CN102139517A - Method for cutting water/oxygen-sensitive rare-earth halide crystal - Google Patents
Method for cutting water/oxygen-sensitive rare-earth halide crystal Download PDFInfo
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- CN102139517A CN102139517A CN2010106012659A CN201010601265A CN102139517A CN 102139517 A CN102139517 A CN 102139517A CN 2010106012659 A CN2010106012659 A CN 2010106012659A CN 201010601265 A CN201010601265 A CN 201010601265A CN 102139517 A CN102139517 A CN 102139517A
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Abstract
The invention relates to a method for cutting a water/oxygen-sensitive rare-earth halide crystal, which adopts a wire cutting method and comprises the following steps: using hydrophobic protective oil or polyimide to protect the crystal surface; mixing aluminum oxide, silicon carbide, cerium oxide or mixture thereof with protective cutting oil in a certain proportion to obtain cutting mud; and cutting the water/oxygen-sensitive rare-earth halide crystal by using a wire cutting machine. In the invention, the crystal surface protective layer and the water/oxygen-proof protective oil in the cutting process are designed for common protection, and the wire cutting machine provided with a stainless steel cutting wire which is plated or not plated with diamonds, is adopted, thereby implementing continuous cutting of the water/oxygen-sensitive rare-earth halide crystal. The crystal cut by the method provided by the invention has the advantages of uniform thickness and no air slaking on the surface, and ensures the subsequent processing and utilization of the crystal.
Description
[technical field]
The present invention relates to a kind of in air the cutting method of the rotten water oxygen responsive type rare earth halide crystal of deliquescence very easily, belong to the crystalline material manufacture field.
[technical background]
The rare earth halide crystal is the new lover in the artificial lens family, is widely used in fields such as high-energy physics, nuclear physics, Radiation Medicine, geological prospecting, explosion-proof detection.Rare earth halide crystal involved in the present invention is meant that doping with rare-earth ions is (such as Ce
3+) scintillation crystal, under the irradiation of high energy particle (X ray or gamma-rays), can send the large single crystal of ultraviolet light, visible light or infrared light.
The rare earth doped halide of cerium, Ce:LnX
3(Ln=La, Lu, Gd, Y; X=Cl, Br I), is the hot fields of Recent study, because of it has characteristics such as high light output efficiency, fast decay, very high energy resolution and growth temperature are low, aspect medical imaging technology and the radioactive substance detection great application prospect is being arranged.Representational halogenation lanthanum crystal LaCl
3And LaBr
3, be water white hexagonal crystal system, its space point group is P63/m, UCl3 type structure.LaCl
3Be a kind of novel scintillation crystal of finding in 1999, density is 3.86g/cm
3, fusing point is 859 ℃.LaBr
3Be a kind of new crystal of finding calendar year 2001, density is 5.29g/cm
3, fusing point is 783 ℃.Ce:LaBr
3Have the output of high light, response fast, excellent energy resolution and temporal resolution, its energy resolution of 2.6% that has is classic in the present inorganic scintillation crystal.France company of Saint-Gobain has obtained the exclusiveness mandate (P.Dorenbos of the exclusive patent of invention of rare earth halide, et.al., Scintillator crystals, method for making same, user thereof, US Patent 7067816B2,2006), and realized the commercialization of radiation detecting device with LaCl3 and LaBr3 monocrystalline.
Rare earth halide has lower fusing point, therefore is fit to use Bridgman-Stockbarge method for growing.But because easy deliquescence of raw material and oxidation adopt anhydrous raw material to overcome this difficult point in the harsh conditions of silica crucible Vacuum Package at present in the world mostly.The rare earth halide device also is encapsulated in the closed container and uses, but the processing of crystal is difficult to realize particularly extremely responsive to water oxygen Ce:LaBr3 crystal by the closed container encapsulation.Rare earth halide has very strong hygroscopy, the Ce:LaBr that 2mm is square
3Crystal, behind the exposure 15mins, the surface will absorb water and slight bluring in 25 ℃ atmosphere, then can become cotton spherical by deliquescence behind the placement 24h, even by solid-state monocrystalline liquefy shape.This is that when the water of crystal absorption reached a certain amount of, dissolution of crystals formed solution in water because the rare earth halide crystal easily absorbs airborne water.
