CN102989373B - The method of HTHP synthesized semiconductor diamond - Google Patents
The method of HTHP synthesized semiconductor diamond Download PDFInfo
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- CN102989373B CN102989373B CN201210499962.7A CN201210499962A CN102989373B CN 102989373 B CN102989373 B CN 102989373B CN 201210499962 A CN201210499962 A CN 201210499962A CN 102989373 B CN102989373 B CN 102989373B
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Abstract
The present invention relates to a kind of method of HTHP synthesized semiconductor diamond.The method take pure boron as diamond modifying element, with FeNiCo alloyed powder and high purity graphite powder for raw material, synthesized semiconductor graphite used for synthesizing diamond post is prepared through operations such as mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shapings, assemble with annexes such as pyrophillite mould, steel bowl, magnesia cup, graphite flake, conductive steel caps again, utilize cubic hydraulic press to make graphite be converted into semiconductor diamond in HTHP mode, then high-quality semiconductor diamond can be drawn through chemical treatment.The inventive method freely regulates and controls semiconductor diamond resistivity by regulating raw material different ratio mode, and output is high, and the semiconductor diamond prepared is more high temperature resistant than common diamond, and chemical inertness is better, and self-sharpening is strong.
Description
Technical field
The present invention relates to Diamond Synthesizing Technology field, be specifically related to a kind of method of HTHP synthesized semiconductor diamond.
Background technology
Diamond is commonly called as " spark ", the diamond that namely it has often been said, it is a kind of mineral be made up of pure carbon, is also the hardest material of occurring in nature.After confirming that diamond is made up of pure carbon 18th century, people just start the research to diamond, progress just in the 1950's by high pressure research and High-Voltage Experimentation technology, just obtain real success and develop rapidly, diamond is also widely used in various industry, technique industry.
Semiconductor diamond due to have more heat-resisting than common diamond, self-sharpening is strong. intensity is high, impact resistance is strong, chemical inertness is better, and the characteristic such as resistivity controllable.Making instrument except can be used for the original general diamond tool machinable material of processing, because its heat resistance is higher, therefore Fe race metal can be processed.Because under the high temperature of processing, general diamond can be changed into graphite by iron group metal, present industry processing iron group metal all adopts cubic boron nitride tool, but the various working ability of cubic boron nitride is the low level of diamond all comparatively, therefore can there be higher working (machining) efficiency semiconductor diamond replacement cubic boron nitride processing iron group metal.According to current development, it is expected to semiconductor diamond and will substitute common diamond gradually.But current known semiconductor artificial diamond synthesis process technology, not only cost is high, efficiency is low, and various performance is still difficult to the needs meeting people.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of HTHP synthesized semiconductor diamond of high efficiency, low cost, the method freely regulates and controls semiconductor diamond resistivity by regulating raw material different ratio mode, output is high, the semiconductor diamond prepared is more high temperature resistant than common diamond, chemical inertness is better, and self-sharpening is strong.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Design a kind of method of HTHP synthesized semiconductor diamond, mainly comprise the following steps: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, with pure boron (modifying element), FeNiCo alloyed powder (catalyst powder) and high purity graphite powder for raw material, and the weight ratio of three is pure boron: FeNiCo alloyed powder: high purity graphite powder=0.0001 ~ 0.5:30 ~ 70:70 ~ 30; Purity > 95%, the FeNiCo alloyed powder purity > 95%, high purity graphite powder purity > 98% of described pure boron.
When carrying out described HTHP mode and transforming, wherein Stress control is at 4.5 ~ 5.5GPa, and temperature controls at 1250 ~ 1500 DEG C.
Described FeNiCo alloyed powder is granularity 200 order ~ 500 object Fe70:Ni27:Co3 (wt%) alloyed powder.
The good scope of described raw-material part by weight is pure boron: FeNiCo alloyed powder: high purity graphite powder=0.001 ~ 0.4:30 ~ 70:70 ~ 30.
