KR100280771B1 - Synthesis method and apparatus for solid lubricants by solid-phase reaction in high pressure atmosphere - Google Patents
Synthesis method and apparatus for solid lubricants by solid-phase reaction in high pressure atmosphere Download PDFInfo
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- KR100280771B1 KR100280771B1 KR1019980020475A KR19980020475A KR100280771B1 KR 100280771 B1 KR100280771 B1 KR 100280771B1 KR 1019980020475 A KR1019980020475 A KR 1019980020475A KR 19980020475 A KR19980020475 A KR 19980020475A KR 100280771 B1 KR100280771 B1 KR 100280771B1
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
- C10M103/06—Metal compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/22—Compounds containing sulfur, selenium or tellurium
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/08—Solids
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Abstract
본 발명은 500℃ 이상의 고온 및 10-5torr 이하의 진공 분위기에서도 윤활효과를 나타내는 고체윤활제의 합성방법 및 합성장치에 관한 것으로, 특히 4B족 또는 5B족 전이금속 분말과 6A족 원소 분말을 일정한 몰비로 혼합한 원료분말을 고압 분위기에서 교반을 하면서 반응시켜 WS2, MoS2, WSe2등의 디찰코게나이드 (dichalcogenide)계 고체윤활제 분말을 합성하는 방법과 이에 사용된 장치에 관한 것이다.The present invention relates to a method for synthesizing and synthesizing a solid lubricant having a lubricating effect even at a high temperature of 500 ° C. or higher and a vacuum atmosphere of 10 −5 torr or less. Particularly, a constant molar ratio of a Group 4B or 5B transition metal powder and a Group 6A element powder a raw material powder mixture to react with stirring in the high-pressure atmosphere relates to WS 2, MoS 2, WSe 2, etc. dichal chalcogenides (dichalcogenide) type method for synthesizing a solid lubricant powder with the device used to this.
텅스텐(W), 몰리브덴(Mo), 니오븀(Nb), 탈륨(Ta) 등이 4B족 또는 5B족 전이 금속과 황(S), 셀레늄(Se), 텔륨(Te) 등이 6A족 원소를 1: 2.2 ∼ 3.0의 몰비로 균일하게 혼합한 원료분말을 반응드럼(1)내에 투입한 후, 개폐식 밸브( 3 )의 반복조작으로 반응드럼( 1 )의 내부를 일정한 고압으로 유지하며 모터( 6 )로 반응드럼( 1 )을 교반시키면서 약 800∼1000℃에서 2 시간 이하로 열처리하여 고체윤활제를 합성하였다.Tungsten (W), molybdenum (Mo), niobium (Nb), thallium (Ta) are Group 4B or Group 5B transition metals, and sulfur (S), selenium (Se), tellurium (Te), etc. : The raw material powder uniformly mixed at a molar ratio of 2.2 to 3.0 was introduced into the reaction drum 1, and the inside of the reaction drum 1 was maintained at a constant high pressure by repeating operation of the open / close valve 3 and the motor 6 While stirring the reaction drum (1) at about 800 ~ 1000 ℃ heat treatment for 2 hours or less to synthesize a solid lubricant.
기존의 원료분말을 진공 용기속에서 열처리하는 방법, 전이금속 산화물에 H2S 가스를 흘려주며 반응시키는 방법, 전이금속 산화물을 수용성염으로 전환시켜 6A족을 포함하는 염과 반응시킨 후 침전시키는 방법과 달리, 공정을 단순화시켜서 생산설비 및 생산비를 절감할 수 있으며 대량 생산이 가능하다.Method of heat treating existing raw material powder in vacuum vessel, flowing H 2 S gas to transition metal oxide and reacting, converting transition metal oxide into water-soluble salt and reacting with salts containing group 6A In contrast, by simplifying the process, production facilities and production costs can be reduced and mass production is possible.
Description
일반적으로 자기 윤활성이 있는 층상 디찰코게나이드(dichalcogenide)계 무기물질이란 4B족 또는 5B족 전이금속과 6A족 원소가 결합한 화합물을 일컫는다. 이러한 디찰코게나이드계 무기물질에는 WS2, MoS2, NbS2, TaS2, WSe2등이 있으며 고온 및 고진공 분위기에서도 윤활효과를 나타내어 고체윤활제로 이용되고 있다.In general, a self-lubricating layered dichalcogenide-based inorganic material refers to a compound in which a Group 4B or Group 5B transition metal and a Group 6A element are bonded. Such dichalcogenide-based inorganic materials include WS 2 , MoS 2 , NbS 2 , TaS 2 , WSe 2 , and the like, and are used as solid lubricants because they exhibit lubricating effects even at high temperatures and high vacuum atmospheres.
