[go: up one dir, main page]

CN102963895A - Preparation method of chromium carbide powder - Google Patents

Preparation method of chromium carbide powder Download PDF

Info

Publication number
CN102963895A
CN102963895A CN2012104674860A CN201210467486A CN102963895A CN 102963895 A CN102963895 A CN 102963895A CN 2012104674860 A CN2012104674860 A CN 2012104674860A CN 201210467486 A CN201210467486 A CN 201210467486A CN 102963895 A CN102963895 A CN 102963895A
Authority
CN
China
Prior art keywords
powder
chromium carbide
preparation
carbide powder
chromium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2012104674860A
Other languages
Chinese (zh)
Other versions
CN102963895B (en
Inventor
林晨星
林文汉
张海涛
王大忠
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JINZHOU NEWROUTE HYPERPURE MATERIAL CO Ltd
Original Assignee
JINZHOU NEWROUTE HYPERPURE MATERIAL CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JINZHOU NEWROUTE HYPERPURE MATERIAL CO Ltd filed Critical JINZHOU NEWROUTE HYPERPURE MATERIAL CO Ltd
Priority to CN201210467486.0A priority Critical patent/CN102963895B/en
Publication of CN102963895A publication Critical patent/CN102963895A/en
Application granted granted Critical
Publication of CN102963895B publication Critical patent/CN102963895B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Carbon And Carbon Compounds (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention provides a preparation method of chromium carbide powder, comprising the following steps of: evenly mixing chromic oxide powder and carbon black powder, adding deionized water, evenly stirring, forming in a pressing way to obtain wet powder blocks, and drying to obtain mixed power blocks; filling the mixed power blocks into a graphite crucible in a vacuum heating furnace, and vacuumizing to preheat; charging carbon dioxide gas, and carrying out high-temperature reduction; vacuumizing, and continuously carrying out vacuum treatment; cooling, and discharging from the furnace to obtain chromium carbide power; and smashing to obtain chromium carbide power. According to the preparation method, the raw materials are easy to obtain, the carbon black powder is taken as a reducing agent, the chromium carbide powder is small in particle size and large in specific surface area, the reduction reaction is easier to carry out, the reaction time can be shortened, and the production cost can be reduced; and after the manner of excessive reducing agent carbon black is adopted, the reaction speed can be effectively accelerated, the reaction temperature can be reduced, the rudimental carbon black powder can be removed by charging the carbon dioxide, the stability of the production quality can be guaranteed, and the preparation method is suitable for the industrial production.

