CN109321249A - Rare earth hydroxide nanosheet luminescent material based on lanthanum and preparation method thereof - Google Patents

Rare earth hydroxide nanosheet luminescent material based on lanthanum and preparation method thereof Download PDF

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CN109321249A
CN109321249A CN201811364051.7A CN201811364051A CN109321249A CN 109321249 A CN109321249 A CN 109321249A CN 201811364051 A CN201811364051 A CN 201811364051A CN 109321249 A CN109321249 A CN 109321249A
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马菲
张琳
汤颖珂
金凤
白翠冰
盛良全
乔瑞
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Fuyang Normal University
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Abstract

本发明公开了一种镧基质的稀土氢氧化物纳米片发光材料及制备方法，其制备方法：首先采用溶剂热法制备以稀土La3+为基质Tb3+掺杂的稀土氢氧化物层状材料La1.9Tb0.1(OH)5NO3·1.5H2O；然后利用微波辅助的方法，以苯甲酸钠作为插层材料与稀土氢氧化物层状材料层间阴离子(NO3 ‑)进行离子交换，制备层间距离扩大的层状化合物中间体；该中间体材料在甲酰胺中经超声剥离、高速离心后得到稀土氢氧化物纳米片发光材料La1.9Tb0.1(OH)5‑C6H5COO。本发明的纳米片材料在农作物光转换薄膜的制备以及荧光粉等领域有较大的应用价值。

The invention discloses a lanthanum-based rare earth hydroxide nano-sheet luminescent material and a preparation method. The preparation method: first, a solvothermal method is used to prepare a rare earth hydroxide layer doped with rare earth La 3+ as a matrix Tb 3+ Material La 1.9 Tb 0.1 (OH) 5 NO 3 ·1.5H 2 O; then use the microwave-assisted method to perform ion exchange with sodium benzoate as the intercalation material and the interlayer anion (NO 3 ‑ ) of the rare earth hydroxide layered material , to prepare a layered compound intermediate with an enlarged interlayer distance; the intermediate material is ultrasonically stripped in formamide and centrifuged at high speed to obtain a rare earth hydroxide nanosheet luminescent material La 1.9 Tb 0.1 (OH) 5 -C 6 H 5 COO. The nano-sheet material of the invention has great application value in the fields of preparation of crop light conversion films, phosphor powder and the like.

