CN209144025U - A kind of semiconductor grade silica crucible - Google Patents
A kind of semiconductor grade silica crucible Download PDFInfo
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- CN209144025U CN209144025U CN201821804915.8U CN201821804915U CN209144025U CN 209144025 U CN209144025 U CN 209144025U CN 201821804915 U CN201821804915 U CN 201821804915U CN 209144025 U CN209144025 U CN 209144025U
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Abstract
A kind of semiconductor grade silica crucible, including silica crucible ontology, first protective layer, second protective layer, third protective layer, first protective layer is set on the inner surface of silica crucible ontology, second protective layer is set to the upper surface of the first protective layer, the third protective layer is set to the lower surface of the first protective layer, the height of second protective layer is identical as the height of the third protective layer, second protective layer thickness is identical as the third protective layer thickness, second protective layer is in contact on the first protective layer with the third protective layer, form the level of complete and smooth, the micro-bubbles of first protective layer compared with the prior art are thicker, second protective layer reduces the shake of silicon liquid level caused by microbubble, third protective layer realizes semiconductor grade silicon rod not crystallization during crystal pulling, realize that silica crucible production is partly led Body grade silicon rod, hence it is evident that the crystal defect of semiconductor grade silicon rod is reduced, seeding number is reduced, it will not crystallization during crystal pulling.
Description
Technical field
The utility model relates to crucible production field more particularly to a kind of semiconductor grade silica crucibles.
Background technique
Silica crucible is the important auxiliary of pulling monocrystal silicon rod, is generally employed to produce conventional crystal bar.
Silica crucible generallys use natural siliceous sand (SiO2Content is 99.99%) to be made, and there are one between quartz sand particle
Fixed gap, in silica crucible production process, even if under vacuum and 1700 DEG C of reaction condition, it is also difficult to remove quartz sand
Air between particle in gap, the quartz sand that the quartz of partial melting can not melt surrounding wrap up and form quartz sand gas-liquid
Inclusion enclave, eventually leading to manufactured quartz crucible inner surface has very high microbubble content, and the diameter of microbubble belongs to micron
Grade, is primarily present in quartz crucible inner surface 1mm depth.Micro- gas in the growth course of silicon single crystal rod, in silica crucible
Bubble is slowly expanded under continuous high temperature environment, is grown up, and is merged into bigger microbubble, once rupture, it can be by quartz chips, impurity
It is brought into the silicon liquid of melting, aggravation silica crucible and the extent of reaction for melting silicon liquid cause at silica crucible inside liquid level line
Silicon liquid level shake, lead to crystal pulling failure or the broken string during crystal pulling.
Silica crucible contains more impurity, and content of impurities is close to the gold such as 100ppm, especially potassium, sodium, calcium, magnesium, aluminium
Belong to ion, and the temperature of thermal field during entire crystal pulling is up to 1700 DEG C, causes the change of the metal ions such as potassium, sodium, calcium, magnesium, aluminium
Activity is higher, and the metal ions such as potassium, sodium, calcium, magnesium, aluminium are easy to chemically react with quartz crucible inner surface, in quartzy earthenware
Crucible inner surface generates a chromatography crystal layer, and with the extension of crystal pulling time, crystallization layer gradually thickens, and leads to the crystal knot being growing
Structure occur mutation and can not normal or Optimal growth, cause the crystal bar crystal defect of growth to increase.
Although the prior art quartz crucible surface be provided with composite layer, silica crucible itself and composite layer there are still compared with
More microbubbles simultaneously contain more impurity, and silica crucible is caused not to be able to satisfy the production requirement of semiconductor grade crystal bar.
Summary of the invention
Deficiency against the above technical problems, the utility model proposes a kind of semiconductor grade silica crucibles.
A kind of semiconductor grade silica crucible, including the protection of silica crucible ontology, the first protective layer, the second protective layer, third
Layer, first protective layer are set on the inner surface of silica crucible ontology, and second protective layer is set to the first protective layer
Upper surface, the third protective layer is set to the lower surface of the first protective layer, the height of second protective layer and described the
The height of three protective layers is identical, and second protective layer is in contact on the first protective layer with the third protective layer, shape
At the level of complete and smooth.
Preferably, second protective layer upper end is arranged higher than initial liquid level line, and the second protective layer lower end is lower than initial liquid
Bit line setting, the third protective layer are arranged lower than initial liquid level line.
Preferably, first protective layer thickness is 8-10mm, and second protective layer thickness is 1.5-3mm, described the
Three protective layer thickness are 1.5-3mm.
Preferably, microbubble contained by first protective layer is 20-34/mm3, microbubble contained by second protective layer
For 3-8/mm3, microbubble contained by the third protective layer is 3-8/mm3。
Preferably, first protective layer is micro-bubbles, and second protective layer is hyaline layer, the third protective layer
For inhibit crystallization layer, second protective layer, third protective layer contact surface be tilting contact surface.
Preferably, first protective layer is made of glass sand, each impurity content in the glass sand
≤ 1ppm, and each content of impurities≤12ppm, size range are 140 mesh ~ 300 mesh；Second protective layer by efficiently every
Be made from quartz sand, in the efficient isolation quartz sand each impurity content≤1ppm, and each content of impurities≤
10ppm, size range are 75 mesh ~ 140 mesh；The third protective layer is made of high-purity artificial synthesized amorphous state quartz sand,
In high-purity artificial synthesized amorphous state quartz sand each impurity content≤0.3ppm, and each content of impurities≤
3ppm, size range are 75 mesh ~ 200 mesh.
