CN104192905B - Continuous synthesis Cr 2the salt bath furnace of AlC powder and synthetic method - Google Patents
Continuous synthesis Cr 2the salt bath furnace of AlC powder and synthetic method Download PDFInfo
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- CN104192905B CN104192905B CN201410379999.5A CN201410379999A CN104192905B CN 104192905 B CN104192905 B CN 104192905B CN 201410379999 A CN201410379999 A CN 201410379999A CN 104192905 B CN104192905 B CN 104192905B
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Abstract
The invention discloses a kind of continuous synthesis Cr
2the salt bath furnace of AlC powder and synthetic method, this salt bath furnace has elongated neck, makes salt bath liquid level be positioned at the elongated the height of neck scope of salt bath furnace, the contact area of salt bath and air can be reduced, prevent material oxidation, also can reduce the volatilization of salt bath, conservation is to reduce costs simultaneously; And there is not the problems such as the contaminated equipment caused because of fused salt effusion in this salt bath furnace; Salt bath furnace is respectively arranged with charging opening and discharge port, can constantly feed in raw material into until once produce end aborning; Form protective layer with activated carbon powder, building-up reactions can be completed at ambient pressure, neither need vacuum and protective atmosphere, also do not need impressed pressure; The Cr of preparation
2alC powder purity can reach more than 95wt%; Because the neck cross section of salt bath furnace is relatively little, fused salt volatilization loss in synthesis is less, can recycle and not pollute the environment.
Description
Technical field
The invention belongs to field of material synthesis technology, relate to a kind of salt bath process that adopts and synthesize Cr
2the Apparatus and method for of AlC powder, is specifically related to a kind of continuous synthesis 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 metallic bond again.Cr
2alC not only has the over-all properties of metal and pottery, i.e. high heat conduction, high connductivity, the performance such as anti-oxidant, wear-resistant, also have good self-lubricating property because of the laminate structure of its uniqueness.Have broad application prospects at industrial circles such as space flight and aviation, petrochemical complex, electronic information.
Cr
2the primary synthetic methods 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 synthesize the very high Cr of purity above
2alC material, but equipment is all costly, and production efficiency is lower, is not easy to suitability for industrialized production.
Molten-salt growth method is with chromium powder, aluminium powder, carbon dust for raw material, KCl and NaCl is auxiliary agent, and its Homogeneous phase mixing is pressed into bulk, carries out under vacuum or under protective atmosphere condition in 900 ~ 1200 DEG C, then obtains Cr through pulverizing, washing
2alC powder.Obviously, under vacuum, need the Special Equipment providing vacuum, this synthetic method is still unfavorable for a large amount of production, too increases cost simultaneously.Synthesize 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 effusion, 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 continuous kiln two kinds.If the cycle of employing stove is produced, then energy consumption is higher, if adopt continuous kiln to produce, then the fused salt volatilized can be overflowed crucible and pollute burner hearth, also needs consumption crucible material simultaneously, greatly improves production cost.
In sum, existing synthesis 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 continuous synthesis Cr
2the salt bath furnace of AlC powder and synthetic method, can synthesize the high Cr of purity efficiently
2alC powder.
Summary of the invention
Object of the present invention aims to provide a kind of continuous synthesis Cr
2the salt bath furnace of AlC powder, equipment is simple, easy to operate, almost pollution-free, can realize Cr
2the continuous prodution of AlC powder.
Another object of the present invention is to provide one and utilizes above-mentioned salt bath furnace continuous synthesis Cr
2the method of AlC powder, can realize Cr
2the continuous prodution of AlC powder, and preparation technology is simple, cost is low, is conducive to Cr
2applying of AlC material.
Above-mentioned purpose of the present invention, can be realized by the salt bath furnace that provided by following technical proposals and method.
The invention provides a kind of continuous synthesis 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; It is charging opening above neck; Bottom, back taper portion 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, prevent material oxidation, also can reduce the volatilization of salt bath simultaneously, save raw material, decrease pollution.
