JP2001170474A - Method for producing conductive diamond fine particles - Google Patents
Method for producing conductive diamond fine particlesInfo
- Publication number
- JP2001170474A JP2001170474A JP35874399A JP35874399A JP2001170474A JP 2001170474 A JP2001170474 A JP 2001170474A JP 35874399 A JP35874399 A JP 35874399A JP 35874399 A JP35874399 A JP 35874399A JP 2001170474 A JP2001170474 A JP 2001170474A
- Authority
- JP
- Japan
- Prior art keywords
- diamond
- fine particles
- graphite
- boron
- conductive diamond
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000010432 diamond Substances 0.000 title claims abstract description 67
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 66
- 239000010419 fine particle Substances 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052796 boron Inorganic materials 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 28
- 239000010439 graphite Substances 0.000 claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 22
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 4
- 229910052580 B4C Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- -1 for example Chemical compound 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
(57)【要約】
【課題】 導電性ダイヤモンド微粒子の製造方法の開
発。
【解決手段】 ホウ素を黒鉛に対して０．５ｗｔ％以上
１５ｗｔ％以下含む黒鉛をダイヤモンド転換金属触媒と
共存させ、１２００℃以上の温度および４．５ＧＰａ以
上の圧力の高温高圧下で黒鉛をダイヤモンドに変換して
平均粒径２０〜３０μｍの導電性ダイヤモンド微粒子を
製造する。
(57) [Abstract] [PROBLEMS] To develop a method for producing conductive diamond fine particles. SOLUTION: Graphite containing 0.5 wt% to 15 wt% of boron with respect to graphite coexists with a diamond conversion metal catalyst, and converts graphite into diamond at a temperature of 1200 ° C. or higher and a high pressure of 4.5 GPa or higher. By conversion, conductive diamond fine particles having an average particle diameter of 20 to 30 μm are produced.
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、結晶格子中に多量
のホウ素を含有するダイヤモンド微粒子の製造方法に関
する。The present invention relates to a method for producing diamond fine particles containing a large amount of boron in a crystal lattice.
【０００２】[0002]
【従来の技術】導電性ダイヤモンド粒子を合成する方法
として、ダイヤモンド転換触媒または原料黒鉛粉末にホ
ウ素を混合した混合粉末体を使用することは従来から提
案されてきた。しかし、半導体ダイヤモンドが実現する
ホウ素濃度は１００−１０００ｐｐｍ（０．０１−０．
１ｗｔ％）とされており、このような低濃度ホウ素の半
導体ダイヤモンドは研究されていた。2. Description of the Related Art As a method for synthesizing conductive diamond particles, it has been conventionally proposed to use a diamond conversion catalyst or a mixed powder obtained by mixing boron with raw graphite powder. However, the boron concentration realized by semiconductor diamond is 100-1000 ppm (0.01-0.
1 wt%), and such a low-concentration boron semiconductor diamond has been studied.
【０００３】（１）ベントルフとボベンカークは１００
ｐｐｍ程度のホウ素を添加した半導体ダイヤモンドの合
成方法について報告している(R.H.Wentorf, Jr. and H.
P.Bovenkark, J.Chem.Phys., 36, 1987-90(1962)) 。
（２）ウイリアムスらはホウ素を約１００ｐｐｍ含有す
るダイヤモンド結晶が室温で約１００−１０００Ω・ｃ
ｍの導電率を持つ半導体であることを報告している(A.
W.S.Williams, E.C.Lightowlers, A.T.Collins, J.Phy
s.C. Solid St. Phys., 3,1727-1735(1970))。(1) Bentolf and Bobenkirk are 100
A method for synthesizing semiconductor diamond doped with about ppm of boron is reported (RHWentorf, Jr. and H.
P. Bovenkark, J. Chem. Phys., 36, 1987-90 (1962)).
(2) Williams et al. Found that a diamond crystal containing about 100 ppm of boron was about 100-1000 Ω · c at room temperature.
m has been reported to be a semiconductor (A.
WSWilliams, ECLightowlers, ATCollins, J.Phy
sC Solid St. Phys., 3,1727-1735 (1970)).
