CN1260402C - Combined gas-phase pre-doping and neutron irradiation doping area fused silicon monocrystal production method - Google Patents
Combined gas-phase pre-doping and neutron irradiation doping area fused silicon monocrystal production method Download PDFInfo
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- CN1260402C CN1260402C CN 03109067 CN03109067A CN1260402C CN 1260402 C CN1260402 C CN 1260402C CN 03109067 CN03109067 CN 03109067 CN 03109067 A CN03109067 A CN 03109067A CN 1260402 C CN1260402 C CN 1260402C
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Abstract
The present invention discloses a method for producing zone melting silicon single crystals through the combination of gas-phase predoping and neutron irradiation doping. The method comprises: q. in gas-phase predoping, furnace charging, vacuum pumping, argon filling, preheating of silicon rods, material melting, doping, welding of seed crystals, crystal seeding, growth of narrow necks, shouldering, isodiametric growth, ending, tensile failure, gas stopping, furnace shutdown and furnace disassembly are carried out; in neutron irradiation doping, neutron irradiation doping is carried out to silicon single crystals produced through gas-phase predoping. Neutron irradiation doping comprises the calculation of the fluence of neutron irradiation doping, the design of a neutron irradiation device, the selection of the irradiation condition of neutron irradiation doping and the control of the irradiation condition of neutron irradiation doping. The present invention has the advantages that the irradiation yield of nuclear reactors is improved in multiples, and crystal lattice damage of neutron irradiation doping to silicon single crystals is effectively lowered.
Description
Technical field
The present invention relates to a kind of production method of zone-melted silicon single crystal, particularly relate to the production method of the zone-melted silicon single crystal of pre-doping of a kind of gas phase and neutron irradiation doping combination.
Background technology
As everyone knows, the core of modern information technologies and modern electronic technology is a semiconductor technology, and the semiconductor silicon single crystal material is most important semiconductor material (according to statistics in 2000: the semiconductor silicon single crystal material accounted for more than 95% of global semiconductor material).Main employing vertical pulling method or zone melting method production in the production process of semiconductor silicon single crystal.Wherein the silicon single-crystal of vertical pulling method production causes resistivity thermolability and reversibility owing to the oxygen level in the monocrystalline is high, cause the deficiency of czochralski silicon monocrystal normalization method difficulty and performance perameter in fabrication of semiconductor device such as high-frequency and high-voltage device and power device: zone melting and refining silicon Dan Pin is because its production characteristics, relatively total impurities low (particularly oxygen level is than low 2 orders of magnitude of pulling of crystals) so be the excellent material of manufacturing power device.For a long time, because zone-melted silicon single crystal adopts the adulterated mode of neutron irradiation that monocrystalline is mixed traditionally in a large number, the production cycle is long, the production cost height, industrial scale is limited by the throughput of nuclear reactor, limits and influenced the industry development of zone melting single-crystal greatly.
Summary of the invention
Technical problem to be solved by this invention is: under the prerequisite of guaranteeing the monocrystalline quality, a kind of effective shortening neutron irradiation time is provided, reduces the neutron irradiation cost, increase substantially the pre-doping of gas phase of nuclear reactor irradiation processing zone-melted silicon single crystal throughput and the production method of the zone-melted silicon single crystal that the neutron irradiation doping is made up.
The technical solution adopted in the present invention is: the production method of the zone-melted silicon single crystal of pre-doping of a kind of gas phase and neutron irradiation doping combination is to be finished by following steps:
1) at first carry out gas phase and mix in advance, step is as follows:
(1) shove charge, vacuumize, applying argon gas;
(2) silicon rod preheating: open generator power, start filament voltage;
(3) change material: the regulating voltage set(ting)value transfers the 2-4rpmization material to 40-00% in the startup;
(4) mix: open the doping switch on the touch-screen, on the impurity gas control device, set the gas flow controlled variable
(5) welding seed crystal: start down and go to 10rpm, seed crystal is moved up and contact with melting zone point, produce a melt back district, transmission adjustment zone shape in startup top makes it into a funnel type;
(6) seeding: start the upper and lower part transport unit simultaneously, adjust voltage setting value;
(7) the thin neck of growing;
(8) shouldering: begin shouldering behind the thin neck of having grown;
(9) isodiametric growth: shouldering after require diameter, beginning isodiametric growth monocrystalline;
(10) finish up, break;
(11) stop the supple of gas or steam;
(12) blowing out, tear stove open;
2) neutron irradiation mixes
The pre-silicon single-crystal of producing that mixes of gas phase is carried out the neutron irradiation doping again, and concrete steps are as follows:
(1) calculating of neutron irradiation doping fluence, that is: the calculating of flux-time;
(2) neutron irradiation device design;
(3) selection of neutron irradiation doping radiation parameter;
(4) neutron irradiation doping radiation parameter control.
