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Fe-Al(Ga)-O 01.04.07

-

­ 2014


. . .

: - : , - , , «» , - , , : . .. " 15" 2014 . . 501.002.01 . . : 119991, -1, , , .1, . 35, , -. .. ( ., .27) " " 20 . ,

501.002.01 -
2

. .


Al2O3, Ga2O3, Cr2O3 : , . , ,



,

. . , , . , . / , . , Fe2O3­Al, Fe2O3­Ga, Fe2O3­Ga­Fe, Fe­Al Fe­Al­Cr2O3 . Fe:Al FeAl-O, , ( Fe Al
3





.


) , .

. ( , , (), -)

, . Fe Al, Ga, Fe, Fe2O3­Al, Fe2O3­ Ga, Fe2O3­Ga­Fe, Fe­Al Fe­Al­Cr2O3 . Fe2O3­Al ( ), / Al2O3. , Fe2O3­Ga Fe2O3­Ga­Fe Fe2O3­Al. FeAl-O Fe2O3­Al , . Fe-Al-O, , ,
4


. 1. , Fe2O3­Al, Fe2O3­Ga Fe2O3­ Ga­Fe. 2. Fe2O3­Al , /. 3. , Fe­Al Fe­Al­Cr2O3

-Fe(Cr,Al)/Fe0.7-xCrxAl0.3/Al2O3 4. Fe-Al-O, , , . 5. . , , Fe2O3­Al, Fe2O3­Ga, Fe2O3­Ga­Fe, Fe­Al Fe­Al­Cr2O3, Fe-Al-O .

5


, , , ( , ). . : 10- «-2007» (2007 ., , ); , , - (2007 ., 2009 . , ); 14
th

International Syphosium on Metastable and Nano- Materials

ISMANAM-2007 (2007, Corfu, Greece); III - , IC-CCPCM'2008 (2008, , ); 16th International Conference on Solid Compounds of Transition Elements SCTE-2008 (2008, Dresden, Germany); CALPHAD XXXVIII (2009, Prague, Czech Republic); III " " FNM-2010 (2010, , ); International Symposium on Advanced Complex Inorganic Nanomaterials ACIN 2011 (2011, Namur, Belgium). . 15 : 6 ( 5 , ) 9 . . 125 , 47 12 , , , 163 . .. .
6


, , , , . . /(), . , - , , , . / - Fe2O
3

-. . . , : · ­ , ­ , , . · () ­ , ,

7


. · () . · - , . , , . III-VI. , . III Fe2O3 ­ xAl (x = 2; 4; 6; 8) (t = 40" 2') . (, ) - () -Fe2O3 -Fe : -Fe2O3 + Fe2-xxO3 Fe3-xxO4 Fe1-xxO -Fe + Me2O3 , .. Fe.
8


, Fe2O3­2Al, -, - , . 1.