Description

A kind of the rare-earth hydroxide Nanoflake luminescent material and preparation method of lanthanum matrix
Technical field
The present invention relates to technical field of material, the rare-earth hydroxide nanometer sheet of specifically a kind of lanthanum matrix is sent out Luminescent material and preparation method.
Background technique
Since terbium has property of certain photon from excitation state transition time ground state as lanthanide series.If excited If, rare earth terbium ion can green light.This characteristics of luminescence of rare earth terbium ion can be applied to the fields such as fluorescent powder: commonly use at present Green light fluorescent powder mainly have terbium activate phosphate matrix, terbium activation silicate substrate, terbium activation cerium Mg aluminate base Matter etc. shows excellent optical property under excited state.Rare-earth hydroxide stratiform LRHs(Layered Rare- Earth Hydroxides) material be as certain specific structure basic unit pass through share angle, side or face accumulation made of sky Between layer structure.The nanometer sheet that the material obtains after being stripped carries positive charge and hair because of its ultra-thin laminated structure, surface It is narrow and influenced the advantages that small by ligand to penetrate peak, constructs equal fields in illumination field and rare earth nano device and has obtained widely answering With.
Due to the influence for the factors such as ionic radius is bigger than normal, lanthanum can't be prepared using traditional hydrothermal synthesis mode at present The rare-earth hydroxide stratified material of matrix:, can only if the pH value of solution is greater than 7 when conventional hydrothermal synthetic method prepares the material It is made La (OH)3, and when solution ph is less than 7, cannot get target product.
Summary of the invention
The object of the present invention is to provide a kind of rare-earth hydroxide Nanoflake luminescent material of lanthanum matrix and preparation method, Preparation method is with lanthanum nitrate hexahydrate, six nitric hydrate terbiums and cesium hydroxide for basic raw material, using solvent-thermal method with La3+For matrix LLaH, Tb3+Doping, using sodium benzoate as intercalation material and LRH (Layered Rare-earth Hydroxide) interlayer anion ion exchange prepares the widened lamellar compound intermediate of interfloor distance, the intermediary material Rare-earth hydroxide Nanoflake luminescent material La is obtained after ultrasound removing, high speed centrifugation in formamide1.9Tb0.1(OH)5- C6H5COO。
Realizing the specific technical solution of the object of the invention is:
A kind of rare-earth hydroxide Nanoflake luminescent material preparation method, this method comprising the following specific steps
A, the preparation of presoma rare-earth hydroxide stratiform (LRHs) material:
Take lanthanum nitrate hexahydrate (La (NO3)3·6H2O it) is dissolved in dehydrated alcohol, in N2It is uniformly mixed in protective atmosphere； The molar ratio for pressing La: Tb=19: 1 again, is added six nitric hydrate terbium (Tb (NO3)3·6H2O) ethanol solution；Then according to 1: 2 Rare earth nitrades and CsOH are added to absolute ethanol by molar ratio (nitrate: cesium hydroxide), after being sufficiently stirred；By acquired solution It is placed in the reaction kettle of teflon lined, is reacted 24 hours under the conditions of 120-160 DEG C；After the reaction was completed, gained sample It is filtered, repeatedly with being dried in vacuo 1-2 hours under the conditions of ethanol washing, 40 DEG C, stratiform presoma La can be obtained1.9Tb0.1 (OH)5NO3·1.5H2O；
B, the preparation of the LRHs of sodium benzoate intercalation
Take gained La in above-mentioned steps1.9Tb0.1(OH)5NO3·1.5H2O, according to the ratio between the amount of sodium benzoate and its substance 4:1's Ratio is added in PhCOONa solution, N2Microwave heating 15min under the conditions of protective atmosphere is filtered, vacuum is dry under the conditions of 40 DEG C It is 1-2 hours dry, the rare earth stratified material La of benzoate anion intercalation can be obtained1.9 Tb0.1(OH)5C6H5COO·1.5H2O；
C, the preparation of the rare-earth hydroxide Nanoflake luminescent material of lanthanum matrix
The product for taking step b to obtain is placed in formamide solvent, N according to the ratio of 0.01g/10ml2It is held under the conditions of protective atmosphere Suspension is obtained after continuous ultrasound 30-60 min, after twenty minutes through 8000r/min high speed centrifugation, the lanthanum matrix can be obtained Rare-earth hydroxide Nanoflake luminescent material La1.9Tb0.1(OH)5-C6H5COO。
A kind of rare-earth hydroxide Nanoflake luminescent material of lanthanum matrix made from the above method.
The present invention uses the rare-earth hydroxide stratified material La of the terbium doped lanthanum matrix of solvent structure1.9Tb0.1(OH)5NO3·1.5H2O；Using dehydrated alcohol as solvent in solvent-thermal method, CsOH provides hydroxide ion, so that solution ph 6 or so, be conducive to synthesizing rare-earth hydroxide stratiform material La1.9Tb0.1(OH)5NO3·1.5H2O.The material by from Rare-earth hydroxide Nanoflake luminescent material La can be obtained after ultrasound removing in formamide solvent in son exchange1.9Tb0.1(OH)5- C6H5COO.(rear gained nanometer sheet is stripped by positively charged rare-earth hydroxide mainboard layer { La1.9Tb0.1(OH)5 +Peace The anion C of weighing apparatus mainboard layer surface charge6H5COO-It is constituted)
