CN101624288A - Production method of coarse-grain Cr3C2 ceramic powder - Google Patents
Production method of coarse-grain Cr3C2 ceramic powder Download PDFInfo
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- CN101624288A CN101624288A CN200910060292A CN200910060292A CN101624288A CN 101624288 A CN101624288 A CN 101624288A CN 200910060292 A CN200910060292 A CN 200910060292A CN 200910060292 A CN200910060292 A CN 200910060292A CN 101624288 A CN101624288 A CN 101624288A
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Abstract
The invention belongs to a production method of coarse-grain Cr3C2 ceramic powder, comprising the following steps: Cr2O3 and C are adopted as main raw materials, Fe (Co, Ni), FexOy and Al-Ni alloyed powder are added according to proportion and are ball-milled and mixed, and then boat loading, melting and carbonization, ball-milling and grinding, deironing and acid-washing, washing and drying, screen separation and package are carried out. In the invention, FexOy catalyst is added and carries out melting reaction by aluminothermy for accelerating the diffusion speed of carbon, in the reaction process, chrome and carbon atoms are dissolved in Fe solution and the like and are separated out in a Cr3C2 way after being saturated, so as to lead the produced coarse-grain Cr3C2 ceramic powder to have less internal disadvantages, high purity, good performance and millimeter-sized granularity and fully meet the performance requirements of rigidity, abrasive resistance and plastic deformation; the coarse-grain Cr3C2 ceramic powder can be used independently, and can be matched with casting WC and casting Cr3C2 ceramic powder for being used as hard-surface material, and can be directly used as alloy raw material for producing metal ceramic products.
Description
Technical field
The invention belongs to hard material Cr
3C
2The production method of ceramic powders, particularly a kind of purity height, excellent coarse-grain Cr of performance of producing
3C
2The production method of ceramic powders.The Cr that adopts this method to produce
3C
2Ceramic powders both can be used as in the production that hard material is widely used in mine instrument, diel, petroleum drilling and mining instrument, can directly produce ceramic-metal combination as alloy raw material again.
Background technology
Chromium carbide (Cr
3C
2) basic hard material has hardness and wear-resisting, the corrosion resistance characteristic almost identical with cast tungsten carbide (WC).Along with making rapid progress of the development of its manufacturing process and operation technique, and corresponding reinforcement, stiff dough treatment technology become better and approaching perfection day by day chromium carbide (Cr
3C
2) range of application of hard material is more and more wide, not only relate to some bases and conventional industries, and also demonstrate boundless application prospect at high-technology field.Traditional chromium carbide is the additive usefulness as welding material, because anti-wear performance is good, with the welding rod that it is made, built-up welding is (such as coal pulverizer, ball mill, jaw etc.) on the working face of some plant equipment, can be improved more than several times service life.Along with high-abrasive material is used constantly extensively, goed deep into, the demand of carbonization chromium powder increases day by day.Chromium and carbon can form three kinds of compounds: i.e. Cr
23C
6, Cr
7C
3, Cr
3C
2At present in the world to Cr
3C
2The demand of ceramic powders is two kinds of trend, and a kind of is ultra-fine Cr
3C
2Ceramic powders, another kind are coarse-grain Cr
3C
2Ceramic powders.The results show, coarse-grain Cr
3C
2Ceramic powders has the advantages such as fault of construction is less, microhardness is high, microstrain is little under hot conditions, have higher intensity and toughness in order to the alloy product of production and as hard material.Tradition is with Cr
2O
3For raw material prepares Cr
3C
2The method of ceramic powders is with Cr
2O
3Mix, directly form through the secondary carbonization with the solid carbon ball milling; Employing the method carburizing temperature is higher, carbonization time is longer, and is forming Cr
3C
2There is fusing point to be respectively the Cr of 1665 ℃ and 1550 ℃ in the process of phase
7C
3And Cr
23C
6Form mutually in the middle of two, again because Cr
2O
3The granularity of precursor is smaller, the Cr that this method is produced
3C
2The general Powder Particle Size of ceramic powders is the thin Cr of 2~5 μ m
3C
2Powder is limit additive that can only be used as alloy material, welding material etc. because of its performance, make hard material to the requirement of its performance and can not satisfy.
Summary of the invention
The objective of the invention is to research and develop a kind of coarse-grain Cr
3C
2The production method of ceramic powders is in order to the coarse-grain Cr of production high-purity, excellent performance
3C
2Ceramic powder.To reach when having high rigidity and good wearability, also has stronger plastic degeneration's ability; Both can be independent, again can with the casting WC, the casting Cr
3C
2Ceramic powders cooperates as hard material, is used for surfacing (being coated with), the built-up welding on surface easy to wear, also can directly produce the purposes such as ceramic-metal combination as alloy raw material.
