CN104192905A - Salt bath furnace and method for continuously synthesizing Cr2AlC powder - Google Patents
Salt bath furnace and method for continuously synthesizing Cr2AlC powder Download PDFInfo
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- CN104192905A CN104192905A CN201410379999.5A CN201410379999A CN104192905A CN 104192905 A CN104192905 A CN 104192905A CN 201410379999 A CN201410379999 A CN 201410379999A CN 104192905 A CN104192905 A CN 104192905A
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Abstract
The invention discloses a salt bath furnace and a method for continuously synthesizing Cr2AlC powder. The salt bath furnace comprises a slender neck, so that the liquid level of the salt bath is positioned in a height range of the slender neck of the salt bath furnace, the contact area between the salt bath and air can be reduced, raw materials are prevented from being oxidized, volatilization of the salt bath can be reduced, the raw materials are saved, and the cost is reduced. Moreover, the problems that equipment is polluted due to escape of fused salts and the like do not exist in the salt bath furnace. The salt bath furnace is respectively provided with a feeding hole and a discharge opening, and materials can be continuously fed until primary production is ended during production; a protective layer is formed by virtue of activated carbon powder, a synthetic reaction can be finished under normal pressure, vacuum and a protective atmosphere are not needed, and extra pressure is not needed either; the purity of the prepared Cr2AlC powder can be over 95wt%; moreover, because the section of the neck of the salt bath furnace is relatively small, volatilization loss of the fused salts is small during synthesis, the fused salt can be recycled, and the environment is not polluted.
Description
Technical field
The invention belongs to field of material synthesis technology, relate to a kind of synthetic Cr of salt bath method that adopts
2the Apparatus and method for of AlC powder, is specifically related to a kind of continuously synthetic Cr
2the salt bath furnace of AlC powder and synthetic method.
Background technology
Cr
2alC is M
n+1aX
ntypical Representative in series lamellar compound, wherein existing ionic linkage, covalent linkage have again metallic bond.Cr
2alC not only has metal and ceramic over-all properties, i.e. high heat conduction, high conduction, the performance such as anti-oxidant, wear-resistant, also because its unique laminate structure has good self-lubricating property.Have broad application prospects at industrial circles such as space flight and aviation, petrochemical complex, electronic information.
Cr
2the main synthetic method of AlC material has magnetron sputtering method, pressure sintering, hot isostatic pressing method, discharge plasma sintering method and molten-salt growth method.Although four kinds of methods can be synthesized the Cr that purity is very high above
2alC material, but equipment is all more expensive, and production efficiency is lower, is not easy to suitability for industrialized production.
Molten-salt growth method is taking chromium powder, aluminium powder, carbon dust as raw material, and KCl and NaCl are auxiliary agent, and its homogenious charge compression is made to bulk, under vacuum condition or under protective atmosphere condition, carry out in 900～1200 DEG C, then through pulverizing, washing obtains Cr
2alC powder.Obviously, under vacuum condition, need to provide the Special Equipment of vacuum, this synthetic method is still unfavorable for a large amount of production, has also increased cost simultaneously.Synthetic in protective atmosphere, not only will consume a large amount of gas, and with a large amount of volatilizations of fused salt, the fused salt of volatilization can form steam and overflow, and pollutes synthesis device.In addition, existing likely realization utilizes molten-salt growth method to synthesize Cr
2the equipment of AlC material mainly contains cycle stove and two kinds of continuous kilns.If the cycle of employing stove is produced, energy consumption is higher, if adopt continuous kiln to produce, the fused salt of volatilization can be overflowed crucible and be polluted burner hearth, also needs to consume crucible material simultaneously, greatly improves production cost.
In sum, existing synthetic Cr
2the equipment of AlC powder and method, because production cost is higher, be difficult to be promoted use.For the deficiencies in the prior art, the invention provides a kind of continuously synthetic Cr
2the salt bath furnace of AlC powder and synthetic method, can synthesize the Cr that purity is high efficiently
2alC powder.
Summary of the invention
Object of the present invention aims to provide a kind of continuously synthetic Cr
2the salt bath furnace of AlC powder, equipment is simple, easy to operate, almost pollution-free, can realize Cr
2the serialization of AlC powder is produced.