The present invention has following positive effect:
(1) increased exponentially the irradiation output of nuclear reactor, (2) have effectively reduced neutron irradiation and have mixed to the lattice damage of silicon single-crystal.Promptly because the production technology of the zone-melted silicon single crystal that the present invention adopts pre-doping of gas phase and neutron irradiation to mix to be made up, more traditional single neutron irradiation doped single crystal production method, shortened duct holding time and the irradiation doping processing cycle of silicon single-crystal in nuclear reactor, reduction by a relatively large margin the adulterated production cost of neutron irradiation, and significantly improved at the limited nuclear reactor of china natural resources in the throughput aspect the doping of neutron irradiation doped silicon monocrystalline neutron irradiation.Gas phase is pre-mixes and the mix production technology of the zone-melted silicon single crystal that makes up of neutron irradiation, and the macroscopic view that more traditional single gas phase doping monocrystalline production method has improved zone-melted silicon single crystal is resistivity evenness, the microcell resistivity striped that has reduced zone-melted silicon single crystal and the accuracy of single-crystal doped target radially.
Description of drawings
Fig. 1 is mix the in advance gas mixing device gas circuit synoptic diagram in stage of gas phase of the present invention;
Fig. 2 is the adulterated irradiator synoptic diagram of neutron irradiation of the present invention
Wherein:
1, nuclear reactor 2, silicon single-crystal
3, irradiation vessel 4, irradiator
5, locating device 6, swivel arrangement
7, monitoring device
Embodiment
Provide specific embodiment below, further specify the present invention and how to realize.
1. at first carry out gas phase and mix in advance, the example of the pre-doped portion of gas phase is as follows:
1) major equipment and the starting material of production vapor doping zone-melted silicon single crystal:
Zone melting furnace: model: FZ-14-1, FZ-30; Doping controller: model: 0154E
Polysilicon: one-level material: basic boron 〉=9000.cm base phosphorus 〉=900 Ω .cm
CFZ material: basic boron 〉=600 Ω .cm base phosphorus 〉=400 Ω .cm
2) concrete steps of the production method of the pre-doped region silicon crystal of gas phase:
(1) shove charge, find time, applying argon gas:
The operator cleans burner hearth and coil, reverberator and crystal clamper with vacuum cleaner, adjusts coil and reverberator level.From the vinyl film of cleaning, take out polycrystalline rod, then polycrystalline rod is fixed on the crystal clamper.Seed crystal is packed on the seed crystal fixed chuck.Polycrystalline rod is moved down, make its head enter graphite annulus inside, and as much as possible near coil.Close furnace chamber, fire door, tighten the fire door standing bolt, vacuumize, applying argon gas.Chamber pressure is 0.050mbar after finding time, and evacuated time depends on evacuation pressure, and when chamber pressure was 0.050mbar, evacuated time was about 240 seconds, is evacuated to automatically to find time automatically to finish.
(2) silicon rod preheating:
Open generator power, start filament voltage.Start high pressure, slowly regulate its set(ting)value to 35%-45%, present embodiment selects 40% for use.Generally redden with polycrystal and be as the criterion warm up time, is 5-20 minute between optional time.When anode voltage descends fast (the hint polycrystalline rod is warm), increase voltage to polycrystalline rod and be blush.
(3) change material:
The regulating voltage set(ting)value is to 40-60%, and present embodiment selects 50% for use, transfers in the startup changing material about 3rpm, prepares the welding seed crystal after the fusing fully of polycrystalline rod head.
