CN105948055B - The method of purification of semiconductor high-purity silicon carbide micro-powder - Google Patents
The method of purification of semiconductor high-purity silicon carbide micro-powder Download PDFInfo
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- CN105948055B CN105948055B CN201610370116.3A CN201610370116A CN105948055B CN 105948055 B CN105948055 B CN 105948055B CN 201610370116 A CN201610370116 A CN 201610370116A CN 105948055 B CN105948055 B CN 105948055B
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- silicon carbide
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 64
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000000843 powder Substances 0.000 title claims abstract description 61
- 239000004065 semiconductor Substances 0.000 title claims abstract description 32
- 238000000746 purification Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 37
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002002 slurry Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000005554 pickling Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Carbon And Carbon Compounds (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a kind of method of purification of semiconductor high-purity silicon carbide micro-powder, belong to silicon carbide micro-powder production technical field.Solves the problem of silicon carbide micro-powder impurity content of prior art production is higher, and purification difficulty is big.It comprises the following steps：(1) size mixing：By in ground silicon carbide micro-powder input agitator, deionized water is added to adjust pulp density；(2) pickling：Add the sulfuric acid that mass fraction is 98%；(3) heating stirring：Slurry is heated to 40 80 DEG C, and stirred old；(4) mixed acid is added：Mixed acid is added in old good slurry；(5) heating stirring：Slurry after addition mixed acid is heated to 50 80 DEG C, stirs, is old；(6) rinse：Material after will be old squeeze into filter press with deionized water rinsing to pH value be 5 6.5, produce product.The inventive method is adapted to purify semiconductor high-purity silicon carbide micro-powder.
Description
Technical field
The present invention relates to a kind of method of purification of semiconductor high-purity silicon carbide micro-powder, belong to silicon carbide micro-powder production technology
Field.
Background technology
Carborundum because with inoxidizability is strong, elevated temperature strength is big, wear resistance is good, heat endurance is good, thermal coefficient of expansion is small,
Thermal conductivity is big, consistency and elasticity modulus is high, thermal shock resistance is good and the good characteristic such as resistant to chemical etching, in recent years as high-tech
One of the preferred material in skill field.In field of semiconductor manufacture, many engineerings are also all using silicon carbide ceramics.As semiconductor
The material powder of manufacture high-performance ceramic, must be requested that silicon carbide micro-powder has high-purity, ultra-fine, good dispersion characteristic, but
It is the silicon carbide micro-powder of prior art production because using mechanical crushing, impurity content is higher in silicon carbide micro-powder, and purity is difficult to
Reach semiconductor with requiring, cause product to devalue, added value is low.Such as Application No. 201310507885.X Chinese invention is special
Sharp " the pickling method of purification of miropowder of silicon carbide in submicro level ", is purified in pickling kettle using a pickling, although the work
Skill is simple, but product whole content is 99.0% after purification, does not reach the quality requirement of semiconductor high-purity silicon carbide micro-powder.
The content of the invention
It is simple to operation it is an object of the invention to provide a kind of method of purification of semiconductor high-purity silicon carbide micro-powder,
Product purity is more than 99.9% after purification.
The method of purification of described semiconductor high-purity silicon carbide micro-powder, comprises the following steps：
(1) size mixing：By in ground silicon carbide micro-powder input agitator, deionized water is added to adjust pulp density；
(2) pickling：Add the sulfuric acid that mass fraction is 98%；
(3) heating stirring：Slurry after acid adding is heated to 40-80 DEG C, it is old after stirring 5-10 hours at this temperature
8-15 hours；
(4) mixed acid is added：Add mixed acid in old good slurry, the mass ratio of mixed acid and silicon carbide micro-powder is 1:
15-20；
(5) heating stirring：Slurry after addition mixed acid is heated to 50-80 DEG C, stirs 5-10 hours at this temperature,
Old 8-15 hours；
(6) rinse：It is 5-6.5 that material after will be old, which is squeezed into filter press with deionized water rinsing to pH value, produces institute
The semiconductor high-purity silicon carbide micro-powder stated.
Described deionized water electrical conductivity is 5-30 μ s/cm.
The mass ratio of deionized water and silicon carbide micro-powder described in step (1) is 2-3:1.
The addition of sulfuric acid described in step (2) accounts for the 2-8% of silicon carbide micro-powder quality.
The addition of sulfuric acid described in step (2) accounts for the 5% of silicon carbide micro-powder quality.
In heating whipping process described in step (3), the slurry after acid adding is heated to 50-60 DEG C.
Mixed acid described in step (4) be the nitric acid that mass fraction is 68% and mass fraction be 47% hydrofluoric acid according to
2-3:What 1 mass ratio mixed.
The purity of described semiconductor high-purity silicon carbide micro-powder is more than 99.9%.
