CN108046259A - The preparation method of coarseness carbonization chromium powder - Google Patents
The preparation method of coarseness carbonization chromium powder Download PDFInfo
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- CN108046259A CN108046259A CN201810031795.0A CN201810031795A CN108046259A CN 108046259 A CN108046259 A CN 108046259A CN 201810031795 A CN201810031795 A CN 201810031795A CN 108046259 A CN108046259 A CN 108046259A
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Abstract
One kind can simplify process, save energy consumption, raising powder process accepted product percentage, more preferably meets the preparation method that the industries such as hard material, flux-cored wire, high temperature alloy prepare wear-resisting, corrosion-resistant, resistance to high temperature oxidation new material demand coarseness carbonization chromium powder, and step is as follows：By chrome green powder and carbon dispensing, binding agent mixing is added in；It is molded after mixing with forcing press；Molding mass block is placed in high-temperature vacuum induction heater graphite crucible, is vacuumized, power transmission heat temperature raising is maintained in 200~400Pa of vacuum degree；Chrome green powder controls 1350~1550 DEG C, when the carburizing reagent time 8~15 is small with carbon vacuum carburization reaction generation chromium carbide, carbonation reaction temperature；Vacuum degree is less than 100Pa, and carburizing reagent is completed, and argon gas is filled with into stove, and furnace pressure control melts chromium carbide sintered body in 40~80kPa, then raising heating power, obtains chromium carbide melted ingot；Chromium carbide melted ingot is mechanically broken into granularity less than 10mm particles, with impact crusher powder, by 60 mesh sieves, coarseness carbonization chromium powder is made.
Description
Technical field
The invention belongs to vacuum metallurgy technology field, more particularly to a kind of preparation method of coarseness carbonization chromium powder.
Background technology
Chromium carbide is that one kind has good wear-resisting, corrosion-resistant, anti-oxidant, Gao Rong for (1000~1100 DEG C) in high temperature environments
The high inorganic metal ceramic material of point (1870 DEG C), bond strength, because of its special high-temperature behavior, is widely used as metal surface
Protect thermal spraying material, build up electrode or the flux-cored wire of technique and hard alloy additive.
Existing chrome green is prepared with carbon carbonization in chromium carbide powder technology of preparing, and equipment heats carbon using traditional resistor
Pipe furnace, carbonisation are carbonized using hydrogen shield.This method carburizing temperature is at 1300~1500 DEG C, less than chromium carbide fusing point, instead
The chromium carbide that should be produced is fluffy or sintered body, and by Mechanical Crushing method powder, powder size is thinner, wherein 60 mesh~
200 mesh powder quality ratios 5~20%, can not meet high temperature alloy, hard material and Flux-cored Wire Industry use demand.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of coarseness carbonization chromium powder preparation method, it can be achieved that carbonization and
Fusing ingot casting process is carried out continuously, and simplifies process, saves energy consumption, more preferably meets the row such as hard material, flux-cored wire, high temperature alloy
Industry prepares wear-resisting, corrosion-resistant, resistance to high temperature oxidation new material demand.
The preparation method of coarseness carbonization chromium powder of the present invention, is characterized in that step is as follows：
Step 1
By chrome green powder and carbon in mass ratio 1：0.3~1：0.4 ratio dispensing, binding agent by chrome green powder with
1%~3% ratio of carbon mixture quality adds in mixing；Material is molded with forcing press after mixing, 5~8KN/cm of briquetting pressure2,
Forming shape is cylindric or pelletizing shape, and molding mass block is placed in drying, 60~80 DEG C of drying temperature, drying time in drying chamber
When 60-80 is small；
Step 2
Molding mass block is placed in high-temperature vacuum induction heater graphite crucible, is vacuumized, vacuum degree is less than 40Pa, power transmission
Heat temperature raising, temperature-rise period persistently vacuumize, and maintain in the range of 200~400Pa of vacuum degree；Chrome green powder and carbon vacuum
Carburizing reagent generates chromium carbide, and carbonation reaction temperature controls 1350~1550 DEG C, when the carburizing reagent time 8~15 is small；Vacuum degree
Less than 100Pa, carburizing reagent is completed, and argon gas is filled with into stove, and furnace pressure control heats work(in 40~80kPa, then raising
Rate melts chromium carbide sintered body, obtains chromium carbide melted ingot；Step 3
Chromium carbide melted ingot is mechanically broken into granularity less than 10mm particles, with impact crusher powder, is passed through
60 mesh sieves are made coarseness carbonization chromium powder by 60 mesh sieves, coarseness carbonization chromium powder are made.
