CN1994972A - Production method of high purity cured charcoal felt silicon crystal growth oven - Google Patents
Production method of high purity cured charcoal felt silicon crystal growth oven Download PDFInfo
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- CN1994972A CN1994972A CN 200610136811 CN200610136811A CN1994972A CN 1994972 A CN1994972 A CN 1994972A CN 200610136811 CN200610136811 CN 200610136811 CN 200610136811 A CN200610136811 A CN 200610136811A CN 1994972 A CN1994972 A CN 1994972A
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Abstract
The invention discloses a making method of high-purity solidified carbon cushion in the silicon crystal growing stove, which is characterized by the following: selecting flexible cushion with low metal impurity as blank material; disposing under high temperature to form graphite cushion; using graphite cushion as blank; solidifying the blank to shape with evenly permeable hardener; carbonizing the blank; proceeding chemical gas-phase deposition for blank; cutting part of element surface mechanically; disposing blank under high temperature; removing metal impurity and volatile substance; coating the working piece; strengthening the element surface; improving the corrosion resistant of blank surface.
Description
Technical field
The present invention relates to the preparation method of a kind of silicon crystal growth oven with the insulation component, exactly is the production method of high purity cured charcoal felt that a kind of silicon crystal growth oven is used.
Background technology
The working temperature of silicon crystal growth oven is more than 1500 ℃.The thermal field system of silicon crystal stove becomes crystal bar spare, very big to the i.e. influence to the use properties of silicon chip of the integrity of semi-conductor silicon crystal to silicon crystal.Therefore, the material of various component is selected and use in thermal field system design, the thermal field, is subjected to paying attention to widely.Since the beginning of the nineties, just the someone proposes to make the thermal field part with carbon-carbon composite.The issues of purification of making the silicon crystal growth oven part of carbon-carbon composite has been introduced by Germany SGL carbon composite company in the US5800924 United States Patent (USP); Japan KOMATSU electronic metal Materials Co., Ltd, Japan's carbon element and French SNECMA Moteurs company propose to make with carbon-carbon composite the various technical schemes of the crucible of silicon crystal growth oven respectively in the United States Patent (USP) of US5871582, US6136094, US6877952; Japan's carbon element public affairs can have been introduced the analog reslt of the thickness of crucible surface RESEARCH OF PYROCARBON to the influence in the work-ing life of crucible in the US6399203 United States Patent (USP); In the US6455160 of Japan's carbon element United States Patent (USP), introduced the purification process process.
Carbon-carbon composite is made the solution of silicon crystal growth oven lagging material, insulation component and is not seen relevant discussion.At the pulled crystal device of usefulness,, extensively adopt the soft charcoal felt to be wrapped on the interior heat-preservation cylinder that graphite does for heat preservation member cylindraceous; To the guide shell of taper, then adopt graphite taper inner core and graphite taper urceolus therebetween one deck charcoal felt as heat preservation member; For the flat-type part, also be to do support with graphite cake, insert the felt interlayer body between two graphite cakes, reach heat preservation effect.The weak point of doing like this: 1) owing to have many impurity to evaporate in the polysilicon of fusing, on the well heater of these volatile matter accumulation in furnace roof, furnace bottom, stove, the graphite sleeve, also can accumulation on insulation soft charcoal felt.Accumulation can be cleaned out after each blowing out substantially at closely knit object such as the impurity on the graphite; Soft charcoal felt itself is just as a suction cleaner, and the impurity of accumulation on the soft charcoal felt can't be cleaned out; Residual pollutent may pollute the polysilicon molten mass at any time, causes brilliant difficulty; 2) adopted many graphite piece as supporter in the hot system, graphite is crisp, will consider its processing technology during design, proof strength, and the wall thickness of graphite piece can not be done too thinly, so weight is bigger; Tie up the space; The thermal field part that fragility is big and heavy is given to manipulate and is brought inconvenience.3) graphite is the good conductor of heat, and the ratio that graphite piece accounts in the thermal field system is big, and the heat that body of heater is derived is more, has reduced the heat-insulating property of system.