【０００４】低濃度ホウ素を混合して得られた半導体ダ
イヤモンドに関する研究報告はこれら以外にも多数報告
されている。しかし、５０００ｐｐｍ（０．５ｗｔ％）
以上のホウ素を混合して得られる導電性ダイヤモンドに
関する研究は皆無である。また、導電性ダイヤモンド粒
子を利用した産業製品は現在まで皆無である。[0004] There have been many other reports on semiconductor diamonds obtained by mixing low-concentration boron. However, 5000ppm (0.5wt%)
There is no study on conductive diamond obtained by mixing the above boron. There is no industrial product using conductive diamond particles.
【０００５】このような低濃度ホウ素を含むダイヤモン
ドやホウ素を含まないダイヤモンドの粒径は、１００μ
ｍ以上である。研磨剤として使用される微粒ダイヤモン
ドは、この粒径の結晶を粉砕することによって製造され
ているが、高硬度のダイヤモンドの粉砕は容易ではな
い。[0005] The diameter of diamond containing such a low concentration of boron and diamond containing no boron is 100 μm.
m or more. Fine diamond used as an abrasive is produced by crushing crystals of this particle size, but crushing of diamond with high hardness is not easy.
【０００６】[0006]
【発明が解決しようとする課題】導電性ダイヤモンド皮
膜をたとえば電気分解用電極（特に陽極）材料として使
用すれば、高電流密度、長寿命、耐酸化性皮膜が実現す
るであろうことは想定されていたが、均質なダイヤモン
ド皮膜を形成するには１０μｍ以下の微粒子が必要であ
る。このような微粒子を１００μｍ程度のダイヤモンド
粒子を粉砕して製造するのはきわめて能率が悪い。しか
し、予め導電性ダイヤモンド微粒子を得る方法が未解決
であったために、用途開発が著しく遅れていた。そこ
で、本発明は、平均粒径２０〜３０μｍの導電性ダイヤ
モンド微粒子を製造する技術を開発することを課題とし
ている。It is envisioned that the use of a conductive diamond film, for example, as a material for an electrode for electrolysis (especially the anode) would provide a high current density, long life, and oxidation resistant film. However, fine particles of 10 μm or less are required to form a uniform diamond film. It is extremely inefficient to produce such fine particles by grinding diamond particles of about 100 μm. However, since the method for obtaining the conductive diamond fine particles had not been solved in advance, the development of the application was significantly delayed. Therefore, an object of the present invention is to develop a technique for producing conductive diamond fine particles having an average particle size of 20 to 30 μm.
【０００７】[0007]
【問題を解決するための手段】本発明者らは、従来研究
されていなかった高濃度ホウ素添加黒鉛を使用すること
によって所望の導電性微粒ダイヤモンドが得られる可能
性を探求した結果、平均粒径２０〜３０μｍの導電性ダ
イヤモンド粒子が得られるという知見を得た。Means for Solving the Problems The present inventors have investigated the possibility of obtaining desired conductive fine diamond by using high-concentration boron-doped graphite, which has not been studied so far, and as a result, have found that the average particle size is small. It has been found that conductive diamond particles of 20 to 30 μm can be obtained.
【０００８】本発明は、上記の知見に基づき、従来のダ
イヤモンド粒子の製造条件と同じ実用的な圧力温度範囲
で優れた導電性ダイヤモンド微粒子が得られるという特
徴を持っている。The present invention has the feature that, based on the above findings, excellent conductive diamond fine particles can be obtained in the same practical pressure temperature range as the conventional diamond particle production conditions.
【０００９】すなわち、本発明は、ホウ素を黒鉛に対し
て０．５ｗｔ％以上１５ｗｔ％以下含む黒鉛をダイヤモ
ンド転換金属触媒と共存させ、１２００℃以上の温度お
よび４．５ＧＰａ以上の圧力の高温高圧下で黒鉛をダイ
ヤモンドに変換することを特徴とする平均粒径２０〜３
０μｍの導電性ダイヤモンド微粒子の製造方法である。
ホウ素の量が黒鉛に対して０．５ｗｔ未満では、生成
するダイヤモンドの粒径が大きく（１００μｍ以上）、
また、１５ｗｔ％を越えるとダイヤモンドを生成させる
ことができない。これは、炭化ホウ素の生成がダイヤモ
ンドの生成に優先されるためと思われる。[0009] That is, the present invention provides a graphite conversion metal catalyst containing boron in an amount of 0.5 wt% to 15 wt% with respect to graphite in the presence of a high temperature and high pressure of 1200 ° C or more and a pressure of 4.5 GPa or more. Converting graphite to diamond with an average particle size of 20 to 3
This is a method for producing conductive diamond fine particles of 0 μm.
