CN109797374A - A kind of preparation method and its batch preparation of silicon carbide substrates - Google Patents
A kind of preparation method and its batch preparation of silicon carbide substrates Download PDFInfo
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- CN109797374A CN109797374A CN201910036447.7A CN201910036447A CN109797374A CN 109797374 A CN109797374 A CN 109797374A CN 201910036447 A CN201910036447 A CN 201910036447A CN 109797374 A CN109797374 A CN 109797374A
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Abstract
The invention discloses a kind of preparation method of silicon carbide substrates and its batch preparations.After etching silicon carbide wafer, one layer of graphene is grown on its surface, then using it as seed crystal, the growth on its surface is continued using chemical vapour deposition technique, silicon carbide substrates is prepared.This method short preparation period, the consistency of performance for the silicon carbide substrates being prepared is good, and qualification rate is up to 90% or more, and the resistivity for the p-type silicon carbide substrates being prepared is below 0.5 Ω cm, the resistivity of N-type silicon carbide substrates is in 0.01-0.02 Ω cm, and micropipe density is in 0.1cm‑2Below.
Description
Technical field
The invention belongs to technical field of semiconductor, and in particular to a kind of preparation method and its batch of silicon carbide substrates
The preparation method and its batch preparation of preparation method more particularly to a kind of p-type or N-type silicon carbide substrates.
Background technique
Silicon carbide (SiC) is after first generation Semiconducting Silicon Materials, germanium and the second carrying semiconductor material GaAs, indium phosphide
The third generation semiconductor material to grow up.The forbidden bandwidth of carbofrax material is 2~3 times of silicon and GaAs, so that partly leading
Body device can 500 DEG C or more at a temperature of work and with transmitting blue light ability；Carbofrax material is than silicon and GaAs
It is intended to the high breakdown electric field of high an order of magnitude, determines that sic semiconductor device has high pressure, powerful performance；High
Saturated electron drift velocity and low-k determine the high frequency of device, high speed operation performance；Thermal conductivity is 3.3 times of silicon,
10 times of GaAs, it is meant that its good heat conductivity can greatly improve the integrated level of circuit, reduce cooling heat radiation system, from
And greatly reduce the volume of complete machine.
Therefore, constantly improve with carbofrax material and device technology, part silicon field is carbonized silicon gradually and is substituted.
It is special since silicon carbide has the characteristics that broad-band gap, high critical breakdown strength, high thermal conductivity, high electronics are saturated elegant rate
It is not suitble to high-power, high-voltage power electronic device, becomes the research hotspot of current field of power electronics.
Current main problem is: one, silicon carbide substrates are grown by PVT, are being processed into substrate by cutting throwing, total
Process-cycle as long as the wheat harvesting period so that the production cost of silicon carbide substrates is high, delayed silicon carbide power
The fast development of electronic device；Second is that low resistance p-type silicon carbide substrates can not be produced, the growth of traditional p-type silicon carbide substrates
Method is, by chemical vapor deposition method growing P-type silicon carbide epitaxial layers in N-type silicon carbide substrates, then by the back side
Reduction process all removes N-type silicon carbide substrates to obtain p-type silicon carbide wafer, as shown in Figure 1.But this technology needs
N-type silicon carbide substrates are all ground away, the process-cycle is longer, and the N-type silicon carbide substrates after use cannot recycle,
Production cost is higher, is unfavorable for industrialization promotion.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of silicon carbide substrates and its batch preparations.By by carbon
After SiClx wafer engraving, one layer of graphene is grown on its surface and is continued then using it as seed crystal using chemical vapour deposition technique
On its surface, silicon carbide substrates are prepared in growth.This method short preparation period, the performance one for the silicon carbide substrates being prepared
Cause property is good, and qualification rate is up to 90% or more.
The technical scheme adopted by the invention is as follows:
A kind of preparation method of silicon carbide substrates, the preparation method comprises the following steps:
(1) etching in situ is carried out to silicon carbide wafer；
(2) the silicon carbide wafer surface after etching in situ grows graphene, obtains the silicon carbide that graphene is contained on surface
Seed crystal；
(3) silicon carbide substrates are grown in the silicon carbide seed that graphene is contained on surface using chemical vapour deposition technique；
(4) silicon carbide substrates are removed from the silicon carbide seed containing graphene, the silicon carbide substrates can be obtained.
