CN106755729B - A kind of RAFM steel nano reinforcement agent and its preparation and application - Google Patents
A kind of RAFM steel nano reinforcement agent and its preparation and application Download PDFInfo
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- CN106755729B CN106755729B CN201611103925.4A CN201611103925A CN106755729B CN 106755729 B CN106755729 B CN 106755729B CN 201611103925 A CN201611103925 A CN 201611103925A CN 106755729 B CN106755729 B CN 106755729B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/0006—Adding metallic additives
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/0056—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00 using cored wires
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
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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
- C22C33/04—Making ferrous alloys by melting
- C22C33/06—Making ferrous alloys by melting using master alloys
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Abstract
A kind of RAFM steel nano reinforcement agent and its preparation and application, belong to special steel metallurgical technology field.The component and its mass percent that the RAFM steel is contained with nano reinforcement agent be：Effective particle Y2TiO5And Y2Ti2O7It is 5~13%, surplus is pure iron.Preparation method is：According to a certain concentration configuration precursor liquid (FeCl3、Y(NO3)3With Ti (SO4)2Mixed liquor)；Thereafter it is titrated using concentrated ammonia liquor, obtains precursor colloids, after carrying out centrifuge washing, dehydration dechlorination processing, nanometer presoma is made；Nano-particle is prepared using CO reduction is pre-dispersed；With addition of electrolytic iron powder, in vacuum carbon deoxidization melting in vaccum sensitive stove, ingot casting and roll forming；Using wire injection procedure, molten steel is added in hardening agent in refining process.Nanometer efficient hardening particle Y is added in nano reinforcement agent prepared by this method in RAFM smelting processes2TiO5And Y2Ti2O7Steel performance is improved, saves manufacturing cost, and be conducive to the cleaner production of RAFM steel.
Description
Technical field
The invention belongs to special steel metallurgical technology field, more particularly to a kind of RAFM steel nano reinforcement agent and its prepare and
Application method.
Background technology
Low activation ferrite/martensite steel (RAFM) is because it is with lower void swelling and coefficient of thermal expansion, higher
The excellent ermal physics such as thermal conductivity, mechanical performance, and comparatively ripe technical foundation, are generally considered the following fusion
The preferred structural material of demonstration reactor and fusion power reactor.With the development of nuclear power technology, to midium-carbon steel high temperature and Flouride-resistani acid phesphatase
More stringent requirements are proposed for energy.Due to the requirement of low activity, addible alloying element is limited, passes through the method for alloying merely
It is difficult to greatly improve its performance.Correlative study shows to make a large amount of nano reinforcement particles of Dispersed precipitate in steel using certain technological means
Preparing ODS-RAFM steel becomes an effective solution approach.
The oxide dispersion intensifying low activity martensitic steel material and preparation method that Chinese patent CN101328562A is announced,
By CLAM comminuted steel shots, Y2O3Powder and Ti powder are placed in sealing container after degasification the mechanical alloy under high-purity argon gas protection after evenly mixing
Change, hot isostatic pressing or hot pressed sintering densification molding prepare oxide dispersion intensifying low activity martensite steel ODS-CLAM steel.
The oxide dispersion intensifying type powder of stainless steel preparation method and stainless steel that Chinese patent CN102277525A is announced,
It is atomized to obtain Fe-Cr-W-Si-Zr-Ti-Y pre-alloyed powders using vacuum induction melting furnace refining master alloy and argon gas, then will
This powder and Y2O3It is placed in mechanical alloying in ball mill, followed by vacuum heating-press sintering prepares oxide dispersion intensifying type not
Become rusty steel.The patent refers to a kind of a kind of method preparing comminuted steel shot.
No matter which kind of technique to prepare comminuted steel shot using, it is required for first smelting the steel grade, is then prepared into certain particle size
Powder, it is conceivable that, it needs to consume a large amount of manpower and materials, and processing capacity is very low, it is difficult to meet the needs of industrialized production,
It is in the laboratory research stage at present.
The new approaches that second phase particles are added in steel smelting procedure have certain realistic meaning.
