CN104313448A - High-density bulky high-purity cementite and preparation method thereof - Google Patents
High-density bulky high-purity cementite and preparation method thereof Download PDFInfo
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- CN104313448A CN104313448A CN201410573349.4A CN201410573349A CN104313448A CN 104313448 A CN104313448 A CN 104313448A CN 201410573349 A CN201410573349 A CN 201410573349A CN 104313448 A CN104313448 A CN 104313448A
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- cementite
- purity
- powder
- preparation
- block
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- 229910001567 cementite Inorganic materials 0.000 title claims abstract description 68
- KSOKAHYVTMZFBJ-UHFFFAOYSA-N iron;methane Chemical compound C.[Fe].[Fe].[Fe] KSOKAHYVTMZFBJ-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000007731 hot pressing Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000005551 mechanical alloying Methods 0.000 claims abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 claims description 8
- 229910000859 α-Fe Inorganic materials 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 16
- 238000005275 alloying Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000011056 performance test Methods 0.000 abstract 1
- 238000004445 quantitative analysis Methods 0.000 description 13
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The invention discloses high-density bulky high-purity cementite and a preparation method thereof. The absolute density of the cementite is 7.40-7.58g/cm<3>, and the purity is greater than 92.45%. The preparation method comprises the following steps: mixing iron powder with graphite powder and mechanically alloying by way of ball milling; putting the mechanically alloyed powder in a die and carrying out hot pressing on the powder by adopting a vacuum hot pressing manner to form a bulky test sample, wherein the sintering temperature is 600-1300 DEG C and the vacuum hot pressing press is 15-85MPa; and after demoulding the bulky test sample, annealing in a vacuum annealing furnace to obtain the cementite. The cementite has the advantages that the cementite material is good in performance. By optimizing parameters of mechanical alloying and hot pressing processes and combining vacuum annealing, the high-density bulky cementite can be prepared, thereby providing an effective cementite preparation method for subsequent physical and mechanical performance tests of the cementite phase.
Description
Technical field
The present invention relates to a kind of cementite and preparation method thereof, particularly relate to block cementite of a kind of high-compactness and preparation method thereof.
Background technology
Cementite is the important composition phase in steel, and its pattern and the Physical and mechanical properties etc. of the distribution in steel to steel all can produce material impact.Adding and producing the character of cementite itself of steel interalloy element inevitably affects.Cementite is the metalwork compound with complicated orthohormbic structure, and its all temperature in iron-carbon system are metastable phase, so the preparation of simple substance cementite is particularly difficult, to such an extent as to the research of cementite nature is a difficult point always.In existing research, high-purity pure cementite that also rarely had scholar to prepare, and the report of the high-purity cementite of the bulk of densification is deficient especially.
Summary of the invention
Goal of the invention: the first object of the present invention is to provide the block high-purity cementite of a kind of high-compactness; The present invention second object is to provide the preparation method of this cementite.
Technical scheme: cementite of the present invention, its absolute density is 7.40-7.58g/cm
3, purity >92.45%.
The preparation method of the block high-purity cementite of high-compactness of the present invention, comprise the steps, wherein each material content represents with weight percent:
(1) iron powder 92.50-93.50% is mixed with Graphite Powder 99 6.50-7.50%, adopt ball milling method mechanical alloying;
(2) the above-mentioned powder after mechanical alloying is placed in mould, adopt vacuum hotpressing mode that this powder hot-pressing sintering is formed block sample, wherein, sintering temperature is 600 DEG C-1300 DEG C, and the pressure of vacuum hotpressing is 15-85MPa;
(3) by after the block sample demoulding, anneal in vacuum annealing furnace, i.e. the block high-purity cementite of obtained described high-compactness.
Wherein, in step (1), iron powder 92.50-93.40%%, Graphite Powder 99 6.50-7.40% are mixed with dispersion agent 0.1-1.0%, adopt ball milling method mechanical alloying.Dispersion agent is wherein stearic acid or methyl alcohol, is preferably stearic acid.
Meanwhile, in the process of ball milling, argon gas is adopted to make protective atmosphere, Ball-milling Time 75-200h; Powder delivery after ball milling, powder delivery environment also adopts argon shield, and uses liquid nitrogen cooling to cool.