Further, the silicon carbide seed for containing graphene in surface obtained by step (2), continuous circulation step are reused
(3) and batch preparation silicon carbide substrates can be realized in (4), and the consistency of performance of the silicon carbide substrates prepared in batches in this way is protected
It holds preferably, and qualification rate is up to 90% or more.
The step (1) is specifically includes the following steps: silicon carbide wafer is placed in epitaxial furnace, in maintenance extension furnace cavity
Pressure be 10mbar-1000mbar, hydrogen is passed through at 1200-1300 DEG C and carries out etching in situ.
Further, the flow of the hydrogen is 10slm-200slm.The time etched in situ is 3-10min.
The step (2) is specifically includes the following steps: increase temperature to 1400-1600 DEG C, in pressure same as step (1)
Under strong, carbon source is introduced, reacts 5-20min, the silicon carbide wafer surface after etching in situ grows graphene.
Further, the carbon source is C2H4Or C3H8；The flow of the carbon source is 0.5~20sccm.
The step (3) specifically includes the following steps: the silicon carbide seed that graphene is contained on surface is placed in epitaxial furnace,
Maintaining the pressure in extension furnace cavity is 20mbar-200mbar, and hydrogen, silicon source, carbon source are passed through at 1500-1680 DEG C and is mixed
It miscellaneous dose, maintains 3~6 hours, growth obtains the silicon carbide of 300~600um thickness in the silicon carbide seed that graphene is contained on surface
Substrate.
Further, the hydrogen, silicon source, carbon source, dopant flow be respectively 10slm-200slm, 2sccm-
100sccm、2sccm-100sccm、0.2sccm-50sccm。
Further, the silicon source is SiH4Or SiHCl3；The carbon source is C2H4Or C3H8；The dopant be nitrogen or
Trimethyl aluminium；When the dopant is nitrogen, N-type silicon carbide substrates are prepared；When the dopant is trimethyl aluminium,
The p-type silicon carbide substrates being prepared.
In step (4), the stripping means are as follows: the two sides for the silicon carbide plate that step (3) obtains is attached to two panels resin
On plate, apply the cross force of opposite direction to upper and lower two panels resin plate, the silicon carbide for making carborundum crystals and surface contain graphene
The separation of seed crystal.
Further, after the step (4), further include the steps that cleaning and degumming, what is obtained after cleaning and degumming contains stone
The silicon carbide seed of black alkene can reuse, for regrowing silicon carbide substrates.
Compared with prior art, the invention has the following advantages that
1. the period for preparing silicon carbide substrates is short, can be completed within a few hours；
2. processing flow of the invention is simple relative to traditional diamond-making technique, the processes such as slice, grinding can not be used,
Reduce equipment investment；
3. reduce relative to traditional diamond-making technique and the processes such as cut, grind, not the cutting of silicon carbide substrates, abrasive wear can be with
Greatly improve the utilization rate of silicon carbide substrates；
4. it can be used repeatedly after degumming for the silicon carbide seed containing graphene for growing silicon carbide substrates in batches,
The consistency of performance of the silicon carbide substrates of batch production out in this way is good；
5. the qualification rate for the silicon carbide substrates that method of the invention prepares is higher, and up to 90% or more；
6. the resistivity for the p-type silicon carbide substrates that the method according to the invention prepares is in 0.5 Ω .cm hereinafter, N-type carbon
The resistivity of silicon substrate is in 0.01-0.02 Ω .cm, and micropipe density is in 0.1cm-2Below.
Detailed description of the invention
Fig. 1 is the flow process chart of Conventional silicon carbide substrate；
Fig. 2 is the flow process chart of silicon carbide substrates in the present invention.
Fig. 3 is the raman spectrogram for the silicon carbide seed that graphene is contained on surface in the present invention；
Fig. 4 is the micro-pipe distribution map of 4 inches of N-type silicon carbide substrates prepared by the embodiment of the present invention 1.
Specific embodiment
The present invention is described in detail for aggregate embodiment and Figure of description below.