(4) mix:
Open the doping switch on the touch-screen, and on impurity gas control device as shown in Figure 1, set this flow control of gas parameter.Example: draw Ф 60mm under 1/10000 phosphine gas concentration, resistivity 5-10 Ω .cm monocrystalline needs
Select for use:
Polycrystal N type (111) resistivity 400 Ω .cm Ф 75-85mm
Dopant dose phosphine gas flow: 4L/min.
(5) welding seed crystal:
Start down and go to 10rpm, seed crystal is moved up and contact with melting zone point, produce a melt back district, transmission adjustment zone shape in startup top makes it into a funnel type.After seed crystal red heat, reduce about voltage setting value to 40%
(6) seeding:
Its process: start the upper and lower part transport unit simultaneously, adjust voltage setting value; Guarantee that zone length is 8～10mm, silicon rod warm up time is 5～20 minutes.The diameter in melt back district reduces power and stops the bottom transmitting at 7～9mm, and increasing down changes, and stops top and transmits;
(7) the thin neck of growing:
This moment, thin neck wanted continuous regulatory work rate to keep constant melting zone height (15mm) in this process, constantly regulate speed to keep the constant diameter.
(8) shouldering:
Having grown begins shouldering behind the thin neck, speed control system shouldering angle in the use, and the shouldering angle should≤60 °.Control the shape in melting zone with the variation of power.
(9) isodiametric growth:
Shouldering after require diameter, beginning isodiametric growth monocrystalline.Calculate upward pressure speed according to material loading diameter, single crystal diameter and monocrystalline walking speed, calculation formula is as follows: V
On=(D
Down/ D
On)
2* V
Down
According to the lower run of the size of material loading and single crystal growing furnace regularly 1～2 hour, present embodiment regularly was 1.5 hours.Timer begins to discharge clamper when reporting to the police.
(10) finish up, break:
When upper limit was reported to the police, beginning reduces slowly went up speed, keeps growing at last of monocrystalline to break.Reduce top when breaking crystal gradually and press speed and power, make single crystal diameter be decreased to 10mm, break crystal.
(11) stop the supple of gas or steam:
On touch-screen, close the doping switch, and close the impurity gas control device.
(12) blowing out, tear stove open:
After break in the melting zone, carry out temperature-fall period at a slow speed.When observing the crystal blackening, stop heating.After the crystal cooling, open fire door and bottom furnace chamber, take out monocrystalline.
2. neutron irradiation mixes
The pre-silicon single-crystal of producing that mixes of gas phase is carried out the neutron irradiation doping again, and concrete steps are as follows:
The major equipment of this example is a light-water nuclear reactor.The adulterated concrete steps of neutron irradiation are as follows:
(1) calculating of neutron irradiation doping fluence (flux-time)
The calculating of the adulterated neutron fluence of neutron irradiation adopts currently known methods to calculate
Concrete formula: Ф=f (1/ ρ L-1/ ρ O)
In the formula: Ф: be thermal neutron fluence (n/cm2) f: be the doping coefficient
ρ L, ρ O: the target resistivity and the original resistivity that are respectively silicon single-crystal;
(2) neutron irradiation Design of device:
Neutron irradiation Design of device of the present invention will satisfy the location and the rotation of silicon single-crystal irradiation process;
(3) selection of neutron irradiation doping radiation parameter
Because mix and neutron irradiation mixes in the production of the zone-melted silicon single crystal that makes up in that gas phase is pre-, the neutron irradiation time is short relatively.Therefore, select during irradiation nuclear reactor move metastable time and irradiator place neutron fluence rate relatively low carry out irradiation.
(4) neutron irradiation doping radiation parameter control
Because the neutron fluence (flux-time) of the pre-zone-melted silicon single crystal that doping is made up with neutron irradiation that mixes of gas phase is relative little.Therefore, the irradiation process monitoring selects sensitivity higher with detector, so that more accurate monitoring neutron fluence, the model of present embodiment detector is: ZTTRb123.
