CN100579723C - Laser glass mechanical chemical polishing method - Google Patents
Laser glass mechanical chemical polishing method Download PDFInfo
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- CN100579723C CN100579723C CN200810034960A CN200810034960A CN100579723C CN 100579723 C CN100579723 C CN 100579723C CN 200810034960 A CN200810034960 A CN 200810034960A CN 200810034960 A CN200810034960 A CN 200810034960A CN 100579723 C CN100579723 C CN 100579723C
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Abstract
The invention relates to a chemically mechanical polishing method for laser glass. The method comprises the following keys points: in the fine-grinding and polishing process, the fine sorting process of the abrasive materials with different granularity is used and the processing removal is controlled accurately, in order to ensure the removal of the destruction layer produced by the last process; during the process, the processing surface and the sub surface are corroded using corrosive solution, so that the destruction layer is loose; the regulating agent of pH value is added to the polishing agent to change the polishing efficiency. The corrosion of the processing surface and the sub surface improves the quality of the surface processing and the processing effect of the post process. The method improves the toughness of the surface processing of the laser glass. In the embodiments, the chemically mechanical polishing method is used for obtaining super-smooth laser glass surface with 5 angstrom root mean square of the roughness of the surface.
Description
Technical field
The present invention relates to laser glass, particularly a kind of laser glass mechanical chemical polishing method that is applicable to.
Background technology
At present, along with the fast development of light laser industry, the laser glass quality of finish requires more and more higher, and becomes the key of restriction laser aid light beam output performance.Laser glass precise polished still adopted traditional glass polishing technology, promptly substrate is carried out mechanical lapping and reach certain face shape and thickness deviation with diamond shot abrasive material operation break-down on cast iron plate, then the polishing machine with cerium oxide or iron oxide mixing water polishes on polishing pitch dish, finally reaches certain surface figure accuracy and surface roughness.The tradition glossing had not in depth been paid close attention to the chemical factor of substrate and polishing agent and polishing disk in the physics of laser glass itself and chemical characteristic and the polishing process, and operation is simple, and the efficient of polishing is not high, and the roughness of polished surface is generally all in nanometer scale.
Summary of the invention
The objective of the invention is to improve the deficiency of above-mentioned traditional glass polishing technology, a kind of laser glass mechanical chemical polishing method is provided, to improve the efficient and the surface quality of the polishing of laser glass tradition, processing roughness (RMS) is the ultra-smooth neodymium glass surface of 5 dusts.This method should be applicable to the ultra-smooth polishing of the laser glass that chemical stability is relatively poor, also is applicable to the ultra-smooth polishing of other optical glass.
Basic thought of the present invention is that the thought with chemical mechanical polishing is applied in the glossing of laser glass, takes into full account the chemical factor in physics, chemical property and the polishing process of laser glass in processing method.The key of laser glass mechanical chemical polishing method of the present invention is:
(1) operation is segmented, adopted different grinding and polish abrasive, the material removal amount of strict control operation in different operations;
(2) defective that last process produces is corroded with corrosive solution at inter process;
(3) in polishing fluid, add acidity-basicity regulator, the Acidity of Aikalinity of control polishing fluid.