The utility model uses higher purity, the less glass sand of impurity content, quartz sand is efficiently isolated, is high-purity
Artificial synthesized amorphous state quartz sand generates the first protective layer in silica crucible body surface, raw in the first protective layer
At the second protective layer, third protective layer, a kind of semiconductor grade silica crucible has been made, compared with prior art, the first protection
The micro-bubbles microbubble of layer compared with the prior art is lower, and the microbubble for reducing by the first protective layer enters in silicon liquid, reduces silicon liquid
The degree of jitter in face, the micro-bubbles impurity content of the first protective layer compared with the prior art is less, reduces in silica crucible ontology
The impurity in portion enters in silicon liquid, realizes that silica crucible produces semiconductor grade silicon rod；Microbubble in second protective layer substantially drops
Low, contained microbubble is only 3-8/mm3, the shake of silicon liquid level caused by microbubble is reduced, is solved in silica crucible ontology
The problem of portion's silicon liquid level shake；The third protective layer content of impurities≤3ppm, impurities content is extremely low, being capable of very big journey
Degree reduces degree of crystallization, or even prevents that Crystallization Process occurs, and realizes semiconductor grade silicon rod not crystallization during crystal pulling, solves
The problem that crystallization causes semiconductor grade silicon rod crystal defect to increase.
The utility model is provided with the first protective layer, the second protective layer, third protective layer, system in silica crucible body surface
A kind of semiconductor grade silica crucible was obtained, compared with prior art, the micro-bubbles of the first protective layer compared with the prior art are thicker,
And the first each content of impurities≤12ppm of protective layer, it can prevent the impurity of silica crucible ontology from entering in silicon liquid, substantially subtract
Few impurity realizes that silica crucible produces semiconductor grade silicon rod to defect caused by semiconductor grade silicon rod, while the first protective layer contains
Have the microbubble of certain content, be conducive to uniformly transfer outside heat into silicon liquid, both ensure that pulling operation it is normal into
Row, in turn ensures that the first protective layer does not rupture during crystal pulling；The microbubble content of second protective layer, third protective layer
The microbubble content being significantly less than in the first protective layer reduces the shake of silicon liquid level caused by microbubble, solves silica crucible
The problem of body interior silicon liquid level shake, realizes the preparation of semiconductor grade silicon rod；Each content of impurities of third protective layer
≤ 3ppm, impurities content is extremely low, can high degree reduce degree of crystallization, or even prevent that Crystallization Process occurs, realize half
Conductor level silicon rod not crystallization during crystal pulling, solves the problems, such as that crystallization causes semiconductor grade silicon rod crystal defect to increase.
Detailed description of the invention
Fig. 1 is a kind of schematic diagram of semiconductor grade silica crucible.
In figure: silica crucible ontology 11, the first protective layer 12, the second protective layer 13, third protective layer 14, the first blanking barrel
21, the second blanking barrel 22, third blanking barrel 23；Initial liquid level line L.
Specific embodiment
In conjunction with the embodiments, the present invention will be further described for the utility model, and following embodiment is intended to illustrate practical
It is novel rather than the utility model is further limited, it should not limit the protection scope of the present invention.
The utility model proposes a kind of manufacturing method of semiconductor grade silica crucible, the silica crucible includes quartz
Crucible body 11, the first protective layer 12, the second protective layer 13, third protective layer 14, the manufacturing method the following steps are included:
Raw material preparation: glass sand that is up-to-standard, meeting manufacturing technique requirent, efficiently isolation quartz are weighed respectively
Quartz sand, high-purity artificial synthesized amorphous is efficiently isolated in sand, high-purity artificial synthesized amorphous state quartz sand, the glass sand
The mass ratio of posture quartz sand is 3 ~ 5:1:1；
For example, the mass ratio of the glass sand, efficiently isolation quartz sand, high-purity artificial synthesized amorphous state quartz sand
It can be such that
Mass ratio 1: glass sand, the mass ratio that quartz sand, high-purity artificial synthesized amorphous state quartz sand is efficiently isolated
For 3:1:1；
Mass ratio 2: glass sand, the mass ratio that quartz sand, high-purity artificial synthesized amorphous state quartz sand is efficiently isolated
For 4:1:1；
Mass ratio 3: glass sand, the mass ratio that quartz sand, high-purity artificial synthesized amorphous state quartz sand is efficiently isolated
For 5:1:1；
Charging: after getting out three kinds of raw materials, glass sand being pre-set inside the first blanking barrel 21 of melting machine,
Efficient isolation quartz sand is set to inside the second blanking barrel 22, high-purity artificial synthesized amorphous state quartz sand is pre-set at
Inside the third blanking barrel 23 of melting machine, and blanking sequence is set gradually as the first blanking barrel 21, the second blanking barrel 22, third
Blanking barrel 23；
Material molding prepares: after the completion of charging, silica crucible ontology 11 being set on crucible die, and crucible die is set
It is placed in rotation axis, and crucible die axis and horizontal plane, is conducive to the protection that raw material is formed in quartz crucible inner surface
Layer height having the same, starting rotation axis rotate crucible die, and the revolving speed of crucible die is 70 ~ 90r/min, while by the
One blanking barrel 21 or the second blanking barrel 22 or third blanking barrel 23 are set to apart from 11 40 ~ 80mm of inner surface of silica crucible ontology
Place；
For example, first blanking barrel 21, the second blanking barrel 22, third blanking barrel 23 are set in silica crucible ontology 11
The distance H1 on surface can be such that
First blanking barrel 21, the second blanking barrel 22, third blanking barrel 23 are respectively arranged in silica crucible ontology 11
The distance H1 on surface be respectively 40mm, 40mm, 40mm or H1 be respectively 50mm, 50mm, 50mm or H1 be respectively 60mm,
60mm, 60mm or H1 are respectively that 70mm, 70mm, 70mm or H1 are respectively 80mm, 80mm, 80mm；
Realize the first blanking barrel 21, the second blanking barrel 22, third blanking barrel 23 in distance quartz by automatic blanking device
Flow rotation is taken turns at 11 inner surface H1 of crucible body, and the first blanking barrel 21 or the second blanking barrel 22 or third blanking barrel 23 is made to work
Before be placed exactly at 11 inner surface H1 of silica crucible ontology；
First blanking barrel 21, the second blanking barrel 22, third blanking barrel 23 are set to the table in silica crucible ontology 11
At the H1 of face, is conducive to the first blanking barrel 21 and the first uniform and stable protection preformed layer is set in 11 inner surface of silica crucible ontology,
Be conducive to the second blanking barrel 22 and the second uniform and stable protection preformed layer is set in the first prefabricated layer surface of protection, is conducive to the
Three blanking barrels 23 are arranged uniform and stable third in the first prefabricated layer surface of protection and protect preformed layer；Second blanking barrel 22 is fallen
