Mechanochemical process for the production of BP, B12P2 and mixtures thereof, in particular as nanopowders

Patent metadata

Field	Value
Publication number	US-10519039-B2
Application number	US-201615575028-A
Country	US
Kind code	B2
Filing date	Apr 8, 2016
Priority date	May 20, 2015
Publication date	Dec 31, 2019
Grant date	Dec 31, 2019

Abstract

The present invention relates to a process for the preparation of a boron phosphide, more specifically BP and/or B 12 P 2 , comprising the mechanochemical reaction of boron phosphate (BPO 4 ) with at least one alkaline earth metal (EA). In particular, the process of the invention allows for the selective preparation of either BP or B 12 P 2 with more than 95% purity, through the reduction of boron phosphate (BPO 4 ) with at least one alkaline earth metal (EA) according to reaction (1) for BP and according to reaction (2) for B 12 P 2 : BPO 4 +4 EA→BP+4 EA(O) (1) 2BPO 4 +5 (EA)B 2 +3 EA→B 12 P 2 +8 EA(O) (2). The present invention further relates to boron phosphide powders, in particular BP or B 12 P 2 powders, of nanometric or micrometric size.

First claim

The invention claimed is:

1. A process for the preparation of a boron phosphide, wherein the process is a mechanochemical reaction of a powder of boron phosphate (BPO 4 ) mixed with a powder of at least one alkaline earth metal (EA) by a mechanical device providing mechanical energy which allows to initiate and carry out the mechanochemical reaction between the powder of boron phosphate (BPO4) and the powder of at least one alkaline earth metal (EA), for directly obtaining said boron phosphide without any external thermal heating, said boron phosphide being BP and/or B 12 P 2 , and the mechanochemical reaction is carried out in a mill.

2. The process of claim 1 , wherein the mechanochemical reaction is carried out thanks to mechanical stresses between the powder of boron phosphate (BPO4) and the powder of at least one alkaline earth metal (EA).

3. The process of claim 1 , wherein the temperature of the reaction is below 80° C.

4. The process of claim 1 , wherein the particle size of the boron phosphide obtained by the mechanochemical reaction is a function of the time of the mechanochemical reaction between, which is between 30 s and 20 min.

5. The process of claim 1 , wherein the mechanical device is a rotative device and the rotation speed of the rotative device is between 50 and 1100 rpm.

6. The process of claim 5 , wherein the mechanochemical reaction comprises a ball-milling step of a powder mixture comprising boron phosphate and the at least one alkaline earth metal.

7. The process of claim 1 , wherein the mechanochemical reaction is carried out in air.

8. The process of claim 1 , wherein the boron phosphide is BP, and the process comprises the reduction of boron phosphate (BPO 4 ) with at least one alkaline earth metal (EA) according to mechanochemical reaction (1):
BPO 4 +4 EA→BP+4 EA(O)  (1).

9. The process of claim 1 , wherein the boron phosphide is B 12 P 2 , and the process comprises the reduction of boron phosphate (BPO 4 ) with at least one alkaline earth metal (EA) according to mechanochemical reaction (2):
2BPO 4 +5(EA)B 2 +3EA→B 12 P 2 +8EA(O)  (2).

10. The process of claim 1 , wherein the at least one alkaline earth metal is magnesium and/or calcium.

11. The process of claim 1 , wherein the mixture comprising boron phosphate and the at least one alkaline earth metal further comprises a chemically inert diluent.

12. The process of claim 6 , wherein it comprises:
(a) mixing boron phosphate, the at least one alkaline earth metal, optionally alkaline earth metal boride, and optionally a chemically inert diluent, provided as powders, so as to obtain a mixed powder,
(b) pre-milling said mixed powder with at least one ball at a first rotation speed of the ball-mill of between 50 and 200 rpm allowing for grinding the reagents,
(c) milling said pre-milled powder with at least one ball at a second rotation speed of the ball mill of between 400 and 1100 rpm enabling the reaction to occur, so as to obtain a milled powder which comprises the boron phosphide, the second rotation speed being superior to the first rotation speed,
(d) recovering boron phosphide from the milled powder.

13. The process of claim 10 , wherein the at least one alkaline earth metal is magnesium.

14. The process of claim 11 , wherein the chemically inert diluent is sodium chloride.

Assignees

• Univ Pierre Et Marie Curie Paris 6
• Centre Nat Rech Scient
• Univ Paris Xiii Paris Nord Villetaneuse
• Univ Paris Xii Nord Villetaneuse

Inventors

• Le Godec Yann
• Mukhanov Vladimir A
• Solozhenko Vladimir L
• Sokolov Petr S
• Vrel Dominique

Classifications

• C01B35/10

  Compounds containing boron and oxygen (C01B35/06 takes precedence) · CPC title

• C01B25/084 Primary

  of boron · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C01P2004/61

  Micrometer sized, i.e. from 1-100 micrometer · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title