CN1552660A - Indium-tin oxide powder with low radiation rate at infrared spectrum and its preparation - Google Patents
Indium-tin oxide powder with low radiation rate at infrared spectrum and its preparation Download PDFInfo
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- CN1552660A CN1552660A CNA031289053A CN03128905A CN1552660A CN 1552660 A CN1552660 A CN 1552660A CN A031289053 A CNA031289053 A CN A031289053A CN 03128905 A CN03128905 A CN 03128905A CN 1552660 A CN1552660 A CN 1552660A
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Abstract
An indium tin oxide powder with low emissivity (0.65-0.75) in infrared waveband is prepared from tin oxide (2-15 wt.%) and indium oxide (85-98 wt.%). It can be used for infrared camouflage of weapon or photoelectric hiding engineering.
Description
Technical field
The present invention relates to a kind of tin indium oxide (Indium Tin Oxide) powder and preparation method thereof, relate in particular to a kind of tin indium oxide as infrared low-emissivity material.
Background technology
Tin indium oxide (Indium Tin Oxide) is a kind of n N-type semiconductorN material, is called for short ITO.Because it has excellent photoelectric characteristic, thereby is developed rapidly in recent years.For the ito thin film material, it is ripe that technology of preparing has been tending towards, and product is widely used in many fields such as plane liquid-crystal display, electrode of solar battery, thermal radiation speculum, has formed certain market scale.And ito powder as transparent electrode material, the preparation ito thin film target and infrared low-emissivity material also be subjected to extensive concern recently.
Infrared stealth technology is at means such as infrared imaging, infrared guidance and infrared reconnaissances and the infrared target control techniques that grows up.The infrared stealth material is a military material of hi-tech that emerges the middle and later periods in 20th century, makes infrared stealth coating or the stealthy shield of infrared camouflage color with different infrared emittances with it, can realize stealthy for military target.Because the emittance of general material makes present research emphasis concentrate on the infrared low-emissivity material with the stealthy performance of compatible multiband all than higher, it is " bottleneck " in the infrared stealth material.
Metal is the pigment that is used for infrared stealth coating of reporting maximum up to now, it can reduce the infrared emittance of coating greatly, but has very strong reflection for visible light and radar wave, therefore be unfavorable for visible light and radar invisible, and metallic pigment oxidation easily in air, infrared emittance can increase substantially after the oxidation.
The ito powder of high temperature sintering, stable performance has the stealthy compatible basis of good multiband; Can change emittance by changing doping control infrared external reflection spectrum, make it meet the requirement of infrared stealth; Multiple preparation method is arranged.The ito powder of high temperature sintering is good semiconductor material.Through high temperature sintering, Sn
4+Replaced In
2O
3In in the lattice
3+, in order to keep electric neutrality, the Sn that easily appraises at the current rate
4+To capture an electronics and become Sn
4+.e, this electronics and Sn
4+Contact be that weak beam is tied up, move easily, be the main source of current carrier, and carrier concentration is a principal element that influences the ito powder emittance.
Ito powder generally has two kinds of preparation methods: solid phase method and liquid phase method, solid phase method are with In
2O
3And SnO
2Directly mixed also sintering.The ito powder size distribution that makes thus is inhomogeneous, and the semiconductor degree is poor; Liquid phase method is with In
3+And Sn
4+Form with oxyhydroxide deposits out, obtains precursor powder sintering again.The ito powder that obtains thus, semiconductor is complete, and size distribution is even, and process repeatability obviously is better than solid phase method.
Because the research to the infrared low-emissivity powder directly applies to military field, various countries strictly maintain secrecy, and open report is very few.Domestic aspect, PLA's Institute Of Electrical Engineering employing solid phase method prepares ito powder and is used for infrared stealth coating as infrared low-emissivity material.Similarly work was done in space flight 703, but did not see disclosed technology report.The patent of being reported at present mainly concentrates on the research to ito thin film, the research of ito powder is then mainly concentrated on the target aspect of transparent electrode material and preparation ito thin film.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of tin indium oxide powder that has low-launch-rate at infrared band and preparation method thereof, overcoming defectives such as the inhomogeneous and semiconductor of size distribution that prior art exists is incomplete, and satisfy the needs that have association area to use.
Technical scheme of the present invention:
Component and the weight content that has a tin indium oxide powder of low-launch-rate at infrared band of the present invention comprises: stannic oxide 2%～15%, Indium sesquioxide 85～98%, be the powder of a kind of median size 0.5～2 μ m, (wavelength 8～14 μ m) average emitted rate of its infrared band is 0.60～0.75.
Tin indium oxide powder of the present invention adopts chemical coprecipitation to be prepared, and comprises the steps:
(1) will contain In
3+And Sn
4+Acidic solution and certain basic solution reaction, co-precipitation obtains precursor powder after washing, filtration, the drying;
(2) with the precursor powder sintering, the solid solution diffusion takes place, and finishes semiconductor doping process, be tin indium oxide powder of the present invention.