Material be set in sequence in front of 23 blanking of third blanking barrel, can be avoided the efficient isolation quartz sand in the second blanking barrel 22 be scattered to
Third is protected in prefabricated layer surface, and then preformed layer will not be protected to have an adverse effect third；
Referring to Fig. 1, the first blanking barrel 21 material molding: is controlled on 11 inside edge of silica crucible ontology by automatic blanking device
The position O, P position to the position Q move back and forth, while crucible die being kept to rotate, and glass sand is uniformly arranged on quartzy earthenware
On the entire inner surface of crucible ontology 11, so that 11 inner surface of silica crucible ontology forms the first protection preformed layer；First blanking barrel
After 21 feed intake, by automatic blanking device control the second blanking barrel 22 inside silica crucible ontology 11 along the position O to P
Reciprocating motion is set, efficient isolation quartz sand is uniformly arranged in the prefabricated layer surface of the first protection, so that the first protection preformed layer
The second protection preformed layer is formed on surface；After second blanking barrel 22 feeds intake, third blanking is controlled by automatic blanking device
Cylinder 23 moves back and forth inside silica crucible ontology 11 along P position to the position Q, and high-purity artificial synthesized amorphous state quartz sand is equal
It is even to be set in the prefabricated layer surface of the first protection, so that forming third in the first prefabricated layer surface of protection protects preformed layer, third
Blanking barrel 23 feeds intake end, makes the contact surface tilting contact surface of the second protection preformed layer, third protection preformed layer, relatively flat
Line contact has bigger contact area, is conducive to the second protection of enhancing preformed layer, the intensity that third protection preformed layer combines,
Make contact surface that can combine closely in the case where environment is melted, and protects preformed layer and second to protect preformed layer contact area third
Surface is polished, and third blanking barrel 23 understands some high-purity artificial synthesized amorphous state quartz during P position feeds intake
Sand splashes down in the second protection preformed layer bottom surface, protects the table of preformed layer and the second protection preformed layer contact area in third
Male and female face or salient point are formed on face, by way of polishing, make third protection preformed layer and the second protection preformed layer contact area
Surfacing, smooth, contact area surface and third protection preformed layer after polishing, the second protection preformed layer are having the same
Surface flatness；
It is melted and prepares: will expect that crucible die after molding is set to small melted chamber interior, crucible die one end is set to 6
The positive lower end of high pure graphite electrode, crucible die rotation center and 6 high pure graphite electrodes are coaxial, adjust 6 high purity graphite electricity
Gap between pole is in gap between 30 ~ 50mm, so that the high temperature heat that 6 high pure graphite electrodes generate is uniformly distributed
To around crucible die, expect that the crucible die other end after molding is additionally provided with vacuum evacuation device, the small melted interior is also
Air-intake device, air exhausting device and blowning installation are set；The small melted room is set to chamber interior melted greatly；
Silica crucible ontology described in the present embodiment 11 has size of different sizes, and is provided with crucible matched with its
Mold, and vacuum evacuation device is arranged in the crucible die other end, for being vacuumized inside silica crucible ontology 11；It vacuumizes
When device inside small size silica crucible ontology 11 to vacuumizing, its various places inside can uniformly be vacuumized,
But when to vacuumizing inside large scale silica crucible ontology 11, large scale silica crucible ontology 11 is because having deeper bottom
With wider inner wall, it is difficult to uniformly be vacuumized to its various places inside, cause the second protective layer 13 to be formed, third protection
Microbubble in layer 14 is unevenly distributed, it is possible to so that microbubble reunited under high temperature environment, grown up, therefore, to large scale
When silica crucible ontology 11 is vacuumized, the vacuum pumping valve of vacuum evacuation device is set in large scale silica crucible ontology 11
At portion center, so that 11 various places inside of large scale silica crucible ontology can be vacuumized uniformly, microbubble point is advantageously formed
Uniform second protective layer 13 of cloth, third protective layer 14, the vacuum pumping valve is sphere structure, and is provided on sphere structure
Several are equally distributed to vacuumize sucker, to realize that vacuum pumping valve is true to the uniform pumping of 11 various places inside of silica crucible ontology
It is empty；
It is melted: being melted after being ready to complete, crucible die revolving speed is maintained at 70 ~ 90r/min, opens the air inlet of small melted room
Device and air exhausting device, for keeping small melted room pressure constant；6 high purity graphite electricity are slowly opened by opening device
Pole, voltage 380V, current control make the positive lower end of 6 high pure graphite electrodes generate plasma electric between 2200A ~ 3000A
Arc；While opening 6 high pure graphite electrodes, also unlatching vacuum evacuation device and blowning installation, vacuum evacuation device are used for crucible
Mold is vacuumized, and reacts the silica crucible ontology 11 inside crucible die under vacuum conditions, is protected for extracting second
The gas that shield preformed layer wherein contains when changing to the second protective layer 13 makes in the second protective layer 13 as far as possible without containing micro- gas
Bubble, the gas for protecting preformed layer wherein to contain when changing to third protective layer 14 for extracting third, protects third as far as possible
Microbubble is not contained in layer 14, blowning installation is used to remove the quartz crystals ash on high pure graphite electrode, prevents quartz crystals grey
It falls into inside silica crucible ontology 11, semiconductor grade silicon rod is polluted, close vacuum valve after 4-8min is melted, the period
Interior, the second protective layer 13, the preparation of third protective layer 14 are completed, and the revolving speed of crucible die are adjusted to 65 ~ 85r/min, continue
10 ~ 20min is melted, the first protection preformed layer is made, without vacuum, to be conducive to the first protective layer into 12 transition process of the first protective layer
Uniform microbubble is formed in 12, during crystal pulling, microbubble of the silica crucible ontology 11 containing certain content is advantageous
It uniformly transfers in by outside heat into silicon liquid, both ensure that being normally carried out for pulling operation, in turn ensure the first protective layer 12
It is not ruptured during crystal pulling, until being prepared into the first protective layer 12, power supply is closed after the completion of being melted, by 6 root graphite electrode liters
It rises；The first protection preformed layer forms the first protective layer 12 under melting conditions, and the second protection preformed layer is in melted item
The second protective layer 13 is formed under part, the third protection preformed layer forms third protective layer 14 under melting conditions；
Post-processing: after being melted, crucible die is removed from melter, is cooled to room temperature, by silica crucible ontology 11
It is taken out out of crucible die, the semiconductor grade silica crucible is made.
