CN108838745B - A kind of efficient chemical mechanical polishing method of yag crystal - Google Patents

A kind of efficient chemical mechanical polishing method of yag crystal Download PDF

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Publication number
CN108838745B
CN108838745B CN201810675798.8A CN201810675798A CN108838745B CN 108838745 B CN108838745 B CN 108838745B CN 201810675798 A CN201810675798 A CN 201810675798A CN 108838745 B CN108838745 B CN 108838745B
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mechanical polishing
chemical mechanical
polishing
concentration
yag crystal
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CN108838745A (en
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金洙吉
安润莉
张自力
韩晓龙
康仁科
朱祥龙
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Dalian University of Technology
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Dalian University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/11Lapping tools
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents

Abstract

The invention belongs to hard brittle material Ultra-precision Turning fields, provide a kind of efficient chemical mechanical polishing method of yag crystal.The method includes the steps of: 1) at room temperature, abrasive material zirconium oxide, chemical reaction reagent sodium hydroxide, additive being added in deionized water, ultrasonic vibration prepares chemical mechanical polishing liquid;2) polishing pad is modified as polishing pad for chemomechanical polishing using IC1000 polishing pad;3) technological parameter is chosen, yttrium-aluminium-garnet chip is chemically-mechanicapolish polished.By the invention it is possible to which higher material removing rate obtains the yttrium-aluminium-garnet chip of low damage.