고체윤활제의 윤활성능은 분말의 입자형상에 의해 좌우된다. 디찰코게나이드계 무기물질은 흑연과 유사한 층상 구조를 가지고 있으며 층 내에서는 4B족 또는 5B족 전이금속과 6A족 원소가 강한 공유결합을 하고, 층과 층사이는 6A족 원소간에 약한 반데르발스 결합을 하고 있다. 따라서 전단력을 받을 때, 약한 반데르발스 결합을 하고 있는 층과 층사이에 미끄러짐이 일어나 윤활효과를 나타내게 된다. 그러므로 우수한 윤활효과를 나타내는 고체윤활제를 얻기 위해서는 잘 발달된 육각판상형의 층상구조를 가지는 분말의 획득이 중요하다.The lubricating performance of the solid lubricant depends on the particle shape of the powder. Dichalcogenide-based inorganic materials have a layered structure similar to graphite, in which the 4B or 5B transition metal and the Group 6A element have strong covalent bonds, and the weak van der Waals bond between the Group 6A elements between layers. Doing Therefore, when a shear force is applied, a slip occurs between the layers having weak van der Waals bonds and the lubricating effect is exhibited. Therefore, in order to obtain a solid lubricant showing excellent lubricating effect, it is important to obtain a powder having a well-developed hexagonal plate-like layered structure.
종래의 경우에 있어서, 이러한 디찰코게나이드계 무기물질은 원료분말을 진공 상태로 밀폐한 후 고온 열처리하는 방법, 전이금속 산화물과 H2S 가스와의 고상-기상 반응을 이용한 방법, 염형태의 전이금속 산화물을 수용성염으로 전환시켜 6A족을 포함하는 염과 반응시킨 후 침전시키는 방법 등으로 제조되었다.In the conventional case, such a dichalcogenide-based inorganic material is a method of high temperature heat treatment after sealing the raw powder in a vacuum state, a method using a solid-phase reaction of a transition metal oxide and H 2 S gas, a transition metal in the form of a salt It was prepared by a method of converting an oxide into a water-soluble salt, reacting with a salt containing a group 6A, and then precipitation.
원료분말을 상온에서 반응용기 내에 투입하고 반응용기를 진공으로 밀폐하여 900℃ 이상의 고온에서 열처리하는 방법은 진공 분위기를 만들기 위한 여러 단계의 공정이 필요하며 1주일 이상의 반응시간이 요구될 뿐 아니라 반응용기의 재사용이 불가능하다는 단점이 있으며, 전이금속 산화물과 H2S 가스와의 고상-기상 반응은 고가이면서 유독성인 H2S 가스를 장시간 흘려주어야 하므로 생산비가 많이 소요될 뿐 아니라 재해의 위험 때문에 공업적인 대량생산이 불가능한 문제점이 있다. 그리고 염 형태의 전이금속 산화물을 수용성염으로 전환시켜 6A족을 포함하고 있는 염과 반응시킨 후 침전시키는 방법은 염 형태의 전이금속 산화물이 잔존하며 생성물이 비정질형태이므로 결정질을 얻기 위하여 다시 고온에서 열처리해야하는 단점이 있다.The method of putting the raw material powder into the reaction vessel at room temperature and sealing the reaction vessel with vacuum to heat treatment at a high temperature of 900 ° C. or more requires several steps to create a vacuum atmosphere, and requires a reaction time of more than one week. It is disadvantageous that it cannot be reused, and the solid-gas reaction between transition metal oxide and H 2 S gas requires expensive and toxic H 2 S gas to be flowed for a long time. There is a problem that cannot be produced. In addition, the method of converting the salt-form transition metal oxide into a water-soluble salt, reacting with a salt containing Group 6A, and precipitating the same is heat-treated again at high temperature to obtain crystalline because the transition metal oxide remains in the salt form and the product is amorphous. There are drawbacks to this.
