CN103467100B - Preparation method for corrosion-resistant and abrasion-resistant Cr7C3 - Google Patents

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 3preparation method

Technical field

The invention belongs to anti-corrosion wear field of material technology, relate to a kind of preparation method of anti-corrosion wear material, especially a kind of Cr of anti-corrosion wear ₇c ₃preparation method.

Background technology

Cr ₇c ₃be that there is orthohormbic structure transition metal carbide, there is the character of pottery.Its hardness is high, wear resistance good, good oxidation-resistance and thermostability and have the advantages such as excellent acid-and base-resisting corrodibility.Domestic scholars is mainly applied plasma and is covered the techniques such as molten technology and prepare one deck with Cr at steel surface ₇c ₃for the compound coating of hard phase, except Cr in coating structure ₇c ₃, also have matrix as austenite structure etc. outward, and the thinner thickness of this layer of coating, in practical engineering application, still cannot meet the requirement of high life.Current foreign scholar prepares single-phase Cr ₇c ₃the method of mainly attempting has: (a) prepares one deck Cr by the method for thermospray ₇c ₃film; (b) plasma activated sintering; (c) self-propagating high-temperature Reactive Synthesis; (d) vacuum non-pressure sintering; Wherein (b) method has obtained and has organized the comparatively ideal Cr containing second-phase ₇c ₃block 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 DEG C to utilize the method for mechanical ball milling and vacuum (applying argon gas) pressureless sintering; Soaking time is 1 hour) prepare block Cr ₇c ₃.The block tissue obtained in this report is apart from Cr ₇c ₃outward, Cr is also had ₂o ₃phase is not obviously pure single block Cr ₇c ₃compound.

Japanese scholars Ken Hirota etc., after Cr and the wet-milling of carbon powder machinery being mixed, having prepared with spark plasma sintering is not single-phase block Cr ₇c ₃(containing Cr ₃c ₂phase), through performance measures its toughness and shows: this block compound toughness still fails to reach desirable performance index.

Summary of the invention

The object of the invention is to the shortcoming overcoming above-mentioned prior art, a kind of Cr of anti-corrosion wear is provided ₇c ₃preparation method, the method utilizes Cr ₃c ₂powder and Cr powder carry out Cr ₇c ₃preparation, single Cr can be prepared ₇c ₃block compound.

The object of the invention is to be achieved through the following technical solutions:

The Cr of this anti-corrosion wear ₇c ₃preparation 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 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 nucleidic mass of molecular formula Atom ratio and each element calculates and Cr powder of weighing;

3) Cr will be filled ₃c ₂the ball grinder of powder is opened, and 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 ₂powder and the rear mixture of Cr sphere of powder mill are filled in mould;

4) Cr will be filled ₃c ₂the mould of powder and Cr powder mixture is put into sintering oven and is sintered, and sintering carries 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 DEG C/sec; Pressure is: 0-30MPa; Sintering temperature is: 900 DEG C ~ 1550 DEG C; Soaking time is: 30 ~ 90 minutes, together cool after sintering with sintering oven, obtains pure Cr ₇c ₃.

Further, above-mentioned steps 1) in, described Cr ₃c ₂the atomic ratio of powder: 1.5:1, granularity :≤300 μm, purity: > 99.0%.

Further, above-mentioned steps 2) in, the purity of described Cr powder is > 99.9%, granularity≤200 μm.

Further, above-mentioned steps 1) middle employing Cr 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 ₃preparation 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 Main Mechanical index is more excellent.Not only be suitable for wear-resisting field occasion, and anti-corrosion (chemical corrosion, high temperature oxidation and corrosion etc.) field can also be used for, and the wear-resisting and mutual field of corrosion.

Embodiment

The Cr of the anti-corrosion wear that the present invention proposes ₇c ₃preparation method specifically carries out according to following:

First, by business Cr ₃c ₂powder (atomic ratio: 1.5:1; Granularity :≤300 μm; Purity: > 99.0%), under vacuum (≤10 ^-1pa) carry out ball milling 3-10 hour and make 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 nucleidic mass of molecular formula Atom ratio (about 2.3:1) and each element calculate and Cr powder of weighing (purity is > 99.9%; Granularity≤200 μm).(namely 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, Cr will be filled ₃c ₂the ball grinder of powder is opened, and the Cr powder weighed up is added in tank, and then seal and vacuumize reach≤10 ^-1pa, after carrying out ball milling 5-20 hour, rapidly by Cr ₃c ₂powder and the rear mixture of Cr sphere of powder mill are filled in mould.

Finally, Cr will be filled ₃c ₂the mould of powder and Cr powder mixture is put into sintering oven and is sintered, and sintering carries 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 DEG C/sec; Pressure is: 0-30MPa; Sintering temperature is: 900 DEG C ~ 1550 DEG C; Soaking time is: 30 ~ 90 minutes, together cool after sintering with sintering oven, obtains single Cr ₇c ₃block compound.Cr prepared in the present invention ₇c ₃the preparation process simple (without the need to adding the supplementary additives such as resol) of material, Main Mechanical index is excellent.

