CHUN B MU NGHIN CU T CHC KIM LOI

1. MC CH YU CU
Sinh vin nm c:
1. Phng php lm mu nghin cu t chc t vi gm cc khu: chn mu, ct mu, mi, nh bng
v tm thc.
2. Tm quan trng ca cng tc chun b mu v nh hng ca n n kt qu nghin cu.
3. Lm quen vi nhng vt liu v thit b cn thit cho cng vic lm mu.
4. Chn dung dch tm thc cho thch hp.

2. L THUYT
nghin cu t chc t vi ca kim loi, ngi ta dng mt thit b quang hc c bit gi l knh hin vi
kim tng. Phng php dng knh hin vi kim tng nh gi, phn tch t chc t vi gi l phng php
phn tch kim tng.
Knh hin vi kim tng c phng i t 80 n 2000 ln. Mun quan st vi phng i cao hn,
ta phi dng knh hin vi in t.
Nh knh hin vi, ta c th quan st c t chc ca cc pha, s phn b, hnh dng v kch thc ca
chng. Vi gang, ta d dng xc nh hnh dng, kch thc ca graphit. Ngoi ra, ta cn c th thy c cc
khuyt tt ca vt liu nh: nt t vi, r v cc tp cht.
Trnh t ch to mu nh sau
2.1 Chn v ct mu
Ty theo nhim v nghin cu v th nghim m chng ta chn mu. Yu cu mu phi c trng cho vt
cn nghin cu. V d: khi mun quan st s thay i t chc t b mt vo li, ta phi ct mu theo tit din
ngang, cn mun nghin cu t chc dng th, si, ta phi ct theo dc trc
Khi ct mu, c th dng cc my ct kim loi nh tin, phay hoc ca my, ca tay
Cc mu qu cng, c th dng mi ct. Vi cc thp v gang qua nhit luyn, yu cu i vi
nhit ni ct khng qu 100o C.
Mu c dng hnh tr vi kch thc 10 15mm, chiu cao h= 15 20mm, hoc hnh hp c kch thc
10 x 10 x 10mm v 15 x 15 x 15mm.
Nu mu c kch thc nh, mng, phi nhin cu lp b mt (thm cacbon, n mn b mt) th mu
cn phi c kp vo cc g hoc khun bao quanh. Cht khun thng l cc hp kim c nhit
chy thp nh hp kim:
Bi = 50%

Cd = 10%

Pb = 27%

Sn = 13%

to nc = 70o C

Bi =56%

Cd = 18%

Pb = 14%

Sn = 14%

to nc = 56o C

hoc cc cht nha do, bakelit

2.2 Mi mu
a) Mi th
Mu sau khi ct c mi th trn mi hoc giy nhm t th n mn.
Cc giy nhm thng c nh s t nh n ln. S cng ln th ht ca giy cng mn. V d: 80,
100, 150, 180400 l cc s thng dng.
trnh lm rch giy nhm khi mi, ngi ta thng vt mp mu.
Giy nhm phi c t trn b mt tht phng hoc mt tm knh dy. B mt mu phi p st vo giy.
Khi mi tin hnh theo 1 chiu. Yu cu l to trn b mt tng i phng, c cc vt xc song song v u
nhau. Sau , ta quay mu i 90o v mi tip, cho n khi to ra b mt phng mi, h xc mi xa ht cc
vt ca h xc c. Mi loi giy nhm, ta mi nhu th 3-5 ln, v lp li cc s giy nhm mn hn, c nh
vy, cho n t giy nhm mn nht.
Mi th cng c th tin hnh trn my. My n gin l mt mt thng ng, trn c gn 1 a kim loi
phng. Ngi ta ln lt dn cc giy nhm c s t th n mn ln a cho mt quay ri mi. Ch khng
nhit tng qu nhit chuyn bin pha ca mu mi.
b) nh bng
nh bng mu, ngi ta tin hnh trn my nh bng. Cng tng t nh my mi th, thay v dn
t giy nhm ln a, ngi ta gn mt ming d hay n ln trn, khi nh bng, ngi ta phi cho dung dch
mi nh lin tc ln ming n. Thnh phn ca dung dch nh bng nu bng 1. Vi cc vt liu mm nh
kim loi mu, nn dng cc loi dung dch mn. trnh b oxy ha khi nh bng, ngi ta pha vo dung
dch cc cht th ng ha nh NaNO2 , KNO2
Bng 1. Dung dch dng nh bng
Tn gi cc cht
Cr2 O3
Al2 O3
Paraphin
Axit leic C17 H33 CO2 H
Du ha
Na2 CO3

Dung dch oxit crm (%)

Mn
Trung bnh
Th
72
76
86
24
20
12
1,8
1,8
2
2
2
0,2
0,2
-

Dung dch oxit nhm (%)

Mn
Trung bnh
Th
32
35
37
32
35
37
30
24
20
3
2
3
2
2
2
1
1
1

nh bng ko di cho dn khi b mt khng cn vt xc no. Khng nn nh bng qu lu, d lm

trc cc pha qu cng hoc qu mm. Sau khi nh bng, em ra sch v sy kh. Nu quan st trn knh
hin vi thy vn cn nhiu vt xc, th phi nh bng li.
c) nh bng in phn
Nguyn tc ca nh bng in phn l dng phng php ha tan anod trong dung dch in phn di
tc dng ca dng in mt chiu (Hnh 1).