The better scope of described raw-material part by weight is pure boron: FeNiCo alloyed powder: high purity graphite powder=0.01 ~ 0.2:30 ~ 40:60 ~ 40.
The part by weight of described raw material the best is pure boron: FeNiCo alloyed powder: high purity graphite powder=0.01 ~ 0.05:36:54.
The present invention has actively useful effect:
The inventive method freely regulates and controls semiconductor diamond resistivity by regulating raw material different ratio mode, and output is high, and the semiconductor diamond prepared is more high temperature resistant than common diamond, and chemical inertness is better, and self-sharpening is strong.
Detailed description of the invention
The present invention is set forth further below in conjunction with specific embodiment.Tool equipment involved in following embodiment, if no special instructions, is conventional tool equipment, involved step method, if no special instructions, is conventional steps method.
The method of embodiment 1 one kinds of HTHP synthesized semiconductor diamonds: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, can obtain semiconductor diamond, key step is as follows:
Claim Fe70:Ni27:Co3 (wt%) alloyed powder 360 grams, 540 grams, high purity graphite powder, pure boron powder 5 grams of Homogeneous phase mixing, after make graphite column 10 post of Φ 37.5 × 27.5, with pyrophillite mould, steel bowl, magnesia cup, graphite flake, the accessory combinations such as conductive steel cap, after 120 DEG C of drying box dryings, on cubic hinge press, HTHP mode transforms, pressure is 4.8 ± 0.2GPa, temperature is 1350 DEG C, through conventional chemical purification process, obtain semiconductor diamond 316.53ct, per unit area yield 31.65ct crystal formation is irregular, black non transparent, there is incompleteness on crystalline form surface, related index refers to table 1.
The method of embodiment 2 one kinds of HTHP synthesized semiconductor diamonds: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, can obtain semiconductor diamond, its detailed step is as follows:
Claim Fe70:Ni27:Co3 (wt%) alloyed powder 360 grams, graphite powder 540 grams, pure boron powder 2 grams of Homogeneous phase mixing, after make graphite column 10 post of Φ 37.5 × 27.5, assemble with annexes such as pyrophillite mould, steel bowl, magnesia cup, graphite flake, conductive steel caps, after 120 DEG C of drying box dryings, on cubic hinge press, HTHP mode transforms, pressure is 5.0GPa, temperature is 1350 DEG C, through chemical purification process, obtains semiconductor diamond 482.26ct, per unit area yield 48.23ct crystal formation is octahedra, black non transparent, crystal thin silk fabric line is coarse, and related index refers to table 1.
The method of embodiment 3 one kinds of HTHP synthesized semiconductor diamonds: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, can obtain semiconductor diamond, its detailed step is as follows:
Claim Fe70:Ni27:Co3 (wt%) alloyed powder 360 grams, graphite powder 540 grams, pure boron powder 1 gram of Homogeneous phase mixing, after make graphite column 10 post of Φ 37.5 × 27.5, with accessory combinations such as pyrophillite mould, steel bowl, magnesia cup, graphite flake, conductive steel caps, after 120 DEG C of drying box dryings, on cubic hinge press, HTHP mode transforms, pressure is 5.0GPa, temperature is 1350 DEG C, through chemical purification process, obtains semiconductor diamond 579.10ct, per unit area yield 579.1ct, black non transparent, the complete octahedron of crystal formation, related index refers to table 1.
The method of embodiment 4 one kinds of HTHP synthesized semiconductor diamonds: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, can obtain semiconductor diamond, its detailed step is as follows:
Claim Fe70:Ni27:Co3 (wt%) alloyed powder 360 grams, graphite powder 540 grams, pure boron powder 0.5 gram of Homogeneous phase mixing, after make graphite column 10 post of Φ 37.5 × 27.5, with accessory combinations such as pyrophillite mould, steel bowl, magnesia cup, graphite flake, conductive steel caps, after 120 DEG C of drying box dryings, on cubic hinge press, HTHP mode transforms, pressure is 5.0GPa, temperature is 1350 DEG C, through chemical purification process, obtains semiconductor diamond 542.35ct, per unit area yield 54.24ct, black non transparent, the complete octahedron of crystal formation, related index refers to table 1.
