CN103643302A - Thermal sapphire compounding method - Google Patents
Thermal sapphire compounding method Download PDFInfo
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- CN103643302A CN103643302A CN201310614083.9A CN201310614083A CN103643302A CN 103643302 A CN103643302 A CN 103643302A CN 201310614083 A CN201310614083 A CN 201310614083A CN 103643302 A CN103643302 A CN 103643302A
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Abstract
The invention relates to a thermal sapphire compounding method and aims to prevent cracks from being formed and expanded so as to improve the strength of sapphire. According to the method, two or more layers of sapphire sheets with different crystal surfaces or with the same crystal surface and different side surface crystal axis directions are thermally compounded, so that two or more vertical layers of cleavage surfaces are staggered in direction and mutually enhanced. A material is prevented from being cracked in the presence of external force along a certain crystallization direction of the cleavage surfaces. According to the compounding method, the compounded surfaces of two or more layers of sapphire sheets needing to be compounded are polished to obtain certain finish and flatness, are overlapped and are loaded in a high-temperature furnace in a certain loading manner, and the polished surfaces of a sapphire material are bonded and integrated through protective gas at high temperature lower than a crystalline melting point to form a sapphire sheet. The required size and the required finish are obtained through machining. Therefore, the phenomena of edge breakage and cracking of a sapphire sheet material caused by the external force in the machining and using processes can be reduced.
Description
Technical field
The present invention relates to the hot complex method of a kind of sapphire.
Background technology
Because sapphire has the hardness that is close to diamond, Mohs' hardness 9.Good visible ray and infrared light, uv transmittance T>85% (400-800 nano wave length).And there is good bending strength and Young's modulus, so be used in high-end Mobile phone screen primary mirror sheet, wrist-watch eyeglass, laser window sheet, camera head protecting eyeglass, laser bar code projection scanner form sheet, touch screen protective cover plate.But while using at present, be all that individual layer sapphire sheet material is being used, the two-layer or two-layer above compound working method relating to here, has improved the yield rate of processing and anti-isostatic pressing strength, the resistance to impact shock of sheet material.
Sapphire has anisotropy, and sapphire crystal structure has a plurality of different crystal faces.Although sapphire each crystal face is higher compared with other hardness of minerals, some crystal faces have some other different feature.For example, C surface sapphire has good optical transmittance and fracture toughness property, and A surface sapphire has higher ultimate compression strength and wear resistance than the sapphire of other crystal faces.The sapphire of R face and M face also has other some advantages.
American documentation literature US20130236699 discloses a kind of sapphire rhythmo structure, comprise: the first layer sapphire sheet with the first high preferred orientation forms the major surfaces of sapphire rhythmo structure, the second layer sapphire sheet with the second high preferred orientation forms second principal plane of sapphire rhythmo structure, two-layer sapphire sheet fuses together, and forms sapphire rhythmo structure.Applicant thinks that such scheme is impossible really to realize, sapphire belongs to crystalline structure, if described in the 24th section, its specification sheets, " temperature of fusion sapphire sheet; can approach or surpass sapphire melt temperature ", the characteristic of crystal is to have certain fusing point, once be greater than melting temperature material, will melt.Cannot keep original shape, can there is the avalanche of lattice, cannot keep sapphire solid lamellar morphology, once upper and lower two sapphire sheet fuse, while lowering the temperature after material melts, polycrystalline is become in sporadic nucleation, the monocrystalline that its crystal orientation cannot be consistent, the sapphire rhythmo structure therefore obtaining by the method cannot keep the shape of former sheet material can not be for touch-screen.
Summary of the invention
The invention provides the hot complex method of a kind of sapphire, the technical problem that solved monolithic sapphire limit, cracks, even breaks.
Individual layer sapphire crystal sheet material in the course of processing because crystal itself exists knot reason face, so in the course of processing and use procedure when being subject to certain large External Force Acting crystalline material meeting itself along tying the certain crystallization direction of reason face, collapse limit, crack, even break.This is the natural characteristics of crystalline material.For reducing generation, the expansion of crackle when being subject to External Force Acting in the course of processing and use procedure, the present invention proposes the compound scheme of multi-layer sheet, utilize compound between the different plates of crystal orientation, increase the intensity of product, be more suitable for the use at large size Mobile phone screen and touch panel computer and military laser window; Solved the application limitation existing because of strength problem, can allow jewel sheet material does thinner lighter and there is good performance.