Compared with prior art the beneficial effects of the invention are as follows：
The present invention is purified using special pickling, is segmented, a point species adds, and makes the impurity in material repeat to dissolve, after purification
Silicon carbide micro-powder content can reach more than 99.9%, improve value-added content of product, time and labour saving and suitable production in enormous quantities.This
Invention overcomes the defects of traditional handicraft purifies repeatedly, greatly reduces the processing cost of high-purity carborundum micropowder, improves
Production efficiency.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
The method of purification of described semiconductor high-purity silicon carbide micro-powder, comprises the following steps：
(1) size mixing：By in ground silicon carbide micro-powder input agitator, deionized water is added to adjust pulp density；
(2) pickling：The sulfuric acid that mass fraction is 98% is added, the addition of sulfuric acid accounts for the 2% of silicon carbide micro-powder quality；
(3) heating stirring：Slurry after acid adding is heated to 40-50 DEG C, old 15 after stirring 10 hours at this temperature
Hour；
(4) mixed acid is added：The nitric acid and mass fraction that are 68% by mass fraction are added in old good slurry is
47% hydrofluoric acid is according to 2:The mass ratio of the mixed acid that 1 mass ratio mixes, mixed acid and silicon carbide micro-powder is 1:15；
(5) heating stirring：Slurry after addition mixed acid is heated to 50-60 DEG C, stirred 10 hours at this temperature, it is old
It is rotten 15 hours；
(6) rinse：It is 5 that material after will be old, which is squeezed into filter press with deionized water rinsing to pH value, is produced described
Semiconductor high-purity silicon carbide micro-powder.
Described deionized water electrical conductivity is 5 μ s/cm.
The purity of described semiconductor high-purity silicon carbide micro-powder is 99.95%.
Embodiment 2
The method of purification of described semiconductor high-purity silicon carbide micro-powder, comprises the following steps：
(1) size mixing：By in ground silicon carbide micro-powder input agitator, deionized water is added to adjust pulp density；
(2) pickling：The sulfuric acid that mass fraction is 98% is added, the addition of sulfuric acid accounts for the 8% of silicon carbide micro-powder quality；
(3) heating stirring：Slurry after acid adding is heated to 60-80 DEG C, old 8 is small after stirring 5 hours at this temperature
When；
(4) mixed acid is added：The nitric acid and mass fraction that are 68% by mass fraction are added in old good slurry is
47% hydrofluoric acid is according to 3:The mass ratio of the mixed acid that 1 mass ratio mixes, mixed acid and silicon carbide micro-powder is 1:20；
(5) heating stirring：Slurry after addition mixed acid is heated to 70-80 DEG C, stirred 5 hours at this temperature, it is old
It is rotten 8 hours；
(6) rinse：It is 6.5 that material after will be old, which is squeezed into filter press with deionized water rinsing to pH value, is produced described
Semiconductor high-purity silicon carbide micro-powder.
Described deionized water electrical conductivity is 30 μ s/cm.
The purity of described semiconductor high-purity silicon carbide micro-powder is 99.96%.
Embodiment 3
The method of purification of described semiconductor high-purity silicon carbide micro-powder, comprises the following steps：
(1) size mixing：By in ground silicon carbide micro-powder input agitator, deionized water is added to adjust pulp density；
(2) pickling：The sulfuric acid that mass fraction is 98% is added, the addition of sulfuric acid accounts for the 6% of silicon carbide micro-powder quality；
(3) heating stirring：Slurry after acid adding is heated to 50-60 DEG C, old 12 is small after stirring 8 hours at this temperature
When；
(4) mixed acid is added：The nitric acid and mass fraction that are 68% by mass fraction are added in old good slurry is
47% hydrofluoric acid is according to 2:The mass ratio of the mixed acid that 1 mass ratio mixes, mixed acid and silicon carbide micro-powder is 1:16；
(5) heating stirring：Slurry after addition mixed acid is heated to 60-70 DEG C, stirred 9 hours at this temperature, it is old
It is rotten 10 hours；
(6) rinse：It is 6 that material after will be old, which is squeezed into filter press with deionized water rinsing to pH value, is produced described
Semiconductor high-purity silicon carbide micro-powder.
Described deionized water electrical conductivity is 20 μ s/cm.
The purity of described semiconductor high-purity silicon carbide micro-powder is 99.94%.
Embodiment 4
The method of purification of described semiconductor high-purity silicon carbide micro-powder, comprises the following steps：
(1) size mixing：By in ground silicon carbide micro-powder input agitator, deionized water is added to adjust pulp density；
(2) pickling：The sulfuric acid that mass fraction is 98% is added, the addition of sulfuric acid accounts for the 5% of silicon carbide micro-powder quality；
(3) heating stirring：Slurry after acid adding is heated to 50-60 DEG C, old 12 is small after stirring 8 hours at this temperature
When；
(4) mixed acid is added：The nitric acid and mass fraction that are 68% by mass fraction are added in old good slurry is
47% hydrofluoric acid is according to 2.5:The mass ratio of the mixed acid that 1 mass ratio mixes, mixed acid and silicon carbide micro-powder is 1:
17；
(5) heating stirring：Slurry after addition mixed acid is heated to 60-70 DEG C, stirred 8 hours at this temperature, it is old
It is rotten 12 hours；
(6) rinse：It is 5.5 that material after will be old, which is squeezed into filter press with deionized water rinsing to pH value, is produced described
Semiconductor high-purity silicon carbide micro-powder.