본 발명은 상기한 문제를 해결하기 위하여 안출된 것으로, 그 목적은 4B족 또는 5B족 전이금속 분말과 6A족 원소 분말을 혼합한 원료분말을 고압 분위기에서 교반을 하면서 반응시켜 WS2, MoS2, WSe2등의 디찰코게나이드계 고체윤활제 분말을 합성하는 방법과 이에 사용된 장치를 제공하고자 하는 것이다.The present invention has been made to solve the above problems, the object is to react the raw material powder mixed with Group 4B or 5B transition metal powder and Group 6A element powder while stirring in a high-pressure atmosphere, WS 2 , MoS 2 , SUMMARY To provide a method for synthesizing a dichalcogenide-based solid lubricant powder such as WSe 2 and an apparatus used therein.
즉, 본 발명의 목적은 일정한 몰비로 혼합한 원료분말을 고압 분위기에서 교반을 하면서 800∼1000℃ 에서 2 시간 이하로 반응시킨 보다 간편한 방법으로 짧은 시간내에 윤활특성이 우수한 육각 판상형이 잘 발달된 고체윤활제를 제조하는 방법을 제공하는데 있다.That is, the object of the present invention is a solid, well-developed hexagonal plate-type solid having excellent lubrication properties in a short time by a simpler method in which the raw material powder mixed in a constant molar ratio is stirred under a high pressure atmosphere at 800 to 1000 ° C. for 2 hours or less. It is to provide a method for producing a lubricant.
본 발명의 또 다른 목적은 반응용기의 재사용이 가능하며 설비 및 생산비를 절감할 수 있는 고체윤활제 분말의 염가양산제조 장치를 제공하는데 있다.Still another object of the present invention is to provide a low-cost mass production apparatus of solid lubricant powder capable of reusing a reaction vessel and reducing equipment and production costs.
제1도는 본 발명에 따른 합성장치의 개략도.1 is a schematic diagram of a synthesizing apparatus according to the present invention.
제2도는 고압 분위기를 위한 압력조절 부분의 상세도.2 is a detailed view of the pressure regulation portion for high pressure atmosphere.
제3도는 본 발명에 따른 합성 WS2의 XRD 분석 선도.3 is an XRD analysis diagram of synthetic WS 2 according to the present invention.
제4도는 본 발명에 따른 합성 WS2의 주사전자현미경(SEM) 사진.4 is a scanning electron microscope (SEM) photograph of the synthetic WS 2 according to the present invention.
제5도는 본 발명에 따른 합성 WS2의 입도 분석 선도.5 is a particle size analysis diagram of synthetic WS 2 according to the present invention.
제6도는 본 발명에 따른 합성 MoS2의 XRD 분석 선도.6 is an XRD analysis diagram of synthetic MoS 2 according to the present invention.
제7도는 본 발명에 따른 합성 MoS2의 주사전자현미경(SEM) 사진.7 is a scanning electron microscope (SEM) photograph of the synthetic MoS 2 according to the present invention.
제8도는 본 발명에 따른 합성 MoS2의 입도 분석 선도.8 is a particle size analysis diagram of synthetic MoS 2 according to the present invention.
〈도면의 주요부분에 대한 부호의 설명〉<Explanation of symbols for main parts of drawing>
1 : 반응드럼 2 : 가스배출관1: reaction drum 2: gas discharge pipe
3 : 개폐식 밸브 4 : 안전밸브3: retractable valve 4: safety valve
5 : 압력계 6 : 모터5: pressure gauge 6: motor
7 : 열전대 8 : 기어7: thermocouple 8: gear
9 : 전기로 10 : 발열체9: electric furnace 10: heating element
11 : 컨트롤박스11: control box
상기한 목적을 실현하기 위해서, 본 발명은 텅스텐(W), 몰리브덴(Mo), 니오븀(Nb), 탈륨(Ta) 등의 4B족 또는 5B족 전이금속과 황(S), 셀레늄(Se), 텔륨(Ta) 등의 6A족 원소를 1 : 2.2∼3.0의 몰비로 균일하게 혼합한 원료분말을 고압 분위기에서 교반을 하면서 약 800∼1000℃에서 2 시간 이하로 열처리하여 고체윤활제를 합성하였다.In order to realize the above object, the present invention provides a Group 4B or 5B transition metal such as tungsten (W), molybdenum (Mo), niobium (Nb), thallium (Ta), sulfur (S), selenium (Se), A solid lubricant was synthesized by heat-treating the raw material powder, which was uniformly mixed with a group 6A element such as tellurium (Ta) at a molar ratio of 1: 2.2 to 3.0, at about 800 to 1000 ° C. for 2 hours while stirring in a high pressure atmosphere.
