CN103420373A - Preparation method for high temperature corrosion resistant Cr23C6 cermet - Google Patents
Preparation method for high temperature corrosion resistant Cr23C6 cermet Download PDFInfo
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- CN103420373A CN103420373A CN2013103325142A CN201310332514A CN103420373A CN 103420373 A CN103420373 A CN 103420373A CN 2013103325142 A CN2013103325142 A CN 2013103325142A CN 201310332514 A CN201310332514 A CN 201310332514A CN 103420373 A CN103420373 A CN 103420373A
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- powder
- sintering
- cr23c6
- oven
- vacuum
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Abstract
The invention discloses a preparation method for high temperature corrosion resistant Cr23C6 cermet. The preparation method comprises the following steps: performing ball milling on Cr3C2 powder under vacuum condition; calculating and weighing the weight of Cr powder according to the Cr content in Cr3C2 powder, and atom ratio and atomic weight of each element in the molecular formula of Cr23C6; adding the Cr powder into a tank containing the Cr3C2 powder; performing vacuum ball milling, and vacuum sintering; cooling together with a sintering oven to obtain pure Cr23C6. According to the invention, the Cr3C2 powder and the Cr powder are adopted to prepare the pure and single Cr23C6 cermet through the ball milling and the sintering, the procedure of the preparation technology is simple, no phenolic resin and other auxiliary additives are need, the relative density is high, and the Cr23C6 cermet is suitable for the field of corrosion resistance (such as electrochemical corrosion, chemical corrosion or high temperature oxide corrosion).
Description
Technical field
The invention belongs to the sintering metal technical field, relate to a kind of sintering metal preparation method, especially a kind of Cr of high-temperature corrosion resistance
23C
6The sintering metal preparation method.
Background technology
Cr
23C
6To there is face-centered cubic transition metal pottery.It has good oxidation-resistance and thermostability and has the excellent advantages such as resistance to chemical attack.Domestic scholars is mainly applied plasma and is covered the technique such as molten technology and prepare one deck with Cr at steel surface
23C
6For the compound coating of hard phase, remove Cr in coating structure
23C
6Also has Cr outward,
7C
3Phase, Cr
3C
2Phase and matrix (as austenite structure) etc., and the thinner thickness of this layer of coating still can't meet the requirement of high life in practical engineering application.In addition, if as contained Cr in high temperature steel
23C
6The time, its high-temperature oxidation resistance significantly improves; Also have, in High Chrome Alloy Steel and rich chromium cast iron, if hard phase is Cr
23C
6The time, because this compound is compared other compound (as Cr with the electropotential of matrix
7C
3, Cr
3C
2) the most approaching, so it has good resistance to electrochemical corrosion energy.
The applicant is in earlier stage about Cr
23C
6The preparation of block materials is mainly to adopt Cr powder and Graphite Powder 99 and be aided with resol etc. to be undertaken by suitable ball milling, sintering method, if but obtain pure single Cr
23C
6Sintering metal, technique wayward (the particularly control of the add-on of resol).
Summary of the invention
The object of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of Cr of high-temperature corrosion resistance is provided
23C
6The sintering metal preparation method, the method is utilized Cr
3C
2Powder and Cr powder carry out Cr
23C
6Ceramic-metallic preparation, can prepare single Cr
23C
6Sintering metal block compound.
The objective of the invention is to be achieved through the following technical solutions:
The Cr of this high-temperature corrosion resistance
23C
6The sintering metal preparation method comprises the following steps:
1) by Cr
3C
2Powder carries out ball milling 10-20 hour under vacuum condition makes the powder surface energetic, then by stop of ball grinder;
2) in conjunction with Cr
3C
2Measuring containing Cr in powder, then press Cr
23C
6The molecular formula Atom than and the nucleidic mass of each element Cr powder that calculates and weigh;
3) will fill Cr
3C
2The ball grinder of powder is opened, the Cr powder weighed up is added in tank, and then vacuumize reach≤10
-1P
aGet final product, after carrying out ball milling 10-40 hour, rapidly by Cr
3C
2Mixture filling after powder and Cr sphere of powder mill is in mould;
4) will fill Cr
3C
2The mould of powder and Cr powder mixture is put into sintering oven and is carried out sintering, and sintering is to carry out in vacuum sintering funace, and during sintering, the vacuum tightness of vacuum oven is :≤10
-1Pa; The heat-up rate of sintering oven is: 3-10 ℃/sec; Pressure is: 5-30MPa; Sintering temperature is: 1000 ℃~1500 ℃; Soaking time is: 60~120 minutes, and together cooling with sintering oven after sintering, obtain Cr
23C
6Material.
