CN102229113B - Method for recovering sapphire powder - Google Patents
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- CN102229113B CN102229113B CN 201110151101 CN201110151101A CN102229113B CN 102229113 B CN102229113 B CN 102229113B CN 201110151101 CN201110151101 CN 201110151101 CN 201110151101 A CN201110151101 A CN 201110151101A CN 102229113 B CN102229113 B CN 102229113B
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Abstract
The invention discloses a method for recovering sapphire powder formed by ingot processing, which comprises the following steps of: (1) mixing the sapphire powder and a dispersed medium to form dispersed suspension; (2) performing solid-liquid separation on the dispersed suspension to obtain dispersed sapphire powder, and drying the dispersed sapphire powder to obtain dry and dispersed sapphire powder; and (3) performing at least one of electric separation and magnetic separation on the dry and dispersed sapphire powder and separating to obtain the sapphire powder and impurity powder containing diamond powder. By the method, the sapphire powder can be effectively recovered.
Description
Technical field
The present invention relates to semiconductor applications, especially relate to the recovery method of processing formed sapphire powder for crystal ingot.
Background technology
Sapphire has good thermal conductance, fabulous electrical characteristic and dielectric property, and translucidus can be strong, and rub resistance, corrosion-resistant, chemical property are stable, and its hardness reaches 9 grades of Mohs, is only second to diamond, fusing point is higher than 2000 degrees centigrade, at high temperature still has fabulous stability.So sapphire is widely used in industry, national defence, scientific research, field such as civilian.For example during light emitting diode (LED), need cut into wafer to the sapphire crystal ingot, and in the process of cutting, material unaccounted-for (MUF) is very big for the preparation of semiconductor element.If adopt diamond fretsaw to cut, in slicing slurry, also have the diamond dust of a small amount of costliness, these diamond dusts also can slattern along with the discarded of slicing slurry.Also there is not suitable sapphire powder to reclaim technology at semiconductor applications at present.
Summary of the invention
For this reason, one object of the present invention be to propose a kind of organic efficiency high be used for the recovery method that crystal ingot is processed formed sapphire powder.
The cutting that diamond fretsaw is used for the sapphire crystal ingot is high volume applications to some extent just recently, sapphire powder in the slicing slurry that produces during therefore to diamond wire saw cuts sapphire crystal ingot and the recovery of bortz powder do not have mature technique as yet, need suitable sapphire powder and the bortz powder recovery technology of brand-new exploitation.The present invention is based on that inventor's following discovery carries out: when utilizing diamond fretsaw cutting sapphire crystal ingot, the sapphire powder that forms is generally very tiny, most of tens of to hundreds of nanometer scale, these tiny powder itself are very easy to reunite, and also are easy to reunite together with diamond dust.Thereby, in order to develop effective sapphire powder recovery technology, it is highly important that at first to need to solve how the abundant dispersion of the powder (containing sapphire powder and diamond dust) of these reunions is also further obtained high-purity sapphire powder and diamond dust thus.The applicant finds: the artificial bortz powder of general use in diamond fretsaw, synthesizing of synthetic diamond, be raw material with the carbon element, alloy is catalyst, its crystals often contains catalyst alloy inclusion enclave such as Co, Ni, the Fe etc. of some, make diamond have certain magnetic, and the sapphire powder does not have magnetic.Thus, can separate with diamond dust the sapphire powder by magnetic separation.In addition, the applicant further finds: in the process that the sapphire crystal ingot is cut, and the coming off of the metal dust that invariably accompanies when diamond dust comes off, and most diamond dust and metal dust bonding state; In addition; before the plating of diamond fretsaw, can adopt the diamond particles surface metalation to handle usually, namely at diamond particles surface plating skim metal; the electroplating technology of diamond fretsaw is carried out smoothly, and surface metalation is handled and to be made diamond particles become conduction.Therefore, can carry out sorting to the sapphire powder that contains diamond dust by applying electric field or magnetic field, can obtain sapphire powder and the impurity that contains diamond dust through sorting thus.
Process the recovery method of formed sapphire powder according to a kind of of the embodiment of first aspect present invention for crystal ingot, it is characterized in that may further comprise the steps: mix described sapphire powder (1) with decentralized medium, form dispersion suspension liquid; (2) described dispersion suspension liquid is carried out Separation of Solid and Liquid and obtain sapphire powder through disperseing, and carry out drying with described through the sapphire powder that disperses, obtain sapphire powder dry and that disperse; And (3) be selected from least a processing of electric separation and magnetic separation to the sapphire powder of described drying and dispersion, to separate the impurity powder that obtains the sapphire powder and contain diamond dust.