Below specific embodiments of the invention are described:

Embodiment 1

First, business is used powder Cr ₃c ₂(purity: > 99.0%; Granularity :≤300 μm) and Cr powder (purity is > 99.9%; Granularity≤200 μm) by Cr ₇c ₃the nucleidic mass of molecular formula Atom ratio and each element is converted into weight ratio and weighs, subsequently by Cr ₃c ₂load in ball grinder, seal and carry out vacuumizing that (vacuum tightness is 10 ^-1pa), ball milling 3 hours is carried out by stop of ball grinder.

Then, Cr will be filled ₃c ₂the ball grinder of powder is opened, and the Cr powder weighed up is added in tank, again vacuumizes and reach 10 ^-1pa, carries out ball milling after 5 hours, rapidly by Cr ₃c ₂powder and the rear mixture of Cr sphere of powder mill are filled in mould.

Finally, Cr will be filled ₃c ₂the mould of powder and Cr powder mixture is put into sintering oven and is sintered, and sintering carries 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 DEG C/sec; Mould is plus-pressure not; Sintering temperature is: 1550 DEG C; Soaking time is: 90 minutes, together cool after sintering with sintering oven.

The pure single Cr of gained in this embodiment ₇c ₃compound main performance index is as shown in table 1.

Table 1Cr ₇c ₃compound salient features

Embodiment 2

First, business is used powder Cr ₃c ₂(purity: > 99.0%; Granularity :≤300 μm) and Cr powder (purity is > 99.9%; Granularity≤200 μm) by Cr ₇c ₃the nucleidic mass of molecular formula Atom ratio and each element is converted into weight ratio and weighs, subsequently by Cr ₃c ₂load in ball grinder, seal and carry out vacuumizing that (vacuum tightness is 10 ^-2pa), ball milling 10 hours is carried out by stop of ball grinder.

Then, Cr will be filled ₃c ₂the ball grinder of powder is opened, and the Cr powder weighed up is added in tank, again vacuumizes and reach 10 ^-2pa, carries out ball milling after 20 hours, rapidly by Cr ₃c ₂powder and the rear mixture of Cr sphere of powder mill are filled in mould.

Finally, Cr will be filled ₃c ₂the mould of powder and Cr powder mixture is put into sintering oven and is sintered, and sintering carries 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 DEG C/sec; Pressure: 30MPa; Sintering temperature is: 900 DEG C; Soaking time is: 30 minutes, together cool after sintering with sintering oven.

The pure single Cr of gained in this embodiment ₇c ₃compound main performance index is as shown in table 2.

Table 2Cr ₇c ₃compound salient features

Embodiment 3

First, business is used powder Cr ₃c ₂(purity: > 99.0%; Granularity :≤300 μm) and Cr powder (purity is > 99.9%; Granularity≤200 μm) by Cr ₇c ₃the nucleidic mass of molecular formula Atom ratio and each element is converted into weight ratio and weighs, subsequently by Cr ₃c ₂load in ball grinder, seal and carry out vacuumizing that (vacuum tightness is 10 ^-1pa), ball milling 6 hours is carried out by stop of ball grinder.

Then, Cr will be filled ₃c ₂the ball grinder of powder is opened, and the Cr powder weighed up is added in tank, again vacuumizes and reach 10 ^-2pa, carries out ball milling after 15 hours, rapidly by Cr ₃c ₂powder and the rear mixture of Cr sphere of powder mill are filled in mould.

Finally, Cr will be filled ₃c ₂the mould of powder and Cr powder mixture is put into sintering oven and is sintered, and sintering carries 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 DEG C/sec; Pressure: 20MPa; Sintering temperature is: 1200 DEG C; Soaking time is: 60 minutes, together cool after sintering with sintering oven.

The pure single Cr of gained in this embodiment ₇c ₃compound main performance index is as shown in table 3.

Table 3Cr ₇c ₃compound salient features

Claims (2)

1. the Cr of an anti-corrosion wear ₇c ₃preparation 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 powder surface energetic, then by stop of ball grinder; Described Cr ₃c ₂the atomic ratio of powder: 1.5:1, granularity :≤300 μm, purity: > 99.0%;

2) in conjunction with Cr ₃c ₂measuring containing Cr in powder, then press Cr ₇c ₃the nucleidic mass of molecular formula Atom ratio and each element calculates and Cr powder of weighing; The purity of described Cr powder is > 99.9%, granularity≤200 μm;

3) Cr will be filled ₃c ₂the ball grinder of powder is opened, and 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 ₂powder and the rear mixture of Cr sphere of powder mill are filled in mould;

4) Cr will be filled ₃c ₂the mould of powder and Cr powder mixture is put into sintering oven and is sintered, and sintering carries 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 DEG C/sec; Pressure is: 0-30MPa; Sintering temperature is: 900 DEG C ~ 1550 DEG C; Soaking time is: 30 ~ 90 minutes, together cool after sintering with sintering oven, obtains pure Cr ₇c ₃.

2. the Cr of anti-corrosion wear according to claim 1 ₇c ₃preparation method, is characterized in that, step 1) middle employing Cr ₃c ₂powder is business Cr ₃c ₂powder.