CN103420373A - Preparation method for high temperature corrosion resistant Cr23C6 cermet - Google Patents

Preparation method for high temperature corrosion resistant Cr23C6 cermet Download PDF

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Publication number
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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CN2013103325142A
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皇志富
高义民
邢建东
马胜强
李烨飞
符寒光
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Xian Jiaotong University
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Xian Jiaotong University
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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

A kind of Cr of high-temperature corrosion resistance 23C 6The sintering metal preparation method
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
Figure BDA00003608921500041
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
Figure BDA00003608921500051
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
Figure BDA00003608921500061

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.
CN2013103325142A 2013-08-01 2013-08-01 Preparation method for high temperature corrosion resistant Cr23C6 cermet Pending CN103420373A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
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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Cited By (4)

* Cited by examiner, † Cited by third party
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