Another object of the present invention is to provide one and utilizes above-mentioned salt bath furnace synthetic Cr continuously
2the method of AlC powder, can realize Cr
2the serialization of AlC powder is produced, and preparation technology is simple, cost is low, is conducive to Cr
2applying of AlC material.
Above-mentioned purpose of the present invention, can realize by the salt bath furnace and the method that are provided by following technical proposals.
The invention provides a kind of continuously synthetic Cr
2the salt bath furnace of AlC powder, the burner hearth of salt bath furnace is followed successively by tapered portion, cylindrical portion and back taper portion from top to bottom; Tapered portion top is provided with neck; Neck top is charging opening; Back taper portion bottom is provided with discharge port; The sectional area of neck and discharge port is all less than the sectional area of cylindrical portion.The burner hearth of this structure, makes salt bath liquid level be positioned at the altitude range of slender neck, can reduce the contact area of salt bath and air, prevents raw material oxidation, also can reduce the volatilization of salt bath simultaneously, has saved raw material, has reduced pollution.
Salt bath furnace structure provided by the invention can realize by following two kinds of modes:
(1) salt bath furnace can be internal heat type salt bath furnace, and burner hearth is built into refractory brick, and burner hearth inner side-wall two corresponding positions are provided with electrode (comprising positive electrode and negative potential); Electrode is by being connected with external power source through the wire of refractory brick.In order not affect Cr
2alC powder purity, the most handy Cr of electrode
2alC or be coated with Cr
2the electro-conductive material of AlC is made.Further, in order well to control the temperature of salt bath in salt bath furnace, can be in salt bath furnace burner hearth or at burner hearth inner side-wall set temperature sensor (as thermopair).Further, in order to control the take-off rate of fused salt, can valve be set at discharge port.
(2) salt bath furnace can be also external-heat salt bath furnace, and burner hearth is made of silica tube; Burner hearth is arranged in vertical resistance furnace.The outsourcing from the market of vertical resistance furnace.Further, in order to control the take-off rate of fused salt, can valve be set at discharge port.
Salt bath furnace provided by the invention, the height of neck refer to from neck bottom (being tapered portion top) to neck top the height of (be charging opening bottom), the height of neck is preferably 100～500mm, when highly lower than 100mm, can not effectively control the effusion of fused salt; And neck is too high, not only can makes the utilization ratio of neck reduce, and can increase the manufacturing cost of equipment.
Based on above continuously synthetic Cr
2the salt bath furnace of AlC powder, the invention provides a kind of continuously synthetic Cr
2the method of AlC powder, with Cr
3c
2powder, chromium powder and aluminium powder are raw material, according to conventional ratio, are containing the NaCl of activated carbon powder, KCl and BaCl
2mixed salt-bath at conventional temperature, carry out the synthetic and conventional processing of conventional salt bath reaction and obtain Cr
2alC powder; In salt bath, the mass parts of each material is: NaCl20～40 part, KCl20～40 part, BaCl
240～60 parts, 0.5～3 part of activated carbon powder.
In above synthetic method, the inventor finds through large quantity research, with NaCl, KCl, BaCl
2with activated carbon powder be salt bath prepared by raw material, activated carbon powder, because density is little, is positioned at the upper strata of salt bath, can be used as protective layer and prevents raw material and the airborne oxygen reaction in salt bath; And the neck area of the salt bath furnace that the present invention adopts is relatively little; Both match, and can form thicker activated carbon layer at neck place, play the effect of extraordinary isolation oxygen, ensure the purity of final product.Because carbon dust is not volatile, its consumption is little, also can greatly reduce salt bath cost.Traditional molten salt react ion under protective atmosphere, owing to being a dynamic process, needs constantly to consume gas in process of production, causes cost higher.Even employing protective atmosphere, salt bath furnace provided by the invention is compared with traditional salt liquid furnace, and due to neck relative narrower, gas is not volatile, and in the situation that other condition is identical, the gas volume of consumption also can greatly reduce, and then reduces costs.