The cmp method of described laser glass comprises the following steps:
Step 1: on the common grinding machine, adopt conventional shot abrasive material to carry out mechanical lapping laser glass to be processed, using average grain diameter at last is 40 microns diamond dust shot abrasive material, the glass flatness is worked into 10～20 microns, be at least following operation according to tolerance and stay 300 microns allowance, ultrasonic wave cleans;
Step 2: lapped face and inferior surface are corroded with corrosive agent, remove the blemish and the pollution of process of lapping, and deeply process inferior crizzle by strong acid and make it to become loose, the material of being convenient to next procedure is removed, the corrosive agent that is adopted is hydrofluoric acid and ammonium fluoride mixed solution: hydrofluoric acid concentration is 10%～15%, ammonium fluoride concentration is 10%～20%, cleans then;
Step 3: with average grain diameter is that 28 microns diamond dust finish grindes, and removes defective and micro-crack that step 1 produces, and removal amount is greater than 200 microns, to remove the defective that step 1 causes fully;
Step 4: repeating step 2:;
Step 5: with the diamond dust shot abrasive material of average grain diameter less than 14 microns, or finish grind less than 14 microns diamond set ball sheet, 1～5 micron of control surface figure accuracy is removed the manufacturing deficiency that step 3 produced, removal amount is 50～100 microns, and ultrasonic wave cleans;
Step 6: with concentration is that 5%～7% hydrofluoric acid and concentration are the mixed solution of 15% ammonium fluoride, corrodes, and cleans subsequently;
Step 7: with particle mean size is the polishing agent that the oxide cmp powder of 0.5～2 μ m mixes with distilled water, and its concentration is every liter of 50～100 gram, and to regulate the pH value of described polishing agent be 3～9 by adding pH value conditioning agent; Polishing disk is selected polishing pitch for use, and its hardness is 20 ℃ of needle penetrations 0.5 * 10
-1～2 * 10
-1Mm, control polish pressure and polishing rotating speed polish workpiece, and surperficial face shape error is required in the error range near final machined surface shape, and ultrasonic wave cleans;
Step 8: repeating step 6;
Step 9: the polishing agent of selecting for use particle mean size 0.2～0.5 μ m polishing powder, distilled water to mix with ethylene glycol, concentration than step 7 reduces one times, and use the polishing pitch dish softer to polish than step 7, reduce polish pressure and polishing rotating speed, adjusting the polishing kinematics parameters does not make the deformation of workpiece face poor to ensure, polish a quarter of an hour with pure distilled water low speed, remove the polishing residue;
Step 10: ultrasonic wave cleans, drying;
Step 11: check face shape and roughness.
In the described step 5, adopt diamond set ball sheet processing laser glass.
Described pH value conditioning agent is inorganic acid or organic acid acid regulator; Or the alkaline conditioner of inorganic base or organic base or basic salt.Described acid regulator is hydrochloric acid, citric acid, acetic acid or oxalic acid.
Described alkaline conditioner is NaOH or ammoniacal liquor.
The cmp method of described laser glass when being used for the polishing of phosphate laser glass, adopts the pH value conditioning agent of hydrochloric acid as polishing agent, and the pH value is controlled at 6～7.
Add ethylene glycol described in the described step 9 in polishing agent, the content that reduces water is to reduce the chemical action in the polishing.
Set ball sheet correct grinding has higher grinding efficiency to laser glass, can remove the blemish that last process produces fast, reach very little surface roughness (as making final surface roughness reach 0.05 micron less than 8 microns set ball sheet) with grain diameter, make workpiece machining surface become minute surface, the load of being convenient to check face shape error and reducing polishing process.But; fixed abrasive material grinds clearance can be tending towards slow in reasons such as the filling on surface and processing temperatures owing to glass chip; and easily generation " line "; this is owing to individual coarse abrasive particle in the ball sheet or the generation of ball sheet sharp edge; so will reasonably use cooling fluid when finish grinding and accurately control allowance with fixed abrasive material; avoid dark " line " to occur as far as possible, otherwise can cause fatal trouble the postorder polishing process.
To sum up, comprise three keys in the inventive method: the one, to operation break-down, adopt different grinding and polish abrasive in different operations, adjust different technological parameters; The 2nd, the defective that last process produces is corroded with corrosive solution at inter process; The 3rd, the Acidity of Aikalinity of polishing agent pH conditioning agent control polishing fluid.
Description of drawings
Fig. 1 is shot abrasive lapping of the present invention and polishing principles figure.
Fig. 2 makes the schematic diagram of set ball sheet correct grinding instrument of the present invention.
Fig. 3 is the process chart of laser glass processing.
Fig. 4 is the defective schematic diagram of laser glass attrition process face.
