CN107555998A - High-purity Fe2AlB2The preparation method of ceramic powder and compact block - Google Patents
High-purity Fe2AlB2The preparation method of ceramic powder and compact block Download PDFInfo
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Abstract
The invention discloses high-purity Fe2AlB2The preparation method of powder and compact block.Prepare high-purity Fe2AlB2The method of powder is：Using FeB powder and Al powder as raw material, by FeB：Al=2：The molar ratio ingredient of (1.1~1.5), after dry-mixed 5~24 hours, by batch mixing on tablet press machine pressed compact, base substrate is put into the graphite jig in non-press stove, argon gas atmosphere, furnace temperature is risen to 1000~1200 DEG C with 10~50 DEG C/min speed, 10~120min is incubated, obtains high-purity Fe2AlB2Material.By Fe2AlB2Material crushed the sieve of different meshes in ball mill, and the Fe of different-grain diameter can be made2AlB2Powder.Prepare high-purity Fe2AlB2The method of compact block is：According to " preparation high-purity Fe2AlB2After dispensing described in the method for powder " carries out batch mixing, batch mixing is put into the graphite jig in hot pressing furnace, argon gas atmosphere, furnace temperature is risen to 1000~1200 DEG C with 10~50 DEG C/min speed, pressurize 10 40MPa, is incubated 10~120min, obtains high-purity Fe2AlB2Compact block material.The present invention prepares Fe2AlB2Material time is short, purity is high, cost is low.It is suitable for prepare other MAB materials.
Description
Technical field
The invention belongs to the preparation field of ceramic material, specially Fe2AlB2The synthesis side of ceramic powder and compact block
Method.
Background technology
(formula is " MAB " to novel tertiary transition metal boride, and wherein M is transition metal, and A is aluminium element or zinc
Element, B are boron elements.) received much attention because with nanometer laminated structure and having the excellent properties of metal and ceramic material concurrently.
" MAB " mutually mainly includes Cr4AlB6, Cr3AlB4, Fe2AlB2, Cr2AlB2, Mn2AlB2, Ru2ZnB2, the compound such as MoAlB, WAlB
(document 1, Inorg.Chem.54 (2015) 6122；Document 2, J.Solid State Chem.224 (2015) 52.).Fe2AlB2
It is a kind of distinctive material in " MAB " material family, it has good electric conductivity, thermal conductivity, high damage tolerance and is easy to
Processing etc. excellent properties, especially it there is excellent magnetothermal effect, can be as the critical material of high magnetothermal effect refrigeration plant.
But single-phase Fe2AlB2Materials synthesis is difficult, often contains impurities phase in synthetic material.Both at home and abroad in high-purity
Fe2AlB2Synthesis in terms of also without Patents report, which greatly limits Fe2AlB2The scale metaplasia of material
Production and the application in engineering field.Synthesis Fe at present2AlB2Material mainly adds the method for annealing using electric arc melting.
Document 3 (J.Alloys Compd.650 (2015) 482.) reports that, with Al powder, Fe powder and B powder are raw material, by Al：Fe：B=
1.5：2：2 mol ratio carries out electric arc melting, and the sample after melting carries out annealing 14 days in 1400 DEG C in a vacuum furnace,
Obtain Fe2AlB2Material.Document 4 (J.Solid State Chem.224 (2015) 52.) reports that, with Al powder, Fe powder and B powder are
Raw material, by Al：Fe：B=3：2：2 molar ratio ingredient, the base substrate by dispensing pressure for diameter 10mm, base substrate enter in argon atmosphere
Row electric arc melting, the sample after melting is placed in vacuum-packed quartz glass tube, is incubated 7 days at 900 DEG C, obtains Fe2AlB2
Material, but the purity of material is not high, contains a certain amount of ferroaluminium phase.
Above-mentioned synthesis Fe2AlB2Generated time length, preparation technology complexity, time consumption and energy consumption, efficiency be present in the method for ceramic material
The problems such as impurities phase in low, synthetic material be present, therefore shorten preparation time, improve the purity of sample, for promoting Fe2AlB2
The large-scale production tool of material is of great significance.
The content of the invention
The present invention provides high-purity Fe2AlB2The synthetic method of ceramic powder and compact block, solve to prepare at present
Fe2AlB2The problems of material.The Fe of synthesis2AlB2Powder, it can be raw material with it, prepare various composites and device.
The Fe of preparation2AlB2Compact block, it can be used to test its various performance, also can directly be processed into variously-shaped device.
Normal pressure and hot pressing synthetic technology is respectively adopted in the present invention, by the use of FeB and Al as dispensing, in a short time, it is low into
This synthesis high-purity Fe2AlB2Ceramic powder and compact block.
