CN111977680A - Preparation method of yttrium oxide lutetium cerium for scintillator crystal - Google Patents
Preparation method of yttrium oxide lutetium cerium for scintillator crystal Download PDFInfo
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- CN111977680A CN111977680A CN202010945105.XA CN202010945105A CN111977680A CN 111977680 A CN111977680 A CN 111977680A CN 202010945105 A CN202010945105 A CN 202010945105A CN 111977680 A CN111977680 A CN 111977680A
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Abstract
The invention relates to a preparation method of yttrium oxide lutetium cerium for a scintillation crystal, belonging to the technical field of rare earth extraction and separation. The preparation method comprises the following steps: step 1: uniformly mixing back extraction solutions of three rare earth ions according to the stoichiometric ratio of the three rare earth elements of yttrium, lutetium and cerium, adjusting the pH value of the solution to 2-3 by using ammonia water, and heating to obtain a solution a; step 2: according to the molar ratio of the total rare earth to the oxalic acid as a precipitator of 1: 1.8-2.2, preparing an oxalic acid solution, and heating the oxalic acid solution to obtain a solution b; and step 3: slowly adding the solution a into the solution b under the stirring condition, stirring, standing and aging for 3-6 h, and filtering to obtain yttrium lutetium cerium oxalate precipitate; and 4, step 4: and (3) depositing yttrium lutetium cerium oxalate in a muffle furnace, and burning for 2-4 h at 800-1200 ℃ to obtain yttrium lutetium cerium oxide powder. The yttrium oxide lutetium cerium powder prepared by the invention has the advantages of uniform distribution of rare earth elements, accurate and adjustable element content and the like, and can provide raw materials for preparation of scintillation crystals such as LYSO, LuYAP and the like.
Description
Technical Field
The invention belongs to the technical field of rare earth extraction and separation, and particularly relates to a preparation method of yttrium lutetium cerium oxide for a scintillation crystal.
Background
The rare earth element has excellent physical and chemical properties such as light, electricity, magnetism and the like due to the unique electronic structure, is widely applied to high-tech fields such as electronic information, energy environmental protection, national defense and military industry, high and new materials, biomedical and the like, and is a key dominant strategic mineral resource in China. For example, scintillation crystals such as cerium-doped yttrium lutetium silicate (LYSO) and yttrium lutetium aluminate (LuYAP) have excellent performances such as high density, high light output, short decay time and the like, and have wide application prospects in the fields of high-energy physics, nuclear medicine and safety detection. For example: currently, LYSO scintillation crystals are key materials for manufacturing Positron Emission Tomography (PET) high-end diagnosis and treatment equipment, and lutetium oxide has an irreplaceable effect in scintillation crystal preparation. Domestic heavy rare earth separation enterprises have produced 4N-5N products such as high-purity lutetium oxide and the like, and market demands in the fields of scintillation crystals and the like are met. In the preparation process of the scintillation crystal, a plurality of high-purity rare earth oxides such as high-purity lutetium oxide (> 4N-5N), yttrium oxide (> 4N-5N), cerium oxide (> 4N-5N) and the like need to be uniformly mixed to form a rare earth mixture. The scintillation crystal prepared from the rare earth mixture has the problems of unreasonable product cost performance and the like caused by unclear standards of rare earth oxide products and blind pursuit of high purification, and restricts the application and development of downstream industries.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides a preparation method of yttrium oxide lutetium cerium for a scintillation crystal. The yttrium oxide lutetium cerium powder prepared by the invention has the advantages of uniform distribution of rare earth elements, accurate and adjustable element content and the like, and can provide raw materials for preparation of scintillation crystals such as LYSO, LuYAP and the like.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the invention provides a flashThe preparation method of the yttrium oxide lutetium cerium for the crystal comprises the following steps: (Y)yLu(1-x-y))2O3xCe, wherein x is 0.001-0.01, and y is 0.05-0.3;
the preparation method comprises the following steps:
step 1: uniformly mixing back extraction solutions of three rare earth ions according to the stoichiometric ratio of three rare earth elements of yttrium, lutetium and cerium in the chemical general formula, adjusting the pH value of the solution to 2-3 by using ammonia water, and heating to obtain a solution a;
step 2: according to the molar ratio of the total rare earth to the oxalic acid as a precipitator of 1: 1.8-2.2, preparing an oxalic acid solution, and heating the oxalic acid solution to obtain a solution b;
and step 3: slowly adding the solution a into the solution b under the stirring condition, stirring, standing and aging for 3-6 h, and filtering to obtain yttrium lutetium cerium oxalate precipitate;
and 4, step 4: and (3) depositing yttrium lutetium cerium oxalate in a muffle furnace, and burning for 2-4 h at 800-1200 ℃ to obtain yttrium lutetium cerium oxide powder.
