[go: up one dir, main page]

CN109312212A - Grinding liquid - Google Patents

Grinding liquid Download PDF

Info

Publication number
CN109312212A
CN109312212A CN201780033332.1A CN201780033332A CN109312212A CN 109312212 A CN109312212 A CN 109312212A CN 201780033332 A CN201780033332 A CN 201780033332A CN 109312212 A CN109312212 A CN 109312212A
Authority
CN
China
Prior art keywords
grinding
solvent
system solvent
grinding liquid
ether
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201780033332.1A
Other languages
Chinese (zh)
Other versions
CN109312212B (en
Inventor
井上裕昭
竹村幸二
笹岛启佑
西藤和夫
田浦歳和
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Creative Ltd By Share Ltd
Bando Chemical Industries Ltd
SpeedFam Co Ltd
Original Assignee
Creative Ltd By Share Ltd
Bando Chemical Industries Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Creative Ltd By Share Ltd, Bando Chemical Industries Ltd filed Critical Creative Ltd By Share Ltd
Publication of CN109312212A publication Critical patent/CN109312212A/en
Application granted granted Critical
Publication of CN109312212B publication Critical patent/CN109312212B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304Mechanical treatment, e.g. grinding, polishing, cutting

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Grinding-Machine Dressing And Accessory Apparatuses (AREA)

Abstract

The relatively high grinding liquid of the recovery efficiency that the dispersibility when inhibiting containing abrasive grains that the purpose of the present invention is to provide a kind of is centrifugated while reduction.In grinding liquid of the invention, total content of alcohol system solvent and ether system solvent in all solvents of grinding liquid is 95 mass % or more, 100 mass % are hereinafter, ether system solvent relative to the mass ratio of alcohol system solvent is 1 times or more, 5 times or less.The viscosity of ether system solvent at 25 DEG C is lower than the viscosity of alcohol system solvent, and ether system solvent and the differences in viscosity of alcohol system solvent are preferably 15mPas or more, 20mPas or less.