Iron powder is preferably the α-iron powder of purity >99.50%, and Graphite Powder 99 is preferably the Graphite Powder 99 of purity >99.90%.
In step (2), the vacuum tightness of described vacuum hotpressing is 1.0-3.0 × 10
-2mPa, sintering time 0.5-5h.
In step (3), the vacuum tightness in described vacuum annealing furnace is 1.0-2.5 × 10
-2mPa, the temperature of annealing is 500-600 DEG C, the time 1.0-5.0h of annealing.
Beneficial effect: compared with prior art, its remarkable advantage is in the present invention: cementite of the present invention is the block cementite of high-compactness, its absolute density 7.40-7.58g/cm
3, cementite purity >92.45%.In preparation method of the present invention, by optimizing the parameter of mechanical alloying and heat pressing process, in conjunction with vacuum annealing technology, the block high-purity cementite of obtained high-compactness, the Physical and mechanical properties testing research for follow-up cementite phase provides a kind of effective cementite preparation method.
Accompanying drawing explanation
The outside drawing of the block high-purity cementite of Fig. 1 high-compactness of the present invention.
Embodiment
Embodiment 1: preparation process is divided into three steps:
(1) adopt two parts of 99g ball milling raw materials, wherein every part of 92.37g α-iron powder, 6.63g Graphite Powder 99, is placed in the stainless cylinder of steel of hard of two 500ML respectively; be filled with argon shield, sealing, is symmetrically placed in ball mill; after ball milling 75h, be cooled to room temperature, then powder delivery.Powder delivery process is protective atmosphere with argon gas, adopts liquid nitrogen cooling simultaneously, prevents powder to be oxidized;
(2) after ball milling, powder puts into mould, zinc stearate lubricant is smeared by mould sleeve inwall and push rod, is beneficial to the demoulding.Put into hot pressing furnace after being compressed by the mould that powder is housed, cover tightly bell, be evacuated to 3.0 × 10
-2mPa, pressurization 50MPa, sintering temperature 600 DEG C, sintering time 4h.Be cooled to room temperature with stove, the demoulding of coming out of the stove obtains block sample;
(3) the block sample of gained is carried out annealing to eliminate internal stress in vacuum annealing furnace, vacuum tightness 1.5 × 10
-2mPa, annealing temperature 500 DEG C, annealing time 5h, cools to room temperature with the furnace after annealing terminates and comes out of the stove, and namely makes the block high-purity cementite of high-compactness of the present invention, as shown in Figure 1.
Carry out test to gained cementite character and obtain following data: be 92.45% through its cementite content of XRD quantitative analysis, absolute density is 7.45g/cm
3.
Embodiment 2: operation steps is substantially the same manner as Example 1: another interpolation 0.1g stearic acid dispersant in every part of powder in step (1), this stearic acid also can substitute with methyl alcohol certainly, and effect is slightly poor; Step (2) and step (3) processing parameter and embodiment 1 completely the same.
Carry out test to gained cementite character and obtain following data: be 95.55% through its cementite content of XRD quantitative analysis, absolute density is 7.50g/cm
3.
Embodiment 3: operation steps is substantially the same manner as Example 2: step (1) processing parameter is consistent with embodiment 2; In step (2), sintering temperature is 800 DEG C, sintering time 0.5 hour, vacuum tightness 1.0 × 10
-2mPa, pressurization 15MPa; In step (3), vacuum tightness 1.0 × 10
-2mPa, annealing temperature 600 DEG C, annealing time 1.0h.
Carry out test to gained cementite character and obtain following data: be 96.45% through its cementite content of XRD quantitative analysis, absolute density is 7.40g/cm
3.
Comparative example 1: operation steps is substantially the same manner as Example 3, difference is: in step (2), pressurization 13MPa.
Carry out test to gained cementite character and obtain following data: be 96.50% through its cementite content of XRD quantitative analysis, absolute density is 6.58g/cm
3.
Embodiment 4: operation steps is substantially the same manner as Example 2: step (1) processing parameter and embodiment 2 completely the same; In step (2), sintering temperature is 1000 DEG C, sintering time 5 hours, vacuum tightness 3.0 × 10
-2mPa, pressurization 85MPa; In step (3), vacuum tightness 2.5 × 10
-2mPa, annealing temperature 500 DEG C, annealing time 5h.