Summary of the invention
Purpose of the present invention is intended to overcome existing thermal field technology of preparing deficiency, for silicon crystal growth oven provides a kind of high insulating effect, production efficiency height, production method of high purity cured charcoal felt that foreign matter content is low.
For achieving the above object, the present invention has adopted following technical scheme:
Select the very low soft felt body of metals content impurity to make blank of material, the high temperature pre-treatment makes it to become the graphite felt body; By means of mould, mold, make base substrate with graphite felt system through pyroprocessing; Need evenly to infiltrate an amount of solidifying agent in the base substrate; Preformed base substrate is cured typing to be handled: handle doing charing through the base substrate of solidification treatment again; The base substrate of the first one-step forming vacuum chemistry gaseous phase deposition stove of packing into is carried out the chemical gas phase pre-deposition; Part to part needs the surface of machining to carry out mechanical cutting processing; At this moment part base substrate need be made pyroprocessing, removes metallic impurity and volatile matter; Pyroprocessing need be taken measures, and prevents the part thermal distortion; Machined surface to the part after coming out of the stove need carry out the top coat processing: again part is done chemical vapour deposition, carry out surface Hardening Treatment, improve the billet surface corrosion resistance.
Blank of material of the present invention adopts polypropylene cyanogen (PAN) felt body, pretreatment stage, and thermal treatment temp is at 1800 ℃ to 2300 ℃, preferably at 2100 ℃-2300 ℃:
The solidifying agent that the present invention uses is carbon-hydrogen-oxygen monomer-polymer, realizes the curing of base substrate under certain heating cycle.Curing process is:
The technology that charing of the present invention is handled is:
Pyroprocessing after the machining of the present invention, the temperature of processing are at 1800 ℃-2300 ℃, and high-temperature holding time is 2 hours to 5 hours.
The machining surface of base substrate of the present invention will carry out top coat.The prescription of top coat mainly by binding agent, contain thing admittedly and form, binding agent is to contain silicon sol-gel; Admittedly contain thing is carbon fiber, high purity graphite powder etc., is 10: 1 to 2: 1 admittedly contain the weight ratio of thing and certain density binder solution.
Adopt solid-state charcoal felt to make lagging material, part can be regulated and control from the surface to core density, for example part is made the gradient material that table portion density is low, heart portion density is high along thickness direction; Inner low density guarantees heat-insulating property, and outside high-density layer guarantees the geometrical dimension and the shape of part, guarantees intensity, the rigidity of part.For guaranteeing the shape-holding property and the corrosion stability of part, can be at the top coat or the stickup carbon cloth of part.With the heat-preservation cylinder that this material is made, insulation base plate, insulation cover plate, guide shell etc. can support that single part can be finished two functions without graphite piece, can satisfy the service requirements of silicon crystal stove.Improved heat insulation effect, energy-conservation; Reduce the thermal inertia of system, shortened intensification, the temperature-fall period of crystal pulling.Alleviate the component weight of hot system significantly, reduced working strength of workers; Improve intensity, the rigidity of system zero parts, improved the work reliability and the serviceability of system; Saved the space, can only adorn in the equipment of 18 inches systems originally, can adorn the hot system of 19 inches even 20 inches, effectively enlarged the throughput of equipment, improved quality product and improved production efficiency; Use cured charcoal felt, in the stove, especially the pollutent cleaning on the lagging material has improved workman's labor condition easily.
Description of drawings
Fig. 1 is the process flow sheet of high purity cured charcoal felt silicon crystal growth oven manufacture method of the present invention.