Description

A kind of preparation method of chromium carbide powder
Technical field
The present invention relates to a kind of preparation method of chromium carbide powder.
Background technology
Chromium carbide is a kind of hard, wear-resisting, sludge proof high-temperature material, is widely used in alloy, welding rod, heat spray coating layer material and abrasive material and makes.Along with the development of aeronautical and space technology, the requirement of alloy performance is more and more higher, and chromium carbide powder plays a key effect to the preparation of high duty alloy tungsten.
At present, the production method of chromium carbide powder mainly is carborization and carbon reduction method.Carborization is that hafnium metal powfer and carbon dust are mixed, and adds the compressed with adhesive moulding, carries out carbonization under High Temperature High Pressure, pulverizes, and screening gets chromium carbide.Because carbonization process can not be removed the metallic impurity of raw material chromium, therefore, the method is higher to the purity requirement of raw material chromium, and production cost is high; And chromium metal and chromium carbide hardness are very large, need to adopt the hard pulverizer to pulverize, and equipment cost is high, production rate is slow and contaminate environment.Carbon reduction method be with carbonaceous material as reductive agent, be granularity that the chromium sesquioxide of 1 μ m~5 μ m is reduced into chromium carbide at high temperature.The method production cost is high; Owing to be the reduction reaction of solid-solid, require powder to mix and close contact, such as high pressure compacting or ball milling; Reductive agent and the chromium sesquioxide amount of allocating into are strict, otherwise easily because reaction not exclusively causes oxygen to exceed standard (chromium sesquioxide of surplus) or uncombined carbon exceeds standard (carbonaceous material of surplus), make unstable product quality; During reduction reaction, the reductive agent usage quantity is few, and temperature of reaction need to be higher than 1480 ℃, to accelerate speed of reaction, and over reduction occurs when being higher than 1500 ℃ in temperature of reaction easily, generates the chromium carbon alloy and sticks together, therefore, the temperature of reaction controlled range is little, is not suitable for suitability for industrialized production.
CN101955184A discloses a kind of preparation method of novel nanoscale chrome carbide powder; the method is that Nanoscale Chromic Oxides and carbonaceous reducing agent are mixed; add alcohol or acetone as ball-milling medium; after ball milling, drying; under argon gas or hydrogen shield atmosphere or vacuum condition; in 800 ℃~1100 ℃ carbonization 0.5h~1h, obtain chromium carbide powder.The method raw material need adopt Nanoscale Chromic Oxides, and consumes a large amount of alcohol or acetone, and production cost is high; And need to use the nano level raw material of ball mill ball milling, be not suitable for suitability for industrialized production.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of chromium carbide powder, and the method raw material is easy to get, and production cost is low, and constant product quality is fit to suitability for industrialized production.
Technical solution of the present invention is:
A kind of preparation method of chromium carbide powder, its concrete steps are:
1.1 chromium sesquioxide powder and carbon black powder are mixed according to mass ratio 1:0.35~1:0.48, get mixed powder, adding quality is the deionized water of mixed powder total mass 20%~50%, stir, compression moulding gets the wet mash piece, drying gets the mixed powder piece;
1.2 in the packaged plumbago crucible that enters to be located in the vacuum furnace of mixed powder, vacuumize, making the heating under vacuum furnace pressure is 1Pa~200Pa, under 100 ℃~500 ℃, and thermal pretreatment 5h~10h; Pass into carbon dioxide, making the heating under vacuum furnace pressure is 5000Pa~10000Pa, under 1250 ℃~1450 ℃, and high temperature reduction 1.5h~2h; Vacuumize, making the heating under vacuum furnace pressure is 1Pa~100Pa, under 1200 ℃~1500 ℃, and vacuum-treat 0.5h~1.5h;
1.3 cooling is come out of the stove, and gets the chromium carbide powder ball;
1.4 the chromium carbide powder ball is pulverized, is got the chromium carbide powder.
Described chromium sesquioxide powder is pigmentary chromium sesquioxide powder.
During thermal pretreatment, first with temperature increase to 100 ℃~120 ℃, insulation 2h~3h, then under 120 ℃~500 ℃, insulation 3h~5h to avoid the water evaporation rate in the mixed powder piece too fast, causes the mixed powder piece cracked.
The particle diameter of described carbon black powder is 500 orders~2000 orders.
The pressing pressure that the powder piece is closed in described wet mixing is 0.1MPa~1MPa.
During high temperature reduction, temperature is 1200 ℃~1400 ℃ in the vacuum furnace, and the time is 1.5h~1.8h.
Beneficial effect of the present invention:
(1) use carbon black powder to make reductive agent, granularity is little, and specific surface area is large, and the easier reduction reaction of carrying out has shortened the reaction times, has reduced production cost.
(2) because the water absorbing properties of carbon black powder is good, can adopt deionized water and material and compression moulding, need not to adopt tackiness agent, pollution-free to raw material; During mixing, need not pressing machine, the moulding of energy direct pressing has been shortened the production time and has been reduced the equipment investment cost; After the drying, mixed powder piece internal defect helps carbon dioxide in the internal flow of mixed powder piece, has shortened the carbon dioxide reaction times; The chromium carbide that makes is smashed to pieces powdered easily.
