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第四章 热分析 PowerPoint PPT Presentation


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第四章 热分析. Thermal Analysis. 第一节 热分析技术的概述. 一、热分析的定义 热分析是在程序控制温度下,测量物质的物理性质与温度之间关系的一类技术。 这里所说的 “ 程序控制温度 ” 一般指线性升温或线性降温,也包括恒温、循环或非线性升温、降温。这里的 “ 物质 ” 指试样本身和 ( 或 ) 试样的反应产物,包括中间产物 。. 热物理性质变化. 1.运输性质变化 2. 热力学性质(比热等)变化 3. 溶解(固相转变为液相) 4. 凝固(液相转变为固相) 5. 升华(固态直接转变为气态)

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第四章 热分析

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3505750

Thermal Analysis


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()


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1.

2.

3.

4.

5.

6.

7.

8.

9.

10.


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  • (ICTA)


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1.

2.

3.

4. 0.1g - 10mg

5. 10-5

6.

7.


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DTA

(Differencial Thermal Analysis)

  • DTA

  • (T)


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1

1-2-3-4-5-6-7-8-9-10-11-x-y


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TsTr

T=Ts-Tr tDTA()DTA


S r t t s t t s t r t

SRTTS;TTSTRT


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  • ATiBTmCTf

  • BDABC


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  • 1

  • N2Ne


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2 ,

  • :


Mnco 3 10 min 80 min

MnCO3 ():10/min,80/min


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  • 3

    100200


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  • NH4NO3DTA

  • a.5mg;b.50mg; c.5g


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CuSO45H2ODTA

  • a.1418

  • b.5272

  • c.72100

  • abc


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  • 4

  • -Al2O3)MgOSiCFe2O3Al2O3


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  • 5

  • ;


Thermogravimetric analysis

(Thermogravimetric Analysis)

(Thermogravimetry, TG)(Curve)


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  • TG

    m=f(T)


Curve

CURVE

WTtTGDTGTGdW/dT dW/dt

TG


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100

80

60

40

20

0

1.0

1.0

3.0

5.0

7.0

9.0

11.0

A

B

G

(%/min)

(%)

C

Tp

H

0 100 200 Ti 400 500 Tf 700

T(K)

DTG


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100

80

60

40

20

0

1.0

1.0

3.0

5.0

7.0

9.0

11.0

A

B

G

(%/min)

(%)

C

Tp

H

0 100 200 Ti 400 500 Tf 700

T(K)

TGBTiCTf(TG)


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100

80

60

40

20

0

1.0

1.0

3.0

5.0

7.0

9.0

11.0

A

B

G

(%/min)

(%)

C

Tp

H

0 100 200 Ti 400 500 Tf 700

T(K)

TiTfGTi(5%10%)TiHTfTpDTG


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TG

1

2

3

4

5


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1.

TiTf1020Kmin-1

0

100

0.42 2.5 10 40 100 240 480 Kmin

700 800 900 1000 1100

()


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CaCO3 CaO+CO2

CO2

1mg

400 600 800 1000 1200

()

2O2N2HeH2CO2 Cl2TGPPN2150-180C


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CaCO3 CaO+CO2

CO2

1mg

400 600 800 1000 1200

()

TG40-50ml/min


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3

W


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4


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TG

1

2

3

4

5

6


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(CuSO45H2O)

CuSO45H2O CuSO4 + 5H2O


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CuSO45H2OTGABBC CuSO45H2OCuSO43H2O+2H2O

A B

W0

W1

W2

W3

W0 -W1

W1-W2

W2- W3

W3

C D

(mg)

E F

G H

45 78 100 118 212 248

()


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CDDDE CuSO43H2OCuSO4H2O+2H2O

A B

W0

W1

W2

W3

W0 -W1

W1-W2

W2- W3

W3

C D

(mg)

E F

G H

45 78 100 118 212 248

()


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EFFGGH

CuSO4H2OCuSO4+H2O

A B

W0

W1

W2

W3

W0 -W1

W1-W2

W2- W3

W3

C D

(mg)

E F

G H

45 78 100 118 212 248

()


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A B

W0

W1

W2

W3

W0 -W1

W1-W2

W2- W3

W3

C D

E F

(mg)

G H

45 78 100 118 212 248

()

:

ABWo=10.8 mg

BCWo-W1=1.55mg=(Wo-W1)/ Wo=14.35%

DE1.6 mg,14.8%

FG0.8 mg,7.4%

= (Wo-W3)/ Wo=36.6%

36%


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A B

W0

W1

W2

W3

W0 -W1

W1-W2

W2- W3

W3

C D

E F

(mg)

G H

45 78 100 118 212 248

()

CuSO45H2O CuSO43H2O + 2H2O 14.4%

CuSO43H2O CuSO4H2O + 2H2O 14.4%

CuSO4H2O CuSO4 + H2O 7.2%


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(Differential Scanning CalorimeterDSC)

  • (DSC)ISO 11357-1DSCDSCDSC


Dsc dta

DSCDTA

DSC

DTAT-T DSCT = 0H-T DTADSC

DTADSC1960


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  • DSCDTATTt


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DSCdH/dtmWTt

DTADSC(endothermic) ()(exothermic)()


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T()

dH/dt(ail/s)

DTA

DSC

Tg Tc Tm Td


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