The additive and its preparation method of what Chinese patent CN101302572A was announced be used to prepare fine oxide dispersion steel and
That 0.25~22mm composite spheres are constituted by core and shell using, additive, shell by calcium oxide or magnesia one kind
Or two kinds of mixture, such higher melting point compound is difficult to be melted in molten steel, and have the possibility of sintering curing, even if few molten
Change, granularity 1nm~3.5mm core raw materials are also harmful in molten steel (it is generally acknowledged that the field trash less than 10 μm is nothing in steel
Evil field trash).
A kind of nano-particle that is added into molten steel that Chinese patent CN103243194A is announced to optimize the method for structure of steel,
Nano-powder is carried out mixing dispersion with straight iron powder using manually milling or mechanical ball mill, thereafter by mixture in indifferent gas
Under body atmosphere, sinters nano-powder stick into using hot-pressing technique, be added in molten steel by mechanical hydraulic unit.Chinese patent
The micron/nano metallurgical addition agent that CN101875112A is announced, by powder and micron, nano powder and metal powder through ball milling mixing, base material gold
Belong to powder as binder, briquet.Such patent can be improved using straight iron powder or base metals powder as carrier to a certain degree
The recovery rate of powder, but the mode for being all made of ball milling carries out mixing dispersion, dispersion effect is poor, and due to " powder metallurgy " at
Type technique inevitably causes to be added in molten steel and be easy to containing the impurity such as a large amount of oxygen, nitrogen, such additive in product
It causes molten steel oxygen content to increase, pollutes molten steel.
The particle that patent disclosed above simultaneously uses is the mixture of single oxide particle or several particles.
The particle that invigoration effect is played in ODS-RAFM steel is Y2TiO5Or Y2Ti2O7, currently without the preparation process of such nano-particle
Report.
Invention content
To solve the above-mentioned problems, the present invention provides a kind of RAFM steel nano reinforcement agent and its preparation and application,
This method is according to a certain concentration configuration precursor liquid (FeCl3、Y(NO3)3With Ti (SO4)2Mixed liquor)；Thereafter use concentrated ammonia liquor into
Row titration, obtains precursor colloids, and after carrying out centrifuge washing, dehydration dechlorination processing, nanometer presoma is made；Using pre- point of CO reduction
It dissipates and prepares nano-particle；With addition of electrolytic iron powder, in vacuum carbon deoxidization melting in vaccum sensitive stove, ingot casting and roll forming；Using
Molten steel is added in hardening agent by wire injection procedure in refining process.Nano reinforcement agent prepared by the present invention is in RAFM smelting processes
Add nanometer efficient hardening particle Y2TiO5And Y2Ti2O7Steel performance is improved, saves manufacturing cost, and be conducive to the clean of RAFM steel
Purification production.
A kind of RAFM steel nano reinforcement agent, the component and its mass percent contained are：Effective particle Y2TiO5With
Y2Ti2O7It is 5~13%, surplus is pure iron, wherein Y2TiO5And Y2Ti2O7Mass ratio be 306n: 386m, wherein n, m be
Natural number, and cannot be 0 simultaneously.
The RAFM steel is with nano reinforcement agentBar.
A kind of RAFM steel preparation method of nano reinforcement agent, includes the following steps：
(1) preparation of precursor colloids
By raw material FeCl3·6H2O、Y(NO3)3·6H2O and Ti (SO4)2It is dissolved in deionized water, obtains precursor liquid；Its
In, in precursor liquid, wherein in molar ratio, Ti2+∶Y3+=(2m+n): 2 (m+n), wherein m, n are natural number, and cannot be simultaneously
It is 0；Fe3+∶(Ti2++Y3+)=3~5；
Into precursor liquid, concentrated ammonia liquor is added dropwise while stirring and is settled, control ph is 7~7.5, obtains forerunner's glue
Body；Wherein, the rate of addition of concentrated ammonia liquor is 5~8mL/min, and the ingredient of precursor colloids is Fe (OH)3、Y(OH)3With Ti (OH)4；
(2) preparation of presoma
Precursor colloids are centrifuged, after washing, Muffle furnace is placed in and carries out dehydration dechlorination processing, dehydration dechlorination processing is completed
Afterwards, 90~110 DEG C are cooled to the furnace, obtains a nanometer presoma, the ingredient of nanometer presoma is (Fe2O3)x(Y2TiO5)n
(Y2Ti2O7)m, wherein x, n, m are determined according to the material molar ratio of addition；Wherein, the technological parameter for being dehydrated dechlorination is：Temperature is
780~830 DEG C, the time is 1~3h；
(3) nano-particle is pre-dispersed
Nanometer presoma is placed in reduction shaft furnace and restore pre-dispersed, reducing agent CO, reduction temperature be 1000~
1050 DEG C, the recovery time is 1~1.5h, obtains restoring pre-dispersed nano-particle；Wherein, CO flows are 15 000~20
000m3/h；
(4) vacuum fusion ingot casting
Pre-dispersed nano-particle will be restored and electrolytic iron powder carries out vacuum melting removing carbon oxygen and then poured into a mould, poured into a mould
The degree of superheat is controlled at 50~60 DEG C, obtains ingot casting；
Wherein, in mass ratio, pre-dispersed nano-particle: electrolytic iron powder=1 is restored: (2~5)；
(5) rolling is become a useful person
By ingot rolling, RAFM steel nano reinforcement agent is obtained, it is for use after curling.