Can process formed sapphire powder to crystal ingot effectively by the above-mentioned recovery method of processing formed sapphire powder for crystal ingot reclaims, the sapphire powder is separated with other materials that wherein contain, improved the purity of the sapphire powder that reclaims.
According to embodiments of the invention, the recovery method of processing formed sapphire powder for crystal ingot can also have following additional technical feature:
According to one embodiment of present invention, described sapphire powder is to sapphire crystal ingot cutting processing gained by diamond fretsaw.
According to one embodiment of present invention, described decentralized medium is be selected from water, ethanol, diethanol amine, isopropyl alcohol, oxolane, acetone, dimethyl sulfoxide (DMSO) at least a.
According to one embodiment of present invention, when described decentralized medium was water, it further contained the polyacrylic dispersant.
According to one embodiment of present invention, described polyacrylic dispersant is ammonium polyacrylate.
According to one embodiment of present invention, in the described step (1) with described sapphire powder with carry out ultrasonic agitation or mechanical agitation after described decentralized medium mixes.
According to one embodiment of present invention, before described sapphire powder and decentralized medium mix or described dispersion suspension solid and liquid separate before or described Separation of Solid and Liquid after and before described sapphire powder through dispersion is carried out drying, using flotation medium that described sapphire powder is carried out flotation handles, to separate the particle that the density that is comprised in the described sapphire powder is lower than the sapphire powder, wherein, the density of described flotation medium is 1-3.9g/cm
3
According to one embodiment of present invention, further comprise: to the described sapphire powder that obtains through electric separation or magnetic separation wash, drying, obtain dry sapphire powder.
According to one embodiment of present invention, the described process that the sapphire powder of described process electric separation or magnetic separation is washed may further comprise the steps: at first, described sapphire powder through electric separation and/or magnetic separation is carried out pickling, removing the metal impurities in the sapphire powder, and obtain containing the pickle of sapphire powder; Then, the described pickle that contains the sapphire powder is carried out Separation of Solid and Liquid, separate pickle and through the sapphire powder of overpickling; At last, described sapphire powder through overpickling is washed, to remove the acid solution of sapphire powder remained on surface, wherein, described pickle is one or more in the aqueous solution of mixed liquor of the mixed liquor, sulfuric acid and the hydrogen peroxide that are selected from hydrochloric acid, sulfuric acid, nitric acid, hydrochloric acid and hydrogen peroxide.
According to one embodiment of present invention, further comprise: to electric separation and/or the resulting impurity powder of magnetic separation wash, drying, to obtain diamond dust.
According to one embodiment of present invention, further comprise: the described impurity powder that contains bortz powder is selected from least a sorting of electric separation and magnetic separation, to be further purified described diamond dust.
According to one embodiment of present invention, described dispersion suspension liquid is being carried out after Separation of Solid and Liquid obtains through the sapphire powder that disperses, wash through the sapphire powder that disperses described, dry, obtain dry sapphire powder, and the sapphire powder of described drying and dispersion is selected from least a sorting of magnetic separation and electric separation, to separate the impurity powder that obtains the sapphire powder and contain diamond dust.
According to one embodiment of present invention, described dispersion suspension liquid is being carried out after Separation of Solid and Liquid obtains through the sapphire powder that disperses, use pickle to carry out pickling to described through the sapphire powder that disperses, removing the metal impurities in the sapphire powder, and obtain containing the pickle of sapphire powder; The described pickle that contains the sapphire powder is carried out Separation of Solid and Liquid, separate pickle and through the sapphire powder of overpickling; Described sapphire powder through overpickling is washed, to remove the acid solution of sapphire powder remained on surface; To carry out drying through the sapphire powder of washing handles, and described sapphire powder carried out the magnetic separation sorting, to separate the impurity powder that obtains the sapphire powder and contain diamond dust, wherein, described pickle is one or more in the aqueous solution of mixed liquor of the mixed liquor, sulfuric acid and the hydrogen peroxide that are selected from hydrochloric acid, sulfuric acid, nitric acid, hydrochloric acid and hydrogen peroxide.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously and easily understanding becoming the description of embodiment in conjunction with following accompanying drawing, wherein:
Fig. 1 is used for the schematic flow sheet that crystal ingot is processed the recovery method of formed sapphire powder according to an embodiment of the invention;
Fig. 2 is used for the schematic flow sheet that crystal ingot is processed the recovery method of formed sapphire powder in accordance with another embodiment of the present invention;
Fig. 3 is used for the schematic flow sheet that crystal ingot is processed the recovery method of formed sapphire powder in accordance with another embodiment of the present invention;
Fig. 4 is used for the schematic flow sheet that crystal ingot is processed the recovery method of formed sapphire powder in accordance with another embodiment of the present invention;
Fig. 5 is used for the schematic flow sheet that crystal ingot is processed the recovery method of formed sapphire powder in accordance with another embodiment of the present invention;
Fig. 6 is used for the schematic flow sheet that crystal ingot is processed the recovery method of formed sapphire powder in accordance with another embodiment of the present invention; And
Fig. 7 is used for the schematic flow sheet that crystal ingot is processed the recovery method of formed sapphire powder in accordance with another embodiment of the present invention.
