CN101181754A - Method for preparing WC/MgO nano composite powder - Google Patents
Method for preparing WC/MgO nano composite powder Download PDFInfo
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- CN101181754A CN101181754A CNA2007101716343A CN200710171634A CN101181754A CN 101181754 A CN101181754 A CN 101181754A CN A2007101716343 A CNA2007101716343 A CN A2007101716343A CN 200710171634 A CN200710171634 A CN 200710171634A CN 101181754 A CN101181754 A CN 101181754A
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Abstract
The invention relates to a preparation method of a WC/MgO nano-composite powder, comprising the steps that: (1) 1 to 5Mum graded WO3, graphite and magnesium powder are mixed according to the molar ratio of 1: (1-2) : (2-3), and put into a ball mill pot: (2) stearic acid is added with mass percentage of 0.5 to 3 percent to prevent the powder from being attached to the pot wall and mill ball and enhance the yield; (3) 0 to 1 time of molar quantity of WO3 of MgO is added to act as a diluting agent to avoid the explosion reaction; (3) the ratio between the ball and material is 4: 1-10 : 1; (4) the ball mill pot is sealed and vacuumed and filled with inert gas; (5) ball mill pot is installed on a ball mill, and continuously mills for 0 to 70 hours at the rotation speed of 100 to 500r/min, and WC/MgO nano-composite powder is prepared. The invention has the advantages of simple technique, low cost and investment, and high yield etc, and the granularity of the synthesized powder ranges from 1 to 150nm and is suitable for industrialization production.
Description
Technical field
The invention belongs to the nano composite material preparation field, particularly relate to a kind of preparation of WC/MgO nano composite powder.
Background technology
Tungsten carbide (WC) is compared with other carbide alloy and refractory metal, has high rigidity, certain plasticity and with melt metal good a series of good physical and mechanical properties such as wettability arranged, be widely used in departments such as metallurgy, machinery, in modern industry, occupy crucial status.(Co) has good wet performance to WC in view of cobalt, and WC has certain solubility in Co, so Co is the topmost binding agent of carbide alloy for many years always.But Co is a kind of valuable and rare, resource with its own strategic significance, the Co ore resources poorness of China, and distribute and disperse, grade is low, the cost of winning height.China needs a large amount of Co ore deposit of import every year at present.As resources consumption big country, utilize external resource can cause the rising of international market resource price in large quantities, the while is also caused huge market and price risk to the demand of self, so seek the substitute of Co, reduce cost of alloy, be subjected to the extensive concern of vast researcher already.Simultaneously, with the carbide alloy of Co as binding agent, its corrosion resistance is relatively poor, when under some mal-condition, using, workpiece is corroded very soon, and the lost of life is difficult to satisfy the instructions for use to workpiece, though magnesia (MgO) toughness is slightly poorer than Co, but price is compared cheap many with Co, the more important thing is corrosion resistance, heat-resisting quantity and Heat stability is good, can satisfy the requirement under the mal-condition, so replace noble metal Co to have certain practical value with MgO.
Traditional Hardmetal materials, its hardness and toughness are the paradox of a pair of mutual restriction, under the situation that hardness improves, can sacrifice toughness; Toughness improves, and hardness descends.And discover that when WC-Co crystal grain drops to 1 μ m when following, the hardness of carbide alloy and intensity can improve simultaneously, when the grainiess size reduced to 5nm, the performance of alloy can be undergone mutation.Discover if the crystal grain crystallite dimension of WC-Co carbide alloy when reaching the nano-scale rank, will have higher hardness, wearability and fatigue strength, so the preparation composite nano-powder is the prerequisite of preparation high performance alloys material.
The advantage that the nano material specific surface is big makes them compare with block materials, and the atom number that arrange on its surface obviously increases with the ratio of inner atom number.Because the bonding state of surface atom is different with inner atom, key attitude mismatch, thereby balance non-chemically appears, the chemism of nano material is strengthened.In the ma process of WC and MgO, the extensive chemical activity that just is being based on nano material just causes taking place mechanical solid-state phase reduction reaction, thereby forms the WC/MgO nano composite powder.
The preparation nano composite powder has following several method usually:
(1) mechanical alloying
Mechanical alloying (MA) is one of a kind of important means for preparing new material that grows up early 1970s, it is with the two or more metals or the mixture of non-metal powder, by high-energy ball milling, final alloy or the ceramic powders that form with micro organization's structure.Produce serious distortion of lattice, highdensity defective in the high-energy ball milling process, form nano level fine structure, make the solid-state reaction of the thermodynamics and kinetics of mechanical alloying and normal temperature different, have feature away from equilibrium state.Existing expert has prepared the WC powder of crystallite dimension less than 10nm with the method both at home and abroad at present, though this method cost is low, technology is simple, synthetic tiny, the easy control of components of nanometer powder crystallite dimension, but producing serious powder in its preparation process pollutes, and be easy between powder react and emit a large amount of heat and lure that other powder reacts, and finally forms another kind of powder into.
