CN106381439B - A kind of method that nano oxide dispersion reinforcing martensite heat-resistant steel is prepared using explosive sintering - Google Patents
A kind of method that nano oxide dispersion reinforcing martensite heat-resistant steel is prepared using explosive sintering Download PDFInfo
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- CN106381439B CN106381439B CN201610802469.6A CN201610802469A CN106381439B CN 106381439 B CN106381439 B CN 106381439B CN 201610802469 A CN201610802469 A CN 201610802469A CN 106381439 B CN106381439 B CN 106381439B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/08—Compacting only by explosive forces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The method that nano oxide dispersion strengthens martensite heat-resistant steel is prepared using explosive sintering the present invention relates to a kind of, oxide powder and martensite steel powder ball milling mixing uniformly and are realized into solid solution of the oxide in martensite steel powdered base.Then the powder densification after ball milling is loaded in molding cavity, and welded seal is carried out to molding cavity, ball powder-grinding need to be carried out under high purity inert gas protection, and powder-tight need to be placed under vacuum environment when molding cavity；Afterwards, the compacting between molding cavity inner powder end is realized by using high speed impact ripple caused by explosive charge, the complete fusion of powder is finally realized using high temperature solid-phase sintering, and make oxide with nanometer phase disperse educt.The present invention can realize that large scale high-compactness nano oxide dispersion strengthens the preparation of martensite heat-resistant steel sheet material, bar and tubing.
Description
Technical field
The present invention relates to a kind of method that nano oxide dispersion reinforcing martensite heat-resistant steel is prepared using explosive sintering.
Background technology
Martensite heat-resistant steel has high antioxygenic property and high temperature resistance steam corrosion performance, but also is rushed with good
Hit toughness and high and stable rupture ductility and thermostrength.The martensite heat-resistant steel of wherein 8-15Cr series, such as making for P91 steel
With ceiling temperature within 600 DEG C, it is widely used in the high-temperature and pressure pipeline in all kinds of power stations.The low activation horse of 8-10Cr series
Family name's body steel has good anti-neutron irradiation swelling performance, and such as Chinese low activation martensitic steel has been chosen as the head of Chinese fusion reactor
Structural material is selected, and may be applied to other advanced reactors.Martensite heat-resistant steel is that common thermal power station and nuclear power make extensively
Pipeline and thermal structure steel.As society is for environmentally friendly and energy-efficient pursuit, people are for power station thermoelectrical efficiency
Requirement more and more higher, it is proposed that overcritical or even ultra supercritical concept, in order to further improve making for martensite heat-resistant steel
, can be by the SC service ceiling temperature of martensite heat-resistant steel by present 550~600 by way of nano-oxide enhancing with temperature
DEG C improve to 650~700 DEG C, so as to effectively lifted power station thermoelectrical efficiency.
At present, oxide dispersion intensifying martensite heat-resistant steel is mainly sintered by high temperature insostatic pressing (HIP) or by mechanical cold
Solid-phase sintering is carried out after pressure.Hot Isostatic Pressing Diffusion due to by equipment size limited and powder in rub caused by pressure
Drop, is difficult to the preparation of macro nanometer oxide dispersion intensifying martensite heat-resistant steel section bar at present.And be cold-pressed consistency by
To having a great influence for powder air content, thus after being cold-pressed solid-phase sintering material porosity it is very high, consistency only reaches about
98%.This plasticity to material, especially impact property cause strong influence, and its impact absorbing energy is only that vacuum environment is protected
The impact absorbing energy 1/10th or so of the lower prepared material of shield, and cold moudling is equally limited by equipment size size.
The present invention propose it is a kind of by explode and sinter the method being combined with realize high-compactness macro nanometer oxide strengthen
The preparation of martensite heat-resistant steel.
The content of the invention
The technology of the present invention solves problem：One kind is provided nano oxide dispersion reinforcing martensite is prepared using explosive sintering
The method of heat resisting steel, by high pressure shock wave caused by explosive charge, the instant shock between powder and fusion are realized, without mould
With other formers.On the one hand overcome Hot Isostatic Pressing Diffusion to be limited by equipment size, on the other hand overcome
Compactness is low and the shortcomings that the parts-moulding size that equally exists is by equipment limit between cold moudling powder.
