WO2019233174A1 - 一种发光元件及发光元件的高能粒子辐射方法、抛光方法 - Google Patents
一种发光元件及发光元件的高能粒子辐射方法、抛光方法 Download PDFInfo
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- WO2019233174A1 WO2019233174A1 PCT/CN2019/081652 CN2019081652W WO2019233174A1 WO 2019233174 A1 WO2019233174 A1 WO 2019233174A1 CN 2019081652 W CN2019081652 W CN 2019081652W WO 2019233174 A1 WO2019233174 A1 WO 2019233174A1
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- light
- emitting element
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B29/00—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents
- B24B29/02—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents designed for particular workpieces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/48—Ion implantation
Definitions
- the invention belongs to the technical field of light-emitting materials, and particularly relates to a light-emitting element for a light-emitting device and a high-energy ion radiation method and a polishing method of the light-emitting element.
- a light-emitting element obtained by mixing and sintering a fluorescent powder with a glass powder or a ceramic powder, such as a light-emitting ceramic / light-emitting glass.
- the light-emitting ceramic / light-emitting glass forms a light-emitting device by adhering a reflective layer and a thermally conductive support device on a side facing away from the excitation light, and is used to convert the excitation light into a laser light with a predetermined wavelength.
- the phase formed by sintering the phosphor is different from the phase formed by sintering the glass powder or the ceramic powder, resulting in different grinding rates. Therefore, when the light-emitting element is polished, a concave-convex surface is formed. The unevenness of the concave-convex surface is on the micrometer level.
- the reflective layer causes the reflective layer to fall off easily.
- the object of the present invention is to provide a light-emitting element and a high-energy ion radiation method and a polishing method of the light-emitting element, so as to solve the problem of forming a micro-level undulated uneven surface during the prior art polishing, and covering the uneven surface
- the reflection layer causes a problem that the reflection layer is not firmly bonded and is easy to fall off.
- a light-emitting element is provided by sintering at least two kinds of raw materials including an A-phase raw material and a Y-phase raw material to form a multi-phase structure including at least two phases of the A-phase and the Y-phase.
- the Mohs hardness of the Y phase is greater than the Mohs hardness of the Y phase
- the DPA value of the A phase is greater than the DPA value of the Y phase
- the Mohs hardness of the A phase is reduced to approximately the same as the Y phase after being damaged by ion radiation.
- the light-emitting element is a sheet-shaped wavelength conversion layer obtained by sintering Y 3 Al 5 O 12 : Ce 3+ phosphor and Al 2 O 3 particles, the A phase is an Al 2 O 3 phase, and the The Y phase is a Y 3 Al 5 O 12 : Ce 3+ phase.
- the thickness of the wavelength conversion layer is 350 ⁇ m-450 ⁇ m.
- the present invention also provides a high-energy ion radiation method of a light-emitting element, wherein the light-emitting element uses the light-emitting element having a complex phase structure as described above, and the energy gradient of the light-emitting element is increased by using high-energy ions.
- the radiation causes the A-phase of the light-emitting element to have uniform damage within a predetermined depth range below the surface of the light-emitting element until the Mohs hardness of the A-phase is substantially the same as that of the Y-phase.
- the high-energy ion is a C ion or an N ion with an energy of 70 MeV-80 MeV.
- the difference between the Mohs hardness of the A phase and the Mohs hardness of the Y phase is not more than 0.5.
- the dose of the C ion radiation is 1 ⁇ 10 15 ions / cm 2
- the radiation rate is 1 ⁇ 10 13 ions / cm 2 ⁇ s
- the radiation energy is 70 MeV.
- the radiant energy of each radiation increases with a tolerance of 1 MeV.
- the present invention also provides a polishing method for a light emitting element, which includes the high-energy ion radiation method as described above, including the following steps:
- Step S1 providing a light-emitting element having a complex phase structure, and adhering the light-emitting element to a sample stage of an ion implanter, exposing the polished surface;
- Step S2 high-energy ion radiation is performed on the polished surface of the light-emitting element, and after each energy radiation is completed, the sample is not taken out, the radiation parameters are modified for the next radiation, and repeated multiple times until uniform damage occurs within a predetermined depth range;
- Step S3 polishing to a flat surface to obtain a flat surface.
- the step S1 is to realize the bonding of the light emitting elements by using a conductive tape or an adhesive, and the bonding area is smaller than the surface area of the light emitting elements.