In step 2, in temperature-rise period, heating power is stepped up by gradient increased temperature, temperature-rise period is divided into 700~900
DEG C, 1000~1200 DEG C, 1350~1550 DEG C of three gradients, 700~900 DEG C of gradient sections raise 200~300 DEG C of speed on an hourly basis
Degree heating, 1000~1200 DEG C of gradient sections raise 100~200 DEG C of speed heatings on an hourly basis, and 1350~1550 DEG C of gradient sections are pressed
Raise the heating of 50~100 DEG C of speed per hour, reach 1350~1550 DEG C of heat preservations 1~2 it is small when.
In step 2, it is that graphite crucible temperature is made to be kept for 1700~1900 DEG C to improve heating power, 5~15 points of retention time
Have a power failure cooling after clock, and carburizing reagent is carried out continuously with fusing ingot casting.
In step 1, the chrome green powder purity is more than 99%, and granularity is less than 0.15mm.
Carbon described in step 1 is a kind of or two kinds of arbitrary proportions mixture in graphite powder, carbon black, purity
It is all higher than 99%.
Binding agent described in step 1 is methylcellulose, one kind in carboxymethyl cellulose, phenolic resin.
The graphite paper of graphite crucible liner described in step 2.
The purity of argon is more than 99.99%.
Reaction mechanism of the present invention：
Chrome green has with carbon carburizing reagent master equation
Cr2O3+81/23C=2/23Cr23C6+3CO (1)
Cr2O3+27/7C=2/7Cr7C3+3CO (2)
Cr2O3+13/3C=2/3Cr3C2+3CO (3)
Chromium carbide theoretical carbon content 5.68% in reaction equation (1), chromium carbide theoretical carbon content 9.00% in reaction equation (2),
Theoretical mixed carbon comtent 1:0.30, chromium carbide theoretical carbon content 13.33% in reaction equation (3), theoretical mixed carbon comtent 1:0.34.It is actual to prepare
Carbon amount of allocating excessive 5~20% in the process, it is therefore an objective to it is thorough to ensure that carburizing reagent carries out, while chromium carbide sintered body is avoided to melt
With carbon loss during ingot casting.
The beneficial effects of the invention are as follows：Carbonization and fusing ingot casting process are carried out continuously, and are simplified process, are saved energy consumption, simultaneously
Chromium carbide melts ingot casting compared with chromium carbide sintered body, the former is more conducive to Mechanical Crushing and obtains coarseness carbonization chromium powder, improves system
Powder process accepted product percentage more preferably meets the industries such as hard material, flux-cored wire, high temperature alloy and prepares wear-resisting, corrosion-resistant, high temperature resistance
Aoxidize new material demand.
Specific embodiment
Embodiment 1
1st, by chrome green powder and graphite powder in mass ratio 1：0.32 ratio weighs chrome green powder 5kg, graphite powder
1.6kg is mixed, and the chrome green powder purity is 99.1%, and granularity is less than 0.15mm, and graphite powder purity 99.1% adds in
The carboxymethyl cellulose binding agent mixing of mixture quality 2%；Material is molded with forcing press after mixing, briquetting pressure 5.5KN/
cm2, forming shape is cylindric；Molding mass block is placed in temperature as when drying 80 is small in 60 DEG C of drying chambers.
2nd, by the 2 layers of graphite paper in graphite crucible bottom in high-temperature vacuum induction heater and circumference liner, it is then charged into drying
Molding mass block, material block height is the 2/3 of crucible height；It vacuumizes, vacuum degree is 35Pa feeding temperature-raisings, and temperature-rise period is persistently taken out
Vacuum, and maintain in the range of 200~400Pa of vacuum degree；Carburizing temperature is set as 1400 DEG C, is stepped up heating power by gradient
Heating, temperature-rise period are divided into 800 DEG C, 1100 DEG C, 1400 DEG C of three gradients, and room temperature~800 DEG C gradient section raises on an hourly basis
200 DEG C of speed heatings, 800~1100 DEG C of gradient sections raise 130 DEG C of speed and heat up on an hourly basis, 1100~1400 DEG C of gradient sections,
Raise the heating of 50 DEG C of speed on an hourly basis, reach 1400 DEG C of heat preservations 2 it is small when, when carbonization time 14.5 is small, vacuum degree 90Pa is complete
Into carburizing reagent；Argon gas, the purity of argon 99.991% are filled with into stove, furnace pressure reaches 50kPa, improves heating work(
Rate makes graphite crucible temperature be kept for 1700~1900 DEG C, and the retention time has a power failure cooling after ten minutes；It is down to room temperature to come out of the stove, by stone
Graphite paper and chromium carbide melted ingot are toppled in black crucible, are removed graphite paper and are obtained chromium carbide melted ingot.