Above-mentioned with Cr
3c
2powder, chromium powder and aluminium powder raw material can carry out proportioning according to conventional ratio, at conventional Cr
3c
2under powder, chromium powder and aluminium powder synthesis temperature, synthesize Cr according to conventional salt bath reaction
2alC, then obtains Cr through the later stage of salt bath conventional treatment method
2alC powder.As one preferred embodiment, continuously synthetic Cr provided by the invention
2the method of AlC powder comprises the following steps:
(a) preparation mixing salt, by NaCl, KCl and BaCl
2after drying, mix and be mixed with mixing salt with activated carbon powder; The mass parts of above-mentioned material is: NaCl20～40 part, KCl20～40 part, BaCl
240～60 parts, 0.5～3 part of activated carbon powder;
(b) raw materials piece, by Cr
3c
2powder, chromium powder and aluminium powder are according to mol ratio (1～1.1): 1:(2.2～2.6) preparation raw material, then by above-mentioned raw materials by raw material and mixing salt mass ratio 1:(1～2) mix in joining mixing salt, and be pressed into raw material block;
(c) prepare salt bath, mixing salt is joined in salt bath furnace, be warmed up to 950～1000 DEG C, form salt bath, and make salt bath liquid level in salt bath furnace be positioned at the height of neck scope;
(d) building-up reactions, raw material block is joined in salt bath, control adds the speed of raw material block and the take-off rate of salt bath furnace discharge port place fused salt, make the residence time of raw material in salt bath be 1.5～4h to carry out building-up reactions, make salt bath liquid level be positioned at all the time the height of neck scope of salt bath furnace simultaneously;
(e) aftertreatment: allow from the Cr that contains of discharge port outflow
2the fused salt mixt of AlC powder is cooling, then through pulverizing, wash, leave standstill and/or filter, drying, obtains Cr
2alC powder.
Below preferred embodiment in, a mixing salt part for step (a) preparation is for forming salt bath at salt bath furnace in advance; Another part is used for and Cr
3c
2powder, chromium powder and aluminium powder mix and are pressed into raw material block, and its object has two, and first raw material dispersion can disperse and be dissolved in fused salt after making raw material enter salt bath quickly; It two is in adding raw material, is convenient to supplement in proportion fused salt and activated carbon, to ensure that building-up process can carry out continuously.
Below preferred embodiment in, step (d) remains in salt bath furnace slender neck altitude range salt bath liquid level, its object has two, the first makes the activated carbon floating in salt bath collect in neck, form thicker sealing coat, reduce salt bath Raw and the chance that oxygen in air contacts as far as possible, avoid raw material oxidation; It two is to reduce the evaporation area of salt bath, saves fused salt and reduces and pollute.The residence time of raw material in salt bath refers to and enters salt bath from raw material and start to flow out during this period of time from discharge port with fused salt to raw material, and the object that is controlled to 1.5～4h the residence time is to make Cr
3c
2powder, chromium powder and aluminium powder sufficient reacting.Add the take-off rate of raw material block speed and fused salt just to realize making salt bath liquid level be arranged in the height of neck scope of salt bath furnace burner hearth and make raw material by regulate is simultaneously a kind of mode that 1.5～4h carries out building-up reactions in the residence time of salt bath, can also be the object that 1.5～4h carries out building-up reactions in the residence time of salt bath by controlling respectively that salt bath furnace discharge port place fused salt take-off rate or control add raw material block speed to realize to make salt bath liquid level be arranged in the height of neck scope of salt bath furnace burner hearth and make raw material.
Below preferred embodiment in, the post-treating method of step (e) all adopts ordinary method.Cooling referring to the Cr that contains flowing out from discharge port
2the fused salt mixt of AlC powder forms solids through being cooled to room temperature.Pulverizing refers to pulverizes cooled solids.Washing refers to that water (preferably deionized water) washing pulverizes the material obtaining, and directly removes above liquid or filter out liquid to be above precipitated thing after leaving standstill, and also can not need to leave standstill to be directly precipitated thing by the mode of filtering; The liquid obtaining can reclaim salt through aftertreatment and be reused for preparation mixing salt.Oven dry refers to dries the throw out after washing except anhydrating (can carry out oven drying at low temperature, temperature≤150 DEG C), obtains Cr
2alC powder.