(3) adopt the excessive mode of reductive agent carbon black powder, effectively improved speed of response, reduced temperature of reaction, pass into co 2 removal and remain in carbon black powder in the chromium carbide, guaranteed the stability of the quality of production.
(4) vacuum-treat behind the high temperature reduction has become the high price sulphur that is difficult to remove and holds volatile low price sulphur, can effectively reduce the sulphur content among the carbon Chrome.
Description of drawings
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is the Laser particle-size distribution analysis chart of the present invention (corresponding embodiment 1);
Fig. 3 is the Laser particle-size distribution analysis chart of the present invention (corresponding embodiment 2).
Embodiment
Embodiment 1
When 1, producing, as shown in Figure 1, be that 500 orders~2000 purpose carbon black powders are put into two-dimensional mixing machine with the pigmentary chromium sesquioxide powder of 100kg and 40kg particle diameter, stir 0.5h, get mixed powder; Mixed powder is put into stirring tank, evenly add the 42kg deionized water, stir, make mixed powder moistening fully, and under 0.1MPa pressure, be pressed into diameter and be 3cm, high be the cylindrical wet mash piece of 4cm, in air, dry 2h, get cylindrical mixed powder piece.
2, with in the packaged plumbago crucible that enters to be located in the vacuum furnace of cylindrical mixed powder, vacuumize, make the heating under vacuum furnace pressure remain on 1Pa, adopt the Medium frequency induction coil that plumbago crucible is heated, with temperature increase to 100 ℃, then thermal pretreatment 3h continues heating, under 500 ℃, thermal pretreatment 5h; Pass into carbon dioxide, make the heating under vacuum furnace pressure remain on 5000Pa, under 1450 ℃, high temperature reduction 1.5h; Be evacuated to 1Pa, under 1500 ℃, vacuum-treat 0.5h.
3, cooling is come out of the stove, and gets the chromium carbide powder ball, and the chromium carbide powder ball is pulverized, and gets the chromium carbide powder, purity〉99.95%; The chromium carbide powder is carried out respectively Laser particle-size distribution analysis (as shown in Figure 2) and analysis of chemical elements (as shown in table 1).
Embodiment 2
1, is that 500 orders~2000 purpose carbon black powders are put into two-dimensional mixing machine with the pigmentary chromium sesquioxide powder of 100kg and 38kg particle diameter, stirs 0.5h, get mixed powder; Mixed powder is put into stirring tank, evenly add the 28kg deionized water, stir, make mixed powder moistening fully, and under 0.5MPa pressure, be pressed into the square wet mash piece that the length of side is 4cm, in air, dry 2h, get square mixed powder piece.
2, with in the packaged plumbago crucible that enters to be located in the vacuum furnace of square mixed powder, vacuumize, make the heating under vacuum furnace pressure remain on 100Pa, adopt the Medium frequency induction coil that plumbago crucible is heated, with temperature increase to 120 ℃, thermal pretreatment 10h; Pass into carbon dioxide, make the heating under vacuum furnace pressure remain on 10000Pa, under 1250 ℃, high temperature reduction 2h; Be evacuated to 100Pa, under 1200 ℃, vacuum-treat 1.5h.
3, cooling is come out of the stove, and gets the chromium carbide powder ball, and the chromium carbide powder ball is pulverized, and gets the chromium carbide powder, purity〉99.95%; The chromium carbide powder is carried out respectively Laser particle-size distribution analysis (as shown in Figure 3) and analysis of chemical elements (as shown in table 1 |), and as seen from Figure 2, the particle diameter of chromium carbide powder is 0.1 μ m~0.5 μ m.
Embodiment 3
1, is that 500 orders~2000 purpose carbon black powders are put into two-dimensional mixing machine with the pigmentary chromium sesquioxide powder of 100kg and 48kg particle diameter, stirs 1h, get mixed powder; Mixed powder is put into stirring tank, evenly add the 74kg deionized water, stir, make mixed powder moistening fully, and under 1MPa pressure, be pressed into the spherical wet mash piece of diameter 4cm, in air, dry 2h, get spherical mixed powder piece.
2, with in the packaged plumbago crucible that enters to be located in the vacuum furnace of spherical mixed powder, vacuumize, make the heating under vacuum furnace pressure remain on 200Pa, adopt the Medium frequency induction coil that plumbago crucible is heated, with temperature increase to 100 ℃, insulation 2h, then continue heating, under 400 ℃, insulation 3h; Pass into carbon dioxide, make the heating under vacuum furnace pressure remain on 8000Pa, under 1350 ℃, high temperature reduction 1.8h; Be evacuated to 50Pa, under 1400 ℃, vacuum-treat 1h.
3, cooling is come out of the stove, and gets the chromium carbide powder ball, and the chromium carbide powder ball is pulverized, and gets the chromium carbide powder, purity〉99.95%; The chromium carbide powder is carried out analysis of chemical elements (as shown in table 1 |), and after testing, the particle diameter of chromium carbide powder is 0.1 μ m~0.5 μ m.
Analysis of chemical elements result (the unit: wt%) of table 1 chromium carbide powder
? C Fe Al Si Cu O S N
Embodiment 1 13.0 0.0110 0.0008 0.0040 0.0002 0.015 0.006 0.0050
Embodiment 2 12.8 0.0130 0.0008 0.0042 0.0002 0.010 0.005 0.0030
Embodiment 3 13.2 0.0210 0.0006 0.0044 0.0001 0.020 0.003 0.0045