In the step (1), in the precursor liquid, the molar concentration of ion is：Ti2+For 0.1~0.2mol/L,
Y3+For 0.1~0.3mol/L；
In the step (1), the mass concentration of the concentrated ammonia liquor is 25~28%, and it acts as neutralizers.
In the step (1), the stirring is one kind in electromagnetic agitation or mechanical agitation.
In the step (2), the equipment of the centrifugation uses centrifuge；
In the step (2), wash to wash precursor colloids 3~5 times with absolute ethyl alcohol.
In the step (2), the grain size of the nanometer presoma is 10~60nm.
In the step (3), the reduction is pre-dispersed, and process will ensure that iron oxide is reduced sufficiently, CO with
Y2TiO5And Y2Ti2O7It does not react, ensure that Y2TiO5And Y2Ti2O7It is not reduced.
In the step (4), the vacuum melting carries out in vaccum sensitive stove.
A kind of RAFM steel is with the application method of nano reinforcement agent：In low activity martensite/ferritic steel refining process,
Hardening agent is fed in molten steel, the feed quantity of molten steel RAFM steel nano reinforcement agent per ton is 1~1.5kg.
The feeding, the equipment used is feeding wire machine.
A kind of RAFM steel nano reinforcement agent and its preparation and application of the present invention has compared with the prior art
Beneficial effect is：
Nanometer efficient hardening particle Y is added in nano reinforcement agent prepared by the present invention in RAFM smelting processes2TiO5And
Y2Ti2O7Steel performance is improved, saves manufacturing cost, and be conducive to the cleaner production of RAFM steel.
Description of the drawings
Fig. 1 is the preparation technology figure of the RAFM steel nano reinforcement agent of the present invention；
Specific implementation mode
With reference to embodiment, the present invention is described in further detail.
In following embodiment, the preparation technology figure of RAFM steel nano reinforcement agent is shown in Fig. 1.
Embodiment 1
A kind of RAFM steel nano reinforcement agent, the component and its mass percent contained are：Effective particle Y2TiO5For
12.6%, surplus is pure iron.