The beneficial effects of the present invention are:
(1) present invention uses solvent heat to prepare the LLaH:Tb rare-earth hydroxide stratified material adulterated using La as matrix, Tb.
(2) present invention has prepared rare-earth hydroxide Nanoflake luminescent material La1.9Tb0.1(OH)5-C6H5COO。
(3) method that microwave is used during intercalation (ion exchange), saves the time.
Detailed description of the invention
Fig. 1 is nanometer sheet scanning electron microscope (SEM) photograph made from the embodiment of the present invention 2；
Fig. 2 is nanometer sheet scanning electron microscope (SEM) photograph made from the embodiment of the present invention 4；
Fig. 3 is the fluorescence spectra of nanometer sheet material made from embodiment 5.
Specific embodiment
Embodiment 1
A, lanthanum nitrate hexahydrate 0.6170g, six nitric hydrate terbium solution 11.88ml is taken (to take six nitric hydrate terbium of 1.4324g molten The concentration being configured in 500ml ethanol solution is the solution of 0.00632mol/L), cesium hydroxide solution 50ml(takes 5.0750g cesium hydroxide is dissolved in the solution for being configured to that concentration is 0.060442mol/L in 500ml ethanol solution), and in room Temperature is lower to be uniformly mixed and is sufficiently stirred；Obtained suspension is moved into the reaction kettle of the polytetrafluoroethyllining lining of 150ml, then Baking oven is put into heat 24 hours under the conditions of 155 DEG C；Take out reaction kettle cooling after reaction, supernatant in liner is outwelled, Suitable absolute ethyl alcohol and stirring is added to wash 2 ~ 3 removing soluble-salts, filter, then sediment is dried to 1h at 40 DEG C, Obtain white powder La1.9 Tb0.1(OH)5NO3·1.5H2O；
B, the product 0.3997g for taking a step to obtain, sodium benzoate 0.4975g is placed in 300ml water, in N2It is held in protective atmosphere Continuous microwave 15min；It filtering, massive laundering, ethyl alcohol is washed, and it is dry, the rare earth stratified material La of benzoate intercalation is made1.9 Tb0.1(OH)5C6H5COO·1.5H2O.(microwave frequency 2.45G Hz；NO3 -: sodium benzoate=1:4)
C, the product 0.05g for taking b step to obtain, is placed in 50ml formamide solvent, N according to the ratio of 0.01g/10ml2Protection Suspension is obtained after 30 min of continual ultrasonic under atmospheric condition, after 8000r/min high speed centrifugation 15 minutes, rare earth can be obtained Hydroxide nano piece luminescent material La1.9Tb0.1(OH)5-C6H5COO。
Embodiment 2
A, lanthanum nitrate hexahydrate 0.6172g, six nitric hydrate terbium solution 11.90ml is taken (to take six nitric hydrate terbium of 1.4324g molten The concentration being configured in 500ml ethanol solution is the solution of 0.00632mol/L), cesium hydroxide solution 50ml(takes 5.0750g cesium hydroxide is dissolved in the solution for being configured to that concentration is 0.060442mol/L in 500ml ethanol solution), and in room Temperature is lower to be uniformly mixed and is sufficiently stirred；Obtained suspension is moved into the reaction kettle of the polytetrafluoroethyllining lining of 150ml, then Baking oven is put into heat 24 hours under the conditions of 135 DEG C；Take out reaction kettle cooling after reaction, supernatant in liner is outwelled, Suitable absolute ethyl alcohol and stirring is added to wash 2 ~ 3 removing soluble-salts, filter, it is then that sediment is dry at 50 DEG C, it obtains To white powder La1.9 Tb0.1(OH)5NO3·1.5H2O；
B, 0. 4724g of product for taking a step to obtain, sodium benzoate 0.5879g is placed in 300ml water, in N2In protective atmosphere Standing wave 15min；It filtering, massive laundering, ethyl alcohol is washed, and it is dry, the rare earth stratified material La of benzoate intercalation is made1.9 Tb0.1(OH)5C6H5COO·1.5H2O；(microwave frequency 2.45G Hz；NO3 -: sodium benzoate=1:4)；
C, the product 0.05g for taking b step to obtain, is placed in 50ml formamide solvent, N according to the ratio of 0.01g/10ml2Protection Suspension is obtained after 40 min of continual ultrasonic under atmospheric condition, after 8000r/min high speed centrifugation 15 minutes, rare earth can be obtained Hydroxide nano piece luminescent material La1.9Tb0.1(OH)5-C6H5COO；Gained nanometer sheet scanning electron microscope is as shown in Figure 1, from figure It can clearly find out that material prepared shows typical laminated structure, size is in 1 ~ 2 micron range.
Embodiment 3
