CN103467100A - Preparation method for corrosion-resistant and abrasion-resistant Cr7C3 - Google Patents

Preparation method for corrosion-resistant and abrasion-resistant Cr7C3 Download PDF

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CN103467100A
CN103467100A CN2013103325157A CN201310332515A CN103467100A CN 103467100 A CN103467100 A CN 103467100A CN 2013103325157 A CN2013103325157 A CN 2013103325157A CN 201310332515 A CN201310332515 A CN 201310332515A CN 103467100 A CN103467100 A CN 103467100A
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powder
sintering
resistant
corrosion
cr7c3
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CN103467100B (en
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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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Abstract

The invention discloses a preparation method for corrosion-resistant and abrasion-resistant Cr7C3. The method comprises the steps of firstly ball-milling Cr3C2 powder under a vacuum condition; calculating according to atomic ratios and atom atomic weight of all elements in a Cr7C3 molecular formula, in combination of Cr content in the Cr3C2 powder; weighing Cr powder; adding the Cr powder in a tank with the Cr3C2 powder; ball-milling again in the vacuum; then sintering in the vacuum; and cooling together with a sintering furnace to obtain pure Cr7C3 powder. The Cr3C2 powder and the Cr powder are used in the preparation method for the corrosion-resistant and abrasion-resistant Cr7C3; and an ideal single phase block Cr7C3 compound is obtained by ball-milling and sintering. The method is simple in process; main mechanical performance indexes of Cr7C3 are relatively good; the prepared Cr7C3 is not only suitable for use in the abrasion-resistant field but also suitable for use in the corrosion-resistant (chemical corrosion, high-temperature oxidation corrosion, etc.) field and the abrasion-resistant and corrosion-resistant interacted field.

Description

A kind of Cr of anti-corrosion wear 7c 3the preparation method
Technical field
The invention belongs to anti-corrosion wear material technology field, relate to a kind of preparation method of anti-corrosion wear material, especially a kind of Cr of anti-corrosion wear 7c 3the preparation method.
Background technology
Cr 7c 3be to there is the orthohormbic structure transition metal carbide, there is ceramic character.Its hardness is high, wear resistance good, good oxidation-resistance and thermostability and have the excellent advantages such as acid-and base-resisting corrodibility.Domestic scholars is mainly applied plasma and is covered the technique such as molten technology and prepare one deck with Cr at steel surface 7c 3for the compound coating of hard phase, remove Cr in coating structure 7c 3, also have matrix as austenite structure etc. outward, and the thinner thickness of this layer of coating, still can't meet the requirement of high life in practical engineering application.The foreign scholar prepares single-phase Cr at present 7c 3be mainly that the method for attempting has: (a) method by thermospray prepares one deck Cr 7c 3film; (b) plasma activated sintering; (c) the self-propagating high-temperature reaction is synthetic; (d) vacuum non-pressure sintering; Wherein (b) method has made and has organized the comparatively ideal Cr that contains second-phase 7c 3the block tissue, this material toughness is obviously not enough.At present, about Cr 7c 3the preparation of block materials is mainly and adopts Cr powder and Graphite Powder 99 to be undertaken by suitable ball milling, sintering method.
Iran scholar S.Sharafi, the people such as S.Gomari, (sintering temperature is 1100 ℃ to utilize the method for mechanical ball milling and vacuum (applying argon gas) pressureless sintering; Soaking time is 1 hour) prepared block Cr 7c 3.In this report, resulting block tissue is except Cr is arranged 7c 3also has Cr outward, 2o 3phase is not obviously pure single block Cr 7c 3compound.
Japanese scholars Ken Hirota etc., after the wet-milling of Cr and carbon powder machinery is mixed, with spark plasma sintering, having prepared not is single-phase block Cr 7c 3(contain Cr 3c 2phase), through performance is measured its toughness and shown: this block compound toughness still fails to reach desirable performance index.
Summary of the invention
The object of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of Cr of anti-corrosion wear is provided 7c 3the preparation method, the method is utilized Cr 3c 2powder and Cr powder carry out Cr 7c 3preparation, can prepare single Cr 7c 3the block compound.
The objective of the invention is to be achieved through the following technical solutions:
The Cr of this anti-corrosion wear 7c 3the preparation method comprises the following steps:
1) by Cr 3c 2powder is in vacuum tightness≤10 -1carry out ball milling 3-10 hour under the vacuum condition of Pa and make the powder surface energetic, then by stop of ball grinder;
2) in conjunction with Cr 3c 2measuring containing Cr in powder, then press Cr 7c 3the 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, after carrying out ball milling 5-20 hour, rapidly by Cr 3c 2after powder and Cr sphere of powder mill, the mixture filling 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: 0-30MPa; Sintering temperature is: 900 ℃～1550 ℃; Soaking time is: 30～90 minutes, and together cooling with sintering oven after sintering, obtain pure Cr 7c 3.
Further, above-mentioned steps 1) in, described Cr 3c 2the atomic ratio of powder: 1.5:1, granularity :≤300 μ m, purity:>99.0%.
Further, above-mentioned steps 2) in, the purity of described Cr powder is>99.9%, granularity≤200 μ m.
Further, above-mentioned steps 1) the middle Cr that adopts 3c 2powder is business Cr 3c 2powder.
The present invention has following beneficial effect:
The Cr of anti-corrosion wear of the present invention 7c 3the preparation method utilizes Cr 3c 2powder and Cr powder, prepared desirable single-phase block Cr by ball milling and sintering 7c 3compound.This method technological process is simple, and the Main Mechanical index is better.Applicable wear-resisting field occasion not only, and can also be for anti-corrosion (chemical corrosion, high temperature oxidation and corrosion etc.) field, and the wear-resisting and mutual field of corrosion.
Embodiment
The Cr of the anti-corrosion wear that the present invention proposes 7c 3the preparation method specifically carries 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 3-10 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 7c 3the molecular formula Atom than the nucleidic mass of (about 2.3:1) and each element, calculate and the Cr powder of weighing (purity is>99.9%; Granularity≤200 μ m).(supplement the Cr powder lacked, make the weight ratio of Cr and C reach Cr 7c 3the weight ratio of two atoms 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 5-20 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: 0-30MPa; Sintering temperature is: 900 ℃～1550 ℃; Soaking time is: 30～90 minutes, and together cooling with sintering oven after sintering, obtain single Cr 7c 3the block compound.Prepared Cr in the present invention 7c 3the 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 7c 3the 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 3 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 5 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: 3 ℃/secs; Mould is plus-pressure not; Sintering temperature is: 1550 ℃; Soaking time is: 90 minutes, together cooling with sintering oven after sintering.
The pure single Cr of gained in this embodiment 7c 3the compound main performance index is as shown in table 1.
Table 1Cr 7c 3the compound salient features
Figure BDA00003608780800051
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 7c 3the 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 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 20 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: 10 ℃/secs; Pressure: 30MPa; Sintering temperature is: 900 ℃; Soaking time is: 30 minutes, together cooling with sintering oven after sintering.
The pure single Cr of gained in this embodiment 7c 3the compound main performance index is as shown in table 2.
Table 2Cr 7c 3the compound salient features
Figure BDA00003608780800052
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 7c 3the 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 6 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 15 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: 6 ℃/secs; Pressure: 20MPa; Sintering temperature is: 1200 ℃; Soaking time is: 60 minutes, together cooling with sintering oven after sintering.
The pure single Cr of gained in this embodiment 7c 3the compound main performance index is as shown in table 3.
Table 3Cr 7c 3the compound salient features
Figure BDA00003608780800061