Embodiment 1
A kind of preparation method of the silicon carbide substrates of 4 inches of 350um thickness of N-type, comprising the following steps:
(1) silicon carbide wafer of 4 inches of N-types of 1mm thickness is placed in the extension furnace cavity of 100mbar air pressure, temperature
At 1250 DEG C of degree, it is passed through 50slm H2Carry out etching in situ, time 5min；
(2) temperature is increased to 1550 DEG C, under same pressure, introduces C2H4, flow 10sccm, maintenance 8min are obtained
Contain the silicon carbide seed of graphene in surface；
(3) silicon carbide seed that graphene is contained in face is put into same epitaxial furnace, heating temperature is to 1650 DEG C, pressure
It maintains between 100mbar, is passed through the H of 100slm2, 40sccm SiH4, 20sccm C2H4, while being passed through dopant N2,
Flow is 10sccm, is maintained 3.5 hours, forms the silicon carbide substrates of 0.35mm thickness in seed crystal face；
(4) two sides for the silicon carbide plate that step (3) obtains is attached on two panels resin plate, upper and lower two panels resin plate is applied
The cross force of opposite direction, the separation for the silicon carbide seed for making carborundum crystals and surface contain graphene；
(5) the N-type silicon carbide substrates can be obtained in cleaning and degumming, and resistivity is 0.017 Ω .cm, and micropipe density exists
0.04cm-2, as shown in Figure 4；It is re-used after the silicon carbide seed recycling containing graphene after cleaning and degumming.
Embodiment 2
A kind of batch preparation of the silicon carbide substrates of 6 inches of 350um thickness of N-type, comprising the following steps:
(1) silicon carbide wafer of 6 inches of N-types of 1.5mm thickness is placed in the extension furnace cavity of 100mbar air pressure,
At 1250 DEG C of temperature, it is passed through 50slm H2Carry out etching in situ, time 5min；
(2) temperature is increased to 1550 DEG C, under same pressure, introduces C2H4, flow 10sccm, maintenance 8min are obtained
Contain the silicon carbide seed of graphene in surface；
(3) silicon carbide seed that graphene is contained in face is put into same epitaxial furnace, heating temperature is to 1650 DEG C, pressure
It maintains between 100mbar, is passed through the H of 100slm2, 40sccm SiH4, 20sccm C2H4, while being passed through dopant N2,
Flow is 10sccm, is maintained 3.5 hours, forms the silicon carbide substrates of 0.35mm thickness in seed crystal face；
(4) two sides for the silicon carbide plate that step (3) obtains is attached on two panels resin plate, upper and lower two panels resin plate is applied
The cross force of opposite direction, the separation for the silicon carbide seed for making carborundum crystals and surface contain graphene；
(5) silicon carbide substrates, the silicon carbide seed containing graphene after cleaning and degumming can be obtained in cleaning and degumming
It is re-used after recycling, and repeats step (3)-(5), the batch preparation of the N-type silicon carbide substrates can be realized.
The resistivity for the silicon carbide substrates that the present embodiment obtains is 0.015 Ω .cm, and micropipe density is in 0.06cm-2。
Embodiment 3
A kind of preparation method of the silicon carbide substrates of 6 inches of 500um thickness of N-type, comprising the following steps:
(1) silicon carbide wafer of 6 inches of N-types of 1.5mm thickness is placed in the extension furnace cavity of 100mbar air pressure,
At 1250 DEG C of temperature, it is passed through 50slm H2Carry out etching in situ, time 5min；
(2) temperature is increased to 1550 DEG C, under same pressure, introduces C2H4, flow 10sccm, maintenance 8min are obtained
Contain the silicon carbide seed of graphene in surface；
(3) silicon carbide seed that graphene is contained in face is put into same epitaxial furnace, heating temperature is to 1650 DEG C, pressure
It maintains between 100mbar, is passed through the H of 100slm2, 40sccm SiH4, 20sccm C2H4, while being passed through dopant N2,
Flow is 10sccm, is maintained 5 hours, forms the silicon carbide substrates of 0.5mm thickness in seed crystal face；
(4) two sides for the silicon carbide plate that step (3) obtains is attached on two panels resin plate, upper and lower two panels resin plate is applied
The cross force of opposite direction, the separation for the silicon carbide seed for making carborundum crystals and surface contain graphene；
(5) the N-type silicon carbide substrates can be obtained in cleaning and degumming, and resistivity is 0.018 Ω .cm, and micropipe density exists
0.07cm-2；It is re-used after the silicon carbide seed recycling containing graphene after cleaning and degumming.