Salt bath furnace structure provided by the invention can be realized by following two kinds of modes:
(1) salt bath furnace can be internal heat type salt bath furnace, and burner hearth refractory brick is built into, and burner hearth inner side-wall two corresponding position is provided with electrode (comprising positive electrode and negative potential); Electrode is connected with external power source by the wire through refractory brick.In order to not affect Cr
2alC powder purity, the most handy Cr of electrode
2alC or be coated with Cr
2the electro-conductive material of AlC makes.Further, in order to well control the temperature of salt bath in salt bath furnace, can 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, valve can be set at discharge port.
(2) salt bath furnace also can be external-heat salt bath furnace, and burner hearth silica tube makes; Burner hearth is arranged in vertical resistance furnace.Vertical resistance furnace can outsourcing from the market.Further, in order to control the take-off rate of fused salt, valve can be set at discharge port.
Salt bath furnace provided by the invention, the height of neck refers to the height from neck bottom (i.e. tapered portion top) to neck top (namely bottom charging opening), the height of neck is preferably 100 ~ 500mm, when height is lower than 100mm, effectively can not control the effusion of fused salt; And neck is too high, the utilization ratio of neck not only can be made to reduce, and the manufacturing cost of equipment can be increased.
Based on above continuous synthesis Cr
2the salt bath furnace of AlC powder, the invention provides a kind of continuous synthesis Cr
2the method of AlC powder, with Cr
3c
2powder, chromium powder and aluminium powder are raw material, conveniently ratio, at NaCl, KCl and BaCl containing activated carbon powder
2mixed salt-bath under ordinary temperature, carry out conventional salt bath Reactive Synthesis and conventional processing obtains Cr
2alC powder; In salt bath, the mass parts of each material is: NaCl20 ~ 40 part, KCl20 ~ 40 part, BaCl
240 ~ 60 parts, activated carbon powder 0.5 ~ 3 part.
In above synthetic method, the present inventor finds through large quantity research, with NaCl, KCl, BaCl
2be salt bath prepared by raw material with activated carbon powder, activated carbon powder is little due to density, is positioned at the upper strata of salt bath, can prevent the raw material in salt bath and the oxygen reaction in air as protective layer; 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, play the effect of extraordinary isolation oxygen, ensure the purity of final product at neck place.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, needing in process of production constantly to consume gas, causes cost higher.Even if 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 when 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 conveniently ratio can carry out proportioning, at conventional Cr
3c
2conveniently salt bath Reactive Synthesis Cr under powder, chromium powder and aluminium powder synthesis temperature
2alC, the later stage conventional treatment method then through salt bath obtains Cr
2alC powder.As one preferred embodiment, continuous synthesis Cr provided by the invention
2the method of AlC powder comprises the following steps:
A () preparation mixing salt, by NaCl, KCl and BaCl
2mix with activated carbon powder after drying and be mixed with mixing salt; The mass parts of above-mentioned material is: NaCl20 ~ 40 part, KCl20 ~ 40 part, BaCl
240 ~ 60 parts, activated carbon powder 0.5 ~ 3 part;
B () raw materials block, 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) join mixing salt in mix, and be pressed into raw material block;
C () prepares salt bath, joined by mixing salt in salt bath furnace, is warmed up to 950 ~ 1000 DEG C, forms salt bath, and makes 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 to add the speed of raw material block and the take-off rate of salt bath furnace discharge outlet 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 the height of neck scope of salt bath furnace all the time simultaneously;
(e) aftertreatment: allow from discharge port flow out containing Cr
2the fused salt mixt cooling of AlC powder, then through pulverizing, washing, leave standstill and/or filter, dry, namely obtain Cr
2alC powder.
Below preferred embodiment in, step (a) prepare mixing salt a part for forming salt bath in advance in salt bath furnace; 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, first raw material dispersion, can disperse quickly and be dissolved in fused salt after making raw material enter salt bath; It two is adding raw material while, is convenient to supplement fused salt and activated carbon in proportion, to ensure that building-up process can be carried out continuously.