40''
. , % . , %
1.00 1.00

120''
a-Fe2O3 a-Fe Fe2Al5

0.99



0.99

0.98

0.97

2Al
-10 -8 -6 -4 -2

0.98

2Al
-10 -8 -6 -4 -2

0.96

-12

V, /

0

2

4

6

8

10

12

-12

V, /

0

2

4

6

8

10

12

1.00

. , %

. , %
-8 -6 -4 -2 0 2 4 6 8 10 12

1.00 0.98 0.96 0.94 0.92

0.95



0.90

4Al
0.85 -12 -10

4Al
-10 -8 -6 -4 -2 0 2 4 6 8 10 12

0.90 -12

V, /

V, /

1.0

. , %

. , %
-8 -6 -4 -2 0 2 4 6 8 10 12

1.00



0.99

0.5

0.98

6Al
-12 -10

0.97

6Al
-10 -8 -6 -4 -2 0 2 4 6 8 10 12

-12

V, /
1.01 1.01

V, /

. , %

1.00 0.99 0.98 0.97 0.96 0.95 -12

. , %
-8 -6 -4 -2 0 2 4 6 8 10 12

1.00 0.99 0.98 0.97 0.96



8Al
-10

8Al
-10 -8 -6 -4 -2 0 2 4 6 8 10 12

V, /

0.95 -12

V, /

. 1. ( =300 ) Fe2O3 ­ xAl (x = 2; 4; 6; 8), 40 120 .
9


40''
Fe2Al5 , FeAl AlxO
90 80 70 60 50 40 30 20 10 0 2Al

120''
100 90 80 70 60 50 40 30 20 10 0

2

AlxO

4

100

FeAl Fe2Al5 , FeAl FeAl Fe2Al5 , FeAl
2

4

2

-Fe2O

Fe3O

3-x

-Fe


-Fe2O
3

Fe

Fe3O

FeAl

3

50 40 30 20 10 0

-Fe2O

50 40 30 20 10 0

4Al

4Al
100

Fe3-x AlxO

-Fe2O



100 90 80 70 60 50 40 30 20 10 0

2

Fe2Al5 , FeAl

3

4

80 70 60 50

Fe2Al5 , FeAl
6Al

4

2
90 70 60 50 30 20 10 0

90

Fe3O

FeAl

-Fe

40 30 20 10 0

6Al

100 90 80

100

2

Fe2Al5 , FeAl

-Fe2O

50 40 30 20 10 0

-Fe

8Al

Fe3O

FeAl

8Al

. 2. Fe2O3 ­ xAl (x = 2; 4; 6; 8), 40 120 . , (. 2), ,
10

-Fe

40

-Fe2O

Fe3O

60

4

3

70

FeAl Fe2Al5 , FeAl

80

3

4

2

-Fe

-Fe

60

-Fe

70

80

Fe3-x AlxO

4

90

Fe2Al5 , FeAl

2

100

100 90 80 70 60

Fe

4

3-x

2Al

-Fe

3

4












. (. 2) 40 -Fe (41% ), Fe2Al5 , FeAl2 (5%), Fe3O4 (6%) Fe3-xAlxO4 (44%). 120 : - Fe2O3 (2% ), -Fe (60%), Fe2Al5 , FeAl2 (6%), Fe3O4 (6%) Fe3-xAlxO4 (27%), FeAl (2%). (. 2) (. 2) Al , 2 -Fe FeAl, Fe2Al (FeAl2) (. 2). Al (. 2) 40 , -Fe . , , , . (. 3) .
5

11


8Al

-

-Fe2O3 Al FeAl2 Fe2Al5

. 3. , 2 Fe2O3 + 8Al , (. 4), . -Fe2O3

Fe2O3, . . %

. . %

100 80 60 40 20 0 0 20

Fe3-xAlxO4, . . %

40

100 80 60 40 20 0 0 20 40

Fe3-xAlxO4

Fe2Al5, . . %

60 80 100 120 ,

100 90 80 70 60 50 40 30 20 10 0 0 100 80 60 40 20 0 0

-Fe

alpha e, -F

20

40

60 80 100 120 ,

Fe2Al

5

60 80 100 120 ,

20

40

- 2Al - 4Al

- 6Al - 8Al

60 80 100 120 ,

. 4. Fe2O3 + xAl (x = 2, 4, 6, 8)

12


Al . Al . Al , . IV Fe2O3­Ga, Fe. Ga - , (III ). Fe-Al Fe-Ga «» . - Al -1.67 , 3 Ga (-0.52 ). Al Ga. (Ga T=29.6 oC, Al T=660.2 oC). , , Ga , . , ( 40 1, 2, 4 8 . ) Fe2O3­Ga , . 5. , -Fe2O3. 8 48% , .
13


a-Fe2O3 Fe3O4 Fe3Ga Fe2-xGaxO3

1.005 1.000

FeGa3

Ga x O

Ga x O

0.995 0.990 0.985 0.980 0.975
40

2- x

3- x

0.970 -12

-10

-8

-6

-4

-2

0

2

4

6

8

10

12

v, /

1.005

100 90

Fe

Fe

0.980 0.975 0.970 -12
1

-10

-8

-6

-4

-2

0

2

4

6

8

10

12

10 0

v, /

1.005 1.000

100 90

Fe

0.990 0.985 0.980 0.975 0.970 -12
2

Fe

Fe

-10

-8

-6

-4

-2

0

2

4

6

8

10

12

10 0

v, /

1.005

.