The present invention provides a kind of method that nano oxide dispersion reinforcing martensite heat-resistant steel is prepared using explosive sintering, will
This technique is used for the preparation of the P91 steel or low activation martensitic steel of nano-oxide enhancing, by reducing the air content of powder,
Solid solution of the oxide in martensite heat-resistant steel powdered base is realized by ball milling simultaneously, and powder is realized by way of blast
Compacting and it is preliminary combine, the cmpletely diffusion between powder is then realized by high temperature solid-phase sintering, and make oxide to receive
The form disperse educt of rice phase, is finally reached good elevated temperature strength.
Technical scheme is as follows：
A kind of method that nano oxide dispersion reinforcing martensite heat-resistant steel is prepared using explosive sintering, by the oxygen of enhancing
Compound powder is well mixed by mechanical alloying with martensite heat-resistant steel powder and realizes oxide in martensite steel powder base
Solid solution in body；Then the powder densification after ball milling is loaded in molding cavity, and vacuum sealing is carried out to molding cavity；Again
The compacting of powder in cavity is realized by high speed impact ripple caused by explosive charge, obtains the material of densification；Finally utilize high temperature
Solid-phase sintering realizes the further fusion between powder, and makes oxide in martensite heat-resistant steel in the form of the phase of nanoscale second
Disperse educt.
The oxide powder is yittrium oxide, aluminum oxide or thorium oxide；The particle diameter of the oxide powder is 30~80nm,
So that oxide enters martensite heat-resistant steel by mechanical alloying as early as possible.
The martensite heat-resistant steel is the martensite heat-resistant steel that amount containing Cr is 8-15%；The particle diameter of martensite heat-resistant steel is 30
~80 μm, in order to avoid meticulous powder is reunited, and excessive powder is difficult to and the uniform mechanical alloy of oxide powder
Change.
The mass fraction of the oxide powder is 0.1~0.5%, and the mass fraction of martensite heat-resistant steel powder is 99.5
~99.9%, to obtain optimal oxide machinery alloying effect.
The ball milling mixing ratio of grinding media to material, the i.e. mass ratio of abrading-ball and powder are 10:1~15:1, Ball-milling Time is 36~48
Hour, rotational speed of ball-mill is in 200~300rpm, in vacuum higher than 10Pa (or high purity inert gas (purity is more than 99.99%) protections
Mechanical alloying is realized by ball milling down, the powder diameter after ball milling is 50% powder diameter for D50 particle diameters, has reached good
The powder diameter uniformity.
When the molding cavity carries out vacuum sealing, the powder after ball milling is loaded in molding cavity under vacuum,
Sealed simultaneously using electron beam or laser, then by lighting detonator, ignite the gunpowder around molding cavity, produce with quick-fried
The shock wave that fried speed is propagated, pressure reach more than 5GPa, make the powder of filling under Shock Wave sharp impacts, extrude and rub
Wipe, finally can obtain the material that consistency is up to more than 99.5%.
During the high temperature solid-phase sintering, high temperature sintering temperature is 1000~1200 DEG C, solid-phase sintering 2~4 hours, to realize
Abundant diffusion between powder, and make oxide again with nanometer phase disperse educt.
The present invention compared with prior art the advantages of be：
(1) present invention can not be limited by HIP sintering by equipment size, realize that nano-oxide strengthens martensite
The preparation of heat resisting steel large scale section bar, it, which prepares rank, can reach more than hundred feather weight even tonne.
(2) present invention requires the air content of control powder by condition of high vacuum degree, and realizes that big pressure is made by explosive manner
With the compacting between lower powder, and the complete diffusion bond of powder is realized under high temperature solid-phase sintering, it is fine and close to obtain high material
Degree.
Brief description of the drawings
Fig. 1 is that nano-oxide strengthens the flow chart that martensite heat-resistant steel prepares scheme.
Embodiment
Below in conjunction with the accompanying drawings and the present invention is discussed in detail in specific embodiment.But following embodiment is only limitted to explain this hair
Bright, protection scope of the present invention should include the full content of claim, be not limited only to the present embodiment.
A kind of method that nano oxide dispersion reinforcing martensite heat-resistant steel is prepared using explosive sintering, oxide powder are
Yittrium oxide, aluminum oxide or thorium oxide, by oxide and martensite of the D50 particle diameters after ball milling (50% powder diameter) at 30~80 μm
Powdered steel mixing and ball milling is uniform, and the mass fraction of oxide powder is 0.1~0.5%, in mechanical milling process, ratio of grinding media to material 10:1
~15:1, Ball-milling Time is 36~48 hours, and rotating speed realizes the uniform mixing of powder, while reached grain in 200-300rpm
Footpath is distributed optimal with flour extraction.