The method of embodiment 5 one kinds of HTHP synthesized semiconductor diamonds: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, can obtain semiconductor diamond, its detailed step is as follows:
Claim Fe70:Ni27:Co3 (wt%) alloyed powder 360 grams, graphite powder 540 grams, pure boron powder 0.2 gram of Homogeneous phase mixing, after make graphite column 10 post of Φ 37.5 × 27.5, with accessory combinations such as pyrophillite mould, steel bowl, magnesia cup, graphite flake, conductive steel caps, after 120 DEG C of drying box dryings, on cubic hinge press, HTHP mode transforms, pressure is 5.0GPa, temperature is 1350 DEG C, through chemical purification process, obtains semiconductor diamond 747.16ct, per unit area yield 74.72ct, blueness has impurity transparent, and the complete hexakisooctahedron of crystal formation, related index refers to table 1.
The method of embodiment 6 one kinds of HTHP synthesized semiconductor diamonds: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, can obtain semiconductor diamond, its detailed step is as follows:
Claim Fe70:Ni27:Co3 (wt%) alloyed powder 360 grams, graphite powder 540 grams, pure boron powder 0.1 gram of Homogeneous phase mixing, after make graphite column 10 post of Φ 37.5 × 27.5, with accessory combinations such as pyrophillite mould, steel bowl, magnesia cup, graphite flake, conductive steel caps, after 120 DEG C of drying box dryings, on cubic hinge press, HTHP mode transforms, pressure is 5.0GPa, temperature is 1350 DEG C, through chemical purification process, obtains semiconductor diamond 723.85ct, per unit area yield 72.39ct, light yellow clear, the complete hexakisooctahedron of crystal formation, related index refers to table 1.
Embodiment 7 one kinds of semiconductor diamond production method main flow: a kind of method of HTHP synthesized semiconductor diamond: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, can obtain semiconductor diamond, its detailed step is as follows:
Claim Fe70:Ni27:Co3 (wt%) alloyed powder 360 grams, graphite powder 540 grams, pure boron powder 0.5 gram of Homogeneous phase mixing, after make graphite column 10 post of Φ 37.5 × 27.5, with accessory combinations such as pyrophillite mould, steel bowl, magnesia cup, graphite flake, conductive steel caps, after 120 DEG C of drying box dryings, on cubic hinge press, HTHP mode transforms, pressure is 5.0GPa, temperature is 1450 DEG C, through chemical purification process, obtains semiconductor diamond 697.89ct, per unit area yield 69.79ct, black non transparent, the complete octahedron of crystal formation, related index refers to table 1.
The method of embodiment 8 one kinds of HTHP synthesized semiconductor diamonds: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, can obtain semiconductor diamond, its detailed step is as follows:
Claim Fe70:Ni27:Co3 (wt%) alloyed powder 360 grams, graphite powder 540 grams, pure boron powder 0.2 gram of Homogeneous phase mixing, after make graphite column 10 post of Φ 37.5 × 27.5, with accessory combinations such as pyrophillite mould, steel bowl, magnesia cup, graphite flake, conductive steel caps, after 120 DEG C of drying box dryings, on cubic hinge press, HTHP mode transforms, pressure is 5.0GPa, temperature is 1450 DEG C, through chemical purification process, obtains semiconductor diamond 714.62ct, per unit area yield 71.46ct, blue-tinted transparent free from admixture, the complete octahedron of crystal formation, related index refers to table 1.
