CN106756480A - A kind of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material and preparation method thereof - Google Patents
A kind of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material and preparation method thereof Download PDFInfo
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- CN106756480A CN106756480A CN201611123439.9A CN201611123439A CN106756480A CN 106756480 A CN106756480 A CN 106756480A CN 201611123439 A CN201611123439 A CN 201611123439A CN 106756480 A CN106756480 A CN 106756480A
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- thermal shock
- intermetallic compound
- corrosion
- ball milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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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
Abstract
The invention provides a kind of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material and preparation method thereof.The preparation method is comprised the following steps：Iron powder and silica flour are mixed carries out ball milling；Powder obtained by ball milling is made annealing treatment, the temperature of the annealing is 850 950 DEG C, and the time is 34 hours；To mix with alumino-silicate adhesive by the powder of annealing, by compacting, drying, sintering, obtain the corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material.Present invention also offers corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material prepared by the above method.The material has anti-Zn solution erosion performance and resistance to heat shocks energy higher.
Description
Technical field
The present invention relates to a kind of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material and preparation method thereof, belong to material system
Standby technical field.
Background technology
Intermetallic compound refer to by two or more metal constituent elements constitute in proportion with constituting unit different from it
Element long-range order crystal structure and metal fundamental characteristics compound, with elevated temperature strength it is high, fusing point is high, density is low, than strong
Degree many unique process based prediction models such as high, anti-oxidant and anticorrosive, be widely used in space flight and aviation, turbine, industry plus
In needing the equipment of strong corrosion resistant in hot equipment and generator and chemical industry.
Current Fe-Si intermetallic compound has been obtained for necessarily as internal heater protection sleeve pipe in galvanizing by dipping field
Application, but mechanical alloying prepares intermetallic compound and need to expend ample resources, in addition iron powder and silica flour even across it is long when
Between ball milling, can not completely obtain Fe-Si intermetallic compound.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide a kind of Fe-Si intermetallic compound and its preparation side
Method, is combined with annealing process by mechanical alloying and prepares Fe-Si intermetallic compound, and it has anti-Zn solution higher
Erosion performance and resistance to heat shocks energy.
To reach above-mentioned purpose, the invention provides a kind of preparation of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material
Method, it is comprised the following steps：
Iron powder and silica flour are mixed carries out ball milling；
Powder obtained by ball milling is made annealing treatment, the temperature of the annealing is 850-950 DEG C, and the time is 3-
4 hours；
To mix with alumino-silicate adhesive by the powder of annealing, by compacting, drying, sintering, obtain described
Corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material.
Using in ma process, the die break of ball-milled powder deforms when institute to preparation method provided by the present invention
Nonequilibrium state with big energy, and the high temperature holding process in vacuum annealing, make the simple substance in ball-milled powder and unit
Element diffusion be mutually changed into Fe-Si intermetallic compound, so as to shorter Ball-milling Time, suitable annealing time and at a temperature of obtain
Complete Fe-Si intermetallic compound.
In above-mentioned preparation method, it is preferable that the atomic ratio of iron powder and silica flour is 3:More than 1.
In above-mentioned preparation method, it is preferable that the purity of the iron powder for being used is 98.5%, granularity is 200 mesh.
In above-mentioned preparation method, it is preferable that the purity of the silica flour for being used is 99.9%, granularity is 200 mesh.
In above-mentioned preparation method, ball milling is carried out using stainless steel jar mill, and ball milling is preferably carried out under an argon atmosphere, tool
Gymnastics is made as follows：After powder is placed in stainless steel jar mill, vacuumizes and be then charged with argon gas, be then placed on ball grinder
Ball milling on ball mill.The ratio of grinding media to material of ball milling is preferably controlled to 30:More than 1；The abrading-ball of ball milling preferably from it is a diameter of it is small (3,
5mm), (10,15mm) in the, steel ball of big (20,30mm), the heavyweight of abrading-ball is with by big：In：Small=3:5:4；What ball milling was used
Drum's speed of rotation is preferably controlled to 250-300r/ minutes, and the time of ball milling is preferably controlled to more than 30 hours.
In above-mentioned preparation method, annealing can be carried out using electric tube furnace, and concrete operations are as follows：By the Fe- after ball milling
Si mixed-powders are put into silica dish, and then silica dish is placed in electric tube furnace, are preferably pressed into high-purity argon gas and are protected, and are prevented
Oxidation, is then to slowly warm up to 850-950 DEG C, is kept for 3-4 hours, is then taken out after after its cooling.