Because the consistency of nano-oxide enhancing martensite heat-resistant steel is influenceed very big, ball milling system by the air content of powder
Powder needs to carry out under the conditions of high purity inert gas or vacuum protection.Powder after ball milling mixing is filled in under vacuum
In cavity, and realize by electron beam or laser the sealing of forming cavity, environment vacuum degree<10Pa.
Explosive around molding cavity is evenly distributed on by cap sensitive, powder is realized under high speed shock wave caused by blast
The compacting at end.Pressure of the Shock Wave caused by blast on powder can reach more than 5GPa, the powder in the presence of the pressure
Sharp impacts between end, compress and rub against, closely knit and preliminary combination fusion is realized rapidly, then by the powder after explosive compaction in height
Solid-phase sintering is carried out in warm stove, sintering temperature is 1000~1200 DEG C, and sintering time is 2~4 hours, to realize filling between powder
Point diffusion, and make oxide again with 10~50nm the second phase in martensite heat-resistant steel matrix disperse educt.
The present invention is suitable to prepare sheet material, bar that large scale high-compactness nano oxide dispersion strengthens martensite heat-resistant steel
And tubing, it is possible to achieve more than hundred feather weight even prepared by the section bar of tonne scale, and its consistency is up to more than 99.5%.
Nano-oxide enhancing martensite heat-resistant steel prepared by the present invention needs large-size components to carry out consistency detection, micro-
See fabric analysis and Mechanics Performance Testing, especially impact property.
Embodiment 1：
1 flow with reference to the accompanying drawings, the 9Cr1.5WVTa martensite heat-resistant steel powder of particle diameter~62 μm is prepared first, then will
Particle diameter autumn Mo after~48nm yttrium oxide powder mixes with martensite comminuted steel shot is uniform, and realizes oxide in martensite steel
Solid solution.The ratio of grinding media to material of ball milling is 15:1, the rotating speed of ball milling is in 220rpm, and the time of ball milling is in about 36h.Carried out 4 times before ball milling
Vacuumize and be filled with Ar to be cleaned, finally in purity>The ball milling of powder is carried out under 99.99% Ar gas shieldeds, powder goes out powder
Rate reaches 80%.
Prepared powder is loaded into a diameter of 60mm, length is in 1200mm bar-shaped cavity, then utilizes electron beam
Carry out the Vacuum Package of cavity.Whole powder processed is carried out to dress powder process in glove box, vacuum in glove box<5Pa.
Then explosive is symmetrically arranged in the bar-shaped cavity surrounding for loading powder, the detonator that top is placed in by lighting draws
Bursting charge, column shock wave from top to bottom is produced, oppress bar-shaped molding cavity and produce radial contraction, oppress powder densification, finally
Material after explosive forming is placed in high temperature furnace and carries out solid-phase sintering, sintering temperature is about in 1100 ± 5 DEG C, sintering time
3 hours.
Finally, the detection of material density, its consistency are carried out after being sampled on the bar of preparation by densimetry
Reach 99.6%, and the pick-up behavior of its nano-oxide is analyzed and characterized by electron microscope, nano-oxide
Particle diameter is no more than 15nm, in Dispersed precipitate.
Embodiment 2：
1 flow with reference to the accompanying drawings, the 9Cr1.5WVTa martensite heat-resistant steel powder of particle diameter~63 μm is prepared first, then will
Particle diameter autumn Mo after~56nm yttrium oxide powder mixes with martensite comminuted steel shot is uniform, and realizes oxide in martensite steel
Solid solution.The ratio of grinding media to material of ball milling is 13:1, the rotating speed of ball milling is in 280rpm, and the time of ball milling is in about 45h.Carried out 4 times before ball milling
Vacuumize and be filled with Ar to be cleaned, finally in purity>The ball milling of powder is carried out under 99.99% Ar gas shieldeds, powder goes out powder
Rate reaches 85%.
It is 1500mm that prepared powder is loaded into length, and wide 1000mm, thickness is Ran Houli in 30mm tabular cavity
The Vacuum Package of cavity is carried out with electron beam.Whole powder processed is carried out under vacuum to dress powder process, vacuum<10Pa.
Then explosive is evenly arranged above the tabular cavity for loading powder, the cap sensitive that side is placed in by lighting is fried
Medicine, produces shock wave, and compressing tabular molding cavity produces contraction, oppresses powder densification, finally places the material after explosive forming
Solid-phase sintering is carried out in high temperature furnace, for sintering temperature at 1080 ± 5 DEG C, sintering time is about 3 hours.
