CN1053225C - Method for preparing nanometer materials by solidification reaction - Google Patents
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Abstract
一种过渡金属合金超细微粒的制备方法，它用固态的金属氯化物和固态的硼氢化钾(钠)一起研磨，然后在氮气氛下200-450℃焙烧，再经水洗即得非晶态的金属-硼合金超细微粒。A method for preparing transition metal alloy ultrafine particles, which is ground together with solid metal chloride and solid potassium borohydride (sodium), then roasted at 200-450°C under a nitrogen atmosphere, and then washed with water to obtain an amorphous state metal-boron alloy ultrafine particles.
Description
本发明涉及制备合金超细微粒的方法，具体地说，是一种以固相化学反应制备非晶态纳米级的过渡金属合金超细微粒的方法。The invention relates to a method for preparing alloy ultrafine particles, in particular to a method for preparing amorphous nanoscale transition metal alloy ultrafine particles by solid phase chemical reaction.
自Duwez六十年代用快速急冷法制成非晶态合金以来，已经发展了多种制备非晶态合金的方法[参见：A.L.Greer，Science 267(1995)1947；W.L.Johnson，Progress in Mater.Sci.30(1986)81]其中有高能机械球磨法。该法是以基元混合粉或不同合金混合粉在高能机械球磨条件下的机械合金化方法。该法不易得到均一的非晶合金组份，往往带有一些晶态组份的残余，并且球磨条件苛刻，有的需要球磨几百甚至上千个小时，[参见：梁国宪等《材料科学与工程》12(1994)47；H.Okumura et al，J.Mater.Sci.27(1992)153]，因此该法产品不可避免地要被球磨罐及球的材料所污染，所得非晶微粒一般为微米级。Since Duwez made amorphous alloys by rapid quenching in the sixties, a variety of methods for preparing amorphous alloys have been developed [see: A.L.Greer, Science 267 (1995) 1947; W.L.Johnson, Progress in Mater.Sci. 30 (1986) 81] Among them is the high-energy mechanical ball milling method. The method is based on the mechanical alloying method of basic element mixed powder or different alloy mixed powder under the condition of high-energy mechanical ball milling. This method is not easy to obtain uniform amorphous alloy components, often with some residual crystalline components, and the ball milling conditions are harsh, some need ball milling for hundreds or even thousands of hours, [see: Liang Guoxian et al. "Material Science and Engineering "12 (1994) 47; H.Okumura et al, J.Mater.Sci.27 (1992) 153], so the product of this method will inevitably be polluted by the material of the ball mill jar and the ball, and the resulting amorphous particles are generally Micron.
另一种方法是液相沉积法[参见J.Van Wonterghem，S.Morup et al.，Nature322(1986)622；S.Linderoth，Hyperfine Interactions 68(1991)107]。该方法是在水溶液中以KBH4(NaBH4等)还原过渡金属离子，制备非晶态过渡金属-类金属合金超细微粒。该方法制得的过渡金属合金的成份有一定限制，以非晶Fe-B微粒为例，用液相法只能制得合B量小于40at％的合金[参见Z.HU，Y.Fan，et al.，J.Chem，Soc，chem.Commun，1995，247]，并且该法的原料不能充分利用，相当一部分KBH4或NaBH4在水溶液中自发分解，造成很大浪费。Another method is liquid phase deposition [see J. Van Wonderghem, S. Morup et al., Nature 322 (1986) 622; S. Linderoth, Hyperfine Interactions 68 (1991) 107]. The method is to reduce transition metal ions with KBH 4 (NaBH 4 etc.) in aqueous solution to prepare amorphous transition metal-metalloid alloy ultrafine particles. The composition of transition metal alloys prepared by this method has certain limitations. Taking amorphous Fe-B particles as an example, only alloys with a B content of less than 40at% can be produced by the liquid phase method [see Z.HU, Y.Fan, et al., J.Chem, Soc, chem.Commun, 1995, 247], and the raw materials of this method cannot be fully utilized, and a considerable part of KBH 4 or NaBH 4 spontaneously decomposes in aqueous solution, causing a lot of waste.