A, lanthanum nitrate hexahydrate 0.6248g, six nitric hydrate terbium solution 11.85ml is taken (six nitric hydrate terbium of 1.4324g to be taken to be dissolved in The concentration being configured in 500ml ethanol solution is the solution of 0.00632mol/L), cesium hydroxide solution 50ml(takes 5.0750g cesium hydroxide is dissolved in the solution for being configured to that concentration is 0.060442mol/L in 500ml ethanol solution), and in room Temperature is lower to be uniformly mixed and is sufficiently stirred；Obtained suspension is moved into the reaction kettle of the polytetrafluoroethyllining lining of 150ml, then Baking oven is put into heat 24 hours under the conditions of 160 DEG C；Take out reaction kettle cooling after reaction, supernatant in liner is outwelled, Suitable absolute ethyl alcohol and stirring is added to wash 2 ~ 3 removing soluble-salts, filter, it is then that sediment is dry at 50 DEG C, it obtains To white powder La1.9 Tb0.1(OH)5NO3·1.5H2O；
B, the product 0.5277g for taking a step to obtain, sodium benzoate 0.6567g is set in 300ml water, in N2Continue in protective atmosphere Microwave 15min；It filtering, massive laundering, ethyl alcohol is washed, and it is dry, the rare earth stratified material La of benzoate intercalation is made1.9 Tb0.1 (OH)5C6H5COO·1.5H2O, (microwave frequency 2.45G Hz；NO3 -: sodium benzoate=1:4)；
C, the product 0.05g for taking b step to obtain, is placed in 50ml formamide solvent, N according to the ratio of 0.01g/10ml2Protection Suspension is obtained after 50 min of continual ultrasonic under atmospheric condition, after 8000r/min high speed centrifugation 15 minutes, rare earth can be obtained Hydroxide nano piece luminescent material La1.9Tb0.1(OH)5-C6H5COO。
Embodiment 4
A, lanthanum nitrate hexahydrate 0.6173g, six nitric hydrate terbium solution 11.90ml is taken (six nitric hydrate terbium of 1.4324g to be taken to be dissolved in The concentration being configured in 500ml ethanol solution is the solution of 0.00632mol/L), cesium hydroxide solution 50ml(takes 5.0750g cesium hydroxide is dissolved in the solution for being configured to that concentration is 0.060442mol/L in 500ml ethanol solution), and in room Temperature is lower to be uniformly mixed and is sufficiently stirred；Obtained suspension is moved into the reaction kettle of the polytetrafluoroethyllining lining of 150ml, then Baking oven is put into heat 24 hours under the conditions of 125 DEG C；Take out reaction kettle cooling after reaction, supernatant in liner is outwelled, Suitable absolute ethyl alcohol and stirring is added to wash 2 ~ 3 removing soluble-salts, filter, it is then that sediment is dry at 50 DEG C, it obtains To white powder La1.9 Tb0.1(OH)5NO3·1.5H2O；
B, 0. 5110g of product for taking a step to obtain, 0.6360 g of sodium benzoate is placed in 300ml water, in N2In protective atmosphere Standing wave 15min；It filtering, massive laundering, ethyl alcohol is washed, and it is dry, the rare earth stratified material La of benzoate intercalation is made1.9 Tb0.1(OH)5C6H5COO·1.5H2O；(microwave frequency 2.45G Hz；NO3 -: sodium benzoate=1:4)；
C, the product 0.05g for taking b step to obtain, is placed in 50ml formamide solvent, N according to the ratio of 0.01g/10ml2Protection Suspension is obtained after continual ultrasonic 30-60 min under atmospheric condition, after 8000r/min high speed centrifugation 15 minutes, can be obtained Rare-earth hydroxide Nanoflake luminescent material La1.9Tb0.1(OH)5-C6H5COO；Gained nanometer sheet scanning electron microscope (SEM) photograph as shown in Fig. 2, It can clearly find out that material prepared shows typical laminated structure from figure, size is mainly in 1 ~ 2 micron range.
Embodiment 5
A, lanthanum nitrate hexahydrate 0.6249g, six nitric hydrate terbium solution 11.87ml is taken (six nitric hydrate terbium of 1.4324g to be taken to be dissolved in The concentration being configured in 500ml ethanol solution is the solution of 0.00632mol/L), cesium hydroxide solution 50ml(takes 5.0750g cesium hydroxide is dissolved in the solution for being configured to that concentration is 0.060442mol/L in 500ml ethanol solution), and in room Temperature is lower to be uniformly mixed and is sufficiently stirred；Obtained suspension is moved into the reaction kettle of the polytetrafluoroethyllining lining of 150ml, then Baking oven is put into heat 24 hours under the conditions of 140 DEG C；Take out reaction kettle cooling after reaction, supernatant in liner is outwelled, Suitable absolute ethyl alcohol and stirring is added to wash 2 ~ 3 removing soluble-salts, filter, it is then that sediment is dry at 50 DEG C, it obtains To white powder La1.9 Tb0.1(OH)5NO3·1.5H2O；
B, the product 0.6229g for taking a step to obtain, 0.7752 g of sodium benzoate is placed in 300ml water, in N2It is held in protective atmosphere Continuous microwave 15min；It filtering, massive laundering, ethyl alcohol is washed, and it is dry, the rare earth stratified material La of benzoate intercalation is made1.9 Tb0.1(OH)5C6H5COO·1.5H2O.(microwave frequency 2.45G Hz；NO3 -: sodium benzoate=1:4)
C, the product 0.05g for taking b step to obtain, is placed in 50ml formamide solvent, N according to the ratio of 0.01g/10ml2Protection Suspension is obtained after 60 min of continual ultrasonic under atmospheric condition, after 8000r/min high speed centrifugation 15 minutes, rare earth can be obtained Hydroxide nano piece luminescent material La1.9Tb0.1(OH)5-C6H5COO；The fluorescence spectra of gained nanometer sheet is as shown in figure 3, institute It is 366nm with excitation wavelength, as can be seen from the figure gained nanometer sheet material has preferable fluorescence property.