Embodiment 4
A kind of preparation method of the silicon carbide substrates of 4 inches of 350um thickness of p-type, comprising the following steps:
(1) silicon carbide wafer of 4 inches of N-types of 1.0mm thickness is placed in the extension furnace cavity of 100mbar air pressure,
At 1250 DEG C of temperature, it is passed through 80slm H2Carry out etching in situ, time 3min；
(2) temperature is increased to 1550 DEG C, under same pressure, introduces C3H8, flow 10sccm, maintenance 10min are obtained
Contain the silicon carbide seed of graphene to surface；
(3) silicon carbide seed that graphene is contained in face is put into same epitaxial furnace, heating temperature is to 1630 DEG C, pressure
It maintains between 150mbar, is passed through the H of 150slm2, 40sccm SiH4, 20sccm C2H4, while being passed through dopant front three
Base aluminium, flow 20sccm are maintained 3.5 hours, form the p-type silicon carbide substrates of 0.35mm thickness in seed crystal face；
(4) two sides for the silicon carbide plate that step (3) obtains is attached on two panels resin plate, upper and lower two panels resin plate is applied
The cross force of opposite direction, the separation for the silicon carbide seed for making carborundum crystals and surface contain graphene；
(5) the p-type silicon carbide substrates can be obtained in cleaning and degumming, and resistivity is in 0.39 Ω .cm hereinafter, micro-pipe is close
Degree is in 0.05cm-2；It is re-used after the silicon carbide seed recycling containing graphene after cleaning and degumming.
Embodiment 5
A kind of preparation method of the silicon carbide substrates of 6 inches of 350um thickness of p-type, comprising the following steps:
(1) silicon carbide wafer of 6 inches of N-types of 1.5mm thickness is placed in the extension furnace cavity of 100mbar air pressure,
At 1250 DEG C of temperature, it is passed through 80slm H2Carry out etching in situ, time 3min；
(2) temperature is increased to 1550 DEG C, under same pressure, introduces C3H8, flow 10sccm, maintenance 10min are obtained
Contain the silicon carbide seed of graphene to surface；
(3) silicon carbide seed that graphene is contained in face is put into same epitaxial furnace, heating temperature is to 1630 DEG C, pressure
It maintains between 150mbar, is passed through the H of 150slm2, 40sccm SiH4, 20sccm C2H4, while being passed through dopant front three
Base aluminium, flow 20sccm are maintained 3.5 hours, form the p-type silicon carbide substrates of 0.35mm thickness in seed crystal face；
(4) two sides for the silicon carbide plate that step (3) obtains is attached on two panels resin plate, upper and lower two panels resin plate is applied
The cross force of opposite direction, the separation for the silicon carbide seed for making carborundum crystals and surface contain graphene；
(5) the p-type silicon carbide substrates can be obtained in cleaning and degumming, and resistivity is in 0.45 Ω .cm hereinafter, micro-pipe is close
Degree is in 0.07cm-2；It is re-used after the silicon carbide seed recycling containing graphene after cleaning and degumming.
Embodiment 6
A kind of preparation method of the silicon carbide substrates of 6 inches of 500um thickness of p-type, comprising the following steps:
(1) silicon carbide wafer of 6 inches of N-types of 1.5mm thickness is placed in the extension furnace cavity of 100mbar air pressure,
At 1250 DEG C of temperature, it is passed through 80slm H2Carry out etching in situ, time 3min；
(2) temperature is increased to 1550 DEG C, under same pressure, introduces C3H8, flow 10sccm, maintenance 10min are obtained
Contain the silicon carbide seed of graphene to surface；
(3) silicon carbide seed that graphene is contained in face is put into same epitaxial furnace, heating temperature is to 1630 DEG C, pressure
It maintains between 150mbar, is passed through the H of 150slm2, 40sccm SiH4, 20sccm C2H4, while being passed through dopant front three
Base aluminium, flow 20sccm are maintained 5 hours, form the p-type silicon carbide substrates of 0.5mm thickness in seed crystal face；
(4) two sides for the silicon carbide plate that step (3) obtains is attached on two panels resin plate, upper and lower two panels resin plate is applied
The cross force of opposite direction, the separation for the silicon carbide seed for making carborundum crystals and surface contain graphene；
(5) the p-type silicon carbide substrates can be obtained in cleaning and degumming, and resistivity is in 0.47 Ω .cm hereinafter, micro-pipe is close
Degree is in 0.06cm-2Below；It is re-used after the silicon carbide seed recycling containing graphene after cleaning and degumming.