Finally, the detection of material density, its consistency are carried out after being sampled on the sheet material of preparation by densimetry
Reach 99.5%, and the pick-up behavior of its nano-oxide is analyzed and characterized by electron microscope, nano-oxide
Particle diameter is no more than 15nm, in Dispersed precipitate.
Embodiment 3：
1 flow with reference to the accompanying drawings, the 9Cr1.5WVTa martensite heat-resistant steel powder of particle diameter~50 μm is prepared first, then will
Particle diameter autumn Mo after~62nm yttrium oxide powder mixes with martensite comminuted steel shot is uniform, and realizes oxide in martensite steel
Solid solution.The ratio of grinding media to material of ball milling is 15:1, the rotating speed of ball milling is in 250rpm, and the time of ball milling is in about 42h.Carried out 4 times before ball milling
Vacuumize and be filled with Ar to be cleaned, finally in purity>The ball milling of powder is carried out under 99.99% Ar gas shieldeds, powder goes out powder
Rate reaches 90%.
It is 1800mm that prepared powder is loaded into length, and wide 1000mm, thickness is Ran Houli in 10mm tabular cavity
The Vacuum Package of cavity is carried out with electron beam.Whole powder processed is carried out to dress powder process in glove box, vacuum in glove box<
1Pa。
Then explosive is evenly arranged above the tabular cavity for loading powder, the cap sensitive that side is placed in by lighting is fried
Medicine, produces shock wave, and compressing tabular molding cavity produces contraction, oppresses powder densification, finally places the material after explosive forming
Solid-phase sintering is carried out in high temperature furnace, for sintering temperature at 1150 ± 5 DEG C, sintering time is about 3 hours.
Finally, the detection of material density, its consistency are carried out after being sampled on the sheet material of preparation by densimetry
Reach 99.8%, and the pick-up behavior of its nano-oxide is analyzed and characterized by electron microscope, nano-oxide
Particle diameter is no more than 15nm, in Dispersed precipitate.
Embodiment 4：
1 flow with reference to the accompanying drawings, the 9Cr1.5WVTa martensite heat-resistant steel powder of particle diameter~50 μm is prepared first, then will
Particle diameter autumn Mo after~62nm yttrium oxide powder mixes with martensite comminuted steel shot is uniform, and realizes oxide in martensite steel
Solid solution.The ratio of grinding media to material of ball milling is 10:1, the rotating speed of ball milling is in 300rpm, and the time of ball milling is in about 38h.Carried out 4 times before ball milling
Vacuumize and be filled with Ar to be cleaned, finally in purity>The ball milling of powder is carried out under 99.99% Ar gas shieldeds, powder goes out powder
Rate reaches 85%.
Prepared powder is loaded into a diameter of 80mm, length is in 1800mm bar-shaped cavity, then utilizes electron beam
Carry out the Vacuum Package of cavity.Whole powder processed is carried out to dress powder process in glove box, vacuum in glove box<5Pa.
Then explosive is evenly arranged in the bar-shaped cavity surrounding for loading powder, the cap sensitive that side is placed in by lighting is fried
Medicine, shock wave is produced, oppress bar-shaped molding cavity and produce contraction, oppress powder densification, finally place the material after explosive forming
Solid-phase sintering is carried out in high temperature furnace, for sintering temperature at 1060 ± 5 DEG C, sintering time is about 3 hours.
Finally, the detection of material density, its consistency are carried out after being sampled on the bar of preparation by densimetry
Reach 99.5%, and the pick-up behavior of its nano-oxide is analyzed and characterized by electron microscope, nano-oxide
Particle diameter is no more than 10nm, in Dispersed precipitate.
Embodiment 5：
1 flow with reference to the accompanying drawings, the 9Cr1.5WVTa martensite heat-resistant steel powder of particle diameter~75 μm is prepared first, then will
Particle diameter autumn Mo after~38nm yttrium oxide powder mixes with martensite comminuted steel shot is uniform, and realizes oxide in martensite steel
Solid solution.The ratio of grinding media to material of ball milling is 15:1, the rotating speed of ball milling is in 300rpm, and the time of ball milling is in about 48h.Carried out 4 times before ball milling
Vacuumize and be filled with Ar to be cleaned, finally in purity>The ball milling of powder is carried out under 99.99% Ar gas shieldeds, powder goes out powder
Rate reaches 88%.