本发明的目的是提供一种制备均一的非晶的过渡金属-类金属合金超细微粒的方法，一种不需要长时间球磨，合金组份可调变，原料能充分利用的制备纳米级非晶态过渡金属-类金属合金超细微粒的方法。The purpose of the present invention is to provide a method for preparing uniform amorphous transition metal-metalloid alloy ultrafine particles, which does not require long-term ball milling, the alloy components can be adjusted, and the raw materials can be fully utilized to prepare nano-scale amorphous particles. Method for Ultrafine Particles of Crystalline Transition Metal-Metalloid Alloys.
本发明的技术解决方案如下。The technical solution of the present invention is as follows.
本发明是采用固相化学反应的方法，以MXn和M′YH4为起始原料制备M-Y系列合金超细微粒。The invention adopts the method of solid-phase chemical reaction to prepare MY series alloy ultrafine particles by using MXn and M'YH4 as starting materials.
本发明的过渡金属合金超细微粒的制备方法是在无氧无水条件下，将固态的MXn与固态的M′YH4一同研磨，然后在氮气氛下焙烧，经水和丙酮洗涤，即得非晶态M-Y合金超细微粒，或MXn中M为过渡金属，X为囟素，N为M的价数，式M′YH4中M′为碱金属，Y为B或Al。The preparation method of transition metal alloy ultrafine particles of the present invention is to grind solid MXn and solid M'YH together under anaerobic and anhydrous conditions, then roast under a nitrogen atmosphere, and wash with water and acetone to obtain Amorphous MY alloy ultrafine particles, or M in MXn is transition metal, X is halogen, N is the valence of M, M' in the formula M'YH 4 is alkali metal, Y is B or Al.
过渡金属可以是Fe，Ni，Co，Pd，Pt等。Transition metals can be Fe, Ni, Co, Pd, Pt, etc.
将固态的MXn与固态的M′YH4一同研磨后，在氮气氛下200-450℃焙烧，经水和丙酮洗涤后，在氮气氛下纯化2天左右，即得纳米级的非晶态M-Y合金超细微粒。若在高温焙烧可得晶态的M-Y合金超细微粒。Grinding solid MXn and solid M'YH 4 together, roasting at 200-450°C under a nitrogen atmosphere, washing with water and acetone, and purifying for about 2 days under a nitrogen atmosphere to obtain nanoscale amorphous MY Alloy ultrafine particles. If calcined at high temperature, crystalline MY alloy ultrafine particles can be obtained.
本发明的制备方法，MXn和M′YH4用量的摩尔比可以1.0∶1.0-1.0∶4.4，所得M-Y合金Y的含量可以从40at％至60at％之间调节。所得超细微粒的粒度可小于10nm，粒子的均匀度受球磨的时间影响，球磨8小时以上，粒子的粒度较均匀。In the preparation method of the present invention, the molar ratio of MXn and M'YH 4 can be 1.0:1.0-1.0:4.4, and the content of the obtained MY alloy Y can be adjusted from 40at% to 60at%. The particle size of the obtained ultrafine particles can be less than 10nm, and the uniformity of the particles is affected by the time of ball milling, and the particle size of the particles is relatively uniform after ball milling for more than 8 hours.
以本发明的制备方法，用无水FeCl3和M′BH4一同研磨，在氮气氛下200-450℃焙烧。经水洗得到非晶态Fe-B合金超细微粒。当Fecl3与M′BH4摩尔比为1∶3.3时，经研磨后，在700℃以上焙烧水洗得到单一物相的α-FeB合金超细微粒。With the preparation method of the present invention, anhydrous FeCl 3 and M'BH 4 are ground together, and roasted at 200-450° C. under a nitrogen atmosphere. The amorphous Fe-B alloy ultrafine particles are obtained by washing with water. When the molar ratio of Fecl 3 to M'BH 4 is 1:3.3, after grinding, roasting and washing with water above 700°C, single-phase α-FeB alloy ultrafine particles can be obtained.
