CN103643302B - Thermal sapphire compounding method - Google Patents
Thermal sapphire compounding method Download PDFInfo
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- CN103643302B CN103643302B CN201310614083.9A CN201310614083A CN103643302B CN 103643302 B CN103643302 B CN 103643302B CN 201310614083 A CN201310614083 A CN 201310614083A CN 103643302 B CN103643302 B CN 103643302B
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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 a kind of Thermal sapphire complex method.
Background technology
Because sapphire has the hardness being close to diamond, Mohs' hardness 9.Excellent visible ray and infrared light, ultraviolet
Light transmission rate t > 85% (400-800 nano wave length).And there is excellent bending strength and elastic modelling quantity, so it is used in high-end
Mobile phone screen primary mirror piece, wrist-watch eyeglass, laser window piece, camera head protecting eyeglass, laser bar code projection scanner form piece, touch screen protection
Protecting cover plate.But it is all that monolayer sapphire sheet material is using during current use, more than the two-layer referring here to or two-layer compound adding
Work method, improves the yield rate of processing and the anti-isostatic pressing strength of sheet material, impact strength.
Sapphire has anisotropy, and its sapphire crystal structure has multiple different crystal faces.Although, sapphire
Each crystal face is higher compared with other hardness of minerals, but some crystal faces have the characteristics that some other is different.For example, c surface sapphire has
Well optical transmittance and fracture toughness, a surface sapphire has higher comprcssive strength and resistance to than the sapphire of other crystal faces
Mill property.The sapphire in r face and m face also has some other advantages.
American documentation literature us20130236699 discloses a kind of sapphire laminated construction, comprising: have the first crystal face
The ground floor sapphire sheet of orientation forms the first type surface of sapphire laminated construction, and the second layer with second high preferred orientation is blue precious
Flag forms second principal plane of sapphire laminated construction, and two-layer sapphire sheet fuses together, and forms sapphire lamination knot
Structure.Applicant thinks that such scheme can not possibly really be realized, and sapphire belongs to crystal structure, if according to its description
Described in 24 sections, " temperature of fusion sapphire sheet, can be near or above sapphire melt temperature ", the characteristic of crystal is that have one
Determine fusing point, once will melt more than melting-temperature material.Original shape cannot be kept, then the avalanche of lattice can occur it is impossible to
Keep sapphire solid sheet form, upper and lower two panels sapphire sheet once fuses, spontaneous one-tenth when lowering the temperature after melt material
Core becomes polycrystalline, the monocrystalline that its crystal orientation cannot be consistent, and the sapphire laminated construction therefore being obtained by the method cannot be protected
The shape holding former sheet material cannot be used for touch screen.
Content of the invention
The invention provides a kind of Thermal sapphire complex method, solve monolithic sapphire side, crack, even rupture
Technical problem.
There is knot reason face due to crystal itself in process in monolayer sapphire crystal sheet material, thus in the course of processing and
During use, when being subject to necessarily big external force effect, crystalline material itself can be along knot reason face certain crystallization direction chipping, product
Give birth to crackle, even rupture.This is the inherent character of crystalline material.For reduce the course of processing and use during when by outer masterpiece
The generation of used time crackle, expansion, the present invention proposes the compound scheme of multi-layer sheet, using answering between crystal orientation different plates
Close, increased the intensity of product, the use being more suitable in large scale Mobile phone screen and touching panel computer and military laser window；Solution
Determine the application limitation existing because of strength problem, can allow gem sheet material does thinner lighter and there is excellent performance.
The concrete technical scheme of the present invention is:
A kind of Thermal sapphire complex method, comprises the following steps:
Step one, the compound mirror polish of sapphire the sheet material more than two-layer that will be combined or two-layer, its surface roughness
Ra reaches less than 1 nanometer, flatness ttv < 5 microns, ltv < 1.5 micron, < 10 microns of angularity；
Step 2, by the sapphire sheet material after above-mentioned polishing according to high preferred orientation is different or the crystallographic axis of side is orientated difference and enters
Row crystal orientation heat is compound；The hot compound condition of described sapphire sheet material: sapphire sheet material is placed in high temperature furnace compound, combined temp
It is less than 2050 DEG C of sapphire fusing point higher than 1500 DEG C；It is filled with helium, argon or nitrogen as shielding gas；Temperature retention time is that 1-15 is little
When.