When the amount of boron is less than 0.5 wt% with respect to graphite, the diameter of the generated diamond is large (100 μm or more),
On the other hand, if it exceeds 15% by weight, diamond cannot be produced. This is probably because the formation of boron carbide has priority over the formation of diamond.
【００１０】上記の黒鉛は、ホウ素を含む黒鉛成形体ま
たはホウ素と黒鉛の粉末混合体を用いることができる。
ホウ素を含む黒鉛成形体は、例えば、原子炉用として生
産されているホウ素含有黒鉛などを使用することができ
る。上記のダイヤモンド転換金属触媒は、ダイヤモンド
合成用金属触媒として公知（.P.Bovenkerk,F.P.Bundy,
H.T.Hall,H.M.Strong,R.H.Wentorf,Jr.,Nature,184,109
4-8(1959) ）の鉄、ニッケル、コバルトまたはこれらの
金属を主成分とする合金を使用することができる。温度
および圧力条件は、ダイヤモンドの熱力学的安定条件を
満たす組み合わせとする。１２００℃未満の温度では、
金属触媒が溶解しないため、ダイヤモンドが生成しな
い。４．５ＧＰａ未満の圧力では、ダイヤモンドの熱力
学安定条件を満たすことができない。As the graphite, a graphite compact containing boron or a powder mixture of boron and graphite can be used.
As the graphite compact containing boron, for example, boron-containing graphite produced for a nuclear reactor can be used. The above diamond conversion metal catalyst is known as a metal catalyst for diamond synthesis (.P. Bovenkerk, FPBundy,
HTHall, HMStrong, RHWentorf, Jr., Nature, 184, 109
4-8 (1959)), iron, nickel, cobalt or alloys containing these metals as main components can be used. The temperature and pressure conditions are a combination that satisfies the thermodynamic stability conditions of diamond. At temperatures below 1200 ° C,
Diamond does not form because the metal catalyst does not dissolve. If the pressure is lower than 4.5 GPa, the thermodynamic stability condition of diamond cannot be satisfied.
【００１１】本発明において、上記のように多量のホウ
素を添加した理由を説明する。常圧において１６００℃
で、液相の鉄に対して約１５ｗｔ％のホウ素が溶解する
ことが知られている。ダイヤモンドを合成する超高圧で
どの程度のホウ素が液相に溶解するかは不明であるが、
鉄、ニッケル、コバルトなどは互いに似たような性質を
持つ元素であるから、これらを含む液相でもおよそ１５
ｗｔ％程度のホウ素が液相中に溶解すると想定される。
多量のホウ素を含む黒鉛と接触している転換触媒液相
は、転換触媒液相に対するホウ素の溶解度が炭素に対す
るホウ素の溶解度に比べて相対的に大きいため、すみや
かに、かつ選択的にホウ素を溶解すると考えられる。In the present invention, the reason why a large amount of boron is added as described above will be described. 1600 ° C at normal pressure
It is known that about 15 wt% of boron is dissolved in iron in the liquid phase. It is unknown how much boron dissolves in the liquid phase at ultra high pressure to synthesize diamond,
Since iron, nickel, cobalt, and the like are elements having properties similar to each other, even a liquid phase containing them has a concentration of about 15%.
It is assumed that about wt% of boron dissolves in the liquid phase.
The conversion catalyst liquid phase in contact with graphite containing a large amount of boron dissolves boron promptly and selectively because the solubility of boron in the conversion catalyst liquid phase is relatively higher than the solubility of boron in carbon. It is thought that.
