CN104525954B - Preparation method of layered toughening tungsten - Google Patents
Preparation method of layered toughening tungsten Download PDFInfo
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- CN104525954B CN104525954B CN201410778513.5A CN201410778513A CN104525954B CN 104525954 B CN104525954 B CN 104525954B CN 201410778513 A CN201410778513 A CN 201410778513A CN 104525954 B CN104525954 B CN 104525954B
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Abstract
The invention discloses layered toughening tungsten and a preparation method thereof and belongs to the field of structural materials. The layered toughening tungsten comprises a tungsten layer and a toughening layer which are mutually cascaded mutually; the toughening layer comprises a metal tantalum sheet. The preparation method for the layered toughening tungsten comprises the following steps of S1 mechanically grinding the tungsten powder under protection of inert gases; S2 alternately stacking the tungsten powder and the metal tantalum sheet to obtain a sintering body; S3 performing spark plasma sintering on the sintering body under the protection of the inert gases, wherein the sintering process is divided into three stages, heat preservation is performed at the first stage under the condition that the temperature is from 600 DEG C to 800 DEG C and the pressure is from 5KN to 10 KN; heat preservation is performed at the second stage under the condition that the temperature is from 1100 DEG C to 1300 DEG C and the pressure is from 12 KN to 20 KN; heat preservation is performed under the condition that the temperature is from 1600 DEG C to 1800 DEG C and the pressure is from 30 KN to 35 KN. Compared with pure tungsten, the layered tungsten prepared by the preparation method improves the toughness by 50%.
Description
Technical field
The invention belongs to structural material field is and in particular to toughness reinforcing tungsten of a kind of stratiform and preparation method thereof, it is especially suitable
The first wall construction in fusion reactor.
Background technology
In nuclear fusion stack, facing plasma material (Plasma Facing Materials, abbreviation PFMs) is one
Very important material, it is related to the stability of reactor plasma, is also relate to the first wall construction material and element
The problem damaged from plasma bombardment.Its major function includes:1. effectively prevent from entering the impurity of plasma；②
Effectively transmission is radiated the heat of material surface；3. prevent miscellaneous part subject plasma during improper shutdown from bombarding and damaging
Bad.Therefore, to the general requirement towards plasma material it is high temperature resistant, low sputtering, the delay of low tritium and needs and structural material
Mutually compatibility etc..
The tungsten compatibility good with nuclear fusion plasma has been confirmed, and tungsten itself also has high high temperature simultaneously
Intensity, high-melting-point, high heat conductance, height certainly sputter threshold value, with tritium, do not occur the features such as codeposition and low rate of corrosion, thus quilt
It is considered in fusion reactor a most promising class facing plasma material.But existing pure tungsten material also exists
Following performance deficiency, too high ductile-brittle transition temperature (the Ductile-Brittle Transition of main inclusion
Temperature, abbreviation DBTT), up to 400 DEG C about of its ductile-brittle transition temperature；Relatively low recrystallization temperature, its recrystallization temperature
Degree is at 1200 DEG C about；And under high-energy irradiation steep increase from sputtering raste, especially in fusion high-temperature plasma effect of irradiation
Under, tungsten occurs that radiation embrittlement, surface form nanometer weaker zone, the tritium hold-up drastically phenomenon such as soaring.Above pure tungsten material
Performance deficiency seriously limits its application in nuclear fusion stack.Application in fusion engineering for the tungsten to be realized, is on active service whole
In temperature range, tungsten all must pull against fragility and improves toughness.
Content of the invention
Disadvantages described above for prior art or Improvement requirement, the invention provides a kind of toughness reinforcing tungsten of stratiform and its preparation side
Method, being designed it is therefore intended that improving the fragility of tungsten by the alternate layer structure of soft or hard, strengthening its toughness；Present invention also offers
The preparation method of this toughness reinforcing tungsten.
For achieving the above object, according to one aspect of the present invention, there is provided a kind of toughness reinforcing tungsten of stratiform it is characterised in that
It includes base layer and the toughening layer alternateing stacking, and described matrix layer includes tungsten layer；Described toughening layer includes metal tantalum piece.