Claims (4)

1. the Cr of an anti-corrosion wear 7c 3the preparation method, is characterized in that, comprises the following steps:
1) by Cr 3c 2powder is in vacuum tightness≤10 -1carry out ball milling 3-10 hour under the vacuum condition of Pa and make the powder surface energetic, then by stop of ball grinder;
2) in conjunction with Cr 3c 2measuring containing Cr in powder, then press Cr 7c 3the 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, after carrying out ball milling 5-20 hour, rapidly by Cr 3c 2after powder and Cr sphere of powder mill, the mixture filling 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: 0-30MPa; Sintering temperature is: 900 ℃～1550 ℃; Soaking time is: 30～90 minutes, and together cooling with sintering oven after sintering, obtain pure Cr 7c 3.
2. the Cr of anti-corrosion wear according to claim 1 7c 3the preparation method, is characterized in that, in step 1), and described Cr 3c 2the atomic ratio of powder: 1.5:1, granularity :≤300 μ m, purity:>99.0%.
3. the Cr of anti-corrosion wear according to claim 1 7c 3the preparation method, is characterized in that step 2) in, the purity of described Cr powder is>99.9%, granularity≤200 μ m.
4. the Cr of anti-corrosion wear according to claim 1 7c 3the preparation method, is characterized in that, adopts Cr in step 1) 3c 2powder is business Cr 3c 2powder.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101508572A (en) * 2009-03-27 2009-08-19 北京工业大学 Quick production method for high-compact single-phase TiB2
CN102876951A (en) * 2012-10-09 2013-01-16 西安交通大学 Method for preparing pure metal ceramic Cr7C3 block

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101508572A (en) * 2009-03-27 2009-08-19 北京工业大学 Quick production method for high-compact single-phase TiB2
CN102876951A (en) * 2012-10-09 2013-01-16 西安交通大学 Method for preparing pure metal ceramic Cr7C3 block

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘阳 等: "《非氧化物陶瓷及其应用》", 31 January 2011, article "《非氧化物陶瓷及其应用》", pages: 204 *

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