The cutting of rare earth halide generally utilizes wire cutting machine to realize, its cutting mud is mixed by cutting abrasive material and protectiveness oil.Wire cutting machine is a kind of cutting equipment that develops rapidly the nearly more than ten years, and its principle is: the steel wire drive by a high-speed motion rubs to material attached to the cutting blade material on the steel wire, thereby reaches cutting effect.The line of wire cutting machine directly is generally less than 2mm, once can cut hundreds of simultaneously, and the wafer bending degree of its cutting is little, and angularity is little, the depth of parallelism is good, and the gross thickness tolerance is little, between sheet the cutting loss few, the processed wafer surface damage layer is shallow, roughness is little, slice processing piece rate height, production efficiency height.Therefore, how to realize the line cutting of water oxygen responsive type crystal water proof oxygen barriers such as rare earth halide, have very big economic worth and actual demand.
[summary of the invention]
The objective of the invention is in order to solve water oxygen responsive type rare earth halide crystal problem of deliquescence very easily in cutting; designed the common protection of water proof oxygen barrier protectiveness oil in plane of crystal protective layer and the cutting process; the plating or the wire cutting machine of the stainless steel cut line of gold-plated hard rock not are equipped with in employing, have realized the continuous cutting of water oxygen responsive type crystal.
Technical solution of the present invention is:
A kind of cutting method of water oxygen responsive type rare earth halide crystal by evenly smear the laggard line cutting processing of fish tail and waterproof layer at plane of crystal, need constantly be packed into cutting mud in the line cutting processing.It is characterized in that: described fish tail and waterproof layer is hydrophobicity protection grease or polyimides; Described cutting mud is mixed by cutting abrasive material and protectiveness cutting oil.Described water oxygen responsive type rare earth halide crystal refers in air the very easily rotten rare earth halide crystal of deliquescence, and its chemical formula is Ln
1-xCe
xX
3, Ln=La, Lu, Gd, Y here; X=Cl, Br, I, subscript x refer to the doping content of Ce.The hydrophobicity protection grease that described rare earth halide plane of crystal is smeared is a vaseline, and thickness is 0.1～2mm.The polyimides layer thickness that described rare earth halide plane of crystal is surrounded by is 0.1～1mm's.Described cutting abrasive material can be SiC, Al2O3, CeO or its mixture, and the protectiveness cutting oil can be silicone oil, kerosene or its mixture.Described rare earth halide crystal is fixed on the standard component by anaerobic adhesive.Rare earth halide by the corrosion of having avoided water oxygen in protective layer, the cutting process owing to protectiveness cutting oil guard, utilizes the high speed of line of cut and cutting mud to move back and forth before cutting, realizes the very easily protectiveness cutting of deliquescence crystal.Line cutting processing concrete steps are as follows:
(1) adjust wire cutting machine and be in level, line of cut is installed on the reel, then by regulating wheel and guide roller, the line of cut of adjusting on reel, regulating wheel and the guide roller is in the same plane, and the even tension on the line of cut is distributed;
(2) crystal to be cut that will fix is installed on the Cutting platform;
(3) determine cutting parameter;
(4) by the parameter sliced crystal of setting, the crystal of well cutting is placed in the protectiveness oil.
[specific embodiment]
Embodiment 1:1 inch 5at%Ce doping LaBr
3The cutting of crystal
Adopt homemade multi-line cutting machine, at 5at%Ce doping LaBr
3Plane of crystal is smeared the vaseline protective layer, utilizes the high speed of stainless steel cut line and cutting mud to move back and forth, and realizes LaBr
3The water proof oxygen barrier cutting of crystal.Concrete steps are as follows:
(1) evenly coat the vaseline protective layer at plane of crystal, thickness is about 0.8mm;
(2) wipe part vaseline gently with fine sandpaper, utilize anaerobic adhesive that crystal is fixed on the standard component;
(3) SiC is evenly mixed as cutting mud with silicone oil;
(4) adjust wire cutting machine and be in level, line of cut is installed on the reel, then by regulating wheel and guide roller, the line of cut of adjusting on reel, regulating wheel and the guide roller is in the same plane, and the even tension on the line of cut is distributed;
(5) crystal to be cut that will fix is installed on the Cutting platform;
(6) determine cutting parameter: work takes turns to rotating speed and adopts 80% of its maximum (top) speed, and Wire Wheel speed is made as 20m/min, and cutting speed is 2mm/h, and the angle of waving is 3600 °/min of frequency
(7) by the parameter sliced crystal of setting, the crystal of well cutting is placed in the protectiveness oil.