Above-mentioned Cr
3C
2Powder is business Cr
3C
2Powder, its atomic ratio: 1.5:1, granularity :≤300 μ m, purity:>99.0%.
Further, above-mentioned steps 1) middle vacuum tightness≤10
-1Pa.
Further, above-mentioned steps 2) in, the purity of described Cr powder is>99.9%; Granularity≤
200μm。
The present invention has following beneficial effect:
The Cr of high-temperature corrosion resistance of the present invention
23C
6The sintering metal preparation method adopts Cr
3C
2Powder and Cr powder, prepare pure single Cr by ball milling and sintering
23C
6Sintering metal, this preparation process is simpler, and without supplementary additives such as interpolation resol, relative density is higher.Be specially adapted to anti-corrosion (as, galvanic corrosion, chemical corrosion, high temperature oxidation and corrosion etc.) field.
Embodiment
The Cr of high-temperature corrosion resistance of the present invention
23C
6The sintering metal preparation method, carry out according to following:
At first, by business Cr
3C
2Powder (atomic ratio: 1.5:1; Granularity :≤300 μ m; Purity:>99.0%), under vacuum condition (≤10
-1Pa) carry out ball milling 10-20 hour and make the powder surface energetic, then by stop of ball grinder.
Then, in conjunction with Cr
3C
2Measuring containing Cr in powder, then press Cr
23C
6The molecular formula Atom than the nucleidic mass of (about 3.8:1) and each element, calculate and the Cr powder of weighing (purity is>99.9%; Granularity≤200 μ m).To Cr
3C
2Add Cr in powder, make it meet Cr
23C
6The weight ratio of Cr and C in molecular formula.
Secondly, will fill Cr
3C
2The ball grinder of powder is opened, the Cr powder weighed up is added in tank, and then seal and vacuumize reach≤10
-1Pa gets final product, after carrying out ball milling 10-40 hour, rapidly by Cr
3C
2After powder and Cr sphere of powder mill, the mixture filling is in mould.
Finally, will fill Cr
3C
2The mould of powder and Cr powder mixture is put into sintering oven and is carried out sintering, and sintering is to carry out in vacuum sintering funace, and during sintering, the vacuum tightness of vacuum oven is :≤10
-1Pa; The heat-up rate of sintering oven is: 3-10 ℃/sec; Pressure is: 5-20MPa; Sintering temperature is: 1000 ℃~1500 ℃; Soaking time is: 60~120 minutes, together cooling with sintering oven after sintering.Prepared Cr in the present invention
23C
6The preparation process of material simple (without supplementary additives such as interpolation resol), the Main Mechanical index is good.
Below specific embodiments of the invention are described:
Embodiment 1
At first, business is used to powder Cr
3C
2(purity:>99.0%; Granularity :≤300 μ m) and the Cr powder (purity is>99.9%; Granularity≤200 μ m) press Cr
23C
6The molecular formula Atom is converted into weight ratio and weighs than the nucleidic mass with each element, subsequently by Cr
3C
2Pack in ball grinder, seal and vacuumized that (vacuum tightness is 10
-1Pa), carry out ball milling 10 hours by stop of ball grinder.
Then, will fill Cr
3C
2The ball grinder of powder is opened, and the Cr powder weighed up is added in tank, again vacuumizes and reaches 10
-2Pa gets final product, and carries out ball milling after 10 hours, rapidly by Cr
3C
2After powder and Cr sphere of powder mill, the mixture filling is in mould.