Further, in the glass sand each impurity content≤1ppm, and each content of impurities≤12ppm,
Size range is 140 mesh ~ 300 mesh；In the efficient isolation quartz sand each impurity content≤1ppm, and each impurity is total
Content≤10ppm, size range are 75 mesh ~ 140 mesh；Each impurity element in high-purity artificial synthesized amorphous state quartz sand
Content≤0.3ppm, and each content of impurities≤3ppm, size range is 75 mesh ~ 200 mesh.
Referring to Fig. 1, further, the position O be set in the horizontal direction apart from 11 inner surface 40 of silica crucible ontology ~
At 80mm, so that the position O is overlapped with the first blanking barrel 21, the position in the horizontal direction of the second blanking barrel 22 in the horizontal direction, O
It is set to the initial position of the first blanking barrel 21,22 blanking of the second blanking barrel, the position O is set in vertical direction apart from silica crucible
At 11 top S1=10mm of ontology, be conducive to that the first uniform and stable protection preformed layer is arranged in 11 inner surface of silica crucible ontology,
And prevent glass sand from throwing away in the first 21 blanking of blanking barrel to silica crucible ontology 11, it avoids making melted environment
At pollution, be conducive to that the second uniform and stable protection preformed layer is arranged in the first prefabricated layer surface of protection, and prevent from being efficiently isolated
Quartz sand is thrown away in the second 22 blanking of blanking barrel to silica crucible ontology 11, avoids polluting melted environment；Institute
It states P position and is set to the positive lower end in the position O in vertical direction, so that the first blanking barrel 21 or the second blanking barrel 22 are along the position O to P
Carry out blanking is set, while again falls the initial blanking position of third blanking barrel 23 and the first blanking barrel 21, the second blanking barrel 22
Discharge position is identical, and P position is the final position of 22 blanking of the second blanking barrel, and P position is the initial bit of 23 blanking of third blanking barrel
It sets, and P position is overlapped with the extended line at 11 height midpoint of silica crucible ontology in the horizontal direction, so that the second protection preformed layer,
The prefabricated protective layer of third just forms complete level on the first prefabricated protective layer, and the second prefabricated layer height of protection is
The half of first protection preformed layer, and the prefabricated protection layer height of third is the half of the first protection preformed layer；The position the Q setting
In on the axis of silica crucible ontology 11, the position Q is the final position of the first blanking barrel 21,23 blanking of third blanking barrel, first
Blanking barrel 21 is moved back and forth along the position O, P position to the position Q, is conducive to be arranged on 11 surface of silica crucible ontology uniform and stable
First protection preformed layer, third blanking barrel 23 are moved back and forth along P position to the position Q, are conducive in the first prefabricated layer surface of protection
Uniform and stable third protection preformed layer is set, and the position Q is set to 11 inner bottom of silica crucible ontology and R in vertical direction
Between angle, the angle R is larger with respect to the other positions radian of silica crucible ontology 11, to falling at the angle R of silica crucible ontology 11
When material, with respect to the more difficult blanking of other positions of silica crucible ontology 11 at the angle R, and the position Q is set to silica crucible ontology 11
Between inner bottom and the angle R, be conducive to the first blanking barrel 21 or third blanking barrel 23 blanking at the angle R, so that glass sand
The first uniform and stable protection preformed layer is formed at the angle R by the first blanking barrel 21, so that high-purity artificial synthesized amorphous state
Quartz sand forms uniform and stable third protection preformed layer by third blanking barrel 23 at the angle R.
Referring to Fig. 1, the utility model proposes a kind of semiconductor grade silica crucibles, including silica crucible ontology 11, first
Protective layer 12, the second protective layer 13, third protective layer 14, first protective layer 12 are set to the interior table of silica crucible ontology 11
On face, second protective layer 13 is set to the upper surface of the first protective layer 12, and the third protective layer 14 is set to the first guarantor
The lower surface of sheath 12, the height of second protective layer 13 is identical as the height of the third protective layer 14, and described second protects
13 thickness of sheath is identical as 14 thickness of third protective layer, and second protective layer 13 and the third protective layer 14 are first
Protective layer is in contact on 12 surface, forms the level of complete and smooth.
Referring to Fig. 1, further, 13 upper end of the second protective layer is arranged higher than initial liquid level line L, under the second protective layer 13
End is arranged lower than initial liquid level line L, and the third protective layer 14 is arranged lower than initial liquid level line L.
