CN110484253A - A kind of preparation method of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric - Google Patents
A kind of preparation method of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric Download PDFInfo
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- CN110484253A CN110484253A CN201910664873.5A CN201910664873A CN110484253A CN 110484253 A CN110484253 A CN 110484253A CN 201910664873 A CN201910664873 A CN 201910664873A CN 110484253 A CN110484253 A CN 110484253A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
Abstract
The present disclosure provides a kind of preparation methods of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric, the lanthanium titanate raw material of predetermined amount and the lanthanide ion oxide of predetermined amount are weighed with the balance of a ten thousandth, are dispersed to be put into sufficient mixed grinding in ball mill with organic solvent.Then remove to obtain rear-earth-doped metatitanic acid lanthanum nanometer sheet through liquid phase by double sintering.Preparation process of the invention is simple: this method is prepared by high-temperature solid-phase sintering method and liquid phase stripping method, and two-step synthesis method is easy to operate and more mature in this；Temperature limit is wide: lanthanium titanate prepared by this method is that one kind has high-melting-point ceramic ferroelectric body, and the temperature region for being used for thermometric is wide, has reached -100~1600 DEG C.Nanometer sheet yield is high: this method is that rear-earth-doped lanthanium titanate nanometer sheet is prepared by liquid phase stripping method, by adjusting the parameters such as ultrasonic time power and frequency, can prepare a large amount of nanometer sheets.
Description
Technical field
The invention belongs to low-dimension nano material preparation field, in particular to a kind of up-conversion luminescence for optics thermometric is dilute
The preparation method of native doped titanic acid lanthanum nanometer sheet.
Background technique
Up-conversion luminescence is defined as anti-stoke emission process i.e. longer-wave photons by being converted into shortwave after material
Photon.Research in recent years it is most to count rare earth up-conversion luminescent material, especially lanthanide-doped regular atom row
The crystalline material of column is a kind of functional luminescent material that lower energy photon can be become high-energy photon.Relative to quantum dot, have
The down-conversion luminescent materials such as engine dyeing material and fluorescin possess many properties outstanding, for example luminescent lifetime is longer, transmitting band
The photostability that width is relatively narrow, launches is higher, is influenced by background fluorescence weak etc..
Nanothermometer is intended to extract the knowledge of the local temperature of given system with sub-micron spatial resolution.These knowledge
It is to be understood completely necessary to microcosmic and nanostructure system, the strong decision of dynamics and performance by temperature.Nearest nanometer
The development of technology and nanosecond medical science brings the appearance of a large amount of such systems.But in the research of rare earth up-conversion luminescence nanomaterial
It also needs further to reinforce.
N-Methyl pyrrolidone, Chinese nickname: NMP；- 2 pyrrolidones of 1- methyl；N-methyl-2-pyrrolidone.It is colourless
Bright oily liquids, micro- smell for having amine.Volatility is low, and thermal stability, chemical stability are good, can volatilize with vapor.There is suction
It is moist.It is light sensitive.Soluble easily in water, ethyl alcohol, ether, acetone, ethyl acetate, chloroform and benzene can dissolve most of organic and nothing
Machine compound, polar gas, natural and synthetic macromolecular compound.N-Methyl pyrrolidone lithium electricity, medicine, pesticide, pigment,
It is widely applied in the industries such as cleaning agent, insulating materials.
Temperature is ceramics and glass industry, biological field, the important parameter of many different fields such as material formation field.It is existing
The present causes temperature inaccuracy and detector to be damaged, there are also the temperature since contact type thermometric indicator is likely to generate heat transfer with object
Degree meter scale is below with regard to being not suitable for carrying out temperature measurement at 10 μm, and in recent years, temperature sensing is based on rare earth up-conversion luminescence conduct
Non-contact type temperature measurement causes great interest.Therefore it needs to develop a kind of non-with micron order and nanometer resolution
Contact type thermometric indicator.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provides one kind by high-temperature solid-phase sintering method and
The preparation of liquid phase stripping method has reached -100~1600 DEG C using temperature region, has adjusted the parameters such as ultrasonic time power and frequency,
The preparation method of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of the up-conversion luminescence for optics thermometric of nanometer sheet yield is improved,
The technical solution adopted by the present invention to solve the technical problems is: it is of the present invention for optics thermometric upper turn
The preparation method of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of light is changed, this method comprises the following steps:
(a) the lanthanium titanate raw material of predetermined amount and the lanthanide ion oxide of predetermined amount are weighed with the balance of a ten thousandth, and
Dispersed to be put into sufficient mixed grinding in ball mill with organic solvent.