(2) spray conversion method
Had producer to carry out large-scale production with the method abroad, still, they also can't produce the WC grain degree less than the block carbide alloy of the nanometer of 150nm.This complex process, wayward, and cost is higher.
(3) other synthetic method
(a) gas phase synthesis method, (b) high-frequency plasma synthetic method, (c) high-frequency induction heating synthetic method, (d) ionic arc method, these synthetic method general work efficient are all lower, are difficult to realize large-scale production.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of WC/MgO nano composite powder, this method technology is simple, cost is low, small investment, productive rate height, and synthetic powder particle granularity is fit to suitability for industrialized production at 1～150nm.
The preparation method of a kind of WC/MgO nano composite powder of the present invention may further comprise the steps:
(1) with the micron-sized WO of 1-5 μ m
3, graphite and magnesium dust in molar ratio 1: (1-2): (1-3) mix, and in the ball grinder of packing into;
(2) add mass percent be the stearic acid of 0.5-3% to prevent powder bonded on tank skin and abrading-ball, improve the mass output rate of powder;
(3), and add 0-1 times of WO for preventing explosive reaction
3The diluent MgO of mole to reduce the adiabatic temperature of reaction, makes from spreading the reaction of type reaction changing into diffused;
(4) ratio of grinding media to material 4: 1-10: 1;
(5) with the ball grinder sealing, and vacuumize, charge into inert gas then;
(6) again ball grinder is installed on the ball mill, and builds outer cover, under the 100-500r/min rotating speed ball milling 0-70 hour continuously, obtain particle diameter at the 1-150nmWC/MgO nano composite powder.
Described step (1) WO
3, graphite and magnesium powder mol ratio 1: 1: 3.
Described step (1) WO
3, graphite and magnesium powder mol ratio 1: 2: 3.
Described step (2) stearic acid is 0.8%.
Inert gas in the described step (5) is an argon gas.
Controlling agent stearic acid of the present invention and diluent MgO can prevent the bonding and the explosive reaction of powder, have improved the mass output rate of powder and the security of preparation.Stearic adding mainly is the undue cold welding between inhibitory reaction thing constituent element, reduces the bonding of powder particle, obviously improves flour extraction, improves the uniformity of alloy powder; And stearic acid can reduce powder particle the fracture energy needed takes place, and more helps the refinement of particle.And add the energy that diluent MgO can absorption system, and, make to reduce the adiabatic temperature of reaction with the energy that reduces the reaction powder from spreading the reaction of type reaction changing into diffused, preventing the security that blast improves the powder preparation process.
Carry out tests such as XRD, SEM and TEM with the WC/MgO nano composite powder and to it, see Fig. 1,2,3,4,5, by the XRD electron diffraction diagram as can be seen, WO
3, graphite and magnesium mixed-powder behind ball milling 50h, WC is embedded on the soft MgO matrix, has formed WC/MgO nano composite powder (Fig. 4); The relative WO of WC/MgO nano composite powder powder of preparation
3, graphite and three kinds of materials of magnesium mixed-powder simple mixed-powder relatively, the former particle diameter is at 1-150nm, and latter's particle diameter is at 2-10 μ m; On appearance, the former is better dispersed, and many reunions are then but arranged.
Description of drawings
Fig. 1 is the ball milling different time sections, WO
3, graphite and magnesium mixed-powder the phase composition of XRD thing.
After Fig. 2 is ball milling 50h, the SEM photo of WC/MgO mixed-powder.
After Fig. 3 is ball milling 50h, the TEM photo of WC/MgO mixed-powder.
After Fig. 4 is ball milling 50h, the TEM photo of WC/MgO mixed-powder.
Fig. 5 is WO
3, graphite and magnesium mixed-powder original appearance SEM photo.
The specific embodiment
The invention will be further elaborated below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in to limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalences fall within the application's appended claims institute restricted portion equally.
Embodiment 1
WO with 0.1mol particle diameter 5 μ m
3, 0.2mol graphite and 0.3mol magnesium powder mix, and in the ball grinder of packing into; In above-mentioned mixed-powder, add mass percent and be 3% stearic acid and the MgO of 0.1mol; By 10: 1 the ratio of grinding media to material abrading-ball of packing into; With the ball grinder sealing, and vacuumize, charge into argon gas then; Ball grinder is installed on the planetary ball mill again, and builds outer cover, continuous ball milling 50h under 250r/min obtains the WC/MgO nano composite powder of powder diameter less than 150nm, and this powder is carried out the phase composition test of XRD thing and SEM, TEM take pictures.