0.990 0.985 0.980 0.975
4

Fe

Fe

30 20
-8 -6 -4 -2 0 2 4 6 8 10 12

0.970 -12

-10

10 0

v, /

1.005

Ga x O

Ga x O

0.995 0.990 0.985 0.980 0.975
8

2- x

3- x



Fe 3 Ga , F e Ga

.

1.000

0.970 -12

-10

-8

-6

-4

-2

v, /

0

2

4

6

8

10

12

100 90 80 70 60 50 40 30 20 10 0

Fe

3

4

-F e 2 O

Ga x O

3

3

. 5. ( =300 ) Fe2O3­Ga 40 (), 1 (), 2 (), 4 () 8 () .
14

Fe

-F e

Fe

Fe

1- x

-F e

1- x

40

2- x

3- x



50

-F e 2 O

60

Ga x O

3

70

Ga x O

Ga x O

0.995

80

Fe 3 Ga , F e G a

90

3

4

3

1.000

100

Fe

30 20

-F e

1- x



-F e 2 O

2- x

3- x

Ga x O

3

0.995

60 50 40

Fe 3 Ga , F e Ga

.

Ga x O

Ga x O

80 70

3

4

3

-F e

30 20

2- x

3- x



0.985

-F e 2 O

0.990

1- x

Ga x O

0.995

60 50 40

Fe 3 Ga , F e Ga

.

1.000

Ga x O

Ga x O

80 70

Fe

3

3

4

3

-F e



100 90 80 70 60 50 40 30 20 10 0

Fe 3 Ga , F e Ga

.

3

4

-F e 2 O

Fe

Fe

1- x

Ga x O

3

3


, (12%), (30%) -Fe (2%). , Fe2O3­Ga Fe2O3­Al Al (. 2). , , -Fe2O3. , 2 . Fe2O3­Ga, (. 6). -Fe2O3 ( 100-120 ), .

-Fe2O

3

-Fe2O

3





. 6. , 2 Fe2O3 + 2Ga () Fe2O3 + 2Ga+Fe () -Fe -,
15


1.005 1.000

90 80 70

Fe3Ga, FeGa

100

3

.

Fe3-xGaxO

0.985 0.980 0.975 0.970 0.965 40 -12 -10 -8 -6 -4 -2 0 2 4 6 8 10 12

30 20 10 0
V, /



100
1.005 1.000

.

Fe2-xGaxO

Fe3-xGaxO

0.995 0.990 0.985 0.980 0.975 0.970 0.965 1 -12 -10 -8 -6 -4 -2



20 10
V, /
0 2 4 6 8 10 12

0
100 80

.

Fe2-xGaxO

0.985 0.980 0.975 0.970 0.965 2 -12 -10 -8 -6 -4 -2 0 2 4 6 8 10 12

40 30 20 10 0
V, /

-Fe2O

0.990

3

50

Fe1-xGaxO

0.995

Fe3-xGaxO

60

3

4

1.000

Fe(Ga, O) Fe(Ga, O) Fe(Ga, O)

1.005

70

Fe3Ga, FeGa

90

3



100
1.005

80 70

.