Embodiment
As shown in Figure 1, the technical process of high purity cured charcoal felt silicon crystal growth oven manufacture method is: select the very low soft graphite felt body of metals content impurity to make blank of material, high temperature pre-treatment graphite felt body; According to user's drawing, design suitable fixture clamping fixture, with felt body, make base substrate, and make an amount of solidifying agent of infiltration in the base substrate through high-temperature heat treatment; By certain curing process, the preliminary shaping base substrate of an amount of solidifying agent has been infiltrated in heating, makes the felt body solidifying and setting that is impregnated with solidifying agent; The base substrate that solidified is done charing to be handled; The base substrate of the moulding vacuum chemistry gaseous phase deposition stove of packing into carries out the chemical gas phase pre-deposition; Some part of base substrate need be carried out mechanical cutting processing to guarantee the shape and size of part; The pyroprocessing base substrate is removed metallic impurity and volatile matter; Also need carry out top coat through the surface of mechanical cutting processing on the part that pyroprocessing is crossed; After treating that coating is dried, part is done chemical vapour deposition, improve billet surface corrosion resistance and part integral rigidity.The high purity cured charcoal felt component that meet the crystal pulling requirement have been made like this.
1, raw-material selection
The metals content impurity control of cured charcoal felt must be from the source.Adopt polypropylene cyanogen (PAN) charcoal felt on the market, need carry out just entering the cured charcoal felt production process after the pyroprocessing.The temperature of handling and the time of soak are all with the purity of charcoal felt itself, relevant with the treatment capacity of charcoal felt.General treatment temp is good at 1800 ℃ to 2300 ℃ with 2100 ℃ to 2300 ℃.
2, the prescription of cured charcoal felt solidifying agent and use
Adopt charcoal felt,, make body formation by means of mould, mold through pyroprocessing.Need infiltrate an amount of LCM during body formation, mould, mold will guarantee that part meets the requirements of shape and size.For the follow-up surface of not having machinery processing, consider the harmomegathus amount of part in subsequent processes, suitably control the size of base substrate; For the follow-up surface that will carry out mechanical workout, need to reserve certain process redundancy.Shaping base substrate face to be processed stays the surplus of 10mm to 20mm to be advisable.The main component of solidifying agent is carbon-Hydrogen Oxygen polymer of monomers, can consider to add couplant.This solidifying agent is water miscible liquid.Concentration can from 2% to 30%, is preferably 4% to 20%.
3, solidification treatment
Be solidificated in the baking oven and carry out.The maximum heating temperature of baking oven is 400 ℃.Curing process divides multistage to carry out.From room temperature-60 ℃, time spent 1-2 hour; 60 ℃ to 180 ℃, 3 to 5 hours times spent; 180 ℃ are incubated 2-6 hour; From 180 ℃ to 280 ℃, time spent 3-7 hour; 280 ℃ are incubated 2-5 hour; After the blowing out, furnace cooling is lower than 70 ℃ to temperature and comes out of the stove.
4, charing is handled
Need carry out charing to base substrate handles.The charing treatment process divides multistage to carry out.From room temperature-250 ℃, heated 2-4 hour; 250 ℃ to 350 ℃, heated 3 to 6 hours; From 350 ℃ to 650 ℃, heated 8-12 hour; Heating is 6-10 hour from 650 ℃ to 900 ℃.
5, chemical gas phase pre-deposition
Base substrate after solidifying is repaired a little, and the vacuum chemistry gaseous phase deposition stove of packing into carries out the chemical gas phase pre-deposition.Be evacuated to 5-30Pa, measure the voltage rise rate of vacuum oven after the termination of pumping.After meeting the requirements prescribed, could heat up.Be warming up to 800 ℃-1200 ℃, can feed hydrocarbon and mixed gas nitrogen, the ratio of the two was from 1: 0.5 to 1: 3.Furnace pressure remains on 500Pa to 30KPa, depositing time is 5 hours to 50 hours, the cracking under low pressure, high temperature of carbon-hydrogen, and carbon atom deposits on the fiber of the surface of base substrate and part corpus fibrosum, the surface density of base substrate is increased, and the intensity and the rigidity on nearly surface, surface improve.