- step S4 is further included: the light-emitting element is taken out, and the conductive tape or adhesive is removed with acetone.
- the predetermined depth range in step S2 is 100 ⁇ m-145 ⁇ m.
- the beneficial effects of the present invention are as follows: the light-emitting element of the present invention and its high-energy ion radiation method and polishing method utilize high-energy ions to irradiate a light-emitting element with a complex phase structure with increasing energy gradient, so that the light-emitting element
- the phase with a higher Mohs hardness in the medium causes uniform damage in a predetermined depth range below the surface of the light-emitting element, thereby reducing its Mohs hardness to approximately the same as that of the other phase in the light-emitting element.
- the light emitting element is polished to this depth to obtain a flat surface. It can avoid the uneven surface of micron level caused by the different hardness and grinding rate between different phases, so that the reflective layer and the like adhered on the surface are more firm and not easy to fall off.
- FIG. 1 is a schematic diagram of a surface structure of a light-emitting element of the present invention after being directly polished;
- FIG. 2 is a schematic diagram of the damage degree of the Y 3 Al 5 O 12 : Ce 3+ phase after the light emitting device is irradiated multiple times according to the present invention
- FIG. 3 is a schematic diagram of the damage degree of the Al 2 O 3 phase after the light emitting element is irradiated multiple times according to the present invention
- FIG. 4 is a schematic diagram of the degree of damage between different phases of the light-emitting element of the present invention.
- FIG. 5 is a schematic diagram showing the damage degrees of different phases after the light-emitting element of the present invention is polished in advance and then irradiated;
- FIG. 6 is a schematic flowchart of a method for polishing a light emitting element according to the present invention.
- the present invention provides a new method for polishing a light-emitting element for a light-emitting device.
- the light-emitting element of the present invention is a light-emitting ceramic or a light-emitting glass.
- a flat surface can be formed.
- a reflective layer or the like may be attached to this surface to further form a light emitting device.
- the polishing method of the present invention can effectively solve the problem of forming a micro-level undulating surface when polishing in the prior art, and covering the concave-convex surface with a reflective layer, which causes the problem that the reflective layer is not firmly bonded and easily falls off.
- the polishing method of the present invention is applied to a light-emitting element that is sintered by at least two materials including an A-phase raw material and a Y-phase raw material.
- the light-emitting element includes at least two phases of an A-phase and a Y-phase to form a multi-phase structure.
- the Y phase and the A phase have different Mohs hardnesses, and their wear resistance and damage resistance are different. Specifically, the A phase Mohs hardness is greater than the Y phase Mohs hardness.
- the DPA value of the A phase is greater than the DPA value of the Y phase. After being damaged by ion radiation, its Mohs hardness is changed. Specifically, its Mohs hardness is reduced.
- DPA dislacements per atom
- DPA refers to the average number of times each atom is displaced in the irradiated luminescent ceramic, indicating the degree of damage. The larger the DPA value, the more severe the damage.
- the Y-phase raw material is Y 3 Al 5 O 12 : Ce 3+ phosphor
- the A-phase raw material is Al 2 O 3 particles
- the formed A phase is Al 2 O 3 phase
- the Y phase is Y 3 Al 5 O 12 : Ce 3+ phase.
- the polishing method of the present invention is also applicable to other light-emitting elements with a multi-phase structure, and is not limited to the materials and structures described in this embodiment.
- the Y-phase raw material is LuAG: Ce 3+ phosphor and the A-phase raw material is glass. Powder
- the A phase formed is a glass phase
- the Y phase is a LuAG: Ce 3+ phase.
- This embodiment uses a sintered Y 3 Al 5 O 12 : Ce 3+ phosphor and Al 2 O 3 particles to form a sheet-shaped wavelength conversion layer, that is, a light-emitting element, in which Y 3 Al 5 O 12 : Ce 3+ phosphor
- Y 3 Al 5 O 12 Ce 3+ phosphor
- Commercial phosphors can be purchased directly, or a certain amount of Y 2 O 3 (purity 99.99%), Al 2 O 3 (purity 99.99%), and CeO 2 are mixed and sintered.
- the light-emitting element is cut into a disc shape with a thickness of 350 ⁇ m to 450 ⁇ m for use, and the thickness is preferably 400 ⁇ m. As shown in FIG.
- the surface roughness of the light-emitting element directly after polishing is about 20 ⁇ m, in which the convex portion is an Al 2 O 3 phase and the concave portion is a Y 3 Al 5 O 12 : Ce 3+ phase.