In above-mentioned preparation method, it is preferable that the addition of the alumino-silicate adhesive for being used accounts for iron powder, silica flour and silicon
The 30%-35% of aluminate adhesive three's gross mass.
In above-mentioned preparation method, the concrete operations of compacting can be：By by the powder and alumino-silicate of annealing
Adhesive mixes, and is reconciled in alms bowl is ground uniformly, and then the powder for having reconciled is added the mould for having smeared lubrication butter
In, it is compressing on forcing press, it is preferable that the pressure of compacting is 10-12T.
In above-mentioned preparation method, drying can be carried out using forced air oven, and concrete operations are as follows：By the examination after compacting
After sample dries in the shade 72 hours, it is put into forced air oven and is dried, it is fully dried, excludes all of crystallization water and surface
Lubricating oil, it is preferable that the temperature of drying be 180-220 DEG C, the time be 160-220 minutes.
In above-mentioned preparation method, sintering can carry out pressureless sintering using vacuum hotpressing stove, it is preferable that the temperature of sintering
It it is 1100-1200 DEG C, the time is 60-90 minutes.
Present invention also offers a kind of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material, it is by above-mentioned preparation side
Prepared by method.
During preparation method provided by the present invention, Fe, Si elemental powders are formed through prolonged mechanical alloying
Nonequilibrium supersaturated solid solution Fe (Si), and powder grain is refine to nanoscale.Simultaneously in ma process
Introduce highdensity crystal defect, such as room, dislocation, fault, grain boundary, sub boundary in subsequent annealing process,
The energy barrier that solute subrogates diffusion is reduced, the also diffusion for solute element in the base provides passage faster, compared to more single
Pure mechanical alloying prepares Fe-Si intermetallic compound and saves ample resources.
The main performance index of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material of the invention is as follows：
The anti-Zn solution erosion rate of material is less than 0.5mm/a, from 600 DEG C to room temperature, thermal shock 60 times, without apparent crackle.
Corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material prepared by method provided by the present invention has higher resistance to
Zinc liquid erosion performance and resistance to heat shocks energy.
Specific embodiment
In order to be more clearly understood to technical characteristic of the invention, purpose and beneficial effect, now to skill of the invention
Art scheme carry out it is described further below, but it is not intended that to it is of the invention can practical range restriction.
Embodiment
A kind of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material is present embodiments provided, it is through the following steps that system
Standby：
Step 1, weighing：
By Fe:Si atomic ratios are 3:1 weighs powder, wherein, the purity of iron powder is 98.5%, and granularity is 200 mesh；Silica flour
Purity is 99.9%, and granularity is 200 mesh.
Step 2, abrading-ball level are matched somebody with somebody：
Ball mill ratio of grinding media to material uses 30:1, abrading-ball selects the steel ball of a diameter of 5mm, 15mm, 20mm, the heavyweight of abrading-ball to match somebody with somebody
By big：In：Small=3:5:4.
Step 3, ball milling：
The mixed powder that will be weighed is placed in stainless steel jar mill, and argon gas is filled with after vacuumizing, then by ball milling
Tank is placed on ball milling on ball mill, and it is 300r/ minutes to set drum's speed of rotation, and Ball-milling Time is 1800 minutes.
Step 4, annealing：
Take the Fe-Si mixed-powder samples after ball milling and be put into silica dish, silica dish is placed in electric tube furnace, be passed through high-purity
Then Ar gas shieldeds, anti-oxidation is to slowly warm up to 950 DEG C, is heat-treated 3 hours, after taking-up after its natural cooling.
Step 5, shaping：
Addition accounts for the alumino-silicate adhesive of material gross weight 30%-35% in powder after ball milling, is adjusted in alms bowl is ground
With it is uniform, by the powder for having reconciled add smeared lubrication butter mould in, compressing on forcing press, pressure is
10~12T.
Step 6, drying：
By the sample after compacting after drying in the shade 72 hours, it is put into forced air oven and is dried 180 minutes at 200 DEG C, makes it
Fully dry, exclude the lubricating oil on all of crystallization water and surface.
Step 7, sintering：
Sample is placed on carries out pressureless sintering in vacuum hotpressing stove, sintering temperature is 1200 DEG C, and the time is 90 minutes, is obtained
Corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material.
Anti-thermal shock experiment is heated using resistance furnace to sample, and thermal shock temperature is chosen for 900 DEG C, and in this temperature
30 minutes；Then sample is taken out from resistance furnace, places natural cooling in atmosphere, about cool down 15 minutes specimen surface temperature
Degree is down to room temperature；Testing bar is put into resistance furnace is again heated, and so on；Respectively sample complete 5 times, 10 times, 15
It is secondary, 20 times, 25 times, 30 times, take out sample after 35 times and 60 thermal shocks circulation, whether observation specimen surface has crackle to produce and clap
According to record.