The specific embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing, but should not limit protection scope of the present invention with this.
See also Fig. 1 earlier, in Fig. 1,1-1 is abrasive grain (diamond dust shot abrasive material or a polishing powder), and 1-2 is that workpiece pastes mould, and 1-3 is abrasive disk or polishing disk, and 1-4 is the laser glass workpiece, and 1-5 is polishing pad or polishing glue-line.Abrasive disk 1-3 is driven with certain rotating speed rotation by machine tool chief axis in grinding and the polishing process, and laser glass workpiece 1-4 closely contacts servo-actuated rotation realization material with polishing pad or polishing glue-line 1-5 and removes under certain pressure.The tradition polisher lapper, laser glass workpiece 1-4 is realizing Even Grinding and the finishing of face shape along being certain pendulum spoke on the dish axial direction.
Fig. 4 is the defective schematic diagram of laser glass attrition process face.Characterized the abrasive material defective form that processing is produced to fragile material among the figure.4-1 is the raw surface layer (0.01～2 μ m) after grinding, and by the brittle fracture of densification, scratching and chips of glass are filled and formed, and the processing roughness of testing with the roughness tester device of contact promptly characterizes the fluctuating and the degree of roughness of this layer.4-2 is the crushing layer (being about tens microns) of the densification that formed by bulk cargo abrasive material or set grinding in the process of lapping, because fixed abrasive material mainly works by radially cutting force, so fixed abrasive material produces less crushing layer.4-3 is the fine fisssure lamina, and this layer is because under the different processing modes, the degree of depth can be from 100 μ m to 300 μ m, and the total depth that makes correct grinding and polishing to remove generally is greater than this degree of depth.
Laser glass workpiece to 40 millimeters bores polishes.The laser glass material of experiment usefulness is the phosphate neodymium glass of Shanghai Optics and Precision Mechanics institute, Chinese Academy of Sciences.Its characteristic parameter sees Table 1.
Table 1
Referring to Fig. 3, Fig. 3 is the process chart of laser glass processing.Concrete processing step is as follows:
Carry out conventional shot abrasive material machinery at the common grinding machine and grind to form type, last procedure is about 40 microns diamond dust with particle diameter, and flatness is machined to 15 microns, and record grinds the surface roughness that produces.Workpiece is carried out ultrasonic wave to be cleaned.
With 10% hydrofluoric acid and 20% ammonium fluoride mixed solution lapped face and inferior surface were corroded 3 hours.
The silicon carbide abrasive that is about 28 microns with particle diameter carries out lapped face, 30 minutes process times.Used lathe schematic diagram as shown in Figure 1, speed of mainshaft 150rpm, workpiece is with commentaries on classics.Write down removal amount and surface roughness every 10 minutes.
With 10% hydrofluoric acid and 20% ammonium fluoride mixed solution lapped face and inferior surface were corroded 2 hours.
The silicon carbide abrasive that is about 14 microns with particle diameter finish grindes machined surface, control 1～5 micron of surface figure accuracy (detecting with testplate), 30 minutes process times.150 rpms of the speeds of mainshaft, workpiece is with commentaries on classics.Write down removal amount and surface roughness every 10 minutes.Ultrasonic wave cleans.
With concentration is that 5% hydrofluoric acid and concentration are that 15% ammonium fluoride mixed solution corroded 2 hours machined surface.
The phase I polishing.For the repeatability of testing, the polishing powder technical parameter that we adopt is: cerium oxide content is greater than 99%, 1 micron of particle mean size, density 1.6 grams per liters.Polishing agent concentration 100 grams per liters.Adding hydrochloric acid in polishing agent makes polishing agent keep pH value 6～7.Polishing disk adopts harder polishing pitch casting (rosin and pitch mixing ratio are about 7: 3).The buff spindle rotating speed is 120 rpms, and workpiece is with commentaries on classics.Polishing time was 120 minutes, every 30 minutes record polishing removal amounts.Ultrasonic wave cleaned after polishing was finished, and detected surface roughness with Zaser contourgraph.