Concrete technical scheme of the present invention is:
The hot complex method of sapphire, comprises the following steps:
Step 1, the composite surface polishing of two-layer or two-layer above sapphire sheet material that will be compound, its surface roughness Ra reaches below 1 nanometer, planeness TTV<5 micron, LTV<1.5 micron, angularity <10 micron;
Step 2, the sapphire sheet material after above-mentioned polishing is orientated to difference according to the crystallographic axis of high preferred orientation difference or side, and to carry out crystal orientation heat compound; The hot compound condition of described sapphire sheet material: it is compound that sapphire sheet material is placed in High Temperature Furnaces Heating Apparatus, combined temp higher than 1500 ℃ lower than 2050 ℃ of sapphire fusing points; Be filled with helium, argon gas or nitrogen as protection gas; Soaking time is 1-15 hour.
Applicant finds, between sapphire sheet material, under the environment lower than its hot melting temperature, because the thermal motion between molecule aggravates, under the specified conditions of specific such scheme, can form the bonding between sapphire sheet material molecule.And sapphire sheet material surfaceness, planeness, LTV and angularity and hot compound good article rate are closely bound up, its principle may be that above-mentioned factor can affect two physical distances between sheet material, and then affects the molecular linkage process between sapphire sheet material.
Vertical near being positioned in the molybdenum crucible of High Temperature Furnaces Heating Apparatus between described sapphire sheet material polished surface.Vertically near the advantage of placing, be that (please supplement) sheet material is not easy to deform, can be at high temperature compound fast.
Described sapphire sheet material level overlays in the jewel back up pad that a planeness is consistent with sapphire sheet material, but back up pad is not carried out polishing, then using back up pad as carrier, puts into the molybdenum crucible of High Temperature Furnaces Heating Apparatus.The advantage of this horizontal positioned is that (please supplement) is because the compound jewel of upper and lower two needs produces positive pressure under action of gravity, and surface is easily sturdy and produce at a lower temperature compound.
Described sapphire sheet material is comprised of the first sapphire sheet and the second sapphire sheet, wherein the first sapphire sheet high preferred orientation be a to, the second sapphire sheet high preferred orientation be c to.
Described sapphire sheet material is comprised of sapphire table sheet and sapphire egative film, and sapphire egative film is comprised of a centre slice and four gusset plates, and centre slice is consistent with sapphire table sheet with gusset plate amalgamation area.
This programme has overcome the defect of monolithic sapphire sheet material, simultaneously the scheme compound with 2 complete sapphire sheet materials compared, there is better intensity and toughness, because the combination of the crystal orientation of sapphire table sheet and centre slice, gusset plate is more various, can make full use of the characteristic in each crystal orientation of sapphire.And reduced cost.In the practical application of touch-screen, while falling, most situation is that corner line lands, therefore the special reinforcement at position, corner has realistic meaning, and large multipurpose circular chamfering alleviates stress concentration in prior art, but this scheme does not fundamentally solve the frangible problem in corner, and the scheme of centre slice and gusset plate has thoroughly solved the problems referred to above.
There is straight line chamfering in two corners of described gusset plate.The effect of right angle chamfering is from a contact, to change the way of contact between gusset plate into line contact, has improved the anti-shearing force of composite structure.
Described centre slice is prismatic sheet, and described gusset plate is the triangular plate that corner is provided with straight line chamfering.
The top layer crystal face of described centre slice be a to, c to or r to, the top layer crystal face of described sapphire table sheet is not identical with centre slice top layer crystal face, the crystal orientation, edge of described gusset plate is not identical with the edge crystal face of sapphire table sheet.
The crystal orientation, edge of described gusset plate be m to.
Heat up and cooling rate be less than 200 degree/hour, in order to avoid thermal shocking brings fragmentation.In order to make in stove that impurity volatilizees, polluted product controling of the pressure of the oven is not at negative normal atmosphere, and shielding gas can be helium, argon gas or nitrogen, and in protection stove, thermal field is not oxidated.For the good bonding of material must be reached more than 1500 degrees Celsius, but will be lower than 2050 degrees Celsius of the fusing points of jewel, if fusing is scrapped higher than fusing point crystalline material.Soaking time is wanted 1 ~ 15 hour, and jewel polished surface just can stick together by bonding.
1, composite surface technical parameter is controlled:
The composite surface polishing of two-layer or two-layer above sapphire sheet material that first will be compound, surface roughness Ra reaches below 1 nanometer, planeness TTV<5 micron, LTV<1.5 micron, angularity <10 micron.Such polished surface is laminating well, is unlikely to have wedge angle and occur that the outward appearance that interference ring affects product causes defect afterwards compound.
