CN105110653B - A kind of sol-gal process for configuring colloidal sol based on peptisation prepares Sm2O3The method of film - Google Patents
A kind of sol-gal process for configuring colloidal sol based on peptisation prepares Sm2O3The method of film Download PDFInfo
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Abstract
The present invention discloses a kind of sol-gal process for configuring colloidal sol based on peptisation and prepares Sm2O3The method of film：1) by analytically pure SmCl3·6H2O is dissolved in deionized water；Its pH is adjusted with ammonia spirit and white precipitate is obtained；2) centrifuge washing is carried out to white precipitate and removes excessive Cl—And NH4 +；3) white precipitate of washes clean is washed into suspension with water；Peptization is carried out to suspension with peptizing agent, pH is to 3~6 for regulation, obtains light blue vitreosol；4) by clean glass substrate or silicon substrate at the uniform velocity to immerse colloidal sol and at the uniform velocity lifting is out dried after stopping, plated film again after drying is repeated multiple times with this, and film plate inserted in Muffle furnace at 300~500 DEG C to 1~3h of calcining obtains Sm2O3Film.The inventive method equipment requirement is low, technique is simple, and easy to operate, energy consumption is low, be easily controlled, security is good.
Description
【Technical field】
The present invention relates to field of thin film material preparation, and in particular to a kind of sol-gel that colloidal sol is configured based on peptisation
Method prepares Sm2O3The method of film.
【Background technology】
Sm2O3It is a kind of pale yellow powder, chemical property is stable, water insoluble, is soluble in inorganic acid.Sm2O3It is a new generation
Energy converting material and optoelectronic thin film material.Thin-film material species is various, is widely used, and conventional at present has：Superconducting thin film,
Conductive film, resistance film, semiconductive thin film, dielectric film, insulation film, passivation and protective film, piezoelectric membrane, ferroelectric thin
Film, optoelectronic film, Magnetoelectric film, magneto-optic thin film etc..Sm2O3Film can be not only used for preparing optical switch, data storage, photoelectricity turn
Change element and electrical switch etc., it may also be used in the filter of electronics body, magnetic material and special glass, therefore prepare Sm2O3It is thin
Membrane material has very big researching value.
The method of thin-film material that is reported at present prepare be mainly hydro-thermal method [Xin Yu, Cao Li-yun,
Influence of S/Mn molar ratio on the morphology and optical property ofγ-MnS
thin films prepared by microwave hydrothermal[J],Journal of Alloys and
Compounds,2013,549:1-5], vapour deposition process [Pei Zhao, Zhiliang Huang, Preparation of
(100)-oriented CeO2film on(100)MgO single crystal substrate by laser chemical
vapor depositionusing solid precursor[J],Ceramics International,2014,40(10)：
15919-15923].Wherein hydro-thermal method is high to equipment requirement, and technical difficulty is big, and security performance is poor；Vapour deposition process prepares thin
Film requires higher to equipment requirement and experiment condition, and preparation cost is higher and is not easy to be controlled product.
【The content of the invention】
Sm is prepared it is an object of the invention to provide a kind of sol-gel process for configuring colloidal sol based on peptisation2O3Film
Method, this method equipment requirement is low, technique is simple, and easy to operate, energy consumption is low, be easily controlled, security is good.
In order to achieve the above object, the present invention is adopted the following technical scheme that：
A kind of sol-gel process for configuring colloidal sol based on peptisation prepares Sm2O3The method of film, comprises the following steps：
1) by analytically pure SmCl3·6H2O is dissolved in deionized water, is configured to Sm3+Concentration is 0.05~0.1mol/L
Solution；Its pH is adjusted with ammonia spirit and white precipitate is obtained；
2) it is aged at room temperature after 1~6h of stirring and centrifuge washing is carried out to white precipitate and removes excessive Cl—And NH4 +；
3) white precipitate of washes clean is washed into suspension with water；Peptization is carried out to suspension with peptizing agent, is adjusted
PH obtains light blue vitreosol to 3~6；
4) clean glass substrate or silicon substrate are out dried with the uniform velocity immersing at the uniform velocity lifting after colloidal sol and stop,
Plated film again after drying, it is repeated multiple times with this, the film plated is inserted and calcines 1~3h at 300~500 DEG C in Muffle furnace and obtains
To Sm2O3Film.