The specific embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein identical or similar label is represented identical or similar elements or the element with identical or similar functions from start to finish.Embodiment below by Fig. 1-2 description with reference to the accompanying drawings is exemplary, only is used for explaining the present invention, and can not be interpreted as limitation of the present invention.
A) preparation dispersion suspension liquid
According to embodiments of the invention, when formed sapphire powder reclaims in to the crystal ingot process, at first formed sapphire powder in the crystal ingot process is mixed with decentralized medium, thus, make the sapphire powder can be well dispersed in the decentralized medium, obtain dispersion suspension liquid, and then can solve the reluctant problem of some impurity that the agglomeration owing to the sapphire powder causes.
According to embodiments of the invention, can be applied to the abundant disperse blue jewel of the present invention powder decentralized medium kind and be not particularly limited, can be any not with the known solvent of sapphire powder generation chemical reaction.According to concrete examples more of the present invention, the solvent that adopts is be selected from water, ethanol, diethanol amine, isopropyl alcohol, oxolane, acetone, dimethyl sulfoxide (DMSO) at least a.When these decentralized media mix with the sapphire powder, not can with sapphire powder generation chemical reaction, can guarantee that the sapphire powder that reclaims can be directly used in industrial circle, semiconductor applications for example is such as the LED field.In addition, water, ethanol, diethanol amine, isopropyl alcohol, oxolane, acetone, dimethyl sulfoxide (DMSO) can be used as the solvent of multiple solute, and can be compatible mutually with multiple solute, thereby are convenient to subsequent treatment.According to concrete example of the present invention, can adopt one or more mixture of above-mentioned dispersant as decentralized medium, for example can adopt the ethanol water of 50% (percent by volume) as decentralized medium.According to concrete example of the present invention, when described decentralized medium is water, it can further contain the polyacrylic dispersant, can be by the polyacrylic dispersant adsorption on sapphire powder surface, by the repulsive interaction between the identical charges of sapphire powder surface, further avoid the gathering between the sapphire powder.The concrete example of operable polyacrylic dispersant includes but not limited to ammonium polyacrylate.
According to embodiments of the invention, the sapphire powder that can handle is not particularly limited, and can be by any method crystal ingot to be added resulting sapphire powder in man-hour, especially by diamond fretsaw the sapphire crystal ingot is carried out line cutting processing gained.Can utilize the source of the sapphire powder that method of the present invention handles also to be not particularly limited, can be the slurry that carries out reclaiming from mortar pin groove in the crystal ingot cutting process after the cooling fluid, also can be through dried sapphire powder.Because the powdery waste main component that produces when by diamond fretsaw the sapphire crystal ingot being carried out the line cutting processing is sapphire powder (accounting for about 99.9wt%), the content of bortz powder is lower than one thousandth, thereby utilize existing isolation technics, be difficult to the sapphire powder is separated with bortz powder.In addition, although the content of bortz powder is relatively low, work as the sapphire powder of recovery for the preparation of the sapphire crystal ingot, when cutting again, the bortz powder that comprises can can't carry out owing to hardness causes cutting greatly, causes waste.And utilize recovery method of the present invention, can with impurity in the recovery sapphire powder for example adamantine content be reduced to below 0.01% (weight ratio), even below 0.005%, thereby the sapphire powder of being convenient to reclaim has improved industrial value for the preparation of the sapphire crystal ingot.
