CN101054661A - Method of improving integrated capability for diamond film by high-temperature high-pressure method - Google Patents
Method of improving integrated capability for diamond film by high-temperature high-pressure method Download PDFInfo
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- CN101054661A CN101054661A CN 200610039409 CN200610039409A CN101054661A CN 101054661 A CN101054661 A CN 101054661A CN 200610039409 CN200610039409 CN 200610039409 CN 200610039409 A CN200610039409 A CN 200610039409A CN 101054661 A CN101054661 A CN 101054661A
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 86
- 239000010432 diamond Substances 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000011812 mixed powder Substances 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 27
- 230000005540 biological transmission Effects 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 230000007547 defect Effects 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 239000012528 membrane Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 60
- 239000013078 crystal Substances 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 10
- 238000012545 processing Methods 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 5
- 229910052903 pyrophyllite Inorganic materials 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000012010 growth Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000003698 laser cutting Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000005491 wire drawing Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- 239000010437 gem Substances 0.000 description 2
- 229910001751 gemstone Inorganic materials 0.000 description 2
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- 238000003786 synthesis reaction Methods 0.000 description 2
- 101000911390 Homo sapiens Coagulation factor VIII Proteins 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 230000002950 deficient Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 102000057593 human F8 Human genes 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000009931 pascalization Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000005381 potential energy Methods 0.000 description 1
- 229940047431 recombinate Drugs 0.000 description 1
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- 239000010409 thin film Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a process for improving all-round properties of diamond film by adoping a high-temperature high-pressure method. The main steps are as follows: preparing a mixing powder body by using catalyst powder, solvent metal powder, graphite powder and powder of a pressure transmission material; putting a diamond film blank into the mixed powder body and pressing them into compact synthesized blocks; baking the synthesized blocks for a preheating; dealing with the synthesized blocks at a high-temperature of 1300-2000 DEG C and a high-pressure of 5-10 GPa.In addition, instead of mixing the mixing powder body with the pressure transmission material, the pressure transmission material is processed into model and is held in the synthesized blocks to form assembling synthesized blocks. The present invention possesses the advantages than it reduces or eliminates some element impurities such as nitrogen, oxygen and hydrogen at grain boundary of the diamond and non-diamond carbon content at the grain boundary to remarkably improve the purity; it reduces or eliminates some diamond membrane structure defects including microscopic view defects such as location erroneous, layer erroneous and the like, upgrowth stress and internal microcracks, and then to improve the breakingstress and improve remarkably its all-round properties.
Description
One, technical field
The present invention relates to a kind of method that adopts improving integrated capability for diamond film by high-temperature high-pressure method.
Two, background technology
Chemical vapour deposition (Chemical Vapor Deposition, be called for short CVD) diamond film, the particulate state of high temperature and high pressure method preparation and the nanometer powdery diamond shape attitude restriction of explosion method preparation have been overcome, make diamond excellent especially mechanical property, light transmission, heat conductivility, sound conductivity and semiconductive to give full play of, therefore the research of CVD diamond is subjected to developed countries' great attentions such as U.S., day, Europe, drops into a large amount of manpower and financial resources and researchs and develops.At present, the nearly all physical and chemical performance of optical grade self-supporting CVD diamond film of countries such as U.S. preparation all can compare favourably with the natural IIa type gem grade diamond monocrystalline of extra best best, and only still there is a big difference for mechanical property (breaking tenacity).Existing result of study shows that self-supporting CVD diamond film breaking tenacity is 200～400MPa only generally, and the breaking tenacity of the natural IIa type of jewel level diamond single crystal can reach 3GPa.Self-supporting CVD diamond film breaking tenacity is that much smaller than the major cause of natural diamond diamond film is the polycrystalline hard brittle material, exist great number of elastic modulus and fracture surface energy all to be lower than the crystal boundary of several atomic layers thick of pure diamond in the film, the crystal boundary place exists amorphous carbon and a large amount of impurity such as N, H, and the defect size in cavity, crystal boundary place and gap is far longer than intracrystalline defect size.