Description

Grinding liquid
Technical field
The present invention relates to a kind of grinding liquid.
Background technique
In recent years, as the precise electronics machines such as hard disc (hard disk), light emitting diode (light emitting Diode, LED), the substrate of power component (power device) etc., it is difficult to glass, sapphire (saphire), silicon carbide etc. plus The increase in demand of work substrate.
Usually using the grinding pad of fixed abrasive grains in the grinding of such difficult processing substrate.Use the fixed abrasive grains The processing of grinding pad commercially available twin grinder can be used for example to carry out.Specifically, the substrate kept by carrier is pressed from both sides Enter to be fixed between the upper pressing disc of grinding pad, makes a relative move substrate with upper pressing disc, it is thus same to the two sides of substrate Shi Jinhang grinding.At this point, in order to supply grinding liquid to the two sides of substrate by the cooling of the machined surface of substrate or in order to promote processing.
As the grinding liquid, it is known to be ground such as the pulp-like containing abrasive grains aluminium oxide particles or silicon oxide particle Cut liquid.In order to make the abrasive grains contribute effectively to grind in grinding, abrasive grains are needed in grinding liquid in dispersed State.Therefore, for the viewpoint of the dispersibility of the abrasive grains, as the solvent of grinding liquid, usually using alcohol systems such as ethylene glycol Solvent.
The grinding liquid is recycled in order to reduce manufacturing cost or reduce carrying capacity of environment.In the grinding, Meeting self-reference substrate generates grinding clast and is mixed into grinding liquid, therefore, if repeating the recycling of grinding liquid, in grinding liquid The amount of contained grinding clast will increase.If the amount of grinding clast contained in grinding liquid as described above increases, it is easy The reduction of grinding efficiency or the damage to substrate for causing substrate.Therefore, it in order to carry out the recycling to grinding liquid, needs to use certainly Grinding clast is separated and recovered in grinding liquid afterwards.As the separation and recovery method, centrifuge separation can be enumerated, by filter Separation passes through the methods of washing separation of strong acid or highly basic.In these, for the separation by filter, high property is needed The filter of energy, therefore filter is at high cost.In addition, for using the washing of strong acid or highly basic to separate, the place of waste liquid It manages cost and carrying capacity of environment is big.Therefore, usually using centrifuge separation in the separation of grinding clast.
In the case where the grinding liquid to alcohol system solvent is centrifuged, especially it is difficult to recycle partial size to be 100nm Small grinding clast below, the recovery efficiency of grinding liquid are easily reduced.As the method for improving the recovery efficiency, such as have logical The method crossed the further progress UF membrane after being centrifuged and recycle the small grinding clast of partial size is (special referring to Japan Patent Open 2010-221337 bulletin).However, if increasing as described above in order to improve recovery efficiency other than centrifuge separation Separating step, then manufacturing equipment increased costs or the working hour for carrying out grinding liquid recycling increase.Pass through it is therefore desirable to improve The recovery efficiency to grinding liquid of centrifuge separation.
Existing technical literature
Patent document
Patent document 1: Japanese Patent Laid-Open 2010-221337 bulletin
Summary of the invention
Problem to be solved by the invention
The present invention is formed in view of these undesirable conditions, and the purpose of the present invention is to provide one kind to inhibit to contain abrasive grains When dispersibility relatively high grinding liquid of the recovery efficiency that is centrifugated while reduce.
Technical means to solve problem
The present inventor et al. has carried out the recovery efficiency by the grinding liquid being centrifugated to make great efforts research, as a result, it has been found that, By adding the ether system solvent of specified amount in alcohol system solvent as the solvent of grinding liquid, even partial size is 100nm or less Small grinding clast can also be recycled by centrifuge separation from grinding liquid, so as to complete the present invention.
That is, to solve the above technical problems and complete invention be a kind of grinding liquid, be used for baseplate material grinding processing, and Containing alcohol system solvent and ether system solvent, total content of alcohol system solvent and ether system solvent in all solvents of grinding liquid is 95 mass % or more, 100 mass % hereinafter, ether system solvent relative to alcohol system solvent mass ratio be 1 times or more, 5 Times or less.
The grinding liquid contains alcohol system solvent and ether system solvent, by all solvents of grinding liquid alcohol system solvent and Total content of ether system solvent is set as in the range, and the mass ratio by ether system solvent relative to alcohol system solvent is set For in the range.By being set as molten made of the ether system solvent in alcohol system solvent added with specified amount as described above Matchmaker, the grinding liquid can reduce the density of solvent while the viscosity for inhibiting solvent entirety reduces.Pass through the viscous of the solvent Degree is reduced and is inhibited, and the grinding liquid also ensures that the dispersibility of abrasive grains when containing abrasive grains.In addition, grinding clast Density is usually big compared with the density of solvent, and therefore, the grinding liquid can be increased by reducing the density of solvent as described above The density contrast of solvent and grinding clast.The grinding liquid passes through the density contrast for increasing solvent and grinding clast as described above, The even relatively small grinding clast of relatively light substance, i.e. partial size, can also be easy to carry out point by centrifuge separation From.Therefore, by the grinding liquid, can the dispersibility when inhibiting containing abrasive grains make the recycling of centrifuge separation while reduce Efficiency is relatively high.
The viscosity of ether system solvent at 25 DEG C be lower than alcohol system solvent viscosity, and ether system solvent with it is described The differences in viscosity of alcohol system solvent is preferably 15mPas or more, 20mPas or less.Although the easness of centrifuge separation is with solvent Viscosity decline and improves, if but solvent viscosity decline, abrasive grains when being difficult to ensure in grinding liquid containing abrasive grains Dispersibility.Pass through the low ether of the mixing viscosity alcohol system solvent in the relatively high alcohol system solvent of the dispersibility in abrasive grains It is solvent, and the differences in viscosity of ether system solvent and alcohol system solvent is set as in the range, it can be in the dispersibility for ensuring abrasive grains Further promote the recycling by centrifuge separation to grinding clast simultaneously, so that the recovery efficiency of grinding liquid can be improved.