한편, 첨부 도면 제 1 도는 본 발명에 따라 고체윤활제를 합성하는데 사용되는 합성장치의 구성을 개략적으로 나타낸 도면이며 제 2 도는 일정한 고압을 유지하기 위한 압력조절 부분의 상세도이다. 제 1 도에 의하면 합성장치는 고압을 유지하기 위하여 개폐식 밸브( 3 )와 안전밸브( 4 ) 그리고 압력계( 5 )로 구성된 압력조절 부분이 부착된 가스배출관( 2 )이 연결된 반응드럼(1)을 적재하고 있다. 상기 반응드럼( 1 )의 한 측면은 교반을 하기 위하여 기어( 8 )를 설치하여 모터( 6 )와 체인밸트로 연결하였다. 열처리를 위한 전기로( 9 )는 열전대( 7 )와 발열체( 10 )로 구성되었으며 ( 11 )은 컨트롤 박스이다.On the other hand, Figure 1 is a schematic diagram showing the configuration of the synthesis apparatus used to synthesize the solid lubricant according to the present invention and Figure 2 is a detailed view of the pressure control portion for maintaining a constant high pressure. According to FIG. 1, the synthesizing apparatus includes a reaction drum (1) connected with a gas discharge pipe (2) to which a pressure regulating portion consisting of an open / close valve (3), a safety valve (4), and a pressure gauge (5) is maintained to maintain a high pressure. Loading. One side of the reaction drum (1) was connected to the motor (6) and the chain belt by installing a gear (8) to stir. The furnace 9 for heat treatment consists of a thermocouple 7 and a heating element 10 and 11 is a control box.
반응드럼( 1 )은 1000℃까지 견딜 수 있는 두께 5 ㎜의 스테인리스강(SUS)으로 지름 200 ㎜, 길이 600 ㎜의 크기의 원통형에 회전이 가능하도록 길이 방향으로 양측면에 회전축을 접합하였다. 한쪽( 1a )은 지름 40 ㎜의 봉으로 접합하고 끝에 기어( 8 )를 부착하였으며, 다른 한쪽( 1b )은 원료분말의 투입과 반응생성물의 수거를 위하여 바깥지름 40 ㎜, 안지름 20 ㎜의 환봉으로 접합하였다.The reaction drum (1) is a stainless steel (SUS) having a thickness of 5 mm that can withstand up to 1000 ° C was joined to the rotating shaft on both sides in the longitudinal direction to enable rotation in a cylindrical size of 200 mm in diameter, 600 mm in length. One side (1a) was joined by a rod with a diameter of 40 mm, and a gear (8) was attached to the end. The other side (1b) was a round rod with an outer diameter of 40 mm and an inner diameter of 20 mm for input of raw material powder and collection of reaction products. Splicing.
가스배출관( 2 )은 개폐식 밸브( 3 ), 안전밸브( 4 ), 압력계( 5 )를 장착하여 개폐식 밸브( 3 )의 반복조작에 의해 반응드럼( 1 )의 내부를 일정고압으로 유지하고 이상 압력 발생시 자동으로 안전밸브( 4 )가 열려 폭발을 방지할 수 있도록 하였다. 특히 나사형식으로 하여 반응드럼( 1 )의 환봉으로 된 부분( 1b )에 장탈이 가능하도록 구성하였다.The gas discharge pipe (2) is equipped with an open / close valve (3), a safety valve (4), and a pressure gauge (5) to maintain the inside of the reaction drum (1) at a constant high pressure by repeating operation of the open / close valve (3) and an abnormal pressure. When it occurs, the safety valve (4) is automatically opened to prevent the explosion. In particular, it was configured in the form of a screw so that the desorption was possible in the portion (1b) of the round bar of the reaction drum (1).