3rd, chromium carbide melted ingot is broken into granularity less than 10mm particles with jaw crusher, with impact crusher powder,
By 60 mesh sieves, coarseness carbonization chromium powder is made.
After measured, product main chemical compositions and granularity are as follows：
Chemical composition：Cr：89.32%, C：9.85%, chromium carbide purity 99.17%.
Granularity Detection：Mass ratio accounts for 3.4% for+60 mesh in 60 mesh powder, and the mesh of -60 mesh~200 accounts for 65.2%, -200 mesh
Account for 31.4%.
Embodiment 2
1st, by chrome green powder and graphite powder in mass ratio 1：0.33 ratio weighs chrome green powder 5kg, graphite powder
1.65kg is mixed, and the chrome green powder purity is 99.2%, and granularity is less than 0.15mm, and graphite powder purity 99.2% adds
Enter the carboxymethyl cellulose binding agent mixing of mixture quality 2%；Material is molded with forcing press after mixing, briquetting pressure 6KN/
cm2, forming shape is cylindric；Molding mass block is placed in temperature as when drying 70 is small in 70 DEG C of drying chambers.
2nd, by the 2 layers of graphite paper in graphite crucible bottom in high-temperature vacuum induction heater and circumference liner, it is then charged into drying
Molding mass block, material block height is the 2/3 of crucible height；It vacuumizes, vacuum degree is 30Pa feeding temperature-raisings, and temperature-rise period is persistently taken out
Vacuum, and maintain in the range of 200~400Pa of vacuum degree；Carburizing temperature is set as 1450 DEG C, is stepped up heating power by gradient
Heating, temperature-rise period are divided into 750 DEG C, 1050 DEG C, 1450 DEG C of three gradients, and room temperature~750 DEG C gradient section raises on an hourly basis
250 DEG C of speed heatings, 750~1050 DEG C of gradient sections raise 150 DEG C of speed and heat up on an hourly basis, 1050~1450 DEG C of gradient sections,
Raise the heating of 70 DEG C of speed on an hourly basis, reach 1450 DEG C of heat preservations 1 it is small when, when carbonization time 12 is small, vacuum degree 80Pa is completed
Carburizing reagent；Argon gas, the purity of argon 99.992% are filled with into stove, furnace pressure reaches 70kPa, improves heating power,
Graphite crucible temperature is made to be kept for 1700~1900 DEG C, have a power failure cooling after 8 minutes retention times；It is down to room temperature to come out of the stove, by graphite earthenware
Graphite paper and chromium carbide melted ingot are toppled in crucible, are removed graphite paper and are obtained chromium carbide melted ingot.
3rd, chromium carbide melted ingot is broken into granularity less than 10mm particles with jaw crusher, with impact crusher powder,
By 60 mesh sieves, coarseness carbonization chromium powder is made.
After measured, product main chemical compositions and granularity are as follows：
Chemical composition：Cr：88.81%, C：10.51%, chromium carbide purity 99.32%.
Granularity Detection：Mass ratio accounts for 4.5% for+60 mesh in 60 mesh powder, and the mesh of -60 mesh~200 accounts for 67.6%, -200 mesh
Account for 27.9%.
Embodiment 3
1st, by chrome green powder and graphite powder in mass ratio 1：0.36 ratio weighs chrome green powder 5kg, graphite powder
1.8kg is mixed, and the chrome green powder purity is 99.3%, and granularity is less than 0.15mm, and graphite powder purity 99.3% adds in
The carboxymethyl cellulose binding agent mixing of mixture quality 2%；Material is molded with forcing press after mixing, briquetting pressure 8KN/
cm2, forming shape is cylindric；Molding mass block is placed in temperature as when drying 60 is small in 80 DEG C of drying chambers.
