nickel-tungsten of prepared composition-yttrium oxide composite powder is specially:
Nickel salt, tungsten salt, the yttrium salt of solubility are made solution; Employed nickel salt is specially one of nitrate, hydrochloride, vitriol three classes of solubility or its combination, and yttrium salt is nitrate, and tungsten salt is metatungstic acid ammonia; Any chemical reaction should not take place in the nickel salt of solubility, tungsten salt, yttrium salt in the aqueous solution;
Then above-mentioned solution is made precursor powder;
With above-mentioned precursor powder calcination is the oxide composite end;
Again the oxide composite end is reduced into nickel-tungsten-yttrium oxide composite powder;
Second step: nickel-tungsten-yttrium oxide composite powder is carried out moulding, carry out sintering then under protective atmosphere, last cool to room temperature obtains homogeneous microstructure nickel-tungsten-yttrium oxide master alloy;
The precursor powder calcination that will be made by nickel salt, tungsten salt, the yttrium salts solution of solubility is that the calcination process at oxide composite end specifically is divided into two step calcinations: the first step is slow low temperature calcination, and the calcination temperature is 200 ℃～600 ℃, 2～4 hours calcination time; Second step was the high temperature calcination, 650 ℃～780 ℃ of calcination temperature, 1～2 hour calcination time;
The specific requirement that described all kinds of oxide composites end is reduced to nickel-tungsten-yttrium oxide composite powder is: carry out under reducing atmosphere; The two step reduction modes that the concrete employing of described reduction process is carried out successively: the first step, reduction temperature are 600 ℃～630 ℃, soaking time 1～3 hour; In second step, reduction temperature is 700 ℃～750 ℃, soaking time 1～3 hour;
Described method also satisfies following requirement:
1) will be through the nickel-tungsten-yttrium oxide composite powder molding mode that obtains after the reduction reaction: mold pressing or isostatic cool pressing;
2) requirement of carrying out isothermal sintering then under reducing atmosphere is: 1480 ℃～1600 ℃ isothermal sinterings;
3) soaking time is 1～3 hour;
4) after heat preservation sintering finished, with stove insulation cool to room temperature, taking-up got final product;
5) alloy sintering adopts continous way atmosphere protection tube furnace, also can adopt intermittent type atmosphere protection tube furnace;
6) the sintering and reducing protective atmosphere is specially the mixed gas of high-purity hydrogen or decomposition ammonia or high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is between 1: 1～1: 5;
7) traffic requirement of reducing gas is controlled at 5～50ml/min.cm
2
2. according to the preparation method of the described homogeneous microstructure nickel-tungsten of claim 1-yttrium oxide master alloy, it is characterized in that: the precursor powder calcination that will be made by nickel salt, tungsten salt, the yttrium salts solution of solubility is that the calcination process at oxide composite end is carried out under air atmosphere, to guarantee thoroughly finishing of oxidizing reaction.
3. according to the preparation method of the described homogeneous microstructure nickel-tungsten of claim 2-yttrium oxide master alloy, it is characterized in that: it is also should satisfy following specific requirement that described all kinds of oxide composites end is reduced to nickel-tungsten-yttrium oxide composite powder:
Reducing gas is high-purity hydrogen or the mixed gas that decomposes ammonia or high-purity hydrogen and high-purity nitrogen;
The flow control of reducing gas is at 5～50ml/min.cm
2
4. according to the preparation method of the described homogeneous microstructure nickel-tungsten of claim 3-yttrium oxide master alloy, it is characterized in that: it is also should satisfy following specific requirement that described all kinds of oxide composites end is reduced to nickel-tungsten-yttrium oxide composite powder:
The reduction of oxide powder is adopted high-purity hydrogen or is decomposed ammonia or the mixed gas of employing high-purity hydrogen and high-purity nitrogen, and wherein, the ratio of hydrogen and nitrogen is between 1: 1～1: 5.
5. according to the preparation method of the described homogeneous microstructure nickel-tungsten of claim 4-yttrium oxide master alloy; it is characterized in that: when described all kinds of oxide composites end is reduced to nickel-tungsten-yttrium oxide composite powder, specifically adopt continous way atmosphere protection tube furnace or intermittent type atmosphere protection tube furnace.
6. according to the preparation method of one of them described homogeneous microstructure nickel-tungsten-yttrium oxide master alloy of claim 1～3, it is characterized in that:
Described method also comprises following content: at first will carry out moulding through the nickel-tungsten-yttrium oxide composite powder that obtains after the reduction reaction, under reducing atmosphere, carry out isothermal sintering then, behind the cool to room temperature, make uniform nickel tungsten base yttrium oxide master alloy.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044829A (en) * | 1989-02-08 | 1990-08-22 | 英科合金国际有限公司 | Composition with the nickel of mechanical alloyage, cobalt, chromium, iron substance |
| CN1348016A (en) * | 2001-10-19 | 2002-05-08 | 钢铁研究总院 | High-performance high-temperature nickel-base alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044829A (en) * | 1989-02-08 | 1990-08-22 | 英科合金国际有限公司 | Composition with the nickel of mechanical alloyage, cobalt, chromium, iron substance |
| CN1348016A (en) * | 2001-10-19 | 2002-05-08 | 钢铁研究总院 | High-performance high-temperature nickel-base alloy |
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