Claims (2)

1.一种镧基质的稀土氢氧化物纳米片发光材料的制备方法，其特征在于，该方法包括以下具体步骤：1. a preparation method of the rare earth hydroxide nanosheet luminescent material of lanthanum matrix, is characterized in that, this method comprises the following concrete steps: a、前驱体稀土氢氧化物层状LRHs材料的制备a. Preparation of precursor rare earth hydroxide layered LRHs 取La(NO3)3·6H2O溶解于无水乙醇中，在N2保护气氛中搅拌混合均匀；再按La∶Tb=19∶1的摩尔比，加入Tb(NO3)3·6H2O乙醇溶液；然后按硝酸盐∶氢氧化铯为1∶2的摩尔比，将稀土硝酸盐与CsOH加入无水乙醇中，充分搅拌后；将所得溶液置于聚四氟乙烯衬里的反应釜中，在120-160℃条件下反应24小时；反应完成后，所得样品经抽滤、多次用乙醇洗涤、40℃条件下真空干燥1-2小时，即得到层状前驱体La1.9Tb0.1(OH)5NO3·1.5H2O；Dissolve La(NO 3 ) 3 ·6H 2 O in absolute ethanol, stir and mix evenly in a N 2 protective atmosphere; then add Tb(NO 3 ) 3 ·6H according to the molar ratio of La:Tb=19:1 2 O ethanol solution; then according to the molar ratio of nitrate: cesium hydroxide 1: 2, rare earth nitrate and CsOH are added into absolute ethanol, after fully stirring; the obtained solution is placed in a polytetrafluoroethylene-lined reaction kettle , the reaction was carried out at 120-160 °C for 24 hours; after the reaction was completed, the obtained sample was filtered with suction, washed with ethanol for several times, and dried under vacuum at 40 °C for 1-2 hours to obtain the layered precursor La 1.9 Tb 0.1 (OH) 5 NO 3 ·1.5H 2 O; b、苯甲酸钠插层的LRHs的制备 b. Preparation of sodium benzoate intercalated LRHs 取步骤a中所得La1.9Tb0.1(OH)5NO3·1.5H2O，按照苯甲酸钠与其物质的量之比4∶1的比例加入到苯甲酸钠溶液中，N2保护气氛条件下微波加热15min，抽滤、40℃条件下真空干燥1-2小时，即得到苯甲酸根插层的稀土层状材料La1.9 Tb0.1(OH)5C6H5COO·1.5H2O；Take the La 1.9 Tb 0.1 (OH) 5 NO 3 ·1.5H 2 O obtained in step a, add it to the sodium benzoate solution at a ratio of 4:1 in the ratio of the amount of sodium benzoate to its substance, and microwave heating under the condition of N 2 protective atmosphere 15min, suction filtration, and vacuum drying at 40°C for 1-2 hours to obtain a rare earth layered material La 1.9 Tb 0.1 (OH) 5 C 6 H 5 COO·1.5H 2 O intercalated with benzoate; c、镧基质的稀土氢氧化物纳米片发光材料的制备c. Preparation of lanthanum-based rare earth hydroxide nanosheet luminescent materials 取步骤b得到的产物，按照0.01g/10ml的比例置于甲酰胺溶剂中，N2保护气氛条件下持续超声30-60 min后得到悬浊液，经8000r/min高速离心20分钟后，即得到所述镧基质的稀土氢氧化物纳米片发光材料La1.9Tb0.1(OH)5-C6H5COO。Take the product obtained in step b, put it in a formamide solvent according to the ratio of 0.01g/10ml, continue to sonicate for 30-60 min under the condition of N The lanthanum-based rare earth hydroxide nanosheet light-emitting material La 1.9 Tb 0.1 (OH) 5 -C 6 H 5 COO is obtained. 2.一种权利要求1所述方法制得的镧基质的稀土氢氧化物纳米片发光材料。2. A lanthanum-based rare earth hydroxide nanosheet luminescent material prepared by the method of claim 1.
CN201811364051.7A 2018-11-16 2018-11-16 Rare earth hydroxide nanosheet luminescent material based on lanthanum and preparation method thereof Pending CN109321249A (en)

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