It has been found that between sapphire sheet material in the environment of less than its hot melting temperature, due to the heat fortune between molecule
Dynamic aggravation, can form the bonding between sapphire sheet material molecule under the specified conditions of specific such scheme.And sapphire sheet material
Surface roughness, flatness, ltv and angularity are closely bound up with the compound yields of heat, and its principle may is that above-mentioned factor meeting
Physical distance between two sheet materials of impact, and then affect the molecular linkage process between sapphire sheet material.
Vertically it is placed against in the molybdenum crucible of high temperature furnace between described sapphire sheet material burnishing surface.Vertically be placed against is excellent
Point is that (please supplement) sheet material is less likely to occur to deform, and can quickly be combined at high temperature.
Described sapphire sheet material level overlays on the flatness gemstone support plate consistent with sapphire sheet material, but supports
Plate is not polished, then in the molybdenum crucible that gripper shoe is put into high temperature furnace as carrier.The advantage of this horizontal positioned is (please
Supplement) need compound gem to produce normal pressure under gravity due to upper and lower two panels, surface easily sturdy and compared with low temperature
The lower generation of degree is combined.
Described sapphire sheet material is made up of the first sapphire sheet and the second sapphire sheet, and the wherein first sapphire sheet crystal face takes
To be a to, the second sapphire sheet high preferred orientation be c to.
Described sapphire sheet material is made up of sapphire table piece and sapphire egative film, and sapphire egative film is by one piece of centre slice and four
Individual gusset plate composition, centre slice is consistent with sapphire table piece with gusset plate split area.
This programme overcomes the defect of monolithic sapphire sheet material, the scheme phase being simultaneously combined with 2 complete sapphire sheet materials
Ratio has more preferable intensity and toughness, because the crystal orientation of sapphire table piece and centre slice, gusset plate combines more various, Ke Yichong
Divide the characteristic using each crystal orientation of sapphire.And reduce cost.In the practical application of touch screen, most of when falling
Situation land for corner line, the special reinforcement of therefore corner part has realistic meaning, and big multipurpose circular in prior art
Chamfering is mitigating stress concentration, but this scheme does not fundamentally solve the problems, such as that corner is frangible, and centre slice and gusset plate
Scheme thoroughly solves the problems referred to above.
There is straight line chamfering in two corners of described gusset plate.The effect of right angle chamfering is the way of contact between gusset plate
It is changed to linear contact lay from a contact, improve the anti-shearing force of composite construction.
Described centre slice is prismatic piece, and described gusset plate is provided with the triangular plate of straight line chamfering for corner.
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 piece and centre slice table
Layer crystal face differs, and the edge crystal orientation of described gusset plate is differed with the edge crystal face of sapphire table piece.
The edge crystal orientation of described gusset plate be m to.
Rise gentle cooling rate be less than 200 degree/hour, in order to avoid thermal shock bring broken.For making impurity in stove volatilize not
Polluted product controling of the pressure of the oven can be helium, argon or nitrogen in negative atmospheric pressure, protective gas, and in protection stove, thermal field is not subject to oxygen
Change.In order to make material, bonding must reach more than 1500 degrees Celsius well, but 2050 degrees Celsius of the fusing point of gem to be less than, if
Higher than melting crystals material, fusing is scrapped.Temperature retention time wants 1 ~ 15 hour, and gem burnishing surface just can be bonded and stick together.
1st, composite surface technical parameter controls:
The compound mirror polish of sapphire the sheet material more than two-layer first will being combined or two-layer, surface roughness ra reaches 1
Nanometer is following, flatness ttv < 5 microns, ltv < 1.5 micron, < 10 microns of angularity.Such burnishing surface could paste well
Close, the outward appearance being unlikely to there is the light angle of wedge and interference ring impact product after compound causes defect.
2nd, the crystal orientation control of the compound slice, thin piece of heat
For reaching the effect preventing crackle from producing and expanding, the phase of gem the sheet material more than two-layer adopting here or two-layer
The crystal face of adjacent two-layer is different or crystallographic axis orientation different crystal orientations of side are combined, the crystal face of such as the 1st be a to the 2nd be c to；Again
As the 1st crystal face be a to but horizontal orientation be and 45 degree of m axle clamp angle, the crystal face of the 2nd be a to but horizontal orientation is r axle side
To.As more than two-layer only needed adjacent two layers difference to can reach effect.