(b) it by the sample drying after ground and mixed, is placed in alumina crucible and carries out first sintering under air atmosphere
Processing.
(c) by the good substance of first sintering be put into agate mortar with alcohol sufficiently it is levigate after, drying carry out second again
Secondary sintering processes.
(d) after the sample and NMP obtained double sintering mixes in centrifuge tube, then ultrasonic vibration pulverization process is carried out.
(e) sample after ultrasonic vibration pulverization process is put into a centrifuge, adjustment parameter, carries out centrifugal treating.
(f) supernatant liquor after centrifugal treating is collected, rear-earth-doped lanthanium titanate nanometer sheet, the observable under Electronic Speculum are obtained
It arrives.
Preferably, the molar percentage that lanthanide ion oxide is adulterated in the step a) are as follows: 0.01%~10%；
Ball mill operating parameter are as follows: turn 20min clockwise, 20min counterclockwise, revolving speed is 1000~5000r/min, and ball milling total time is
8~36h, ratio of grinding media to material are as follows: 1:1~1:3.
Preferably, temperature schedule in the step b) are as follows: heating rate are as follows: 3~50 DEG C/min；First sintering temperature
It is 1100 DEG C~1250 DEG C；Sintering time is 2~6h.
Preferably, in the step c) alcohol wet grinding time are as follows: 1~2h；Second of sintering temperature are as follows: 1200
~1350 DEG C；Sintering time is 1~4h.
Preferably, frequency ultrasonic in the step d) are as follows: 20~40kHz；Ultrasonic power are as follows: 150~300W；Ultrasound
Time be 1~for 24 hours.
Preferably, in the step e) centrifuge centrifugation rate are as follows: 1000~20000r/min.
Preferably, the lanthanide ion oxide includes lanthana；And at least one of ytterbium oxide and erbium oxide.
The present invention has by lanthanium titanate nanometer sheet rear-earth-doped prepared by solid sintering technology and liquid phase stripping method
Following advantages:
1. preparation process is simple: the method for the present invention is prepared by high-temperature solid-phase sintering method and liquid phase stripping method, both
Synthetic method is easy to operate and more mature；
2. temperature limit is wide: lanthanium titanate prepared by this method is that one kind has high-melting-point ceramic ferroelectric body,
Temperature region for thermometric is wide, has reached -100~1600 DEG C.
3. nanometer sheet yield is high: this method is that rear-earth-doped lanthanium titanate nanometer sheet is prepared by liquid phase stripping method, is led to
The parameters such as ultrasonic time power and frequency are overregulated, a large amount of nanometer sheets can be prepared.
Detailed description of the invention
Fig. 1 is the TEM figure of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of the present invention；
Fig. 2 is the XRD diagram of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of the present invention；
Fig. 3 is the luminescence generated by light figure of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of the present invention；
Specific embodiment
The present invention will be further described with reference to the accompanying drawing, by the following description of the embodiment, will more help
In the public understanding present invention, but the specific embodiment given by applicant should can't be considered as to the technology of the present invention side
The definition of the limitation of case, any pair of component or technical characteristic be changed or to overall structure make form and immaterial transformation
It is regarded as protection scope defined by technical solution of the present invention.
Embodiment 1
Step a weighs 3.1948g titanium dioxide, 5.7016g lanthana, 0.7881g oxidation with the balance of a ten thousandth
Ytterbium, 0.1912g erbium oxide, being put into ratio of grinding media to material in ball grinder is 1:3.Ball mill operating parameter are as follows: turn 20min clockwise, it is inverse
Hour hands 20min, revolving speed 5000r/min, ball milling total time are for 24 hours.