The technical scheme is that：
1. atmospheric synthesis high-purity Fe2AlB2The method of ceramic powder, it is characterised in that：
(1) using FeB powder and Al powder as raw material, by FeB：Al=2：The molar ratio ingredient of (1.1~1.5).
(2) by above-mentioned dispensing and agate ball by ball and the weight ratio 2 of material：1 is put into ball grinder, is done on tumbling ball mill
It is mixed 5~24 hours, well mixed dispensing is put into stainless steel mould on tablet press machine and carries out pressed compact.
(3) above-mentioned base substrate is put into graphite jig, graphite jig is placed in non-press stove, under argon gas atmosphere, with 10~
Furnace temperature is risen to 1000~1200 DEG C by 50 DEG C/min speed, is incubated 10~120min, is then down to room temperature, obtains high-purity
Fe2AlB2Material.
(4) by above-mentioned Fe2AlB2Material crushes in ball mill, crosses the sieve of different meshes, different-grain diameter can be made
Fe2AlB2Powder.
2. hot pressing synthesis high-purity Fe2AlB2The method of compact block, it is characterised in that：
(1) using FeB powder and Al powder as raw material, by FeB：Al=2：The molar ratio ingredient of (1.1~1.5).
(2) by above-mentioned dispensing and agate ball by ball and the weight ratio 2 of material：1 is put into ball grinder, is done on tumbling ball mill
It is mixed 5~24 hours.
(3) well mixed dispensing is put into graphite jig, graphite jig is placed in hot pressing furnace, under argon gas atmosphere,
Furnace temperature is risen to 1000~1200 DEG C with 10~50 DEG C/min speed, pressurize 10-40MPa, is incubated 10~120min, then drops
To room temperature, high-purity densification Fe is obtained2AlB2Block materials.
The compared to the prior art possessed beneficial effect of the present invention is：
(1) present invention is according to FeB：Al=2:1.1 molar ratio ingredient, synthesize the Fe of phase homogenous quantities2AlB2Material, and
Some formulas compare (such as Al：Fe：B=1.5~3：2：2), reduce the content of raw material powder, reduce cost.
(2) according to Fe, Al and B powders synthesis Fe2AlB2, course of reaction is complicated, and interphase is difficult to control.As Fe and B are anti-
FeB, Fe and Al reaction generation Fe-Al compounds should be generated, then again by FeB and Fe-Al compounds reaction generation Fe2AlB2.This
Invention uses FeB and Al powder, as long as reaching temperature, FeB just directly reacts generation Fe with Al2AlB2, reduce Fe-B reaction
Journey and step, accelerate Fe2AlB2Aggregate velocity.
(3) Fe, Al and B powder synthesis Fe are used2AlB2When, Fe powder is easily formed in storage and mixing process with oxygen in air
Oxide, so as to influence the purity of synthetic sample, and the price of high-purity B powder is sufficiently expensive.The present invention uses FeB and Al powder,
FeB avoids the oxidizable adverse effect brought of Fe powder as raw material powder, and especially FeB price is cheap with respect to B powder a lot.Cause
This present invention synthesis Fe2AlB2Cost be greatly lowered.
(4) technological process of the invention is simple, and technological parameter is stable, in the non-press stove and hot pressing furnace of routine, argon gas gas
Under atmosphere, in the short time, high-purity Fe can be synthesized2AlB2Powder and compact block material.
(5) the method applied in the present invention, also it is applied to prepare the powder and compact block of other MAB materials.
Brief description of the drawings
Fig. 1 is the synthetically prepared Fe of the present invention2AlB2X-ray diffraction (XRD) collection of illustrative plates of material.
Fig. 2 is the Fe that the present invention synthesizes2AlB2SEM (SEM) photo of material.
Embodiment
1.Fe2AlB2The preparation of ceramic powder
Embodiment one:
By FeB：Al=2：1.1 molar ratio ingredient, weigh 8.18 grams of FeB powder, 1.82 grams of Al powder.Above-mentioned dispensing is put into
Batch mixing 5 hours in ball grinder.Well mixed dispensing is put into stainless steel mould on tablet press machine and carries out pressed compact, then will be above-mentioned
Base substrate is put into graphite jig, and graphite jig is placed in vacuum sintering furnace, under argon gas atmosphere, with 10 DEG C/min speed by stove
Temperature rise soaking time 120min, is then down to room temperature to 1000 DEG C, you can obtains high-purity Fe2AlB2Material.Will be above-mentioned
Fe2AlB2Material crushes in ball mill, crosses the sieve of different meshes, and the Fe of different-grain diameter can be made2AlB2Powder.To obtaining
Sample carry out X-ray diffraction analysis, its XRD diffracting spectrum is shown in accompanying drawing 1.From XRD results, single-phase has been obtained
Fe2AlB2Material, exist without other impurities phases.Fe2AlB2Fracture Profile in Metallic Materials pattern is as shown in Fig. 2 particle has layer structure.