According to the present invention, the said In that contains
3+And Sn
4+Acidic solution be hydrochloric acid, nitric acid or the sulphuric acid soln of indium and hydrochloric acid, nitric acid or the sulphuric acid soln of tin, In
3+And Sn
4+Concentration be 0.3～1.5mol/L, H
+Molar equivalent at 1～5mol/L;
Said certain basic solution is NaOH solution, KOH solution, ammoniacal liquor or saturated NH
4HCO
3Solution;
According to the preferred scheme of the present invention, can adopt two modes that drip that above-mentioned two kinds of solution are joined in the reactor, mix, co-precipitation takes place, and the acidic solution flow control is at 2～5ml/min, the flow of adjustment of acidity solution and basic solution, make the pH value remain on 3～10, Sn
4+And In
3+Mol ratio be 2%～14%, it is 50～98 ℃ that temperature remains on, the reaction finish after maturation process 1～2h;
According to the preferred scheme of the present invention, drying temperature is 80～150 ℃;
According to the preferred scheme of the present invention, sintering temperature is 700～1500 ℃, insulation 2～4h.
The median size of this powder is 0.5～2 μ m, adopts the special-purpose infrared emittance tester of making by the principle of standard GB 7286-87 that the emittance of this powder is tested, and the average emitted rate of infrared band (wavelength 8～14 μ m) is 0.60～0.75.
By above-mentioned disclosed technical scheme as seen, the tin indium oxide powder that has low-launch-rate at infrared band of the present invention, the average emitted rate of infrared band (wavelength 8～14 μ m) only 0.60～0.75, emittance is low, can be widely used in the infrared camouflage and the eo stealth engineering field of weaponry.
Embodiment
Embodiment 1
Granular metal indium and granular metal tin are dissolved in hydrochloric acid, In respectively
3+Concentration is 0.48mol/L, Sn
4+Concentration is 0.91mol/L; Get InCl
3Solution 225ml, SnCl
4Solution 20ml place same beaker, thorough mixing; Prepare saturated NH
4HCO
3Solution; Carry out two material, In of dripping with the peristaltic pump dominant discharge
3+/ Sn
4+The flow of mixed solution is 2～3ml/min, regulates NH
4HCO
3The flow of solution makes reacting liquid pH value 8～9; Temperature of reaction is 80 ℃; Slaking 2h after scouring, filtration, dry under 80 ℃ then, sintering are then treated in the reinforced back insulation that finishes.The sintering program is, is warming up to 600 ℃ of insulation 3h earlier, is warming up to 1300 ℃ of insulation 4h then, and the stove internal cooling obtains light green ito powder 12g to room temperature then.The average emitted rate of infrared band (wavelength 8～14 μ m) is 0.72.
Embodiment 2
Granular metal indium and granular metal tin are dissolved in nitric acid, In respectively
3+Concentration is 1mol/L, Sn
4+Concentration is 0.91mol/L; Get In (NO
3)
3Solution 110ml, Sn (NO
3)
4Solution 20ml as in the same beaker, thorough mixing; Prepare saturated NH
4HCO
3Solution; Carry out two material, In of dripping with the peristaltic pump dominant discharge
3+/ Sn
4+The flow of mixed solution is 6ml/min, regulates NH
4HCO
3The flow of solution makes reacting liquid pH value 8～9; Temperature of reaction is 80 ℃; Slaking 2h after scouring, filtration, dry under 80 ℃ then, sintering are then treated in the reinforced back insulation that finishes; The sintering program is, is warming up to 600 ℃ of insulation 4h earlier, is warming up to 1450 ℃ of insulation 4h then, and the stove internal cooling obtains light green ito powder 14g to room temperature then.The average emitted rate of infrared band (wavelength 8～14 μ m) is 0.75.
Embodiment 3
Granular metal indium and granular metal tin are dissolved in hydrochloric acid, In respectively
3+Concentration is 1.45mol/L, Sn
4+Concentration is 0.44mol/L; Get InCl
3Solution 150ml, SnCl
4Solution 10ml as in the same beaker, thorough mixing; Compound concentration is the NaOH solution of 1mol/L; Carry out two material, In of dripping with the peristaltic pump dominant discharge
3+/ Sn
4+The flow of mixed solution is 1～2ml/min, and the flow of regulating NaOH solution makes pH value in reaction 5～6; Temperature of reaction is 50 ℃; The reinforced back insulation that finishes, slaking 2h after scouring, filtration, dry under 50 ℃ then, sintering then; The sintering program is, directly is warming up to 1400 ℃ of insulation 4h, and the stove internal cooling obtains light green ito powder 26g to room temperature then.The average emitted rate of infrared band (wavelength 8～14 μ m) is 0.60.