Carry out test to gained cementite character and obtain following data: be 99.45% through its cementite content of XRD quantitative analysis, absolute density is 7.58g/cm
3.
Comparative example 2: operation steps is substantially the same manner as Example 4, difference is: in step (2), and sintering temperature is 500 DEG C.
Carry out test to gained cementite character and obtain following data: be 66.45% through its cementite content of XRD quantitative analysis, absolute density is 7.12g/cm
3.
Comparative example 3: operation steps is substantially the same manner as Example 4, difference is: in step (2), and sintering temperature is 1400 DEG C.
Carry out test to gained cementite character and obtain following data: be 76.45% through its cementite content of XRD quantitative analysis, absolute density is 7.57g/cm
3.
Embodiment 5: operation steps is substantially the same manner as Example 2: step (1) processing parameter and embodiment 2 completely the same; In step (2), sintering temperature is 1300 DEG C, sintering time 3 hours, vacuum tightness 2.0 × 10
-2mPa, pressurization 55MPa; In step (3), vacuum tightness 2.0 × 10
-2mPa, annealing temperature 500 DEG C, annealing time 3h.
Carry out test to gained cementite character and obtain following data: be 96.45% through its cementite content of XRD quantitative analysis, absolute density is 7.50g/cm
3.
Embodiment 6: operation steps is substantially the same manner as Example 2: in step (1), powder is by 93.40g α-iron powder, and 6.50g Graphite Powder 99 and 0.1g stearic acid form, ball milling 200h; In step (2), vacuum tightness 1.0 × 10
-2mPa, pressurization 15MPa, sintering temperature 800 DEG C, sintering time 0.5h; In step (3), vacuum tightness 1.0 × 10
-2mPa, annealing temperature 600 DEG C, annealing time 1h.
Carry out test to gained cementite character and obtain following data: be 98.53% through its cementite content of XRD quantitative analysis, absolute density is 7.40g/cm
3.
Embodiment 7: operation steps is substantially the same manner as Example 2: in step (1), powder is by 92.50g α-iron powder, and 6.50g Graphite Powder 99 and 1.0g stearic acid form, ball milling 150h; In step (2), vacuum tightness 3.0 × 10
-2mPa, pressurization 85MPa, sintering temperature 1000 DEG C, sintering time 5h; In step (3), vacuum tightness 2.5 × 10
-2mPa, annealing temperature 600 DEG C, annealing time 5h.
Carry out test to gained cementite character and obtain following data: be 96.53% through its cementite content of XRD quantitative analysis, absolute density is 7.58g/cm
3.
Embodiment 8: operation steps is substantially the same manner as Example 2: in step (1), powder is by 93.40g α-iron powder, and 6.50g Graphite Powder 99 and 0.1g stearic acid form, ball milling 200h; In step (2), vacuum tightness 2.5 × 10
-2mPa, pressurization 70MPa, sintering temperature 1100 DEG C, sintering time 3h; In step (3), vacuum tightness 2.0 × 10
-2mPa, annealing temperature 550 DEG C, annealing time 2h.
Carry out test to gained cementite character and obtain following data: be 97.23% through its cementite content of XRD quantitative analysis, absolute density is 7.55g/cm
3.
Embodiment 9: operation steps is substantially the same manner as Example 2: in step (1), powder is by 92.50g α-iron powder, and 7.40g Graphite Powder 99 and 0.1g stearic acid form, ball milling 100h; In step (2), vacuum tightness 2.5 × 10
-2mPa, pressurization 80MPa, sintering temperature 1000 DEG C, sintering time 2h; In step (3), vacuum tightness 1.0 × 10
-2mPa, annealing temperature 500 DEG C, annealing time 1h.
Carry out test to gained cementite character and obtain following data: be 98.25% through its cementite content of XRD quantitative analysis, absolute density is 7.52g/cm
3.