The silicon liquid of melting is provided in silica crucible ontology 11, liquid level line of the silicon liquid before pulling operation is initial liquid level
Line L, initial liquid level line L would generally be higher than the middle position of silica crucible ontology 11, for producing more during a crystal pulling
More semiconductor grade silicon rod, but during crystal pulling, especially crystal pulling early period, i.e., carry out the silicon liquid near initial liquid level line L
When crystal pulling, silicon liquid level is easily shaken, and causes the reduction of semiconductor grade silicon rod seeding number, even results in the crystal pulling during crystal pulling
Failure or broken string.Second protective layer, 13 upper end is higher than initial liquid level line L setting, lower end to be arranged lower than initial liquid level line L, it can
It hinders the microbubble in the first protective layer 12 to enter in silicon liquid, is conducive to substantially to slow down the shake of silicon liquid level crystal pulling early period, it is real
The normal crystallization of existing semiconductor grade silicon rod.
With the progress of crystal pulling process, the degree that silicon liquid level is shaken is gradually decreased, but in silica crucible ontology 11
The degree that crystallization occurs for surface is gradually increased, and crystallization easily especially occurs in 11 middle part inner surface below of silica crucible ontology,
If crystallization occurs, it will cause semiconductor grade silicon rod crystal defect to increase, or even scrap semiconductor grade silicon rod.By initial
Liquid level line L is arranged lower end and third protective layer 14 is arranged, and advantageously reduces the degree that crystallization occurs, and is realizing semiconductor grade silicon rod just
Often crystallization.
Further, first protective layer 12 is with a thickness of 8-10mm, and second protective layer 13 is with a thickness of 1.5-3mm, institute
Third protective layer 14 is stated with a thickness of 1.5-3mm.
Silica crucible generallys use natural siliceous sand and is made, and containing more impurity, cannot be directly used to production semiconductor
Grade silicon rod.By being arranged thicker the first protective layer 12 in quartz crucible surface, first protective layer 12 is by glass sand
Be made, in the glass sand each impurity content≤1ppm, and each content of impurities≤12ppm, impurities contain
Amount is far smaller than the content of impurity in silica crucible ontology 11, and therefore, first protective layer 12 can prevent silica crucible sheet
The impurity of body 11 enters in silicon liquid, and impurity is greatly decreased to defect caused by semiconductor grade silicon rod, realizes silica crucible production
Semiconductor grade silicon rod, second protective layer 13, third protective layer 14 thickness less than 12 thickness of the first protective layer, be conducive to big
Width reduces contained when the second protection preformed layer changes to the second protective layer 13, third protection preformed layer changes to third protective layer 14
Some microbubble contents.
Microbubble contained by first protective layer 12 is 20-34/mm3, microbubble contained by second protective layer 13 is
3-8/mm3, microbubble contained by the third protective layer 14 is 3-8/mm3。
First protective layer 12 contains the microbubble of certain content, is conducive to uniformly transfer outside heat to silicon liquid
In, it both ensure that being normally carried out for pulling operation, and in turn ensured that the first protective layer 12 did not ruptured during crystal pulling, described second
Protective layer 13, third protective layer 14 microbubble content be significantly less than the microbubble content in the first protective layer 12, the hole contained
Gap is few, prevents the microbubble of the first protective layer 12 from entering in the second protective layer 13 or third protective layer 14, reduces micro- gas
The shake of silicon liquid level caused by steeping solves the problems, such as the shake of 11 inside silicon liquid level of silica crucible ontology, realizes semiconductor grade silicon
The preparation of stick.
Further, first protective layer 12 is micro-bubbles, and second protective layer 13 is hyaline layer, and the third is protected
Sheath 14 be inhibit crystallization layer, second protective layer, third protective layer contact surface be tilting contact surface.
First protective layer 12 contains more microbubble with respect to the second protective layer 13, third protective layer 14, can incite somebody to action
Outside heat is uniformly transferred into silicon liquid, is stablized the even heat of 11 various places inside of silica crucible ontology, is conducive to semiconductor
The preparation of grade silicon rod；Contained first protective layer, 12 impurity content is far smaller than the content of impurity in silica crucible ontology 11, can
It prevents the impurity of silica crucible ontology 11 from entering in silicon liquid, impurity is greatly decreased to defect caused by semiconductor grade silicon rod.
Second protective layer 13 is made by quartz sand is efficiently isolated, and each impurity element contains in the efficient isolation quartz sand
≤ 1ppm is measured, and each content of impurities≤10ppm, impurities total content further decrease with respect to the first protective layer 12, have
Conducive to the preparation of semiconductor grade silicon rod；Second protective layer 13 is made in the case where vacuumizing environment, has extracted efficient isolation quartz
Air between sand particle, significantly reduces the microbubble in the second protective layer 13, and contained microbubble is only 3-8/mm3, at
For hyaline layer, the shake of silicon liquid level caused by microbubble is reduced, solves the difficulty of 11 inside silicon liquid level of silica crucible ontology shake
Topic.
With the progress of crystal pulling process, the degree that crystallization occurs for 11 inner surface of silica crucible ontology is gradually increased, especially
Crystallization easily occurs in 11 middle part inner surface below of silica crucible ontology, and crystallization is typically due to impurity and causes.The third is protected
Sheath 14 is made of high-purity artificial synthesized amorphous state quartz sand, each impurity in high-purity artificial synthesized amorphous state quartz sand
Constituent content≤0.3ppm, and each content of impurities≤3ppm, impurities content is extremely low, can high degree reduce crystallization
Degree, or even prevent that Crystallization Process occurs, it realizes semiconductor grade silicon rod not crystallization during crystal pulling, solves crystallization and cause half
The problem that conductor level silicon rod crystal defect increases.