Claims (6)

1. the preparation method of a chromium carbide powder is characterized in that:
1.1 chromium sesquioxide powder and carbon black powder are mixed according to mass ratio 1:0.35~1:0.48, get mixed powder, adding quality is the deionized water of mixed powder total mass 20%~50%, stir, compression moulding gets the wet mash piece, drying gets the mixed powder piece;
1.2 in the packaged plumbago crucible that enters to be located in the vacuum furnace of mixed powder, vacuumize, making the heating under vacuum furnace pressure is 1Pa~200Pa, under 100 ℃~500 ℃, and thermal pretreatment 5h~10h; Pass into carbon dioxide, making the heating under vacuum furnace pressure is 5000Pa~10000Pa, under 1250 ℃~1450 ℃, and high temperature reduction 1.5h~2h; Vacuumize, making the heating under vacuum furnace pressure is 1Pa~100Pa, under 1200 ℃~1500 ℃, and vacuum-treat 0.5h~1.5h;
1.3 cooling is come out of the stove, and gets the chromium carbide powder ball;
1.4 the chromium carbide powder ball is pulverized, is got the chromium carbide powder.
2. the preparation method of chromium carbide powder according to claim 1, it is characterized in that: described chromium sesquioxide powder is pigmentary chromium sesquioxide powder.
3. the preparation method of chromium carbide powder according to claim 1 is characterized in that: during thermal pretreatment, and first with temperature increase to 100 ℃~120 ℃, insulation 2h~3h, then under 120 ℃~500 ℃, insulation 3h~5h.
4. the preparation method of chromium carbide powder according to claim 1, it is characterized in that: the particle diameter of described carbon black powder is 500 orders~2000 orders.
5. the preparation method of chromium carbide powder according to claim 1, it is characterized in that: the pressing pressure that the powder piece is closed in described wet mixing is 0.1MPa~1MPa.
6. the preparation method of chromium carbide powder according to claim 1 is characterized in that: during high temperature reduction, temperature is 1200 ℃~1400 ℃ in the vacuum furnace, and the time is 1.5h~1.8h.
CN201210467486.0A 2012-11-19 2012-11-19 Preparation method of chromium carbide powder Expired - Fee Related CN102963895B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210467486.0A CN102963895B (en) 2012-11-19 2012-11-19 Preparation method of chromium carbide powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210467486.0A CN102963895B (en) 2012-11-19 2012-11-19 Preparation method of chromium carbide powder

Publications (2)

Publication Number Publication Date
CN102963895A true CN102963895A (en) 2013-03-13
CN102963895B CN102963895B (en) 2014-07-02

Family

ID=47794374

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210467486.0A Expired - Fee Related CN102963895B (en) 2012-11-19 2012-11-19 Preparation method of chromium carbide powder

Country Status (1)

Country Link
CN (1) CN102963895B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2543902C2 (en) * 2013-04-23 2015-03-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Новосибирский государственный технический университет" Method of obtaining chrome carbide
RU2558601C1 (en) * 2014-03-17 2015-08-10 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" METHOD OF PRODUCTION OF CHROMIUM CARBIDE Cr3C2
CN107511968A (en) * 2017-10-27 2017-12-26 苏州市天星山精密模具有限公司 Precision plastic rubber mould
CN108046259A (en) * 2018-01-12 2018-05-18 锦州市金属材料研究所 The preparation method of coarseness carbonization chromium powder
CN109550946A (en) * 2019-01-29 2019-04-02 攀钢集团钒钛资源股份有限公司 The preparation method of chromium carbide