Herein, " ether " refers to the organic compound for the structure (- O-) that tool is connected there are two organic group via oxygen atom.Separately Outside, " alcohol " refers in the compound replaced with hydrogen atom of the hydroxyl (- OH) to aliphatic hydrocarbon except the compound for belonging to ether Compound in addition.
The effect of invention
As described above, grinding liquid of the invention can inhibit containing abrasive grains when dispersibility reduce while Improve the recovery efficiency of centrifuge separation.
Detailed description of the invention
Fig. 1 is the flow chart for indicating the grinding method of baseplate material of an embodiment of the present invention.
Fig. 2 is the block diagram for indicating the composition of well known grinding device.
Fig. 3 is the photo of the state of the grinding liquid before and after the centrifuge separation indicated in embodiment.
Specific embodiment
Hereinafter, detailed description of embodiments of the present invention.
<grinding liquid>
Grinding of the grinding liquid of an embodiment of the present invention for baseplate material is processed, such as fixes the flat of abrasive grains mode The processing of face grinding.The grinding liquid contains alcohol system solvent and ether system solvent.In addition, the grinding liquid, which has, is scattered in the solvent In abrasive grains.
(solvent)
Alcohol system solvent is not particularly limited, such as can be enumerated: ethylene glycol, propylene glycol, butanediol, oleyl alcohol etc..Wherein Preferably viscosity it is relatively low and it is easy to ensure that abrasive grains dispersibility ethylene glycol.Alcohol system solvent can be used alone, It can be used in mixed way two or more.
Ether system solvent is not particularly limited, and can be enumerated: ethylene glycol monomethyl ether, diethylene glycol dimethyl ether, triethylene glycol methyl ether, Glycol isopropyl ether, diethylene glycol isopropyl ether, butyl glycol ether, butyl, triethylene glycol butyl ether, ethylene glycol isobutyl Ether, diethylene glycol isobutyl ether, glycol hexyl ether, diethylene glycol hexyl ether, ethylene glycol -2- ethyl hexyl ether, diethylene glycol -2- ethyl hexyl Ether, ethylene glycol allyl ether, ethylene glycol phenyl ether, diethylene glycol phenyl ether, ethylene glycol phenyl methyl ether, Ethylene Glycol Methyl propylene ether, diethyl two Alcohol metering system ether, triethylene glycol metering system ether, ethylene glycol propyl propylene ether, diethylene glycol propyl propylene ether, ethylene glycol fourth Base propylene ether, diethylene glycol butyl propyleneglycol ether, ethylene glycol phenyl propylene ether etc..It is wherein preferably easily to improve the recycling of grinding liquid The diethylene glycol isobutyl ether of efficiency.Ether system solvent can be used alone, and can also be used in mixed way two or more.
The lower limit of total content of alcohol system solvent and ether system solvent in all solvents of the grinding liquid is 95 matter Measure %, more preferably 97 mass %.If the less than lower limit of total content, has and is difficult to carry out the small grinding clast of partial size Centrifuge separation anxiety.On the other hand, the upper limit of total content is 100 mass %.
Ether system solvent is 1 times, more preferably 2 times relative to the lower limit of the mass ratio of alcohol system solvent.Another party Face, the upper limit of the mass ratio are 5 times, more preferably 4 times.If the less than lower limit of mass ratio, be difficult to by from The heart separates and recovers the anxiety of the small grinding clast of partial size.On the contrary, having point of abrasive grains if the mass ratio is more than the upper limit Dissipate the anxiety of property deficiency.
Herein, to the dispersibility that can ensure that abrasive grains and in grinding liquid containing alcohol system solvent and ether system solvent, together When the reasons why even small grinding clast of partial size can also be by being centrifugated to recycle investigated.The easness of centrifuge separation It can be indicated by sedimentation coefficient s [s] represented by following formula (1).
[number 1]
In the formula (1), d [cm] indicates the diameter for the particle that should be separated, σ [g/cm3] indicate particle density, ρ [g/ cm3] indicate solvent density, η [g/cms] indicate solvent viscosity.
Think that density σ and the partial size of grinding clast are unrelated and approximately fixed, therefore, is learnt, made according to the formula (1) It is that d is small with the reason of being difficult to recycle the small grinding clast of partial size in the case where the grinding liquid that ethylene glycol is for example used as to solvent. In addition, the sedimentation coefficient s can be improved if improving the density of solvent.In addition, can also be improved by reducing the viscosity of solvent The sedimentation coefficient s.It is learnt as described above according to the formula (1), by adjusting the density or viscosity of solvent, partial size is small The recycling of grinding clast will become easy.However, the dispersibility of abrasive grains reduces if reducing the viscosity of solvent, therefore, grind The processing promotion property for cutting liquid reduces.Therefore, in order to make grinding clast recyclability and grinding liquid processing promote property and deposit and into Effort of having gone is studied, and as a result the present inventor et al. is known, adds the ether system solvent of specified amount in alcohol system solvent as grinding The solvent of liquid.That is, the present inventor et al. is known: as shown in table 1, the viscosity of alcohol system solvent and ether system solvent is compared with density Relatively high (viscosity/density value is relatively large), therefore, by the way that total content of alcohol system solvent and ether system solvent is set as institute There are the 50 mass % or more of solvent, sedimentation coefficient s can be improved while the viscosity for inhibiting solvent reduces.
[table 1]
In turn, mass ratio of the present inventor et al. to ether system solvent relative to alcohol system solvent is investigated, and is as a result learnt, When the mass ratio is 1 times less than, it is difficult to by the small grinding clast of centrifuge separation recycling partial size, when the mass ratio is more than 5 Times when, it is difficult to be scattered in abrasive grains in solvent.According to result above, the present inventor et al. is known: by by ether system solvent phase For the mass ratio of alcohol system solvent be set as 1 times or more, 5 times hereinafter, can make grinding clast recyclability and grinding liquid plus Work promotion property is simultaneously deposited.
The lower limit of the viscosity of alcohol system solvent at 25 DEG C is preferably 15mPas, more preferably 20mPas.It is another The upper limit of aspect, the viscosity of alcohol system solvent is preferably 30mPas, more preferably 25mPas.If alcohol system solvent The less than lower limit of viscosity, the then anxiety for thering is the dispersibility of abrasive grains to become inadequate.On the contrary, if the viscosity of alcohol system solvent More than the upper limit, then it is unable to fully improve sedimentation coefficient s and have the anxiety for being difficult to recycle the small grinding clast of partial size.