Continuous synthetic Cr provided by the invention
2the technical scheme of AlC powder, has changed prior synthesizing method, has brought following very outstanding technique effect:
1, make salt bath liquid level be positioned at the height of neck scope that salt bath furnace is elongated, can reduce the contact area of salt bath and air, prevent raw material oxidation, also can reduce the volatilization of salt bath simultaneously, conservation is to reduce costs; And this salt bath furnace does not exist because of the fused salt problems such as the contaminated equipment causing of overflowing.
2, salt bath furnace is respectively arranged with charging opening and discharge port, can constantly feed in raw material into aborning until once production end, for continuous kiln, has free of contamination advantage; For cycle stove, there is serialization advantage, be very suitable for suitability for industrialized production.
3, the present invention forms protective layer with activated carbon powder, can under normal pressure, complete building-up reactions, neither needs vacuum and protective atmosphere, does not also need impressed pressure.
4, synthetic Cr
2alC powder purity can meet industrial requirement more than can reaching 95wt%.
5,, because the neck cross section of salt bath furnace is relatively little, fused salt volatilization loss in synthetic is less, can recycle, and does not pollute the environment.
Brief description of the drawings
Fig. 1 is the structural representation of the internal heat type salt bath furnace that provides of embodiment 1.
Fig. 2 is the structural representation of silica tube in the external-heat salt bath furnace that provides of embodiment 2.
Fig. 3 is the synthetic Cr of embodiment 6
2the X-ray diffraction spectrogram of AlC powder.
Fig. 4 is the synthetic Cr of embodiment 7
2the X-ray diffraction spectrogram of AlC powder.
Fig. 5 is the synthetic Cr of embodiment 8
2the X-ray diffraction spectrogram of AlC powder.
In above-mentioned accompanying drawing, the object of each drawing reference numeral mark is respectively: 1-tapered portion; 2-cylindrical portion; 3-back taper portion; 4-neck; 5-charging opening; 6-discharge port; 7-electrode; 8-thermopair; 9-valve; 10-wire.
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The salt bath furnace that this enforcement provides is internal heat type salt bath furnace, and as shown in Figure 1, the burner hearth of this salt bath furnace is built into refractory brick, and burner hearth is followed successively by tapered portion 1, cylindrical portion 2 and back taper portion 3 from top to bottom; Tapered portion 1 top is provided with neck 4; Neck 4 tops are charging opening 5; Back taper portion 3 bottoms are provided with discharge port 6; The sectional area of neck 4 and discharge port 6 is all less than the sectional area of cylindrical portion.Two positions that burner hearth inner side-wall faces are provided with electrode 7 (comprising positive electrode and negative potential); Electrode 7 is by being connected with external power source through the wire 10 of refractory brick.Electrode 7 use are coated with Cr
2the electro-conductive material of AlC is made.In salt bath furnace, be provided with the thermopair 8 inserting in salt bath, for measuring the temperature of salt bath.Discharge port 6 places are provided with valve 9, for regulating the take-off rate of discharging.
Embodiment 2
The salt bath furnace that this enforcement provides is external-heat salt bath furnace, as shown in Figure 2, is made into burner hearth with silica tube; Burner hearth is followed successively by tapered portion 1, cylindrical portion 2 and back taper portion 3 from top to bottom; Tapered portion 1 top is provided with neck 4; Neck 4 tops are charging opening 5; Back taper portion 3 bottoms are provided with discharge port 6; The sectional area of neck 4 and discharge port 6 is all less than the sectional area of cylindrical portion; Discharge port 6 places are provided with valve 9, for regulating discharging take-off rate.Burner hearth is arranged in vertical resistance furnace.The outsourcing from the market of vertical resistance furnace.
Embodiment 3
In the present embodiment, salt bath furnace is built into high alumina brick, and volume is about 15L, and the height of neck is 300mm, and the take-off rate of fused salt is 6L/h, has Cr with surperficial sintering
2the technically pure iron of AlC is made electrode.