The Ce:LaBr3 plane of crystal that cutting obtains is smooth, does not have corrosion phenomenon.
Embodiment 2:1.5 in2 at%Ce doping LaCl
3The cutting of crystal
Adopt homemade multi-line cutting machine, at 2at%Ce doping LaCl
3Plane of crystal is smeared the vaseline protective layer, utilizes the high speed of stainless steel cut line and cutting mud to move back and forth realization LaCl
3The water proof oxygen barrier cutting of crystal.Concrete steps are as follows:
(1) evenly coat the vaseline protective layer at plane of crystal, thickness is about 0.5mm;
(2) wipe part vaseline gently with fine sandpaper, utilize anaerobic adhesive that crystal is fixed on the standard component;
(3) with SiC and Al
2O
3After the even mixing of 1: 4 ratio of weight ratio, evenly to mix as cutting mud with kerosene, cutting abrasive material and kerosene ratio are 1: 4;
(4) adjust wire cutting machine and be in level, line of cut is installed on the reel, then by regulating wheel and guide roller, the line of cut of adjusting on reel, regulating wheel and the guide roller is in the same plane, and the even tension on the line of cut is distributed;
(5) crystal to be cut that will fix is installed on the Cutting platform;
(6) determine cutting parameter: work takes turns to rotating speed and adopts 80% of its maximum (top) speed, and Wire Wheel speed is made as 35m/min, and cutting speed is that the angle of waving is 3600 °/min of frequency
(7) by the parameter sliced crystal of setting, the crystal of well cutting is placed in the protectiveness oil.
The Ce:LaCl3 plane of crystal that cutting obtains is smooth, does not have corrosion phenomenon.
Embodiment 3:2 in2 %Ce doping LaBr
3The cutting of crystal
Adopt homemade multi-line cutting machine, at 2at%Ce doping LaBr
3Plane of crystal is surrounded by the polyimides protective layer, utilizes the stainless steel cut line of gold-plated hard rock and the high speed of cutting mud to move back and forth, and realizes LaBr
3The water proof oxygen barrier cutting of crystal.Concrete steps are as follows:
(1) be surrounded by the polyimides protective layer at plane of crystal, thickness is about 0.2mm;
(2) remove part polyimides protective layer, utilize anaerobic adhesive that crystal is fixed on the standard component;
(3) CeO is evenly mixed as cutting mud with protectiveness cutting oil (kerosene and silicone oil equal-volume mix), cutting abrasive material and protectiveness cutting oil ratio are 1: 4;
(4) adjust wire cutting machine and be in level, line of cut is installed on the reel, then by regulating wheel and guide roller, the line of cut of adjusting on reel, regulating wheel and the guide roller is in the same plane, and the even tension on the line of cut is distributed;
(5) crystal to be cut that will fix is installed on the Cutting platform;
(6) determine cutting parameter: work takes turns to rotating speed and adopts 80% of its maximum (top) speed, and Wire Wheel speed is made as 35m/min, and cutting speed is that the angle of waving is 3600 °/min of frequency
(7) by the parameter sliced crystal of setting, the crystal of well cutting is placed in the protectiveness oil.
The Ce:LaBr3 plane of crystal that cutting obtains is smooth, does not have corrosion phenomenon.
Embodiment 4:0.5 in2 %Ce doping LuI
3The cutting of crystal
Adopt homemade multi-line cutting machine, at 2at%Ce doping LaBr
3Plane of crystal is surrounded by the polyimides protective layer, utilizes the stainless steel cut line of gold-plated hard rock and the high speed of cutting mud to move back and forth, and realizes LaBr
3The water proof oxygen barrier cutting of crystal.Concrete steps are as follows:
(1) be surrounded by the polyimides protective layer at plane of crystal, thickness is about 0.2mm;
(2) remove part polyimides protective layer, utilize anaerobic adhesive that crystal is fixed on the standard component;
(3) with CeO with and silicone oil evenly mix as cutting mud, cutting abrasive material and silicone oil ratio is 1: 4;
(4) adjust wire cutting machine and be in level, line of cut is installed on the reel, then by regulating wheel and guide roller, the line of cut of adjusting on reel, regulating wheel and the guide roller is in the same plane, and the even tension on the line of cut is distributed;
(5) crystal to be cut that will fix is installed on the Cutting platform;
(6) determine cutting parameter: work takes turns to rotating speed and adopts 80% of its maximum (top) speed, and Wire Wheel speed is made as 35m/min, and cutting speed is that the angle of waving is 3600 °/min of frequency
(7) by the parameter sliced crystal of setting, the crystal of well cutting is placed in the protectiveness oil.
