A method for producing erbium-doped yttrium aluminum garnet crystal and optical element

Abstract

The invention discloses a production method of erbium-doped yttrium aluminum garnet crystal for optical elements and a preparation method of optical elements, belonging to the preparation of optical elements, comprising the following steps: S1: raw material processing, comprising the following steps: S2: forming erbium-doped yttrium aluminum garnet crystal, comprising the following steps: S21: loading the material processed by S1 into a molybdenum crucible, and loading it into a vacuum resistance heating furnace; S22: closing the furnace door after loading the furnace, and using a vacuum pump diffusion pump to extract the air in the furnace to make it reach vacuum; S23: filling argon and carbon dioxide into the furnace; S24: starting the power supply to heat to 1200-1800°C; S25: controlling the position of the seed crystal to the surface of the solution; S26: starting to pull the crystal, with a pulling speed of 1-10 mm / h and a rotation speed of 50-200 rpm; S27: waiting until the crystal shoulder is completed, performing interface flipping, with a rotation speed of 30-80 r / min and a pulling speed of 1-3 mm / crystal. The invention has low production cost, short production cycle, high crystal utilization rate of 90%, and improved electro-optic slope by 20%.

Description

Technical Field

[0001] The invention relates to the preparation of optical elements, in particular to a production method of erbium-doped yttrium aluminum garnet crystals used for optical elements and a preparation method of optical elements. Background Art

[0002] Er3+:YAG crystal (Er-doped yttrium aluminum garnet) belongs to the cubic crystal system and is a very promising solid laser material in the mid-infrared band. It can output three wavelengths of laser at room temperature: 1.64μm, 1.78μm and 2.94μm. Among them, 1.64μm and 1.78μm are in the human eye safety band, and 2.94μm is at the hydroxyl absorption peak and can be strongly absorbed by biological tissues. Therefore, it has good application prospects in laser medical treatment, laser communication, laser ranging, etc.

[0003] At present, the main methods used at home and abroad to grow ER3+:YAG crystals are medium-frequency induction heating furnaces and the Czochralski method. However, this method has the disadvantages of high growth cost, long growth cycle, and low crystal utilization rate. In addition, the energy value of optical devices made of the produced ER3+:YAG crystals is relatively low.

[0004] The above background technology is for facilitating the understanding of the present invention and is not a known technology disclosed to the general public before the application of the present invention. Summary of the invention

[0005] In view of the above defects, the present invention provides a method for producing erbium-doped yttrium aluminum garnet crystals for optical elements. The method has low production cost, short production cycle, high crystal utilization rate of 90%, and an electro-optic slope increased by 20%.

[0006] The technical solution is: a method for producing erbium-doped yttrium aluminum garnet crystals for optical elements, comprising the following steps:

[0007] S1: Raw material processing, including the following steps:

[0008] S11: taking aluminum oxide, yttrium oxide and erbium oxide;

[0009] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0010] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0011] S22: After the furnace is loaded, the furnace door is closed and the air in the furnace is extracted using a vacuum pump diffusion pump to achieve vacuum;

[0012] S23: filling the furnace with argon and carbon dioxide;

[0013] S24: Start the power supply to heat to 1200-1800°C;

[0014] S25: controlling the seed crystal position to the solution surface;

[0015] S26: Start crystal pulling, with a pulling speed of 1-10 mm / h and a rotation speed of 50-200 rpm;

[0016] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 30-80r / min and a pulling speed of 1-3mm / min for growth;

[0017] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0018] Furthermore, S1 further comprises the following steps:

[0019] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 800-1300° C.;

[0020] S13: batching the calcined raw materials, wherein the Er doping concentration is 1-50 at %;

[0021] S14: shaping according to the size of the molybdenum crucible and finalizing the shape at 100-300 MPa.

[0022] Furthermore, S1 further comprises the following steps:

[0023] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 800-1300° C.;

[0024] S13: The calcined raw materials are mixed, and the Er doping concentration is 1-50at%.