It is above-mentioned to be retouched in detail referring to what preparation method and its batch preparation of the embodiment to a kind of silicon carbide substrates carried out
It states, is illustrative without being restrictive, several embodiments can be enumerated according to limited range, therefore do not departing from this
Change and modification under invention general plotting should belong within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of silicon carbide substrates, which is characterized in that the preparation method comprises the following steps:
(1) etching in situ is carried out to silicon carbide wafer；
(2) the silicon carbide wafer surface after etching in situ grows graphene, obtains the silicon carbide seed that graphene is contained on surface；
(3) silicon carbide substrates are grown in the silicon carbide seed that graphene is contained on surface using chemical vapour deposition technique；
(4) silicon carbide substrates are removed from the silicon carbide seed containing graphene, the silicon carbide substrates can be obtained.
2. the preparation method of silicon carbide substrates according to claim 1, which is characterized in that obtained by recycling step (2)
Contain the silicon carbide seed of graphene to surface, batch preparation silicon carbide substrates can be realized in continuous circulation step (3) and (4).
3. the preparation method of silicon carbide substrates according to claim 1 or 2, which is characterized in that the step (1) is specifically wrapped
It includes following steps: silicon carbide wafer is placed in epitaxial furnace, maintaining the pressure in extension furnace cavity is 10mbar-1000mbar,
It is passed through hydrogen at 1200-1300 DEG C and carries out etching in situ.
4. the preparation method of silicon carbide substrates according to claim 3, which is characterized in that the flow of the hydrogen is
10slm-200slm。
5. the preparation method of silicon carbide substrates according to claim 1 or 2, which is characterized in that the step (2) is specifically wrapped
It includes following steps: increasing temperature to 1400-1600 DEG C, under pressure same as step (1), introduce carbon source, react 5-
20min, the silicon carbide wafer surface after etching in situ grow graphene.
6. the preparation method of silicon carbide substrates according to claim 5, which is characterized in that the carbon source is C2H4Or C3H8；
The flow of the carbon source is 0.5~20sccm.
7. the preparation method of silicon carbide substrates according to claim 1 or 2, which is characterized in that the step (3) is specifically wrapped
It includes following steps: the silicon carbide seed that graphene is contained on surface is placed in epitaxial furnace, the pressure in maintenance extension furnace cavity is
20mbar-200mbar is passed through hydrogen, silicon source, carbon source and dopant at 1500-1680 DEG C, maintains 3~6 hours, on surface
Growth obtains the silicon carbide substrates of 300~600um thickness in silicon carbide seed containing graphene.
8. the preparation method of silicon carbide substrates according to claim 7, which is characterized in that the hydrogen, silicon source, carbon source,
The flow of dopant is respectively 10slm-200slm, 2sccm-100sccm, 2sccm-100sccm, 0.2sccm-50sccm.
9. the preparation method of silicon carbide substrates according to claim 7, which is characterized in that the silicon source is SiH4Or
SiHCl3；The carbon source is C2H4Or C3H8；The dopant is nitrogen or trimethyl aluminium；When the dopant is nitrogen, preparation
Obtain N-type silicon carbide substrates；When the dopant is trimethyl aluminium, p-type silicon carbide substrates are prepared.
10. the preparation method of silicon carbide substrates according to claim 1 or 2, which is characterized in that described in step (4)
Stripping means are as follows: the two sides for the silicon carbide plate that step (3) obtains is attached on two panels resin plate, upper and lower two panels resin plate is applied
The cross force of opposite direction, the separation for the silicon carbide seed for making carborundum crystals and surface contain graphene；The step (4) it
Afterwards, further include the steps that cleaning and degumming.
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| CN111235633A (en) * | 2020-01-16 | 2020-06-05 | 中国科学院半导体研究所 | Method for preparing self-supporting silicon carbide wafer on surface of silicon melt through CVD |
| CN113774494A (en) * | 2021-11-15 | 2021-12-10 | 浙江大学杭州国际科创中心 | Stripping method and stripping device for semi-insulating silicon carbide single crystal wafer |
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Application publication date: 20190524 |