The Ce:LuI3 plane of crystal that cutting obtains is smooth, does not have corrosion phenomenon.
Claims (6)
1. the cutting method of a water oxygen responsive type rare earth halide crystal by evenly smear the laggard line cutting processing of fish tail and waterproof layer at plane of crystal, need constantly be packed into cutting mud in the line cutting processing.It is characterized in that: described fish tail and waterproof layer is hydrophobicity protection grease or polyimides; Described cutting mud is mixed by cutting abrasive material and protectiveness cutting oil.
2. the cutting method of a kind of water oxygen responsive type rare earth halide crystal according to claim 1 is characterized in that described water oxygen responsive type rare earth halide crystal refers in air the very easily rotten rare earth halide crystal of deliquescence, and its chemical formula is Ln
1-xCe
xX
3, Ln=La, Lu, Gd, Y here; X=Cl, Br, I, subscript x refer to the doping content of Ce.
3. the cutting method of a kind of water oxygen responsive type rare earth halide crystal according to claim 1 is characterized in that the hydrophobicity protection grease that described rare earth halide plane of crystal is smeared is a vaseline, and thickness is 0.1～2mm.
4. the cutting method of a kind of water oxygen responsive type rare earth halide crystal according to claim 1 is characterized in that the polyimides layer thickness that described rare earth halide plane of crystal is surrounded by is 0.1～1mm's.
5. the cutting method of a kind of water oxygen responsive type rare earth halide crystal according to claim 1 is characterized in that described cutting abrasive material can be SiC, Al2O3, CeO or its mixture, and the protectiveness cutting oil can be silicone oil, kerosene or its mixture.
6. the cutting method of a kind of water oxygen responsive type rare earth halide crystal according to claim 1 is characterized in that described rare earth halide will be fixed on the standard component by anaerobic adhesive.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0686684A1 (en) * | 1994-06-06 | 1995-12-13 | Bayer Ag | Slicing slurry |
| CN1180726A (en) * | 1996-10-17 | 1998-05-06 | 瓦克硅电子半导体材料股份公司 | Sawing suspension and method for cutting wafers from crystal |
| US6262422B1 (en) * | 1997-02-14 | 2001-07-17 | Hamamatsu Photonics K.K. | Radiation detection device and method of making the same |
| CN1932087A (en) * | 2005-09-14 | 2007-03-21 | 宁波大学 | Bridgman-stockbarge process for growing scintillation crystal LaCl3:Ce3+ |
| WO2008047446A1 (en) * | 2006-10-20 | 2008-04-24 | Mitsubishi Electric Corporation | Slurry for silicon ingot cutting and method of cutting silicon ingot therewith |
| CN101386192A (en) * | 2008-10-08 | 2009-03-18 | 中国科学院上海硅酸盐研究所 | Cutting method of super-hard crystal |
| CN101900824A (en) * | 2010-06-24 | 2010-12-01 | 江苏康众数字医疗设备有限公司 | Scintillator packaging film and packaging method |
-
2010
- 2010-12-23 CN CN2010106012659A patent/CN102139517A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0686684A1 (en) * | 1994-06-06 | 1995-12-13 | Bayer Ag | Slicing slurry |
| CN1180726A (en) * | 1996-10-17 | 1998-05-06 | 瓦克硅电子半导体材料股份公司 | Sawing suspension and method for cutting wafers from crystal |
| US6262422B1 (en) * | 1997-02-14 | 2001-07-17 | Hamamatsu Photonics K.K. | Radiation detection device and method of making the same |
| CN1932087A (en) * | 2005-09-14 | 2007-03-21 | 宁波大学 | Bridgman-stockbarge process for growing scintillation crystal LaCl3:Ce3+ |
| WO2008047446A1 (en) * | 2006-10-20 | 2008-04-24 | Mitsubishi Electric Corporation | Slurry for silicon ingot cutting and method of cutting silicon ingot therewith |
| CN101386192A (en) * | 2008-10-08 | 2009-03-18 | 中国科学院上海硅酸盐研究所 | Cutting method of super-hard crystal |
| CN101900824A (en) * | 2010-06-24 | 2010-12-01 | 江苏康众数字医疗设备有限公司 | Scintillator packaging film and packaging method |
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Application publication date: 20110803 |