Further, the thickness of described metal tantalum piece is 30 μm.
Further, the thickness of described tungsten layer is 150～250 μm.When the thickness of tungsten layer is 150～250 μm, and metal tantalum
When the thickness of piece is 30 μm, the toughness reinforcing tungsten of stratiform has preferable combination property.
It is another aspect of this invention to provide that additionally providing a kind of method preparing the toughness reinforcing tungsten of stratiform it is characterised in that being used for
The preparation toughness reinforcing tungsten material including tungsten layer and toughening layer as above, comprises the steps：
S1：Tungsten powder is carried out under inert gas shielding mechanical lapping, then screening obtains the tungsten powder that particle diameter is less than 40 μm
End；
S2：By alternately laminated for the described tungsten powder of metal tantalum piece and the acquisition of step S1 to obtain body to be sintered；
S3：Under inert gas shielding, described body to be sintered is obtained to step S2 and carry out discharge plasma sintering, sintered
Journey is divided into three phases：First stage is incubated 3min～5min under the conditions of 600 DEG C～800 DEG C, pressure 5KN～10KN；Second
Stage is incubated 10min～15min under the conditions of 1100 DEG C～1300 DEG C, pressure 12KN～20KN；Phase III 1600 DEG C～
1800 DEG C, be incubated 5min～10min under the conditions of pressure 30KN～35KN.
Further, the described matrix powder that step S1 obtains, after ammonia or hydrogen reducing, just carries out described step
Rapid S2 and described step S3.
Further, in step S3, the programming rate of discharge plasma sintering is 80 DEG C/min～120 DEG C/min.
Further, in step S1, described mechanical lapping is realized using ball milling method, is first dry grinded, the time be 5h～
10h, is subsequently adding dehydrated alcohol and carries out wet grinding, and the time is 3h～6h.The ratio of grinding media to material of ball milling is 8:1～15:1, ball milling during ball milling
The rotating speed of tank is 250r/min～350r/min.First dry grinded, be to refine powder, add dehydrated alcohol wet grinding be for
Prevent the powder having refined from reuniting.
In the present invention, base layer namely tungsten layer.
In general, by the contemplated above technical scheme of the present invention compared with prior art, can obtain down and show
Beneficial effect：
By the tungsten layer of hard phase is sintered together with the metal tantalum piece of soft phase, obtain that there is soft phase and the superposition that firmly alternates
Composite, as soft toughening layer, during stress effect, it can occur compared with large plastometric set to absorb for the metal tantalum piece of soft phase
Compared with multi-energy, crack tip during On Crack Propagation has a certain degree of passivation moreover it is possible to make crackle deflect, and increases
The extensions path of crackle；Meanwhile, when the base layer of hard phase occurs fracture, the metal tantalum piece of soft phase may also function as bridge linking effect,
Hinder further expanding, thus reaching toughness reinforcing effect of crackle；
The inventive method adopts discharge plasma sintering, is controlled from sintering temperature, makes matrix powder that solid phase to occur
Sintering, can occur recovery and recrystallization and the densification of metal respectively, simultaneously in cold stage, middle thermophase and hot stage
Plus certain pressure, help lend some impetus to the densification of sintered body and the strong bonded at the interface of tungsten layer and metal tantalum piece；
According to the toughness reinforcing tungsten of stratiform of the inventive method preparation, compared with pure tungsten, its toughness improves 50%.Laminate of the present invention
Toughness reinforcing tungsten has important Practical significance to the first wall construction.
Brief description
Fig. 1 is the metallograph after the corrosion of the embodiment of the present invention 3 laminate toughness reinforcing tungsten section；
Fig. 2 is the embodiment of the present invention 1 laminate toughness reinforcing tungsten bending fracture apperance figure.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with drawings and Examples, right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only in order to explain the present invention, and
It is not used in the restriction present invention.As long as additionally, involved technical characteristic in each embodiment of invention described below
The conflict of not constituting each other just can be mutually combined.