Second protective layer 13, third protective layer 14 contact surface be tilting contact surface, opposite run-in index contact tool
There is bigger contact area, is conducive to the intensity for enhancing the second protective layer 13, third protective layer 14 combines, makes contact surface in high temperature
Stabilization is able to maintain under environment.
A kind of semiconductor grade silica crucible has been made in the utility model, can satisfy the production requirement of semiconductor grade silicon rod,
The silica crucible is in use, hence it is evident that the degree of fluctuation for reducing silicon liquid level, crystal pulling silicon liquid level early period shake by 5 ~
8mm is reduced to 1 ~ 3mm, and average seeding number is reduced to 1.15 times/stick by 2.5 times/stick；During crystal pulling, inner surface will not
Crystallization is generated, crystal bar Oi content can control in 8 ~ 18ppm；The semiconductor grade silicon rod as made from silica crucible, 0.12um's
Crystal defect is reduced to 150 ~ 250, and 0.13um crystal defect is reduced to 70 ~ 120, and 0.16um crystal defect can disappear completely
It removes.
Specific embodiment:
Embodiment 1:
Raw material preparation: glass sand that is up-to-standard, meeting manufacturing technique requirent, efficiently isolation quartz are weighed respectively
Quartz sand, high-purity artificial synthesized amorphous is efficiently isolated in sand, high-purity artificial synthesized amorphous state quartz sand, the glass sand
The mass ratio of posture quartz sand is 3:1:1；
Charging: after getting out three kinds of raw materials, glass sand being pre-set inside the first blanking barrel 21 of melting machine,
Efficient isolation quartz sand is set to inside the second blanking barrel 22, high-purity artificial synthesized amorphous state quartz sand is pre-set at
Inside the third blanking barrel 23 of melting machine, and blanking sequence is set gradually as the first blanking barrel 21, the second blanking barrel 22, third
Blanking barrel 23；
Material molding prepares: after the completion of charging, silica crucible ontology 11 being set on crucible die, and crucible die is set
It is placed in rotation axis, and crucible die axis and horizontal plane, starting rotation axis rotates crucible die, and crucible die turns
Speed is 70r/min, while the first blanking barrel 21 or the second blanking barrel 22 or third blanking barrel 23 being set to apart from silica crucible
At 11 inner surface H1=40mm of ontology；
Material molding: the first blanking barrel 21 is controlled inside silica crucible ontology 11 along the position O, P by automatic blanking device
Position to the position Q moves back and forth, while crucible die being kept to rotate, and glass sand is uniformly arranged on silica crucible ontology 11
Inner surface on so that 11 inner surface of silica crucible ontology formed first protection preformed layer；After first blanking barrel 21 feeds intake,
It is moved back and forth inside silica crucible ontology 11 along the position O to P position by automatic blanking device the second blanking barrel 22 of control, it will
Efficiently isolation quartz sand is uniformly arranged in the prefabricated layer surface of the first protection, so as to form second in the first prefabricated layer surface of protection
Protect preformed layer；After second blanking barrel 22 feeds intake, third blanking barrel 23 is controlled in silica crucible by automatic blanking device
It is moved back and forth inside ontology 11 along P position to the position Q, high-purity artificial synthesized amorphous state quartz sand is uniformly arranged on the first guarantor
It protects in prefabricated layer surface, so that forming third in the first prefabricated layer surface of protection protects preformed layer, third blanking barrel 23 feeds intake knot
Beam, and polish third protection preformed layer and the surface of the second protection preformed layer contact area；
It is melted and prepares: will expect that crucible die after molding is set to small melted chamber interior, crucible die one end is set to 6
The positive lower end of high pure graphite electrode, crucible die rotation center and 6 high pure graphite electrodes are coaxial, adjust 6 high purity graphite electricity
Gap between pole is in gap between 30mm, expects that the crucible die other end after molding is additionally provided with vacuum evacuation device, institute
It states small melted interior and also sets up air-intake device, air exhausting device and blowning installation；The small melted room is set to chamber interior melted greatly；
It is melted: being melted after being ready to complete, crucible die revolving speed is maintained at 70r/min, open the air inlet dress of small melted room
It sets and air exhausting device, for keeping small melted room pressure constant；6 high pure graphite electrodes are slowly opened by opening device,
Voltage is 380V, and current control makes the positive lower end of 6 high pure graphite electrodes generate plasma-arc between 2200A ~ 3000A；It opens
While opening 6 high pure graphite electrodes, also unlatching vacuum evacuation device and blowning installation, vacuum evacuation device be used for crucible die into
Row vacuumizes, and blowning installation is used to remove the quartz crystals ash on high pure graphite electrode, closes vacuum valve after 4min is melted, and will
The revolving speed of crucible die is adjusted to 65r/min, continues that 10min is melted, and power supply is closed after the completion of being melted, by 6 root graphite electrode liters
It rises；The first protection preformed layer forms the first protective layer 12 under melting conditions, and the second protection preformed layer is in melted item
The second protective layer 13 is formed under part, the third protection preformed layer forms third protective layer 14 under melting conditions；
Post-processing: after being melted, crucible die is removed from melter, is cooled to room temperature, by silica crucible ontology 11
It is taken out out of crucible die, the semiconductor grade silica crucible is made.