- the Mohs hardness of Al 2 O 3 is greater than the Mohs hardness of Y 3 Al 5 O 12 : Ce 3+ , which causes the wear rate of Al 2 O 3 to be lower than that of Y 3 Al 5 O 12 : Ce 3+ , so the polished surface It is uneven.
- the present invention provides a radiation method for increasing the energy gradient of a light-emitting element using high-energy ions and a polishing method using the method, so that the A phase of the light-emitting element is at a predetermined depth below the surface of the light-emitting element. Uniform damage occurs within the range until the Mohs hardness of the A phase and the Mohs hardness of the Y phase are approximately the same, and then the light emitting element after polishing is polished to this depth to obtain a flat surface.
- the high-energy ions are specifically C ions or N ions with an energy of 70 MeV-80 MeV.
- the Mohs hardness of the A phase and the Mohs hardness of the Y phase are substantially the same, and it should be understood that the difference between the Mohs hardness of the A and Y phases is not more than 0.5, and preferably not more than 0.3.
- the steps of the polishing method of the present invention are:
- Step S1 The light emitting element is adhered to the sample stage of the ion implanter through a conductive tape or an adhesive, and the polished surface is exposed.
- a double-sided carbon conductive tape or a silver adhesive can be applied on a side facing away from the polishing surface, wherein the bonding area formed by the double-sided carbon conductive tape or the silver adhesive is smaller than the surface area of the surface on which the light-emitting element is to be bonded. In this way, it can be ensured that the glue will not be exposed, thereby preventing ions from hitting the tape and causing sputtering pollution.
- Step S2 The high-energy ion irradiation is performed on the polished surface of the light-emitting element. After each energy irradiation is completed, the sample is not removed, and the radiation parameters are modified for the next irradiation, and repeated until a uniform damage occurs within a predetermined depth range.
- high-energy ions can use non-gaseous elements with low chemical activity in the periodic table, such as C (carbon), P (phosphorus), B (boron), N (nitrogen) and other elements. Due to the different atomic weight and electronic structure of different radiating elements, the damage depth distribution and the degree of damage generated in the substrate are different, so the energy, type, dose, etc. of the radiation particles can be set according to the actual situation.
- the polishing depth of complex phase luminescent ceramics must match the depth of radiation damage in the luminescent ceramics.
- C ions or N ions may be used.
- C ion radiation is used at a dose of 1 ⁇ 10 15 ions / cm 2 and a radiation rate of 1 ⁇ 10 13 ions / cm 2 ⁇ s.
- the radiation energy is 70 MeV
- the next dose of radiation and each injection rate remains constant and the tolerance for the radiant energy to 1MeV increment
- the X-axis represents the depth below the surface of the luminescent ceramic
- the Y-axis represents the use of C ions The degree of damage caused by radiation.
- the 11 single peak shapes from left to right in each of Figures 2 and 3 are single damage patterns.
- the reason why the present invention uses multiple energy combinations to radiate multiple times is that a single energy radiation can only generate Gaussian-distributed damage, as shown in the single damage pattern in Figure 2 and Figure 3.
- the multiple radiation methods with different energies used in the present invention can generate a uniform damage distribution in a predetermined depth interval. See the total damage shown in FIG. 2 and FIG. 3.
- FIG. 2 shows that the Y 3 Al 5 O 12 : Ce 3+ phase forms relatively uniform damage in a depth range of 125 ⁇ m to 165 ⁇ m below the surface of the light emitting element
- FIG. 3 shows Al in a depth range of 105 ⁇ m to 145 ⁇ m below the surface of the light emitting element.
- the 2 O 3 phase forms more uniform damage.
- FIG. 4 is a comparison of the total damage of the Y 3 Al 5 O 12 : Ce 3+ phase and the Al 2 O 3 phase after being irradiated with C ions under the same conditions as above. It can be seen that the damage depth in Y 3 Al 5 O 12 : Ce 3+ is larger than that in Al 2 O 3.
- the damage distribution in the Y 3 Al 5 O 12 : Ce 3+ phase is 125 ⁇ m-165 ⁇ m below the surface.
- the damage distribution in the three phases is 105 ⁇ m-145 ⁇ m below the surface, and the radiation in the same conditions, the damage in the Al 2 O 3 phase is larger than that in the Y 3 Al 5 O 12 : Ce 3+ phase.
- the inventors polished the light-emitting element in advance, and then performed high-energy ion irradiation. Because the wear rates of the Y and A phases are different, the former has a lower wear rate.