Embodiment 1
The present embodiment is used for preparing the toughness reinforcing tungsten of stratiform, and it includes tungsten layer and the toughening layer alternateing stacking, the thickness of tungsten layer
Degree is about 200 μm and toughening layer thickness is 30 μm, and toughening layer is 30 μm of metal tantalum piece.Comprise the following steps that：
S1：Tungsten powder is carried out mechanical lapping under Ar gas shield, to prepare base tungsten powder.
First dry grinded during ball milling, dry grind time 8h, is subsequently adding dehydrated alcohol wet grinding, wet grinding time 5h.The ball of ball milling
Material ratio is 10:1, the rotating speed of ball grinder is 300r/min.
After ball milling terminates, the sieve screening using 400 mesh obtains the matrix powder that particle diameter is less than 40 μm, thinner using particle diameter
Powder be conducive to sintering quality.This tungsten powder, after ammonia reduction, just carries out follow-up step S2 and step S3.Reduction is also
Hydrogen can be adopted, the tungsten powder that reduction can suppress tiny is oxidized, finally ensure that the performance of the tungsten layer that sintering obtains.
S2：Step S1 is obtained described tungsten powder and metal tantalum piece is alternately laminated in graphite jig and obtains body to be sintered,
Graphite jig inner wall size is Φ 20 × 5mm, first lays one layer of matrix powder, then lays layer of metal tantalum piece, then repave
If one layer of matrix powder, in this way, repeatedly lay multilamellar, until body thickness to be sintered is close to 5mm.Metal tantalum piece passes through
Surface treatment, its surfacing and cleaning, thickness is 30 μm.The thickness of every layer of tungsten powder with the Weight control of this layer of powder, when
During thinner thickness, the quality weighing is slightly light.Because tungsten powder sintering does not lose, or loss is few, is negligible, because
This, the tungsten layer quality obtaining after tungsten powder sintering is equal to the quality of tungsten powder.
S3：Under noble gases Ar gas shielded, described body to be sintered is obtained to step S2 and carry out discharge plasma sintering, burn
Knot process is divided into three phases：First stage is incubated 4min under the conditions of 700 DEG C, pressure 5KN；Second stage is in 1200 DEG C, pressure
It is incubated 15min under the conditions of power 15KN；Phase III is incubated 8min under the conditions of 1700 DEG C, pressure 30KN.Heat up in sintering process
Speed is 100 DEG C/min.
Take out graphite jig after molding, be air cooled to room temperature, the sample the preparing demoulding is obtained the toughness reinforcing tungsten of stratiform.
Toughness reinforcing for the stratiform of the present embodiment tungsten and pure tungsten are carried out crooked test, its bending displacement is respectively 0.078mm
And 0.052mm, bending displacement can be used to characterize its toughness, and the more big then toughness of bending displacement is better, therefore the toughness reinforcing tungsten of this stratiform is purer
The toughness of tungsten improves 50%.
Embodiment 2
The present embodiment is used for preparing the toughness reinforcing tungsten of stratiform, and it includes tungsten layer and the toughening layer alternateing stacking, the thickness of tungsten layer
Spend and be 30 μm for 150 μm and toughening layer thickness.Toughening layer is 30 μm of metal tantalum piece.Comprise the following steps that：
S1：Tungsten powder is carried out mechanical lapping under Ar gas shield, to prepare tungsten powder.
First dry grinded during ball milling, dry grind time 10h, is subsequently adding dehydrated alcohol wet grinding, wet grinding time 3h.The ball of ball milling
Material ratio is 15:1, the rotating speed of ball grinder is 250r/min.
After ball milling terminates, the sieve screening using 400 mesh obtains the tungsten powder that particle diameter is less than 40 μm, thinner using particle diameter
Powder is conducive to sintering quality.This tungsten powder, after hydrogen reducing, just carries out follow-up step S2 and step S3.Reduction can press down
Make tiny tungsten powder oxidized, finally ensure that the performance of the tungsten layer that sintering obtains.