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1176224A (en) * 1996-09-06 1998-03-18 汪兆泉 Production process of chromium carbide
CN101767204A (en) * 2010-02-03 2010-07-07 株洲硬质合金集团有限公司 Fluidized preparation method for WC-Co composite powder
CN101955184A (en) * 2010-09-20 2011-01-26 河南工业大学 Method for preparing novel nanoscale chrome carbide powder
CN101693974B (en) * 2009-10-09 2011-02-02 陈启丰 Process for producing tungsten carbide cobalt chrome metal composite powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1176224A (en) * 1996-09-06 1998-03-18 汪兆泉 Production process of chromium carbide
CN101693974B (en) * 2009-10-09 2011-02-02 陈启丰 Process for producing tungsten carbide cobalt chrome metal composite powder
CN101767204A (en) * 2010-02-03 2010-07-07 株洲硬质合金集团有限公司 Fluidized preparation method for WC-Co composite powder
CN101955184A (en) * 2010-09-20 2011-01-26 河南工业大学 Method for preparing novel nanoscale chrome carbide powder

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
赵立伟 等: "碳化铬粉的研制与生产", 《铁合金》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2543902C2 (en) * 2013-04-23 2015-03-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Новосибирский государственный технический университет" Method of obtaining chrome carbide
RU2558601C1 (en) * 2014-03-17 2015-08-10 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" METHOD OF PRODUCTION OF CHROMIUM CARBIDE Cr3C2
CN107511968A (en) * 2017-10-27 2017-12-26 苏州市天星山精密模具有限公司 Precision plastic rubber mould
CN108046259A (en) * 2018-01-12 2018-05-18 锦州市金属材料研究所 The preparation method of coarseness carbonization chromium powder
CN108046259B (en) * 2018-01-12 2021-04-30 锦州市金属材料研究所 Preparation method of coarse-grained chromium carbide powder
CN109550946A (en) * 2019-01-29 2019-04-02 攀钢集团钒钛资源股份有限公司 The preparation method of chromium carbide

Also Published As

Publication number Publication date
CN102963895B (en) 2014-07-02

Similar Documents

Publication Publication Date Title
CN102382997B (en) A method for preparing WC-Co cemented carbide by microwave sintering
CN102963895B (en) Preparation method of chromium carbide powder
CN100572264C (en) A kind of preparation method of flying saucer shaped nano-hexagonal boron nitride powder
CN108080649B (en) Method for preparing superfine iron powder by low-temperature hydrocarbon duplex reduction
CN104831100A (en) Method for preparing graphene reinforced metal-based composite material through discharge plasma (SPS) sintering
CN103695685B (en) Method for preparing WC-Co hard alloy by microwave reaction sintering
CN103924111B (en) The preparation method of a kind of Wimet nanometer particle size powder and high performance sintered block materials
CN106735176A (en) Sub- titanium oxide metal composite is spherical or spherical powder and preparation method thereof
CN107338372A (en) A kind of preparation and its application of the aluminum-based composite hydrogen manufacturing material of discharge plasma sintering
CN102275918B (en) Method for producing vanadium carbide
CN102807207A (en) Method for producing high-density and high-strength graphite product with fine structure
CN102249687B (en) Method for preparing hafnium boride powder
CN108465817A (en) A kind of high-compactness pure tungsten article fabrication methods of even tissue
CN104232961B (en) A kind of high-strength height hard Cu-Cr composite and its preparation method and application
CN111872414B (en) Preparation method of micro-nano pre-alloyed powder
CN107116227B (en) A kind of preparation method of ultrafine WC-Ni composite powder
CN105345007A (en) Preparation method for highly dense chromium-tungsten alloy target
CN102285661B (en) Preparation method of tungsten boride powder
CN112713264A (en) Artificial graphite negative electrode material, preparation method, application and battery
CN102659100A (en) Preparation method of high-density fine-grain graphite material
CN107324796B (en) A kind of carbon/magnesium aluminate spinel composite powder
CN112795794B (en) Method for preparing high-purity metal chromium block by adopting wet-process mixed metal powder
CN102249689B (en) Preparation method of aluminum nitride powder
CN115305399A (en) Rare earth tungsten electrode material and preparation method thereof
CN111940752B (en) Preparation method of superfine Fe-Cu alloy powder

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20140702

Termination date: 20181119