2nd, by the 2 layers of graphite paper in graphite crucible bottom in high-temperature vacuum induction heater and circumference liner, it is then charged into drying
Molding mass block, material block height is the 2/3 of crucible height；It vacuumizes, vacuum degree is 20Pa feeding temperature-raisings, and temperature-rise period is persistently taken out
Vacuum, and maintain in the range of 200~400Pa of vacuum degree；Carburizing temperature is set as 1500 DEG C, is stepped up heating power by gradient
Heating, temperature-rise period are divided into 900 DEG C, 1200 DEG C, 1500 DEG C of three gradients, and room temperature~900 DEG C gradient section raises on an hourly basis
300 DEG C of speed heatings, 900~1200 DEG C of gradient sections raise 180 DEG C of speed and heat up on an hourly basis, 1200~1500 DEG C of gradient sections,
Raise the heating of 80 DEG C of speed on an hourly basis, reach 1500 DEG C of heat preservations 1.5 it is small when, when carbonization time 10 is small, vacuum degree 60Pa is complete
Into carburizing reagent；Argon gas, the purity of argon 99.995% are filled with into stove, furnace pressure reaches 80kPa, improves heating work(
Rate makes graphite crucible temperature be kept for 1700~1900 DEG C, and have a power failure cooling after 15 minutes retention times；It is down to room temperature to come out of the stove, by stone
Graphite paper and chromium carbide melted ingot are toppled in black crucible, are removed graphite paper and are obtained chromium carbide melted ingot.
3rd, chromium carbide melted ingot is broken into granularity less than 10mm particles with jaw crusher, with impact crusher powder,
By 60 mesh sieves, coarseness carbonization chromium powder is made.
After measured, product main chemical compositions and granularity are as follows：
Chemical composition：Cr：86.03%, C：13.13%, chromium carbide purity 99.16%.
Granularity Detection：Mass ratio accounts for 2.7% for+60 mesh in 60 mesh powder, and the mesh of -60 mesh~200 accounts for 62.5%, -200 mesh
Account for 34.8%.
In 1~embodiment of above-described embodiment 3, the graphite powder carbon black either mixture of graphite powder and carbon black is pure
It spends for 99.2%.
In 1~embodiment of above-described embodiment 3, generation in the carboxymethyl cellulose methylcellulose or phenolic resin
It replaces.
Comparative example
1st, by chrome green powder and graphite powder in mass ratio 1：0.32 ratio weighs chrome green powder 5kg, graphite powder
1.6kg is mixed, and the chrome green powder purity is 99.1%, and granularity is less than 0.15mm, and graphite powder purity 99.1% adds in
The carboxymethyl cellulose binding agent mixing of mixture quality 2%；Material is molded with forcing press after mixing, briquetting pressure 5.5KN/
cm2, forming shape is cylindric；Molding mass block is placed in temperature as when drying 70 is small in 70 DEG C of drying chambers.
2nd, by the 2 layers of graphite paper in graphite crucible bottom in high-temperature vacuum induction heater and circumference liner, it is then charged into drying
Molding mass block, material block height close at the 2/3 of crucible height；It vacuumizes, vacuum degree is 35Pa feeding temperature-raisings, and temperature-rise period is held
It is continuous to vacuumize, and maintain in the range of 100~400Pa of vacuum degree；Carburizing temperature is set as 1400 DEG C, be stepped up heating power by
Gradient increased temperature, temperature-rise period are divided into 800 DEG C, 1100 DEG C, 1400 DEG C of three gradients, and room temperature~800 DEG C gradient section is on an hourly basis
200 DEG C of speed heatings of rise, 800~1100 DEG C of gradient sections raise 130 DEG C of speed heatings, 1100~1400 DEG C of gradients on an hourly basis
Section raises the heating of 50 DEG C of speed on an hourly basis, reach 1400 DEG C of heat preservations 2 it is small when, carbonization time for 14.5 it is small when；Vacuum degree is
90Pa completes carburizing reagent, and argon gas, the purity of argon 99.99% are filled with into stove, and furnace pressure reaches 50kPa, and have a power failure drop
Temperature；It is down to room temperature to come out of the stove, graphite paper in graphite crucible and chromium carbide agglomerate is toppled over, remove graphite paper and obtain chromium carbide sintering
Block.
3rd, chromium carbide agglomerate is broken into granularity less than 10mm particles with jaw crusher, with impact crusher system
By 60 mesh sieves, carbonization chromium powder is made in powder.
After measured, product main chemical compositions and granularity are as follows：
Chemical composition：Cr：89.01%, C：10.25%, chromium carbide purity 99.26%.
Granularity Detection：Mass ratio accounts for 0% for+60 mesh in 60 mesh powder, and the mesh of -60 mesh~200 accounts for 18.5%, and -200 mesh account for
81.5%.
