CN112981155A - Preparation method of binary intermetallic compound - Google Patents
Preparation method of binary intermetallic compound Download PDFInfo
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- CN112981155A CN112981155A CN201911282422.1A CN201911282422A CN112981155A CN 112981155 A CN112981155 A CN 112981155A CN 201911282422 A CN201911282422 A CN 201911282422A CN 112981155 A CN112981155 A CN 112981155A
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- intermetallic compound
- metal hydride
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- 229910000765 intermetallic Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 45
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 229910052987 metal hydride Inorganic materials 0.000 claims abstract description 14
- 150000004681 metal hydrides Chemical class 0.000 claims abstract description 14
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 11
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 8
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 34
- 229910052786 argon Inorganic materials 0.000 description 17
- 229910001220 stainless steel Inorganic materials 0.000 description 11
- 239000010935 stainless steel Substances 0.000 description 11
- 238000000634 powder X-ray diffraction Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 6
- 238000007789 sealing Methods 0.000 description 5
- 229910052723 transition metal Inorganic materials 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- SIAPCJWMELPYOE-UHFFFAOYSA-N lithium hydride Chemical compound [LiH] SIAPCJWMELPYOE-UHFFFAOYSA-N 0.000 description 1
- 229910000103 lithium hydride Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000005616 pyroelectricity Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The application discloses a preparation method of a binary intermetallic compound, which at least comprises the following steps: ball-milling raw materials containing ternary metal hydride to obtain powder; reacting the powder to obtain a binary intermetallic compound; wherein the ternary metal hydride comprises an element A1Elemental palladium, elemental hydrogen; element A1Including at least one of alkali metals and alkaline earth metals. The preparation method has the advantages of simple operation, low reaction temperature, normal reaction pressure, short material synthesis time and high product purity.
Description
Technical Field
The application relates to a preparation method of a binary intermetallic compound, belonging to the field of intermetallic compound materials.
Background
Intermetallic compounds are composed of two or more metal/nonmetal elements, and their crystal structures and electronic structures are different from their constituent elements. The special structure of intermetallic compounds, which have various characteristics such as pyroelectricity, hydrogen storage and superconductivity, has attracted extensive interest and intensive research by researchers.
The most common method for synthesizing intermetallic compound of alkali (earth) metal-transition metal is to mix the components of intermetallic compound according to stoichiometric ratio, raise the temperature to a certain high temperature and then quench. However, this method requires a high temperature and is complicated to operate.
Disclosure of Invention
According to one aspect of the application, the preparation method of the binary intermetallic compound is provided, and the method is simple to operate, mild in reaction conditions, easy in raw material obtaining, high in product purity and high in yield.
The method for preparing the binary intermetallic compound takes alkali metal or alkaline earth metal-transition metal as raw materials, finely grinds reactants by ball milling, places finely ground powdery reactants in a reactor, and obtains the binary intermetallic compound of the alkali metal or the alkaline earth metal and the transition metal with different proportions by going through different temperature conditions in an inactive atmosphere.
The present application provides a method for producing a binary intermetallic compound, the method at least comprising: ball-milling raw materials containing ternary metal hydride to obtain powder;
reacting the powder to obtain the binary intermetallic compound;
wherein the ternary metal hydride comprises an element A1Elemental palladium, elemental hydrogen; the element A1Including at least one of alkali metals and alkaline earth metals.
Alternatively, the ternary metal hydride is selected from any of the compounds having the formula shown in formula I,
A1 xPdHyformula I
Wherein x and y each represents A1H in a molar ratio;
x＝1、2、3、4；
the value range of y is more than or equal to 0.7 and less than or equal to 5.
Optionally, in the ternary metal hydride; the alkali metal is selected from any one of Li, Na and K; the alkaline earth metal is selected from any one of Ca and Ba.
Alternatively, the ternary metal hydride is selected from Li2PdH2、LiPdH0.70、Li4PdH4、LiPdH0.73、LiPdH0.96、Na2PdH2、Na2PdH4、K2PdH4、K3PdH5、CaPdH2、Ba2PdH4Any one of the above.
