Preparation method of transition metal nano-boride
A nano-boride, transition metal technology, applied in the direction of metal borides, boron/borides, nanotechnology, etc., can solve the problem of inability to obtain crystalline or amorphous particles with nanostructures, and achieve high practical value, The effect of reducing process conditions and mild reaction conditions
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Embodiment 1
[0029] Preparation of nanocrystalline NbB 2 .
[0030] The raw material used is: anhydrous NbCl 5 (purity 98%), LiBH 4 (purity 98%), LiH (purity 95%), anhydrous LiCl (purity greater than 99%), tetrahydrofuran (purity greater than 99%), metal Na (purity greater than 98%).
[0031] Molar ratio NbCl 5 : LiBH 4 : LiH = 1 : 2 : 3, weigh NbCl in glove box 5 , LiBH 4 and LiH. Weigh anhydrous LiCl, whose mass is 8 times the total mass of the above three samples. NbCl to be weighed 5 Grind evenly with anhydrous LiCl, then weigh the LiBH 4 and LiH into NbCl 5 And LiCl mixture, further grinding evenly. The above uniformly ground sample was transferred into a ball mill jar, the ball-to-material ratio was 40:1, and the speed was set at 400 rpm for ball milling, and the ball milling was performed for 20 h to fully proceed the reaction. The reaction product was collected, washed with tetrahydrofuran, centrifuged, and repeated 4-5 times in order to ensure that all LiCl in the sa...
Embodiment 2
[0034] Preparation of Nano ZrB 2 .
[0035] The raw material used is: anhydrous ZrCl 4 (purity 98%), NaBH 4 (purity 98%), NaH (purity 95%), anhydrous NaCl (purity greater than 99%), glycerin (purity greater than 99%), ethanol (purity greater than 99%).
[0036] Molar ratio of ZrCl 4 : NaBH 4 : NaH = 1 : 2 : 2, weigh ZrCl in the glove box4 , NaBH 4 and NaH. Weigh anhydrous NaCl, its mass is 6 times of the total mass of the above three samples. ZrCl to be weighed 4 Grind evenly with anhydrous NaCl, then weigh the NaBH 4 and NaH into ZrCl 4 And NaCl mixture, further grinding evenly. The uniformly ground sample was transferred into a ball mill jar with a ball-to-material ratio of 30:1, and the ball milling speed was set at 380 rpm for ball milling, and the ball milling was carried out for 25 h to fully proceed the reaction. The reaction product is collected, washed alternately with glycerol and alcohol, centrifuged, and repeated 4-5 times in order to ensure that all N...
Embodiment 3
[0039] Preparation of nano-TiB 2 .
[0040] The raw material used is: TiCl 4 (purity 98%), LiBH 4 (purity 98%), LiH (purity 95%), anhydrous LiCl (purity greater than 99%), tetrahydrofuran (purity greater than 99%), metal Na (purity greater than 98%).
[0041] Molar ratio TiCl 4 : LiBH 4 : LiH = 1 : 2 : 3, weigh TiCl in the glove box 4 , LiBH 4 and LiH. Weigh anhydrous LiCl, whose mass is 8.5 times the total mass of the above three samples. LiBH to be weighed 4 Grind with LiH and anhydrous LiCl evenly, then transfer the above-mentioned uniformly ground sample into a ball mill jar, and add the weighed TiCl drop by drop 4 . The ball-to-material ratio was 40:1, and the set speed was 350 rpm for ball milling, and the ball milling was carried out for 30 h to fully proceed the reaction. The reaction product was collected, washed with tetrahydrofuran, centrifuged, and repeated 4-5 times in order to ensure that all LiCl in the sample was dissolved by tetrahydrofuran. Prio...
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Application Information
- IPC
- C01B35/04; B82Y30/00
- Inventors
- 陈立新; 范修林