A kind of RAFM steel preparation method of nano reinforcement agent, includes the following steps：
(1) preparation of precursor colloids
By raw material FeCl3·6H2O、Y(NO3)3·6H2O and Ti (SO4)2It is dissolved in deionized water, obtains precursor liquid；Its
In, in precursor liquid, wherein in molar ratio, Ti2+∶Y3+=1: 2, Fe3+∶(Ti2++Y3+)=3；The molar concentration of ion is：Ti2 +For 0.15mol/L, Y3+For 0.3mol/L, Fe3+For 1.35mol/L；
Using magnetic stirrer precursor liquid, into precursor liquid, it is 28% dense that mass concentration is added dropwise while stirring
Ammonium hydroxide is settled, and control ph 7.1 obtains precursor colloids；Wherein, the rate of addition of concentrated ammonia liquor is 6mL/min, forerunner's glue
The ingredient of body is Fe (OH)3、Y(OH)3With Ti (OH)4；
(2) preparation of presoma
Precursor colloids are placed in centrifuge and are centrifuged, and washing 5 times is carried out using absolute ethyl alcohol, after washing,
Be placed in Muffle furnace carry out dehydration dechlorination processing, dehydration dechlorination processing after the completion of, cool to 100 DEG C with the furnace, obtain grain size be 10~
The ingredient of the nanometer presoma of 50nm, nanometer presoma is (Fe2O3)0.675(Y2TiO5)0.15；Wherein, it is dehydrated the technique ginseng of dechlorination
Number is：Temperature is 780 DEG C, time 2.5h；
(3) nano-particle is pre-dispersed
Nanometer presoma is placed in reduction shaft furnace and restore pre-dispersed, reducing agent CO, reduction temperature is 1020 DEG C,
Recovery time is 1.5h, obtains restoring pre-dispersed nano-particle；Wherein, CO flows are 15 000m3/h；
(4) vacuum fusion ingot casting
In mass ratio, pre-dispersed nano-particle: electrolytic iron powder=1 is restored: 2, pre-dispersed nano-particle and electrolysis will be restored
Iron powder is placed in progress vacuum melting removing carbon oxygen in vaccum sensitive stove and is then poured into a mould, and the cast degree of superheat is controlled at 50 DEG C,
Obtain ingot casting；
(5) rolling is become a useful person
By ingot rolling, obtainRodlike RAFM steel nano reinforcement agent, it is for use after curling.
A kind of RAFM steel is with the application method of nano reinforcement agent：In low activity martensite/ferritic steel refining process,
Feeding wire machine will be used to feed hardening agent in molten steel, molten steel RAFM steel per ton is 1.2kg with the feed quantity of nano reinforcement agent.
Embodiment 2
A kind of RAFM steel nano reinforcement agent, the component and its mass percent contained are：Effective particle Y2Ti2O7For
9.1%, surplus is pure iron.
A kind of RAFM steel preparation method of nano reinforcement agent, includes the following steps：
(1) preparation of precursor colloids
By raw material FeCl3·6H2O、Y(NO3)3·6H2O and Ti (SO4)2It is dissolved in deionized water, obtains precursor liquid；Its
In, in precursor liquid, wherein in molar ratio, Ti2+∶Y3+=1: 1, Fe3+∶(Ti2++Y3+)=3；The molar concentration of ion is：Ti2 +For 0.1mol/L, Y3+For 0.1mol/L, Fe3+For 0.6mol/L；
Using magnetic stirrer precursor liquid, into precursor liquid, it is 28% dense that mass concentration is added dropwise while stirring
Ammonium hydroxide is settled, and control ph 7 obtains precursor colloids；Wherein, the rate of addition of concentrated ammonia liquor is 5mL/min, precursor colloids
Ingredient be Fe (OH)3、Y(OH)3With Ti (OH)4；
(2) preparation of presoma
Precursor colloids are placed in centrifuge and are centrifuged, and washing 3 times is carried out using absolute ethyl alcohol, after washing,
Be placed in Muffle furnace carry out dehydration dechlorination processing, dehydration dechlorination processing after the completion of, cool to 90 DEG C with the furnace, obtain grain size be 20~
The ingredient of the nanometer presoma of 60nm, nanometer presoma is (Fe2O3)0.3(Y2Ti2O7)0.05；Wherein, it is dehydrated the technique ginseng of dechlorination
Number is：Temperature is 800 DEG C, time 2h；
(3) nano-particle is pre-dispersed
Nanometer presoma is placed in reduction shaft furnace and restore pre-dispersed, reducing agent CO, reduction temperature is 1000 DEG C,
Recovery time is 1.5h, obtains restoring pre-dispersed nano-particle；Wherein, CO flows are 20 000m3/h；
(4) vacuum fusion ingot casting
In mass ratio, pre-dispersed nano-particle: electrolytic iron powder=1 is restored: 3, pre-dispersed nano-particle and electrolysis will be restored
Iron powder is placed in progress vacuum melting removing carbon oxygen in vaccum sensitive stove and is then poured into a mould, and the cast degree of superheat is controlled at 60 DEG C,
Obtain ingot casting；
(5) rolling is become a useful person
By ingot rolling, obtainRodlike RAFM steel nano reinforcement agent, it is for use after curling.
A kind of RAFM steel is with the application method of nano reinforcement agent：In low activity martensite/ferritic steel refining process,
Feeding wire machine will be used to feed hardening agent in molten steel, molten steel RAFM steel per ton is 1.5kg with the feed quantity of nano reinforcement agent.