Optionally, the ternary metal hydride is selected from A1 2PdH2、A1PdH2At least one of (1).
Optionally, the reaction conditions are: under the inert atmosphere, the reaction temperature is 300-500 ℃; the reaction time is 2-4 h.
Optionally, the upper temperature limit of the reaction is selected from the group consisting of 500 deg.C, 450 deg.C, 400 deg.C, 350 deg.C, 300 deg.C, 250 deg.C, 200 deg.C, 150 deg.C, 100 deg.C, 50 deg.C, and the lower temperature limit is selected from the group consisting of 0 deg.C, 50 deg.C, 100 deg.C, 150 deg.C, 200 deg..
Preferably, the reaction is carried out in a quartz tube reactor.
Preferably, the temperature rise rate of the reaction is 1-5 ℃/min.
Preferably, the reaction conditions are: under the inert atmosphere, the reaction temperature is 300-500 ℃; the reaction time is 2-4 h.
Optionally, the ball milling is solid phase ball milling; the weight ratio of the grinding balls to the sample to be treated in the ball milling process is 1-100: 1.
Optionally, the upper limit of the weight ratio of the grinding balls to the sample to be processed in the ball milling process is selected from 100, 90, 80, 70, 60, 50, 40, 30, 20, 10, 8, 5, 3, and the lower limit is selected from 1, 3, 5, 8, 10, 20, 30, 40, 50, 60, 70, 80, 90.
Preferably, the ball milling time is 1-24 hours; the temperature range of ball milling is 10-100 ℃.
Optionally, the temperature of the ball mill is selected from the upper limit of 100 deg.C, 90 deg.C, 80 deg.C, 70 deg.C, 60 deg.C, 50 deg.C, 40 deg.C, 30 deg.C, 20 deg.C, 10 deg.C, and the lower limit is selected from the lower limit of 0 deg.C, 10 deg.C, 20 deg.C, 30 deg.C, 40 deg.C.
Optionally, the ball milling is performed under an inert atmosphere.
Preferably, the gas flow rate of the inactive atmosphere in the ball milling process is 1-200 mL/min.
Optionally, the upper limit of the gas flow rate of the inert atmosphere during ball milling is selected from 200mL/min, 190mL/min, 180mL/min, 170mL/min, 160mL/min, 150mL/min, 140mL/min, 130mL/min, 120mL/min, 110mL/min, 100mL/min, 90mL/min, 80mL/min, 70mL/min, 60mL/min, 50mL/min, 40mL/min, 30mL/min, 20mL/min, 10mL/min, and the lower limit is selected from 1mL/min, 10mL/min, 20mL/min, 30mL/min, 40mL/min, 50mL/min, 60mL/min, 70mL/min, 80mL/min, 90mL/min, 100mL/min, 110mL/min, 120mL/min, 130mL/min, 140mL/min, 150mL/min, 160mL/min, 170mL/min, 180mL/min, 190 mL/min.
Optionally, the ball milling comprises mechanical mixing or mechanical ball milling on any one of a robotic powder mixer, a planetary ball mill, an oscillating ball mill, a vibratory ball mill.
Preferably, the rotating speed of the planetary ball mill is 10-500 rpm.
Preferably, the oscillating frequency of the oscillating ball mill is 50-600 weeks/min.
Preferably, the rotating speed of the automatic powder mixing machine is 10-100 rpm.
Optionally, the grinding balls comprise at least one of stainless steel balls, tungsten carbide balls, corundum balls, agate balls, zirconia balls.
Alternatively, the binary intermetallic compound is selected from any one of the compounds having the chemical formula shown in formula II;
A2 mPdnformula II
Wherein A is2Represents an alkali metal or an alkaline earth metal;
m and n are each A2The mole ratio of Pd;
the value range of m is more than or equal to 1 and less than or equal to 2.48;
the value range of n is more than or equal to 1 and less than or equal to 5.52.