Step b cleans ball grinder and sample with water repeatedly, collects liquid and the drying in 100 DEG C of baking ovens.Then it is set
It is put into shaft furnace together in alumina crucible, carries out first sintering.Temperature schedule is set are as follows: from room temperature with 10 DEG C/min liter
To 900 DEG C, 1150 DEG C then are risen to 3 DEG C/min, keeps the temperature 4h, is taken out with room temperature is furnace-cooled to.
Sample after first sintering is put into agate mortar and carries out wet grinding 2h with alcohol, after dry by step c
Second is carried out to be sintered.Temperature schedule is set are as follows: rises to 900 DEG C from room temperature with 10 DEG C/min, then rises to 1320 with 3 DEG C/min
DEG C, 4h is kept the temperature, is taken out with room temperature is furnace-cooled to.
Step d is put into the powder that double sintering is completed in agate mortar and regrinds, takes the powder of 10mg in centrifuge tube
In, while 10ml NMP is added, centrifuge tube is placed in Ultrasound Instrument, adjuster power is 150W, and time 8h guarantees simultaneously
Bath temperature is 10 DEG C or less progress ultrasonic vibration processing.
The centrifuge tube of sonicated mistake is put into centrifuge, adjusts centrifugation system are as follows: first with 1000r/min by step e
Centrifugation rate be centrifuged 5min, then 5min is centrifuged again with the centrifugation rate of 4000r/min.
Step f, the clear solution in upper layer after collecting centrifugal treating, can be observed rear-earth-doped lanthanium titanate under Electronic Speculum
Nanometer sheet.
In the present embodiment, Fig. 1 is the TEM figure of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of the present invention, the result shows that the rare earth
The grain diameter of doped titanic acid lanthanum nanometer sheet is about 50-200nm, particle favorable dispersibility.
Fig. 2 is the X ray diffracting spectrum of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of the present invention, according to powder diffraction standard association meeting
(JCPDS) " it is responsible for " powder diffraction card (the PDF card) " edited and publish and carries out material phase analysis, the result shows that main component
For La2Ti2O7And the ionic compound of partial Yb and Tm, it can be deduced that the made primary product rare earth of the method for the present invention is mixed
Miscellaneous lanthanium titanate nanometer sheet purity is high.
Embodiment 2
Step a weighs 3.1948g titanium dioxide, 5.7016g lanthana, 0.7881g oxygen with the balance of a ten thousandth
Change ytterbium, 0.1912g erbium oxide, being put into ratio of grinding media to material in ball grinder is 1:3.Ball mill operating parameter are as follows: turn 20min clockwise,
20min counterclockwise, revolving speed 4000r/min, ball milling total time are 36h.
Step b cleans ball grinder and sample with water repeatedly, collects liquid and the drying in 100 DEG C of baking ovens.Then it is set
It is put into shaft furnace together in alumina crucible, carries out first sintering.Temperature schedule is set are as follows: from room temperature with 10 DEG C/min liter
To 900 DEG C, 1100 DEG C then are risen to 3 DEG C/min, keeps the temperature 4h, is taken out with room temperature is furnace-cooled to.
Step c, sintered sample, which is put into agate mortar, carries out wet grinding 2h with alcohol, carries out second after dry
Secondary sintering.Temperature schedule is set are as follows: rises to 900 DEG C from room temperature with 10 DEG C/min, then rises to 1300 DEG C with 3 DEG C/min, heat preservation
4.5h takes out with room temperature is furnace-cooled to.
Step d is put into the powder that double sintering is completed in agate mortar and regrinds, takes the powder of 10mg in centrifuge tube
In, while 10ml NMP is added.
Step e, centrifuge tube is placed in Ultrasound Instrument, and adjuster power is 300W, time 6h, while guaranteeing water-bath temperature
Degree is 10 DEG C or less progress ultrasonic vibration processing, and the centrifuge tube of sonicated mistake is put into centrifuge, adjusts centrifugation system
Are as follows: 5min is first centrifuged with the centrifugation rate of 2000r/min, then 5min is centrifuged again with the centrifugation rate of 5000r/min.