Embodiment 3
A kind of RAFM steel nano reinforcement agent, the component and its mass percent contained are：Effective particle Y2Ti2O7For
9.1%, surplus is pure iron.
A kind of RAFM steel preparation method of nano reinforcement agent, includes the following steps：
(1) preparation of precursor colloids
By raw material FeCl3·6H2O、Y(NO3)3·6H2O and Ti (SO4)2It is dissolved in deionized water, obtains precursor liquid；Its
In, in precursor liquid, wherein in molar ratio, Ti2+∶Y3+=1: 1, Fe3+∶(Ti2++Y3+)=3；The molar concentration of ion is：Ti2 +For 0.2mol/L, Y3+For 0.2mol/L, Fe3+For 1.2mol/L；
Using magnetic stirrer precursor liquid, into precursor liquid, it is 28% dense that mass concentration is added dropwise while stirring
Ammonium hydroxide is settled, and control ph 7.5 obtains precursor colloids；Wherein, the rate of addition of concentrated ammonia liquor is 8mL/min, forerunner's glue
The ingredient of body is Fe (OH)3、Y(OH)3With Ti (OH)4；
(2) preparation of presoma
Precursor colloids are placed in centrifuge and are centrifuged, and washing 3 times is carried out using absolute ethyl alcohol, after washing,
Be placed in Muffle furnace carry out dehydration dechlorination processing, dehydration dechlorination processing after the completion of, cool to 90 DEG C with the furnace, obtain grain size be 15~
The ingredient of the nanometer presoma of 55nm, nanometer presoma is (Fe2O3)0.6(Y2Ti2O7)0.1；Wherein, it is dehydrated the technological parameter of dechlorination
For：Temperature is 830 DEG C, time 1h；
(3) nano-particle is pre-dispersed
Nanometer presoma is placed in reduction shaft furnace and restore pre-dispersed, reducing agent CO, reduction temperature is 1050 DEG C,
Recovery time is 1h, obtains restoring pre-dispersed nano-particle；Wherein, CO flows are 18 000m3/h；
(4) vacuum fusion ingot casting
In mass ratio, pre-dispersed nano-particle: electrolytic iron powder=1 is restored: 3, pre-dispersed nano-particle and electrolysis will be restored
Iron powder is placed in progress vacuum melting removing carbon oxygen in vaccum sensitive stove and is then poured into a mould, and the cast degree of superheat is controlled at 60 DEG C,
Obtain ingot casting；
(5) rolling is become a useful person
By ingot rolling, obtainRodlike RAFM steel nano reinforcement agent, it is for use after curling.
A kind of RAFM steel is with the application method of nano reinforcement agent：In low activity martensite/ferritic steel refining process,
Feeding wire machine will be used to feed hardening agent in molten steel, molten steel RAFM steel per ton is 1kg with the feed quantity of nano reinforcement agent.
Embodiment 4
A kind of RAFM steel nano reinforcement agent, the component and its mass percent contained are：Effective particle Y2TiO5For
5.3%, surplus is pure iron.