In the above technical solution, it is preferable that: the back extraction solution of the rare earth ions in the step 1 is hydrochloric acid or nitric acid back extraction solution of the rare earth ions.
In the above technical solution, it is preferable that: in step 1, the solution is heated to 80 ℃.
In the above technical solution, it is preferable that: heating in the step 2 until the temperature of the oxalic acid solution is 80 ℃.
In the above technical solution, it is preferable that: the stirring time in step 3 was 30 min.
In the above technical solution, it is preferable that: in the step 1, the three rare earth ions of yttrium, lutetium and cerium respectively account for 15%, 84.9% and 0.1% of the total rare earth.
In the above technical solution, it is preferable that: in the step 1, ammonia water is used for adjusting the pH value of the solution to 2.
In the above technical solution, it is preferable that: in the step 2, according to the molar ratio of the total rare earth to the precipitator oxalic acid of 1: 1.8 preparing oxalic acid solution.
In the above technical solution, it is preferable that: and standing and aging for 3 hours in the step 3.
In the above technical solution, it is preferable that: in the step 4, the yttrium lutetium cerium oxalate precipitate is burnt in a muffle furnace at 900 ℃ for 3 h.
The invention has the beneficial effects that:
1. compared with a solid phase mixing method of various rare earth oxides, the yttrium oxide lutetium cerium powder prepared by adopting the coprecipitation method has the advantages of uniform distribution of rare earth elements and the like, and can meet the requirements of scintillation crystals such as LYSO, LuYAP and the like.
2. Compared with the existing preparation process of the heavy rare earth such as high-purity lutetium oxide, the invention combines the market and product technical requirements of the scintillation crystal on the rare earth such as lutetium oxide, and the like, properly reduces the content control standard of specific elements such as yttrium oxide, cerium oxide, silicon dioxide (or aluminum oxide) and the like in lutetium oxide products in the lutetium oxide separation process, and can effectively reduce the production cost of the lutetium oxide and other products.
3. The method is closely linked with a rare earth extraction separation production process, adopts rare earth strip liquor as a raw material, can realize accurate and controllable preparation of yttrium lutetium cerium oxide by regulating and controlling the proportion of three rare earth elements of yttrium lutetium cerium, and has the advantages of simple preparation process, low cost and easy control and amplification.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is an XRD spectrum of the yttrium lutetium cerium oxide powder prepared in example 1.
FIG. 2 is an SEM image of the yttrium lutetium cerium oxide powder prepared in example 1.
FIG. 3 is a mapping map of the yttrium lutetium cerium oxide powder prepared in example 1.
Detailed Description
The invention idea of the invention is as follows: according to the market and product technical requirements of the scintillation crystal on lutetium oxide, the content control standard of specific elements such as yttrium oxide, cerium oxide, silicon dioxide (or aluminum oxide) and the like in lutetium oxide products is properly reduced in the lutetium oxide separation production process, so that the lutetium oxide production cost can be effectively reduced, and a new thought is provided for heavy rare earth separation process design. In the preparation process of the rare earth oxide, the preparation of the yttrium oxide lutetium cerium for the scintillator is realized by accurately regulating and controlling the stoichiometric ratio of three rare earth elements of yttrium lutetium cerium. In order to solve the problem, the invention uses rare earth back extraction liquid in a rare earth separation process as raw material liquid to prepare yttrium lutetium cerium oxide by a rare earth element coprecipitation technology around the important requirement of scintillation crystals such as LYSO, LuYAP and the like on yttrium lutetium cerium oxide products, so that the scintillation crystals can be prepared by accurately adjusting rare earth elements in the yttrium lutetium cerium oxide. The yttrium oxide lutetium cerium prepared by the invention has the advantages of uniform distribution of rare earth elements, accurate and adjustable element content and the like, and can provide raw materials for preparation of scintillation crystals such as LYSO, LuYAP and the like.