Claims (11)
1. one kind has the tin indium oxide powder of low-launch-rate at infrared band, it is characterized in that component and weight content comprise: stannic oxide 2%～15%, Indium sesquioxide 85～98%.
2. tin indium oxide powder according to claim 1 is characterized in that, median size is 0.5～2 μ m, and the average emitted rate of its infrared band (wavelength 8～14 μ m) is 0.60～0.75.
3. the preparation method of tin indium oxide powder according to claim 1 and 2 is characterized in that, adopts chemical coprecipitation to be prepared.
4. the preparation method of tin indium oxide powder according to claim 3 is characterized in that, comprises the steps:
(1) will contain In
3+And Sn
4+Acidic solution and basic solution reaction, co-precipitation obtains precursor powder after washing, filtration, the drying;
(2), promptly make tin indium oxide powder of the present invention with the precursor powder sintering.
5. the preparation method of tin indium oxide powder according to claim 4 is characterized in that, the said In that contains
3+And Sn
4+Acidic solution be hydrochloric acid, nitric acid or the sulphuric acid soln of indium and hydrochloric acid, nitric acid or the sulphuric acid soln of tin, In
3+And Sn
4+Concentration be 0.3～1.5mol/L, H
+Molar equivalent at 1～5mol/L.
6. the preparation method of tin indium oxide powder according to claim 4 is characterized in that, said basic solution is NaOH solution, KOH solution, ammoniacal liquor or saturated NH
4HCO
3Solution.
7. according to the preparation method of claim 4,5 or 6 described tin indium oxide powder, it is characterized in that above-mentioned two kinds of solution stirring are mixed, and the pH value remains on 3～10, Sn
4+And In
3+Mol ratio be 2%～14%, temperature remains on 50～98 ℃, the reaction finish after maturation process 1～2h.
8. the preparation method of tin indium oxide powder according to claim 7 is characterized in that adopting two modes that drip material will contain In
3+And Sn
4+Acidic solution and basic solution mixed.
9. the preparation method of tin indium oxide powder according to claim 7 is characterized in that, drying temperature is 80～150 ℃.
10. the preparation method of tin indium oxide powder according to claim 9 is characterized in that, sintering temperature is 700～1500 ℃.
11. the preparation method of tin indium oxide powder according to claim 9 is characterized in that, sintered heat insulating 2～4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03128905 CN1260167C (en) | 2003-05-28 | 2003-05-28 | Indium-tin oxide powder with low radiation rate at infrared spectrum and its preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03128905 CN1260167C (en) | 2003-05-28 | 2003-05-28 | Indium-tin oxide powder with low radiation rate at infrared spectrum and its preparation |
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| Publication Number | Publication Date |
|---|---|
| CN1552660A true CN1552660A (en) | 2004-12-08 |
| CN1260167C CN1260167C (en) | 2006-06-21 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131384A (en) * | 2013-02-28 | 2013-06-05 | 湖南大学 | Nanometer composite wave absorbing powder having low density and porous structure, and its preparation method |
| CN103508484A (en) * | 2013-09-30 | 2014-01-15 | 西北大学 | Infrared low-emissivity nanocrystalline thin-film material SnO2 and preparation method thereof |
| CN110921700A (en) * | 2019-12-19 | 2020-03-27 | 上海大学 | Method for preparing ITO powder through coprecipitation and stirring paddle |
| CN114623728A (en) * | 2022-03-22 | 2022-06-14 | 湖南中泰特种装备有限责任公司 | Preparation method of bulletproof plate with infrared stealth function and bulletproof plate |
-
2003
- 2003-05-28 CN CN 03128905 patent/CN1260167C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131384A (en) * | 2013-02-28 | 2013-06-05 | 湖南大学 | Nanometer composite wave absorbing powder having low density and porous structure, and its preparation method |
| CN103131384B (en) * | 2013-02-28 | 2014-06-04 | 湖南大学 | Nanometer composite wave absorbing powder having low density and porous structure, and its preparation method |
| CN103508484A (en) * | 2013-09-30 | 2014-01-15 | 西北大学 | Infrared low-emissivity nanocrystalline thin-film material SnO2 and preparation method thereof |
| CN103508484B (en) * | 2013-09-30 | 2015-03-25 | 西北大学 | Infrared low-emissivity nanocrystalline thin-film material SnO2 and preparation method thereof |
| CN110921700A (en) * | 2019-12-19 | 2020-03-27 | 上海大学 | Method for preparing ITO powder through coprecipitation and stirring paddle |
| CN114623728A (en) * | 2022-03-22 | 2022-06-14 | 湖南中泰特种装备有限责任公司 | Preparation method of bulletproof plate with infrared stealth function and bulletproof plate |
| CN114623728B (en) * | 2022-03-22 | 2024-03-26 | 湖南中泰特种装备有限责任公司 | Preparation method of bulletproof plate with infrared stealth function and bulletproof plate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1260167C (en) | 2006-06-21 |
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