2, the crystal orientation control of hot compound slice, thin piece
For reaching, prevent that crackle from producing and the effect of expansion, the crystal face difference of adjacent two layers of the two-layer or two-layer above jewel sheet material adopting here or the crystallographic axis of side orientation different crystal orientations are compound, as the crystal face of the 1st be a to the 2nd be c to; And for example the 1st crystal face be a to but horizontal orientation is and m axle clamp angle 45 degree, the crystal face of the 2nd be a to but horizontal orientation is r direction of principal axis.As more than two-layer, only need adjacent two layers difference to be effective.
3, for reaching a high temperature the compound High Temperature Furnaces Heating Apparatus tote science and engineering method for position of taking
The first scheme is that the polished surface that will meet is superimposed, does not need compound slice, thin piece not want polishing, with free bonding, cannot take away.Vertically be placed on can be compound in molybdenum crucible slice, thin piece all by real, be convenient to polished surface and contact completely, favourable high temperature bonding.
First scheme is to overlay in the thick jewel back up pad that a planeness is the same with slice, thin piece by compound slice, thin piece, but back up pad is wanted polishing, does not cling with product.Using back up pad as carrier, put into the molybdenum crucible of High Temperature Furnaces Heating Apparatus, interlayer pressure is more conducive to slice, thin piece bonding and is integrated so again.
4, for making the compound High Temperature Furnaces Heating Apparatus technical parameter that needs control of sheet material
When the jewel sheet material that will meet is put into High Temperature Furnaces Heating Apparatus, heat up and cooling rate be less than 200 degree/hour, in order to avoid thermal shocking brings fragmentation.In order to make in stove that impurity volatilizees, polluted product controling of the pressure of the oven is not at negative normal atmosphere, and shielding gas can be helium, argon gas or nitrogen, and in protection stove, thermal field is not oxidated.For the good bonding of material must be reached more than 1500 degrees Celsius, but will be lower than 2050 degrees Celsius of the fusing points of jewel, if fusing is scrapped higher than fusing point crystalline material.Soaking time is wanted 115 hours, and jewel polished surface just can stick together by bonding.
5, two-layer or two-layer above jewel sheet material Yin Gaowen bonding being bonded as one carries out the technical requirements that physical dimension processing and polishing reach workpiece.
Accompanying drawing explanation
The 1st sapphire crystal face of Fig. 1 be a to, the 2nd be that c becomes the structural representation of after compound.
Fig. 2 be the 1st sapphire crystal face be a to but horizontal orientation and m axle clamp angle 45 degree, the crystal face of the 2nd be a to but horizontal orientation is the structural representation of after to be r direction of principal axis compound.
Fig. 3 be the 1st sapphire crystal face be c to but horizontal orientation be with m axle clamp angle 90 degree, the crystal face of the 2nd be c to but the horizontal orientation axial 2 inches of sapphire circular piece that are m become the structural representation of after compound.
Fig. 4 is the structural representation of sapphire table sheet and egative film.
Fig. 5 is the structural representation (rib sheet) of sapphire table sheet and egative film.
Fig. 6 is the structural representation (chamfering) of sapphire table sheet and egative film.
Embodiment
Embodiment 1
By a slice crystal face, be that a face and a slice crystal face are 5 inches of rectangle sapphire sheet materials of r face, thickness is the sapphire single-sided polishing of 0.4mm, surface of polished roughness Ra <0.2 nanometer, TTV<3 micron, LTV<0.5 micron.Polished surface is superimposed, vertically puts into molybdenum crucible, between slice, thin piece, is close to, and does not stay gap.Put into helium protection stove, furnace pressure is 25 holders, with 150 degree/hour temperature rise rate be heated to 1900 degrees Celsius, under 1900 degrees Celsius, be incubated 10 hours, then with 150 degree/hour rate of temperature fall be down to normal temperature.Take out the coherent compound sapphire crystal sheet material of Yin Gaowen bonding, then grind profiling, punching, polishing, be processed into 0.75 thick sapphire main mobile phone lens (screen cover plate).There is damage resistant, high permeability, high-intensity mobile-phone lens.
Embodiment 2
By the 1st crystal face be a to but horizontal orientation is and m axle clamp angle 45 degree, the crystal face of the 2nd be a to but horizontal orientation is r direction of principal axis, 4.5 rectangle inch sapphire sheet materials, thickness is the sapphire single-sided polishing of 0.35mm, surface of polished roughness Ra <0.1 nanometer, TTV<2 micron, LTV<0.3 micron.Polished surface is superimposed, vertically puts into molybdenum crucible, between slice, thin piece, is close to, and does not stay gap.Put into helium protection stove, furnace pressure is 25 holders, with 150 degree/hour temperature rise rate be heated to 1800 degrees Celsius, under 1800 degrees Celsius, be incubated 15 hours, then with 150 degree/hour rate of temperature fall be down to normal temperature.Take out the coherent compound sapphire crystal sheet material of Yin Gaowen bonding, then grind profiling, punching, polishing, be processed into 0.65 thick sapphire main mobile phone lens (screen cover plate).There is damage resistant, high permeability, high-intensity mobile-phone lens.