S2：Identical with step S2 in embodiment 1；
S3：Under noble gases Ar gas shielded, described body to be sintered is obtained to step S2 and carry out discharge plasma sintering, burn
Knot process is divided into three phases：First stage is incubated 3min under the conditions of 800 DEG C, pressure 4KN；Second stage is in 1300 DEG C, pressure
It is incubated 10min under the conditions of power 12KN；Phase III is incubated 5min under the conditions of 1800 DEG C, pressure 33KN.Heat up in sintering process
Speed is 80 DEG C/min.Take out graphite jig after molding, be air cooled to room temperature, the sample the preparing demoulding obtained stratiform toughness reinforcing
Tungsten.
Embodiment 3
The present embodiment is used for preparing the toughness reinforcing tungsten of stratiform, and it includes alternateing stacking tungsten layer and toughening layer, the thickness of tungsten layer
It is 30 μm for 250 μm and toughening layer thickness.Toughening layer is 30 μm of metal tantalum piece.Comprise the following steps that：
S1：Tungsten powder is carried out under Ar gas shield high-energy ball milling machinery to grind, to prepare tungsten powder.
First dry grinded during ball milling, dry grind time 5h, is subsequently adding dehydrated alcohol wet grinding, wet grinding time 6h.The ball of ball milling
Material ratio is 8:1, the rotating speed of ball grinder is 350r/min.
After ball milling terminates, the sieve screening using 400 mesh obtains the tungsten powder that particle diameter is less than 40 μm, thinner using particle diameter
Powder is conducive to sintering quality.This tungsten powder, after hydrogen reducing, just carries out follow-up step S2 and step S3.Reduction can press down
Make tiny tungsten powder oxidized, finally ensure that the performance of the tungsten layer that sintering obtains.
S2：Identical with step S2 in embodiment 1；
S3：Under noble gases Ar gas shielded, described body to be sintered is obtained to step S2 and carry out discharge plasma sintering, burn
Knot process is divided into three phases：First stage is incubated 5min under the conditions of 600 DEG C, pressure 10KN；Second stage is in 1100 DEG C, pressure
It is incubated 13min under the conditions of power 20KN；Phase III is incubated 10min under the conditions of 1600 DEG C, pressure 35KN.Heat up in sintering process
Speed is 120 DEG C/min.
Take out graphite jig after molding, be air cooled to room temperature, the sample the preparing demoulding is obtained the toughness reinforcing tungsten of stratiform.
Fig. 1 is the metallograph after the corrosion of the embodiment of the present invention 3 laminate toughness reinforcing tungsten section, and as seen from the figure, it includes white
The tungsten layer of color and the toughening layer of black, tungsten layer thickness is about 200 μm, and the thickness of toughening layer is about 30 μm.
Fig. 2 is the embodiment of the present invention 1 laminate toughness reinforcing tungsten bending fracture apperance, wherein, seems with regular polygon knot
Structure for tungsten layer, seem in irregular shape for toughening layer, tantalum piece border and tungsten layer are well combined, and crackle occurs in tantalum layer and replys
Place and mid portion.
In the present invention, it is incubated in the thickness of tungsten layer, the sintering temperature of discharge plasma sintering, sintering pressure, sintering process
Time, programming rate, ratio of grinding media to material, the rotating speed of ball grinder, Ball-milling Time etc. are not particularly limited as above enforcement in mechanical milling process
The numerical value of example, and it is not limited to the combinations of values of above example.It is true that the three phases of discharge plasma sintering process：
First stage is incubated 3min～5min under the conditions of 600 DEG C～800 DEG C, pressure 5KN～10KN；Second stage 1100 DEG C～
1300 DEG C, be incubated 10min～15min under the conditions of pressure 12KN～20KN；Phase III is in 1600 DEG C～1800 DEG C, pressure 30KN
It is incubated 5min～10min under the conditions of～35KN；And ratio of grinding media to material 8 in mechanical milling process:1～15:1st, the rotating speed 250r/ of ball grinder
Min～350r/min, dry grinding time are 5h～10h, when the wet grinding time is 3h～6h, in conjunction with other conditions, all can prepare
The toughness reinforcing tungsten of stratiform, but can there is a little difference in preparation process and effect.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not in order to
Limit the present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., all should comprise
Within protection scope of the present invention.
