CN1283853C - Preparation process for lithium niobate crystal with near stoichiometric ratio - Google Patents
Preparation process for lithium niobate crystal with near stoichiometric ratio Download PDFInfo
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- CN1283853C CN1283853C CN 200410019732 CN200410019732A CN1283853C CN 1283853 C CN1283853 C CN 1283853C CN 200410019732 CN200410019732 CN 200410019732 CN 200410019732 A CN200410019732 A CN 200410019732A CN 1283853 C CN1283853 C CN 1283853C
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- lithium niobate
- fusant
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- niobate crystals
- crystal
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Abstract
The present invention relates to preparation of lithium niobate crystals approaching stoichiometric proportion, particularly to preparation technology of lithium niobate crystals with uniform ingredients, which belongs to the technical field of photoelectric material preparation. Because lithium niobate crystals are not in congruent melting, crystallized solid ingredients and fusant ingredients are inconsistent; when the fusant ingredients continuously change, the crystallized solid ingredients also continuously change; therefore, lithium niobate crystals with uniform ingredients are difficult to obtain. Thus, the present invention discloses preparation technology for lithium niobate crystals approaching the stoichiometric proportion; the preparation technology has the technical scheme that in the technology for growing lithium niobate crystals in double crucibles by a Czochralski method, melt feed particles of which the ration of Nb to Li is 64:36 are added to fusant along with crystal growth so that the fusant ingredients are constant. The present invention has the advantages that the fusant addition is favorable for diffusion so that the crystal growth speed is quickened, and the production efficiency is enhanced; raw materials are 36 mol% of Li, and are eutectic point raw materials with the lowest melting point in the system of Li2O. Nb2O5 of which the Li content is smaller than 50 mol%; the raw materials are favorable for fusant addition.
Description
Technical Field
The invention relates to preparation of a lithium niobate crystal with a near chemical ratio, in particular to a preparation process of a lithium niobate crystal with uniform components, belonging to the technical field of photoelectric material preparation.
Background
Because the lithium niobate crystal is not eutectic with different components, namely the molten lithium niobate melt with the molar ratio of Nb to Li being 1, the crystallized solid component is inconsistent with the melt component, and the ratio of Nb to Li being more than 1, the components of the melt are changed continuously, and the crystallized solid component is also changed continuously. It is therefore difficult to obtain lithium niobate crystals having a uniform composition. The solid component crystallized from the molten lithium niobate melt having a molar ratio of Nb to Li of 51.4 to 48.6 was consistent with the melt component, and a lithium niobate crystal having a uniform composition could be obtained relatively easily, but the crystal composition deviated from the chemical ratio.
In order to obtain the lithium niobate crystal with uniform components and near stoichiometric ratio, the following technologies are adopted at present:
1. flux method. Potassium oxide is added into the lithium niobate raw material as a fluxing agent, so that the eutectic point of the same components of the lithium niobate is close to the chemical ratio.
2. Double crucible technology. During crystal growth, a melt of Nb and Li of 42: 58-41: 59 is used to grow a crystal of Nb and Li of 1. Meanwhile, as the crystal grows, solid raw material particles of Nb: Li 1 are added into the melt. The composition of the melt is maintained constant.
3. Gas phase equilibrium method. The lithium niobate crystal with the same component ratio is put into an Li-rich atmosphere, and the content of Li in the lithium niobate crystal is increased through diffusion, so that the lithium niobate crystal with the uniform components and the near chemical ratio is obtained.
4. A zone melting method. Melting and crystallizing in the micro-area, so that the diffusion of the melt in the lithium niobate is limited, and thus, the lithium niobate crystal with near chemical ratio is obtained.
Disclosure of Invention
The invention discloses a preparation process of a near stoichiometric lithium niobate crystal, which aims to obtain the near stoichiometric lithium niobate crystal with uniform components, and the technical scheme is as follows: in the process of growing lithium niobate crystals by the double-crucible Czochralski method, a melt of Nb and Li of 42: 58-41: 59 is used for growing crystals of Nb and Li of 1, and the method is characterized in that: adding Nb-Li (64: 36) molten raw materials into the melt along with the growth of the crystal to keep the components of the melt unchanged,
the invention has the beneficial effects that: a. the added melt is favorable for diffusion, so that the crystal growth speed can be accelerated, and the production efficiency is improved; the raw material having a Li content of 36mol% is Li having a Li content of less than 50mol%2O·Nb2O5The eutectic point raw material with the lowest melting point in the system is beneficial to adding a melt because the melting point is closest to the melting point of the growth raw material with the Li content of 58-59 mol%.
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Detailed Description
The preparation process of the near-stoichiometric lithium niobate crystal is characterized in that in the process of growing the lithium niobate crystal by a double-crucible Czochralski method, a melt of Nb and Li of 42: 58-41: 59 is used for growing the crystal of Nb and Li of 1, and the preparation process is characterized in that: adding molten raw material particles of Nb and Li (64:36) into the melt along with the growth of the crystal to keep the components of the melt unchanged,
expressed in simplified form as follows:
Claims (1)
1. a preparation process of a lithium niobate crystal with a near chemical ratio utilizes a melt with the molar ratio of Nb to Li being 41-42: 58-59 to grow a crystal with the molar ratio of Nb to Li being 1 in a process of growing the lithium niobate crystal by a Czochralski method, and is characterized in that: adding a molten raw material with the molar ratio of Nb to Li being 64 to 36 into the melt along with the growth of the crystal to keep the components of the melt unchanged,
expressed in simplified form as follows:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410019732 CN1283853C (en) | 2004-06-23 | 2004-06-23 | Preparation process for lithium niobate crystal with near stoichiometric ratio |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410019732 CN1283853C (en) | 2004-06-23 | 2004-06-23 | Preparation process for lithium niobate crystal with near stoichiometric ratio |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1594673A CN1594673A (en) | 2005-03-16 |
| CN1283853C true CN1283853C (en) | 2006-11-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410019732 Expired - Fee Related CN1283853C (en) | 2004-06-23 | 2004-06-23 | Preparation process for lithium niobate crystal with near stoichiometric ratio |
Country Status (1)
| Country | Link |
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| CN (1) | CN1283853C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105839178B (en) * | 2016-04-12 | 2019-01-04 | 盐城市振弘电子材料厂 | A kind of preparation method of lithium niobate monocrystal |
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2004
- 2004-06-23 CN CN 200410019732 patent/CN1283853C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
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| CN1594673A (en) | 2005-03-16 |
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