6, mechanical workout
The part billet surface need be carried out machining.Because the density of base substrate is low, intensity and rigidity are much lower than metallic substance.Need design specific frock according to the size and dimension of workpiece during mechanical workout, clamping workpiece is fixed on the lathe; Rotating speed is advisable with 2 to 100rpm during the workpiece cutting, and diameter of work is big more, and rotating speed is low more; The blade of the cutter of processing is thin more, sharp more good more.
7, pyroprocessing
The base substrate that the experience multiple tracks is handled need carry out pyroprocessing.1800 ℃-2300 ℃ of treatment temps, 2000 ℃-2300 ℃ better.Main purpose is except that metallic impurity and removes volatilization and grade.Temperature increasing schedule: room temperature to 1200 ℃ was got 2 to 5 hours, got 3 to 6 hours for 1200 ℃-1800 ℃, 1800 ℃-top temperature, 2-4 hour, to top temperature, can be incubated 2 to 5 hours.
8, topcoating
To carrying out top coat through the surface of mechanical cutting processing, the prescription of top coat mainly by binding agent, contain thing admittedly and form, binding agent is to contain silicon sol-gel, if, be 10: 1 to 2: 1 admittedly contain the weight ratio of thing and certain density binding agent colloidal sol admittedly contain owner's carbon fiber, high purity graphite powder.
9, final surface chemistry vapour deposition is strengthened
Be operated in the curing felt body part in the crystal furnace with certain vacuum, because it is limited that polysilicon melts the cleanliness factor of body, the particularly at high temperature continuous and carbon reaction of quartz crucible, therefore, more or less can produce oxidizing gas such as carbon monoxide, carbonic acid gas in the stove, the carbon product surface be produced corrode.The base substrate of the mistake of experience pyroprocessing if the deposit carbon of one deck 5 μ m to 50 μ m is arranged, particularly has the deposit carbon of one deck 10 μ m to 40 μ m, and surperficial corrosion resistance will greatly greatly improve.Higher temperature is adopted in final surface chemistry vapour deposition, as 1100 ℃-1300 ℃, adopts lower furnace pressure, as 300Pa-800Pa.About 5 hours-50 hours time.
Made silicon crystal growth oven with a complete set of solid-state heat-insulation system part with this method.Except component such as muff, insulation base plate, furnace bottom protection plate, also make the monoblock type guide shell, vital parts such as large cover, carriage with the curing felt.The heat-insulation system of carbon-carbon composite is equipped in and has carried out the industrialness use on the TDR-80 stove; The 48.6kg that feeds intake, polycrystal all are pot bottom material and material end to end, and the proportion that its medium or low resistance pot bottom material accounts for is 71.6%.Adopt new system, pulled out complete single crystal rod smoothly.This system adopts cured charcoal felt (carbon-carbon composite (CFC)) to replace guide shell, large cover, carriage, base plate that traditional graphite material is made silicon monocrystalline furnace thermal field system first, has cancelled the graphite piece that plays the support effect; Parts such as the base plate that employing carbon-carbon composite (CFC) is made, cover plate, guide shell have possessed the effect of structural part and lagging material simultaneously, have simplified the thermal field system design, have improved heat insulation effect and work reliability; The weight of the complete hot system of carbon-carbon composite (CFC) and the main conventional hot systematic comparison of adopting the popular use of isostatic pressing formed graphite material, weight has reduced more than 50%; Part important spare part such as weight such as guide shell, bottom plate have reduced more than 60%, and physical strength has increased more than ten times.The use of novel material has improved the reliability and the use properties of system greatly, has alleviated working strength of workers significantly.Under the situation of equal heat-insulating property, the thickness of heat preservation member can reduce 30%, and structure in the stove is compact more.In the silicon crystal growth oven equipment that can only adorn 18 inches systems originally, can adorn the hot system of 19 inches even 20 inches, improved the charge amount of single stove, effectively utilized the ability of equipment, improved quality product, improved production efficiency; The cured charcoal felt heat-preservation cylinder of carbon-carbon composite (CFC) making and traditional soft carbon felt compare structured size, surface clean.The soft carbon felt of tradition lagging material can produce a large amount of carbon dusts, contaminate environment, the skin that stimulates the people in operating process.And the in use easy deterioration of soft carbon felt often needs to repair/augment/twine again, and complicated operation is wasted time and energy.And solid-state heat-preservation cylinder is whole assembled, and is simple to operate.The solid-state insulation quilt of carbon-carbon composite (CFC) has certain intensity and rigidity, and the shape and size retentivity is good, and shove charge and to tear stove open very easy has improved workman's Working environment and labor condition greatly.Use the thermal field system and the hot systematic comparison of conventional graphite material of full carbon-carbon composite (CFC), heat-insulating property improves greatly.With the another set of systematic comparison that is equipped on the equipment on the same stage, the thickness of thermal insulation layer has reduced 25%, when changing material energy-conservation 15%; During isometrical crystal pulling energy-conservation 10%.Because the purity height of the solid-state insulation quilt that this technology is made, discharge quantity is minimum, has saved 40% by the thermal field system calcination time of the fabrication techniques of this patent than traditional system.