The lower limit of the viscosity of ether system solvent at 25 DEG C is preferably 3mPas, more preferably 4mPas.Another party The upper limit in face, the viscosity of ether system solvent is preferably 10mPas, more preferably 7mPas.If ether system solvent is viscous The less than lower limit is spent, then the viscosity of solvent entirety is easy to reduce because of ether system solvent, therefore has point for being difficult to ensure abrasive grains Dissipate the anxiety of property.On the contrary, can not sufficiently be improved by ether system solvent if the viscosity of ether system solvent is more than the upper limit Sedimentation coefficient s, to there is the anxiety for being difficult to recycle the small grinding clast of partial size.
The lower limit of the viscosity of solvent entirety at 25 DEG C is preferably 7mPas, more preferably 8mPas.On the other hand, institute The upper limit for stating the viscosity of solvent entirety is preferably 15mPas, more preferably 12mPas.If the viscosity of the solvent entirety is not The full lower limit, the then anxiety for thering is the dispersibility of abrasive grains to become inadequate.On the contrary, if the viscosity of solvent entirety is more than institute The upper limit is stated, then is unable to fully improve sedimentation coefficient s and have the anxiety for being difficult to recycle the small grinding clast of partial size.
The viscosity of ether system solvent at 25 DEG C is lower than the viscosity of alcohol system solvent.By that will glue as described above In the degree alcohol system solvent relatively high lower than the dispersibility that the ether system solvent of alcohol system solvent is added to abrasive grains, it can ensure to grind Further promote the recycling by centrifuge separation to grinding clast while the dispersibility of grain, to improve the recycling effect of grinding liquid Rate.
The lower limit of the differences in viscosity of ether system solvent and alcohol system solvent at 25 DEG C is preferably 15mPas, more preferably For 17mPas.On the other hand, the upper limit of the differences in viscosity is preferably 20mPas, more preferably 19mPas.If described viscous The less than lower limit of degree difference, then can not sufficiently improve sedimentation coefficient s by ether system solvent, to be difficult to recycle partial size small The anxiety of grinding clast.On the contrary, the viscosity of solvent entirety is easy because of ether system solvent if the differences in viscosity is more than the upper limit Reduce, therefore has the anxiety for being difficult to improve sedimentation coefficient s while the dispersibility for ensuring abrasive grains.Furthermore as the ether Be solvent or alcohol system solvent and use mixing there are many solvent and in the case where winner, it is described " ether system solvent and alcohol system solvent Differences in viscosity " refers to the difference of the viscosity of the ether system solvent equalized respectively according to mass ratio and the viscosity of alcohol system solvent.
The upper limit of the density of alcohol system solvent at 20 DEG C is preferably 1.3g/cm3, more preferably 1.2g/cm3.If described The density of alcohol system solvent is more than the upper limit, even if then addition ether system solvent is also unable to fully improve sedimentation coefficient s, thus in distress To recycle the anxiety of the small grinding clast of partial size.On the other hand, the lower limit of the density of alcohol system solvent is not particularly limited, but logical It is often 0.7g/cm3Left and right.
The upper limit of the density of ether system solvent at 20 DEG C is preferably 1.1g/cm3, more preferably 1g/cm3, and then preferably For 0.95g/cm3.If the density of ether system solvent is more than the upper limit, sedimentation can not be sufficiently improved by ether system solvent Coefficient s, to there is the anxiety for being difficult to recycle the small grinding clast of partial size.On the other hand, the lower limit of the density of ether system solvent is simultaneously It is not particularly limited, but usually 0.7g/cm3Left and right.
The upper limit of the density of solvent entirety at 20 DEG C is preferably 1.2g/cm3, more preferably 1.1g/cm3.If described The density of solvent entirety is more than the upper limit, then is unable to fully to improve sedimentation coefficient s and has that be difficult to recycle the small grinding of partial size broken The anxiety of bits.On the other hand, the lower limit of the density of the solvent entirety is not particularly limited, but usually 0.7g/cm3Left and right.
The lower limit of the boiling point of alcohol system solvent is preferably 150 DEG C, and more preferably 180 DEG C.On the other hand, the alcohol system is molten The upper limit of the boiling point of matchmaker is preferably 300 DEG C, and more preferably 250 DEG C.If the less than lower limit of the boiling point of alcohol system solvent, has Solvent frictional heat caused by grinding due to, evaporates the anxiety that the composition to grinding liquid changes.On the contrary, if the alcohol system The boiling point of solvent is more than the upper limit, then has the viscosity of solvent to become excessively high and be difficult to recycle the anxiety of the small grinding clast of partial size.
The lower limit of the boiling point of ether system solvent is preferably 150 DEG C, and more preferably 180 DEG C.On the other hand, the ether system is molten The upper limit of the boiling point of matchmaker is preferably 300 DEG C, and more preferably 250 DEG C.If the less than lower limit of the boiling point of ether system solvent, has Solvent frictional heat caused by grinding due to, evaporates the anxiety that the composition to grinding liquid changes.On the contrary, if the ether system The boiling point of solvent is more than the upper limit, then has the viscosity of solvent to become excessively high and be difficult to recycle the anxiety of the small grinding clast of partial size.
The upper limit of the absolute value of the difference of the boiling point of the boiling point and ether system solvent of alcohol system solvent is preferably 60 DEG C, more preferably It is 30 DEG C.If the absolute value of the difference of the boiling point is more than the upper limit, the solvent that the evaporates due to frictional heat caused by the grinding The difference of amount becomes significant between alcohol system solvent and ether system solvent.Therefore, during the grinding process ether system solvent relative to alcohol system The mass ratio of solvent changes, and has the anxiety of the dispersibility of abrasive grains or the recovery efficiency reduction of grinding liquid.On the other hand, described The lower limit of the absolute value of the difference of boiling point is not particularly limited, and can be 0 DEG C.
(abrasive grains)
Abrasive grains contained in the grinding liquid are not particularly limited, can enumerate alumina lap grain, silica abrasive grain, The various abrasive grains such as cerium oxide abrasive grain, silicon carbide abrasive grains.
The lower limit of the average grain diameter of the abrasive grains is preferably 1 μm, and more preferably 3 μm.On the other hand, the average grain diameter The upper limit be preferably 20 μm, more preferably 15 μm.If the less than lower limit of the average grain diameter of the abrasive grains, is unable to fully Obtain the anxiety of the processing facilitation effect of abrasive grains.On the contrary, having if the average grain diameter of the abrasive grains is more than the upper limit Baseplate material impaired anxiety when processing.Furthermore so-called " average grain diameter ", refers to the volume reference by measurements such as laser diffractometries Cumulative particle sizes distribution curve 50% value (50% partial size, D50).