[0025] Furthermore, S1 further comprises the following steps:

[0026] S13: mixing aluminum oxide, yttrium oxide and erbium oxide, wherein the Er doping concentration is 1-50 at%;

[0027] S14: shaping the molybdenum crucible according to the size of the crucible, and finalizing the shape by using a hydraulic press at 100-300 MPa.

[0028] Furthermore, S1 further comprises the following steps:

[0029] S12: mixing aluminum oxide, yttrium oxide and erbium oxide, wherein the Er doping concentration is 1-50 at%;

[0030] S13: shaping the molybdenum crucible according to the size of the crucible, and finalizing the shape at 100-300 MPa using a hydraulic press;

[0031] S14: placing the shaped body in a corundum crucible and calcining at a temperature of 800-1300°C.

[0032] Furthermore, the volume ratio of argon to carbon dioxide is 10:10-1.

[0033] Furthermore, the volume ratio of argon to carbon dioxide is 10:2-1.

[0034] Furthermore, the Er doping concentration is 15at%.

[0035] The invention also provides a method for preparing an optical element.

[0036] The technical solution is: a method for preparing an optical element, comprising the following steps:

[0037] S3, coating, comprises the following steps:

[0038] S31, taking the erbium-doped yttrium aluminum garnet crystal produced by the above-mentioned production method of the erbium-doped yttrium aluminum garnet crystal for optical elements, cutting it to form an optical element original;

[0039] S32, fix the original optical element to the fixture, place the vacuum chamber, evacuate the vacuum, heat the workpiece, and keep it warm;

[0040] S33, bombarding the optical element with an ion source;

[0041] S34, evaporation to form a film layer, comprising the following steps:

[0042] S341, applying the first low refractive index film material YbF3;

[0043] S342, making the first high refractive index film material ZnS material;

[0044] S343, evaporating a second low refractive index film material Al2O3;

[0045] S344, evaporating the second highest refractive index film material HfO2;

[0046] S345, repeat S341~S344;

[0047] S4, coating is finished and the vacuum chamber is cooled;

[0048] S5, taking out the original optical element to obtain the optical element.

[0049] Compared with the prior art, the present invention has the following beneficial effects:

[0050] The invention has low production cost, short production cycle, high crystal utilization rate of 90%, and improved electro-optic slope by 20%. DETAILED DESCRIPTION

[0051] The present invention will be further described below.

[0052] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected" and "connected" should be understood in a broad sense, for example, it can be a fixed connection, or it can be an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0053] In the description of the present invention, it should be understood that the terms "upper", "lower", "front", "back", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate positions or positional relationships, which are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In the description of the present invention, "plurality" means two or more, unless otherwise precisely and specifically specified.

[0054] The terms "first", "second", "third", "fourth", etc. (if any) in the specification and claims of the present application are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequential order. It should be understood that the data used in this way can be interchangeable where appropriate, so that the embodiments of the present application described herein can, for example, be implemented in an order other than those described herein. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions, for example, a process, method, system, product or device comprising a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or devices.

[0055] In order to make the purpose, technical scheme and advantages of the embodiments of the present application clearer, the technical scheme in the embodiments of the present application will be clearly and completely described below in combination with the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0056] The technical solution of the present invention is described in detail with specific embodiments below. The following specific embodiments can be combined with each other, and the same or similar concepts or processes may not be described in detail in some embodiments.

[0057] In the present invention, high purity refers to a purity greater than or equal to 99.999wt%. In the present invention, unless otherwise specified, it is a common technology in the art.

[0058] Example 1

[0059] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0060] S1: Raw material processing, including the following steps:

[0061] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0062] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 1000° C.;

[0063] S13: batching the calcined raw materials, wherein the Er doping concentration is 15 at %, and the batching is uniformly mixed;

[0064] S14: shaping the molybdenum crucible according to its size and finalizing the shape at 200 MPa using a hydraulic press;

[0065] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0066] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0067] S22: After loading the furnace, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0068] S23: Fill the furnace with argon and carbon dioxide gas to 0.15MPa (the volume ratio of argon to carbon dioxide is 10:1);

[0069] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0070] S25: controlling the seed crystal position to the solution surface;