Optionally, the binary intermetallic compound prepared by the method comprises Li2Pd、LiPd、Li2.48Pd5.52、Li1.12Pd2.88、Li1.24Pd2.76、CaPd、CaPd2At least one of (1).
The following introduces a specific preparation procedure of the binary intermetallic compound in the present application:
(1) under the inactive atmosphere, alkali metal or alkaline earth metal-transition metal ternary hydride is filled into a ball milling tank;
(2) finely grinding the alkali metal or alkaline earth metal-transition metal ternary hydride by adopting a temperature-controlled mechanical mixing or mechanical ball milling mode;
(3) transferring the ground solid powder into a reactor, and introducing an inert gas;
(4) and heating the reactor to 300-500 ℃, reacting for 2-4 h, then cooling in an inactive atmosphere, and collecting a solid sample, namely the target product.
The beneficial effects that this application can produce include:
the preparation method of the binary intermetallic compound is simple and convenient to operate, mild in reaction conditions, easy to obtain raw materials, high in product purity and high in yield.
Drawings
FIG. 1 shows Li2PdH2X-ray powder diffraction pattern of the LiPd synthesized as the starting material.
FIG. 2 shows Li2PdH2Li synthesized as raw material2X-ray powder diffraction pattern of Pd.
FIG. 3 shows CaPdH2CaPd synthesized as raw material2X-ray powder diffraction pattern of (a).
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
Li2PdH2The preparation method comprises the following steps: in an argon glove box, palladium powder (Aladdin, purity 99.9%) and lithium hydride (Aladdin, purity 97%) are accurately weighed according to the molar ratio of 1:2 and placed in a self-made stainless steel ball milling tank. Sealing the ball milling tank, and then filling the ball milling tank into a planetary ball mill under the ball milling condition of 150rpm 3And (4) hours. Placing the obtained mixture in a self-made stainless steel reactor in an argon glove box, vacuumizing, heating the sample to 300 ℃ (the heating rate is 5 ℃/min) under the hydrogen pressure of 10bar, keeping the temperature for 36 hours, cooling to room temperature, and taking out the obtained sample;
CaPdH2the preparation method comprises the following steps: accurately weighing palladium powder (Aladdin, purity 99.9%) and calcium hydride (AlfaAesar, purity 97%) in an argon glove box according to a molar ratio of 1:1, placing the palladium powder and the calcium hydride in a self-made stainless steel ball milling tank, adding hydrogen pressure of 260psi, sealing the ball milling tank, then putting the ball milling tank into a planetary ball mill, carrying out ball milling for 2 hours under the ball milling condition of 200rpm, transferring a ball milling product to a stainless steel reaction tube, adding 210psi hydrogen pressure at room temperature, heating to 430 ℃ (heating rate of 5 ℃/min), keeping the temperature for 8 hours, cooling to room temperature, and taking out an obtained sample;
the X-ray powder diffraction patterns in this application were analyzed using a panalytical X' pert Pro type transtarget X-ray powder diffractometer.
Example 1
In an argon glove box, Li is accurately weighed2PdH2400mg, and placing in a self-made stainless steel ball milling tank. And sealing the ball milling tank, and then filling the ball milling tank into a planetary ball mill under the ball milling condition of 150rpm for 1 hour. And then placing the obtained mixture in a self-made stainless steel reactor in an argon glove box, introducing argon into a sample at normal pressure, introducing the argon at the flow rate of 30mL/min, heating to 350 ℃ (the heating rate is 2 ℃/min), keeping the temperature for 3 hours, cooling to room temperature in argon gas flow, taking out the obtained sample, and testing the obtained product by using an X-ray powder diffractometer.