Prepared powder is loaded into a diameter of 50mm, length is in 2000mm bar-shaped cavity, then utilizes electron beam
Carry out the Vacuum Package of cavity.Whole powder processed is carried out to dress powder process in glove box, vacuum in glove box<5Pa.
Then explosive is evenly arranged in the bar-shaped cavity surrounding for loading powder, the cap sensitive that side is placed in by lighting is fried
Medicine, shock wave is produced, oppress bar-shaped molding cavity and produce contraction, oppress powder densification, finally place the material after explosive forming
Solid-phase sintering is carried out in high temperature furnace, for sintering temperature at 1180 ± 5 DEG C, sintering time is about 3 hours.
Finally, the detection of material density, its consistency are carried out after being sampled on the bar of preparation by densimetry
Reach 99.8%, and the pick-up behavior of its nano-oxide is analyzed and characterized by electron microscope, nano-oxide
Particle diameter is no more than 20nm, in Dispersed precipitate.
In a word, by the various embodiments described above as can be seen that the nano-oxide enhancing martensite prepared by the present invention is heat-resisting
Steel has the features such as consistency is high, and part dimension is big, is advantageous to promote the scale application of nano-oxide enhancing heat resisting steel.
It is further to note that according to the various embodiments described above of the present invention, those skilled in the art are can to realize completely
The four corner of the claims in the present invention 1 and appurtenance, implementation process and the same the various embodiments described above of method；And the present invention is not
Elaborate and partly belong to techniques well known.
It is described above, part embodiment only of the present invention, but protection scope of the present invention is not limited thereto, and is appointed
What those skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in should all be covered
Within protection scope of the present invention.
Claims (5)
- A kind of 1. method that nano oxide dispersion reinforcing martensite heat-resistant steel is prepared using explosive sintering, it is characterised in that：Will The oxide powder of enhancing is well mixed by mechanical alloying with martensite heat-resistant steel powder and realizes oxide in geneva Solid solution in body powdered steel matrix；Then the powder densification after ball milling is loaded in molding cavity, and molding cavity is carried out Vacuum sealing；The compacting of powder in cavity is realized by high speed impact ripple caused by explosive charge again, obtains the material of densification；Most The further fusion between powder is realized using high temperature solid-phase sintering afterwards, and makes oxide in martensite heat-resistant steel with nanoscale The form disperse educt of two-phase；When the molding cavity carries out vacuum sealing, the powder after ball milling is loaded in molding cavity under vacuum, simultaneously Sealed using electron beam or laser, then by lighting detonator, ignite the gunpowder around molding cavity, produce with speed of exploding Spend the shock wave propagated, pressure reaches more than 5GPa, make the powder of filling under Shock Wave sharp impacts, compress and rub against, most The material that consistency is up to more than 99.5% is obtained afterwards；During the high temperature solid-phase sintering, high temperature sintering temperature is 1000~1200 DEG C, solid-phase sintering 2~4 hours, to realize powder Between abundant diffusion, and make oxide again with nanometer phase disperse educt.
- A kind of nano oxide dispersion is prepared using explosive sintering strengthen martensite heat-resistant steel 2. according to claim 1 Method, it is characterised in that：The oxide powder is yittrium oxide, aluminum oxide or thorium oxide；The particle diameter of the oxide powder is 30~80nm.
- A kind of nano oxide dispersion is prepared using explosive sintering strengthen martensite heat-resistant steel 3. according to claim 1 Method, it is characterised in that：The martensite heat-resistant steel is the martensite heat-resistant steel that amount containing Cr is 8-15%；Martensite heat-resistant steel Particle diameter is 30~80 μm.
- A kind of nano oxide dispersion is prepared using explosive sintering strengthen martensite heat-resistant steel 4. according to claim 1 Method, it is characterised in that：The mass fraction of the oxide powder is 0.1~0.5%, the quality point of martensite heat-resistant steel powder Number is 99.5~99.9%.
- A kind of nano oxide dispersion is prepared using explosive sintering strengthen martensite heat-resistant steel 5. according to claim 1 Method, it is characterised in that：The ball milling mixing ratio of grinding media to material, the i.e. mass ratio of abrading-ball and powder are 10:1~15:1, Ball-milling Time For 36~48 hours, rotational speed of ball-mill passed through ball milling in 200~300rpm in the case where vacuum is higher than 10Pa or high purity inert gas protection Realize mechanical alloying, the powder diameter after ball milling is 50% powder diameter for D50 particle diameters.
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