3rd, it is the compound high temperature furnace tote science and engineering method for position taken that reaches a high temperature
The first scheme is the burnishing surface overlapping that will meet it is not necessary to compound slice, thin piece must not polish, with free bonding no
Method is taken away.Vertically it is placed on the slice, thin piece being combined in molybdenum crucible all by real, be easy to burnishing surface and completely attach to, favourable high temperature
Bonding.
Second scheme is that the slice, thin piece that will be combined overlays on the gemstone support plate of the flatness thickness the same with slice, thin piece,
But gripper shoe must not polish in order to avoid clinging with product.In the molybdenum crucible again gripper shoe being put into high temperature furnace as carrier, such layer
Between pressure be more conducive to slice, thin piece bonding be integrated.
4th, it is to make sheet material be combined the high temperature furnace technical parameter needing to control
When gem sheet material to be met is put in high temperature furnace, rise gentle cooling rate and be less than 200 degree/hour, in order to avoid
Thermal shock brings broken.In order to make impurity in stove volatilize, in negative atmospheric pressure, protective gas can be helium to not polluted product controling of the pressure of the oven
Gas, argon or nitrogen, in protection stove, thermal field is not aoxidized.In order to make material, bonding must reach more than 1500 degrees Celsius well,
But fusing is scrapped by 2050 degrees Celsius of the fusing point of gem to be less than if above melting crystals material.Temperature retention time wants 115 little
When, gem burnishing surface just can be bonded and stick together.
5th, gem the sheet material more than two-layer being bonded as one because of high temperature bonding or two-layer is carried out overall dimensions processing
Reach the technical requirements of workpiece with polishing.
Brief description
The 1st sapphire crystal face of Fig. 1 be a to, the 2nd be c to the structural representation becoming a piece after compound.
Fig. 2 be the 1st sapphire crystal face be a to but the crystal face at horizontal orientation and 45 degree of m axle clamp angle, the 2nd be a to but horizontal
It is the structural representation for a piece after r direction of principal axis is combined to orientation.
Fig. 3 be the 1st sapphire crystal face be c to but horizontal orientation be with the crystal face at 90 degree of m axle clamp angle, the 2nd be c to but
Horizontal orientation is to become one piece of structural representation after the axial 2 inches sapphire circular piece of m are combined.
Fig. 4 is the structural representation of sapphire table piece and egative film.
Fig. 5 is the structural representation (rib piece) of sapphire table piece and egative film.
Fig. 6 is the structural representation (chamfering) of sapphire table piece and egative film.
Specific embodiment
Embodiment 1
By a piece of crystal face be a face and a piece of crystal face is 5 inches of rectangle sapphire sheet materials in r face, and thickness is the indigo plant of 0.4mm
Gem single-sided polishing, surface of polished roughness ra < 0.2 nanometer, ttv < 3 micron, ltv < 0.5 micron.Burnishing surface overlaps, vertically
Put in molybdenum crucible, be close between slice, thin piece, leave no gaps.Put in helium protection stove, furnace pressure be 25 supports, with 150 degree/little
When heating rate be heated to 1900 degrees Celsius, be incubated 10 hours under 1900 degrees Celsius, then with the cooling of 150 degree/hour
Speed is down to room temperature.Take out because high temperature be bonded coherent composite sapphire crystal sheet material, then be ground profiling, punching,
Polishing, is processed into the Sapphire mobile phone primary mirror piece (screen cover plate) of 0.75 thickness.There are the handss of damage resistant, high permeability, high intensity
Machine eyeglass.
Embodiment 2
By the 1st crystal face be a to but horizontal orientation be and 45 degree of m axle clamp angle, the crystal face of the 2nd be a to but horizontal orientation
R direction of principal axis, 4.5 rectangle inches sapphire sheet materials, thickness is the sapphire single-sided polishing of 0.35mm, and surface of polished is thick
Rugosity ra < 0.1 nanometer, ttv < 2 micron, ltv < 0.3 micron.Burnishing surface overlaps, and vertically puts in molybdenum crucible, leans between slice, thin piece
Tightly, leave no gaps.Put in helium protection stove, furnace pressure is 25 supports, is heated to 1800 with the heating rate of 150 degree/hour
Degree Celsius, it is incubated 15 hours under 1800 degrees Celsius, then room temperature is down to the rate of temperature fall with 150 degree/hour.Take out because of high temperature
It is bonded coherent composite sapphire crystal sheet material, then is ground profiling, punching, polishing, be processed into the blue precious of 0.65 thickness
Stone main mobile phone lens (screen cover plate).There are the mobile-phone lens of damage resistant, high permeability, high intensity.