A
1
2

V
+

Hnh 1. S nh bng in phn

S nguyn l gm mu nh bng 1, nhng trong cht in phn 2 v ni vi cc dng ca ngun.
Cc m l tm km hay niken, t cch b mt mu 1 khong nht nh. Khi mt dng in ln, th
nhp nh ca mu b ha tan v mu s phng v bng.
Ty theo ch in, m ta c th nh bng v tm thc mu ngay trn my.
nh bng in phn c u im l rt bng v khng to ra lp bin dng trn b mt mu, thi gian
tng i nhanh.
Dung dch v ch nh bng in phn ca cc vt liu xem trong bng 2.
Bng 2. Ch nh bng in phn thng dng
STT

Kim loi

Tt c cc kim
loi en

Thp khng g

5
6
7

ng v ng
thau
ng thanh
Nhm v hp
kim nhm

Thic

Thnh phn dung dch

in phn (ml)
HCl
185
CH3 COOH
768
Nc
50
HCl
70
Cn etilic
800
Nc
130
H3 PO4
38
Glixerin
53
Nc
9
HCl
85
Cn etilic
800
Nc
115
H3 PO4 (1,48)
H3 PO4 (1,55)
H2 SO4 (1,19)
H3 PO4
Nc
H3 PO4
HF
Nc
HCl(1,6)

38
48
14
40
100
2800
100

Mt dng
in (A/dm2 )

Ch in phn
in p Nhit
(V)
(0 C)

Thi gian
(pht)

47

50

30

410

250 400

35 70

35

0,25 0,5

0,2 2

20 - 100

50 - 60

25 - 30

26

12

20

12

35

1,4 2

20

35

90 95

5 10

7,5

0,02 0,06

10 25

30 35

5 10

0,4

50 60

< 35

0,2 0,3

2.3 Tm thc
Mu sau khi nh bng, em ra sch, thm v sy kh ri quan st trn knh hin vi. Ta c th thy trn
mu c c vt xc nh do nh bng cha tt, cc vt nt t vi, r kh, x tp cht, mt s pha v t chc nh
cacbit, graphit, ch
3

Mun nghin cu nn kim loi, phi tm mc mu. Tm thc l qu trnh n mn b mt mu bng cc

dung dch ho hc thch hp, gi l dung dch tm thc. Khi tm thc, bin gii cc pha, cc vng t chc s
b n mn, nhng vi nhng tc khc nhau. Sau khi tm thc b mt mu s li, lm tng ng vi cc
pha v t chc. Do , c th nhn bit c hnh dng, kch thc v s phn b ca cc pha.

Bng en

a)

Xe

Sng

b)

Hnh 2. Mu peclit tm trc v sau tm thc

Trn hnh 2 nu ln s phn x nh sng ca thp cng tch peclit tm trc (H2a) v sau (H2b) tm
thc.
Khi tm thc, c th nhng b mt mu vo dung dch, hoc ly que tre, c thy tinh c qun bng u
ri nhng vo dung dch tm thc v bi u ln b mt mu. Thi gian tm thc ty thuc vo t chc v
trng thi ca vt liu, c th t vi giy cho n vi gi. Cng c th tm thc da vo kinh nghim. Sau khi
bi dung dch tm thc, b mt mu s ng t mu sng sang mu xm th ta c th kt thc tm thc. lu
qu, mu s c mu en v khng quan st c.
Tm thc xong, phi dng bng nn ra sch b mt vi nc chy, sau ra li bng cn v em sy
kh.
Nu quan st sau tm thc, ta thy cc ng bin gii nh, t on l tm thc cha thi gian, phi
em tm thc li. Ngc li, cc ng bin gii qu to, m, tng phn b mt km, l do thi gian
tm thc qu di, hoc nng dung dch cao. Ta phi em nh bng v tm thc li.
Thng khi quan st vi phng i b th thi gian di hn khi quan st vi phng i ln
Thnh phn v ch tm thc nu trong bng 3.
Bng 3. Cc dung dch tm thc thng dng
Thnh phn dung dch
- 4% acid HNO3 trong cn
- 4% acid picric trong cn
- Dung dch picrat natri
- 20 cm3 HCl m c + 5g CuSO4
- 3 phn HCl + 1 phn HNO3
- Dung dch 0,5% HF trong nc
- 1%HF + 2,5%HNO3 + 1,5%HCl + 95%H2 O
- 3% FeCl2 trong dung dch 10%HCl
- 2 4 % HNO3 trong cn

Cng dng
Gang, thp cacbon
-ntPhn bit F v Xe
Thp bn nng
Thp khng g
Hp kim nhm
-ntHp kim ng
Babit v hp kim magi
4

Ghi ch

Dng ngay sau pha

3. THIT B VT T
-

My ct mu
My mi mu
My nh bng mu
My tm thc in phn mu
Knh hin vi kim tng
Giy nhm cc c
Ha cht
Mu gang, thp cc loi
Bng nn
Thit b sy

4. NI DUNG TH NGHIM
-

Mi sinh vin c giao mt mu thp hoc gang v giy nhm cc c.

Nhim v ca sinh vin: mi th bng giy nhm, nh bng v tm thc mu. Quan st mu trc v
sau khi tm thc.

5. NI DUNG BO CO
-

Tm tt trnh t lm mu d nghin cu t chc t vi vo v th nghim.

Nhn xt mu trc v sau khi tm thc, cc t chc quan st thy.
Gio vin hng dn s chm kt qu lm mu ngay ti phng th nghim.

H v tn: ..........
MSSV:
Lp: .......
Nhm T: ......
Mu th nghim s: ......
Ngy lm th nghim: ..........

BO CO TH NGHIM CHUN B
MU NGHIN CU T CHC
KIM LOI

1. Tm tt trnh t lm mu th nghim

.
2. Kt qu quan st t chc kim loi

Mu trc khi tm thc

Mu su khi tm thc

4. Nhn xt