The lower limit of the content of abrasive grains described in the grinding liquid is preferably 2.5 mass %, more preferably 5 mass %.Separately On the one hand, the upper limit of the content of the abrasive grains is preferably 50 mass %, more preferably 30 mass %.If the abrasive grains contain The less than lower limit is measured, then has the anxiety for the processing facilitation effect for being unable to fully obtain abrasive grains.On the contrary, if the abrasive grains Content is more than the upper limit, then has the anxiety of the service life reduction of grinding pad, the impaired anxiety of baseplate material or abrasive grains in processing Disperse the anxiety become difficult.
(other compositions)
Optionally it can also contain various additives in the grinding liquid.As the additive, raising grinding can be enumerated The dispersing agent of the dispersibility of grain, the grinding rate elevator for promoting grinding rate, the concave-convex smooth agent for reducing surface to be polished, PH is adjusted to the pH regulator of desired value, the pH buffer of variation for inhibiting pH etc..These can be used alone, can also group It closes and uses two or more additives.In addition, the content of additive described in the grinding liquid is not particularly limited, such as can set For 0.0001 mass % or more, 5 mass % or less.
It in addition, the grinding liquid can also be optionally and containing other solvents such as water, but is preferably by the institute in all solvents The total content for stating alcohol system solvent and ether system solvent is set as 100 mass %, is set as the grinding liquid without containing other solvents.If institute It states grinding liquid and contains other solvents, then have and grind the anxiety of reduced performance because of the reduction of the dispersibility of slurry abrasive grains or pass through The anxiety of the recovery efficiency reduction to grinding liquid of centrifuge separation.
<the grinding method of baseplate material>
As shown in Figure 1, specifically including that baseplate material configuration step using the grinding method of the baseplate material of the grinding liquid S1, baseplate material grinding step S2, grinding liquid store up the rapid S3 that do not bother to see me out, grinding clast removal step S4 and grinding liquid and resupply step Rapid S5.
(grinding device)
The grinding method can by well known grinding device, it is for example as shown in Figure 2 it is main include that slot 1, grinding are stayed in storage The grinding device of machine 2, accumulator tank 3 and centrifugal separator 4 carries out.The storage stays slot 1 to store grinding liquid, and being configured to can be to matching It is placed in the baseplate material supply grinding liquid of grinder 2.The grinder 2 is the grinder ground to baseplate material, and can Use grinder well known to single-sided lapping machine or twin grinder etc..The accumulator tank 3 is configured to that the grinder 2 can be recycled Grinding liquid used in grinding to baseplate material.The centrifugal separator 4 is configured to can be to being recycled in the accumulator tank 3 Grinding liquid be centrifuged.In addition, the centrifugal separator 4 is also configured to that the grinding liquid after centrifuge separation storage can be sent to Stay slot 1.
(baseplate material configuration step)
In baseplate material configuration step S1, the baseplate material that should be ground is configured at grinder 2.For example, if Twin grinder, then the fixed abrasive pad on the upper pressing disc of grinder 2, and the baseplate material kept by carrier is held on institute It states between pressing disc.
The baseplate material is not particularly limited, and can be enumerated: compound semiconductors such as glass, sapphire, GaN, SiC etc.. The shape of the baseplate material is not particularly limited as long as being securable to grinder 2, such as can be set as plate.
(baseplate material grinding step)
In baseplate material grinding step S2, rotation while supplying grinding liquid through the grinding pad is to the base Plate material carries out grinding.It is stayed in slot 1 specifically, being stayed on one side to the baseplate material supply storage ground using grinder 2 in storage Grinding liquid makes the platen for being fixed with grinding pad rotate and make a relative move baseplate material with grinding pad, thus to base on one side Plate material carries out grinding.
The grinding liquid enters between grinding pad and baseplate material, and the machined surface of baseplate material is cooling, or passes through institute The abrasive grains contained promote processing.The supply amount of the grinding liquid can suitably determine according to the type or size of baseplate material It is fixed, such as 10ml/min or more, 50ml/min or less can be set as.
(storage of grinding liquid is not bothered to see me out rapid)
It is stored up in the rapid S3 that do not bother to see me out in grinding liquid, the storage of grinding liquid used in the baseplate material grinding step S2 is stayed in recycling In slot 3.The grinding liquid contains grinding clast because having carried out grinding to baseplate material.In addition, usually in the accumulator tank 3 It stores up the grinding liquid stayed to be stirred, so that abrasive grains contained by grinding liquid etc. do not occur to precipitate or agglomerate.
(grinding clast removes step)
It is broken from removal grinding in the grinding liquid stayed is stored up by centrifuge separation in grinding clast removal step S4 Bits.Specifically, regularly or continuously being sent the grinding liquid stayed is stored up in the accumulator tank 3 into centrifugal separator 4, described in Recycling removal grinding clast in grinding liquid.
The centrifugal separator 4 is not particularly limited, and can be selected according to the amount etc. of handled grinding liquid.Wherein, The centrifugal separator of decanter (decanter) type of separating treatment preferably can be steadily carried out in a long time.
The lower limit for the centrifugal force being centrifugated in the grinding clast removal step S4 is preferably 1500G, more preferably 2000G.If the less than lower limit of centrifugal force, there is the anxiety that can not be sufficiently separated the small grinding clast of especially partial size.Separately On the one hand, the upper limit of the centrifugal force is not particularly limited, such as can be set as 5000G.It is more than the upper limit in the centrifugal force In the case where, the price of centrifugal separator 4 is got higher, and has the anxiety of manufacturing equipment increased costs.
Though the time being centrifugated in the grinding clast removal step S4 also depends on capacity or the place of centrifugal separator 4 Reason amount, but the lower limit of the time of the centrifuge separation is preferably 3 minutes, more preferably 5 minutes.On the other hand, the centrifugation point From the upper limit of time be preferably 30 minutes, more preferably 20 minutes.If the time of the centrifuge separation less than lower limit, There is the anxiety that can not be sufficiently separated the small grinding clast of especially partial size.On the contrary, if the time of the centrifuge separation is more than described The upper limit then has the anxiety to the treatment effeciency reduction recycled to grinding liquid.