With concentration 5% hydrofluoric acid and concentration is that 15% ammonium fluoride mixed solution slightly corroded 30 minutes machined surface.
The second stage polishing.The polishing powder that adopts is a kind of high-purity (99.98%) aluminum oxide polishing powder, density 0.15 grams per liter, and particle mean size is 0.4 micron.Polishing agent concentration is 50 grams per liters.Adding hydrochloric acid in polishing agent makes polishing agent keep pH value 6～7.Polishing disk adopts softer polishing pitch casting (rosin and pitch mixing ratio are about 6: 4).The buff spindle rotating speed is 60 rpms, and workpiece is with commentaries on classics.Polishing time was 60 minutes, every 30 minutes record polishing removal amounts.Pure water low speed (40 rpms) polishing 15 minutes.Ultrasonic wave disappeared and washes after polishing was finished, detect surface roughness with Zaser contourgraph, the root mean square RMS of surface roughness is 0.758nm, and these data are the systematic errors that comprise instrument, the actual systematic error of removing apparatus measures, surface roughness should reach the ultra-smooth level of 5 dusts.
Detect the final machined surface shape of workpiece with laser plane interferometer.Surface figure accuracy finally can remain to PV value λ/10.
Experimental data sees Table 2, and roughness characterizes and is root mean square RMS and arithmetic mean of instantaneous value Ra in the table.
Find out from embodiment,, obtained the super-smooth surface processing of the laser glass of Subnano-class by adopting the committed step in the aforementioned inventive method.
Table 2
This experiment in step 7, we are by changing the pH value of polishing agent, verified the influence of polishing agent pH value to the phosphate laser glass polishing efficiency, with pitch lacquer disk(-sc) polishing phosphate laser glass the time, polishing agent has higher polishing efficiency when neutral and subacidity.
Embodiment 2
On the basis of embodiment 1, step 3 changes into and adopts particle diameter is that 12 microns diamond set ball sheet adds under 150 rpms of situations of the cooling fluid speed of mainshaft and ground 30 minutes, it is that 8 microns diamond set ball sheet adds under 150 rpms of situations of the cooling fluid speed of mainshaft and ground 30 minutes that step 5 is used particle diameter instead, the final stage of step 9 adds 50% ethylene glycol in pure water, other machined parameters and step are constant.The diamond pellet sheet machining tool schematic diagram that adopts in the test is seen Fig. 2,2-1 is the fixed ball sheet of varigrained diamond, 2-2 is cast iron or stainless steel holder mould, will be when actual fabrication by making the holder mould reach certain surface figure accuracy to grinding, at last the ball sheet is arranged and density degree is bonded on the holder mould with glue by certain, be trimmed to required machining accuracy after the drying.Experimental data sees the following form 3.
From embodiment 2 and embodiment 1 to recently: adopting the most significant advantage of diamond pellet sheet is to reduce surface roughness rapidly in the correct grinding stage to drop to tens nanometers (seeing Table 3) from several microns, and make workpiece machining surface become minute surface, can adopt method of optics detection faces shape in the grinding stage.And the good set ball sheet polishing tool of surface figure accuracy own can be easy to process high-precision workpiece face shape, so just alleviated the task amount in polishing stage.But, find to adopt set ball sheet material removing rate of (150 rpms) when low speed grinds to be significantly less than the processing of bulk cargo abrasive material in the experiment, and along with time duration, because the filling of machining chips, the efficient meeting descends rapidly, thereby and adopts grinding at a high speed to certainly lead to higher processing heat and reduce surface figure accuracy.So, adopt the diamond pellet slice lapping will adopt the circulation cooling to reduce processing temperature, and accurately removal amount, the removal fully of guaranteeing to process breakable layer are ground in control.Consider that in the step 3 of embodiment 2 particle diameter is about 40 microns diamond dust shot abrasive material generation breakable layer and the removal fully of fine fisssure lamina (being about 40～100 microns) was processed again 30 minutes, just a kind of conservative approach of in reality processing, taking.