- the Y phase is a Y 3 Al 5 O 12 : Ce 3+ phase
- the A phase is an Al 2 O 3 phase.
- the surface formed after polishing is shown in FIG. 1.
- the surface of the Y 3 Al 5 O 12 : Ce 3+ phase is lower than that of the Al 2 O 3 phase, and its surface roughness is 20 ⁇ m.
- the polished light-emitting element is subjected to high-energy ion radiation to take into account the unevenness of the surface roughness.
- the surface of phase A is used as the surface of the light-emitting element, and Y 3 Al 5 O 12 :
- the uniform damage of Ce 3+ phase occurs in a depth range of 145 ⁇ m-185 ⁇ m below the surface, and the uniform damage of Al 2 O 3 phase still occurs at 105 ⁇ m-145 ⁇ m below the surface. Therefore, it should be understood that no matter whether the light-emitting element directly performs multiple high-energy ion irradiations or undergoes a polishing process and then multiple high-energy ion irradiations, the A phase with a higher Mohs hardness is at a more stable depth. Uniform damage occurs within the range, and the depth range is the predetermined depth range described in the present invention.
- step S2 uniform damage is caused to the A phase within a predetermined depth range, and it is only necessary to ensure that the damage can reduce the Mohs hardness of the A phase to approximately the same as that of the Y phase. To facilitate subsequent polishing.
- the inventors have found through experiments that the Dpa value of the Al 2 O 3 phase is 16 under the aforementioned experimental parameters, which means that each atom in the Al 2 O 3 phase has been knocked out of the original position 16 times on average. Such a high dislocation rate is sufficient As a result of Al 2 O 3 amorphization. Amorphous Al 2 O 3 has a reduced hardness and a higher wear rate. Under this damage, the Mohs hardness of Al 2 O 3 changed from the original 9 to 8.5, which is approximately equal to the Mohs hardness of Y 3 Al 5 O 12 : Ce 3+ . That is, at a depth of 105 ⁇ m-145 ⁇ m, the grinding rate is the same. Therefore, in the subsequent polishing process, polishing the irradiated sample within this depth range can form a flat surface.
- Step S3 polishing the light-emitting element after the high-energy ion irradiation to the above-mentioned predetermined depth range, thereby obtaining a flat surface.
- the predetermined depth is 105 ⁇ m to 145 ⁇ m.
- Step S4 Take out the light emitting element, and remove the conductive tape or adhesive with acetone.
- a light-emitting element with a smooth and flat surface can be obtained, and then a reflective layer can be attached to the polished surface of the light-emitting element for further processing, thereby realizing the processing of the wavelength replacement device.
- the method for polishing a light-emitting element of the present invention uses high-energy ions to radiate a light-emitting element with a complex phase structure with increasing energy gradient, so that the light-emitting element has a higher Mohs.
- the hardness phase causes uniform damage in a predetermined depth range below the surface of the light emitting element, thereby reducing its Mohs hardness to approximately the same as that of the other phase in the light emitting element, and then polishing the radiated light emitting element to this Depth results in a flat surface. It can avoid the uneven surface of micron level caused by the different hardness and grinding rate between different phases, so that the reflective layer and the like adhered on the surface are more firm and not easy to fall off.