1.000 0.995 0.990 0.985 0.980 0.975 0.970 0.965 4 -10 -8 -6 -4 -2 0 2 4 6 8 10 12

Fe2-xGaxO

Fe3-xGaxO

40 30 20 10 0
V, /

-Fe2O

3

50

Fe1-xGaxO

60

Fe3Ga, FeGa

3

4

3

90



-12

90
1.005 1.000

80

.

Fe2-xGaxO

Fe3-xGaxO

0.995 0.990 0.985 0.980 0.975 0.970 0.965 8 -12 -10 -8 -6 -4 -2 0 2 4 6 8 10 12



30 20 10 0

V, /

. 7. ( =300 ) Fe2O3­ Ga­Fe 40 (), 1 (), 2 (), 4 () 8 ()

16

-Fe

40

-Fe2O

50

3

60

Fe1-xGaxO

70

Fe3Ga, FeGa

100

3

4

3

-Fe

-Fe

-Fe

30

-Fe2O

50 40

Fe1-xGaxO

60

Fe(Ga, O)

3

70

Fe3Ga, FeGa

90 80

3

4

3

-Fe

40

-Fe2O

50

3

0.990

60

Fe1-xGaxO

0.995

Fe2-xGaxO

Fe(Ga, O)

3

4


(T

. Fe

=1539 oC) =29.6 oC) Al (T
. Al

Ga (T

. Ga

=660.3 oC).

, ( 40 1, 2, 4 8 . ), . 7. Fe(O) . , .. Fe2O3 +4Fe. Fe2O3­Ga Fe2O3­Ga­Fe , , -Fe2O3. ­ , Fe , -Fe2O3 . . (. 7): , 120-140 . , ­ ­ . , Fe2O3 + Ga + Fe -Fe2O3 , Fe2O3­Ga, Fe(O). , ,
17


. -Fe2O3 4 . V , () Fe-Al Fe-Al-Cr2O3. . .

. 8. : () 1 ; () 2 ; () 1 ; () 2 ;
18


, Fe-Al (. 8 , ) , 1 Fe2Al5/FeAl2. 2 7%. (. 8 , ). (. 9) , 2 FeAl 1 -Fe(Al) Fe2Al5.

. 9. : () 1 ; () 2 , Fe­Al, Fe Al 19


Cr2O3 . (. 10 ), 1 , Fe Al Fe2Al5.

. 10. (=300 ) 8.1 .% Cr2O3 + 66.9 .% Fe + 24.0 .% Al () 1 () 1 Fe­Al­Cr2O3 -Fe(Cr,Al)/Fe0.7-xCrxAl0.3/Al2O3.

20


VI Fe:Al Fe-Al-O, . , . -FeOOH Al(OH)3, = 400 . Fe Al . , , Fe . , 15 % Fe (. 11 ), , Fe3O4, , FeAl2O4. , 90 %, : (.. ), , , . , (. 12), , , , . , , , .
21




A


a-Fe
1.02

a-Fe
1.02

Sp Fe3O4
.

Sp Fe3O

4

.

1.00 0.98 0.96 0.94 0.92 0.90 0.88 0.86 0.84 -12 -10 -8 -6 -4 -2 0 2 4 6 8 10

1.00 0.98 0.96 0.94 0.92 0.90 0.88 0.86 0.84 -1 2

15Fe - 85Al2O3 V, /

15Fe - 85Al2O3
-1 0 -8 -6 -4 -2

12

V, /

0

2

4

6

8

10

12

1.02

1.02

.

1.00 0.98 0.96 0.94 0.92 0.90 0.88 -12 -10 -8 -6 -4 -2 0 2 4 6 8 10

.

1.00 0.98 0.96 0.94 0.92 0.90 0.88 -1 2

25Fe - 75Al2O

3

25Fe - 75Al2O
-1 0 -8 -6

3

12

-4

-2

0

2

4

6

8

10

12

V, /
1.01 1.01

V, /

.

0.99 0.98 0.97 0.96 0.95 -12

.