【００１２】このように、ホウ素を選択的に溶解した液
相に炭素が溶解すると、その炭素はダイヤモンドに変化
すると同時に、炭化ホウ素を析出させようとする反応も
伴う。特に、多量のホウ素を液相に溶解した系では、こ
のような二種類の反応が競合的に進むと考えられる。な
ぜ、多量のホウ素を液相に溶解させると微粒ダイヤモン
ドが析出するかという正確な機構は未知であるが、ダイ
ヤモンドと炭化ホウ素が競合して析出しようとする過程
で、ダイヤモンド粒子の粒成長が阻害されると考えられ
る。As described above, when carbon is dissolved in a liquid phase in which boron is selectively dissolved, the carbon is converted into diamond, and at the same time, there is a reaction to precipitate boron carbide. Particularly, in a system in which a large amount of boron is dissolved in a liquid phase, it is considered that such two kinds of reactions proceed competitively. The exact mechanism of why a large amount of boron is dissolved in the liquid phase to precipitate fine diamond is unknown, but diamond and boron carbide compete with each other to precipitate and hinder the growth of diamond particles. It is thought to be done.
【００１３】比較のためにホウ素を添加していない等方
性黒鉛板を原料としてダイヤモンドを合成した結果、生
成したダイヤモンドの粒径は１００〜２００μｍであっ
た。For comparison, as a result of synthesizing diamond using an isotropic graphite plate to which boron was not added as a raw material, the particle diameter of the generated diamond was 100 to 200 μm.
【００１４】本発明の方法によって得られたダイヤモン
ド微粒子は、導電性耐薬品皮膜などに使用し、従来材料
では得られない長寿命の導電性皮膜を実現することがで
きる。また、導電性でかつ高硬度であるから、放電と機
械的研削プロセスを結合させた高能率研削砥石用砥粒と
しても好適である。The fine diamond particles obtained by the method of the present invention can be used for a conductive chemical-resistant film or the like, and can realize a long-lived conductive film that cannot be obtained with conventional materials. Further, since it is conductive and has high hardness, it is also suitable as an abrasive grain for a high-efficiency grinding wheel combining a discharge and a mechanical grinding process.
【００１５】[0015]
【実施例】以下に本発明の実施例を説明する。 実施例１ ニッケル円板（７ｍｍφ×０．５ｍｍ，２００ｍｇ）
と、等方性黒鉛（１００ｍｇ）とホウ素（１０ｍｇ）と
の混合粉末を積層した。これをＮａＣｌ成形体からなる
カプセルに入れ、これをベルト型高圧装置を用いて高温
高圧（５．５万気圧、１５００℃）に１０分間保持し
た。取り出した試料を王水中で煮沸してニッケルを溶解
除去しダイヤモンドを回収した。得られたダイヤモンド
は、径７ｍｍの円盤状であったが、２０〜３０μｍの微
粒子の集合体であった。これを乳鉢で擦りつぶすことに
より、簡単に２０〜３０μｍの粉末を得ることができ
た。Embodiments of the present invention will be described below. Example 1 Nickel disk (7 mmφ × 0.5 mm, 200 mg)
And a mixed powder of isotropic graphite (100 mg) and boron (10 mg). This was put into a capsule made of a NaCl molded body, and this was kept at a high temperature and a high pressure (550,000 atm, 1500 ° C.) for 10 minutes using a belt type high pressure device. The removed sample was boiled in aqua regia to dissolve and remove nickel and recover diamond. The obtained diamond had a disk shape of 7 mm in diameter, but was an aggregate of fine particles of 20 to 30 μm. By crushing this with a mortar, a powder of 20 to 30 μm could be easily obtained.
【００１６】実施例２ ニッケル円板（７ｍｍφ×０．５ｍｍ，２００ｍｇ）
と、等方性黒鉛（１００ｍｇ）とホウ素（０．５ｍｇ）
との混合粉末を積層し、実施例１と同様な処理を行っ
た。２０〜３０μｍのダイヤモンド微粒子の集合体が得
られ、粉砕により２０〜３０μｍの粉末を得ることがで
きた。Example 2 Nickel disk (7 mmφ × 0.5 mm, 200 mg)
And isotropic graphite (100mg) and boron (0.5mg)
And the same treatment as in Example 1 was performed. An aggregate of 20 to 30 μm diamond fine particles was obtained, and a powder of 20 to 30 μm was obtained by pulverization.