The method of embodiment 9 one kinds of HTHP synthesized semiconductor diamonds: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, can obtain semiconductor diamond, its detailed step is as follows:
Claim Fe70:Ni27:Co3 (wt%) alloyed powder 360 grams, graphite powder 540 grams, pure boron powder 0.2 gram of Homogeneous phase mixing, after make graphite column 10 post of Φ 37.5 × 27.5, assemble with annexes such as pyrophillite mould, steel bowl, magnesia cup, graphite flake, conductive steel caps, after 120 DEG C of drying box dryings, on cubic hinge press, HTHP mode transforms, pressure is 5.5GPa, temperature is 1450 DEG C, through chemical purification process, obtains semiconductor diamond 784.44ct, per unit area yield 78.44ct, blue-tinted transparent has impurity, and the complete octahedron of crystal formation, related index refers to table 1.
The performance indications of table 1 HTHP synthesized semiconductor diamond
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (5)
1. the method for a HTHP synthesized semiconductor diamond, mainly comprise the following steps: raw material mixing, isostatic cool pressing, fragmentation, shaping, vacuum high-temperature roasting, shaping, assembling, HTHP mode transform, chemical purification process, it is characterized in that, with pure boron, FeNiCo alloyed powder and high purity graphite powder for raw material, and the weight ratio of three is pure boron: FeNiCo alloyed powder: high purity graphite powder=0.0001 ~ 0.6:30 ~ 70:70 ~ 30; Purity > 95%, the FeNiCo alloyed powder purity > 95%, high purity graphite powder purity > 98% of described pure boron; When carrying out described HTHP mode and transforming, wherein Stress control is at 4.5 ~ 5.5GPa, and temperature controls at 1250 ~ 1500 DEG C.
2. the method for HTHP synthesized semiconductor diamond according to claim 1, is characterized in that, described FeNiCo alloyed powder is granularity 200 order ~ 500 object Fe
70ni
27co
3alloyed powder.
3. the method for HTHP synthesized semiconductor diamond according to claim 1, is characterized in that, described raw-material part by weight is pure boron: FeNiCo alloyed powder: high purity graphite powder=0.001 ~ 0.4:30 ~ 70:70 ~ 30.
4. the method for HTHP synthesized semiconductor diamond according to claim 3, is characterized in that, described raw-material part by weight is pure boron: FeNiCo alloyed powder: high purity graphite powder=0.01 ~ 0.2:30 ~ 40:60 ~ 40.
5. the method for HTHP synthesized semiconductor diamond according to claim 4, is characterized in that, described raw-material part by weight is pure boron: FeNiCo alloyed powder: high purity graphite powder=0.01 ~ 0.05:36:54.
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| US20130266678A1 (en) | 2012-04-09 | 2013-10-10 | Smith International, Inc. | Thermal insulation layer and pressure transfer medium for high pressure high temperature cell |
| US9586376B2 (en) | 2012-04-09 | 2017-03-07 | Smith International, Inc. | High pressure high temperature cell |
| CN103357353B (en) * | 2013-07-04 | 2015-03-25 | 河南金六方超硬材料有限公司 | Synthesis process of self-sharpening resin diamond |
| CN104907003A (en) * | 2015-06-24 | 2015-09-16 | 河南黄河旋风股份有限公司 | Manufacturing method ofdiamond with rough surface |
| CN105525345B (en) * | 2016-02-18 | 2018-06-26 | 长春阿尔玛斯科技有限公司 | Polycrystalline diamond synthesizing superhard material and its production technology |
| CN112403394A (en) * | 2020-11-18 | 2021-02-26 | 亳州市宝旗赫超硬材料有限公司 | Environment-friendly artificial diamond production process |
| CN112495303B (en) * | 2020-11-25 | 2022-08-05 | 内蒙古唐合科技有限公司 | Self-sharpening diamond and preparation method thereof |
| CN115007067B (en) * | 2022-06-14 | 2023-04-25 | 上海征世科技股份有限公司 | Device and method for preparing high-purity monocrystalline diamond piece |
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