Embodiment 10: operation steps is substantially the same manner as Example 2: in step (1), powder is by 93.00g α-iron powder, and 6.60g Graphite Powder 99 and 0.4g stearic acid form, ball milling 120h; In step (2), vacuum tightness 1.5 × 10
-2mPa, pressurization 85MPa, sintering temperature 1050 DEG C, sintering time 4h; In step (3), vacuum tightness 1.5 × 10
-2mPa, annealing temperature 550 DEG C, annealing time 5h.
Carry out test to gained cementite character and obtain following data: be 99.65% through its cementite content of XRD quantitative analysis, absolute density is 7.58g/cm
3.
Claims (8)
1. the block high-purity cementite of high-compactness, is characterized in that: the absolute density of described cementite is 7.40-7.58g/cm
3, purity >92.45%.
2. the preparation method of the block high-purity cementite of high-compactness according to claim 1, it is characterized in that comprising the steps, wherein each material content represents with weight percent:
(1) iron powder 92.50-93.50% is mixed with Graphite Powder 99 6.50-7.50%, adopt ball milling method mechanical alloying;
(2) the above-mentioned powder after mechanical alloying is placed in mould, adopt vacuum hotpressing mode that this powder hot-pressing sintering is formed block sample, wherein, sintering temperature is 600 DEG C-1300 DEG C, and the pressure of vacuum hotpressing is 15-85MPa;
(3) by after the block sample demoulding, anneal in vacuum annealing furnace, i.e. the block high-purity cementite of obtained described high-compactness.
3. the preparation method of the block high-purity cementite of high-compactness according to claim 2, it is characterized in that: in step (1), iron powder 92.50-93.40%%, Graphite Powder 99 6.50-7.40% are mixed with dispersion agent 0.1-1.0%, adopts ball milling method mechanical alloying.
4. the preparation method of the block high-purity cementite of high-compactness according to claim 3, is characterized in that: described dispersion agent is stearic acid or methyl alcohol.
5. the preparation method of the block high-purity cementite of high-compactness according to Claims 2 or 3, is characterized in that: in step (1), adopt argon gas to make protective atmosphere in the process of described ball milling, Ball-milling Time 75-200h; Powder delivery after ball milling, powder delivery environment also adopts argon shield, and uses liquid nitrogen cooling to cool.
6. the preparation method of the block high-purity cementite of high-compactness according to Claims 2 or 3, it is characterized in that: in step (1), described iron powder is the α-iron powder of purity >99.50%, and described Graphite Powder 99 is the Graphite Powder 99 of purity >99.90%.
7. the preparation method of the block high-purity cementite of high-compactness according to Claims 2 or 3, it is characterized in that: in step (2), the vacuum tightness of described vacuum hotpressing is 1.0-3.0 × 10
-2mPa, sintering time 0.5-5h.
8. the preparation method of the block high-purity cementite of high-compactness according to Claims 2 or 3, it is characterized in that: in step (3), the vacuum tightness in described vacuum annealing furnace is 1.0-2.5 × 10
-2mPa, the temperature of annealing is 500-600 DEG C, the time 1.0-5.0h of annealing.
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Cited By (1)
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CN106282742A (en) * | 2015-05-26 | 2017-01-04 | 东南大学 | A kind of preparation method of high efficiency bulk alloy cementite |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH03193822A (en) * | 1989-12-22 | 1991-08-23 | Nippon Steel Corp | Production of non-oriented electrical sheet having high magnetic flux density and low iron loss |
JPH03193821A (en) * | 1989-12-22 | 1991-08-23 | Nippon Steel Corp | Production of non-oriented electrical sheet having high magnetic flux density and low iron loss |
CN101053806A (en) * | 2007-01-22 | 2007-10-17 | 山东大学 | Method for preparing cementite |
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2014
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH03193822A (en) * | 1989-12-22 | 1991-08-23 | Nippon Steel Corp | Production of non-oriented electrical sheet having high magnetic flux density and low iron loss |
JPH03193821A (en) * | 1989-12-22 | 1991-08-23 | Nippon Steel Corp | Production of non-oriented electrical sheet having high magnetic flux density and low iron loss |
CN101053806A (en) * | 2007-01-22 | 2007-10-17 | 山东大学 | Method for preparing cementite |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106282742A (en) * | 2015-05-26 | 2017-01-04 | 东南大学 | A kind of preparation method of high efficiency bulk alloy cementite |
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