Embodiment 2
WO with 0.3mol particle diameter 2 μ m
3, 0.3mol graphite and 0.9mol magnesium powder mix, and in the ball grinder of packing into; The adding mass percent is 1% stearic acid in above-mentioned mixed-powder, the MgO of 0.2mol; By 8: 1 the ratio of grinding media to material abrading-ball of packing into; With the ball grinder sealing, and vacuumize, charge into argon gas then; Again ball grinder is installed on the planetary ball mill, and builds outer cover, continuous ball milling 60h under 300r/min, obtaining powder diameter is the WC/MgO nano composite powder of 90nm, and this powder is carried out the phase composition test of XRD thing and SEM, TEM take pictures.
Embodiment 3
WO with 0.1mol particle diameter 1 μ m
3, 0.2mol graphite and 0.3mol magnesium powder mix, and in the ball grinder of packing into; The adding mass percent is 0.8% stearic acid in above-mentioned mixed-powder; By 6: 1 the ratio of grinding media to material abrading-ball of packing into; With the ball grinder sealing, and vacuumize, charge into argon gas then; Again ball grinder is installed on the planetary ball mill, and builds outer cover, continuous ball milling 70h under 300r/min, obtaining powder diameter is the WC/MgO nano composite powder of 80nm, and this powder is carried out the phase composition test of XRD thing and SEM, TEM take pictures.
Claims (6)
1. the preparation method of a WC/MgO nano composite powder may further comprise the steps:
(1) with the micron-sized WO of 1-5 μ m
3, graphite and magnesium dust mix, and in the ball grinder of packing into;
(2) adding mass percent is the stearic acid of 0.5-3%, 0-1 times of WO
3The diluent MgO of mole;
(3) ratio of grinding media to material 4: 1-10: 1 abrading-ball of packing into;
(4) with the ball grinder sealing, and vacuumize, charge into inert gas then;
(5) again ball grinder is installed on the ball mill, and builds outer cover, under the 100-500r/min rotating speed ball milling 0-70 hour continuously, obtain particle diameter 1-150nm WC/MgO nano composite powder.
2. the preparation method of a kind of WC/MgO nano composite powder according to claim 1 is characterized in that, described step (1) WO
3, graphite and magnesium powder mol ratio 1: (1-2): (2-3).
3. the preparation method of a kind of WC/MgO nano composite powder according to claim 1 is characterized in that, described step (1) WO
3, graphite and magnesium powder mol ratio 1: 1: 3.
4. the preparation method of a kind of WC/MgO nano composite powder according to claim 1 is characterized in that, described step (1) adds the diluent MgO of 0-1 times of WO3 mole.
5. the preparation method of a kind of WC/MgO nano composite powder according to claim 1 is characterized in that, described step (2) stearic acid is 0.8%.
6. the preparation method of a kind of WC/MgO nano composite powder according to claim 1 is characterized in that, described step (4) inert gas is an argon gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007101716343A CN101181754B (en) | 2007-11-30 | 2007-11-30 | Method for preparing WC/MgO nano composite powder |
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| CN2007101716343A CN101181754B (en) | 2007-11-30 | 2007-11-30 | Method for preparing WC/MgO nano composite powder |
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| CN101181754A true CN101181754A (en) | 2008-05-21 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360074A (en) * | 2013-07-11 | 2013-10-23 | 东华大学 | Preparation method for WC-Al2O3 nanometer composite material |
| CN104084591A (en) * | 2014-07-03 | 2014-10-08 | 哈尔滨工业大学 | Method for preparing Ag-Cu-Ti nano-alloy solder |
| CN105948767A (en) * | 2016-05-03 | 2016-09-21 | 上海应用技术学院 | Nanometer high temperature coating used for ladles |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4598212B2 (en) * | 1999-10-27 | 2010-12-15 | 日本タングステン株式会社 | Method for producing WC-based composite ceramic sintered body |
| CN1280046C (en) * | 2004-07-24 | 2006-10-18 | 中国工程物理研究院核物理与化学研究所 | Ball milling for preparing Mg2Method for preparing Ni nano hydrogen-storage alloy material |
| CN100340481C (en) * | 2006-04-14 | 2007-10-03 | 北京科技大学 | Process for self-propagating high-temperature synthesis of nano tungsten carbide powder |
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2007
- 2007-11-30 CN CN2007101716343A patent/CN101181754B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360074A (en) * | 2013-07-11 | 2013-10-23 | 东华大学 | Preparation method for WC-Al2O3 nanometer composite material |
| CN104084591A (en) * | 2014-07-03 | 2014-10-08 | 哈尔滨工业大学 | Method for preparing Ag-Cu-Ti nano-alloy solder |
| CN104084591B (en) * | 2014-07-03 | 2016-08-17 | 哈尔滨工业大学 | A kind of method preparing Ag-Cu-Ti Nanoalloy solder |
| CN105948767A (en) * | 2016-05-03 | 2016-09-21 | 上海应用技术学院 | Nanometer high temperature coating used for ladles |
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