According to the synthetic Cr of following steps
2alC powder:
(a) by NaCl, KCl and BaCl
280 DEG C of oven dry; By NaCl20 mass parts, KCl20 mass parts and the BaCl of drying
260 mass parts mix, then obtain mixing salt after adding the activated carbon powder of 3 mass parts again to mix;
(b) by Cr
3c
2powder, chromium powder and the aluminium powder in molar ratio ratio of 1:1:2.6 mix and obtain mixing raw material, and mixing raw material is mixed by the mass ratio of 1:2 again with mixing salt, are pressed into raw material block;
(c) mixing salt is joined in salt bath furnace and melted, be warmed up to 1000 DEG C, continue slowly to add mixing salt, fused salt liquid level is adjusted in neck 4 altitude ranges;
(d) valve 9 at unlatching salt bath furnace bottom discharge mouth 6 places, adjusts fused salt take-off rate to 6L/h, adds raw material block simultaneously, keeps fused salt liquid level to be positioned at neck 4 altitude ranges of salt bath furnace;
(e) after the fused salt cool to room temperature that contains synthetic powder flowing out, pulverize, through washing, standing and filtration, obtain Cr 40 DEG C of oven dry
2alC powder.
The Cr that the present embodiment is synthetic
2alC powder, in its X-ray diffraction spectrogram except Cr
2outside the diffraction peak of AlC, also can be observed Cr
3c
2diffraction peak, purity approaches 95%wt.
Embodiment 4:
In the present embodiment, salt bath furnace is built into high alumina brick, and volume is about 15L, and the height of neck is 300mm, and the take-off rate of fused salt is 6L/h, has Cr with surperficial sintering
2the technically pure iron of AlC is made electrode.
According to the synthetic Cr of following steps
2alC powder:
(a) by NaCl, KCl and BaCl
280 DEG C of oven dry; By NaCl20 mass parts, KCl40 mass parts and the BaCl of drying
240 mass parts mix, then obtain mixing salt after adding the activated carbon powder of 0.5 mass parts again to mix;
(b) by Cr
3c
2powder, chromium powder and the aluminium powder in molar ratio ratio of 1:1:2.2 mix and obtain mixing raw material, and mixing raw material is mixed by the mass ratio of 1:1 again with mixing salt, are pressed into raw material block;
(c) mixing salt is joined in salt bath furnace and melted, be warmed up to 950 DEG C, continue slowly to add mixing salt, fused salt liquid level is adjusted in neck 4 altitude ranges;
(d) valve 9 at unlatching salt bath furnace bottom discharge mouth 6 places, adjusts fused salt take-off rate to 6L/h, adds raw material block simultaneously, keeps fused salt liquid level to be positioned at neck 4 altitude ranges of salt bath furnace;
(e) after the fused salt cool to room temperature that contains synthetic powder flowing out, pulverize, through washing, filtration, obtain Cr 150 DEG C of oven dry
2alC powder.
The Cr that the present embodiment is synthetic
2alC powder, in its X-ray diffraction spectrogram except Cr
2outside the diffraction peak of AlC, also can be observed Cr
3c
2diffraction peak, purity approaches 95%wt.
Embodiment 5:
In the present embodiment, salt bath furnace is built into high alumina brick, and volume is about 15L, and the height of neck is 300mm, and the take-off rate of fused salt is 6L/h, has Cr with surperficial sintering
2the technically pure iron of AlC is made electrode.
According to the synthetic Cr of following steps
2alC powder:
(a) by NaCl, KCl and BaCl
280 DEG C of oven dry; By NaCl40 mass parts, KCl20 mass parts and the BaCl of drying
240 mass parts mix, then obtain mixing salt after adding the activated carbon powder of 2 mass parts again to mix;
(b) by Cr
3c
2powder, chromium powder and the aluminium powder in molar ratio ratio of 1.1:1:2.4 mix and obtain mixing raw material, and mixing raw material is mixed by the mass ratio of 1:1 again with mixing salt, are pressed into raw material block;
(c) mixing salt is joined in salt bath furnace and melted, be warmed up to 950 DEG C, continue slowly to add mixing salt, fused salt liquid level is adjusted in neck 4 altitude ranges;
(d) valve 9 at unlatching salt bath furnace bottom discharge mouth 6 places, adjusts fused salt take-off rate to 6L/h, adds raw material block simultaneously, keeps fused salt liquid level to be positioned at neck 4 altitude ranges of salt bath furnace;
(e) after the fused salt cool to room temperature that contains synthetic powder flowing out, pulverize, after washing, standing removal supernatant liquid, obtain Cr 100 DEG C of oven dry
2alC powder.