Further improve of the invention is：Step 1) in ammonia spirit mass concentration be 5~10%.
Further improve of the invention is：Step 1) in ammonia spirit rate of addition be 1~2mL/min.
Further improve of the invention is：Step 1) in pass through ammonia spirit adjust pH to 7~10.
Further improve of the invention is：Step 2) in digestion time be 12h.
Further improve of the invention is：Step 3) described in peptizing agent use acetic acid.
Further improve of the invention is：Step 3) in using peptizing agent 25~75 DEG C to suspension carry out peptization.
Further improve of the invention is：Step 4) in by clean glass substrate or silicon substrate at the uniform velocity to immerse colloidal sol
Speed be 1~20cm/min.
Further improve of the invention is：Step 4) in the residence time be 20s.
Further improve of the invention is：Specifically include following steps：
1) by analytically pure SmCl3·6H2O is dissolved in deionized water, is configured to Sm3+Concentration is molten for 0.1mol/L's
Liquid；Its pH is adjusted with 8% ammonia spirit to be 8.5 and obtain white precipitate；The rate of addition of ammonia spirit is 1~2mL/
min；
2) 12h is aged after stirring 5h at room temperature and centrifuge washing is carried out to white precipitate and removes excessive Cl—And NH4 +；
3) white precipitate of washes clean is washed into suspension with water；Suspension is carried out at 45 DEG C with peptizing agent acetic acid
Peptization, pH is to 4 for regulation, obtains light blue vitreosol；
4) clean glass substrate or silicon substrate are immersed into light blue vitreosol with the uniform velocity 1-20cm/min and stops 20s
At the uniform velocity lifting is out dried afterwards, plated film again after drying, repeated multiple times with this, by the film plated insert in Muffle furnace
2h is calcined at 500 DEG C and obtains Sm2O3Film.
Relative to prior art, the invention has the advantages that：
The present invention prepares Sm with the sol-gel process that colloidal sol is configured based on peptisation2O3Thin-film material, utilizes SmCl3·
6H2O is raw material, and ammoniacal liquor regulation pH, acetic acid prepares colloidal sol as peptizing agent, and substrate is through being repeated several times lifting plated film and through drying heat
Sm is made after processing2O3Thin-film material large area, thickness are uniform.The raw material of the reaction is easy to get and cost is low, and process equipment is simple,
Aerosol particle size is uniform, and energy consumption is low, and the reaction is carried out at normal temperatures and pressures, with water as reaction dissolvent, and security is good, feasibility
By force, so very economical, practicality, with extraordinary industrial prospect.
【Brief description of the drawings】
Fig. 1 is Sm prepared by the embodiment of the present invention 42O3The XRD of thin-film material；
Fig. 2 is the Sm prepared by the embodiment of the present invention 42O3The AFM photos of film.
【Embodiment】
Embodiment 1：
1) by analytically pure SmCl3·6H2O is dissolved in deionized water, is configured to Sm3+Concentration is molten for 0.05mol/L's
Liquid；Its pH is adjusted with 5% ammonia spirit to be 10 and obtain white precipitate；The rate of addition of ammonia spirit is 1~2mL/min；
2) 12h is aged after stirring 1h at room temperature and centrifuge washing is carried out to white precipitate and removes excessive Cl—(use
0.5mol/L silver nitrate detection) and NH4 +；
3) white precipitate of washes clean is washed into suspension with water；Suspension is carried out at 60 DEG C with peptizing agent acetic acid
Peptization, pH is to 3 for regulation, produces light blue vitreosol.
4) clean glass substrate or silicon substrate are immersed into step 3 with the uniform velocity (1-20cm/min)) prepared by it is light blue
Vitreosol simultaneously stops after 20s at the uniform velocity lifting and is out dried, plated film again after drying, repeated multiple times with this, by what is plated
Film, which is inserted in Muffle furnace, to be calcined 1h at 300 DEG C and obtains Sm2O3Film.