Described deionized water electrical conductivity is 15 μ s/cm.
The purity of described semiconductor high-purity silicon carbide micro-powder is 99.93%.
The impurity component such as table 1 in embodiment 4 is detected with SPECTROX-LabPro：
Table 1
As can be seen from Table 1, the semiconductor described in embodiment 4 is with the content of impurities of high-purity silicon carbide micro-powder
0.07%, i.e. silicon carbide micro-powder purity is 99.93%.
Claims (5)
1. a kind of method of purification of semiconductor high-purity silicon carbide micro-powder, it is characterised in that comprise the following steps：
(1) size mixing：By in ground silicon carbide micro-powder input agitator, deionized water is added to adjust pulp density；
(2) pickling：Add the sulfuric acid that mass fraction is 98%；
(3) heating stirring：Slurry after acid adding is heated to 40-80 DEG C, stirs old 8-15 after 5-10 hours at this temperature
Hour；
(4) mixed acid is added：Add mixed acid in old good slurry, the mass ratio of mixed acid and silicon carbide micro-powder is 1:15-
20；
(5) heating stirring：Slurry after addition mixed acid is heated to 50-80 DEG C, stirred at this temperature 5-10 hours, it is old
8-15 hours；
(6) rinse：It is 5-6.5 that material after will be old, which is squeezed into filter press with deionized water rinsing to pH value, is produced described
Semiconductor high-purity silicon carbide micro-powder, purity are more than 99.9%；
The mass ratio of deionized water and silicon carbide micro-powder described in step (1) is 2-3:1；
Mixed acid described in step (4) be the nitric acid that mass fraction is 68% and mass fraction be 47% hydrofluoric acid according to 2-3:
What 1 mass ratio mixed.
2. the method for purification of semiconductor high-purity silicon carbide micro-powder according to claim 1, it is characterised in that：Described goes
Ion water conductivity is 5-30 μ s/cm.
3. the method for purification of semiconductor high-purity silicon carbide micro-powder according to claim 2, it is characterised in that：Step (2)
The addition of described sulfuric acid accounts for the 2-8% of silicon carbide micro-powder quality.
4. the method for purification of semiconductor high-purity silicon carbide micro-powder according to claim 3, it is characterised in that：Step (2)
The addition of described sulfuric acid accounts for the 5% of silicon carbide micro-powder quality.
5. the method for purification of semiconductor high-purity silicon carbide micro-powder according to claim 4, it is characterised in that：Step (3)
In described heating whipping process, the slurry after acid adding is heated to 50-60 DEG C.
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|---|---|---|---|---|
| CN101525134A (en) * | 2009-04-02 | 2009-09-09 | 山东大学 | Method for preparing cubic silicon carbide ultrafine powder by using waste plastic at low temperature |
| CN101659412A (en) * | 2009-09-18 | 2010-03-03 | 江苏乐园新材料集团有限公司 | Preparation method of single crystal silicon carbide special materials |
| CN102328929A (en) * | 2011-07-22 | 2012-01-25 | 周彬 | Purifying process of silicon carbide micropowder |
| CN103232039A (en) * | 2013-05-16 | 2013-08-07 | 周彬 | Silicon carbide filter cake cyclone purifying process |
| CN103523783A (en) * | 2013-10-25 | 2014-01-22 | 宁夏机械研究院（有限责任公司） | Device and process for synchronously removing free carbon in silicon carbide micro powder |
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2016
- 2016-05-30 CN CN201610370116.3A patent/CN105948055B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525134A (en) * | 2009-04-02 | 2009-09-09 | 山东大学 | Method for preparing cubic silicon carbide ultrafine powder by using waste plastic at low temperature |
| CN101659412A (en) * | 2009-09-18 | 2010-03-03 | 江苏乐园新材料集团有限公司 | Preparation method of single crystal silicon carbide special materials |
| CN102328929A (en) * | 2011-07-22 | 2012-01-25 | 周彬 | Purifying process of silicon carbide micropowder |
| CN103232039A (en) * | 2013-05-16 | 2013-08-07 | 周彬 | Silicon carbide filter cake cyclone purifying process |
| CN103523783A (en) * | 2013-10-25 | 2014-01-22 | 宁夏机械研究院（有限责任公司） | Device and process for synchronously removing free carbon in silicon carbide micro powder |
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Address after: 276700 Hou Gao Hu Village, Linshu Town, Linshu County, Linyi, Shandong Patentee after: Yamada New Material Group Co.,Ltd. Address before: 276700 Hou Gao Hu Cun, Linshu Town, Linyi City, Shandong Province Patentee before: SHANTIAN ABRASIVE CO.,LTD. |
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Denomination of invention: Purification method of high purity silicon carbide powder for semiconductor Effective date of registration: 20220111 Granted publication date: 20171222 Pledgee: Shandong Linshu Rural Commercial Bank Co.,Ltd. Pledgor: Yamada New Material Group Co.,Ltd. Registration number: Y2022980000330 |
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