The Cr that the present embodiment is synthetic
2alC powder, in its X-ray diffraction spectrogram except Cr
2outside the diffraction peak of AlC, also can be observed Cr
3c
2diffraction peak, purity approaches 95%wt.
Embodiment 6:
In the present embodiment, salt bath furnace is built into high alumina brick, and volume is about 15L, and the height of neck is 300mm, and the take-off rate of fused salt is 6L/h, has Cr with surperficial sintering
2the technically pure iron of AlC is made electrode.
According to the synthetic Cr of following steps
2alC powder:
(a) by NaCl, KCl and BaCl
280 DEG C of oven dry; By NaCl26 mass parts, KCl36 mass parts and the BaCl of drying
238 mass parts mix, then obtain mixing salt after adding the activated carbon powder of 2 mass parts again to mix;
(b) by Cr
3c
2powder, chromium powder and the aluminium powder in molar ratio ratio of 1.04:1:2.4 mix and obtain mixing raw material, and mixing raw material is mixed by the mass ratio of 1:1 again with mixing salt, are pressed into raw material block;
(c) mixing salt is joined in salt bath furnace and melted, be warmed up to 970 DEG C, continue slowly to add mixing salt, fused salt liquid level is adjusted in neck 4 altitude ranges;
(d) valve 9 at unlatching salt bath furnace bottom discharge mouth 6 places, adjusts fused salt take-off rate to 6L/h, adds raw material block simultaneously, keeps fused salt liquid level to be positioned at neck 4 altitude ranges of salt bath furnace;
(e) after the fused salt cool to room temperature that contains synthetic powder flowing out, pulverize, through washing, filtration, obtain Cr 80 DEG C of oven dry
2alC powder.
The Cr that the present embodiment is synthetic
2alC powder, as shown in Figure 3, wherein there is not observable assorted peak in its X-ray diffraction spectrogram, purity is more than 95%wt.
Embodiment 7
In the present embodiment, with silica tube making salt bath furnace burner hearth, stove internal diameter 150mm, equal-diameter part length is about 600mm, and the height of neck is 100mm, and volume is about 11L, and the take-off rate of fused salt is 5L/h.
According to the synthetic Cr of following steps
2alC powder:
(1) by NaCl, KCl and BaCl
280 DEG C of oven dry; By NaCl30 mass parts, KCl30 mass parts and the BaCl of drying
240 mass parts mix, then obtain mixing salt after adding the activated carbon powder of 1 mass parts again to mix;
(3) by Cr
3c
2powder, chromium powder and the aluminium powder in molar ratio ratio of 1:1:2.4 mix and obtain mixing raw material, and mixing raw material is mixed by the mass ratio of 1:1.5 again with mixing salt, are pressed into raw material block;
(4) mixing salt is joined in salt bath furnace and melted, be warmed up to 970 DEG C, continue slowly to add mixing salt, fused salt liquid level is adjusted in neck 4 altitude ranges;
(5) valve 9 at unlatching salt bath furnace bottom discharge mouth 6 places, adjusts fused salt take-off rate to 5L/h, adds raw material block simultaneously, keeps fused salt liquid level to be positioned at neck 4 altitude ranges of salt bath furnace;
(6) after the fused salt cool to room temperature that contains synthetic powder flowing out, pulverize, through washing, filtration, obtain Cr 80 DEG C of oven dry
2alC powder.
The Cr that the present embodiment is synthetic
2the X-ray diffraction spectrogram of AlC powder as shown in Figure 4.Wherein do not occur observable assorted peak, purity is more than 95%wt.
Embodiment 8
In the present embodiment, salt bath furnace is built into silica brick, and volume is about 20L, and the height of neck is 500mm, and the take-off rate of fused salt is 7L/h, has Cr with surface spraying
2the red copper of AlC is done electrode.