The invention relates to a preparation method of yttrium oxide lutetium cerium for a scintillator, wherein the chemical general formula of the yttrium oxide lutetium cerium is as follows: (Y)yLu(1-x-y))2O3xCe, wherein x is 0.001-0.01, and y is 0.05-0.3;
step 1: according to the stoichiometric ratio of three rare earth elements of yttrium, lutetium and cerium in the chemical general formula, hydrochloric acid or nitric acid back extraction solutions of three rare earth ions are uniformly mixed, ammonia water is used for adjusting the pH value of the solution to be 2-3, and the solution a is obtained by heating to 80 ℃.
Step 2: according to the molar ratio of the rare earth to the oxalic acid as the precipitant of 1: 1.8-2.2, preparing an oxalic acid solution, and heating the oxalic acid solution to 80 ℃ to obtain a solution b;
and step 3: slowly adding the solution a into the solution b under the stirring condition, stirring for 30min, standing and aging for 3-6 h, and filtering to obtain yttrium lutetium cerium oxalate precipitate;
and 4, step 4: and (3) depositing yttrium lutetium cerium oxalate in a muffle furnace, and burning for 2-4 h at 800-1200 ℃ to obtain yttrium lutetium cerium oxide powder.
In the above production method, it is preferable that: in the step 1: the three rare earth ions of yttrium, lutetium and cerium respectively account for 15 percent, 84.9 percent and 0.1 percent of the total rare earth, and the pH value of the solution is adjusted to 2 by ammonia water; in the step 2, according to the molar ratio of the total rare earth to the precipitator oxalic acid of 1: 1.8 preparing an oxalic acid solution; standing and aging for 3 hours in the step 3; in the step 4, the yttrium lutetium cerium oxalate precipitate is burnt in a muffle furnace at 900 ℃ for 3 h.
Example 1 (Y)0.15Lu0.849)2O31 per mill Ce preparation
Uniformly mixing 0.01mol of yttrium chloride, lutetium chloride and cerium chloride back extraction solution according to the proportion of yttrium, lutetium and cerium in the total rare earth of 15%, 84.9% and 0.1%, adjusting the pH value of the solution to 2.00 by using ammonia water, and heating the solution to 80 ℃; preparing 0.018mol of oxalic acid solution, and heating the solution to 80 ℃; slowly dripping the mixed rare earth solution into an oxalic acid solution under the condition of magnetic stirring, stirring for 30min, standing and aging for 3 h; precipitating and filtering to obtain solid yttrium lutetium cerium oxalate, and burning for 3h in a muffle furnace at 900 ℃ to obtain yttrium lutetium cerium oxide powder. FIG. 1 is an XRD pattern of this sample, consistent with JCPDS standard card of lutetium oxide (43-1021). FIG. 2 is the SEM of the sample, FIG. 3 is the mapping spectrum of the sample, and it can be seen from FIGS. 2 and 3 that the distribution of the three rare earth elements of yttrium, lutetium and cerium is relatively uniform.
Example 2 (Y)0.05Lu0.945)2O3Preparation of 5 per mill Ce
Uniformly mixing 0.01mol of yttrium chloride, lutetium chloride and cerium chloride back extraction solution according to the proportion of 5%, 94.5% and 0.5% of yttrium, lutetium and cerium in the total rare earth, adjusting the pH value of the solution to 3.00 by using ammonia water, and heating the solution to 80 ℃; preparing 0.02mol of oxalic acid solution, and heating the solution to 80 ℃; slowly dripping the mixed rare earth solution into an oxalic acid solution under the condition of magnetic stirring, stirring for 30min, standing and aging for 4 h; precipitating and filtering to obtain solid yttrium lutetium cerium oxalate, and burning for 2h in a muffle furnace at 1200 ℃ to obtain yttrium lutetium cerium oxide powder.
The yttrium oxide lutetium cerium powder prepared by the embodiment has the advantages of uniform distribution of rare earth elements and the like, and can meet the requirements of scintillation crystals such as LYSO, LuYAP and the like.