Below preferred embodiment in, step (d) makes salt bath liquid level remain in salt bath furnace slender neck altitude range, its object has two, the first makes the activated carbon floated in salt bath collect in neck, form thicker sealing coat, reduce the chance that salt bath Raw contacts with oxygen in air as far as possible, avoid material oxidation; It two is reduce the evaporation area of salt bath, saves fused salt and decreasing pollution.The residence time of raw material in salt bath refers to flows out during this period of time from discharge port to raw material with fused salt from raw material enters salt bath, is controlled the residence time to be to make Cr in the object of 1.5 ~ 4h
3c
2powder, chromium powder and aluminium powder sufficient reacting.By regulating the take-off rate adding raw material block speed and fused salt just 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 be a kind of mode that 1.5 ~ 4h carries out building-up reactions in the residence time of salt bath simultaneously, raw material block speed can also be added realize and make salt bath liquid level be arranged in the height of neck scope of salt bath furnace burner hearth and make raw material be the object that 1.5 ~ 4h carries out building-up reactions in the residence time of salt bath by controlling salt bath furnace discharge outlet fused salt take-off rate or control respectively.
Below preferred embodiment in, the post-treating method of step (e) all adopts ordinary method.Cooling refers to and contains Cr by what flow 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 the material that obtains is pulverized in water (preferred deionized water) washing, directly removes liquid or filter out liquid above and be precipitated thing above after leaving standstill, and also can not need to leave standstill directly to be precipitated thing by the mode of filtration; The liquid obtained can reclaim salt through aftertreatment and be reused for preparation mixing salt.Dry and refer to that the throw out after by washing is dried except anhydrate (can carry out oven drying at low temperature, temperature≤150 DEG C), namely obtain Cr
2alC powder.
Continuous synthesis Cr provided by the invention
2the technical scheme of AlC powder, changes prior synthesizing method, brings following very outstanding technique effect:
1, make salt bath liquid level be positioned at the elongated the height of neck scope of salt bath furnace, can reduce the contact area of salt bath and air, prevent material oxidation, also can reduce the volatilization of salt bath, conservation is to reduce costs simultaneously; And there is not the problems such as the contaminated equipment caused because of fused salt effusion in this salt bath furnace.
2, salt bath furnace is respectively arranged with charging opening and discharge port, can constantly feed in raw material into until once produce end aborning, 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 complete building-up reactions at ambient pressure, neither needs vacuum and protective atmosphere, does not also need impressed pressure.
4, the Cr of synthesis
2alC powder purity can reach more than 95wt%, can meet industrial requirement.
5, the neck cross section due to salt bath furnace is relatively little, and fused salt volatilization loss in synthesis is less, can recycle, not pollute the environment.
Accompanying drawing explanation
Fig. 1 is the structural representation of the internal heat type salt bath furnace that embodiment 1 provides.
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 Cr that embodiment 6 is synthesized
2the X-ray diffraction spectrogram of AlC powder.
Fig. 4 is the Cr that embodiment 7 is synthesized
2the X-ray diffraction spectrogram of AlC powder.
Fig. 5 is the Cr that embodiment 8 is synthesized
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 clearly, 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 refractory brick of this salt bath furnace is built into, 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; It is charging opening 5 above neck 4; Bottom, back taper portion 3 is 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 connected with external power source by the wire 10 through refractory brick.Electrode 7 is with being coated with Cr
2the electro-conductive material of AlC makes.The thermopair 8 inserted in salt bath is provided with, for measuring the temperature of salt bath in salt bath furnace.Discharge port 6 place is 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; It is charging opening 5 above neck 4; Bottom, back taper portion 3 is 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 place is provided with valve 9, for adjusting material take-off rate.Burner hearth is arranged in vertical resistance furnace.Vertical resistance furnace can outsourcing from the market.
Embodiment 3
In the present embodiment, salt bath furnace high alumina brick is built into, 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 surface sintering
2electrode made by the technically pure iron of AlC.
According to following steps synthesis Cr
2alC powder:
A () is 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 the activated carbon powder adding 3 mass parts again mix after obtain mixing salt;
B () is 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, again mixed by mixing raw material, be pressed into raw material block with the mass ratio of mixing salt by 1:2;
C mixing salt joins in salt bath furnace and melts by (), be warmed up to 1000 DEG C, continues slowly to add mixing salt, is adjusted to by fused salt liquid level in neck 4 altitude range;
D () opens the valve 9 at salt bath furnace bottom discharge mouth 6 place, adjustment 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 range of salt bath furnace;
(e) wait flow out containing synthetic powder fused salt cool to room temperature after pulverize, through washing, leave standstill and filter, obtain Cr 40 DEG C of oven dry
2alC powder.