Finally, will fill Cr
3C
2The mould of powder and Cr powder mixture is put into sintering oven and is carried out sintering, and sintering is to carry out in vacuum sintering funace, and during sintering, the vacuum tightness of vacuum oven is: 10
-2Pa; The heat-up rate of sintering oven is: 3 ℃/secs; Pressure: 5MPa; Sintering temperature is: 1000 ℃; Soaking time is: 60 minutes, together cooling with sintering oven after sintering.
The pure single Cr of gained in this embodiment
23C
6The compound main performance index is as shown in table 1.
Table 1Cr
23C
6The sintering metal salient features
Embodiment 2
At first, business is used to powder Cr
3C
2(purity:>99.0%; Granularity :≤300 μ m) and the Cr powder (purity is>99.9%; Granularity≤200 μ m) press Cr
23C
6The molecular formula Atom is converted into weight ratio and weighs than the nucleidic mass with each element, subsequently by Cr
3C
2Pack in ball grinder, seal and vacuumized that (vacuum tightness is 10
-2Pa), carry out ball milling 20 hours by stop of ball grinder.
Then, will fill Cr
3C
2The ball grinder of powder is opened, and the Cr powder weighed up is added in tank, again vacuumizes and reaches 10
-1Pa gets final product, and carries out ball milling after 40 hours, rapidly by Cr
3C
2After powder and Cr sphere of powder mill, the mixture filling is in mould.
Finally, will fill Cr
3C
2The mould of powder and Cr powder mixture is put into sintering oven and is carried out sintering, and sintering is to carry out in vacuum sintering funace, and during sintering, the vacuum tightness of vacuum oven is: 10
-1Pa; The heat-up rate of sintering oven is: 10 ℃/secs; Pressure: 20MPa; Sintering temperature is: 1500 ℃; Soaking time is: 120 minutes, together cooling with sintering oven after sintering.
The pure single Cr of gained in this embodiment
23C
6The compound main performance index is as shown in table 2.
Table 2Cr
23C
6The sintering metal salient features
Embodiment 3
At first, business is used to powder Cr
3C
2(purity:>99.0%; Granularity :≤300 μ m) and the Cr powder (purity is>99.9%; Granularity≤200 μ m) press Cr
23C
6The molecular formula Atom is converted into weight ratio and weighs than the nucleidic mass with each element, subsequently by Cr
3C
2Pack in ball grinder, seal and vacuumized that (vacuum tightness is 10
-1Pa), carry out ball milling 15 hours by stop of ball grinder.
Then, will fill Cr
3C
2The ball grinder of powder is opened, and the Cr powder weighed up is added in tank, again vacuumizes and reaches 10
-2Pa gets final product, and carries out ball milling after 25 hours, rapidly by Cr
3C
2After powder and Cr sphere of powder mill, the mixture filling is in mould.
Finally, will fill Cr
3C
2The mould of powder and Cr powder mixture is put into sintering oven and is carried out sintering, and sintering is to carry out in vacuum sintering funace, and during sintering, the vacuum tightness of vacuum oven is: 10
-1Pa; The heat-up rate of sintering oven is: 5 ℃/secs; Pressure: 15MPa; Sintering temperature is: 1250 ℃; Soaking time is: 90 minutes, together cooling with sintering oven after sintering.
The pure single Cr of gained in this embodiment
23C
6The compound main performance index is as shown in table 3.
Table 3Cr
23C
6The sintering metal salient features
Claims (4)
1. the Cr of a high-temperature corrosion resistance
23C
6The sintering metal preparation method, is characterized in that, comprises the following steps:
1) by Cr
3C
2Powder carries out ball milling 10-20 hour under vacuum condition makes the powder surface energetic, then by stop of ball grinder;
2) in conjunction with Cr
3C
2Measuring containing Cr in powder, then press Cr
23C
6The molecular formula Atom than and the nucleidic mass of each element Cr powder that calculates and weigh;
3) will fill Cr
3C
2The ball grinder of powder is opened, the Cr powder weighed up is added in tank, and then vacuumize reach≤10
-1Pa gets final product, after carrying out ball milling 10-40 hour, rapidly by Cr
3C
2Mixture filling after powder and Cr sphere of powder mill is in mould;
4) will fill Cr
3C
2The mould of powder and Cr powder mixture is put into sintering oven and is carried out sintering, and sintering is to carry out in vacuum sintering funace, and during sintering, the vacuum tightness of vacuum oven is :≤10
-1Pa; The heat-up rate of sintering oven is: 3-10 ℃/sec; Pressure is: 5-30MPa; Sintering temperature is: 1000 ℃~1500 ℃; Soaking time is: 60~120 minutes, and together cooling with sintering oven after sintering, obtain Cr
23C
6Material.