1.00

1.00 0.99 0.98 0.97 0.96 0.95 -1 2

50Fe - 50Al2O
-10 -8 -6

3

50Fe - 50Al2O
-1 0 -8 -6

3

-4

-2

V, /

0

2

4

6

8

10

12

-4

-2

V, /

0

2

4

6

8

10

12

1.01

1.01

.

1.00 0.99 0.98 0.97 0.96 0.95 0.94

.

1.00 0.99 0.98 0.97 0.96 0.95 0.94 -1 2

75Fe - 25Al2O3
-12 -10 -8 -6 -4 -2

75Fe - 25Al2O3
-1 0 -8 -6 -4 -2

V, /

0

2

4

6

8

10

12

V, /

0

2

4

6

8

10

12

1.01

1.01

.

0.99 0.98 0.97 0.96 0.95

.

1.00

1.00 0.99 0.98 0.97 0.96 0.95
-12

90Fe - 10Al2O3
-12 -10 -8 -6 -4 -2

90Fe - 10Al2O
-10 -8 -6

3

V, /

0

2

4

6

8

10

12

-4

-2

V, /

0

2

4

6

8

10

12





. 11. , 400 .
22


100 90 80 70

100 90 80 70

Sp Fe3O4

15Fe

Fe Al2O4

50 40 30 20 10 0

50

-Fe

40 30 20 10 0

100

90 80 70 60 50 40 30 20 10 0

100 90 80

Sp Fe3O4

Sp Fe3O4

25Fe

Fe Al2O4

Fe Al2O4 (Fe,Al)O (Fe,Al)O

-Fe

-Fe

100 90 80

100 90 80 70 60 50 40 30 20

20 10 0

Fe3-x AlxO4

50Fe

(Fe,Al)O

Fe3-x AlxO4

20 10 0 100 90

10 0 100

90

-Fe

(Fe,Al)O

50 40 30 20 10 0 100 90

Fe3-x AlxO4

30 20 10 0 100 90 80 70 60 50 40 30 20 10 0

Fe3-x AlxO4

Fe3-x AlxO4

90Fe

(Fe,Al)O

30 20 10 0

(A)

(B)

. 12. , (A) ­ , () ­ 400

23

-Fe

60 50 40

-Fe

80 70

-Fe

60 50 40

Fe3-x AlxO4

75Fe

80 70 60

80 70

-Fe

70 60 50 40 30

-Fe

70 60 50 40 30

Fe Al2O4

60

60

Sp Fe3O4


, : Fe . . , , , -Fe. . , , 75 % Fe 77% . , . 12 , Al2O3, . 15 % Fe 78% Al2O3 22% . 90 % Fe , , 91% 9% Al2O3. Fe-Al-O, Fe Al 1 : 2 (. 13). (. 13) -Fe , : Fe3-xAlxO4. , ,

-Fe2O3 /Al2O3.
24


.

1.01 1.00 0.99 0.98 0.97 0.96 0.95 -1 2


.

1.0 1 1.0 0 0.9 9 0.9 8 0.9 7 0.9 6 0.9 5 -1 2



50 F e - 50 A l 2O
-1 0 -8 -6

3

50 F e - 50 A l 2O
-1 0 -8 -6

3

-4

-2

0

2

4

6

8

10

12

-4

-2

0

2

4

6

8

10

12

V, /

V, /

1.00

.

0.98 0.96 0.94 0.92 0.90 - 12

4A l
- 10 -8 -6 -4 -2 0 2 4 6 8 10 12

V, /



. 13. , ( - , - ) 400 () , , , . , , , . 750 1 . 90 % Fe, , (. 14)

. , , (.
25


14 ). . , , , (. 14 ). , , (Fe3) Fe3-xAlxO4. , , , - . . .

A



. 14. 90 % Fe . VII , .