Self-supporting CVD diamond film growth and subsequent machining cost are higher relatively, therefore, thereby how to reduce textural defect in the film improve its breaking tenacity and just seem very important for the commercial application of CVD diamond film.At present, the method that overcomes this textural defect both at home and abroad mainly contains: (1) improves stabilization of equipment performance and optimal preparation technology parameter, reduce the various textural defect in the CVD diamond film, as surface imperfection, intracrystalline imperfection and grain boundary defects, and the CVD diamond both macro and micro crackle that produces because of internal stress.But chemical vapor deposition processes itself just is difficult to prepare high-quality CVD diamond film, mainly contain following reason: the one, the many and accurately control difficulty of changeable processing parameter in the deposition process, even processing parameter can obtain stable control, the micro of deposition CVD diamond film also is difficult to unanimity.The 2nd, processing parameter is a mutual restriction to the influence of CVD diamond deposition process, thereby has influenced the preparation of high quality CVD diamond film; (2) utilize epitaxy large single crystal diamond film, especially heteroepitaxial growth single-crystal diamond film, but technical development can only be carried out texture growing on small area iso-epitaxy and the foreign substrate so far, and big area hetero epitaxy single-crystal diamond film growing technology is difficult in the near future big breakthrough is arranged.(3) the preparation average grain size is at the high nanocrystalline diamond film of the following toughness of 200nm (nanocrystalline diamond is called for short NCD).Use the microwave plasma body technology in Ar atmosphere, to introduce a small amount of C from U.S. Gruen reported first in 1994
60Since the preparation nanocrystalline diamond film, the nanocrystalline diamond film has become a new focus of diamond film research field.Ganoid nanocrystalline diamond film need not following process and can directly use, but because the thinner thickness (1～2 μ m) of preparation, research at present mainly concentrates on optical thin film, cold cathode device, the medical science film, can't prepare self-supporting nanometer diamond film.
Chinese patent CN1431929A, CN1238103C provide with high temperature and high pressure method and provide enough all to pressure and potential energy for the lattice imperfection in the isabelline diamond of monocrystalline, make the lattice imperfections such as dislocation of crystals climb, recombinate, bury in oblivion, propagation and slippage, thereby change the method for particulate state monocrystalline diamond color.But lattice imperfection and impurity to impurity, cavity and gaps such as the amorphous carbon that can reduce the crystal boundary place of polycrystalline diamond film with high temperature and high pressure method, a large amount of N, H and single crystal grain inside, thereby improve the breaking tenacity and the purity of diamond film, the method for improving integrated capability for diamond film does not relate to.
Three, summary of the invention
The object of the present invention is to provide a kind of method that adopts high temperature and high pressure method to handle diamond film,, improve its breaking tenacity and purity, improve its over-all properties to reduce the diamond film defective.
A kind of method of improving integrated capability for diamond film by high-temperature high-pressure method is characterized in that may further comprise the steps:
(1), with catalyst powder, solvent metal powder, Graphite Powder 99, pressure transmission material powder configuration mixed powder, content of graphite is 0～20wt% in the mixed powder; (2), the diamond film blank of well cutting is put in the mixed powder that configures, and with pressure the mixed powder that contains the diamond film blank is pressed into fine and close synthetic piece; (3), to synthetic piece preheating baking; (4), will add through the synthetic piece of preheating baking and hold high temperature and high pressure and handle, temperature is 1300 ℃～2000 ℃, pressure is 5GPa～10GPa.。
Wherein, described synthetic piece preheating baking, its preheating storing temperature is 100 ℃～400 ℃, storing time is 10～30 hours.
In the said process, the pressure transmission material is incorporated in preparation with powdery and closes in the caked mixed powder.Can in mixed powder, not add the pressure transmission material yet, put into synthetic piece, become the synthetic piece of assembling but the pressure transmission material is made die sleeve.Mainly may further comprise the steps:
(1), with catalyst powder, solvent metal powder, Graphite Powder 99 configuration mixed powder, content of graphite is 0～20wt% in the mixed powder; (2), make the pressure transmission die sleeve with the pressure transmission material; (3) the diamond film blank is mixed in is pressed into synthetic piece in certain mixed powder; (4), to synthetic piece preheating baking; (5), will put into the pressure transmission die sleeve through the synthetic piece of preheating baking and be assembled into compound synthetic piece, add then and hold high temperature and high pressure and handle, temperature is 1300 ℃～2000 ℃, pressure is 5GPa～10GPa.Wherein, the preheating storing temperature is 100 ℃～400 ℃, and storing time is 10～30 hours.