[0071] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0072] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0073] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0074] Example 2

[0075] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0076] S1: Raw material processing, including the following steps:

[0077] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0078] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 1000° C.;

[0079] S13: batching the calcined raw materials, wherein the Er doping concentration is 10 at %, and the batching is performed and the mixture is mixed uniformly;

[0080] S14: shaping the molybdenum crucible according to its size and finalizing the shape at 200 MPa using a hydraulic press;

[0081] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0082] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0083] S22: After loading the furnace, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0084] S23: Fill the furnace with argon and carbon dioxide gas to 0.15MPa (the volume ratio of argon to carbon dioxide is 10:1);

[0085] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0086] S25: controlling the seed crystal position to the solution surface;

[0087] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0088] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0089] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0090] Example 3

[0091] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0092] S1: Raw material processing, including the following steps:

[0093] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0094] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 1000° C.;

[0095] S13: batching the calcined raw materials, wherein the Er doping concentration is 30 at%, and the batching is followed by uniform mixing;

[0096] S14: shaping the molybdenum crucible according to its size and finalizing the shape at 200 MPa using a hydraulic press;

[0097] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0098] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0099] S22: After loading the furnace, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0100] S23: Fill the furnace with argon and carbon dioxide gas to 0.15MPa (the volume ratio of argon to carbon dioxide is 10:1);

[0101] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0102] S25: controlling the seed crystal position to the solution surface;

[0103] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0104] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0105] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0106] Example 4

[0107] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0108] S1: Raw material processing, including the following steps:

[0109] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0110] S12: mixing aluminum oxide, yttrium oxide and erbium oxide, wherein the Er doping concentration is 15 at%, and mixing the mixture evenly;

[0111] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0112] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0113] S22: After the furnace is loaded, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0114] S23: Fill the furnace with argon and carbon dioxide gas to 0.15MPa (the volume ratio of argon to carbon dioxide is 10:1);

[0115] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0116] S25: controlling the seed crystal position to the solution surface;

[0117] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0118] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0119] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0120] Example 5

[0121] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0122] S1: Raw material processing, including the following steps:

[0123] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0124] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 1000° C.;

[0125] S13: batching the calcined raw materials, wherein the Er doping concentration is 15 at %, and the batching is performed and the mixture is mixed uniformly;

[0126] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0127] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0128] S22: After the furnace is loaded, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0129] S23: Fill the furnace with argon and carbon dioxide gas to 0.15MPa (the volume ratio of argon to carbon dioxide is 10:1);

[0130] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0131] S25: controlling the seed crystal position to the solution surface;

[0132] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0133] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0134] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0135] Example 6

[0136] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0137] S1: Raw material processing, including the following steps:

[0138] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0139] S13: mixing aluminum oxide, yttrium oxide and erbium oxide, wherein the Er doping concentration is 15 at%, and mixing the mixture evenly;

[0140] S14: shaping the molybdenum crucible according to its size and finalizing the shape at 200 MPa using a hydraulic press;

[0141] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0142] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0143] S22: After loading the furnace, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0144] S23: Fill the furnace with argon and carbon dioxide gas to 0.15MPa (the volume ratio of argon to carbon dioxide is 10:1);

[0145] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0146] S25: controlling the seed crystal position to the solution surface;

[0147] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0148] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0149] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0150] Example 7

[0151] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0152] S1: Raw material processing, including the following steps:

[0153] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0154] S12: mixing aluminum oxide, yttrium oxide and erbium oxide, wherein the Er doping concentration is 15 at%, and mixing the mixture evenly;

[0155] S13: shaping the molybdenum crucible according to its size and finalizing the shape by a hydraulic press at 200 MPa;

[0156] S14: placing the shaped body in a corundum crucible and calcining it at a temperature of 1000° C.;

[0157] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0158] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0159] S22: After loading the furnace, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0160] S23: Fill the furnace with argon and carbon dioxide gas to 0.15MPa (the volume ratio of argon to carbon dioxide is 10:1);

[0161] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0162] S25: controlling the seed crystal position to the solution surface;