Example 3 (Y)0.10Lu0.899)2O31 per mill Ce preparation
Uniformly mixing yttrium nitrate, lutetium nitrate and cerium nitrate back-extraction solution with the total rare earth of 0.01mol according to the proportion of yttrium, lutetium and cerium in the total rare earth of 10%, 89.9% and 0.1%, adjusting the pH value of the solution to 2.00 by using ammonia water, and heating the solution to 80 ℃; preparing 0.022mol of oxalic acid solution, and heating the solution to 80 ℃; slowly dripping the mixed rare earth solution into an oxalic acid solution under the condition of magnetic stirring, stirring for 30min, standing and aging for 6 h; precipitating and filtering to obtain solid yttrium lutetium cerium oxalate, and burning for 4h in a muffle furnace at 800 ℃ to obtain yttrium lutetium cerium oxide powder.
The yttrium oxide lutetium cerium powder prepared by the embodiment has the advantages of uniform distribution of rare earth elements and the like, and can meet the requirements of scintillation crystals such as LYSO, LuYAP and the like.
Example 4 (Y)0.30Lu0.69)2O31% Ce preparation
Uniformly mixing yttrium nitrate, lutetium nitrate and cerous nitrate back-extraction solution with the total rare earth of 0.01mol according to the proportion of 30%, 69% and 1% of yttrium, lutetium and cerium in the total rare earth, adjusting the pH value of the solution to 2.50 by using ammonia water, and heating the solution to 80 ℃; preparing 0.02mol of oxalic acid solution, and heating the solution to 80 ℃; slowly dripping the mixed rare earth solution into an oxalic acid solution under the condition of magnetic stirring, stirring for 30min, standing and aging for 4 h; precipitating and filtering to obtain solid yttrium lutetium cerium oxalate, and burning for 3h in a muffle furnace at 1000 ℃ to obtain yttrium lutetium cerium oxide powder.
The yttrium oxide lutetium cerium powder prepared by the embodiment has the advantages of uniform distribution of rare earth elements and the like, and can meet the requirements of scintillation crystals such as LYSO, LuYAP and the like.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A preparation method of yttrium oxide lutetium cerium for a scintillator is characterized in that the chemical general formula of yttrium oxide lutetium cerium is as follows: (Y)yLu(1-x-y))2O3xCe, wherein x is 0.001-0.01, and y is 0.05-0.3;
the preparation method comprises the following steps:
step 1: uniformly mixing back extraction solutions of three rare earth ions according to the stoichiometric ratio of three rare earth elements of yttrium, lutetium and cerium in the chemical general formula, adjusting the pH value of the solution to 2-3 by using ammonia water, and heating to obtain a solution a;
step 2: according to the molar ratio of the total rare earth to the oxalic acid as a precipitator of 1: 1.8-2.2, preparing an oxalic acid solution, and heating the oxalic acid solution to obtain a solution b;
and step 3: adding the solution a into the solution b under the condition of stirring, standing and aging for 3-6 h, and filtering to obtain yttrium lutetium cerium oxalate precipitate;
and 4, step 4: and (3) depositing yttrium lutetium cerium oxalate in a muffle furnace, and burning for 2-4 h at 800-1200 ℃ to obtain yttrium lutetium cerium oxide powder.
2. The method according to claim 1, wherein the stripping solution of rare earth ions in step 1 is hydrochloric acid or nitric acid stripping solution of rare earth ions.
3. The method according to claim 1, wherein the heating in step 1 is carried out to a solution temperature of 80 ℃.
4. The method according to claim 1, wherein the heating in step 2 is carried out to a temperature of the oxalic acid solution of 80 ℃.
5. The method according to claim 1, wherein the stirring time in the step 3 is 30 min.
6. The method according to any one of claims 1 to 5, wherein the three rare earth ions of yttrium, lutetium and cerium in step 1 respectively account for 15%, 84.9% and 0.1% of the total rare earth.
7. The method according to claim 6, wherein the pH of the solution is adjusted to 2 in step 1 with aqueous ammonia.
8. The preparation method according to claim 6, wherein in the step 2, the molar ratio of the total rare earth to the oxalic acid as the precipitant is 1: 1.8 preparing oxalic acid solution.
9. The method according to claim 6, wherein the standing and aging time in step 3 is 3 hours.
10. The method of claim 6, wherein the yttrium lutetium cerium oxalate precipitate in step 4 is burned in a muffle furnace at 900 ℃ for 3 h.
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