Embodiment 3
By the 1st crystal face be a to but horizontal orientation be and 45 degree of m axle clamp angle, the crystal face of the 2nd be a to but horizontal orientation
R direction of principal axis, 7 inches of rectangle sapphire sheet materials, thickness is the sapphire single-sided polishing of 0.4mm, and surface of polished is coarse
Ra < 0.1 nanometer of degree, ttv < 2 micron, ltv < 0.3 micron.Burnishing surface overlaps, be placed horizontally in identical flatness through grinding but not
On polished sapphire plane carrier, if dried layer can be stacked, then carrier is put in molybdenum crucible.Put into helium protection stove
Interior, furnace pressure is 25 supports, is heated to 1700 degrees Celsius with the heating rate of 150 degree/hour, is incubated 15 under 1700 degrees Celsius
Hour, then room temperature is down to the rate of temperature fall with 150 degree/hour.Take out because of high temperature bonding coherent composite sapphire crystalline substance
Body sheet material, then it is ground profiling, punching, polishing, it is processed into the Sapphire mobile phone panel computer screen cover plate of 0.75 thickness.Become
There is the computer main screen eyeglass of damage resistant, high permeability, high intensity.
Embodiment 4
By the 1st crystal face be a to but horizontal orientation be and 45 degree of m axle clamp angle, the crystal face of the 2nd be a to but horizontal orientation
R direction of principal axis, 7 inches of rectangle sapphire sheet materials, thickness is the sapphire single-sided polishing of 0.4mm, and surface of polished is coarse
Ra < 0.1 nanometer of degree, ttv < 2 micron, ltv < 0.3 micron.Burnishing surface overlaps, be placed horizontally in identical flatness through grinding but not
On polished sapphire plane carrier, if dried layer can be stacked, then carrier is put in molybdenum crucible.Put into helium protection stove
Interior, furnace pressure is 25 supports, is heated to 1700 degrees Celsius with the heating rate of 150 degree/hour, is incubated 15 under 1700 degrees Celsius
Hour, then room temperature is down to the rate of temperature fall with 150 degree/hour.Take out because of high temperature bonding coherent composite sapphire crystalline substance
Body sheet material, then it is ground profiling, punching, polishing, it is processed into the Sapphire mobile phone panel computer screen cover plate of 0.75 thickness.Become
There is the computer main screen eyeglass of damage resistant, high permeability, high intensity.
Embodiment 5
By the 1st crystal face be c to but horizontal orientation be and 90 degree of m axle clamp angle, the crystal face of the 2nd be c to but horizontal orientation
M direction of principal axis, 2 inches sapphire circle sheet materials, thickness be 0.7mm sapphire single-sided polishing, surface of polished roughness
Ra < 0.1 nanometer, ttv < 2 micron, ltv < 0.3 micron.Burnishing surface overlaps, be placed horizontally in identical flatness through grinding but without
On the sapphire plane carrier of polishing, if dried layer can be stacked, then carrier is put in molybdenum crucible.Put in helium protection stove,
Furnace pressure is 25 supports, is heated to 2000 degrees Celsius with the heating rate of 150 degree/hour, and under 2000 degrees Celsius, insulation 8 is little
When, then room temperature is down to the rate of temperature fall with 150 degree/hour.Take out and be bonded coherent composite sapphire crystal because of high temperature
Sheet material, then be ground, polish, it is processed into the sapphire laser diaphragm of 1.35 thickness.Become and there is high permeability, high intensity
The military diaphragm of laser guidance.
Embodiment 6
As shown in figure 4, sapphire composite construction is made up of table piece 1, centre slice 21 and gusset plate 22.Centre slice 21 and gusset plate 22
Combined area is equal with table piece 1.
Embodiment 7
As shown in figure 5, as different from Example 6, centre slice 21 is prismatic piece, and gusset plate 22 is triangular plate.
Embodiment 8
As shown in fig. 6, as different from Example 7, gusset plate 22 has straight line chamfering 221.