반응드럼( 1 )의 교반을 위하여, rpm 조절이 가능한 모터( 6 )를 장착하여 축 베어링과 축 기어를 이용하여 반응드럼( 1 )에 부착된 기어( 8 )와 연결하였다.In order to stir the reaction drum (1), a motor (6) with adjustable rpm was mounted and connected to the gear (8) attached to the reaction drum (1) by using a shaft bearing and a shaft gear.
전기로( 9 )는 발열체( 10 )로 칸탈을 사용하였으며 반응드럼( 1 )의 장탈이 용이하도록 개폐식으로 구성하였다.Electric furnace (9) was used as a heating element (10) and was configured to open and close to facilitate the mounting of the reaction drum (1).
본 발명을 첨부한 도면에 의거하여 상세히 설명하면 다음과 같다. 먼저 일정몰비로 균일하게 혼합한 원료분말을 반응드럼( 1 )속에 투입한 후, 가스배출관( 2 )을 반응드럼( 1 )의 환봉부( 1b )에 연결하고 전기로( 9 )에 장착한다. 고른 반응과 반응시간을 단축하기 위하여, 모터( 6 )를 작동시켜 7rpm의 속도로 반응드럼( 1 )을 회전시키며 전기로( 9 )의 온도를 서서히 승온시킨다. 처음에는 반응드럼( 1 ) 내에 존재하는 산소를 제거하기 위하여 여분으로 첨가한 황과 산소를 반응시켜, 가스배출관( 2 )에 연결된 개폐식 밸브( 3 )가 열린 상태에서 서서히 가열하여 아황산가스를 배출한다. 반응이 어느 정도 진행되어 산소가 제거되면 개폐식 밸브( 3 )를 잠근다. 반응이 일어나는 동안 반응드럼( 1 )의 내부를 일정고압으로 유지하기 위하여 압력계( 5 )를 보며 개폐식 밸브( 3 )의 열고 닫는 조작을 반복한다. 800∼1000℃에서 2시간 이하로 유지 후 반응드럼( 1 )을 계속 회전시키며 서서히 노냉시킨다.The present invention will be described in detail with reference to the accompanying drawings. First, the raw material powder uniformly mixed at a constant molar ratio is introduced into the reaction drum (1), and then the gas discharge pipe (2) is connected to the round bar (1b) of the reaction drum (1) and mounted in the electric furnace (9). In order to shorten the reaction and the reaction time, the motor 6 is operated to rotate the reaction drum 1 at a speed of 7 rpm and gradually increase the temperature of the electric furnace 9. At first, sulfur and oxygen are added to react with excess sulfur to remove oxygen present in the reaction drum (1), and the sulfur dioxide gas is slowly heated by slowly opening the open / close valve (3) connected to the gas discharge pipe (2). . When the reaction proceeds to some extent and oxygen is removed, the closing valve 3 is closed. In order to maintain the inside of the reaction drum (1) at a constant high pressure during the reaction, the opening and closing operation of the open / close valve 3 is repeated while looking at the pressure gauge 5. After holding at 800 to 1000 ° C. for 2 hours or less, the reaction drum (1) was continuously rotated and gradually cooled.
[실시예 1]Example 1
WS2고체윤활제의 제조를 위하여, 원료로 텅스텐( 〉순도 99.9%, 평균입도 0.64 ㎛, 대한중석(주))과 황( 〉 순도 99.5%, 미원상사(주))을 사용하였다. 플라스틱 용기에 텅스텐과 황을 몰비로 1 : 2.2∼3.0으로 평량하여 투입하고 테프론 볼을 장입한 후, 건식 회전 혼합 방식으로 24 시간 혼합하였다. 반응드럼( 1 )에 혼합된 분말을 4 ㎏ 장입하고 가스배출관( 2 )을 연결하였다. 반응드럼( 1 )을 전기로( 9 )에 장착한 후, 개폐식 밸브( 3 )를 열고 7 rpm의 속도로 반응드럼( 1 )을 회전시키며 5℃/min의 속도로 가열하였다. 800∼1000℃까지 온도가 올라가는 동안 개페식 밸브( 3 )의 개폐에 의해 반응드럼( 1 )의 내압을 일정하게 유지하며 반응시켰다. 800∼1000℃에서 2시간 이하로 유지하고 로냉하였다. 반응생성물을 수거하고 체가름 하여 XRD, SEM, 입도분석을 하였다.For the preparation of the WS 2 solid lubricant, tungsten (> purity 99.9%, average particle size 0.64 µm, Daehan Soul Co.) and sulfur (> purity 99.5%, Miwon Corp.) were used as raw materials. Tungsten and sulfur were charged at a molar ratio of 1: 2.2 to 3.0 in a plastic container, charged with Teflon ball, and mixed for 24 hours by dry rotary mixing. 4 kg of powder mixed in the reaction drum (1) was charged and the gas discharge pipe (2) was connected. After mounting the reaction drum (1) in the electric furnace (9), the retractable valve (3) was opened and heated at a rate of 5 ° C./min while rotating the reaction drum (1) at a speed of 7 rpm. While the temperature was raised to 800 to 1000 ° C., the internal pressure of the reaction drum 1 was kept constant by opening and closing the open / close valve 3. The mixture was kept at 800 to 1000 ° C. for up to 2 hours and cooled by furnace. The reaction product was collected and screened for XRD, SEM and particle size analysis.