In addition, in the sapphire powder, also may exist density to be lower than the impurity of sapphire powder, for example organic particle.Because can relate to organic substance when by diamond fretsaw the sapphire crystal ingot being carried out the line cutting processing for example leads with resin material, bonded adhesives etc., thereby, can produce organic particle in the process of utilizing diamond fretsaw to cut, these impurity can have adverse influence to the separation of sapphire powder and the application behind the recovery sapphire powder.Thereby, with reference to figure 3, according to embodiments of the invention, randomly, with the sapphire powder with before decentralized medium mixes, at first described sapphire powder is carried out flotation and handles, for example adopt density to be lower than the solution of sapphire powder density, the density of sapphire powder is 3.98g/cm
3, thereby the optimum flotation medium is that density is 1-3.9g/cm
3Solution, can remove low-density impurity as much as possible thus.Because the density of sapphire powder is higher than the density of flotation medium, thereby the sapphire powder can accumulate in the bottom of solution as precipitum, and the lower composition of density for example the density of organic particle be usually less than 1g/cm
3, thereby can swim in the upper strata of flotation medium, thus the lower composition of density that is mingled in the sapphire powder can be separated with the sapphire powder, improve the purity of the sapphire powder that reclaims, and then improved the using value of industry.Can be used for the type of flotation medium of the present invention and be not particularly limited, as long as its density is between 1-3.9g/cm
3, and do not react with the sapphire powder and get final product.For example can adopt aqueous sulfuric acid, liquor zinci chloridi, calcium bromide solution, zinc bromide solution, calcium iodide solution, ferric chloride solution, potassium sulfate solution, metatungstic acid ferrous solution as flotation medium.Certainly, it will be appreciated by persons skilled in the art that and use flotation medium that the sapphire powder is carried out the opportunity of above-mentioned processing and be not particularly limited.With reference to figure 2-4, also can use flotation medium that the sapphire powder is carried out flotation before the Separation of Solid and Liquid or before sapphire dried bean noodles after the Separation of Solid and Liquid is dry after carrying out the dispersion of sapphire powder handles, condition and employed flotation medium are ditto described, repeat no more herein.
In addition, according to embodiments of the invention, can dispersion suspension liquid be stirred in that the sapphire powder is mixed with decentralized medium in the process that obtains dispersion suspension liquid, for example adopt ultrasonic agitation or mechanical agitation.By adopting stir process, can improve the degree of scatter of sapphire powder in decentralized medium, the applicant finds to avoid the sapphire powder to reunite in dispersion suspension liquid thus, reduce the granularity of sapphire particle that powder forms, thereby avoided being difficult to remove some and being swept along wherein impurity bortz powder for example owing to the sapphire powder gathers into bulky grain.Because the sapphire powder degree that line cutting obtains is all smaller, be very easy to other particles for example diamond particles etc. reunite together, be difficult to separately.By stir process, for example adopt ultrasonic agitation can avoid the generation of this type of problem.
B) Separation of Solid and Liquid
The sapphire powder is dispersed in the dispersion suspension liquid fully, next can carry out Separation of Solid and Liquid to this dispersion suspension liquid, can obtain the sapphire powder through disperseing thus, avoided like this since other impurity that the gathering of sapphire powder is mingled with to the influence of recovery sapphire powder.Particularly, can carry out Separation of Solid and Liquid by centrifugation to dispersion suspension liquid by centrifuge and obtain sapphire powder through disperseing, also can carry out Separation of Solid and Liquid with the mode of filtering for example press filtration.Next can carry out drying to the sapphire powder through disperseing that separates.Dry means and equipment are not particularly limited, and can adopt vacuum drying method, and other any known method and apparatus.Thus, obtain sapphire powder dry and that disperse.
C) sorting
Further, according to embodiments of the invention, after dispersion suspension liquid carries out Separation of Solid and Liquid, can be selected from least a processing of electric separation and magnetic separation to the sapphire powder of described drying and dispersion, to separate the impurity powder that obtains the sapphire powder and contain bortz powder.Thus, improved the organic efficiency of sapphire powder, and can separate the product that obtains high value.According to embodiments of the invention, the method for separating that can adopt includes but not limited to electric separation and magnetic separation.Electric separation, magnetic selection method and the equipment that can be used for sorting of the present invention are not particularly limited.Can adjust the electric field and the magnetic field intensity that apply when carrying out electric separation and magnetic separation processing, in order to be enough to make the sapphire powder fully to separate with the diamond dust that is mingled in wherein according to the processing sample.Can be any method as known in the art for electric separation method of the present invention and magnetic selection method.On market, also there are many very ripe electric separations or magnetic separation instrument selective.The user can select suitable condition to carry out sorting according to the specification of product according to conditions such as the granularity of the sapphire powder of required separation and diamond dust, quality to obtain through the sapphire powder of sorting and contain the impurity of diamond dust.
Those skilled in the art can be understood that, when enforcement is of the present invention, can pass through the combined treatment of electric separation, magnetic separation, further improve the treatment effect of sapphire powder and diamond dust.Wherein, the order of electric separation, magnetic separation and number of repetition are not particularly limited.According to one embodiment of present invention, the magnet type that applies magnetic field is not particularly limited, and for example includes but not limited to permanent magnet, electromagnet.According to concrete example of the present invention, adopt permanent magnet, for example have ferromagnetic Nd-Fe-B permanent magnet.Thus, can further improve by magnet and promote the effect that wet concentration separates, and can save electric energy, saving cost.