Example 2
In an argon glove box, Li is accurately weighed2PdH2400mg, and placing in a self-made stainless steel ball milling tank. And sealing the ball milling tank, and then filling the ball milling tank into a planetary ball mill under the ball milling condition of 150rpm for 1 hour. Then placing the obtained mixture in a self-made stainless steel reactor in an argon glove box, introducing argon into the sample at normal pressure, allowing the flow rate to be 30mL/min, heating to 500 ℃ (the heating rate is 2 ℃/min), keeping the temperature for 3 hours, cooling to room temperature in argon gas flow, taking out the obtained sample, and thus obtaining the productThe product obtained is tested by an X-ray powder diffractometer.
Example 3 structural characterization of the products of examples 1 and 2
X-ray powder diffraction analysis was performed on the samples obtained in example 1 and example 2 using a Panalytical X' pert Pro type transtarget X-ray powder diffractometer, respectively, and it can be seen from FIG. 1, which is an X-ray powder diffraction pattern of the sample obtained in example 1, and FIG. 2, which is an X-ray powder diffraction pattern of the sample obtained in example 2, that all diffraction peaks in spectrum 1 are assigned to LiPd, and all diffraction peaks in spectrum 2 are assigned to Li2Pd, so from the XRD characterization result, pure LiPd and pure Li are prepared2Pd。
Example 4
Accurately weighing CaPdH in an argon glove box2400mg, and placing in a self-made stainless steel ball milling tank. And sealing the ball milling tank, and then filling the ball milling tank into a planetary ball mill under the ball milling condition of 150rpm for 1 hour. And then placing the obtained mixture in a self-made stainless steel reactor in an argon glove box, introducing argon into a sample at normal pressure, introducing the argon at the flow rate of 30mL/min, heating to 360 ℃ (the heating rate is 2 ℃/min), keeping the temperature for 3 hours, cooling to room temperature in argon gas flow, taking out the obtained sample, and testing the obtained product by using an X-ray powder diffractometer.
Example 5 structural characterization of the product of example 4
X-ray powder diffraction analysis was performed on the sample obtained in example 4 using a Panalytical X' pert Pro type transtarget X-ray powder diffractometer, and FIG. 3 is an X-ray powder diffraction pattern of the sample obtained in example 4, from which it can be seen that all diffraction peaks in spectrum 3 are assigned to CaPd2Therefore, from the XRD characterization result, pure CaPd is prepared2。
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024098475A1 (en) * | 2022-11-07 | 2024-05-16 | 中国科学院大连化学物理研究所 | Hydrogen anion conductor, preparation method therefor and use thereof |
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| US4828606A (en) * | 1986-04-22 | 1989-05-09 | Studiengesellschaft Kohle Gmbh | Process for preparing intermetallic compounds or hydrides thereof |
| CN103832983A (en) * | 2012-11-22 | 2014-06-04 | 中国科学院大连化学物理研究所 | Synthesis method of amino metal compounds |
| CN107151805A (en) * | 2017-04-10 | 2017-09-12 | 中国科学院高能物理研究所 | Foam rare earth-nickel alloys and preparation method thereof, purposes |
| CN107475596A (en) * | 2017-08-10 | 2017-12-15 | 哈尔滨工业大学 | A kind of high entropy intermetallic compound |
-
2019
- 2019-12-13 CN CN201911282422.1A patent/CN112981155A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| US4828606A (en) * | 1986-04-22 | 1989-05-09 | Studiengesellschaft Kohle Gmbh | Process for preparing intermetallic compounds or hydrides thereof |
| CN103832983A (en) * | 2012-11-22 | 2014-06-04 | 中国科学院大连化学物理研究所 | Synthesis method of amino metal compounds |
| CN107151805A (en) * | 2017-04-10 | 2017-09-12 | 中国科学院高能物理研究所 | Foam rare earth-nickel alloys and preparation method thereof, purposes |
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| Title |
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| EWA RÖNNEBRO ET AL.: "The gigapascal pressure thermal technique for synthesising new ternary metal hydrides in the A–Pd–H (A=Li, Na or Mg) system", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024098475A1 (en) * | 2022-11-07 | 2024-05-16 | 中国科学院大连化学物理研究所 | Hydrogen anion conductor, preparation method therefor and use thereof |
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Application publication date: 20210618 |