Solution of the present invention is still to adopt Cr
2O
3And carbon (C) is as primary raw material, but when batching, add in proportion Fe (Co, Ni), oxide as catalyst iron, not only made catalyst, but also after the Al-Ni alloyed powder of making binding agent mixes, it is synthetic to carry out fusant reaction again, gained cermet piece is through broken, ball milling after synthetic, and magnetic separation is except Fe, pickling and oven dry, thereby screening etc. make high-purity coarse-grain chromium carbide (Cr
3C
2) ceramic powders.Therefore, the inventive method comprises:
A. batching is mixed: with Cr
2O
3Consumption is benchmark, the graphite or the carbon powder that add its weight 23.0~34.0wt%, the oxide of the Fe of 0.15~0.50wt%, the Fe of 0.1~0.4wt% or Co or Ni, 0.1 the Al-Ni alloyed powder of~0.6wt% places the interior ball milling of ball mill to mix in the lump 6~10 hours;
B. fill boat and melting carbonization: will cross 30~100 mesh sieves through A operation gained ball milling compound, screenings is packed in the graphite boat, sends into after the compacting in the carbon shirt-circuiting furnace, and carbonization treatment is 100~160 minutes under 1500~1850 ℃ of temperature, with stove cool off, coarse-grain Cr
3C
2The cermet piece;
C. ball mill grinding: process B gained alloy block Mechanical Crushing to granularity<6.0mm, is sent in the ball mill, and ball milling 20~60 hours gets thick Cr
3C
2Ceramic powder, ratio of grinding media to material 2.5~6: 1;
D. deironing and pickling: with operation C gained Cr
3C
2Ceramic powders is sent in rare nitric acid pickling to go out residual Al, Ni element after the magnet deironing is processed;
E. wash and dry: will send in the vacuum drier by gained material after the step D pickling again with after the washed with de-ionized water, 400~500 ℃ of lower drying and processings 1.5~3.5 hours, namely get object coarse-grain Cr after the cooling
3C
2Ceramic powders;
F. sieve, pack: at first will dry gained Cr
3C
2Ceramic powders is crossed 300 mesh sieves, and screenings is produced ceramic-metal combination as alloy raw material; Oversize then sieves to the powder of variable grain degree according to purposes and subsequent product production requirement, packs.
The oxide of described iron is FeO or Fe
2O
3, Fe
3O
4In order further to improve the quality gained coarse-grain Cr after the carbonization
3C
2The cermet piece carries out Mechanical Crushing and ball mill grinding after removing underburnt, burning and pertusate residual, substandard products again.
The present invention makes catalyst owing to added the oxide of iron, and carry out fusant reaction by Fe (containing Al, Co, the Ni) liquid that forms after the thermit reaction and synthesize, be the present invention utilize gas-liquid reaction mechanism replaced traditional gas-solid, solid-solid reaction is machine-processed, has promoted that by melt the diffusion velocity of diffusion, C of carbon (C) is fast; In the fusant reaction building-up process, chromium, carbon atom all will be dissolved in the liquid such as Fe, arrive to separate out after saturated, thereby change traditional Cr
3C
2Forming core growth pattern (process); This formula growth pattern of separating out is strictly by Cr
3C
2Form is separated out, and it is long to have overcome again background technology carburizing reagent difficulty, carburizing reagent time, at Cr
3C
2There are a large amount of Cr in appearance and the product in the growth course
23C
6, Cr
7C
3Deng dephasign, affect the disadvantage of its performance.Thereby the inventive method has the coarse-grain chromium carbide (Cr that produces
3C
2) the ceramic powders internal flaw is less, purity is high, performance is excellent, Powder Particle Size can reach millimeter (mm) level, can fully satisfy hard material to the requirement of its hardness, wearability and plastic deformation performance; Both can be independent, also can with the casting WC, the casting Cr
3C
2Ceramic powders cooperates as hard material, is used for surfacing (being coated with), the built-up welding on surface easy to wear, also can directly produce the characteristics such as ceramic-metal combination as alloy raw material.