Embodiment 3
By the 1st crystal face be a to but horizontal orientation is and m axle clamp angle 45 degree, the crystal face of the 2nd be a to but horizontal orientation is r direction of principal axis, 7 inches of rectangle sapphire sheet materials, thickness is the sapphire single-sided polishing of 0.4mm, surface of polished roughness Ra <0.1 nanometer, TTV<2 micron, LTV<0.3 micron.Polished surface is superimposed, on the sapphire plane carrier that level is placed on identical planeness through grinding but without polishing, can stack some layers, then carrier is put into molybdenum crucible.Put into helium protection stove, furnace pressure is 25 holders, with 150 degree/hour temperature rise rate be heated to 1700 degrees Celsius, under 1700 degrees Celsius, be incubated 15 hours, then with 150 degree/hour rate of temperature fall be down to normal temperature.Take out the coherent compound sapphire crystal sheet material of Yin Gaowen bonding, then grind profiling, punching, polishing, be processed into 0.75 thick sapphire mobile phone plane plate computer screen cover plate.Become there is damage resistant, high permeability, high-intensity computer main screen eyeglass.
Embodiment 4
By the 1st crystal face be a to but horizontal orientation is and m axle clamp angle 45 degree, the crystal face of the 2nd be a to but horizontal orientation is r direction of principal axis, 7 inches of rectangle sapphire sheet materials, thickness is the sapphire single-sided polishing of 0.4mm, surface of polished roughness Ra <0.1 nanometer, TTV<2 micron, LTV<0.3 micron.Polished surface is superimposed, on the sapphire plane carrier that level is placed on identical planeness through grinding but without polishing, can stack some layers, then carrier is put into molybdenum crucible.Put into helium protection stove, furnace pressure is 25 holders, with 150 degree/hour temperature rise rate be heated to 1700 degrees Celsius, under 1700 degrees Celsius, be incubated 15 hours, then with 150 degree/hour rate of temperature fall be down to normal temperature.Take out the coherent compound sapphire crystal sheet material of Yin Gaowen bonding, then grind profiling, punching, polishing, be processed into 0.75 thick sapphire mobile phone plane plate computer screen cover plate.Become there is damage resistant, high permeability, high-intensity computer main screen eyeglass.
Embodiment 5
By the 1st crystal face be c to but horizontal orientation is and m axle clamp angle 90 degree, the crystal face of the 2nd be c to but horizontal orientation is m direction of principal axis, the circular sheet materials of 2 inches of sapphires, thickness is the sapphire single-sided polishing of 0.7mm, surface of polished roughness Ra <0.1 nanometer, TTV<2 micron, LTV<0.3 micron.Polished surface is superimposed, on the sapphire plane carrier that level is placed on identical planeness through grinding but without polishing, can stack some layers, then carrier is put into molybdenum crucible.Put into helium protection stove, furnace pressure is 25 holders, with 150 degree/hour temperature rise rate be heated to 2000 degrees Celsius, under 2000 degrees Celsius, be incubated 8 hours, then with 150 degree/hour rate of temperature fall be down to normal temperature.Take out the coherent compound sapphire crystal sheet material of Yin Gaowen bonding, then grind, polishing, be processed into 1.35 thick sapphire laser diaphragms.Become there is high permeability, the military diaphragm of high-intensity laser guidance.
Embodiment 6
As shown in Figure 4, sapphire composite structure forms by showing sheet 1, centre slice 21 and gusset plate 22.Centre slice 21 and gusset plate 22 combined area equate with table sheet 1.
Embodiment 7
As shown in Figure 5, as different from Example 6, centre slice 21 is prismatic sheet, and gusset plate 22 is triangular plate.
Embodiment 8
As shown in Figure 6, as different from Example 7, gusset plate 22 has straight line chamfering 221.