Embodiment two:
By FeB：Al=2：1.1 molar ratio ingredient, weigh 8.18 grams of FeB powder, 1.82 grams of Al powder.Above-mentioned dispensing is put into
Batch mixing 24 hours in ball grinder.Well mixed dispensing is put into stainless steel mould on tablet press machine and carries out pressed compact, then will be upper
State base substrate to be put into graphite jig, graphite jig is placed in vacuum sintering furnace, will with 30 DEG C/min speed under argon gas atmosphere
Furnace temperature rises to 1100 DEG C, soaking time 60min, is then down to room temperature, you can obtains high-purity Fe2AlB2Material.Will be above-mentioned
Fe2AlB2Material crushes in ball mill, crosses the sieve of different meshes, and the Fe of different-grain diameter can be made2AlB2Powder.Fe2AlB2
The XRD results and granule-morphology of sample are the same as embodiment one.
Embodiment three:
By FeB：Al=2：1.3 molar ratio ingredient, weigh 7.92 grams of FeB powder, 2.08 grams of Al powder.Above-mentioned dispensing is put into
Batch mixing 10 hours in ball grinder.Well mixed dispensing is put into stainless steel mould on tablet press machine and carries out pressed compact, then will be upper
State base substrate to be put into graphite jig, graphite jig is placed in vacuum sintering furnace, will with 20 DEG C/min speed under argon gas atmosphere
Furnace temperature rises to 1100 DEG C, soaking time 90min, is then down to room temperature, you can obtains high-purity Fe2AlB2Material.Will be above-mentioned
Fe2AlB2Material crushes in ball mill, crosses the sieve of different meshes, and the Fe of different-grain diameter can be made2AlB2Powder.Fe2AlB2
The XRD results and granule-morphology of sample are the same as embodiment one.
Embodiment four:
By FeB：Al=2：1.5 molar ratio ingredient, weigh 7.67 grams of FeB powder, 2.33 grams of Al powder.Above-mentioned dispensing is put into
Batch mixing 15 hours in ball grinder.Well mixed dispensing is put into stainless steel mould on tablet press machine and carries out pressed compact, then will be upper
State base substrate to be put into graphite jig, graphite jig is placed in vacuum sintering furnace, will with 50 DEG C/min speed under argon gas atmosphere
Furnace temperature rises to 1200 DEG C, soaking time 10min, is then down to room temperature, you can obtains high-purity Fe2AlB2Material.Will be above-mentioned
Fe2AlB2Material crushes in ball mill, crosses the sieve of different meshes, and the Fe of different-grain diameter can be made2AlB2Powder.Fe2AlB2
The XRD results and granule-morphology of sample are the same as embodiment one.
2.Fe2AlB2The preparation of ceramic dense block
Embodiment one:
By FeB：Al=2：1.1 molar ratio ingredient, weigh 32.72 grams of FeB powder, 7.28 grams of Al powder.Above-mentioned dispensing is put
Enter batch mixing 5 hours in ball grinder.Well mixed dispensing is put into graphite jig, graphite jig is placed in hot pressing furnace, argon
Under gas shielded atmosphere, furnace temperature is risen to 1000 DEG C with 10 DEG C/min speed, pressurize 40MPa, soaking time 120min, then drops
To room temperature, you can obtain high-purity Fe2AlB2Compact block material.X-ray diffraction result is shown in Fig. 1.
Embodiment two:
By FeB：Al=2：1.1 molar ratio ingredient, weigh 32.72 grams of FeB powder, 7.28 grams of Al powder.Above-mentioned dispensing is put
Enter batch mixing 24 hours in ball grinder.Well mixed dispensing is put into graphite jig, graphite jig is placed in hot pressing furnace, argon
Under gas shielded atmosphere, furnace temperature is risen to 1100 DEG C with 30 DEG C/min speed, pressurize 30MPa, soaking time 60min, then drops
To room temperature, you can obtain high-purity Fe2AlB2Compact block material.X-ray diffraction result is shown in Fig. 1.
Embodiment three:
By FeB：Al=2：1.3 molar ratio ingredient, weigh 31.68 grams of FeB powder, 8.32 grams of Al powder.Above-mentioned dispensing is put
Enter batch mixing 10 hours in ball grinder.Well mixed dispensing is put into graphite jig, graphite jig is placed in hot pressing furnace,
Under argon atmosphere, furnace temperature is risen to 1100 DEG C with 20 DEG C/min speed, pressurize 20MPa, soaking time 90min, then
It is down to room temperature, you can obtain high-purity Fe2AlB2Compact block material.X-ray diffraction result is shown in Fig. 1.