Embodiment 2:
Raw material preparation: glass sand that is up-to-standard, meeting manufacturing technique requirent, efficiently isolation quartz are weighed respectively
Quartz sand, high-purity artificial synthesized amorphous is efficiently isolated in sand, high-purity artificial synthesized amorphous state quartz sand, the glass sand
The mass ratio of posture quartz sand is 5:1:1；
Charging: after getting out three kinds of raw materials, glass sand being pre-set inside the first blanking barrel 21 of melting machine,
Efficient isolation quartz sand is set to inside the second blanking barrel 22, high-purity artificial synthesized amorphous state quartz sand is pre-set at
Inside the third blanking barrel 23 of melting machine, and blanking sequence is set gradually as the first blanking barrel 21, the second blanking barrel 22, third
Blanking barrel 23；
Material molding prepares: after the completion of charging, silica crucible ontology 11 being set on crucible die, and crucible die is set
It is placed in rotation axis, and crucible die axis and horizontal plane, starting rotation axis rotates crucible die, and crucible die turns
Speed is 90r/min, while the first blanking barrel 21 or the second blanking barrel 22 or third blanking barrel 23 being set to apart from silica crucible
At 11 inner surface H1=80mm of ontology；
Material molding: the first blanking barrel 21 is controlled inside silica crucible ontology 11 along the position O, P by automatic blanking device
Position to the position Q moves back and forth, and glass sand is uniformly arranged on the inner surface of silica crucible ontology 11, so that quartzy earthenware
11 inner surface of crucible ontology forms the first protection preformed layer；After first blanking barrel 21 feeds intake, controlled by automatic blanking device
Second blanking barrel 22 moves back and forth inside silica crucible ontology 11 along the position O to P position, and efficient isolation quartz sand is uniformly set
It is placed in the prefabricated layer surface of the first protection, so as to form the second protection preformed layer in the first prefabricated layer surface of protection；Second blanking
After cylinder 22 feeds intake, third blanking barrel 23 is controlled inside silica crucible ontology 11 along P position to Q by automatic blanking device
Position moves back and forth, and high-purity artificial synthesized amorphous state quartz sand is uniformly arranged in the prefabricated layer surface of the first protection, so that
Third is formed in the first prefabricated layer surface of protection and protects preformed layer, and third blanking barrel 23 feeds intake ends, and prefabricated to third protection
It polishes on the surface of layer and the second protection preformed layer contact area；
It is melted and prepares: will expect that crucible die after molding is set to small melted chamber interior, crucible die one end is set to 6
The positive lower end of high pure graphite electrode, crucible die rotation center and 6 high pure graphite electrodes are coaxial, adjust 6 high purity graphite electricity
Gap between pole is in gap between 50mm, expects that the crucible die other end after molding is additionally provided with vacuum evacuation device, institute
It states small melted interior and also sets up air-intake device, air exhausting device and blowning installation；The small melted room is set to chamber interior melted greatly；
It is melted: being melted after being ready to complete, crucible die revolving speed is maintained at 90r/min, open the air inlet dress of small melted room
It sets and air exhausting device, for keeping small melted room pressure constant；6 high pure graphite electrodes are slowly opened by opening device,
Voltage is 380V, and current control makes the positive lower end of 6 high pure graphite electrodes generate plasma-arc between 2200A ~ 3000A；It opens
While opening 6 high pure graphite electrodes, also unlatching vacuum evacuation device and blowning installation, vacuum evacuation device be used for crucible die into
Row vacuumizes, and blowning installation is used to remove the quartz crystals ash on high pure graphite electrode, closes vacuum valve after 8min is melted, and will
The revolving speed of crucible die is adjusted to 85r/min, continues that 20min is melted, and power supply is closed after the completion of being melted, by 6 root graphite electrode liters
It rises；The first protection preformed layer forms the first protective layer 12 under melting conditions, and the second protection preformed layer is in melted item
The second protective layer 13 is formed under part, the third protection preformed layer forms third protective layer 14 under melting conditions；
Post-processing: after being melted, crucible die is removed from melter, is cooled to room temperature, by silica crucible ontology 11
It is taken out out of crucible die, the semiconductor grade silica crucible is made.
Embodiment 1, embodiment 2 use higher purity, the less glass sand of impurity content, efficiently isolation quartz
Sand, high-purity artificial synthesized amorphous state quartz sand are protected in the first protective layer 12 of 11 Surface Creation of silica crucible ontology first
12 Surface Creation of sheath the second protective layer 13, third protective layer 14, have been made a kind of semiconductor grade silica crucible, with existing skill
Art is compared, and the micro-bubbles microbubble of the first protective layer 12 compared with the prior art is lower, reduces the microbubble of the first protective layer 12
Into in silicon liquid, the degree of jitter of silicon liquid level is reduced, the micro-bubbles impurity content of the first protective layer 12 compared with the prior art is more
It is few, it reduces the impurity inside silica crucible ontology 11 and enters in silicon liquid, realize that silica crucible produces semiconductor grade silicon rod；Second
Microbubble in protective layer 13 is greatly reduced, and contained microbubble is only 3-8/mm3, reduce silicon liquid level caused by microbubble and tremble
It is dynamic, solve the problems, such as the shake of 11 inside silicon liquid level of silica crucible ontology；14 content of impurities of the third protective layer≤3ppm,
Impurities content is extremely low, can high degree reduce degree of crystallization, or even prevent occur Crystallization Process, realize semiconductor grade silicon
Stick not crystallization during crystal pulling, solves the problems, such as that crystallization causes semiconductor grade silicon rod crystal defect to increase.
Embodiment 3:
A kind of semiconductor grade silica crucible, including silica crucible ontology 11, the first protective layer 12, the second protective layer 13,
Three protective layers 14, first protective layer 12 are set on the inner surface of silica crucible ontology 11, and second protective layer 13 is set
It is placed in the upper surface of the first protective layer 12, the third protective layer 14 is set to the lower surface of the first protective layer 12, and described second
The height of protective layer 13 is identical as the height of the third protective layer 14, and 13 thickness of the second protective layer and the third are protected
14 thickness of layer are identical, and second protective layer 13 is in contact on 12 surface of the first protective layer with the third protective layer 14, shape
At the level of complete and smooth.