The Cr of the present embodiment synthesis
2alC powder, except Cr in its X-ray diffraction spectrogram
2outside the diffraction peak of AlC, also can be observed Cr
3c
2diffraction peak, purity is close to 95%wt.
Embodiment 4:
In the present embodiment, salt bath furnace high alumina brick is built into, 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 surface sintering
2electrode made by the technically pure iron of AlC.
According to following steps synthesis Cr
2alC powder:
A () is 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 the activated carbon powder adding 0.5 mass parts again mix after obtain mixing salt;
B () is 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, again mixed by mixing raw material, be pressed into raw material block with the mass ratio of mixing salt by 1:1;
C mixing salt joins in salt bath furnace and melts by (), be warmed up to 950 DEG C, continues slowly to add mixing salt, is adjusted to by fused salt liquid level in neck 4 altitude range;
D () opens the valve 9 at salt bath furnace bottom discharge mouth 6 place, adjustment 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 range of salt bath furnace;
(e) wait flow out containing synthetic powder fused salt cool to room temperature after pulverize, through washing, filter, obtain Cr 150 DEG C of oven dry
2alC powder.
The Cr of the present embodiment synthesis
2alC powder, except Cr in its X-ray diffraction spectrogram
2outside the diffraction peak of AlC, also can be observed Cr
3c
2diffraction peak, purity is close to 95%wt.
Embodiment 5:
In the present embodiment, salt bath furnace high alumina brick is built into, 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 surface sintering
2electrode made by the technically pure iron of AlC.
According to following steps synthesis Cr
2alC powder:
A () is 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 the activated carbon powder adding 2 mass parts again mix after obtain mixing salt;
B () is 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, again mixed by mixing raw material, be pressed into raw material block with the mass ratio of mixing salt by 1:1;
C mixing salt joins in salt bath furnace and melts by (), be warmed up to 950 DEG C, continues slowly to add mixing salt, is adjusted to by fused salt liquid level in neck 4 altitude range;
D () opens the valve 9 at salt bath furnace bottom discharge mouth 6 place, adjustment 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 range of salt bath furnace;
(e) wait flow out containing the fused salt cool to room temperature of synthetic powder after pulverize, through washing, leave standstill to remove after supernatant liquid and obtain Cr 100 DEG C of oven dry
2alC powder.
The Cr of the present embodiment synthesis
2alC powder, except Cr in its X-ray diffraction spectrogram
2outside the diffraction peak of AlC, also can be observed Cr
3c
2diffraction peak, purity is close to 95%wt.
Embodiment 6:
In the present embodiment, salt bath furnace high alumina brick is built into, 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 surface sintering
2electrode made by the technically pure iron of AlC.
According to following steps synthesis Cr
2alC powder:
A () is 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 the activated carbon powder adding 2 mass parts again mix after obtain mixing salt;
B () is 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, again mixed by mixing raw material, be pressed into raw material block with the mass ratio of mixing salt by 1:1;
C mixing salt joins in salt bath furnace and melts by (), be warmed up to 970 DEG C, continues slowly to add mixing salt, is adjusted to by fused salt liquid level in neck 4 altitude range;
D () opens the valve 9 at salt bath furnace bottom discharge mouth 6 place, adjustment 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 range of salt bath furnace;
(e) wait flow out containing synthetic powder fused salt cool to room temperature after pulverize, through washing, filter, obtain Cr 80 DEG C of oven dry
2alC powder.
The Cr of the present embodiment synthesis
2alC powder, as shown in Figure 3, wherein do not occur observable assorted peak, purity is at more than 95%wt for its X-ray diffraction spectrogram.
Embodiment 7
In the present embodiment, make salt bath furnace burner hearth with silica tube, 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 following steps synthesis Cr
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 the activated carbon powder adding 1 mass parts again mix after obtain mixing salt;
(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, again mixed by mixing raw material, be pressed into raw material block with the mass ratio of mixing salt by 1:1.5;
(4) mixing salt is joined in salt bath furnace melt, be warmed up to 970 DEG C, continue slowly to add mixing salt, fused salt liquid level is adjusted in neck 4 altitude range;
(5) open the valve 9 at salt bath furnace bottom discharge mouth 6 place, adjustment 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 range of salt bath furnace;
(6) wait flow out containing synthetic powder fused salt cool to room temperature after pulverize, through washing, filter, obtain Cr 80 DEG C of oven dry
2alC powder.