According to the synthetic Cr of following steps
2alC powder:
(a) by NaCl, KCl and BaCl
280 DEG C of oven dry; By NaCl20 mass parts, KCl40 mass parts and the BaCl of drying
240 mass parts mix, and obtain mixing salt after adding the activated carbon powder of 3 mass parts again to mix;
(b) by Cr
3c
2powder, chromium powder and the aluminium powder in molar ratio ratio of 1.08:1:2.5 mix and obtain mixing raw material, and mixing raw material is mixed by the mass ratio of 1:2 again with mixing salt, are pressed into raw material block;
(c) mixing salt is joined in salt bath furnace and melted, be warmed up to 970 DEG C, continue slowly to add mixing salt, fused salt liquid level is adjusted in neck 4 altitude ranges;
(d) valve 9 at unlatching salt bath furnace bottom discharge mouth 6 places, adjusts fused salt take-off rate to 7L/h, adds raw material block simultaneously, keeps fused salt liquid level to be positioned at neck 4 altitude ranges of salt bath furnace;
(e) after the fused salt cool to room temperature that contains synthetic powder flowing out, pulverize, through washing, standing and filtration, obtain Cr 80 DEG C of oven dry
2alC powder.
The Cr that the present embodiment is synthetic
2alC powder, as shown in Figure 5, wherein there is not observable assorted peak in its X-ray diffraction spectrogram, purity is more than 95%wt.
Claims (10)
1. a continuously synthetic Cr
2the salt bath furnace of AlC powder, is characterized in that, the burner hearth of described salt bath furnace is followed successively by tapered portion (1), cylindrical portion (2) and back taper portion (3) from top to bottom; Described tapered portion (1) top is provided with neck (4); Described neck (4) top is charging opening (5); Described back taper portion (3) bottom is provided with discharge port (6); The sectional area of described neck (4) and described discharge port (6) is all less than the sectional area of described cylindrical portion (2).
2. continuously synthetic Cr according to claim 1
2the salt bath furnace of AlC powder, is characterized in that, the burner hearth of described salt bath furnace is built into refractory brick, and two corresponding positions of burner hearth inner side-wall are provided with two electrodes (7).
3. continuously synthetic Cr according to claim 2
2the salt bath furnace of AlC powder, is characterized in that, described electrode (7) is used Cr
2alC or be coated with Cr
2the electro-conductive material of AlC is made.
4. according to the continuously synthetic Cr described in claim 2 or 3
2the salt bath furnace of AlC powder, is characterized in that, described discharge port (6) is provided with valve (9), for regulating the take-off rate of discharging.
5. continuously synthetic Cr according to claim 1
2the salt bath furnace of AlC powder, is characterized in that, the burner hearth of described salt bath furnace is made of silica tube; Described burner hearth is arranged in vertical resistance furnace.
6. continuously synthetic Cr according to claim 5
2the salt bath furnace of AlC powder, is characterized in that, described discharge port (6) is provided with valve (9), for regulating the take-off rate of discharging.
7. according to claim 1,2,3,5,6 arbitrary described continuously synthetic Cr
2the salt bath furnace of AlC powder, is characterized in that, the height of described neck is 100～500mm.
8. continuously synthetic Cr according to claim 4
2the salt bath furnace of AlC powder, is characterized in that, the height of described neck is 100～500mm.
9. one kind is utilized the arbitrary described continuously synthetic Cr of claim 1-8
2the synthetic Cr of salt bath furnace of AlC powder
2the method of AlC powder, is characterized in that, with Cr
3c
2powder, chromium powder and aluminium powder are raw material, according to conventional ratio, are containing the NaCl of activated carbon powder, KCl and BaCl
2mixed salt-bath at conventional temperature, carry out the synthetic and conventional processing of conventional salt bath reaction and obtain Cr
2alC powder; In described salt bath, the mass parts of each material is: NaCl20～40 part, KCl20～40 part, BaCl
240～60 parts, 0.5～3 part of activated carbon powder.