According to embodiments of the invention, the electric separation that can adopt is to be selected from drum electric separation, cell-type electric separation, freely to fall at least a of electric separation, slide carriage formula electric separation, belt-type electric separation, disc type electric separation, shaking table formula electric separation or spiral-flow type electric separation.According to embodiments of the invention, the magnetic separator that can adopt is be selected from belt magnetic separator, drum magnetic separator, roll-type magnetic separator, disk-type magnetic separator, ring type magnetic separator, cage magnetic separator or magnetic-pulley separator at least a, magnetic source wherein can be the permanent magnetism magnetic source, also can be the electromagnetism magnetic source.
D) subsequent treatment
According to embodiments of the invention, can obtain the sapphire powder through super-dry by washing, drying from the sapphire powder through electric separation or magnetic separation acquisition.Particularly, according to instantiation of the present invention, the washing process that can adopt comprises that at first the sapphire powder that obtains through electric separation or magnetic separation is carried out pickling removes metal impurities in the sapphire powder, carry out afterwards the sapphire powder through overpickling is washed, remove the acid solution of sapphire powder remained on surface.With reference to figure 7, according to embodiments of the invention, the washing process that can adopt may further comprise the steps: at first described sapphire powder through electric separation or magnetic separation is carried out pickling, removing the metal impurities in the sapphire powder, and obtain containing the pickle of sapphire powder; Then, the described pickle that contains the sapphire powder is carried out Separation of Solid and Liquid, separate pickle and through the sapphire powder of overpickling; At last, described sapphire powder through overpickling is washed, to remove the acid solution of sapphire powder remained on surface.According to embodiments of the invention, handle the particle diameter of the sapphire powder that obtains afterwards less than 0.1mm through separation, washing, dry step.For example according to embodiments of the invention, the pickle that can adopt is selected from the aqueous solution of mixed liquor of mixed liquor, sulfuric acid and hydrogen peroxide of hydrochloric acid, sulfuric acid, nitric acid, hydrochloric acid and hydrogen peroxide one or more and carries out pickling.Thus, can remove the metal impurities that are attached to sapphire powder surface effectively, and can self not cause damage to the sapphire powder.Be not particularly limited for the method and apparatus that carries out Separation of Solid and Liquid, particularly, can carry out Separation of Solid and Liquid by centrifugation by centrifuge, also can use the mode of filtering.According to embodiments of the invention, dry means and equipment are not particularly limited, and can adopt vacuum drying method, and other any known method and apparatus.Thus, obtain dry and high-purity sapphire powder.
According to embodiments of the invention, be not particularly limited the opportunity of the sapphire powder being carried out carrying out washing treatment.According to a concrete example, dispersion suspension liquid can carried out after Separation of Solid and Liquid obtains through the sapphire powder that disperses, to washing through the sapphire powder that disperses, dry, obtain dry sapphire powder, sapphire powder to described drying and dispersion carries out magnetic separation and/or electric separation then, to separate the impurity powder that obtains the sapphire powder and contain diamond dust.With reference to figure 6, according to concrete example of the present invention, dispersion suspension liquid can be carried out Separation of Solid and Liquid and obtain through after the sapphire powder that disperses, use pickle to carrying out pickling through the sapphire powder that disperses, removing the metal impurities in the sapphire powder, and obtain containing the pickle of sapphire powder; The pickle that will contain the sapphire powder carries out Separation of Solid and Liquid, separates pickle and through the sapphire powder of overpickling; Sapphire powder through overpickling is washed, to remove the acid solution of sapphire powder remained on surface; To carry out drying through the sapphire powder of washing handles, and described sapphire powder carried out sorting process, the preferred magnetic selection method that adopts carries out sorting process, be not particularly limited with the type that separate to obtain the sapphire powder and contain the operable pickle of impurity powder of diamond dust, can be in the aqueous solution of the mixed liquor of the mixed liquor, sulfuric acid and the hydrogen peroxide that are selected from hydrochloric acid, sulfuric acid, nitric acid, hydrochloric acid and hydrogen peroxide one or more.The inventor finds, at the sapphire powder through overpickling, the effect that adopts magnetic selection method to carry out sorting process obviously is better than the effect handled by the electric separation method.
Further, according to embodiments of the invention, can be from obtaining diamond dust through magnetic separation or the resulting impurity powder of electric separation.Because the ratio of diamond dust in raw material sapphire powder is lower, is usually less than one thousandth, thereby separating usually can residual a part of sapphire powder in the diamond dust that obtains.Thus, according to one embodiment of present invention, after the sapphire powder that obtains diamond dust and drying respectively, with reference to figure 5, can carry out further purified treatment to bortz powder by electric separation and/or the magnetic separation means of routine, further to remove the impurity in the diamond dust.In addition, after diamond dust is carried out electric separation or magnetic separation, can isolate highly purified sapphire powder, thereby improve the rate of recovery of sapphire powder.