[0163] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0164] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0165] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0166] Example 8

[0167] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0168] S1: Raw material processing, including the following steps:

[0169] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0170] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 1000° C.;

[0171] S13: batching the calcined raw materials, wherein the Er doping concentration is 15 at %, and the batching is uniformly mixed;

[0172] S14: shaping the molybdenum crucible according to its size and finalizing the shape at 200 MPa using a hydraulic press;

[0173] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0174] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0175] S22: After loading the furnace, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0176] S23: Fill the furnace with argon gas to 0.15MPa;

[0177] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0178] S25: controlling the seed crystal position to the solution surface;

[0179] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0180] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0181] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0182] Example 9

[0183] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0184] S1: Raw material processing, including the following steps:

[0185] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0186] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 1000° C.;

[0187] S13: batching the calcined raw materials, wherein the Er doping concentration is 15 at %, and the batching is performed and the mixture is mixed uniformly;

[0188] S14: shaping the molybdenum crucible according to its size and finalizing the shape at 200 MPa using a hydraulic press;

[0189] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0190] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0191] S22: After the furnace is loaded, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0192] S23: Fill the furnace with carbon dioxide gas to 0.15MPa;

[0193] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0194] S25: controlling the seed crystal position to the solution surface;

[0195] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0196] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0197] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0198] Example 10

[0199] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0200] S1: Raw material processing, including the following steps:

[0201] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0202] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 1000° C.;

[0203] S13: batching the calcined raw materials, wherein the Er doping concentration is 15 at %, and the batching is performed and the mixture is mixed uniformly;

[0204] S14: shaping the molybdenum crucible according to its size and finalizing the shape at 200 MPa using a hydraulic press;

[0205] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0206] S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace;

[0207] S22: After the furnace is loaded, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0208] S23: Fill the furnace with argon and carbon dioxide gas to 0.15MPa (the volume ratio of argon to carbon dioxide is 10:2);

[0209] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0210] S25: controlling the seed crystal position to the solution surface;

[0211] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0212] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0213] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0214] Embodiment 11

[0215] A method for producing erbium-doped yttrium aluminum garnet crystals comprises the following steps:

[0216] S1: Raw material processing, including the following steps:

[0217] S11: taking aluminum oxide (high purity, purchased from the market), yttrium oxide (high purity, purchased from the market) and erbium oxide (high purity, purchased from the market);

[0218] S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 1000° C.;

[0219] S13: batching the calcined raw materials, wherein the Er doping concentration is 15 at %, and the batching is uniformly mixed;

[0220] S14: shaping the molybdenum crucible according to its size and finalizing the shape at 200 MPa using a hydraulic press;

[0221] S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps:

[0222] S21: Load the material processed in S1 into a molybdenum crucible, and load it into a medium frequency induction furnace heating furnace;

[0223] S22: After loading the furnace, close the furnace door and use a vacuum pump diffusion pump to extract the air in the furnace to achieve a high vacuum state (8×10 -3 MPa);

[0224] S23: Fill the furnace with argon and carbon dioxide gas to 0.15MPa (the volume ratio of argon to carbon dioxide is 10:1);

[0225] S24: Start the power supply to heat, and as the temperature rises, observe the situation in the furnace and adjust the pot position until the raw materials are completely melted, adjust to the ideal pot position, and raise the temperature to 1500℃;

[0226] S25: controlling the seed crystal position to the solution surface;

[0227] S26: Start crystal pulling, with a pulling speed of 2 mm / h and a rotation speed of 100 rpm;

[0228] S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 80r / min and a pulling speed of 1.5mm / min for growth;

[0229] S28: The crystal reaches the set length and is finished, then the crystal is cooled to room temperature and taken out.

[0230] Comparisons of Example 1 to Example 11 were made in terms of production cost, production cycle, crystal utilization and detection of erbium-doped yttrium aluminum garnet crystals. The results are shown in Table 1 below.