Embodiment 2：
1) by analytically pure SmCl3·6H2O is dissolved in deionized water, is configured to Sm3+Concentration is molten for 0.1mol/L's
Liquid；Its pH is adjusted with 10% ammonia spirit to be 7 and obtain white precipitate；The rate of addition of ammonia spirit is 1~2mL/min；
2) 12h is aged after stirring 2h at room temperature and centrifuge washing is carried out to white precipitate and removes excessive Cl—(use
0.5mol/L silver nitrate detection) and NH4 +；
3) white precipitate of washes clean is washed into suspension with water；Suspension is carried out at 25 DEG C with peptizing agent acetic acid
Peptization, pH is to 6 for regulation, produces light blue vitreosol.
4) clean glass substrate or silicon substrate are immersed into light blue vitreosol with the uniform velocity (1-20cm/min) and stopped
At the uniform velocity lifting is out dried after 20s, plated film again after drying, repeated multiple times with this, and the film plated is inserted into Muffle furnace
In at 300 DEG C calcine 1h be to obtain Sm2O3Film.
Embodiment 3：
1) by analytically pure SmCl3·6H2O is dissolved in deionized water, is configured to Sm3+Concentration is molten for 0.075mol/L's
Liquid；Its pH is adjusted with 10% ammonia spirit to be 8 and obtain white precipitate；The rate of addition of ammonia spirit is 1~2mL/min；
2) 12h is aged after stirring 4h at room temperature and centrifuge washing is carried out to white precipitate and removes excessive Cl—(use
0.5mol/L silver nitrate detection) and NH4 +；
3) white precipitate of washes clean is washed into suspension with water；Suspension is carried out at 75 DEG C with peptizing agent acetic acid
Peptization, pH is to 5 for regulation, produces light blue vitreosol.
4) clean glass substrate or silicon substrate are immersed into light blue vitreosol with the uniform velocity (1-20cm/min) and stopped
At the uniform velocity lifting is out dried after 20s, plated film again after drying, repeated multiple times with this, and the film plated is inserted into Muffle furnace
In at 400 DEG C calcine 2h be to obtain Sm2O3Film.
Embodiment 4：
1) by analytically pure SmCl3·6H2O is dissolved in deionized water, is configured to Sm3+Concentration is molten for 0.1mol/L's
Liquid；Its pH is adjusted with 8% ammonia spirit to be 8.5 and obtain white precipitate；The rate of addition of ammonia spirit is 1~2mL/
min；
2) 12h is aged after stirring 5h at room temperature and centrifuge washing is carried out to white precipitate and removes excessive Cl—(use
0.5mol/L silver nitrate detection) and NH4 +；
3) white precipitate of washes clean is washed into suspension with water；Suspension is carried out at 45 DEG C with peptizing agent acetic acid
Peptization, pH is to 4 for regulation, produces light blue vitreosol.
4) clean glass substrate or silicon substrate are immersed into light blue vitreosol with the uniform velocity (1-20cm/min) and stopped
At the uniform velocity lifting is out dried after 20s, plated film again after drying, repeated multiple times with this, and the film plated is inserted into Muffle furnace
In at 500 DEG C calcine 2h be to obtain Sm2O3Film.
Embodiment 5：
1) by analytically pure SmCl3·6H2O is dissolved in deionized water, is configured to Sm3+Concentration is molten for 0.05mol/L's
Liquid；Its pH is adjusted with 5% ammonia spirit to be 7.5 and obtain white precipitate；The rate of addition of ammonia spirit is 1~2mL/min；
2) 12h is aged after stirring 1h at room temperature and centrifuge washing is carried out to white precipitate and removes excessive Cl—(use
0.5mol/L silver nitrate detection) and NH4 +；
3) suspension is washed into by the white precipitate of washes clean；Glue is carried out to suspension at 25 DEG C with peptizing agent acetic acid
Molten, pH is to 4.5 for regulation, produces light blue vitreosol.
4) clean glass substrate or silicon substrate are immersed into light blue vitreosol with the uniform velocity (1-20cm/min) and stopped
At the uniform velocity lifting is out dried after 20s, plated film again after drying, repeated multiple times with this, and the film plated is inserted into Muffle furnace
In at 300 DEG C calcine 3h be to obtain Sm2O3Film.