【００１７】実施例３ ニッケル円板（７ｍｍφ×０．５ｍｍ，２００ｍｇ）
と、等方性黒鉛（１００ｍｇ）とホウ素（１５ｍｇ）と
の混合粉末を積層し、実施例１と同様な処理を行った。
２０〜３０μｍのダイヤモンド微粒子の集合体が得ら
れ、粉砕により２０〜３０μｍのの粉末を得ることがで
きた。Example 3 Nickel disk (7 mmφ × 0.5 mm, 200 mg)
And a mixed powder of isotropic graphite (100 mg) and boron (15 mg) were laminated, and the same treatment as in Example 1 was performed.
An aggregate of 20 to 30 μm diamond particles was obtained, and a powder of 20 to 30 μm was obtained by pulverization.
【００１８】実施例４ ニッケル円板（７ｍｍφ×０．５ｍｍ，２００ｍｇ）
と、ホウ素１０ｗｔ％を予め添加した黒鉛成形体とを積
層し、実施例１と同様な処理を行った。２０〜３０μｍ
のダイヤモンド微粒子の集合体が得られ、粉砕により２
０〜３０μｍの粉末を得ることができた。微粒子の集合
体の走査型電子顕微鏡写真を図１に示す。Example 4 Nickel disk (7 mmφ × 0.5 mm, 200 mg)
And a graphite molded body to which 10% by weight of boron was added in advance, and the same treatment as in Example 1 was performed. 20-30 μm
An aggregate of diamond fine particles of
A powder of 0 to 30 μm could be obtained. FIG. 1 shows a scanning electron micrograph of the aggregate of fine particles.
【００１９】実施例５ コバルト円板（７ｍｍφ×０．５ｍｍ，２００ｍｇ）
と、ホウ素１０ｗｔ％を予め添加した黒鉛成形体とを積
層し、実施例１と同様な処理を行った。２０〜３０μｍ
のダイヤモンド微粒子の集合体が得られ、粉砕により２
０〜３０μｍの粉末を得ることができた。Example 5 Cobalt disk (7 mmφ × 0.5 mm, 200 mg)
And a graphite molded body to which 10% by weight of boron was added in advance, and the same treatment as in Example 1 was performed. 20-30 μm
An aggregate of diamond fine particles of
A powder of 0 to 30 μm could be obtained.
【００２０】実施例６ 鉄６３％、ニッケル３１％、コバルト６％の合金板（７
ｍｍφ×０．５ｍｍ，２００ｍｇ）と、ホウ素１０ｗｔ
％を予め添加した黒鉛成形体とを積層し、実施例１と同
様な処理を行った。２０〜３０μｍのダイヤモンド微粒
子の集合体が得られ、粉砕により２０〜３０μｍの粉末
を得ることができた。Example 6 An alloy plate of 63% iron, 31% nickel and 6% cobalt (7
mmφ × 0.5mm, 200mg) and boron 10wt
%, And the same treatment as in Example 1 was performed. An aggregate of 20 to 30 μm diamond fine particles was obtained, and a powder of 20 to 30 μm was obtained by pulverization.
【００２１】比較例１ ニッケル円板（７ｍｍφ×０．５ｍｍ，２００ｍｇ）
と、等方性黒鉛（１００ｍｇ）粉末を積層し、実施例１
と同様な処理を行った。生成したダイヤモンドは１００
〜２００μｍの粒子の集合体であり、実施例１と同様な
条件で粉砕しても１００μｍ以上の粒子が残存した。粒
子の集合体の走査型電子顕微鏡写真を図２に示す。Comparative Example 1 Nickel disk (7 mmφ × 0.5 mm, 200 mg)
And isotropic graphite (100 mg) powder were laminated,
The same processing as described above was performed. The generated diamond is 100
It was an aggregate of particles of up to 200 μm, and particles of 100 μm or more remained even when crushed under the same conditions as in Example 1. FIG. 2 shows a scanning electron micrograph of the aggregate of particles.