Embodiment
A. batching is mixed: every batch of material is with Cr
2O
3Consumption 100Kg is benchmark, adds the graphite of 28.0Kg, the Fe of 0.35Kg
2O
3Powder, the Co powder of 0.3Kg, the Al-Ni alloyed powder of 0.35Kg places the interior ball milling of ball mill to mix after 8 hours discharging in the lump;
B. fill boat and melting carbonization: will cross 80 mesh sieves through A operation gained ball milling compound, screenings is packed in the graphite boat, and by sending in the carbon shirt-circuiting furnace after the compacting of 20Kg briquetting, carbonization treatment is 130 minutes under 1650~1800 ℃ of temperature, with stove cool off coarse-grain Cr
3C
2The cermet piece;
C. ball mill grinding: process B gained alloy block Mechanical Crushing to granularity<6.0mm, is sent in the ball mill, and ball milling 48 hours gets thick Cr
3C
2Ceramic powders, stand-by, the heavy 580Kg (ratio of grinding media to material is about 4.5: 1) of ball;
D. deironing and pickling: be that 10000 Gausses' permanent magnet places stand-by Cr behind the ball milling with magnetic field intensity
3C
2In the ceramic powder, to go out residual Fe; And then it is sent into percent concentration is pickling in 30% the dilute nitric acid solution, to remove residual Al, Ni element;
E. wash and dry: will send in the vacuum drier by gained material after the step D pickling again with after the washed with de-ionized water, 450 ± 10 ℃ of lower drying and processings 2.5 hours, namely get object coarse-grain Cr after the cooling
3C
2Ceramic powders;
F. sieve, pack: at first will dry gained Cr
3C
2Ceramic powders is crossed 300 mesh sieves, and screenings is produced ceramic-metal combination as alloy raw material; Oversize then sieves to the powder of variable grain degree according to purposes and subsequent product production requirement, packs.
Claims (3)
1. coarse-grain Cr
3C
2The production method of ceramic powders comprises:
A. batching is mixed: with Cr
2O
3Consumption is benchmark, the graphite or the carbon powder that add its weight 23.0~34.0wt%, the oxide of the Fe of 0.15~0.50wt%, the Fe of 0.1~0.4wt% or Co or Ni, 0.1 the Al-Ni alloyed powder of~0.6wt% places the interior ball milling of ball mill to mix in the lump 6~10 hours;
B. fill boat and melting carbonization: will cross 30~100 mesh sieves through A operation gained ball milling compound, screenings is packed in the graphite boat, sends into after the compacting in the carbon shirt-circuiting furnace, and carbonization treatment is 100~160 minutes under 1500~1850 ℃ of temperature, with stove cool off, coarse-grain Cr
3C
2The cermet piece;
C. ball mill grinding: process B gained alloy block Mechanical Crushing to granularity<6.0mm, is sent in the ball mill, and ball milling 20~60 hours gets thick Cr
3C
2Ceramic powder, ratio of grinding media to material 2.5~6: 1;
D. deironing and pickling: with operation C gained Cr
3C
2Ceramic powders is sent in rare nitric acid pickling to go out residual Al, Ni element after the magnet deironing is processed;
E. wash and dry: will send in the vacuum drier by gained material after the step D pickling again with after the washed with de-ionized water, 400~500 ℃ of lower drying and processings 1.5~3.5 hours, namely get object coarse-grain Cr after the cooling
3C
2Ceramic powders;
F. sieve, pack: at first will dry gained Cr
3C
2Ceramic powders is crossed 300 mesh sieves, and screenings is produced ceramic-metal combination as alloy raw material; Oversize then sieves to the powder of variable grain degree according to purposes and subsequent product production requirement, packs.
2. by the described coarse-grain Cr of claim 1
3C
2The production method of ceramic powders; The oxide that it is characterized in that described iron is FeO or Fe
2O
3, Fe
3O
4
3. by the described coarse-grain Cr of claim 1
3C
2The production method of ceramic powders; It is characterized in that gained coarse-grain Cr after the carbonization
3C
2The cermet piece carries out Mechanical Crushing and ball mill grinding after removing underburnt, burning and pertusate residual, substandard products again.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102235950A (en) * | 2010-04-27 | 2011-11-09 | 深圳市比克电池有限公司 | Method for detecting magnetic substances in powder material of lithium ion battery |
CN104307838A (en) * | 2014-08-25 | 2015-01-28 | 国家电网公司 | Recovery processing method for waste and old ceramic insulators |
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 |
-
2009
- 2009-08-07 CN CN200910060292A patent/CN101624288A/en active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102235950A (en) * | 2010-04-27 | 2011-11-09 | 深圳市比克电池有限公司 | Method for detecting magnetic substances in powder material of lithium ion battery |
CN104307838A (en) * | 2014-08-25 | 2015-01-28 | 国家电网公司 | Recovery processing method for waste and old ceramic insulators |
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 |
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Open date: 20100113 |