本发明的方法也可以用有结晶水的MXn代替无水的MX，当在无氧条件下，用有结晶水的MXn与M′YH4一起研磨，研磨后不需焙烧，直接水洗，即得非晶态的M-Y合金超细微粒。以此制备M-Y合金超细微粒，M-Y合金中的含量一般低于40at％。The method of the present invention also can use the MXn that has water of crystallization to replace anhydrous MX, when under anaerobic conditions, use the MXn that has water of crystallization to grind together with M'YH 4 , need not roast after grinding, directly wash with water, obtain final product Amorphous MY alloy ultrafine particles. In this way, MY alloy ultrafine particles are prepared, and the content in MY alloy is generally lower than 40 at%.
本发明的过渡金属合金超细微粒的制备方法是固相化学反应，操作简单，研磨时间短，得到的是非晶态的过渡金属-类金属合金超细微粒，粒度可小于10nm，比表面积可大于50m2/g。由于是固相反应，原料M′YH4得到充分利用，调节M′YH4的用量，可以控制M-Y合金超细微粒中Y的含量。因此是一个经济的制得高质量的非晶态的过渡金属-类金属合金超细微粒的制备方法。The preparation method of transition metal alloy ultrafine particles of the present invention is a solid-phase chemical reaction, simple operation, short grinding time, and what is obtained is amorphous transition metal-metalloid alloy ultrafine particles, the particle size can be less than 10nm, and the specific surface area can be greater than 50m 2 /g. Because it is a solid phase reaction, the raw material M'YH 4 is fully utilized, and the content of Y in the MY alloy ultrafine particles can be controlled by adjusting the amount of M'YH 4 . Therefore, it is an economical method for preparing high-quality amorphous transition metal-metalloid alloy ultrafine particles.
以下通过实施例进一步说明本发明。实施例：The present invention is further illustrated by the following examples. Example:
1.在高度无水无氧操作条件下(O2、H2O达ppm量级)，以1∶3.3摩尔比称取无水FeCl3及KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨8h，接着在400℃、氮气氛保护下焙烧3h，再经水洗、钝化，得到粒度小于10nm，比表面积大于50m2/g的Fe49B51非晶合金微粒。1. Under highly anhydrous and oxygen-free operating conditions (O 2 , H 2 O up to ppm level), weigh anhydrous FeCl 3 and KBH 4 with a molar ratio of 1:3.3, seal them in a hard stainless steel ball mill tank, and ball The material ratio is 30:1, ball milled on a planetary ball mill at a speed of 160rpm for 8 hours, then roasted at 400°C for 3 hours under the protection of nitrogen atmosphere, and then washed with water and passivated to obtain a particle size of less than 10nm and a specific surface area of more than 50m 2 /g Fe 49 B 51 amorphous alloy particles.
2.在高度无水无氧操作条件下(O2、H2O达ppm量级)，以1∶3.3摩尔比称取无水FeCl3及KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨8h，接着在800℃、氮气氛保护下焙烧3h，再经水洗、钝化，得到晶态α-FeB超细微粒。2. Under highly anhydrous and oxygen-free operating conditions (O 2 , H 2 O up to ppm level), weigh anhydrous FeCl 3 and KBH 4 with a molar ratio of 1:3.3, seal them in a hard stainless steel ball mill tank, and ball The material ratio is 30:1, ball milled on a planetary ball mill at a speed of 160rpm for 8h, then roasted at 800°C for 3h under the protection of nitrogen atmosphere, washed with water and passivated to obtain crystalline α-FeB ultrafine particles.