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Abstract
一种发光元件的抛光方法,利用高能离子对发光元件进行能量梯度递增的辐射,使发光元件的A相在发光元件的表面以下的预定深度范围内产生均一的损伤,直到A相的莫氏硬度与Y相的莫氏硬度大致相同,随后将辐射后的发光元件抛光到预定深度得到平坦的表面。
Description
本发明属于发光材料技术领域,尤其涉及一种用于发光装置的发光元件及发光元件的高能离子辐射方法、抛光方法。
目前存在一种荧光粉同玻璃粉或陶瓷粉体混合烧结而获得的发光元件,如发光陶瓷/发光玻璃。该发光陶瓷/发光玻璃通过在背向激发光的一侧粘接一层反射层以及导热支撑装置形成发光装置,用于将激发光转换成预定波长的受激光。由于荧光粉烧结形成的相与玻璃粉或陶瓷粉烧结形成的相的莫氏硬度不同,导致研磨速率不同,所以抛光发光元件时形成凹凸表面,凹凸表面的起伏在微米级,在此凹凸表面覆盖反射层,导致反射层容易脱落。
因此,针对上述不足,实有必要提供一种新的用于激光光源的发光元件的高能离子辐射方法和抛光方法,以解决现有抛光方法成本高且性能不足的问题。
发明内容
为了克服现有技术的不足,本发明的目的在于提供一种发光元件及发光元件的高能离子辐射方法和抛光方法,以解决现有技术抛光时形成微米级起伏的凹凸表面,在此凹凸表面覆盖反射层,导致反射层结合不牢固容 易脱落的问题。
具体方式为,提供一种发光元件,由包括A相原料和Y相原料的至少两种原料烧结而成,形成包括A相和Y相至少两个相的复相结构,所述A相的莫氏硬度大于所述Y相的莫氏硬度,所述A相的DPA值大于所述Y相的DPA值,在受到离子辐射造成损伤后A相的莫氏硬度降低到与Y相大致相同。
优选的,所述发光元件为Y
3Al
5O
12:Ce
3+荧光粉和Al
2O
3颗粒经烧结而成的片状波长转换层,所述A相为Al
2O
3相,所述Y相为Y
3Al
5O
12:Ce
3+相。
优选的,所述波长转换层的厚度为350μm-450μm。
为解决上述问题,本发明还提供一种发光元件的高能离子辐射方法,其中,所述发光元件采用如上所述的具有复相结构的发光元件,利用高能离子对所述发光元件进行能量梯度递增的辐射,使所述发光元件的A相在所述发光元件的表面以下的预定深度范围内产生均一的损伤,直到所述A相的莫氏硬度与所述Y相的莫氏硬度大致相同。
优选的,所述高能离子为能量70MeV-80MeV的C离子或N离子。
优选的,所述A相的莫氏硬度与所述Y相的莫氏硬度的差值不超过0.5。
优选的,所述C离子辐射的剂量为1×10
15ions/cm
2,辐射速率为1×10
13ions/cm
2·s,辐射能量为70MeV。
优选的,经过第一次辐射后,每一次辐射的辐射能量以1MeV为公差递增。
为解决上述问题,本发明还提供一种发光元件的抛光方法,其包括如上所述的高能离子辐射方法,包括如下步骤:
步骤S1:提供具有复相结构的发光元件,将发光元件粘到离子注入机的样品台上,抛光面曝露;
步骤S2:对所述发光元件的抛光面进行高能离子辐射,每一个能量辐射完成后不取出样品,修改辐射参数进行下一次辐射,反复多次直到在预定深度范围内产生均一的损伤;
步骤S3:抛光至所述预定深度范围内得到平坦的表面。
优选的,所述步骤S1为通过导电胶带或胶粘剂实现发光元件的粘接,粘接面积小于所述发光元件的表面积。
优选的,在步骤S2后或步骤S3后还包括步骤S4:取出所述发光元件,用丙酮去除导电胶带或粘接剂。
优选的,步骤S2中的所述预定深度范围为100μm-145μm。
相对于现有技术,本发明的有益效果如下:本发明的发光元件及其高能离子辐射方法、抛光方法利用高能离子对具有复相结构的发光元件进行能量梯度递增的辐射,使所述发光元件中具有较高莫氏硬度的相在发光元件表面以下的预定深度范围内产生均一的损伤,从而使其莫氏硬度降低到与发光元件中另一相的莫氏硬度大致相同,随后将辐射后的发光元件抛光到该深度得到平坦的表面。可以避免不同相之间由于硬度和研磨速率不同而造成微米级的凹凸起伏的表面,使得在其表面粘贴的反射层等更加牢固,不容易脱落。
下面将结合附图及实施例对本发明作进一步说明。
图1是本发明发光元件直接进行抛光后的的表面结构示意图;
图2是本发明对发光元件进行多次辐射后Y
3Al
5O
12:Ce