E) industrial applicibility
According to embodiments of the invention, purity by the resulting final sapphire powder product of method of the present invention has reached more than the 99.99wt%, even reach more than the 99.995wt%, the rate of recovery can reach 50-80%, can reclaim a large amount of sapphire powder thus, and can directly the sapphire powder that reclaims be used for the industry use.According to embodiments of the invention, the particle diameter of the sapphire powder that process separation, washing, dry step obtain after handling is generally the sapphire powder of Nano grade less than 0.1mm.The sapphire powder of these recovery can be used for make to be reused for making the sapphire crystal ingot, be further used for LED substrate, optical window material, wearing face as showing lid etc.
Further, can reclaim by method of the present invention and to obtain highly purified bortz powder, the purity of resulting bortz powder has reached more than the 99.9wt%, the rate of recovery can reach 60-90%, can reclaim a large amount of bortz powders thus, and can directly the bortz powder that reclaims be used for the industry use.According to embodiments of the invention, be generally micron level through the bortz powder that separates, washs, dry step obtains after handling.The bortz powder of these recovery can be used for make diamond fretsaw, or for the preparation of conventional cutting tool.
Concrete example
The concrete example of following basis describes the recovery method of processing formed sapphire powder for crystal ingot of the present invention, and concrete example is not made any restriction to scope of the present invention.
Example 1
The sapphire powder (500 gram) that utilizes diamond fretsaw cutting sapphire crystal ingot to produce is joined in 1 premium on currency (dispersant), and ultrasonic agitation was handled 5 minutes, obtained sapphire powder finely dispersed dispersion suspension liquid therein.Dispersion suspension liquid is filtered, carry out Separation of Solid and Liquid, collect sapphire powder precipitation, and carry out vacuum drying, dried sapphire powder joined carry out electric separation in the electrostatic separator and separate, reclaim sapphire powder and the impurity that contains diamond dust through electric separation, again to the pickling of resulting sapphire powder, drying, obtain high-purity sapphire powder.Reach more than 99.995% through the purity that detects the sapphire powder that reclaims.In addition, with the further electric separation of impurity powder, obtain diamond dust.
Example 2
It is 1.5g/cm that the sapphire powder (500 gram) that utilizes diamond fretsaw cutting sapphire crystal ingot to produce is joined density
3Sulfuric acid solution (flotation medium) in carry out flotation, be recovered in the sapphire powder of solution bottom, join after the washing in 1 liter of 50% ethanolic solution (dispersant), ultrasonic agitation was handled 5 minutes, obtained sapphire powder finely dispersed dispersion suspension liquid therein.With dispersion suspension liquid under 200rpm centrifugal 5 minutes, Separation of Solid and Liquid is carried out in filtration, collect sapphire powder precipitation, collected sapphire powder is carried out pickling, washing processing successively, and carry out vacuum drying, dried sapphire powder joined carry out magnetic separation in the magnetic separator and separate, reclaim through the sapphire powder of magnetic separation and contain the impurity of diamond dust.Reach more than 99.99% through the purity that detects the sapphire powder that reclaims.
Example 3
It is 1.6g/cm that the sapphire powder (500 gram) that utilizes diamond fretsaw cutting sapphire crystal ingot to produce is joined density
3Ferric chloride in aqueous solution (flotation medium) in carry out flotation, be recovered in the sapphire powder of solution bottom, join after the washing in 1 liter of oxolane (dispersant), ultrasonic agitation was handled 5 minutes, obtained sapphire powder finely dispersed dispersion suspension liquid therein.With dispersion suspension liquid under 200rpm centrifugal 5 minutes, carry out Separation of Solid and Liquid, collect sapphire powder precipitation, and carry out vacuum drying, dried sapphire powder joined carry out magnetic separation in the magnetic separator and separate, reclaim through the sapphire powder of magnetic separation and contain the impurity of diamond dust.To the pickling of resulting sapphire powder, drying, obtain high-purity sapphire powder again, reach more than 99.99% through the purity that detects the sapphire powder that reclaims.In addition, with the further magnetic separation of impurity powder, obtain diamond dust.
Example 4
It is 1.6g/cm that the sapphire powder (500 gram) that utilizes diamond fretsaw cutting sapphire crystal ingot to produce is joined density
3Ferric chloride in aqueous solution (flotation medium) in carry out flotation, be recovered in the sapphire powder of solution bottom, join after the washing in 1 liter of oxolane (dispersant), ultrasonic agitation was handled 5 minutes, obtained sapphire powder finely dispersed dispersion suspension liquid therein.With dispersion suspension liquid under 200rpm centrifugal 5 minutes, carry out Separation of Solid and Liquid, collect sapphire powder precipitation, and carry out vacuum drying, dried sapphire powder joined carry out electric separation in the electrostatic separator and separate, reclaim through the sapphire powder of electric separation and contain the impurity of diamond dust.To the pickling of resulting sapphire powder, drying, obtain high-purity sapphire powder again, reach more than 99.995% through the purity that detects the sapphire powder that reclaims.In addition, with the further magnetic separation of impurity powder, obtain diamond dust, further reclaim sapphire powder wherein simultaneously.