Superiority of the present invention is: adopt high temperature and high pressure method to handle self-supporting CVD diamond film to reduce or eliminate element impurity and crystal boundary place non-diamond carbon contents such as crystal boundary place nitrogen, oxygen, hydrogen, significantly improve diamond film purity; Adopt high temperature and high pressure method to handle free-standing diamond film to reduce or eliminate the diamond film textural defect, comprise microdefects such as dislocation, fault, growth stress and internal tiny crack, thereby improve its breaking tenacity, significantly improve its over-all properties, thereby solve the commercial application problem of diamond film in fields such as machinery, optics and calorifics at all.
Four, description of drawings
Fig. 1 is that high temperature and high pressure method is handled CVD diamond synoptic diagram.
Label title among Fig. 1: 1. Conducting steel bowl 2. pyrophyllite 3.CVD diamond blanks 4. graphite, catalyst and metal solvent mixed powder.
Five, embodiment
Key step of the present invention is: the self-supporting CVD diamond film → laser cutting diamond film for preparing better quality with methods such as hot wire process, microwave method and DC arc plasma gunitees becomes required shape and big or small blank → usefulness catalyst powder, solvent metal powder, Graphite Powder 99, pressure transmission material configuration mixed powder, content of graphite is lower than 20wt% in the mixed powder, also graphitiferous not; → CVD diamond film blank after will cutting is put in the mixed powder, with enough pressure the fine and close synthetic piece that is mingled with gas → synthetic piece is placed on preheating in the baking oven of not having is substantially made in the mixed powder compacting, its storing temperature is 100 ℃～400 ℃, storing time be 10～30 hours → the synthetic piece after the preheating is put into the High Temperature High Pressure stove, add by processing requirement and to hold high temperature and high pressure, temperature is 1300 ℃～2000 ℃, and pressure is 5GPa～10GPa.。→ take out the diamond film blank and carry out that soda acid is washed and wait processing, removing surface impurity, the diamond film blank that the original shape that has been maintained and big or small over-all properties have significantly improved.
In the said process, the pressure transmission material is incorporated in preparation with powdery and closes in the caked mixed powder.Also can not add the pressure transmission material in mixed powder, put into synthetic piece but the pressure transmission material is made die sleeve, step is slightly different:
With catalyst powder, solvent metal powder, Graphite Powder 99 powder configuration mixed powder, content of graphite is 0～20wt% in the mixed powder; Make the pressure transmission die sleeve with the pressure transmission material; The diamond film blank is mixed in is pressed into synthetic piece in certain mixed powder; To synthetic piece preheating baking; To put into the pressure transmission die sleeve through the synthetic piece of preheating baking and be assembled into compound synthetic piece, and add then and hold the high temperature and high pressure processing, temperature is 1300 ℃～2000 ℃, and pressure is 5GPa～10GPa.Wherein, the preheating storing temperature is 100 ℃～400 ℃, and storing time is 10～30 hours.
The method of improving integrated capability for diamond film by high-temperature high-pressure method of the present invention, be mainly used in diamond thin and diamond thick-film that various physical vapor depositions or chemical vapour deposition or additive method form, preferably refer to the diamond film of various chemical gaseous phase depositing process growths.
Embodiment 1
The thickness of preparing better quality with hot wire process is the self-supporting CVD diamond thick-film of 1mm, and the laser cutting diamond film becomes 4 * 4 * 1mm
3Die core of wire-drawing die blank or suitably big or small welded type thick film cutter cutter blank; Test is carried out on 6 * 800kN hinge type six-plane piercer, and testing used transmission medium is the powder pyrophyllite, and catalyst is the Ni70Mn25Co5 alloy powder, and the synthetic cavity diameter is 20mm, and synthesis temperature and pressure are respectively 1350 ℃ and 5.7Gpa; Graphite Powder 99, diamond film blank, catalyst powder, pyrophyllite, Conducting steel bowl etc. are assembled into synthetic piece, synthetic piece is put into baking oven, preheating is 15 hours under 200 ℃ temperature, put into the hinge type six-plane piercer after the taking-up, obtain containing the synthetic rod of diamond film die core of wire-drawing die blank or welded type thick film cutter cutter blank through high temperature high pressure process; Processing such as take out synthetic rod and carry out that soda acid is washed, removing diamond film blank surface impurity, diamond wire drawing die core blank or welded type thick film cutter cutter blank that the original shape that is maintained and big or small mechanical property have significantly improved.