제 3 도는 합성 WS2고체윤활제의 X-선 회절분석(XRD) 결과이다. CuKαX-ray로 분석하였으며 반응생성물은 2H-WS2결정상의 peak 위치와 일치하였다. 반응하지 않은 텅스텐이나 텅스텐 산화물은 존재하지 않음을 확인하였다.3 is the result of X-ray diffraction analysis (XRD) of synthetic WS 2 solid lubricant. CuKαX-rays were analyzed and the reaction product coincided with the peak position of 2H-WS 2 crystal phase. It was confirmed that no tungsten or tungsten oxide was not reacted.
제 4 도는 합성 WS2의 주사전자현미경(SEM) 사진으로 육각판상형의 고체윤활제 분말이 형성되었음을 보여주고 있다.4 shows that the hexagonal plate-like solid lubricant powder was formed by scanning electron microscopy (SEM) photograph of the synthetic WS 2 .
제 5 도는 입도분석기를 이용한 합성 WS2의 입도 분석 결과이다. 평균 입자 크기는 약 15 ㎛ 이며 입자는 0.5∼50 ㎛ 사이의 분포를 하고 있음을 알 수 있다.5 is a result of particle size analysis of synthetic WS 2 using a particle size analyzer. It can be seen that the average particle size is about 15 μm and the particles have a distribution between 0.5 and 50 μm.
[실시예 2]Example 2
MoS2고체윤활제의 제조를 위하여, 원료로 몰리브덴과 황을 사용하였다. 플라스틱 용기에 몰리브덴과 황을 몰비로 1 : 2.2∼3.0로 평량하여 투입하고 테프론 볼을 장입한 후, 건식 회전 혼합 방식으로 24 시간 혼합하였다. 반응드럼( 1 )에 혼합된 분말을 4 ㎏ 장입하고 가스배출관( 2 )을 연결하였다. 반응드럼( 1 )을 전기로( 9 )에 장착한 후, 개폐식 밸브( 3 )를 열고 7 rpm의 속도로 반응드럼( 1 )을 회전시키며 5℃/min의 속도로 가열하였다. 800∼1000℃까지 온도가 올라가는 동안 개폐식 밸브( 3 )의 개폐에 의해 반응드럼( 1 )의 내압을 일정하게 유지하며 반응시켰다. 800∼1000℃에서 2 시간 이하로 유지하고 로냉하였다. 로냉 동안에 계속 반응드럼( 1 )을 회전시켰다. 반응생성물을 수거한 후, 체가름을하여 XRD, SEM, 입도분석을 하였다.For the preparation of the MoS 2 solid lubricant, molybdenum and sulfur were used as raw materials. Molybdenum and sulfur were charged in a plastic container in a molar ratio of 1: 2.2 to 3.0, and charged with Teflon balls, followed by mixing for 24 hours in a dry rotary mixing method. 4 kg of powder mixed in the reaction drum (1) was charged and the gas discharge pipe (2) was connected. After mounting the reaction drum (1) in the electric furnace (9), the retractable valve (3) was opened and heated at a rate of 5 ° C./min while rotating the reaction drum (1) at a speed of 7 rpm. The temperature of the reaction drum 1 was kept constant by opening and closing the valve 3 while the temperature was raised to 800 to 1000 ° C. The mixture was kept at 800 to 1000 ° C. for up to 2 hours and cooled by furnace. The reaction drum (1) was continuously rotated during furnace cooling. After the reaction product was collected, the resultant was sifted and analyzed by XRD, SEM, and particle size analysis.