A kind of RAFM steel preparation method of nano reinforcement agent, includes the following steps：
(1) preparation of precursor colloids
By raw material FeCl3·6H2O、Y(NO3)3·6H2O and Ti (SO4)2It is dissolved in deionized water, obtains precursor liquid；Its
In, in precursor liquid, wherein in molar ratio, Ti2+∶Y3+=1: 2, Fe3+∶(Ti2++Y3+)=5；The molar concentration of ion is：Ti2 +For 0.1mol/L, Y3+For 0.2mol/L, Fe3+For 1.5mol/L；
Precursor liquid is stirred using mechanical stick, into precursor liquid, it is 25% concentrated ammonia liquor that mass concentration is added dropwise while stirring
It is settled, control ph 7.5 obtains precursor colloids；Wherein, the rate of addition of concentrated ammonia liquor is 5mL/min, precursor colloids
Ingredient is Fe (OH)3、Y(OH)3With Ti (OH)4；
(2) preparation of presoma
Precursor colloids are placed in centrifuge and are centrifuged, and washing 3 times is carried out using absolute ethyl alcohol, after washing,
Be placed in Muffle furnace carry out dehydration dechlorination processing, dehydration dechlorination processing after the completion of, cool to 110 DEG C with the furnace, obtain grain size be 15~
The ingredient of the nanometer presoma of 55nm, nanometer presoma is (Fe2O3)0.75(Y2TiO5)0.1；Wherein, it is dehydrated the technological parameter of dechlorination
For：Temperature is 780 DEG C, time 3h；
(3) nano-particle is pre-dispersed
Nanometer presoma is placed in reduction shaft furnace and restore pre-dispersed, reducing agent CO, reduction temperature is 1050 DEG C,
Recovery time is 1h, obtains restoring pre-dispersed nano-particle；Wherein, CO flows are 18 000m3/h；
(4) vacuum fusion ingot casting
In mass ratio, pre-dispersed nano-particle: electrolytic iron powder=1 is restored: 4, pre-dispersed nano-particle and electrolysis will be restored
Iron powder is placed in progress vacuum melting removing carbon oxygen in vaccum sensitive stove and is then poured into a mould, and the cast degree of superheat is controlled at 55 DEG C,
Obtain ingot casting；
(5) rolling is become a useful person
By ingot rolling, obtainRodlike RAFM steel nano reinforcement agent, it is for use after curling.
A kind of RAFM steel is with the application method of nano reinforcement agent：In low activity martensite/ferritic steel refining process,
Feeding wire machine will be used to feed hardening agent in molten steel, molten steel RAFM steel per ton is 1.4kg with the feed quantity of nano reinforcement agent.
Embodiment 5
A kind of RAFM steel nano reinforcement agent, the component and its mass percent contained are：Effective particle Y2TiO5With
Y2Ti2O7It is 6.2%, surplus is pure iron, wherein in mass ratio：Y2TiO5∶Y2Ti2O7=306: 193.
A kind of RAFM steel preparation method of nano reinforcement agent, includes the following steps：
(1) preparation of precursor colloids
By raw material FeCl3·6H2O、Y(NO3)3·6H2O and Ti (SO4)2It is dissolved in deionized water, obtains precursor liquid；Its
In, in precursor liquid, wherein in molar ratio, Ti2+∶Y3+=2: 3, Fe3+∶(Ti2++Y3+)=4；The molar concentration of ion is：Ti2 +For 0.2mol/L, Y3+For 0.3mol/L, Fe3+For 2.0mol/L；
Precursor liquid is stirred using mechanical stick, into precursor liquid, it is 25% concentrated ammonia liquor that mass concentration is added dropwise while stirring
It is settled, control ph 7.5 obtains precursor colloids；Wherein, the rate of addition of concentrated ammonia liquor is 8mL/min, precursor colloids
Ingredient is Fe (OH)3、Y(OH)3With Ti (OH)4；
(2) preparation of presoma
Precursor colloids are placed in centrifuge and are centrifuged, and washing 4 times is carried out using absolute ethyl alcohol, after washing,
Be placed in Muffle furnace carry out dehydration dechlorination processing, dehydration dechlorination processing after the completion of, cool to 110 DEG C with the furnace, obtain grain size be 10~
The ingredient of the nanometer presoma of 45nm, nanometer presoma is (Fe2O3)(Y2TiO5)0.1(Y2Ti2O7)0.05；Wherein, it is dehydrated dechlorination
Technological parameter is：Temperature is 800 DEG C, time 3h；
(3) nano-particle is pre-dispersed
Nanometer presoma is placed in reduction shaft furnace and restore pre-dispersed, reducing agent CO, reduction temperature is 1030 DEG C,
Recovery time is 1.2h, obtains restoring pre-dispersed nano-particle；Wherein, CO flows are 17 000m3/h；
(4) vacuum fusion ingot casting
In mass ratio, pre-dispersed nano-particle: electrolytic iron powder=1 is restored: 4, pre-dispersed nano-particle and electrolysis will be restored
Iron powder is placed in progress vacuum melting removing carbon oxygen in vaccum sensitive stove and is then poured into a mould, and the cast degree of superheat is controlled at 55 DEG C,
Obtain ingot casting；
(5) rolling is become a useful person
By ingot rolling, obtainRodlike RAFM steel nano reinforcement agent, it is for use after curling.