Claims (9)
1, a kind of high purity cured charcoal felt silicon crystal growth oven manufacture method is characterized in that: select the very low soft felt body of metals content impurity to make blank of material, the high temperature pre-treatment makes it to become the graphite felt body; By means of mould, mold, make base substrate with graphite felt system through pyroprocessing; Evenly infiltrate an amount of solidifying agent in the base substrate, the preformed base substrate that infiltrates solidifying agent is cured typing handles; Handle doing charing again through the base substrate of solidification treatment; The base substrate of the first one-step forming vacuum chemistry gaseous phase deposition stove of packing into is carried out the chemical gas phase pre-deposition; Part to part needs the surface of machining to carry out mechanical cutting processing; Pyroprocessing part base substrate is removed metallic impurity and volatile matter; Machined surface to the part after coming out of the stove carries out the top coat processing; Part is done chemical vapour deposition, carry out surface Hardening Treatment, improve the billet surface corrosion resistance.
2, according to claim 1, described high purity cured charcoal felt silicon crystal growth oven manufacture method is characterized in that: described cured charcoal felt blank of material is polypropylene cyanogen (PAN) felt body.
3, high purity cured charcoal felt silicon crystal growth oven manufacture method according to claim 1 is characterized in that: the pre-treatment of described felt body, thermal treatment temp are at 1800 ℃ to 2300 ℃, preferably at 2100 ℃-2300 ℃;
4, high purity cured charcoal felt silicon crystal growth oven manufacture method according to claim 1 is characterized in that: described solidifying agent is carbon-Hydrogen Oxygen monomer-polymer, and the technology of solidification treatment is:
5, high purity cured charcoal felt silicon crystal growth oven manufacture method according to claim 1 is characterized in that: described charing treatment process is:
6, high purity cured charcoal felt silicon crystal growth oven manufacture method according to claim 1 is characterized in that: the described chemical gas phase pre-deposition time was by 5 hours to 50 hours.
7, high purity cured charcoal felt silicon crystal growth oven manufacture method according to claim 1 is characterized in that: the pyroprocessing after the described machining, the temperature of processing are at 1800 ℃-2300 ℃, and high-temperature holding time is 2 hours to 5 hours.
8, high purity cured charcoal felt silicon crystal growth oven manufacture method according to claim 1, it is characterized in that: the prescription that the machining surface coating of described base substrate is handled mainly by binding agent, contain thing admittedly and form, binding agent is to contain silicon sol-gel, if, be 10: 1 to 2: 1 admittedly contain the weight ratio of thing and certain density binding agent colloidal sol admittedly contain owner's carbon fiber, high purity graphite powder.
9, high purity cured charcoal felt silicon crystal growth oven manufacture method according to claim 1 is characterized in that: described top coat is handled, and the thickness of coating is advisable with 5 μ m to 50 μ m, is preferably 15 μ m to 25 μ m.
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