26


, Fe-Al-O - -Fe2O3 + Al Fe - -Fe2O3 + Al Fe2-x Al xO3 Fe3-x Al xO4 Fe1-x Al xO -Fe + Al 2O3 . . Fe2O3­Ga Fe2O3­Ga­Fe. Fe­Al­Cr2O3
2-x

Al xO3 Fe3-x Al xO4 Fe

1-x

Al xO -Fe + Al 2O3

-Fe(Cr,Al)/Fe0.7-xCrxAl0.3/Al2O3. Fe-Al-O, , . , . : 1. Fe2O3­xAl Fe2O3 /Al2O3 x < 8. 2. , /Al2O3
27


Fe2O3­6Al. 40 . . 3. Al (x=8) (-Fe2O3), . 4. Fe . -Al2O3 Fe3-xAlxO4. 5. Fe2O3­2Ga , (Fe2O3­8Al). 6. Fe2O3­Ga . Fe2O3 , Fe2O3­Ga, Fe(O), . : 1) Fe-Al , . / .. , .. , .. , .. , .. , .. // . 3. . . ­ 2008 ­ 1. ­ . 56­61 2) Mechanoactivated interaction of hematite and gallium. / Falkova A.N., Novakova A.A., Kiseleva T.Yu., T.F. Grigorieva, Barinova A.P. // Journal of Alloys and Compounds. ­ 2009. ­ V. 480. ­ P. 31­34. 3) / / .., .., .., .., .. // . 3. . . ­ 2008. ­ 4. ­ . 62­64. 4) - Fe-Al-O / ..,
28


.., .., .., .. // . ­ 2011. ­ 11. ­ C. 63­64. 5) Fe0.70-xCrxAl0.30 /Al2O3 Cr2O3 + Fe + Al / .., .., .., .., .. // . ­ 2009. ­ . 45. ­ 7. ­ C. 1­5. 6) .., .., .., .. " ". 2009 7) .., .. " Fe2O3 " (XIV , -2007, , , 12 2007, . 278) 8) Novakova A.A., Kiseleva T.Yu., Falkova A.N. ,Potapkin V.B., Grigorieva T.F., Barinova A.P., Lyakhov N.Z "Structural evolution of Fe2O3 during its reduction with aluminum in the process of mechanosynthesis of nanoscaled compounds" (Proceedings of 14th International Symphosium on Metastable and Nano- Materials. ISMANAM-2007, Corfu, Greece 26-30 August. 2007. P.179) 9) .., .., .., .., .. " Fe2O3 ", (VI , , -2007, , , 12-17 2007, . 177) 10) .., .., .., .., .., .. " Fe2O3 .", (III - , IC-CCPCM'2008, , , 24-28 2008, . 78) 11) Falkova A.N., Novakova A.A., Kiseleva T.Yu., T.F. Grigorieva, Barinova A.P. "Mechanoactivated interaction of hematite and gallium" (Proceedings of 16th International Conference on Solid Compounds of Transition Elements, SCTE-2008, Dresden, Germany, 26-31 July, 2008, p. 80-81) 12) A.A. Novakova, A.N. Falkova, T.Yu. Kiseleva, T.F. Grigorieva, A.P. Barinova "Mechanoactivated phase transformations in hematite ­ gallium system" (CALPHAD XXXVIII, Prague, Czech Republic, 17-22 May 2009, p. 111) 13) .. , .. , .. , .. , .. " , - " (VII , ,
29


--- , - 2009, , , 16-21 2009, . 396) 14) .., .., .., .., .. " - Fe-Al-O " (III " ", FNM-2010, , , 4-8 2010) 15) Falkova A.N., Novakova A.A., Levina V.V., Ilinyh I.A., Chuprunov K.O. "The Effect of Fe-Al-O Nanocomposites Morphology on their Catalytic Properties" (Proceedings of International Symposium on Advanced Complex Inorganic Nanomaterials, ACIN 2011, 2011, Namur, Belgium, 11-14 September, 2011, p. 273)

30