Description

A kind of efficient chemical mechanical polishing method of yag crystal
Technical field
The invention belongs to hard brittle material Ultra-precision Turning fields, are related to a kind of processing of laser crystal material, in particular to To the method for the chemically mechanical polishing of yag crystal.
Background technique
Yag crystal (YAG) is the gain media host material being most widely used in solid state laser.Currently, Diamond or Al are generallyd use in the polishing process of YAG crystal2O3Equal hard grinds material is polished, exist processing efficiency is low, surface and The problems such as sub-surface damage is serious.Chemically mechanical polishing is a kind of by abrasive material in the chemical attack effect of polishing fluid and polishing fluid Mechanism coordinated come realize to YAG plane of crystal carry out skin processing processing method.By chemically-mechanicapolish polishing, The low damage even YAG crystal without mechanical processing trauma can be quickly obtained.
Workpiece is contacted with work surface with polishing pad, is processed under certain pressure effect.In polishing fluid Chemical substance can be chemically reacted with workpiece surface, be performed etching to it, form softening layer, while carrying out mechanical removal.
Polishing fluid is generally made of abrasive material, chemical reactor and additive.In process, the abrasive material in polishing fluid is logical It crosses scratching and squeezes workpiece surface and play the role of main mechanical removal.Chemical reactor plays in CMP process The effect chemically reacted, can soften or directly etching workpiece surface.Chemical reactor can also adjust polishing fluid simultaneously The dispersibility of the quantity of electric charge and then influence polishing fluid of pH value, change abrasive material in polishing fluid in system.The kind of additive Class has very much, including improving the dispersing agent of polishing fluid system dispersibility, the emulsifier for playing the role of wetting action, playing defoaming Defoaming agent, foaming agent of foam enhancing effect etc..
Currently, being rarely directed to the disclosure or granted patent of YAG polishing crystal.In paper report, for YAG crystal Chemically mechanical polishing generallys use silica solution abrasive material, neutrality or weak acid alkalescence polishing liquid, but this method polishing efficiency is low, chemical Reaction is nor very clear.The J Mc Kay of University of California in Los Angeles is mentioned in doctoral thesis using silica solution and hydrogen-oxygen Change sodium preparation polishing fluid to be chemically-mechanicapolish polished, obtains YAG crystalline nanometric grade roughness surface, but material removing rate only has 0.3nm/min.Teng Lin " the ultraprecise technology of preparing of yttrium-aluminium-garnet (YAG) and Gd-Ga garnet (GGG) epitaxial substrate " (in State's mechanical engineering, 1997,5:86-87+108.) matched using the reagents such as sodium metasilicate, hydrochloric acid, calcium chloride are added in silica solution in paper Chemical mechanical polishing liquid processed, polishing time are 3-4 hours.
Summary of the invention
In order to solve, polishing fluid classification existing for existing YAG crystal chemistry mechanical polishing method is single, removal efficiency is low The problems such as difficult to control with finished product polishing fluid complicated components, the present invention propose a kind of be used to the mechanical polishing of YAG crystal efficient chemical Method, by the chemical mechanical polishing liquid of the recipe configuration, on IC1000 polishing pad, with defined technological parameter Mechanical polishing test is learned, can be with the material removing rate of 2nm/min or so, it is small that processing can be obtained surface roughness Ra in 1 hour In the YAG plane of crystal of 1nm.
The technical solution adopted by the present invention are as follows:
A kind of efficient chemical mechanical polishing method of yag crystal comprising the steps of:
The first step prepares chemical mechanical polishing liquid
At room temperature, abrasive material zirconium oxide, chemical reaction reagent sodium hydroxide, additive are added in deionized water, ultrasound is set Standby middle concussion 30min obtains chemical mechanical polishing liquid, and the additive is neopelex, polymethylacrylic acid It receives, one or more kinds of compositions of isopropanol, PEG 20000.
In chemical mechanical polishing liquid, the zirconium oxide concentration is 0.04~0.1g/ml, and zirconium oxide partial size is 0.03-1 μ m;The naoh concentration is 0.03~0.07g/ml;The neopelex concentration is 0.25g/L, poly- first Base acrylic acid receives concentration as 2g/L, and isopropyl alcohol concentration is 2g/L or PEG 20000 concentration is 1g/L.
In chemical mechanical polishing liquid, the zirconium oxide concentration is preferably 0.04g/ml, and zirconium oxide partial size is preferably 1 μm; The naoh concentration is preferably 0.07g/ml.
Second step modifies polishing pad using IC1000 polishing pad as polishing pad for chemomechanical polishing.
Third step chemically-mechanicapolish polishes yag crystal, can reach the material removing rate of 2nm/min, The YAG plane of crystal that surface roughness Ra is less than 1nm is obtained after processing 1 hour.The mechanical polishing parameter are as follows: polish pressure 1-4N/cm2, polishing disk rotating speed 40-100r/min, polishing flow quantity 6-9ml/min.