Claims (3)
1. atmospheric synthesis high-purity Fe2AlB2The method of ceramic powder, it is characterised in that：
(1) using FeB powder and Al powder as raw material, by FeB：Al=2：The molar ratio ingredient of (1.1~1.5).
(2) by above-mentioned dispensing and agate ball by ball and the weight ratio 2 of material：1 is put into ball grinder, dry-mixed 5 on tumbling ball mill
~24 hours, well mixed dispensing is put into stainless steel mould on tablet press machine and carries out pressed compact.
(3) above-mentioned base substrate is put into graphite jig, graphite jig is placed in non-press stove, under argon gas atmosphere, with 10~50 DEG C/
Furnace temperature is risen to 1000~1200 DEG C by min speed, is incubated 10~120min, is then down to room temperature, obtains high-purity Fe2AlB2
Material.
(4) by above-mentioned Fe2AlB2Material crushes in ball mill, crosses the sieve of different meshes, and the Fe of different-grain diameter can be made2AlB2
Powder.
2. hot pressing is for high-purity Fe2AlB2The method of compact block, it is characterised in that：
(1) using FeB powder and Al powder as raw material, by FeB：Al=2：The molar ratio ingredient of (1.1~1.5).
(2) by above-mentioned dispensing and agate ball by ball and the weight ratio 2 of material：1 is put into ball grinder, dry-mixed 5 on tumbling ball mill
~24 hours.
(3) well mixed dispensing is put into graphite jig, graphite jig is placed in hot pressing furnace, under argon gas atmosphere, with 10
Furnace temperature is risen to 1000~1200 DEG C by~50 DEG C/min speed, and pressurize 10-40MPa, is incubated 10~120min, is then down to room
Temperature, obtain high-purity densification Fe2AlB2Block materials.
3. according to the preparation method described in claim 1 and 2, it is characterised in that the preparation method is also applied for preparing other MAB
Material (including Cr4AlB6, Cr3AlB4, Cr2AlB2, Mn2AlB2, Ru2ZnB2, the compound such as MoAlB, WAlB) powder and densification
Block.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531991A (en) * | 2018-03-28 | 2018-09-14 | 西南交通大学 | A kind of preparation method for growing needle-shaped and laminar monocrystalline MoAlB |
| CN111763089A (en) * | 2019-12-28 | 2020-10-13 | 松山湖材料实验室 | Preparation method of ternary boride ceramic material with laminated structure and product thereof |
| CN113241425A (en) * | 2021-06-03 | 2021-08-10 | 贵州民族大学 | Molybdenite electrode and preparation method thereof |
| CN114276146A (en) * | 2021-11-11 | 2022-04-05 | 复旦大学 | High-purity compact WAlB MAB phase ceramic block material and preparation method thereof |
| CN115215551A (en) * | 2022-08-12 | 2022-10-21 | 西安石油大学 | Composite glass ceramic particles, high-temperature protective coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106745021A (en) * | 2016-11-28 | 2017-05-31 | 哈尔滨工业大学 | A kind of Fe2AlB2The synthetic method of material |
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- 2017-09-14 CN CN201710824823.XA patent/CN107555998A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745021A (en) * | 2016-11-28 | 2017-05-31 | 哈尔滨工业大学 | A kind of Fe2AlB2The synthetic method of material |
Non-Patent Citations (1)
| Title |
|---|
| SANKALP KOTA ET AL.: "Elastic properties,thermal stability,and thermodynamic parameters of MoAlB", 《PHYSICAL REVIEW B》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531991A (en) * | 2018-03-28 | 2018-09-14 | 西南交通大学 | A kind of preparation method for growing needle-shaped and laminar monocrystalline MoAlB |
| CN108531991B (en) * | 2018-03-28 | 2020-12-18 | 西南交通大学 | Preparation method of long-needle-shaped and thin-sheet-shaped single crystal MoAlB |
| CN111763089A (en) * | 2019-12-28 | 2020-10-13 | 松山湖材料实验室 | Preparation method of ternary boride ceramic material with laminated structure and product thereof |
| CN113241425A (en) * | 2021-06-03 | 2021-08-10 | 贵州民族大学 | Molybdenite electrode and preparation method thereof |
| CN113241425B (en) * | 2021-06-03 | 2021-11-23 | 贵州民族大学 | Molybdenite electrode and preparation method thereof |
| CN114276146A (en) * | 2021-11-11 | 2022-04-05 | 复旦大学 | High-purity compact WAlB MAB phase ceramic block material and preparation method thereof |
| CN115215551A (en) * | 2022-08-12 | 2022-10-21 | 西安石油大学 | Composite glass ceramic particles, high-temperature protective coating and preparation method thereof |
| CN115215551B (en) * | 2022-08-12 | 2023-05-26 | 西安石油大学 | Composite glass ceramic particles, high-temperature protective coating and preparation method thereof |
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