3+相的损伤程度示意图;
图3是本发明对发光元件进行多次辐射后Al
2O
3相的损伤程度示意图;
图4是本发明发光元件不同相之间的损伤程度示意图;
图5是本发明发光元件经提前抛光后再进行辐射后不同相的损伤程度示意图;
图6是本发明发光元件的抛光方法的流程示意图。
本发明提供一种新的用于发光装置的发光元件的抛光方法,本发明的发光元件为发光陶瓷或发光玻璃,在对上述发光元件进行本发明的抛光方法后,可以形成平坦的表面,随后在该表面上可以贴附反射层等,进一步形成发光装置。通过本发明的抛光方法可以有效解决现有技术抛光时形成微米级起伏的凹凸表面,在此凹凸表面覆盖反射层,导致反射层结合不牢固容易脱落的问题。
本发明的抛光方法应用于通过包括A相原料和Y相原料的至少两种原料烧结而成的发光元件,该发光元件包括A相和Y相至少两个相,构成复相结构。其中Y相和A相具有不同的莫氏硬度,其耐磨和耐损伤性均不相同,具体是A相莫氏硬度大于Y相莫氏硬度。且A相的DPA值大于Y相的DPA值,在受到离子辐射被损伤后,其莫氏硬度改变,具体地,其莫氏硬度会降低。应当说明的是,DPA(displacements per atom)是指被辐射的发光陶瓷中平均每个原子被移位的次数,表示损伤程度,DPA值越大,表示损伤越严重。
具体在本实施方式中,Y相原料为Y
3Al
5O
12:Ce
3+荧光粉,A相原料为Al
2O
3颗粒,形成的A相为Al
2O
3相,Y相为Y
3Al
5O
12:Ce
3+相。当然,本发明的抛光方式也适用于其他复相结构的发光元件,而并不限于本实施方式说明的材料和结构,例如:Y相原料为LuAG:Ce
3+荧光粉,A相原料为玻璃粉,形成的A相为玻璃相,Y相为LuAG:Ce
3+相。
本实施方式采用Y
3Al
5O
12:Ce
3+荧光粉和Al
2O
3颗粒经烧结而成片状的波长转换层,即发光元件,其中Y
3Al
5O
12:Ce
3+荧光粉可以直接购买商业用荧光粉,或者用称取一定量的Y
2O
3(纯度99.99%)、Al
2O
3(纯度99.99%),CeO
2混合烧结而成。将上述发光元件切成厚度350μm-450μm的圆片状备用,厚度优选400μm。如图1所示,该发光元件直接进行抛光后的表面粗糙度在20μm左右,其中凸起部分为Al
2O
3相,凹陷部分为Y
3Al
5O
12:Ce
3+相,这是由于Al
2O
3的莫氏硬度大于Y
3Al
5O
12:Ce
3+的莫氏硬度,导致Al
2O
3的磨损速率比Y
3Al
5O
12:Ce
3+低,所以抛光后的表面为凹凸状。
如图2至图4所示,本发明提供一种使用高能离子对该发光元件进行能量梯度递增的辐射方法和应用该方法的抛光方法,使发光元件的A相在发光元件表面以下的预定深度范围内产生均一的损伤,直到A相的莫氏硬度与Y相的莫氏硬度大致相同,随后将辐射后的发光元件抛光到该深度得到平坦的表面。其中高能离子具体为能量在70MeV-80MeV的C离子或N离子。需要说明的是,本发明中所说的A相莫氏硬度与Y相莫氏硬度大致相同应当理解为A相莫氏硬度与Y相莫氏硬度的差值不超过0.5,优选不超过0.3。
具体的,以本实施方式为例,本发明抛光方法的步骤为:
步骤S1:将发光元件通过导电胶带或粘接剂粘到离子注入机的样品台 上,其中抛光面曝露。具体可以采用在背离抛光面的一侧涂覆双面碳导电胶带或银胶粘接剂,其中双面碳导电胶带或银胶形成的粘接面积小于所述发光元件待粘接所在面的表面积,这样,可以保证胶不会露出,从而防止离子打到胶带上引起溅射污染。
步骤S2:对所述发光元件的抛光面进行高能离子辐射,每一个能量辐射完成后不取出样品,修改辐射参数进行下一次辐射,反复多次直到在预定深度范围内产生均一的损伤。
其中高能离子可采用元素周期表中化学活泼性低的非气态元素,如C(碳)、P(磷)、B(硼)、N(氮)等元素。不同辐射元素,由于原子量、电子结构不同,在基材内产生的损伤深度分布、损伤程度不同,因此可以根据实际情况设置辐射粒子的能量、种类、剂量等。以复相的发光陶瓷为例,复相发光陶瓷的抛光深度要与辐射损伤在发光陶瓷中的深度要匹配。优选的,可以采用C离子或N离子,具体在本实施方式中,采用C离子辐射,剂量为1×10
15ions/cm
2,辐射速率为1×10
13ions/cm