Effect and benefit of the present invention is: the present invention, which can achieve, compares the material removing rate that conventional chemical-mechanical polishes 6 times, 2-3 hour process times are saved, while the low injured surface that nothing is obviously damaged after being etched.
Detailed description of the invention
Fig. 1 is by YAG plane of crystal Al 2p detection XPS comparison diagram before and after soaking with sodium hydroxide;It (a) is sodium hydroxide Before immersion;(b) for after soaking with sodium hydroxide.
Fig. 2 is by YAG plane of crystal O 1s detection XPS comparison diagram before and after soaking with sodium hydroxide;(a) it is soaked for sodium hydroxide Before bubble;(b) for after soaking with sodium hydroxide.
Fig. 3 is by YAG plane of crystal Y 3d detection XPS comparison diagram before and after soaking with sodium hydroxide;(a) it is soaked for sodium hydroxide Before bubble;(b) for after soaking with sodium hydroxide.
Fig. 4 is various concentration and type the additive dispersed testing result in chemical mechanical polishing liquid.
Fig. 5 is YAG plane of crystal chemically mechanical polishing front and back microphoto;A) before chemically-mechanicapolish polishing, b) chemical machinery After polishing (after etching).
Fig. 6 is roughness measurement picture of the YAG crystal after chemically mechanical polishing.
Specific embodiment
This present invention is described further below in conjunction with specific embodiment.
The present invention is for the purpose of efficiently polishing, from abrasive hardness, XPS of the analytical chemistry reaction reagent to the surface YAG The dispersion effect of testing result and additive determines chemical mechanical polishing liquid ingredient and machined parameters with actual processing effect.Tool Body the following steps are included:
1) determining selects 1 μm of zirconium oxide as polishing fluid abrasive material.Sodium hydroxide is as chemical reaction reagent, concentration 0.07g/ml。
Fig. 1-3 is to detect XPS comparison diagram by YAG plane of crystal before and after soaking with sodium hydroxide.As can be seen from the figure it passes through Al-O key is significantly reduced in YAG plane of crystal ingredient after crossing naoh treatment, illustrates that sodium hydroxide can be with It is chemically reacted with YAG, and destroys the Al-O key of YAG plane of crystal, YAG crystal surface properties is made to tend to Y2O3Knot Structure.Y2O3Hardness compared to YAG crystal hardness it is low, be more advantageous to and be removed.
The zirconium oxide turbid (zirconium oxide partial size 30nm) containing 5%NaOH is prepared, chemical reaction reagent sodium hydroxide is added Afterwards, the dispersion performance of turbid is tested.Fig. 4 is the Zeta potential and polishing fluid droplet measurement knot of the additive of various concentration and type Fruit.Wherein, the additive that number 2-5 is selected is respectively that neopelex (0.25g/L), polymethylacrylic acid receive (2g/ L), isopropanol (2g/L), PEG 20000 (1g/L), number 1 are used as blank control.It can be seen from the figure that not being added Sodium hydroxide solution is added in the turbid (number 1) of any additive, the particle aggregation in solution is at 3000nm or so.Addition adds After adding agent, the partial size in polishing fluid has apparent reduction, wherein the suspension of the neopelex of 0.25g/L is added Dispersion effect is best, and the partial size of polishing fluid is 900nm.The polymethylacrylic acid that 2g/L is added is received, and the partial size of polishing fluid is 1300nm.The isopropanol of 2g/L is added, the partial size of polishing fluid is 1490nm.1g/L PEG 20000, the grain of polishing fluid is added Diameter is 1490nm.The above results show that additive can make the abrasive material in polishing fluid disperse more uniformly, to reduce machining damage, Promote processing efficiency.
2) it selects IC1000 as polishing pad for chemomechanical polishing, polishing pad finishing is carried out by diamond truer.
3) the chemically mechanical polishing test of YAG crystal, polish pressure 2N/cm are carried out2, polishing disk rotating speed 60r/min, throwing Light flow quantity 6ml/min.
Fig. 5 is microphoto after YAG plane of crystal chemically mechanical polishing front and back microphoto and etching.It can from figure Out, it although comparing polishing front surface (being prepared by thin film abrasive paper smooth grinding) without significant change, finds to use after over etching Cmp method of the invention is after over etching without obvious damage.Illustrate zirconium oxide as the abrasive material softer than YAG crystal There is the effect for reducing surface machining damage well.
Fig. 6 is roughness measurement picture of the YAG crystal after chemically mechanical polishing.
By the above method configure chemical mechanical polishing liquid, on IC1000 polishing pad, with defined technological parameter into Row chemically mechanical polishing test, can be with the material removing rate of 1.99nm/min, and processing 1 hour can be obtained surface roughness Ra YAG plane of crystal less than 1nm.It can achieve and compare the material removing rate that conventional chemical-mechanical polishes 6 times, save 2-3 hours Process time, while without the low injured surface obviously damaged after being etched.