A kind of RAFM steel is with the application method of nano reinforcement agent：In low activity martensite/ferritic steel refining process,
Feeding wire machine will be used to feed hardening agent in molten steel, molten steel RAFM steel per ton is 1.4kg with the feed quantity of nano reinforcement agent.
Claims (6)
1. a kind of preparation method of RAFM steel nano reinforcement agent, which is characterized in that include the following steps：
(1) preparation of precursor colloids
By raw material FeCl3·6H2O、Y(NO3)3·6H2O and Ti (SO4)2It is dissolved in deionized water, obtains precursor liquid；Wherein, preceding
It drives in liquid, wherein in molar ratio, Ti2+：Y3+= (2m+n) ：2 (m+n), wherein m, n are natural number, and cannot be 0 simultaneously；
Fe3+：(Ti2++Y3+)=3~5；
Into precursor liquid, concentrated ammonia liquor is added dropwise while stirring and is settled, control ph is 7 ~ 7.5, obtains precursor colloids；Its
In, the rate of addition of concentrated ammonia liquor is 5 ~ 8mL/min, and the ingredient of precursor colloids is Fe (OH)3、Y(OH)3With Ti (OH)4；
(2) preparation of presoma
Precursor colloids are centrifuged, after washing, Muffle furnace is placed in and carries out dehydration dechlorination processing, after the completion of dehydration dechlorination processing,
It cools to 90 ~ 110 DEG C with the furnace, obtains a nanometer presoma, the ingredient of nanometer presoma is (Fe2O3)x(Y2TiO5)n(Y2Ti2O7)m,
Wherein, x, n, m are determined according to the material molar ratio of addition；Wherein, the technological parameter for being dehydrated dechlorination is：Temperature is 780 ~ 830 DEG C,
Time is 1 ~ 3h；
(3) nano-particle is pre-dispersed
Nanometer presoma is placed in reduction shaft furnace and restore pre-dispersed, reducing agent CO, reduction temperature is 1000 ~ 1050
DEG C, the recovery time is 1 ~ 1.5h, obtains restoring pre-dispersed nano-particle；Wherein, CO flows are 15 000 ~ 20 000m3/h；
(4) vacuum fusion ingot casting
Pre-dispersed nano-particle will be restored and electrolytic iron powder carries out vacuum melting removing carbon oxygen and then poured into a mould, cast overheat
Degree control obtains ingot casting at 50 ~ 60 DEG C；
Wherein, in mass ratio, pre-dispersed nano-particle is restored：Electrolytic iron powder=1:(2~5)；
(5) rolling is become a useful person
By ingot rolling, RAFM steel nano reinforcement agent is obtained, it is for use after curling；
The component and its mass percent that the RAFM steel is contained with nano reinforcement agent be：Effective particle Y2TiO5And Y2Ti2O7
It is 5 ~ 13%, surplus is pure iron, wherein Y2TiO5And Y2Ti2O7Mass ratio be 306n:386m, wherein n, m are natural number, and
Cannot be 0 simultaneously.
2. the preparation method of RAFM steel nano reinforcement agent as described in claim 1, which is characterized in that the step (1)
In, in the precursor liquid, the molar concentration of ion is：Ti2+For 0.1 ~ 0.2 mol/L, Y3+For 0.1 ~ 0.3 mol/L；Institute
In the step of stating (1), the mass concentration of the concentrated ammonia liquor is 25 ~ 28%.
3. the preparation method of RAFM steel nano reinforcement agent as described in claim 1, which is characterized in that the step (1)
In, the stirring is one kind in electromagnetic agitation or mechanical agitation.
4. the preparation method of RAFM steel nano reinforcement agent as described in claim 1, which is characterized in that the step (2)
In, the equipment of the centrifugation uses centrifuge；In the step (2), wash to wash forerunner's glue with absolute ethyl alcohol
Body 3 ~ 5 times.
5. the preparation method of RAFM steel nano reinforcement agent as described in claim 1, which is characterized in that the step (2)
In, the grain size of the nanometer presoma is 10 ~ 60nm.
6. the preparation method of RAFM steel nano reinforcement agent as described in claim 1, which is characterized in that the step (4)
In, the vacuum melting carries out in vaccum sensitive stove.
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