First protective layer 12 is with a thickness of 8mm, and second protective layer 13 is with a thickness of 1.5mm, the third protective layer
14 with a thickness of 1.5mm.
Microbubble contained by first protective layer 12 is 20/mm3, microbubble contained by second protective layer 13 is 3/
mm3, microbubble contained by the third protective layer 14 is 3/mm3。
Embodiment 4:
A kind of semiconductor grade silica crucible, including silica crucible ontology 11, the first protective layer 12, the second protective layer 13,
Three protective layers 14, first protective layer 12 are set on the inner surface of silica crucible ontology 11, and second protective layer 13 is set
It is placed in the upper surface of the first protective layer 12, the third protective layer 14 is set to the lower surface of the first protective layer 12, and described second
The height of protective layer 13 is identical as the height of the third protective layer 14, and 13 thickness of the second protective layer and the third are protected
14 thickness of layer are identical, and second protective layer 13 is in contact on 12 surface of the first protective layer with the third protective layer 14, shape
At the level of complete and smooth.
First protective layer 12 is with a thickness of 10mm, and second protective layer 13 is with a thickness of 3mm, the third protective layer 14
With a thickness of 3mm.
Microbubble contained by first protective layer 12 is 34/mm3, microbubble contained by second protective layer 13 is 8/
mm3, microbubble contained by the third protective layer 14 is 8/mm3。
Embodiment 3, embodiment 4 are provided with the first protective layer 12, the second protective layer 13, the on 11 surface of silica crucible ontology
A kind of semiconductor grade silica crucible has been made in three protective layers 14, and compared with prior art, the first protective layer 12 is compared with the prior art
Micro-bubbles it is thicker, and each content of impurities≤12ppm of the first protective layer 12 can prevent the impurity of silica crucible ontology 11
It enters in silicon liquid, impurity is greatly decreased to defect caused by semiconductor grade silicon rod, realizes that silica crucible produces semiconductor grade silicon
Stick, while the first protective layer 12 contains the microbubble of certain content, is conducive to uniformly transfer outside heat into silicon liquid, both protect
Being normally carried out for pulling operation has been demonstrate,proved, has in turn ensured that the first protective layer 12 does not rupture during crystal pulling；Second protective layer
13, the microbubble content of third protective layer 14 is significantly less than the microbubble content in the first protective layer 12, reduces microbubble and draws
The silicon liquid level shake risen, solves the problems, such as the shake of 11 inside silicon liquid level of silica crucible ontology, realizes semiconductor grade silicon rod
Preparation；Each content of impurities≤3ppm of the third protective layer 14, impurities content is extremely low, being capable of high degree reduction crystallization
Degree, or even prevent that Crystallization Process occurs, it realizes semiconductor grade silicon rod not crystallization during crystal pulling, solves crystallization and cause half
The problem that conductor level silicon rod crystal defect increases.
Above disclosures are merely preferred embodiments of the utility model, the utility model cannot be limited with this certainly
Interest field, those skilled in the art can understand all or part of the processes for realizing the above embodiment, and according to this reality
The equivalent variations made by novel claim, still falls within the scope of the utility model.
Claims (6)
1. a kind of semiconductor grade silica crucible, it is characterised in that: including silica crucible ontology, the first protective layer, the second protective layer,
Third protective layer, first protective layer are set on the inner surface of silica crucible ontology, and second protective layer is set to
The upper surface of one protective layer, the third protective layer are set to the lower surface of the first protective layer, the height of second protective layer
It is identical as the height of the third protective layer, second protective layer phase on the first protective layer with the third protective layer
Contact, forms the level of complete and smooth.
2. a kind of semiconductor grade silica crucible as described in claim 1, it is characterised in that: second protective layer upper end is higher than
The setting of initial liquid level line, the second protective layer lower end are arranged lower than initial liquid level line, and the third protective layer is lower than initial liquid level line
Setting.
3. a kind of semiconductor grade silica crucible as described in claim 1, it is characterised in that: first protective layer thickness is 8-
10mm, second protective layer thickness are 1.5-3mm, and the third protective layer thickness is 1.5-3mm.
4. a kind of semiconductor grade silica crucible as described in claim 1, it is characterised in that: micro- gas contained by first protective layer
Bubble is 20-34/mm3, microbubble contained by second protective layer is 3-8/mm3, microbubble contained by the third protective layer is
3-8/mm3。
5. a kind of semiconductor grade silica crucible as described in one of claim 1-4, it is characterised in that: first protective layer is
Micro-bubbles, second protective layer are hyaline layer, and the third protective layer is to inhibit crystallization layer, second protective layer, the
The contact surface of three protective layers is tilting contact surface.
6. a kind of semiconductor grade silica crucible as described in one of claim 1-4, it is characterised in that: first protective layer by
Glass sand is made, in the glass sand each impurity content≤1ppm, and each content of impurities≤12ppm,
Size range is 140 mesh ~ 300 mesh；Second protective layer is made by quartz sand is efficiently isolated, the efficient isolation quartz sand
In each impurity content≤1ppm, and each content of impurities≤10ppm, size range is 75 mesh ~ 140 mesh；Described
Three protective layers are made of high-purity artificial synthesized amorphous state quartz sand, each miscellaneous in high-purity artificial synthesized amorphous state quartz sand
Prime element content≤0.3ppm, and each content of impurities≤3ppm, size range is 75 mesh ~ 200 mesh.
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Address after: 750021 No.23 Guangming West Road, Xixia District, Yinchuan City, Ningxia Hui Autonomous Region Patentee after: Ningxia dunyuan poly core semiconductor technology Co.,Ltd. Address before: 750021 No.23 Guangming West Road, Xixia District, Yinchuan City, Ningxia Hui Autonomous Region Patentee before: FERROTEC (NINGXIA) ADVANCED QUARTZ MATERIAL Co.,Ltd. |