Claims (5)

1. a kind of efficient chemical mechanical polishing method of yag crystal, which is characterized in that comprise the steps of:
The first step prepares chemical mechanical polishing liquid
At room temperature, abrasive material zirconium oxide, chemical reaction reagent sodium hydroxide, additive are added in deionized water, after ultrasonic vibration Chemical mechanical polishing liquid is obtained, the additive is neopelex, polymethylacrylic acid is received, isopropanol, poly- second One or more kinds of compositions of glycol 20000;In chemical mechanical polishing liquid, the zirconium oxide concentration be 0.04~ 0.1g/ml, zirconium oxide partial size are 0.03-1 μm;The naoh concentration is 0.03~0.07g/ml;The dodecane Base benzene sulfonic acid sodium salt concentration be 0.25g/L, polymethylacrylic acid receive concentration be 2g/L, isopropyl alcohol concentration 2g/L, polyethylene glycol 20000 concentration are 1g/L;
Second step modifies polishing pad using IC1000 polishing pad as polishing pad for chemomechanical polishing;
Third step chemically-mechanicapolish polishes yag crystal, can reach the material removing rate of 2nm/min, processing 1 The YAG plane of crystal that surface roughness Ra is less than 1nm is obtained after hour.
2. a kind of efficient chemical mechanical polishing method of yag crystal according to claim 1, which is characterized in that The zirconium oxide concentration is preferably 0.04g/ml, and zirconium oxide partial size is preferably 1 μm;The naoh concentration is preferably 0.07g/ml。
3. a kind of efficient chemical mechanical polishing method of yag crystal according to claim 1 or 2, feature exist In chemically mechanical polishing parameter are as follows: polish pressure 1-4N/cm2, polishing disk rotating speed 40-100r/min, polishing flow quantity 6-9ml/ min。
4. a kind of efficient chemical mechanical polishing method of yag crystal according to claim 1 or 2, feature exist In the ultrasonic vibration time is 30min in the first step.
5. a kind of efficient chemical mechanical polishing method of yag crystal according to claim 3, which is characterized in that The ultrasonic vibration time is 30min in the first step.
CN201810675798.8A 2018-06-27 2018-06-27 A kind of efficient chemical mechanical polishing method of yag crystal Active CN108838745B (en)

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Publication number Priority date Publication date Assignee Title
CN109913133B (en) * 2019-03-29 2020-09-29 大连理工大学 Efficient high-quality chemical mechanical polishing solution for yttrium aluminum garnet crystals
CN112621557B (en) * 2020-12-17 2022-08-09 江苏集萃精凯高端装备技术有限公司 Polishing method of YAG wafer
CN113480942B (en) * 2021-08-06 2022-06-07 大连理工大学 Polycrystalline YAG ceramic chemical mechanical polishing solution
CN116463061A (en) * 2023-04-20 2023-07-21 大连理工大学 Ultrathin laser crystal chemical mechanical polishing solution based on optical field coupling and preparation and polishing methods thereof

Citations (5)

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Publication number Priority date Publication date Assignee Title
US6046112A (en) * 1998-12-14 2000-04-04 Taiwan Semiconductor Manufacturing Company Chemical mechanical polishing slurry
CN1590026A (en) * 2003-07-17 2005-03-09 Jsr株式会社 Chemical mechanical polishing pad and chemical mechanical polishing method
CN102648265A (en) * 2009-10-13 2012-08-22 株式会社Lg化学 Slurry composition for CMP, and polishing method
CN103732354A (en) * 2011-07-08 2014-04-16 宇部兴产株式会社 Method for producing ceramic composite for photoconversion
CN104592895A (en) * 2014-09-26 2015-05-06 深圳市力合材料有限公司 Preparation method of silica sol

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6046112A (en) * 1998-12-14 2000-04-04 Taiwan Semiconductor Manufacturing Company Chemical mechanical polishing slurry
CN1590026A (en) * 2003-07-17 2005-03-09 Jsr株式会社 Chemical mechanical polishing pad and chemical mechanical polishing method
CN102648265A (en) * 2009-10-13 2012-08-22 株式会社Lg化学 Slurry composition for CMP, and polishing method
CN103732354A (en) * 2011-07-08 2014-04-16 宇部兴产株式会社 Method for producing ceramic composite for photoconversion
CN104592895A (en) * 2014-09-26 2015-05-06 深圳市力合材料有限公司 Preparation method of silica sol

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