Example 5
It is 1.6g/cm that the sapphire powder (500 gram) that utilizes diamond fretsaw cutting sapphire crystal ingot to produce is joined density
3Ferric chloride in aqueous solution (flotation medium) in carry out flotation, be recovered in the sapphire powder of solution bottom, join after the washing in 1 liter of oxolane (dispersant), ultrasonic agitation was handled 5 minutes, obtained sapphire powder finely dispersed dispersion suspension liquid therein.With dispersion suspension liquid under 200rpm centrifugal 5 minutes, carry out Separation of Solid and Liquid, collect sapphire powder precipitation, and carry out vacuum drying, dried sapphire powder joined carry out electric separation in the electrostatic separator and separate, reclaim through the sapphire powder of electric separation and contain the impurity of diamond dust.To carry out magnetic separation through the sapphire powder of electric separation, again to the pickling of resulting sapphire powder, drying, obtain high-purity sapphire powder, be higher than example 4 through the purity that detects the sapphire powder that reclaims.In addition, with the further magnetic separation of impurity powder, obtain diamond dust, further reclaim sapphire powder wherein simultaneously.
In the description of this specification, concrete feature, structure, material or characteristics that the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means in conjunction with this embodiment or example description are contained at least one embodiment of the present invention or the example.In this manual, the schematic statement to above-mentioned term not necessarily refers to identical embodiment or example.And concrete feature, structure, material or the characteristics of description can be with the suitable manner combination in any one or more embodiment or example.
Although illustrated and described embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple variation, modification, replacement and modification to these embodiment under the situation that does not break away from principle of the present invention and aim, scope of the present invention is limited by claim and equivalent thereof.
Claims (11)
1. one kind is used for the recovery method that crystal ingot is processed formed sapphire powder, it is characterized in that, may further comprise the steps:
(1) described sapphire powder is mixed with decentralized medium, form dispersion suspension liquid;
(2) described dispersion suspension liquid is carried out Separation of Solid and Liquid and obtain sapphire powder through disperseing, and carry out drying with described through the sapphire powder that disperses, obtain sapphire powder dry and that disperse; And
(3) the sapphire powder of described drying and dispersion is selected from least a processing of electric separation and magnetic separation, separating the impurity powder that obtains the sapphire powder and contain diamond dust,
Wherein,
Described decentralized medium is be selected from water, ethanol, diethanol amine, isopropyl alcohol, oxolane, acetone, dimethyl sulfoxide (DMSO) at least a,
When described decentralized medium was water, it further contained the polyacrylic dispersant,
Described polyacrylic dispersant is ammonium polyacrylate.
2. recovery method according to claim 1 is characterized in that, described sapphire powder is to sapphire crystal ingot cutting processing gained by diamond fretsaw.
3. recovery method according to claim 1 is characterized in that, in the described step (1) with described sapphire powder with carry out ultrasonic agitation or mechanical agitation after described decentralized medium mixes.
4. recovery method according to claim 1, it is characterized in that, before described sapphire powder and decentralized medium mix or described dispersion suspension solid and liquid separate before or described Separation of Solid and Liquid after and before described sapphire powder through dispersion is carried out drying, using flotation medium that described sapphire powder is carried out flotation handles, to separate the particle that the density that is comprised in the described sapphire powder is lower than the sapphire powder, wherein, the density of described flotation medium is 1-3.9g/cm
3
5. recovery method according to claim 1 is characterized in that, further comprises:
To the described sapphire powder that obtains through electric separation or magnetic separation wash, drying, obtain dry sapphire powder.
6. recovery method according to claim 5 is characterized in that, the described process that the sapphire powder of described process electric separation or magnetic separation is washed may further comprise the steps:
At first, described sapphire powder through electric separation and/or magnetic separation is carried out pickling, removing the metal impurities in the sapphire powder, and obtain containing the pickle of sapphire powder;
Then, the described pickle that contains the sapphire powder is carried out Separation of Solid and Liquid, separate pickle and through the sapphire powder of overpickling;
At last, described sapphire powder through overpickling is washed, with the acid solution of removal sapphire powder remained on surface,
Wherein, described pickle is one or more in the aqueous solution of mixed liquor of the mixed liquor, sulfuric acid and the hydrogen peroxide that are selected from hydrochloric acid, sulfuric acid, nitric acid, hydrochloric acid and hydrogen peroxide.