Step f, the clear solution in upper layer after collecting centrifugal treating, can be observed rear-earth-doped lanthanium titanate under Electronic Speculum
Nanometer sheet.
Preparation process of the invention is simple: this method is prepared by high-temperature solid-phase sintering method and liquid phase stripping method, in this
Two-step synthesis method is easy to operate and more mature；Temperature limit is wide: lanthanium titanate prepared by this method is that one kind has
High-melting-point ceramic ferroelectric body, the temperature region for being used for thermometric is wide, has reached -100~1600 DEG C.Nanometer sheet yield is high: we
Method is that rear-earth-doped lanthanium titanate nanometer sheet is prepared by liquid phase stripping method, by adjusting ultrasonic time power and frequency etc.
Parameter can prepare a large amount of nanometer sheets.
Scheme described above, the only rear-earth-doped metatitanic acid lanthanum of several up-conversion luminescences for optics thermometric of the invention
The preparation preferred embodiment of nanometer sheet not generates any restrictions to protection scope of the present invention, and certainly, the present invention may be used also
To there is other various embodiments, without deviating from the spirit and substance of the present invention, those skilled in the art can
To make various corresponding changes and modifications according to the present invention, but these corresponding changes and modifications all should belong to appended by the present invention
Scope of protection of the claims.
Claims (7)
1. a kind of preparation method of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric, which is characterized in that
Include the following steps:
(a) the lanthanium titanate raw material of predetermined amount and the lanthanide ion oxide of predetermined amount are weighed with the balance of a ten thousandth, and with having
Solvent is dispersed to be put into sufficient mixed grinding in ball mill；
(b) by the sample drying after ground and mixed, progress first sintering processing under air atmosphere is placed in alumina crucible；
(c) by the good substance of first sintering be put into agate mortar with alcohol sufficiently it is levigate after, drying carry out second of burning again
Knot processing；
(d) after the sample and NMP obtained double sintering mixes in centrifuge tube, then ultrasonic vibration pulverization process is carried out；
(e) sample after ultrasonic vibration pulverization process is put into a centrifuge, adjustment parameter, carries out centrifugal treating；
(f) supernatant liquor after centrifugal treating is collected, rear-earth-doped lanthanium titanate nanometer sheet is obtained, can be observed under Electronic Speculum.
2. a kind of system of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric according to claim 1
Preparation Method, it is characterised in that: the molar percentage that lanthanide ion oxide is adulterated in the step a) are as follows: 0.01%~
10%；Ball mill operating parameter are as follows: turn 20min, 20min counterclockwise clockwise, revolving speed is 1000~5000r/min, and ball milling is total
Time is 8~36h；Ratio of grinding media to material are as follows: 1:1~1:3.
3. a kind of system of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric according to claim 1
Preparation Method, it is characterised in that: temperature schedule in the affiliated step b) of step are as follows: first sintering temperature is 1100 DEG C~1250
℃；Sintering time is 2~6h.
4. a kind of system of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric according to claim 1
Preparation Method, it is characterised in that: the time of alcohol wet grinding in affiliated step c) are as follows: 1~2h；Second of sintering temperature are as follows:
1200~1350 DEG C；Sintering time is 1~4h.
5. a kind of system of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric according to claim 1
Preparation Method, it is characterised in that: ultrasonic frequency in the step d) are as follows: 20~40kHz；Ultrasonic power are as follows: 150~300W；It is super
Acoustic shock swing the pulverization process time be 1~for 24 hours.
6. a kind of system of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric according to claim 1
Preparation Method, it is characterised in that: the centrifugation rate of centrifuge in the step e) are as follows: 1000~20000r/min.
7. a kind of system of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric according to claim 1
Preparation Method, it is characterised in that: the lanthanide ion oxide includes lanthana；And at least one in ytterbium oxide and erbium oxide
Kind.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111410514A (en) * | 2020-03-31 | 2020-07-14 | 青海大学 | Optical temperature measuring material, preparation method thereof and non-contact temperature measuring material |
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