【００２２】比較例２ ニッケル円板（７ｍｍφ×０．５ｍｍ，２００ｍｇ）
と、等方性黒鉛（１００ｍｇ）とホウ素（２０ｍｇ）と
の混合粉末を積層し、実施例１と同様な処理を行った。
ホウ素添加量が過剰のためにダイヤモンドはほとんど生
成しなかった。Comparative Example 2 Nickel disk (7 mmφ × 0.5 mm, 200 mg)
And a mixed powder of isotropic graphite (100 mg) and boron (20 mg) were laminated, and the same treatment as in Example 1 was performed.
Almost no diamond was produced due to the excessive amount of boron added.
【図１】本発明の実施例４の製造方法により得られた２
０〜３０μｍのダイヤモンド粒子の集合体の形状を示す
図面代用の走査顕微鏡写真である。FIG. 1 shows a sample 2 obtained by the production method of Example 4 of the present invention.
It is a scanning micrograph instead of a drawing which shows the shape of the aggregate of 0-30 micrometers diamond particles.
【図２】比較例１の製造方法により得られた１００〜２
００μｍのダイヤモンド粒子の集合体の形状を示す図面
代用の走査顕微鏡写真である。FIG. 2 shows 100 to 2 obtained by the production method of Comparative Example 1.
It is a scanning micrograph instead of a drawing which shows the shape of the aggregate of 00 micrometer diamond particles.
Claims (4)
１５ｗｔ％以下含む黒鉛をダイヤモンド転換金属触媒と
共存させ、１２００℃以上の温度および４．５ＧＰａ以
上の圧力の高温高圧下で黒鉛をダイヤモンドに変換する
ことを特徴とする平均粒径２０〜３０μｍの導電性ダイ
ヤモンド微粒子の製造方法。1. A graphite containing boron in an amount of 0.5% by weight or more and 15% by weight or less with respect to graphite coexists with a diamond conversion metal catalyst, and the graphite is converted to diamond at a temperature of 1200 ° C. or more and a high pressure of 4.5 GPa or more. A method for producing conductive diamond fine particles having an average particle diameter of 20 to 30 µm, characterized by converting the fine particles into conductive diamond particles.
またはホウ素と黒鉛の粉末混合体であることを特徴とす
る請求項１記載の導電性ダイヤモンド微粒子の製造方
法。2. The method for producing conductive diamond fine particles according to claim 1, wherein said graphite is a graphite molded body containing boron or a powder mixture of boron and graphite.
鉄、ニッケル、コバルトまたはこれらの金属を主成分と
する合金であることを特徴とする請求項１記載の導電性
ダイヤモンド微粒子の製造方法。3. The above diamond conversion metal catalyst,
2. The method for producing conductive diamond fine particles according to claim 1, wherein the conductive diamond fine particles are iron, nickel, cobalt or an alloy containing these metals as main components.
熱力学的安定条件を満たす組み合わせであることを特徴
とする請求項１記載の導電性ダイヤモンド微粒子の製造
方法。4. The method for producing conductive diamond fine particles according to claim 1, wherein the temperature and pressure conditions are a combination satisfying a thermodynamic stability condition of diamond.
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003057625A1 (en) * | 2001-12-28 | 2003-07-17 | Toyo Tanso Co., Ltd. | Graphite material for synthesizing semiconductor diamond and semiconductor diamond produced by using the same |
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| CN107376786B (en) * | 2017-08-24 | 2020-12-18 | 河南理工大学 | A kind of high hardness polycrystalline diamond sintering equipment and corresponding sintering method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003057625A1 (en) * | 2001-12-28 | 2003-07-17 | Toyo Tanso Co., Ltd. | Graphite material for synthesizing semiconductor diamond and semiconductor diamond produced by using the same |
| KR100742059B1 (en) * | 2001-12-28 | 2007-07-23 | 도요탄소 가부시키가이샤 | Graphite material for synthesizing semiconductor diamond, method for producing same and method for synthesizing semiconductor diamond produced using graphite material |
| CN100354199C (en) * | 2001-12-28 | 2007-12-12 | 东洋炭素株式会社 | Graphite material for synthesizing semiconductor diamond and semiconductor diamond produced by using same |
| US8916125B2 (en) | 2001-12-28 | 2014-12-23 | Toyo Tanso Co., Ltd. | Graphite material for synthesizing semiconductor diamond and semiconductor diamond produced by using the same |
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