Claims (5)
1. a kind of method preparing the toughness reinforcing tungsten of stratiform is it is characterised in that layered toughness reinforcing tungsten includes alternateing the base of stacking
Body layer and toughening layer, described matrix layer is tungsten layer, and described toughening layer includes metal tantalum piece,
Comprise the steps：
S1：Tungsten powder is carried out under inert gas shielding mechanical lapping, then screening obtains the tungsten powder that particle diameter is less than 40 μm；
S2：By alternately laminated for the described tungsten powder of metal tantalum piece and the acquisition of step S1 to obtain body to be sintered；
S3：Under inert gas shielding, described body to be sintered is obtained to step S2 and carry out discharge plasma sintering, sintering process is divided
For three phases, and the temperature and pressure in each stage all raises successively,
In step S3, the three phases of sintering process are specially：First stage is in 600 DEG C～800 DEG C, pressure 5KN～10KN condition
Lower insulation 3min～5min；Second stage be incubated under the conditions of 1100 DEG C～1300 DEG C, pressure 12KN～20KN 10min～
15min；Phase III is incubated 5min～10min under the conditions of 1600 DEG C～1800 DEG C, pressure 30KN～35KN.
2. as claimed in claim 1 a kind of method preparing the toughness reinforcing tungsten of stratiform it is characterised in that step S1 obtain described tungsten
Powder, after ammonia or hydrogen reducing, just carries out described step S2 and described step S3.
3. as claimed in claim 1 a kind of method preparing the toughness reinforcing tungsten of stratiform it is characterised in that plasma discharging in step S3
The programming rate of sintering is 80 DEG C/min～120 DEG C/min.
4. as claimed in claim 1 a kind of method preparing the toughness reinforcing tungsten of stratiform it is characterised in that in step S1 adopt ball milling side
Formula realizes described mechanical lapping, is first dry grinded, and the time is 5h～10h, is subsequently adding dehydrated alcohol and carries out wet grinding, and the time is 3h
～6h.
5. as claimed in claim 4 a kind of method preparing the toughness reinforcing tungsten of stratiform it is characterised in that the ratio of grinding media to material of described ball milling is
8:1～15:1, during ball milling, the rotating speed of ball grinder is 250r/min～350r/min.
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| CN108146031B (en) * | 2017-12-25 | 2020-07-10 | 合肥工业大学 | Layered toughened tungsten-based composite material and preparation method thereof |
| CN108859318B (en) * | 2018-07-13 | 2020-02-07 | 合肥工业大学 | High-temperature-resistant layered toughened tungsten-based composite material and preparation method thereof |
| CN110053328B (en) * | 2019-04-26 | 2021-03-02 | 合肥工业大学 | Layered gradient structure tungsten-based composite material and preparation method thereof |
| CN110331371A (en) * | 2019-08-13 | 2019-10-15 | 合肥工业大学 | Brittle layer structure material of a kind of improvement tungsten and preparation method thereof |
| CN110434338B (en) * | 2019-08-27 | 2021-01-05 | 华中科技大学 | Laser selective melting preparation method of brittle alloy with layered size effect |
| CN112442643B (en) * | 2020-10-23 | 2021-08-27 | 合肥工业大学 | Layered fiber toughened tungsten-based composite material and preparation method thereof |
| CN113183562B (en) * | 2021-05-27 | 2022-12-09 | 合肥工业大学 | Gradient isomeric titanium-tantalum layered composite material, preparation method and application thereof |
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| CN102560257B (en) * | 2012-03-02 | 2014-01-22 | 华中科技大学 | Low-activated steel structure material for fusion reactor |
| CN102765228B (en) * | 2012-08-06 | 2015-04-29 | 重庆国际复合材料有限公司 | Platinum-tantalum laminated composite material and preparation method thereof |
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