10. continuously synthetic Cr according to claim 9
2the method of AlC powder, is characterized in that, comprises the following steps:
(a) preparation mixing salt
:by NaCl, KCl and BaCl
2after drying, mix and be mixed with mixing salt according to aforementioned proportion with activated carbon powder;
(b) raw materials piece
:by Cr
3c
2powder, chromium powder and aluminium powder are according to mol ratio (1～1.1): 1:(2.2～2.6) preparation raw material, then by described raw material by raw material and mixing salt mass ratio 1:(1～2) mix in joining mixing salt, and be pressed into raw material block;
(c) prepare salt bath
:mixing salt is joined in salt bath furnace, be warmed up to 950～1000 DEG C, form salt bath, and make salt bath liquid level in salt bath furnace be positioned at described neck (4) altitude range;
(d) building-up reactions
:described raw material block is joined in described salt bath, control adds the speed of described raw material block and described discharge port (6) to locate the take-off rate of fused salt, making the residence time of raw material in salt bath is 1.5～4h to carry out building-up reactions, makes salt bath liquid level be positioned at all the time described neck (4) altitude range simultaneously;
(e) aftertreatment: allow from the Cr that contains of described discharge port (6) outflow
2the fused salt mixt of AlC powder is cooling, then through pulverizing, wash, leave standstill and/or filter, drying, obtains Cr
2alC powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410379999.5A CN104192905B (en) | 2014-08-04 | 2014-08-04 | Continuous synthesis Cr 2the salt bath furnace of AlC powder and synthetic method |
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|---|---|---|---|
| CN201410379999.5A CN104192905B (en) | 2014-08-04 | 2014-08-04 | Continuous synthesis Cr 2the salt bath furnace of AlC powder and synthetic method |
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|---|---|
| CN104192905A true CN104192905A (en) | 2014-12-10 |
| CN104192905B CN104192905B (en) | 2015-08-12 |
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| CN201410379999.5A Expired - Fee Related CN104192905B (en) | 2014-08-04 | 2014-08-04 | Continuous synthesis Cr 2the salt bath furnace of AlC powder and synthetic method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010307A (en) * | 2020-08-20 | 2020-12-01 | 电子科技大学 | Cr (chromium)2Application method of AlC material |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86203814U (en) * | 1986-06-07 | 1987-05-20 | 机械工业部兰州石油机械研究所 | Electrode-changeable directly started salt bath furnace |
| JPH06279983A (en) * | 1993-03-29 | 1994-10-04 | Honda Motor Co Ltd | Molten salt bath furnace |
| EP0919642A2 (en) * | 1997-11-28 | 1999-06-02 | Maizuru Corporation | Method for treating surface of ferrous material and salt bath furnace used therefor |
| CN101448760A (en) * | 2006-05-30 | 2009-06-03 | 原子能委员会 | MAX-phase powders and method for making same |
| CN103789594A (en) * | 2014-02-17 | 2014-05-14 | 武汉科技大学 | Method for preparing AlCr2C material based on induction furnace melting |
| CN103866097A (en) * | 2012-12-13 | 2014-06-18 | 江苏华东炉业有限公司 | Embedded-type electrode salt-bath furnace |
-
2014
- 2014-08-04 CN CN201410379999.5A patent/CN104192905B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86203814U (en) * | 1986-06-07 | 1987-05-20 | 机械工业部兰州石油机械研究所 | Electrode-changeable directly started salt bath furnace |
| JPH06279983A (en) * | 1993-03-29 | 1994-10-04 | Honda Motor Co Ltd | Molten salt bath furnace |
| EP0919642A2 (en) * | 1997-11-28 | 1999-06-02 | Maizuru Corporation | Method for treating surface of ferrous material and salt bath furnace used therefor |
| CN101448760A (en) * | 2006-05-30 | 2009-06-03 | 原子能委员会 | MAX-phase powders and method for making same |
| CN103866097A (en) * | 2012-12-13 | 2014-06-18 | 江苏华东炉业有限公司 | Embedded-type electrode salt-bath furnace |
| CN103789594A (en) * | 2014-02-17 | 2014-05-14 | 武汉科技大学 | Method for preparing AlCr2C material based on induction furnace melting |
Non-Patent Citations (2)
| Title |
|---|
| 陈辉等: ""外热式坩埚盐浴炉的设计与改进"", 《沈阳建筑大学学报（自然科学版）》 * |
| 雷宇等: ""三元层状陶瓷材料Cr2 A1C的研究进展"", 《西华大学学报（自然科学版）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010307A (en) * | 2020-08-20 | 2020-12-01 | 电子科技大学 | Cr (chromium)2Application method of AlC material |
| CN112010307B (en) * | 2020-08-20 | 2022-07-26 | 电子科技大学 | Cr (chromium) 2 Application method of AlC material |
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| CN104192905B (en) | 2015-08-12 |
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