Key problem in technology point has two in the present invention：One is step 1) in pH when obtaining white precipitate when ammoniacal liquor is added dropwise and
Rate of addition；Two be pH when peptizing agent carries out peptization to white precipitate.Peptisation prepares colloidal sol and passed through chemically or mechanically
Mode destroys the bonding force of primary granule combination, and the bulky grain that particle is temporarily agglomerated into is spread out, size is obtained very small
The dispersiveness preferably hydrosol of (being typically Nano grade).PH is excessive when if ammoniacal liquor is added dropwise or the too fast solution of rate of addition in sink
Form sediment easily explosive formation bulky grain, not easily passs through introducing particle opposite charges and promotes agglomerated particle is scattered to obtain colloidal sol.But
PH is excessive during peptization, introduces that opposite charges is smaller to be completely dispersed bulky grain, and pH is too small, then may introduce H+It is excessive and incite somebody to action
Precipitation dissolves again, can not all form colloidal sol.
Claims (6)
1. a kind of sol-gel process for configuring colloidal sol based on peptisation prepares Sm2O3The method of film, it is characterised in that including with
Lower step：
1) by analytically pure SmCl3·6H2O is dissolved in deionized water, is configured to Sm3+Concentration is molten for 0.05~0.1mol/L's
Liquid；Its pH is adjusted with ammonia spirit and white precipitate is obtained；
2) it is aged at room temperature after 1~6h of stirring and centrifuge washing is carried out to white precipitate and removes excessive Cl—And NH4 +；
3) white precipitate of washes clean is washed into suspension with water；Peptization is carried out to suspension with peptizing agent, pH to 3 is adjusted
~6, obtain light blue vitreosol；
4) clean glass substrate or silicon substrate are out dried with the uniform velocity immersing at the uniform velocity lifting after colloidal sol and stop, dried
Plated film again, repeated multiple times with this afterwards, and the film plated is inserted and calcines 1~3h at 300~500 DEG C in Muffle furnace and obtains
Sm2O3Film；
Step 3) described in peptizing agent use acetic acid；
Step 3) in using peptizing agent 25~75 DEG C to suspension carry out peptization；
Step 1) in ammonia spirit rate of addition be 1~2mL/min；
Step 1) in pass through ammonia spirit adjust pH to 7~10.
2. the mass concentration of ammonia spirit is 5~10% according to the method described in claim 1, it is characterised in that step 1).
3. digestion time is 12h according to the method described in claim 1, it is characterised in that step 2).
4. by clean glass substrate or silicon substrate with even according to the method described in claim 1, it is characterised in that step 4)
The speed of speed immersion colloidal sol is 1~20cm/min.
5. the residence time is 20s according to the method described in claim 1, it is characterised in that step 4).
6. according to the method described in claim 1, it is characterised in that specifically include following steps：
1) by analytically pure SmCl3·6H2O is dissolved in deionized water, is configured to Sm3+Concentration is 0.1mol/L solution；Use matter
The ammonia spirit that amount concentration is 8% adjusts its pH and is 8.5 and obtains white precipitate；The rate of addition of ammonia spirit is 1~2mL/
min；
2) 12h is aged after stirring 5h at room temperature and centrifuge washing is carried out to white precipitate and removes excessive Cl—And NH4 +；
3) white precipitate of washes clean is washed into suspension with water；Glue is carried out to suspension at 45 DEG C with peptizing agent acetic acid
Molten, pH is to 4 for regulation, obtains light blue vitreosol；
4) clean glass substrate or silicon substrate are immersed into light blue vitreosol with the uniform velocity 1-20cm/min and stopped even after 20s
Speed, which lifts out, to be dried, plated film again after drying, repeated multiple times with this, and the film plated is inserted in Muffle furnace 500
2h is calcined at DEG C and obtains Sm2O3Film.
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| CN100386473C (en) * | 2005-09-08 | 2008-05-07 | 陕西科技大学 | Collosol/gel preparation method for Sm2O3 photoelectric film |
| CN100359044C (en) * | 2005-09-08 | 2008-01-02 | 陕西科技大学 | Hydrothermal Sm2O3 film preparing process |
| CN101494170B (en) * | 2009-02-19 | 2010-12-29 | 陕西科技大学 | Method for preparing Sm2O3 film by microwave assisted hydrothermal process |
| CN101697321B (en) * | 2009-10-29 | 2011-06-01 | 彩虹集团公司 | Preparation method of titanium dioxide dense film for dye-sensitized solar cell |
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