Claims (5)
1. a gas phase is pre-mixes and the mix production method of the zone-melted silicon single crystal that makes up of neutron irradiation, it is characterized in that it being to be finished by following steps:
1) at first carry out gas phase and mix in advance, step is as follows:
(1) shove charge, find time, applying argon gas: clean burner hearth and coil, reverberator and crystal clamper; Adjust coil and reverberator level; Take out polycrystalline rod, be fixed on the crystal clamper; Seed crystal is packed on the seed crystal fixed chuck; Close furnace chamber, fire door, vacuumize applying argon gas;
(2) silicon rod preheating: open generator power, start filament voltage;
(3) change material: the regulating voltage set(ting)value transfers the 2-4rpmization material to 40-60% in the startup:
(4) mix: open the doping switch on the touch-screen, on the impurity gas control device, set the gas flow controlled variable;
(5) welding seed crystal: start down and go to 10rpm, seed crystal is moved up and contact with melting zone point, produce a melt back district, transmission adjustment zone shape in startup top makes it into a funnel type;
(6) seeding: start the upper and lower part transport unit simultaneously, adjust voltage setting value;
(7) the thin neck of growing;
(8) shouldering: begin shouldering behind the thin neck of having grown;
(9) isodiametric growth: shouldering after require diameter, beginning isodiametric growth monocrystalline;
(10) finish up, break;
(11) stop the supple of gas or steam;
(12) blowing out, tear stove open;
2) neutron irradiation mixes
The pre-silicon single-crystal of producing that mixes of gas phase is carried out the neutron irradiation doping again, and concrete steps are as follows:
(1) calculating of neutron irradiation doping fluence, that is: the calculating of flux-time;
(2) neutron irradiation device design:
Neutron irradiation device design of the present invention will be satisfied the location and the rotation of silicon single-crystal irradiation process;
(3) selection of neutron irradiation doping radiation parameter;
Select during irradiation nuclear reactor move metastable time and irradiator place neutron fluence rate relatively low carry out irradiation;
(4) neutron irradiation doping radiation parameter control.
2. gas phase according to claim 1 is pre-mixes and the mix production method of the zone-melted silicon single crystal that makes up of neutron irradiation, and it is characterized in that vacuumizing applying argon gas, to reach its constant pressure be 0.050mbar, and the pumpdown time is 240 seconds.
3. gas phase according to claim 1 is pre-mixes and the production method of silicon crystal is melted in the district of neutron irradiation doping group, it is characterized in that described silicon rod warm up time is 5～20 minutes.
4. gas phase according to claim 1 is pre-mixes and the mix production method of the zone-melted silicon single crystal that makes up of neutron irradiation, it is characterized in that the described seeding stage, and zone length is 8～10mm, and silicon rod warm up time is 5～20 minutes.
5. the production method of the zone-melted silicon single crystal of pre-doping of gas phase according to claim 1 and neutron irradiation doping combination is characterized in that the described shouldering stage, and the shouldering angle is answered≤60 °.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371505C (en) * | 2005-08-30 | 2008-02-27 | 河北工业大学 | Germanium blending method for zone-melting silicon monocrystal by liquid smearing method |
| CN100339513C (en) * | 2006-04-19 | 2007-09-26 | 天津市环欧半导体材料技术有限公司 | Electric control system of zone-melted silicon single crystal furnace |
| CN1333114C (en) * | 2006-04-21 | 2007-08-22 | 天津市环欧半导体材料技术有限公司 | Process for preparing vapor doping zone-melted silicon single crystal |
| CN1325701C (en) * | 2006-04-26 | 2007-07-11 | 天津市环欧半导体材料技术有限公司 | Process for preparing vapor pre-doping and neutron irradiation doping combined zone-melted silicon single crystal |
| CN102080265B (en) * | 2009-11-26 | 2012-11-28 | 有研半导体材料股份有限公司 | Improved thermal treatment process for neutron-doped crystal |
| CN103866377A (en) * | 2012-12-14 | 2014-06-18 | 有研半导体材料股份有限公司 | Gas phase mixing system device and method used for obtaining zone-melting silicon single crystal with wide specific resistance range |
| CN106591948B (en) * | 2017-01-21 | 2019-10-25 | 台州市一能科技有限公司 | A kind of N-type polycrystalline silicon used for solar batteries and its production method |
| CN108411357A (en) * | 2018-04-13 | 2018-08-17 | 天津市环欧半导体材料技术有限公司 | A kind of doper and method improving zone-melted vapor doping stability |
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