2·s,首次辐射时的辐射能量为70MeV,经过第一次辐射后,接下来每次辐射的剂量和注入速率保持不变而辐射能量以1MeV为公差递增,得到如图2所示的经过11次辐射的Y
3Al
5O
12:Ce
3+相损伤程度图,以及如图3所示的经过11次辐射的Al
2O
3相损伤程度图,X轴表示发光陶瓷表面以下的深度,Y轴表示采用C离子辐射造成的损伤程度。其中,图2和图3各图从左至右的11支单个峰形图分别是单次损伤图形。本发明采用多个能量组合多次辐射的原因在于,单一能量辐射,只能产生高斯分布的损伤,如图2和图3中的单次损伤图形,每一次能量辐射产生的损伤分布都是在各自深度范围内具有单个峰值的高斯分布,而无法在预定深度内产生均一的损伤。而本发明采用的多次 不同能量的辐射方法可以在预定深度区间,产生均一的损伤分布,参见图2和图3所示的总的损伤。图2示出在发光元件表面以下125μm~165μm的深度范围内Y
3Al
5O
12:Ce
3+相形成较为均一的损伤,图3示出在发光元件表面以下105μm~145μm的深度范围内Al
2O
3相形成较为均一的损伤。
图4是Y
3Al
5O
12:Ce
3+相和Al
2O
3相在受到上述相同条件下的C离子辐射后的总的损伤情况对比。可见,Y
3Al
5O
12:Ce
3+中的损伤深度大于Al
2O
3中的损伤深度,Y
3Al
5O
12:Ce
3+相中损伤分布在表面下125μm-165μm,Al
2O
3相中损伤分布在表面下105μm-145μm,且同样条件的辐射,在Al
2O
3相中的损伤大于在Y
3Al
5O
12:Ce
3+相中产生的损伤。
发明人对发光元件进行提前抛光,然后再进行高能离子辐射。由于Y相和A相的磨损速率不同,前者磨损速率低于后者,具体在本实施方式中,Y相为Y
3Al
5O
12:Ce
3+相,A相为Al
2O
3相,抛光后形成的表面如图1所示,Y
3Al
5O
12:Ce
3+相的表面低于Al
2O
3相的表面,其表面粗糙度在20μm。再根据上述步骤S2方法对该抛光的发光元件进行高能离子辐射将表面粗糙度的凹凸情况考虑到之后,如图5所示,以A相的表面作为发光元件的表面,Y
3Al
5O
12:Ce
3+相的均一损伤发生在表面以下145μm-185μm的深度范围,Al
2O
3相的均一损伤依然发生在表面下105μm-145μm。因此,应当理解的是,无论发光元件是直接进行多次高能离子辐射,还是先经过一道抛光工艺再进行多次高能离子辐射,具有较高莫氏硬度的A相的都是在较为稳定的深度范围内发生均一损伤,该深度范围即为本发明所述的预定深度范围。以上,经过步骤S2的多次辐射后在预定深度范围内使得A相产生均一的损伤,只需确保该损伤可以导致A相的莫氏硬度降低到与Y相的莫氏硬度大致相同即可,以便有助于后续抛光。
发明人经过实验发现,在前述的实验参数下Al
2O
3相的Dpa值为16,表示Al
2O
3相中平均每个原子被撞离开原来的位置16次,如此高的离位率足以导致Al
2O
3非晶化。非晶化的Al
2O
3硬度降低,磨损速率变大。在此损伤下,Al
2O
3的莫氏硬度由原来的9变为8.5,约等于Y
3Al
5O
12:Ce
3+的莫氏硬度。即在105μm-145μm深度,二者研磨速率相同。因此在后续抛光工艺中,在该深度范围内抛光辐射后的样品,就可以形成平坦的表面。
步骤S3:将经过高能离子辐射后的发光元件抛光到上述的预定深度范围,从而得到平坦的表面。以具有Y
3Al
5O
12:Ce
3+相和Al
2O
3相的发光陶瓷为例,预定深度为105μm-145μm。
步骤S4:取出发光元件,用丙酮去除导电胶带或粘接剂。
经过上述步骤,可以得到表面光滑平坦的发光元件,随后可以在发光元件的抛光面进行贴设反光层等进一步加工,从而实现波长装换装置的加工。
相对于现有技术,本发明的有益效果如下:本发明的发光元件的抛光方法利用高能离子对具有复相结构的发光元件进行能量梯度递增的辐射,使所述发光元件中具有较高莫氏硬度的相在发光元件表面以下的预定深度范围内产生均一的损伤,从而使其莫氏硬度降低到与发光元件中另一相的莫氏硬度大致相同,随后将辐射后的发光元件抛光到该深度得到平坦的表面。可以避免不同相之间由于硬度和研磨速率不同而造成微米级的凹凸起伏的表面,使得在其表面粘贴的反射层等更加牢固,不容易脱落。
上述实施方式仅为本发明的优选实施方式,不能以此来限定本发明保护的范围,本领域的技术人员在本发明的基础上所做的任何非实质性的变化及替换均属于本发明所要求保护的范围。