7. recovery method according to claim 1 is characterized in that,
Wash through the sapphire powder that disperses described after Separation of Solid and Liquid obtains through the sapphire powder that disperses in that described dispersion suspension liquid is carried out, drying obtains dry sapphire powder, and
The sapphire powder of described drying and dispersion is selected from least a sorting of magnetic separation and electric separation, to separate the impurity powder that obtains the sapphire powder and contain diamond dust.
8. recovery method according to claim 7 is characterized in that,
Described dispersion suspension liquid is being carried out use pickle to carry out pickling to described through the sapphire powder that disperses after Separation of Solid and Liquid obtains through the sapphire powder that disperses, removing the metal impurities in the sapphire powder, and obtaining containing the pickle of sapphire powder;
The described pickle that contains the sapphire powder is carried out Separation of Solid and Liquid, separate pickle and through the sapphire powder of overpickling;
Described sapphire powder through overpickling is washed, to remove the acid solution of sapphire powder remained on surface;
To carry out drying through the sapphire powder of washing and handle, and
Described sapphire powder is carried out the magnetic separation sorting, obtains sapphire powder and the impurity powder that contains diamond dust to separate,
Wherein, described pickle is one or more in the aqueous solution of mixed liquor of the mixed liquor, sulfuric acid and the hydrogen peroxide that are selected from hydrochloric acid, sulfuric acid, nitric acid, hydrochloric acid and hydrogen peroxide.
9. recovery method according to claim 7 is characterized in that,
The sapphire powder that described separation is obtained carries out pickling, removing the metal impurities in the sapphire powder, and obtains containing the pickle of sapphire powder;
The described pickle that contains the sapphire powder is carried out Separation of Solid and Liquid, separate pickle and through the sapphire powder of overpickling;
Described sapphire powder through overpickling is washed, to remove the acid solution of sapphire powder remained on surface;
To carry out drying through the sapphire powder of washing and handle,
Wherein, described pickle is one or more in the aqueous solution of mixed liquor of the mixed liquor, sulfuric acid and the hydrogen peroxide that are selected from hydrochloric acid, sulfuric acid, nitric acid, hydrochloric acid and hydrogen peroxide.
10. according to each described recovery method of aforementioned claim, it is characterized in that, further comprise:
To electric separation and/or the resulting impurity powder of magnetic separation wash, drying, to obtain diamond dust.
11. recovery method according to claim 10 is characterized in that, further comprises:
The described impurity powder that contains bortz powder is selected from least a sorting of electric separation and magnetic separation, to be further purified described diamond dust.
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| CN 201110151101 CN102229113B (en) | 2011-06-07 | 2011-06-07 | Method for recovering sapphire powder |
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| CN102718243A (en) * | 2012-01-13 | 2012-10-10 | 上海赢奔晶体科技有限公司 | Method for purifying waste sapphire crystals |
| CN104131354A (en) * | 2013-05-02 | 2014-11-05 | 周黎 | Recycling method of residual crystal scrap after processing of sapphire crystal |
| CN103624690B (en) * | 2013-11-23 | 2016-01-13 | 广东创生不锈钢制品有限公司 | A kind of regulation method of stainless steel polishing dust |
| CN105856073B (en) * | 2016-06-20 | 2017-08-22 | 福建晶安光电有限公司 | A kind of sapphire polishes the recovery method of waste liquid |
| CN106241794B (en) * | 2016-08-01 | 2018-02-02 | 北京保利世达科技有限公司 | It is a kind of that the method and product that diamond is reclaimed in slug are ground from sapphire |
| CN106006629B (en) * | 2016-08-01 | 2017-11-14 | 北京保利世达科技有限公司 | A kind of sapphire method and product that diamond is reclaimed in grinding slug |
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| JP2941749B2 (en) * | 1997-08-04 | 1999-08-30 | 三倉物産株式会社 | Method for treating wafer polishing waste liquid and sintered body mainly containing recovered abrasive |
| JP2008115040A (en) * | 2006-11-02 | 2008-05-22 | Sharp Corp | Silicon reclamation apparatus and method of reclaiming silicon |
| CN100528488C (en) * | 2007-09-11 | 2009-08-19 | 西安交通大学 | Method for recycling silica powder and carborundum powder from cut waste mortar |
| CN101879481A (en) * | 2009-05-05 | 2010-11-10 | 上海奇谋能源技术开发有限公司 | Method for recovering silicon powder from silicon crystal cutting fluid by using electrostatic separation |
| CN101823716A (en) * | 2010-03-09 | 2010-09-08 | 江西赛维Ldk太阳能高科技有限公司 | Method for separating silica powder and impurities in mixture |
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