Add ethylene glycol mixture in polishing agent, can effectively reduce the chemical action in the polishing process, make the polishing clearance reduce, this is to prevent because the too fast bad effective ways of face deformation that cause of polishing efficiency in the final stage of polishing.
Claims (6)
1, a kind of cmp method of laser glass is characterized in that comprising the following steps:
Step 1: on the common grinding machine, adopt conventional shot abrasive material to carry out mechanical lapping laser glass to be processed, using average grain diameter at last is 40 microns diamond dust shot abrasive material, the glass flatness is worked into 10～20 microns, be at least following operation according to tolerance and stay 300 microns allowance, ultrasonic wave cleans;
Step 2: lapped face and inferior surface are corroded with corrosive agent, remove the blemish and the pollution of process of lapping, and deeply process inferior crizzle by strong acid and make it to become loose, the material of being convenient to next procedure is removed, the corrosive agent that is adopted is hydrofluoric acid and ammonium fluoride mixed solution: hydrofluoric acid concentration is 10%～15%, ammonium fluoride concentration is 10%～20%, cleans then;
Step 3: with average grain diameter is that 28 microns diamond dust finish grindes, and removes defective and micro-crack that step 1 produces, and removal amount is greater than 200 microns, to remove the defective that step 1 causes fully;
Step 4: repeating step 2;
Step 5: with the diamond dust shot abrasive material of average grain diameter less than 14 microns, or finish grind less than 14 microns diamond set ball sheet, 1～5 micron of control surface figure accuracy is removed the manufacturing deficiency that step 3 produced, removal amount is 50～100 microns, and ultrasonic wave cleans;
Step 6: with concentration is that 5%～7% hydrofluoric acid and concentration are the mixed solution of 15% ammonium fluoride, corrodes, and cleans subsequently;
Step 7: with particle mean size is the polishing agent that the oxide cmp powder of 0.5～2 μ m mixes with distilled water, and its concentration is every liter of 50～100 gram, and to regulate the pH value of described polishing agent be 3～9 by adding pH value conditioning agent; Polishing disk is selected polishing pitch for use, and its hardness is 20 ℃ of needle penetrations 0.510
-1～2 * 10
-1Mm, control polish pressure and polishing rotating speed polish workpiece, and surperficial face shape error is required in the error range near final machined surface shape, and ultrasonic wave cleans;
Step 8: repeating step 6;
Step 9: the polishing agent of selecting for use particle mean size 0.2～0.5 μ m polishing powder, distilled water to mix with ethylene glycol, concentration than step 7 reduces one times, and use the polishing pitch dish softer to polish than step 7, reduce polish pressure and polishing rotating speed, adjusting the polishing kinematics parameters does not make the deformation of workpiece face poor to ensure, polish a quarter of an hour with pure distilled water low speed, remove the polishing residue;
Step 10: ultrasonic wave cleans, drying;
Step 11: check face shape and roughness.
2, the cmp method of laser glass according to claim 1 is characterized in that described step 5, adopts diamond set ball sheet processing laser glass.
3, the cmp method of laser glass according to claim 1 is characterized in that described pH value conditioning agent is inorganic acid or organic acid acid regulator; Or the alkaline conditioner of inorganic base or organic base or basic salt.
4, the cmp method of laser glass according to claim 3 is characterized in that described acid regulator is hydrochloric acid, citric acid, acetic acid or oxalic acid.
5, the cmp method of laser glass according to claim 3 is characterized in that described alkaline conditioner is NaOH or ammoniacal liquor.
6, according to the cmp method of claim 1 or 2 or 3 described laser glasses, it is characterized in that this finishing method is applicable to the polishing of phosphate laser glass, adopt the pH value conditioning agent of hydrochloric acid as polishing agent, the pH value is controlled at 6～7.
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