3.在高度无水无氧操作条件下(O2、H2O达ppm量级)，以1∶3.3摩尔比称取无水FeCl3及KBH4，研磨5min以略加混合，接着在400℃、惰性气体保护下焙烧3h，再经水洗、钝化，得到含B量为52at％的Fe-B纳米非晶合金微粒。3. Under highly anhydrous and oxygen-free operating conditions (O 2 , H 2 O up to ppm level), weigh anhydrous FeCl 3 and KBH 4 with a molar ratio of 1:3.3, grind for 5 minutes to slightly mix, and then mix at 400 ℃ under the protection of inert gas for 3 hours, and then washed with water and passivated to obtain Fe-B nano-amorphous alloy particles with a B content of 52at%.
4.在高度无水无氧操作条件下(O2、H2O达ppm量级)，以1∶1.1摩尔比称取无水FeCl3及KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨10h，接着在400℃、氮气氛保护下焙烧3h，再经水洗、钝化，得到含B量为40at％的Fe-B纳米非晶合金微粒。4. Under highly anhydrous and oxygen-free operating conditions (O 2 , H 2 O up to ppm level), weigh anhydrous FeCl 3 and KBH 4 with a molar ratio of 1:1.1, seal them in a hard stainless steel ball mill jar, and ball The material ratio is 30: 1, ball milling with a rotating speed of 160rpm on a planetary ball mill for 10h, then roasting at 400°C for 3h under the protection of a nitrogen atmosphere, and then washing and passivating to obtain a Fe-B nanometer with a B content of 40at%. Amorphous alloy particles.
5.在高度无水无氧操作条件下(O2、H2O达ppm量级)，以1∶4.3摩尔比称取无水FeCl3及KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨13h，接着在400℃、氮气氛保护下焙烧3h，再经水洗、钝化，得到含B量为60at％的Fe-B纳米非晶合金微粒。5. Under highly anhydrous and oxygen-free operating conditions (O 2 , H 2 O up to ppm level), weigh anhydrous FeCl 3 and KBH 4 with a molar ratio of 1:4.3, seal them in a hard stainless steel ball mill tank, and ball The material ratio is 30: 1, ball milled with a rotating speed of 160rpm on a planetary ball mill for 13h, then roasted for 3h at 400°C under the protection of a nitrogen atmosphere, and then washed with water and passivated to obtain a Fe-B nanometer with a B content of 60at%. Amorphous alloy particles.
6.在一般的无水无氧操作条件下(普N2保护)，以1∶3.3摩尔比称取无水FeCl3及KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨8h，接着在400℃、惰性气体保护下焙烧3h，再经水洗、钝化，得到含B量为48at％的Fe-B纳米非晶合金微粒。6. Under normal anhydrous and oxygen-free operating conditions (common N 2 protection), weigh anhydrous FeCl 3 and KBH 4 with a molar ratio of 1:3.3, and seal them in a hard stainless steel ball mill tank with a ball-to-material ratio of 30: 1. Ball milling on a planetary ball mill at a speed of 160rpm for 8h, then roasting at 400°C for 3h under the protection of an inert gas, and then washing and passivation to obtain Fe-B nano-amorphous alloy particles with a B content of 48at%.
7.在一般的无水无氧操作条件下(普N2保护)，以1∶3.3摩尔比称取FeCl3·6H2O及KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨8h，得到混有少量晶相的含B量为40at％的Fe-B超细合金微粒。7. Under normal anhydrous and oxygen-free operating conditions (common N 2 protection), weigh FeCl 3 6H 2 O and KBH 4 with a molar ratio of 1:3.3, and seal them in a hard stainless steel ball mill tank. The ball-to-material ratio is 30:1, ball milled on a planetary ball mill at a speed of 160rpm for 8h to obtain Fe-B ultrafine alloy particles with a B content of 40at% mixed with a small amount of crystal phase.