[0231] Table 1

[0232] Note: Example 11 is used as the calculation basis, and other examples are comparison values ​​with Example 11. Taking the electro-optical slope as an example, the electro-optical slope ratio of Example 11 = the detected electro-optical slope value of Example 11 ÷ the detected electro-optical slope value of Example 11 = 1, and the electro-optical slope ratio of Example 1 = the detected electro-optical slope value of Example 1 ÷ the detected electro-optical slope value of Example 11.

[0233] It can be seen from Table 1 that Example 1 has certain improvements over Example 11 in terms of production cost, production cycle, and crystal utilization.

[0234] The present invention also provides a method for preparing an optical element, comprising the following steps:

[0235] S3, coating, comprises the following steps:

[0236] S31, taking the erbium-doped yttrium aluminum garnet crystal of Example 1, cutting it to form a desired optical element shape (determined according to customer requirements), that is, a workpiece;

[0237] S32, fix the workpiece to the fixture, place the vacuum chamber, evacuate the chamber, and when the pressure in the chamber is less than 6×10 -3 After Pa, heat the workpiece to 100°C and keep it warm for 30 minutes;

[0238] S33, bombard the workpiece with an ion source for 3 min;

[0239] S34, evaporation to form a film layer, comprising the following steps:

[0240] S341, using an electron gun to evaporating the first low refractive index film material YbF3, the vacuum chamber pressure is less than 3×10-3Pa, the evaporation rate is 7Å / s, the film thickness is monitored by the crystal oscillator method, and the thickness is 400nm;

[0241] S342, using an electron gun to evaporation the first high refractive index film material ZnS material, the vacuum chamber pressure during evaporation is less than 3×10-3Pa, the evaporation rate is 6 Å / s, the film thickness is monitored by the crystal oscillator method, and the thickness is 380nm;

[0242] S343, using electron gun to evaporate the second lowest refractive index film material Al2O3, the vacuum chamber pressure during evaporation is less than 3×10-3Pa, the evaporation rate is 3 Å / s, the film thickness is monitored by crystal oscillator method, and the thickness is 150nm;

[0243] S344, using electron gun to evaporate the second highest refractive index film material HfO2, the vacuum chamber pressure during evaporation is 9×10-4Pa, the evaporation rate is 5 Å / s, the film thickness is monitored by crystal oscillator method, and the thickness is 120nm;

[0244] S345, repeat S341~S344;

[0245] S4, coating is completed and the vacuum chamber is cooled to 50°C;

[0246] S5, take out the workpiece and obtain the optical element.

[0247] The average energy value of the optical element measured at 490V is 473 mJ.

[0248] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for producing erbium-doped yttrium aluminum garnet crystal for optical elements, comprising the following steps: S1: Raw material processing, including the following steps: S11: taking aluminum oxide, yttrium oxide and erbium oxide; S2: forming an erbium-doped yttrium aluminum garnet crystal, comprising the following steps: S21: Load the material processed in S1 into a molybdenum crucible and then into a vacuum resistance heating furnace; S22: After the furnace is loaded, the furnace door is closed and the air in the furnace is extracted using a vacuum pump diffusion pump to achieve vacuum; S23: filling the furnace with argon and carbon dioxide; S24: Start the power supply to heat to 1200-1800°C; S25: controlling the seed crystal position to the solution surface; S26: Start crystal pulling, with a pulling speed of 1-10 mm / h and a rotation speed of 50-200 rpm; S27: Wait until the crystal shoulder is released, and then perform interface flipping, with a rotation speed of 30-80r / min and a pulling speed of 1-3mm / min for growth; S28: The crystal reaches the set length, is finished, and then the crystal is cooled to room temperature and taken out; S1 also includes the following steps: S12: placing aluminum oxide, yttrium oxide, and erbium oxide in a corundum crucible and calcining them at a temperature of 800-1300° C.; S13: batching the calcined raw materials, wherein the Er doping concentration is 1-50 at %; S14: shaping according to the size of the molybdenum crucible and finalizing the shape at 100-300 MPa; The volume ratio of argon to carbon dioxide is 10:2-1.

2. The method for producing erbium-doped yttrium aluminum garnet crystal for optical elements according to claim 1, characterized in that: The Er doping concentration is 15 at %.

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