Specific embodiments of the present invention are above are only, are not intended to limit the invention, for those skilled in the art
For member, the invention may be variously modified and varied.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of coarseness carbonization chromium powder, it is characterized in that：Step is as follows：
Step 1
By chrome green powder and carbon in mass ratio 1：0.3~1：0.4 ratio dispensing, binding agent are mixed by chrome green powder with carbon
1%~3% ratio for closing material quality adds in mixing；Material is molded with forcing press after mixing, 5~8KN/cm of briquetting pressure2, shaping
Shape is cylindric or pelletizing shape, and molding mass block is placed in drying, 60~80 DEG C of drying temperature, drying time 60-80 in drying chamber
Hour；
Step 2
Molding mass block is placed in high-temperature vacuum induction heater graphite crucible, is vacuumized, vacuum degree is less than 40Pa, power transmission heating
Heating, temperature-rise period persistently vacuumizes, and maintains in the range of 200~400Pa of vacuum degree；Chrome green powder and carbon vacuum carburization
Reaction generation chromium carbide, carbonation reaction temperature control 1350~1550 DEG C, when the carburizing reagent time 8~15 is small；Vacuum degree is less than
100Pa, carburizing reagent are completed, and argon gas is filled with into stove, and furnace pressure control is melted in 40~80kPa, then raising heating power
Change chromium carbide sintered body, obtain chromium carbide melted ingot；
Step 3
Chromium carbide melted ingot is mechanically broken into granularity less than 10mm particles, with impact crusher powder, passes through 60 mesh
Sieve is made coarseness carbonization chromium powder by 60 mesh sieves, coarseness carbonization chromium powder is made.
2. the preparation method of coarseness carbonization chromium powder according to claim 1, it is characterized in that：In step 2, temperature-rise period
In, be stepped up heating power by gradient increased temperature, temperature-rise period be divided into 700~900 DEG C, 1000~1200 DEG C, 1350~
1550 DEG C of three gradients, 700~900 DEG C of gradient sections raise 200~300 DEG C of speed heatings, 1000~1200 DEG C of ladders on an hourly basis
Degree section raises 100~200 DEG C of speed heatings on an hourly basis, and 1350~1550 DEG C of gradient sections raise 50~100 DEG C of speed on an hourly basis
Degree heating, reach 1350~1550 DEG C heat preservation 1~2 it is small when.
3. the preparation method of coarseness carbonization chromium powder according to claim 1, it is characterized in that：In step 2, heating is improved
Power is that graphite crucible temperature is made to be kept for 1700~1900 DEG C, and have a power failure cooling after 5~15 minutes retention times, and carburizing reagent is with melting
Change ingot casting to be carried out continuously.
4. the preparation method of coarseness carbonization chromium powder according to claim 1, it is characterized in that：In step 1, described three
Two chromium powder purity are aoxidized more than 99%, granularity is less than 0.15mm.
5. the preparation method of coarseness carbonization chromium powder according to claim 1, it is characterized in that：In step 1, the carbon
It is a kind of or two kinds of arbitrary proportions mixture in graphite powder, carbon black, purity is all higher than 99%.
6. the preparation method of coarseness carbonization chromium powder according to claim 1, it is characterized in that：In step 1, described is viscous
Knot agent is methylcellulose, one kind in carboxymethyl cellulose, phenolic resin.
7. the preparation method of coarseness carbonization chromium powder according to claim 1, it is characterized in that：In step 2, the graphite
Crucible needs liner graphite paper.
8. the preparation method of coarseness carbonization chromium powder according to claim 1, it is characterized in that：In step 2, the argon
Gas purity is more than 99.99%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793165A (en) * | 2018-09-13 | 2018-11-13 | 台山市国峰耐磨金属科技有限公司 | A kind of production method of chromium carbide |
| CN111646511A (en) * | 2020-06-16 | 2020-09-11 | 民乐县锦世建材新材料有限责任公司 | Method for producing melt-blown chromium oxide by vacuum sintering |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793165A (en) * | 2018-09-13 | 2018-11-13 | 台山市国峰耐磨金属科技有限公司 | A kind of production method of chromium carbide |
| CN111646511A (en) * | 2020-06-16 | 2020-09-11 | 民乐县锦世建材新材料有限责任公司 | Method for producing melt-blown chromium oxide by vacuum sintering |
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| CN108046259B (en) | 2021-04-30 |
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