제 6 도는 합성 MoS2의 X-선 회절분석(XRD) 결과이다. CuKαX-ray로 분석하였으며 반응생성물은 2H-MoS2결정상의 peak 위차와 일치하였다. 반응하지 않은 몰리브덴이나 몰리브덴 산화물은 존재하지 않음을 확인하였다.6 is the result of X-ray diffraction (XRD) of synthetic MoS 2 . CuKαX-ray was analyzed and the reaction product was consistent with the peak deviation of 2H-MoS 2 crystal phase. It was confirmed that no molybdenum or molybdenum oxide was present.
제 7 도는 합성 MoS2의 주사전자현미경(SEM) 사진으로 육각판상형의 고체윤활제 분말이 형성되었음을 보여주고 있다.7 shows that the hexagonal plate-like solid lubricant powder is formed by scanning electron microscopy (SEM) photograph of the synthetic MoS 2 .
제 8 도는 입도분석기를 이용한 합성 MoS2의 입도 분석 결과를 도시하였다. 평균 입자 크기는 약 16 ㎛를 이며 입자는 0.5∼50 ㎛ 사이의 분포를 하고 있음을 알 수 있다.8 shows particle size analysis results of synthetic MoS 2 using a particle size analyzer. It can be seen that the average particle size is about 16 μm and the particles have a distribution between 0.5 to 50 μm.
상기와 같이 본 발명에 따른 합성방법과 합성장치를 이용하여 고압 분위기에서 고상-기상 반응에 의해 제조된 WS2와 MoS2고체윤활제는 2H-WS2와 2H-MoS2결정상을 가지는 육각판상형을 입자를 나타내었다.As described above, the WS 2 and MoS 2 solid lubricants prepared by the solid-phase reaction in a high pressure atmosphere using the synthesis method and the synthesis apparatus according to the present invention form hexagonal plate-shaped particles having 2H-WS 2 and 2H-MoS 2 crystal phases. Indicated.
상기한 바와 같이 본 발명은 기존의 원료분말을 진공 용기속에서 열처리하는 방법, 전이금속 산화물에 H2S 가스를 흘려주며 반응시키는 방법, 전이금속 산화물을 수용성염으로 전환시켜 6A족을 포함하는 염과 반응시킨 후 침전시키는 방법과 달리, 공정을 단순화시켜서 생산설비 및 생산비를 절감할 수 있으며 대량 생산이 가능하다.As described above, the present invention provides a method of heat treating a conventional raw material powder in a vacuum container, a method of reacting by flowing H 2 S gas to a transition metal oxide, and converting the transition metal oxide into a water-soluble salt, including salts of Group 6A. Unlike the method of precipitation and then precipitation, the process can be simplified to reduce the production equipment and production cost, and mass production is possible.
현재 미국이나 일본에서는 고체윤활제를 정밀기계류 및 고부가가치 항공기 부품 등에 광범위하게 적용하고 있다. 제조업의 기술 고도화 추세에 따라 정밀기계류, 고부가가치 제품의 수요가 증대되고 있으며 이에 따라 고체윤활제의 수요 또한 증대되고 있다. 그러나 국내에서는 고체윤활제를 전량 수입에 의존하므로 가격이 비싸서 광범위하게 적용하지 못하고 있다.Currently, solid lubricants are widely applied in precision machinery and high value-added aircraft parts in the United States and Japan. As the technology advances in the manufacturing industry, the demand for precision machinery and high value-added products is increasing. Accordingly, the demand for solid lubricants is also increasing. However, in Korea, since the solid lubricants depend entirely on imports, they are expensive and are not widely applied.
본 발명으로 고체윤활제의 염가 대량 생산이 가능하여 건식 고체윤활제의 국산화를 이룰 수 있으며, 가격을 낮출 수 있어 연관 기계 부품에 광범위하게 적용 가능하다.The present invention enables the mass production of cheap solid lubricants to achieve the localization of the dry solid lubricants, it is possible to lower the price can be widely applied to the associated machine parts.
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