In the grinding method, the grinding liquid is used due to as grinding liquid, therefore the even small grinding clast of partial size, It can also be recycled by being centrifugated.Therefore, the method other than the centrifuge separations such as UF membrane need not be passed through in the grinding method Carry out the recycling of the small grinding clast of partial size.Therefore, in the grinding method, grinding clast can be eliminated to by centrifuge separation Grinding liquid directly recycled.
Because abrasive grains are also removed with grinding clast together in grinding clast removal step S4, therefore can also be optionally to institute It states in grinding liquid and adds abrasive grains.New abrasive grains can be used in the abrasive grains, can also remove institute in step S4 to grinding clast The abrasive grains and grinding clast further progress of recycling are centrifugated and are recycled, recycled to abrasive grains.
(grinding liquid resupplies step)
It is resupplied in step S5 in grinding liquid, the institute after resupplying grinding clast removal step S4 to the baseplate material State grinding liquid.Specifically, the grinding liquid after staying slot 1 to supply grinding clast removal step S4 to the storage.Make to supply It stays the grinding liquid of slot 1 to stay the grinding liquid for storing up and staying in slot 1 to mix with storage to storage and abrasive grains content etc. is modulated, then in base It is resupplied in plate material grinding step S2 to baseplate material.
<manufacturing method of substrate>
The grinding method can be used, substrate is manufactured by the grinding of baseplate material.Specifically, can be ground by described Cutting method manufactures substrate using grinding pad and grinding liquid and by the plane grinding self-reference substrate material of fixed abrasive grains mode. Be not particularly limited, can be enumerated by the substrate that the manufacturing method of the substrate manufactures: glass substrate, sapphire substrate, Compound semiconductor substrates such as GaN, SiC etc..
<advantage>
The grinding liquid contains alcohol system solvent and ether system solvent, by all solvents of grinding liquid alcohol system solvent and Total content of ether system solvent is set as 95 mass % or more, 100 mass % hereinafter, and by ether system solvent relative to the alcohol It is that the mass ratio of solvent is set as 1 times or more, 5 times or less.By being set as in alcohol system solvent as described above added with regulation Solvent made of the ether system solvent of amount, the grinding liquid can reduce the close of solvent while the viscosity for inhibiting solvent entirety reduces Degree.It is inhibited by the viscosity reduction of the solvent, the grinding liquid also ensures that point of abrasive grains when containing abrasive grains Dissipate property.In addition, the density of grinding clast is usually big compared with the density of solvent, therefore, the grinding liquid can be by as described above Reduce the density of solvent to increase the density contrast of solvent Yu grinding clast.The grinding liquid by increasing solvent as described above With the density contrast of grinding clast, the even relatively small grinding clast of relatively light substance, i.e. partial size, centrifugation can also be passed through It separates and is easy to carry out separation.Therefore, by the grinding liquid, can the dispersibility when inhibiting containing abrasive grains reduce it is same When make centrifuge separation recovery efficiency it is relatively high.
In addition, by using the grinding liquid, the even small grinding clast of partial size, can also lead in the grinding method Centrifuge separation is crossed to separate.Therefore, by using the grinding method, the manufacture to be recycled to solvent can inhibited Make the recovery efficiency of grinding liquid relatively high while the increase in equipment cost or working hour.Therefore, using the grinding method In the manufacturing method of substrate, the manufacturing cost of substrate is relatively low.
[other embodiments]
The present invention is not limited to the embodiments, in addition to the scheme, can also be applied with various changes, improvement Scheme implement.
In the embodiment, the case where grinding liquid containing abrasive grains, is illustrated, but the present invention includes being free of There is the grinding liquid of abrasive grains.In the grinding liquid without containing abrasive grains, the small grinding of partial size can also be recycled by being centrifugated Clast, therefore the recovery efficiency of the grinding liquid is relatively high.
In the embodiment, as grinding method to the method for staying slot to resupply grinding liquid to baseplate material via storage It is illustrated, but not necessarily stays slot via storage, such as directly can also resupply grinding liquid to baseplate material.
Embodiment
Hereinafter, enumerating Examples and Comparative Examples the present invention is described in more detail, but the invention is not by reality below Apply example restriction.
[embodiment 1]
Prepare as the ethylene glycol (ethylene glycol, EG) of alcohol system solvent and as the diethylene glycol of ether system solvent Isobutyl ether (isobutyl diglycol, isoBDG), and by such a way that the content in all solvents respectively becomes 50 mass %, Mixed in such a way that ether system solvent becomes 1 relative to the mass ratio of alcohol system solvent.In the mixed solvent, in grinding liquid In mode mixed aluminium oxides abrasive grains (white alumina WA#1000, average grain diameter be 12 μm) of the content as 5 mass %, To obtain the grinding liquid of embodiment 1.
[2~embodiment of embodiment 4,1~comparative example of comparative example 4]
Make the changes of contents of EG and isoBDG and the mass ratio with ether system solvent relative to alcohol system solvent becomes shown in table 2 The mode of value mixes, and in addition to this, obtains 2~embodiment of embodiment 4 and 1~comparative example of comparative example 4 similarly to Example 1 Grinding liquid.
[5~embodiment of embodiment 7]
Ether system solvent is set to butyl (butyl diglycol, BDG), diethylene glycol isopropyl ether (isopropyl diglycol, isoPDG) and triethylene glycol methyl ether (methyl triglycol, MTG), and with ether system solvent Mass ratio relative to alcohol system solvent is mixed as 3 mode, in addition to this, obtains embodiment 5~reality similarly to Example 1 Apply the grinding liquid of example 7.
[grinding condition]
Sapphire substrate is ground using the grinding liquid of the 1~embodiment of embodiment 7 and 1~comparative example of comparative example 4 Mill.The sapphire substrate using diameter is 2 inches, specific gravity 3.97, the face c 3 pieces of sapphire substrates.
Well known twin grinder is used in the grinding.The carrier of twin grinder is set as glass epoxy board, is averaged Thickness is set as 0.4mm.Grinding is in upper platen revolving speed 25rpm, pushes the disk rotating speed 50rpm and sun (SUN) gear rotational speed 8rpm Under conditions of carry out 10 minutes.Grinding pressure is set as 200g/cm2.At this point, supplying the 1~implementation of embodiment with 30ml/min The grinding liquid of example 7 and 1~comparative example of comparative example 4.
[evaluation method]
For part or all of the grinding liquid of the 1~embodiment of embodiment 7 and 1~comparative example of comparative example 4, carry out Grinding liquid after the viscosimetric analysis of grinding liquid, the evaluation and the grinding of dispersibility when being ground to sapphire substrate The evaluation of recyclability.It shows the result in table 2.
<viscosimetric analysis>