Embodiment 2
With the dc arc plasma jet self-supporting CVD diamond thick-film that to prepare high-quality diameter 60mm thickness be 0.5mm, the laser cutting diamond film becomes 15 * 15 * 0.5mm
3The optical window blank of heat sink blank or diameter 30mm thickness 0.5mm; Test is carried out on belt type press, and testing used transmission medium is the powder pyrophyllite, and catalyst is the Fe70Ni30 alloy powder, and the synthetic cavity diameter is 40mm, and synthesis temperature and pressure are respectively 1350 ℃ and 5.7Gpa; Graphite Powder 99, diamond film blank, catalyst powder, pyrophyllite in powder, Conducting steel bowl etc. are assembled into synthetic piece, synthetic piece is put into baking oven, preheating is 20 hours under 240 ℃ temperature, put into belt type press after the taking-up, obtain containing the synthetic rod of heat sink blank of diamond film or optical window blank through superhigh-temperature and-pressure; Processing such as take out synthetic rod and carry out that soda acid is washed, removing diamond blank surface impurity, diamond heat-sink sheet blank or optical window blank that the original shape that is maintained and big or small over-all properties have significantly improved.
Claims (4)
1, a kind of method of improving integrated capability for diamond film by high-temperature high-pressure method is characterized in that may further comprise the steps:
(1), with catalyst powder, solvent metal powder, Graphite Powder 99, pressure transmission material powder configuration mixed powder, content of graphite is 0～20wt% in the mixed powder;
(2), the diamond film blank of well cutting is put in the mixed powder that configures, and with pressure the mixed powder that contains the diamond film blank is pressed into fine and close synthetic piece;
(3), to synthetic piece preheating baking;
(4), will add through the synthetic piece of preheating baking and hold high temperature and high pressure and handle, temperature is 1300 ℃～2000 ℃, pressure is 5GPa～10GPa.。
2, the method for improving integrated capability for diamond film by high-temperature high-pressure method according to claim 1 is characterized in that: described synthetic piece preheating baking, and its preheating storing temperature is 100 ℃～400 ℃, storing time is 10～30 hours.
3, a kind of method of improving integrated capability for diamond film by high-temperature high-pressure method is characterized in that may further comprise the steps:
(1), with catalyst powder, solvent metal powder, Graphite Powder 99 configuration mixed powder, content of graphite is 0～20wt% in the mixed powder;
(2), make the pressure transmission die sleeve with the pressure transmission material;
(3) the diamond film blank is mixed in is pressed into synthetic piece in certain mixed powder;
(4), to synthetic piece preheating baking;
(5), will put into the pressure transmission die sleeve through the synthetic piece of preheating baking and be assembled into compound synthetic piece, add then and hold high temperature and high pressure and handle, temperature is 1300 ℃～2000 ℃, pressure is 5GPa～10GPa.
4, the method for improving integrated capability for diamond film by high-temperature high-pressure method according to claim 3 is characterized in that: described synthetic piece preheating baking, and its preheating storing temperature is 100 ℃～400 ℃, storing time is 10～30 hours.
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| CN 200610039409 CN101054661A (en) | 2006-04-10 | 2006-04-10 | Method of improving integrated capability for diamond film by high-temperature high-pressure method |
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| CN 200610039409 CN101054661A (en) | 2006-04-10 | 2006-04-10 | Method of improving integrated capability for diamond film by high-temperature high-pressure method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110697704A (en) * | 2019-11-01 | 2020-01-17 | 陈玉琦 | Diamond optimization method |
| CN113816737A (en) * | 2021-09-09 | 2021-12-21 | 四川大学 | Method for efficiently preparing transparent diamond material |
| CN115201241A (en) * | 2022-07-18 | 2022-10-18 | 吉林大学 | SnBi regulated and controlled by high-voltage technology 2 Te 4 Method for detecting Sn atom defect |
-
2006
- 2006-04-10 CN CN 200610039409 patent/CN101054661A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110697704A (en) * | 2019-11-01 | 2020-01-17 | 陈玉琦 | Diamond optimization method |
| CN113816737A (en) * | 2021-09-09 | 2021-12-21 | 四川大学 | Method for efficiently preparing transparent diamond material |
| CN115201241A (en) * | 2022-07-18 | 2022-10-18 | 吉林大学 | SnBi regulated and controlled by high-voltage technology 2 Te 4 Method for detecting Sn atom defect |
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