Claims (12)
- 一种发光元件,其特征在于,所述发光元件由A相原料和Y相原料至少两种原料烧结而成,形成包括A相和Y相至少两个相的复相结构,所述A相的莫氏硬度大于所述Y相的莫氏硬度,所述A相的DPA值大于所述Y相的DPA值,受到离子辐射造成损伤后A相的莫氏硬度降低到与Y相大致相同。
- 根据权利要求1所述的发光元件,其特征在于,所述发光元件为Y 3Al 5O 12:Ce 3+荧光粉和Al 2O 3颗粒经烧结而成的片状波长转换层,所述A相为Al 2O 3相,所述Y相为Y 3Al 5O 12:Ce 3+相。
- 根据权利要求2所述的发光元件,其特征在于,所述波长转换层的厚度为350μm-450μm。
- 一种发光元件的高能离子辐射方法,其特征在于,所述发光元件采用如权利要求1-3任意一项所述的发光元件,利用高能离子对所述发光元件进行能量梯度递增的辐射,使所述发光元件的A相在所述发光元件的表面以下的预定深度范围内产生均一的损伤,使所述发光元件的A相在所述发光元件的表面以下的预定深度范围内产生均一的损伤,直到所述A相的莫氏硬度与所述Y相的莫氏硬度大致相同。
- 根据权利要求4所述的发光元件的高能离子辐射方法,其特征在于,所述高能离子为能量70MeV-80MeV的C离子或N离子。
- 根据权利要求4所述的发光元件的高能离子辐射方法,其特征在于,所述A相的莫氏硬度与所述Y相的莫氏硬度的差值不超过0.5。
- 根据权利要求5所述的发光元件的高能离子辐射方法,其特征在于,所述C离子辐射的剂量为1×10 15ions/cm 2,辐射速率为1×10 13ions/cm 2·s, 辐射能量为70MeV。
- 根据权利要求7所述的发光元件的高能离子辐射方法,其特征在于,经过第一次辐射后,每一次辐射的辐射能量以1MeV为公差递增。
- 一种发光元件的抛光方法,其包含如权利要求4~8任意一项所述的高能离子辐射方法,其特征在于,包括如下步骤:步骤S1:提供具有复相结构的发光元件,将发光元件粘到离子注入机的样品台上,抛光面曝露;步骤S2:对所述发光元件的抛光面进行高能离子辐射,每一个能量辐射完成后不取出样品,修改辐射参数进行下一次辐射,反复多次直到在预定深度范围内产生均一的损伤;步骤S3:抛光至所述预定深度范围内得到平坦的表面。
- 根据权利要求9所述的发光元件的抛光方法,其特征在于,所述步骤S1为通过导电胶带或胶粘剂实现发光元件的粘接,粘接面积小于所述发光元件的表面积。
- 根据权利要求9所述的发光元件的抛光方法,其特征在于,在步骤S2后或步骤S3后还包括步骤S4:取出所述发光元件,用丙酮去除导电胶带或粘接剂。
- 根据权利要求9所述的发光元件的抛光方法,其特征在于,步骤S2中的所述预定深度范围为100μm-145μm。
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| CN1925128A (zh) * | 2005-08-30 | 2007-03-07 | 中美矽晶制品股份有限公司 | 复合晶片结构的制造方法 |
| CN107540369A (zh) * | 2017-02-28 | 2018-01-05 | 江苏罗化新材料有限公司 | 发光陶瓷、led封装结构及发光陶瓷的制备方法 |
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| CN107797312B (zh) * | 2016-09-07 | 2024-04-16 | 深圳光峰科技股份有限公司 | 陶瓷复合材料及其制备方法、波长转换器 |
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| CN1925128A (zh) * | 2005-08-30 | 2007-03-07 | 中美矽晶制品股份有限公司 | 复合晶片结构的制造方法 |
| CN107540369A (zh) * | 2017-02-28 | 2018-01-05 | 江苏罗化新材料有限公司 | 发光陶瓷、led封装结构及发光陶瓷的制备方法 |
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