The Cr of the present embodiment synthesis
2the X-ray diffraction spectrogram of AlC powder as shown in Figure 4.Wherein do not occur observable assorted peak, purity is at more than 95%wt.
Embodiment 8
In the present embodiment, salt bath furnace silica brick is built into, 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 does electrode.
According to following steps synthesis Cr
2alC powder:
A () is 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 the activated carbon powder adding 3 mass parts mixes again;
B () is 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, again mixed by mixing raw material, be pressed into raw material block with the mass ratio of mixing salt by 1:2;
C mixing salt joins in salt bath furnace and melts by (), be warmed up to 970 DEG C, continues slowly to add mixing salt, is adjusted to by fused salt liquid level in neck 4 altitude range;
D () opens the valve 9 at salt bath furnace bottom discharge mouth 6 place, adjustment 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 range of salt bath furnace;
(e) wait flow out containing synthetic powder fused salt cool to room temperature after pulverize, through washing, leave standstill and filter, obtain Cr 80 DEG C of oven dry
2alC powder.
The Cr of the present embodiment synthesis
2alC powder, as shown in Figure 5, wherein do not occur observable assorted peak, purity is at more than 95%wt for its X-ray diffraction spectrogram.
Claims (9)
1. a continuous synthesis 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. continuous synthesis Cr according to claim 1
2the salt bath furnace of AlC powder, is characterized in that, the burner hearth refractory brick of described salt bath furnace is built into, and corresponding two positions of burner hearth inner side-wall are provided with two electrodes (7).
3. continuous synthesis Cr according to claim 2
2the salt bath furnace of AlC powder, is characterized in that, described electrode (7) uses Cr
2alC or be coated with Cr
2the electro-conductive material of AlC makes.
4. the continuous synthesis Cr according to Claims 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. continuous synthesis Cr according to claim 1
2the salt bath furnace of AlC powder, is characterized in that, the burner hearth silica tube of described salt bath furnace makes; Described burner hearth is arranged in vertical resistance furnace.
6. continuous synthesis 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 the arbitrary described continuous synthesis Cr of claim 1,2,3,5,6
2the salt bath furnace of AlC powder, is characterized in that, the height of described neck is 100 ~ 500mm.
8. continuous synthesis 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 utilizes the arbitrary described continuous synthesis Cr of claim 1-8
2the salt bath furnace synthesis Cr of AlC powder
2the method of AlC powder, is characterized in that, comprises the following steps:
(a) preparation mixing salt: by NaCl, KCl and BaCl
2mix with activated carbon powder after drying and be mixed with mixing salt; The mass parts of above-mentioned material is: NaCl 20 ~ 40 parts, KCl 20 ~ 40 parts, BaCl
240 ~ 60 parts, activated carbon powder 0.5 ~ 3 part;
(b) raw materials block: 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) join mixing salt in mix, and be pressed into raw material block;
C () prepares salt bath: joined by mixing salt in salt bath furnace, is warmed up to 950 ~ 1000 DEG C, forms salt bath, and makes 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 to add the speed of described raw material block and the take-off rate of described discharge port (6) 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 described neck (4) altitude range all the time simultaneously;
(e) aftertreatment: allow from described discharge port (6) flow out containing Cr
2the fused salt mixt cooling of AlC powder, then through pulverizing, washing, leave standstill and/or filter, dry, namely obtain Cr
2alC powder.
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| 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06279983A (en) * | 1993-03-29 | 1994-10-04 | Honda Motor Co Ltd | Molten salt bath furnace |
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2014
- 2014-08-04 CN CN201410379999.5A patent/CN104192905B/en not_active Expired - Fee Related
Patent Citations (5)
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| 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 |
| 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 |
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| 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)》.2013,第29卷(第5期),第907-912页. * |
| 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)》.2013,第32卷(第1期),第77-81页. * |
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| CN104192905A (en) | 2014-12-10 |
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