Claims (4)
1. a kind of Thermal sapphire complex method, comprises the following steps:
Step one, the compound mirror polish of sapphire the sheet material more than two-layer that will be combined or two-layer, its surface roughness ra reaches
To less than 1 nanometer, flatness ttv < 5 microns, ltv < 1.5 micron, < 10 microns of angularity；
Step 2, by the sapphire sheet material after above-mentioned polishing according to high preferred orientation is different or the crystallographic axis of side is orientated difference and carries out crystalline substance
Fever sensation of the face is combined；The hot compound condition of described sapphire sheet material: sapphire sheet material is placed in high temperature furnace and is combined, and combined temp is higher than
1500 DEG C are less than 2050 DEG C of sapphire melting temperature；It is filled with helium, argon or nitrogen as shielding gas；Temperature retention time is 1-15
Hour;
Described sapphire sheet material is made up of sapphire table piece and sapphire egative film, and sapphire egative film is by one piece of centre slice and four angles
Piece forms, and centre slice is consistent with sapphire table piece with gusset plate split area;
There is straight line chamfering in two corners of described gusset plate;
Described centre slice is prismatic piece, and described gusset plate is provided with the triangular plate of straight line chamfering for corner;
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 piece and centre slice top layer
Crystal face differs, and the edge crystal orientation of described gusset plate is differed with the edge crystal face of sapphire table piece.
2. the Thermal sapphire complex method according to claim 1 is it is characterised in that erect between described sapphire sheet material burnishing surface
Directly it is placed against in the molybdenum crucible of high temperature furnace.
3. the Thermal sapphire complex method according to claim 1 is it is characterised in that described sapphire sheet material level overlays
On the one flatness gemstone support plate consistent with sapphire sheet material, but gripper shoe is not polished, then using gripper shoe as carrier
Put in the molybdenum crucible of high temperature furnace.
4. the Thermal sapphire complex method according to claim 1 is it is characterised in that the edge crystal orientation of described gusset plate is m
To.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015077925A1 (en) * | 2013-11-26 | 2015-06-04 | 浙江上城科技有限公司 | Thermal compounding method for sapphire |
| CN103993359B (en) * | 2014-04-30 | 2017-01-04 | 洛阳金诺机械工程有限公司 | A kind of welding process of sapphire wafer |
| CN105279503B (en) * | 2015-11-20 | 2018-12-04 | 浙江水晶光电科技股份有限公司 | A kind of preparation method of fingerprint recognition cover board |
| DE102018209589B4 (en) * | 2017-06-22 | 2023-05-04 | Schott Ag | Composite of a component, in particular an electronic component, and a glass or glass-ceramic material and method for its production |
| 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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| CN101318779A (en) * | 2008-07-23 | 2008-12-10 | 中国科学院上海光学精密机械研究所 | Sapphire and germanate glass infrared composite material and preparation method thereof |
| CN102912449A (en) * | 2012-10-14 | 2013-02-06 | 北京工业大学 | Bonding method for improving bonding force and optical properties of bonding crystal |
| CN102941713A (en) * | 2012-10-24 | 2013-02-27 | 浙江上城科技有限公司 | Sapphire composite material and preparation method thereof |
| CN103103621A (en) * | 2013-02-25 | 2013-05-15 | 无锡鼎晶光电科技有限公司 | Sapphire splicing method, sapphire window and paste size |
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| JP2849602B2 (en) * | 1989-09-29 | 1999-01-20 | 京セラ株式会社 | Joining method of single crystal sapphire |
| JP3264074B2 (en) * | 1994-01-24 | 2002-03-11 | 松下電器産業株式会社 | Laminated ferroelectric and bonding method thereof |
| US10052848B2 (en) * | 2012-03-06 | 2018-08-21 | Apple Inc. | Sapphire laminates |
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| CN101318779A (en) * | 2008-07-23 | 2008-12-10 | 中国科学院上海光学精密机械研究所 | Sapphire and germanate glass infrared composite material and preparation method thereof |
| CN102912449A (en) * | 2012-10-14 | 2013-02-06 | 北京工业大学 | Bonding method for improving bonding force and optical properties of bonding crystal |
| CN102941713A (en) * | 2012-10-24 | 2013-02-27 | 浙江上城科技有限公司 | Sapphire composite material and preparation method thereof |
| CN103103621A (en) * | 2013-02-25 | 2013-05-15 | 无锡鼎晶光电科技有限公司 | Sapphire splicing method, sapphire window and paste size |
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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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