Claims (9)
1. the hot complex method of sapphire, comprises the following steps:
Step 1, the composite surface polishing of two-layer or two-layer above sapphire sheet material that will be compound, its surface roughness Ra reaches below 1 nanometer, planeness TTV<5 micron, LTV<1.5 micron, angularity <10 micron;
Step 2, the sapphire sheet material after above-mentioned polishing is orientated to difference according to the crystallographic axis of high preferred orientation difference or side, and to carry out crystal face heat compound; The hot compound condition of described sapphire sheet material: it is compound that sapphire sheet material is placed in High Temperature Furnaces Heating Apparatus, combined temp higher than 1500 ℃ lower than 2050 ℃ of sapphire melting temperatures; Be filled with helium, argon gas or nitrogen as protection gas; Soaking time is 1-15 hour.
2. the hot complex method of sapphire according to claim 1, is characterized in that between described sapphire sheet material polished surface vertically near being positioned in the molybdenum crucible of High Temperature Furnaces Heating Apparatus.
3. the hot complex method of sapphire according to claim 1, it is characterized in that described sapphire sheet material level overlays in the jewel back up pad that a planeness is consistent with sapphire sheet material, but back up pad is not carried out polishing, then using back up pad as carrier, put into the molybdenum crucible of High Temperature Furnaces Heating Apparatus.
4. the hot complex method of sapphire according to claim 1, is characterized in that described sapphire sheet material is comprised of the first sapphire sheet and the second sapphire sheet, wherein the first sapphire sheet high preferred orientation be a to, the second sapphire sheet high preferred orientation be c to.
5. the hot complex method of sapphire according to claim 1, it is characterized in that described sapphire sheet material is comprised of sapphire table sheet and sapphire egative film, sapphire egative film is comprised of a centre slice and four gusset plates, and centre slice is consistent with sapphire table sheet with gusset plate amalgamation area.
6. the hot complex method of sapphire according to claim 5, is characterized in that two corners of described gusset plate exist straight line chamfering.
7. the hot complex method of sapphire according to claim 5, is characterized in that described centre slice is prismatic sheet, and described gusset plate is the triangular plate that corner is provided with straight line chamfering.
8. the hot complex method of sapphire according to claim 5, the top layer crystal face that it is characterized in that described centre slice be a to, c to or r to, the top layer crystal face of described sapphire table sheet is not identical with centre slice top layer crystal face, and the crystal orientation, edge of described gusset plate is not identical with the edge crystal face of sapphire table sheet.
9. the hot complex method of sapphire according to claim 5, the crystal orientation, edge that it is characterized in that described gusset plate be m to.
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Cited By (5)
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| CN103993359A (en) * | 2014-04-30 | 2014-08-20 | 洛阳金诺机械工程有限公司 | Welding method of sapphire wafer |
| WO2015077925A1 (en) * | 2013-11-26 | 2015-06-04 | 浙江上城科技有限公司 | Thermal compounding method for sapphire |
| CN105279503A (en) * | 2015-11-20 | 2016-01-27 | 浙江水晶光电科技股份有限公司 | Fingerprint identification cover plate and preparation method thereof, and fingerprint identification module |
| CN109111130A (en) * | 2017-06-22 | 2019-01-01 | 肖特股份有限公司 | The component being made of component, especially electronic component and glass or glass ceramic material |
| CN112338344A (en) * | 2020-10-29 | 2021-02-09 | 河海大学常州校区 | High-temperature self-expansion pressure diffusion welding method for sapphire |
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| CN109111130A (en) * | 2017-06-22 | 2019-01-01 | 肖特股份有限公司 | The component being made of component, especially electronic component and glass or glass ceramic material |
| CN109111130B (en) * | 2017-06-22 | 2022-05-31 | 肖特股份有限公司 | Assembly of components, in particular electronic components, and glass or glass-ceramic material |
| CN112338344A (en) * | 2020-10-29 | 2021-02-09 | 河海大学常州校区 | High-temperature self-expansion pressure diffusion welding method for sapphire |
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Effective date of registration: 20170420 Address after: Jiaxing City, Zhejiang province 314400 city of Haining Haining Economic Development Zone Danmeilu No. 8-1 Patentee after: ZHEJIANG HUIFENG FILM TECHNOLOGY CO., LTD. Address before: 314400 Haining City, Zhejiang Province Economic Development Zone in the city of gold on the road No. 11, No. Patentee before: Zhejiang Shangcheng Science & Technology Co., Ltd. |
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Effective date of registration: 20210728 Address after: 314400 Jinchang Road, Haining Economic Development Zone, Haining, Jiaxing, Zhejiang, 11 Patentee after: Zhejiang Huifeng Zhicheng Technology Co.,Ltd. Address before: 314400 No. 8-1, Danmei Road, Haining Economic Development Zone, Haining City, Jiaxing City, Zhejiang Province Patentee before: ZHEJIANG HUIFENG FILM TECHNOLOGY Co.,Ltd. |
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