2. the Cr of high-temperature corrosion resistance according to claim 1
23C
6The sintering metal preparation method, is characterized in that, described Cr
3C
2Powder is business Cr
3C
2Powder, its atomic ratio: 1.5:1, granularity :≤300 μ m, purity:>99.0%.
3. the Cr of high-temperature corrosion resistance according to claim 1
23C
6The sintering metal preparation method, is characterized in that, vacuum tightness in step 1)≤10
-1Pa.
4. the Cr of high-temperature corrosion resistance according to claim 1
23C
6The sintering metal preparation method, is characterized in that step 2) in, the purity of described Cr powder is>99.9%; Granularity≤200 μ m.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106148907A (en) * | 2015-04-27 | 2016-11-23 | 中国科学院金属研究所 | Do not affect high temperature resistance protective coating and the preparation thereof of high-temperature alloy base mechanics performance |
CN114835496A (en) * | 2022-04-21 | 2022-08-02 | 合肥工业大学 | Cr (chromium) 3 C 2 Method for preparing block material |
CN116397123A (en) * | 2023-06-08 | 2023-07-07 | 西安热工研究院有限公司 | Abrasion resistant high nickel chromium/B 2 O 3 Material, preparation method and application thereof |
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US3846084A (en) * | 1973-08-15 | 1974-11-05 | Union Carbide Corp | Chromium-chromium carbide powder and article made therefrom |
US3881910A (en) * | 1973-08-15 | 1975-05-06 | Union Carbide Corp | Chromium-chromium carbide powder |
CN102219215A (en) * | 2011-03-23 | 2011-10-19 | 北京矿冶研究总院 | Preparation method of high-stability chromium carbide powder |
-
2013
- 2013-08-01 CN CN2013103325142A patent/CN103420373A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US3846084A (en) * | 1973-08-15 | 1974-11-05 | Union Carbide Corp | Chromium-chromium carbide powder and article made therefrom |
US3881910A (en) * | 1973-08-15 | 1975-05-06 | Union Carbide Corp | Chromium-chromium carbide powder |
CN102219215A (en) * | 2011-03-23 | 2011-10-19 | 北京矿冶研究总院 | Preparation method of high-stability chromium carbide powder |
Non-Patent Citations (2)
Title |
---|
KEN HIROTA ET AL: "Simultaneous synthesis and consolidation of chromium carbides(Cr3C2, Cr7C3and Cr23C6) by pulsed electric-current pressure sintering", 《MATERIALS SCIENCE AND ENGINEERING A》 * |
S. SHARAFI ET AL: "Effects of milling and subsequent consolidation treatment on the microstructural properties and hardness of the nanocrystalline chromium carbide powders", 《INTERNATIONAL JOURNAL OF REFRACTORY METALS AND HARD MATERIALS》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106148907A (en) * | 2015-04-27 | 2016-11-23 | 中国科学院金属研究所 | Do not affect high temperature resistance protective coating and the preparation thereof of high-temperature alloy base mechanics performance |
CN114835496A (en) * | 2022-04-21 | 2022-08-02 | 合肥工业大学 | Cr (chromium) 3 C 2 Method for preparing block material |
CN116397123A (en) * | 2023-06-08 | 2023-07-07 | 西安热工研究院有限公司 | Abrasion resistant high nickel chromium/B 2 O 3 Material, preparation method and application thereof |
CN116397123B (en) * | 2023-06-08 | 2023-09-08 | 西安热工研究院有限公司 | Abrasion resistant high nickel chromium/B 2 O 3 Material, preparation method and application thereof |
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Application publication date: 20131204 |