For the 1~embodiment of embodiment 7 and 1~comparative example of comparative example 4, each grinding liquid before measuring use is at 25 DEG C Under viscosity.The measurement of the viscosity is carried out to the solvent before mixed grinding grain.Furthermore it is viscous using oscillatory type in measurement Degree meter (" Wei Sikemeite (VISCOMATE) VM-100A " of Yamaichi Electronics Co. Ltd.).
<the dispersibility evaluation of grinding liquid>
In the dispersibility evaluation of grinding liquid, by visual observation come confirm supplied in the grinding grinding liquid with pipeline Interior state, and evaluated using judgement benchmark below.
(the judgement benchmark of dispersibility evaluation)
A: not observing that abrasive grains are detained in pipeline, and the dispersibility of abrasive grains is excellent.
B: slightly observe that abrasive grains are detained in pipeline, but the favorable dispersibility of abrasive grains.
C: observe that abrasive grains are detained in pipeline, the bad dispersibility of abrasive grains.
<recyclability of grinding liquid is evaluated>
By separating and recovering grinding clast in each grinding liquid used in centrifuge separation self-grind, to be eliminated The grinding liquid of grinding clast.The centrifuge separation is that (Kubo field makes limited liability company of institute using platform mo(u)ld top half multi rack centrifuge " 8420 " of manufacture) it carries out.
The photograph of grinding liquid of the grinding liquid of comparative example 1 after before centrifuge separation and centrifuge separation is shown in Fig. 3 Piece.In Fig. 3, (1) is the grinding liquid before being centrifugated, and (2) are after carrying out centrifuge separation in 10 minutes with the centrifugal force of 210G Grinding liquid, (3) be the grinding liquid carried out after centrifuge separation in 10 minutes with the centrifugal force of 2280G, (4) be with 2280G from Mental and physical efforts carry out the grinding liquid after centrifuge separation in 20 minutes.The recovery efficiency being centrifuged as described above has centrifugal force Bigger and centrifuge separation time more long then higher tendency, but in the evaluation of the recyclability of grinding liquid, consider centrifugal separator Performance and treatment effeciency, with the centrifugal force of 1500G carry out 10 minutes, 20 minutes, centrifuge separation in 50 minutes to be to be evaluated.
The recyclability of grinding liquid be by visual observation come confirm the grinding liquid after eliminating grinding clast transparency and benefit It is evaluated with judgement benchmark below.Furthermore the case where transparency that will have 10cm or more, is judged as transparency height.Example Such as, it is judged as transparency height in the case where (3) and (4) in Fig. 3.
(the judgement benchmark of recyclability evaluation)
A: the high grinding liquid of transparency was obtained by centrifuge separation below in 10 minutes, recyclability is excellent.
B: by obtaining the high grinding liquid of transparency more than 10 minutes and for centrifuge separation below in 30 minutes, recyclability is good It is good.
C: the high grinding liquid of transparency can not still be obtained by the centrifuge separation more than 30 minutes, recyclability is poor.
[table 2]
In table 2, the "-" in the mass ratio on " alcohol/ether " column refers to because any one of alcohol system solvent or ether system solvent are 0 therefore nothing The situation of legal justice.
According to table 2, the grinding liquid and the grinding liquid phase of comparative example 1, comparative example 2 of 1~embodiment of embodiment 7 are than dispersibility Equal extent and recyclability is excellent.In addition, the grinding liquid phase of the grinding liquid of 1~embodiment of embodiment 7 and comparative example 3, comparative example 4 Than recyclability be equal extent and dispersibility is excellent.In contrast, the grinding liquid of comparative example 1, comparative example 2 is because only having alcohol system molten The mass ratio less than 1 of matchmaker or ether system solvent relative to alcohol system solvent, therefore, it is considered that the viscosity of solvent entirety is high, recyclability is poor.Separately Outside, the grinding liquid of comparative example 3, comparative example 4 is because only super relative to the mass ratio of alcohol system solvent with ether system solvent or ether system solvent 5 are crossed, therefore, it is considered that the viscosity of solvent entirety is low, bad dispersibility.
It learns according to the above, the grinding liquid is by by the quality described in ether system solvent relative to alcohol system solvent Than be set as 1 times or more, 5 times hereinafter, can inhibit abrasive grains dispersibility reduce while improve centrifuge separation recovery efficiency.
Further in detail from the point of view of, according to ether system solvent be isoBDG 1~embodiment of embodiment 4 comparison, embodiment 2, The grinding liquid phase of the grinding liquid of embodiment 3 and embodiment 1 is equal extent than dispersibility and recyclability is excellent.In addition, embodiment 2, the grinding liquid phase of the grinding liquid of embodiment 3 and embodiment 4 is equal extent than recyclability and dispersibility is excellent.In above Hold and learn, the grinding liquid is by being set as 2 times or more, 4 times for the mass ratio described in ether system solvent relative to alcohol system solvent Hereinafter, can further improve dispersibility and recyclability.
<evaluation of the average grain diameter interdependence and content interdependence of abrasive grains>
[embodiment 8]
In order to evaluate average grain diameter influence caused by dispersibility and recyclability of abrasive grains, will make an addition in mixed solvent Alumina lap grain to be set as average grain diameter be 7 μm of alumina lap grain (white alumina WA#2000), in addition to this, with Embodiment 2 similarly obtains the grinding liquid of embodiment 8.
[9~embodiment of embodiment 11]
In order to evaluate content influence caused by dispersibility and recyclability of abrasive grains, the oxygen that will be made an addition in mixed solvent The content for changing aluminium abrasive grains is set as content shown in table 3, in addition to this, obtains embodiment 9~implementation similarly to Example 2 The grinding liquid of example 11.
[evaluation]
For 8~embodiment of embodiment 11, the dispersibility and recyclability of grinding liquid are evaluated.It shows the result in table 3.
[table 3]
According to the result of table 3, even if making the average grain diameter and changes of contents of abrasive grains, caused by dispersibility and recyclability Influence is also small, and the dispersibility and recyclability and embodiment 2 of 8~embodiment of embodiment 11 are equal extent.According to the above and Learn, average grain diameter and content regardless of abrasive grains, the grinding liquid by by described in ether system solvent relative to alcohol system The mass ratio of solvent is set as 1 times or more, 5 times and divides hereinafter, centrifugation can be improved while the dispersibility of inhibition abrasive grains reduces From recovery efficiency.
Industrial availability
As described above, grinding liquid of the invention can inhibit containing abrasive grains when dispersibility reduce while Improve the recovery efficiency of centrifuge separation.
The explanation of symbol
1: slot is stayed in storage
2: grinder
3: accumulator tank
4: centrifugal separator