The main performance index of the corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material that the present embodiment is provided is as follows：
The anti-Zn solution erosion rate of material is less than 0.5mm/a, from 600 DEG C to room temperature, thermal shock 60 times, without apparent crackle.
Claims (10)
1. a kind of preparation method of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material, it is comprised the following steps：
Iron powder and silica flour are mixed carries out ball milling；
Powder obtained by ball milling is made annealing treatment, the temperature of the annealing is 850-950 DEG C, and the time is that 3-4 is small
When；
To mix with alumino-silicate adhesive by the powder of annealing, by compacting, drying, sintering, obtain the corrosion resistant
Erosion anti-thermal shock Fe-Si intermetallic compound material.
2. preparation method according to claim 1, wherein, the atomic ratio of the iron powder and silica flour is 3:More than 1.
3. preparation method according to claim 1 and 2, wherein, the purity of the iron powder is 98.5%, and granularity is 200 mesh；
The purity of the silica flour is 99.9%, and granularity is 200 mesh.
4. the preparation method according to claim any one of 1-3, wherein, the ball milling is carried out under an argon atmosphere；
Preferably, the ratio of grinding media to material of the ball milling is 30:More than 1；
Preferably, the abrading-ball of the ball milling from it is small, in, big steel ball, the heavyweight of abrading-ball is with by big：In：Small=3:5:4；
Preferably, a diameter of 3mm or 5mm of small steel ball, in steel ball a diameter of 10mm or 15mm, the diameter of big steel ball
It is 20mm or 30mm；
Preferably, the drum's speed of rotation that the ball milling is used is 250-300r/ minutes, and the time of ball milling is more than 30 hours.
5. the preparation method according to claim any one of 1-4, wherein, the annealing is carried out under high-purity argon gas protection.
6. the preparation method according to claim any one of 1-5, wherein, the addition of the alumino-silicate adhesive accounts for iron
The 30%-35% of powder, silica flour and alumino-silicate adhesive three's gross mass.
7. the preparation method according to claim any one of 1-6, wherein, the pressure of the compacting is 10-12T.
8. the preparation method according to claim any one of 1-7, wherein, the temperature of the drying is 180-220 DEG C, time
It is 160-220 minutes.
9. the preparation method according to claim any one of 1-8, wherein, the temperature of the sintering is 1100-1200 DEG C, when
Between be 60-90 minutes.
10. a kind of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material, it is by the system described in claim any one of 1-9
Prepared by Preparation Method；Preferably, the anti-Zn solution erosion rate of the corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material is less than
0.5mm/a, from 600 DEG C to room temperature, thermal shock 60 times, without apparent crackle.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611123439.9A CN106756480A (en) | 2016-12-08 | 2016-12-08 | A kind of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material and preparation method thereof |
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| CN201611123439.9A CN106756480A (en) | 2016-12-08 | 2016-12-08 | A kind of corrosion-resistant anti-thermal shock Fe-Si intermetallic compound material and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1554580A (en) * | 2003-12-22 | 2004-12-15 | 华中科技大学 | Method and its device for preparing beta-FeSi2 thermoelectric material by laser cintering |
| CN102659110A (en) * | 2012-04-19 | 2012-09-12 | 厦门大学 | Method for directionally solidifying and purifying polycrystalline silicon by adopting ferro-silicon alloy |
-
2016
- 2016-12-08 CN CN201611123439.9A patent/CN106756480A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1554580A (en) * | 2003-12-22 | 2004-12-15 | 华中科技大学 | Method and its device for preparing beta-FeSi2 thermoelectric material by laser cintering |
| CN102659110A (en) * | 2012-04-19 | 2012-09-12 | 厦门大学 | Method for directionally solidifying and purifying polycrystalline silicon by adopting ferro-silicon alloy |
Non-Patent Citations (5)
| Title |
|---|
| 曾贵玉等: "《微纳米含能材料》", 31 May 2015, 北京：国防工业出版社 * |
| 李宁等: "机械合金化-退火法制备铁硅金属间化合物", 《热加工工艺》 * |
| 罗康来等: "《特种粘接技术及应用实例》", 31 March 2003, 北京：化学工业出版社 * |
| 贾建刚等: "机械活化-热压Fe3Si有序金属间化合物的制备", 《兰州理工大学学报》 * |
| 陈站等: "机械合金化-热压烧结制备金属间化合物Fe3Si", 《材料科学与工程学报》 * |
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