8.在一般的无水无氧操作条件下(普N2保护)，以1∶1摩尔比称取CoCl2·6H2O和KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨6h，经水洗、钝化，得到含B量为20at％的Co-B纳米非晶合金微粒。8. Under normal anhydrous and oxygen-free operating conditions (normal N 2 protection), weigh CoCl 2 6H 2 O and KBH 4 with a molar ratio of 1:1, and seal them in a hard stainless steel ball mill tank, with a ball-to-material ratio of 30:1, milled on a planetary ball mill at a speed of 160 rpm for 6 hours, washed with water and passivated to obtain Co-B nano-amorphous alloy particles with a B content of 20at%.
9.在一般的无水无氧操作条件下(普N2保护)，以1∶3摩尔比称取CoCl2·6H2O和KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨6h，经水洗、钝化，得到含B量为28at％的Co-B纳米非晶合金微粒。9. Under normal anhydrous and oxygen-free operating conditions (normal N 2 protection), weigh CoCl 2 6H 2 O and KBH 4 with a molar ratio of 1:3, and seal them in a hard stainless steel ball mill jar, with a ball-to-material ratio of 30:1, milled on a planetary ball mill at a speed of 160 rpm for 6 hours, washed with water and passivated to obtain Co-B nano-amorphous alloy particles with a B content of 28 at%.
10.在一般的无水无氧操作条件下(普N2保护)，以1∶1摩尔比称取NiCl2·6H2O和KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨6h，经水洗、钝化，得到含B量为16at％的Ni-B纳米非晶合金微粒。10. Under normal anhydrous and oxygen-free operating conditions (normal N 2 protection), weigh NiCl 2 6H 2 O and KBH 4 with a molar ratio of 1:1, and seal them in a hard stainless steel ball mill jar, the ball-to-material ratio is 30:1, milled on a planetary ball mill at a speed of 160 rpm for 6 hours, washed with water and passivated to obtain Ni-B nano-amorphous alloy particles with a B content of 16at%.
11.在一般的无水无氧操作条件下(普N2保护)，以1∶3摩尔比称取NiCl2·6H2O和KBH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨6h，经水洗、钝化，得到含B量为29at％的Ni-B纳米非晶合金微粒。11. Under normal anhydrous and oxygen-free operating conditions (normal N 2 protection), weigh NiCl 2 6H 2 O and KBH 4 with a molar ratio of 1:3, and seal them in a hard stainless steel ball mill tank, the ball-to-material ratio is 30:1, ball milled on a planetary ball mill at a speed of 160 rpm for 6 hours, washed with water, and passivated to obtain Ni-B nano-amorphous alloy particles with a B content of 29at%.
12.在高度无水无氧操作条件下(O2、H2O达ppm量级)，以1∶3.3摩尔比称取无水FeCl3及LiAlH4，密封于硬质不锈钢球磨罐中，球料比为30∶1，在行星式球磨机上以160rpm的转速球磨13h，接着在400℃、氮气氛保护下焙烧3h，再经水洗、钝化，得到含Al量约50at％的Fe-Al纳米非晶合金微粒。12. Under highly anhydrous and oxygen-free operating conditions (O 2 , H 2 O up to ppm level), weigh anhydrous FeCl 3 and LiAlH 4 with a molar ratio of 1:3.3, seal them in a hard stainless steel ball mill jar, and ball The material ratio is 30:1, ball milling on a planetary ball mill at a speed of 160rpm for 13h, then roasting at 400°C for 3h under the protection of a nitrogen atmosphere, and then washing and passivation to obtain Fe-Al nanometers with an Al content of about 50at%. Amorphous alloy particles.
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| CN109103451A (en) * | 2017-06-21 | 2018-12-28 | 北京大学 | A kind of purposes of lithium-containing transition metal chloride as anode material for lithium-ion batteries |
| CN114472903A (en) * | 2022-02-18 | 2022-05-13 | 江西省科学院应用物理研究所 | A kind of preparation method of ultrafine iron boron nano-amorphous powder |
| CN117123215B (en) * | 2022-05-20 | 2025-12-23 | 中国科学院大连化学物理研究所 | An amorphous alloy catalyst, its preparation method and its application |
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