Claims (2)

1. a kind of grinding liquid is used for the grinding processing of baseplate material, and
Containing alcohol system solvent and ether system solvent,
Total content of alcohol system solvent and ether system solvent in all solvents of grinding liquid is 95 mass % or more, 100 matter Measure % hereinafter,
Ether system solvent is 1 times or more, 5 times or less relative to the mass ratio of alcohol system solvent.
2. grinding liquid according to claim 1, wherein
The viscosity of ether system solvent at 25 DEG C is lower than the viscosity of alcohol system solvent,
Ether system solvent is 15mPas or more, 20mPas or less with the differences in viscosity at 25 DEG C of alcohol system solvent.
CN201780033332.1A 2016-07-22 2017-06-30 Grinding fluid Active CN109312212B (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2016-144915 2016-07-22
JP2016144915A JP2018012821A (en) 2016-07-22 2016-07-22 Grinding liquid
PCT/JP2017/024172 WO2018016297A1 (en) 2016-07-22 2017-06-30 Grinding fluid

Publications (2)

Publication Number Publication Date
CN109312212A true CN109312212A (en) 2019-02-05
CN109312212B CN109312212B (en) 2022-01-04

Family

ID=60992210

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201780033332.1A Active CN109312212B (en) 2016-07-22 2017-06-30 Grinding fluid

Country Status (4)

Country Link
JP (1) JP2018012821A (en)
CN (1) CN109312212B (en)
TW (1) TWI737773B (en)
WO (1) WO2018016297A1 (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000198995A (en) * 1998-12-28 2000-07-18 Fujimi Inc Working fluid for cutting
JP2006111728A (en) * 2004-10-14 2006-04-27 Palace Chemical Co Ltd Wire saw cutting oil
CN104334675A (en) * 2012-05-22 2015-02-04 日立化成株式会社 Slurry, polishing-solution set, polishing solution, substrate polishing method, and substrate

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010221337A (en) * 2009-03-24 2010-10-07 Ngk Insulators Ltd Method for recycling used grinding fluid
CN102234595A (en) * 2010-04-28 2011-11-09 云南中科鑫圆晶体材料有限公司 Organic matter cleaning fluid for precisely polished wafer
US8828262B2 (en) * 2010-05-06 2014-09-09 Lawrence Livemore National Security, Llc Method and system for polishing materials using a nonaqueous magnetorheological fluid
US20120053276A1 (en) * 2010-08-31 2012-03-01 Brilliant Coatings, Inc. Surface polish and wear coating

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000198995A (en) * 1998-12-28 2000-07-18 Fujimi Inc Working fluid for cutting
JP2006111728A (en) * 2004-10-14 2006-04-27 Palace Chemical Co Ltd Wire saw cutting oil
CN104334675A (en) * 2012-05-22 2015-02-04 日立化成株式会社 Slurry, polishing-solution set, polishing solution, substrate polishing method, and substrate

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
冯春宇等: "《固液分离原理与工业水处理装置》", 31 January 2017, 西安:西安电子科技大学出版社 *

Also Published As

Publication number Publication date
CN109312212B (en) 2022-01-04
TWI737773B (en) 2021-09-01
WO2018016297A1 (en) 2018-01-25
TW201803953A (en) 2018-02-01
JP2018012821A (en) 2018-01-25

Similar Documents

Publication Publication Date Title
CN1137231C (en) Abrasive thick liquid and preparation method thereof
CN1282226C (en) Cerium oxide abrasive and method of abrading substrates
CN102189489B (en) Method for recycling cerium oxide abrasive
CN101909816B (en) Polishing slurry, process for producing same, method of polishing, and process for producing glass substrate for magnetic disk
CN101831244A (en) High-precision alumina polishing solution and preparation method thereof
CN1300277C (en) Abrasive material
WO2013125441A1 (en) Abrasive, abrasive set, and method for abrading substrate
JPWO2013125445A1 (en) Abrasive, abrasive set, and substrate polishing method
RU2620836C2 (en) Polishing composition
CN1288920A (en) Polishing composition
EP2406038A2 (en) Abrasive articles including fused zirconia alumina grain having an improved shape
JP2018104711A (en) Production method of cerium salt, cerium oxide and cerium-based polishing agent
CN1422922A (en) Polishing composition of magnetic disk substrate and polishing method using said composition
CN1826684A (en) Method for polishing wafer
CN111548737A (en) Diamond grinding fluid and preparation method thereof
WO2011058929A1 (en) Water-soluble cutting solution for fixed abrasive wire saw, method for cutting ingot using same, method for recycling the solution, and wafer produced by cutting
CN106829954A (en) A kind of preparation method of the nano-diamond micro mist of narrow size distribution
CN108017998A (en) A kind of preparation method of CMP planarization liquid
CN109312212A (en) Grinding liquid
KR20220071187A (en) polishing composition
CN104974714A (en) Polishing composition and method for polishing substrate using the same
CN114958302B (en) Efficient grinding fluid and preparation method and application thereof
CN108367410A (en) The regeneration method of grinding-material slurry
CN102559059A (en) Chemical-mechanical polishing liquid
JP2017119738A (en) Polishing liquid composition for sapphire plate nonpolar surface

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant