TWI815223B - P-containing abrasives and cutting wire containing the abrasives - Google Patents
P-containing abrasives and cutting wire containing the abrasives Download PDFInfo
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- TWI815223B TWI815223B TW110143322A TW110143322A TWI815223B TW I815223 B TWI815223 B TW I815223B TW 110143322 A TW110143322 A TW 110143322A TW 110143322 A TW110143322 A TW 110143322A TW I815223 B TWI815223 B TW I815223B
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- phosphating
- abrasive grains
- nickel
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- phosphorus
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- 238000005520 cutting process Methods 0.000 title claims description 26
- 239000003082 abrasive agent Substances 0.000 title abstract 4
- 238000000034 method Methods 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 13
- 239000011574 phosphorus Substances 0.000 claims abstract description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 56
- 239000006061 abrasive grain Substances 0.000 claims description 50
- 239000010432 diamond Substances 0.000 claims description 36
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 claims description 32
- 239000002245 particle Substances 0.000 claims description 22
- 239000013078 crystal Substances 0.000 claims description 14
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 238000007747 plating Methods 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 7
- 239000010452 phosphate Substances 0.000 claims description 7
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 6
- XXSPKSHUSWQAIZ-UHFFFAOYSA-L 36026-88-7 Chemical compound [Ni+2].[O-]P=O.[O-]P=O XXSPKSHUSWQAIZ-UHFFFAOYSA-L 0.000 claims description 4
- 229910052580 B4C Inorganic materials 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- GJYJYFHBOBUTBY-UHFFFAOYSA-N alpha-camphorene Chemical compound CC(C)=CCCC(=C)C1CCC(CCC=C(C)C)=CC1 GJYJYFHBOBUTBY-UHFFFAOYSA-N 0.000 claims description 4
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910001382 calcium hypophosphite Inorganic materials 0.000 claims description 4
- 229940064002 calcium hypophosphite Drugs 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 229910001380 potassium hypophosphite Inorganic materials 0.000 claims description 4
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- CNALVHVMBXLLIY-IUCAKERBSA-N tert-butyl n-[(3s,5s)-5-methylpiperidin-3-yl]carbamate Chemical compound C[C@@H]1CNC[C@@H](NC(=O)OC(C)(C)C)C1 CNALVHVMBXLLIY-IUCAKERBSA-N 0.000 claims description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 19
- 230000007797 corrosion Effects 0.000 abstract description 19
- 239000010410 layer Substances 0.000 description 51
- 229910003460 diamond Inorganic materials 0.000 description 29
- 238000009713 electroplating Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 229910052759 nickel Inorganic materials 0.000 description 10
- 238000001878 scanning electron micrograph Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 7
- 235000012431 wafers Nutrition 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical class O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- NQXGLOVMOABDLI-UHFFFAOYSA-N sodium oxido(oxo)phosphanium Chemical compound [Na+].[O-][PH+]=O NQXGLOVMOABDLI-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Polishing Bodies And Polishing Tools (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
Description
本發明是有關於一種磨線的改良技術，且特別是有關於一種磷化磨粒的方法、含Ni 2P的磨粒及含前述磨粒的切割線。 The present invention relates to an improved technology for grinding wires, and in particular, to a method of phosphating abrasive grains, abrasive grains containing Ni 2 P and cutting wires containing the aforementioned abrasive grains.
在現今半導體產業及太陽能產業上，矽晶圓的需求越來越大。然而，在傳統製程中的晶圓切割所採用的是內圓切割刀，這個方法是使用一圓形刀片，裡面鑲上鑽石使其具有切割高硬度的矽晶圓的能力。但是，這種內圓切割刀每次只能切割出一片晶圓，造成產出效率太慢，晶圓尺寸也會受到限制，而無法達到需求。In today's semiconductor industry and solar energy industry, the demand for silicon wafers is increasing. However, wafer cutting in the traditional process uses an internal dicing knife. This method uses a circular blade with diamonds embedded inside to make it capable of cutting high-hardness silicon wafers. However, this kind of inner circle cutting knife can only cut one wafer at a time, resulting in too slow output efficiency and limited wafer size, making it impossible to meet demand.
因此，目前使用多條鑽石切割線同時進行切割。例如一次使用10條鑽石線，就能一次產出10片晶圓，產出效率為傳統方法的十倍；依此類推。鑽石切割線主要是在不銹鋼線表面，通過電鍍的方式同時將鑽石粒和鎳沉積於線上，利用鎳金屬包覆鑽石粒並將其固定在不銹鋼線表面，稱為上砂（tack-on process）。之後使用時磨掉外層的鎳層，使鑽石粒裸露出來，即可切割高硬度的矽晶圓。Therefore, multiple diamond cutting lines are currently used to cut simultaneously. For example, using 10 diamond wires at a time can produce 10 wafers at a time, and the output efficiency is ten times that of traditional methods; and so on. The diamond cutting wire is mainly on the surface of the stainless steel wire. Diamond particles and nickel are deposited on the wire at the same time through electroplating. The diamond particles are covered with nickel metal and fixed on the surface of the stainless steel wire. This is called the tack-on process. . When used later, the outer nickel layer is ground off to expose the diamond grains, and high-hardness silicon wafers can be cut.
由於鑽石粒本身不是導體，所以為了滿足上述電鍍要求，會先在鑽石粒表面無電鍍鎳金屬化，賦予導電性。然而，商用鍍鎳鑽石粒在上砂電鍍液中有腐蝕問題亟待解決。一旦鑽石粒表面的鍍層被腐蝕，將影響鑽石粒在不銹鋼線表面的數量與分布密度，導致鑽石切割線的品質變差。Since the diamond particles themselves are not conductors, in order to meet the above electroplating requirements, the surface of the diamond particles is first electrolessly plated with nickel metallization to impart conductivity. However, commercial nickel-plated diamond particles have corrosion problems in the sand plating solution that need to be solved urgently. Once the coating on the surface of the diamond grains is corroded, it will affect the number and distribution density of the diamond grains on the surface of the stainless steel wire, causing the quality of the diamond cutting wire to deteriorate.
本發明提供一種磷化磨粒的方法，能改善鍍鎳磨粒的腐蝕問題。The invention provides a method for phosphating abrasive grains, which can improve the corrosion problem of nickel-plated abrasive grains.
本發明另提供一種含Ni 2P的磨粒，具有優異的抗腐蝕性。 The present invention also provides an abrasive grain containing Ni 2 P, which has excellent corrosion resistance.
本發明再提供一種含前述磨粒的切割線，以改善切割線品質。The present invention further provides a cutting wire containing the aforementioned abrasive particles to improve the quality of the cutting wire.
本發明的磷化磨粒的方法，包括於磨粒的表面形成至少一含鎳磷的金屬層，然後進行磷化反應，以於所述至少一含鎳磷的金屬層的表面形成富磷化層。The method of phosphating abrasive grains of the present invention includes forming at least one nickel-phosphorus-containing metal layer on the surface of the abrasive grains, and then performing a phosphating reaction to form a rich phosphating layer on the surface of the at least one nickel-phosphorus-containing metal layer. layer.
在本發明的一實施例中，上述磷化反應包括在惰性氣體的環境下利用次磷酸鹽或磷化氫（PH 3）進行磷化。 In one embodiment of the present invention, the above-mentioned phosphating reaction includes using hypophosphite or phosphine (PH 3 ) to perform phosphating in an inert gas environment.
在本發明的一實施例中，上述次磷酸鹽包括次磷酸鈉、次磷酸鈣、次磷酸鎳、次磷酸銨或次磷酸鉀。In one embodiment of the present invention, the above-mentioned hypophosphite salt includes sodium hypophosphite, calcium hypophosphite, nickel hypophosphite, ammonium hypophosphite or potassium hypophosphite.
在本發明的一實施例中，上述富磷化層的磷含量為18 wt%以上。In an embodiment of the present invention, the phosphorus content of the above-mentioned phosphate-rich layer is more than 18 wt%.
在本發明的一實施例中，上述磷化反應的溫度在150°C ~350°C，時間為1小時至3小時。In an embodiment of the present invention, the temperature of the above-mentioned phosphating reaction is 150°C ~ 350°C, and the time is 1 hour to 3 hours.
在本發明的一實施例中，上述富磷化層的厚度在0.01微米～1微米之間。In an embodiment of the present invention, the thickness of the above-mentioned phosphate-rich layer is between 0.01 micron and 1 micron.
在本發明的一實施例中，上述富磷化層包括Ni 2P。 In an embodiment of the present invention, the phosphorus-rich layer includes Ni 2 P.
在本發明的一實施例中，形成上述至少一含鎳磷的金屬層的方法包括於所述磨粒的所述表面無電鍍第一鎳磷層，再於所述第一鎳磷層表面電鍍第二鎳磷層。In one embodiment of the present invention, the method for forming the above-mentioned at least one nickel-phosphorus-containing metal layer includes electrolessly plating a first nickel-phosphorus layer on the surface of the abrasive grain, and then electroplating on the surface of the first nickel-phosphorus layer. Second nickel phosphorus layer.
在本發明的一實施例中，上述第一鎳磷層的厚度與上述第二鎳磷層的厚度各自在0.01微米～1微米之間。In an embodiment of the present invention, the thickness of the first nickel phosphorus layer and the thickness of the second nickel phosphorus layer are each between 0.01 micron and 1 micron.
本發明的含Ni 2P的磨粒是在其表面至少包含具有Ni 2P晶相的鍍層。 The Ni 2 P-containing abrasive grain of the present invention contains at least a plating layer having a Ni 2 P crystal phase on its surface.
在本發明的另一實施例中，上述鍍層中的磷含量在18 wt%以上。In another embodiment of the present invention, the phosphorus content in the above-mentioned coating is above 18 wt%.
在本發明的另一實施例中，上述鍍層還可包括Ni 2P晶相以外的鎳磷晶相。 In another embodiment of the present invention, the above-mentioned plating layer may also include a nickel phosphorus crystal phase other than the Ni 2 P crystal phase.
在本發明的以上實施例中，上述磨粒的材料包括天然鑽石、人工鑽石、氮化硼、碳化矽、碳化硼或氧化鋁。In the above embodiments of the present invention, the material of the abrasive grains includes natural diamonds, artificial diamonds, boron nitride, silicon carbide, boron carbide or aluminum oxide.
本發明的切割線包含前述含Ni 2P的磨粒。 The cutting wire of the present invention contains the aforementioned Ni 2 P-containing abrasive grains.
在本發明的再一實施例中，上述切割線為不銹鋼線，且磨粒電鍍於所述不銹鋼線的表面。In yet another embodiment of the present invention, the cutting wire is a stainless steel wire, and abrasive particles are electroplated on the surface of the stainless steel wire.
基於上述，本發明通過特殊的磷化反應，使磨粒表面形成具有優異的抗腐蝕性的Ni 2P晶相，因此能防止上砂過程中磨粒表面的金屬層被上砂電鍍液腐蝕的問題發生，從而可製作出品質佳的切割線。 Based on the above, the present invention uses a special phosphating reaction to form a Ni 2 P crystal phase with excellent corrosion resistance on the surface of the abrasive grains, thereby preventing the metal layer on the surface of the abrasive grains from being corroded by the sanding electroplating solution during the sanding process. problem occurs so that a good quality cutting line can be produced.
為讓本發明的上述特徵和優點能更明顯易懂，下文特舉實施例，並配合所附圖式作詳細說明如下。In order to make the above-mentioned features and advantages of the present invention more obvious and easy to understand, embodiments are given below and described in detail with reference to the accompanying drawings.
以下將參考圖式來全面地描述本發明的例示性實施例，但本發明還可按照多種不同形式來實施，且不應解釋為限於本文所述的實施例。在圖式中，為了清楚起見，各層及顆粒的厚度與大小並未按實際比例繪製。Exemplary embodiments of the present invention will be fully described below with reference to the accompanying drawings, although the invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. In the drawings, the thickness and size of the layers and particles are not drawn to actual scale for the sake of clarity.
圖1是依照本發明的一實施例的一種磷化磨粒的方法示意圖。Figure 1 is a schematic diagram of a method for phosphating abrasive particles according to an embodiment of the present invention.
請參照圖1，本實施例的磷化鑽石粒的方法包括於磨粒100的表面100a形成至少一含鎳磷的金屬層102，例如於磨粒100的表面100a先無電鍍第一鎳磷層102a，再於第一鎳磷層102a表面電鍍第二鎳磷層102b，其中第一鎳磷層102a的厚度例如在0.01微米～1微米之間、第二鎳磷層102b的厚度例如在0.01微米～1微米之間，且通過無電鍍形成的第一鎳磷層102a中的含磷量可為0.1 wt%到14 wt%。上述磨粒100的材料例如天然鑽石、人工鑽石、氮化硼、碳化矽、碳化硼或氧化鋁。然後，進行磷化反應，以於含鎳磷的金屬層102的表面形成富磷化層104，其中富磷化層104的磷含量為18 wt%以上。Referring to FIG. 1 , the method of phosphating diamond grains in this embodiment includes forming at least one
在一實施例中，所述磷化反應包括在惰性氣體的環境下利用次磷酸鹽或磷化氫（PH 3）進行磷化，其反應式如下： 2NaH 2PO 2→ Na 2HPO 4+ PH 32PH 3→ 2P + 3H 22Ni + P → Ni 2P In one embodiment, the phosphating reaction includes phosphating using hypophosphite or phosphine (PH 3 ) in an inert gas environment, and the reaction formula is as follows: 2NaH 2 PO 2 → Na 2 HPO 4 + PH 3 2PH 3 → 2P + 3H 2 2Ni + P → Ni 2 P
上述反應式是以次磷酸鈉（Sodium hypophosphite，NaH 2PO 2）作為次磷酸鹽的實例，但本發明並不限於此，次磷酸鹽也可改用次磷酸鈣（Calcium hypophosphite）、次磷酸鎳（Nickel hypophosphite）、磷酸銨（Ammonium hypophosphite）或次磷酸鉀（Potassium hypophosphite）。上述惰性氣體例如氮氣、氦氣或氬氣。上述磷化反應的溫度例如在150°C ~350°C，時間例如1小時至3小時。 The above reaction formula uses sodium hypophosphite (NaH 2 PO 2 ) as an example of hypophosphite, but the invention is not limited thereto. Calcium hypophosphite (Calcium hypophosphite) or nickel hypophosphite can also be used as the hypophosphite. (Nickel hypophosphite), ammonium hypophosphite (Ammonium hypophosphite) or potassium hypophosphite (Potassium hypophosphite). The above-mentioned inert gases include nitrogen, helium or argon. The temperature of the above-mentioned phosphating reaction is, for example, 150°C to 350°C, and the time is, for example, 1 hour to 3 hours.
磷化反應後得到的富磷化層104即包含Ni
2P，而完成含Ni
2P的磨粒106的製備，其表面至少包含具有Ni
2P晶相的鍍層（即富磷化層104），其磷含量在18 wt%以上，例如20 wt% ~ 22 wt%之間。富磷化層104的厚度例如在0.01微米～1微米之間。再者，上述鍍層還可包括少量的Ni
2P晶相以外的鎳磷晶相（如Ni
12P
5）。
The
圖2是依照本發明的另一實施例的一種切割線的示意圖，其中使用與上一實施例相同的元件符號來表示相同或近似的部分與構件，且相同或近似的部分與構件的相關內容也可參照上一實施例的內容，不再贅述。Figure 2 is a schematic diagram of a cutting line according to another embodiment of the present invention, in which the same element symbols as in the previous embodiment are used to represent the same or similar parts and components, and the related content of the same or similar parts and components Reference may also be made to the contents of the previous embodiment, which will not be described again.
含Ni
2P的磨粒106是電鍍於切割線200的表面200a。舉例來說，含Ni
2P的磨粒106是通過電鍍的方式與電鍍鎳層202一起沉積於切割線200上，利用電鍍鎳層202包覆含Ni
2P的磨粒106並將其固定在切割線200表面，完成前述上砂製程後，於使用時含Ni
2P的磨粒106外層的鎳層會被磨掉，因而成為圖2所示的裸露出來的含Ni
2P的鑽石粒106。由於Ni
2P具有優異抗腐蝕性，所以上砂過程中含Ni
2P的磨粒106仍保有幾乎完整的富磷化層104，使含Ni
2P的鑽石粒106在切割線200表面的數量與分布密度維持在需求範圍內，而完成品質佳的鑽石切割線。
以下列舉實驗來驗證本發明的功效，但本發明並不侷限於以下的內容。The following experiments are listed to verify the efficacy of the present invention, but the present invention is not limited to the following content.
〈比較例1〉<Comparative example 1>
市售僅單層無電鍍鎳、核心為工業鑽石之金屬披覆磨粒。On the market, there is only a single layer of electroless nickel-plated metal-coated abrasive grains with an industrial diamond core.
〈比較例2〉<Comparative example 2>
市售外層電鍍鎳、內層無電鍍鎳磷、核心為工業鑽石之金屬披覆磨粒。利用XRD分析其晶體結構，結果顯示於圖3。Commercially available metal-coated abrasive grains with an outer layer of electroplated nickel, an inner layer of electroless nickel-phosphorus plating, and an industrial diamond core. The crystal structure was analyzed by XRD, and the results are shown in Figure 3.
〈實驗例1〉<Experimental example 1>
使用比較例2作為鑽石粉，然後使用如圖4所示的設備進行磷化。詳細而言，先將50 mg金屬化的前述鑽石粉與1g次磷酸鈉粉體（SHOWA製）分別置入通有氮氣的環境下以每分鐘10°C升溫至300°C，由於次磷酸鹽在300°C時會分解放出磷化氫(PH 3)氣體，所以可作為磷源，並進行持溫一小時的磷化反應。最後尾氣由於包含磷化氫成分，需做尾氣處理，例如利用活性碳、漂白水或是含銅金屬離子之水溶液進行反應或是吸附。 Comparative Example 2 was used as diamond powder, and then the equipment shown in Figure 4 was used for phosphating. Specifically, 50 mg of the metallized diamond powder and 1 g of sodium hypophosphite powder (manufactured by SHOWA) were placed in a nitrogen atmosphere and heated to 300°C at 10°C per minute. It will decompose and release phosphine (PH 3 ) gas at 300°C, so it can be used as a phosphorus source and carry out a phosphating reaction that is maintained at temperature for one hour. Finally, because the exhaust gas contains phosphine components, it needs to be treated by exhaust gas treatment, such as using activated carbon, bleach water or an aqueous solution containing copper metal ions for reaction or adsorption.
將磷化反應後的產物乾燥後，利用XRD分析其晶體結構，結果同樣顯示於圖3。 After drying the product after the phosphating reaction, XRD was used to analyze its crystal structure. The results are also shown in Figure 3.
〈實驗例2〉<Experimental example 2>
採用實驗例1的方式，但是改為持溫兩小時的磷化反應。將產物乾燥後利用XRD分析其晶體結構，結果同樣顯示於圖3。 The method of Experimental Example 1 was adopted, but the phosphating reaction was changed to a two-hour phosphating reaction. The crystal structure of the product was analyzed by XRD after drying, and the results are also shown in Figure 3.
從圖3可得到，實驗例1和2的XRD圖譜在40°附近明顯有一個繞射峰，為Ni 2P晶相，其中實驗例2由於持溫時間加長，可以看出Ni 2P繞射峰比實驗例1為高。顯示時間加長，反應量增加。而比較例2的XRD圖譜在40°附近沒有明顯繞射峰。 It can be seen from Figure 3 that the XRD patterns of Experimental Examples 1 and 2 clearly have a diffraction peak near 40°, which is the Ni 2 P crystal phase. In Experimental Example 2, due to the longer temperature holding time, it can be seen that Ni 2 P diffraction The peak is higher than that of Experimental Example 1. The display time is lengthened and the response volume is increased. However, the XRD pattern of Comparative Example 2 has no obvious diffraction peak near 40°.
〈抗腐蝕性〉〈Corrosion resistance〉
由於上砂電鍍液中含有氫離子，可與鑽石粒表面的金屬鎳起反應，造成腐蝕發生。具體來說，當鑽石粒還沒碰到陰極之前，鑽石粒表面的金屬就無法進行電鍍反應，但是腐蝕反應還是會繼續發生，且鑽石粒的表面積比一般板材大很多，導致腐蝕的問題被放大。因此針對抗腐蝕性進行以下腐蝕試驗。Since the sand plating solution contains hydrogen ions, it can react with the metallic nickel on the surface of the diamond particles, causing corrosion. Specifically, before the diamond particles touch the cathode, the metal on the surface of the diamond particles cannot undergo electroplating reaction, but the corrosion reaction will still continue to occur, and the surface area of the diamond particles is much larger than that of ordinary plates, causing the corrosion problem to be amplified. . The following corrosion tests were therefore carried out for corrosion resistance.
首先，準備的電鍍液配方如下表1。First, prepare the electroplating solution formula as shown in Table 1.
表1 (pH值為3.63、溫度為55至60 °C)
首先，將實驗例1、實驗例2的產物浸泡在上述電鍍液中4小時，再用SEM觀察，分別得到圖5A、圖5B的SEM影像。First, the products of Experimental Example 1 and Experimental Example 2 were immersed in the above-mentioned plating solution for 4 hours, and then observed with SEM to obtain the SEM images of Figure 5A and Figure 5B respectively.
對比較例1、比較例2的產物重複上述腐蝕試驗後，同樣取得浸泡4小時的金屬披覆磨粒的SEM影像，並顯示於圖6A與圖6B。圖6A是比較例1經腐蝕試驗後的SEM影像；圖6B是比較例2經腐蝕試驗後的SEM影像。After repeating the above corrosion test on the products of Comparative Example 1 and Comparative Example 2, SEM images of the metal-coated abrasive grains soaked for 4 hours were also obtained, and are shown in Figures 6A and 6B. Figure 6A is the SEM image of Comparative Example 1 after the corrosion test; Figure 6B is the SEM image of Comparative Example 2 after the corrosion test.
從圖5A與圖5B可觀察到，大部分磨粒表面仍保有金屬層(亮面區域)，同時磨粒彼此團聚現象不明顯。相比之下，圖6A與圖6B的磨粒表面較暗，代表表面的金屬成分包含底層在4小時內均已腐蝕殆盡。It can be observed from Figure 5A and Figure 5B that the surface of most abrasive grains still retains a metal layer (bright surface area), and the agglomeration of the abrasive grains with each other is not obvious. In comparison, the surfaces of the abrasive grains in Figures 6A and 6B are darker, which means that the metal components on the surface, including the bottom layer, have been corroded within 4 hours.
圖7A與圖7B分別是實驗例1~2的產物經由電鍍(使用上述電鍍液電鍍)形成在不銹鋼線上的SEM影像。從圖7A與圖7B可觀察到，磨粒覆著量佳，同時磨粒彼此團聚現象不明顯。Figures 7A and 7B are respectively SEM images of the products of Experimental Examples 1 to 2 formed on stainless steel wires through electroplating (plating using the above electroplating solution). It can be observed from Figure 7A and Figure 7B that the abrasive grain coating amount is good, and the agglomeration of the abrasive grains with each other is not obvious.
綜上所述，本發明通過磷化反應，以於鑽石粒表面形成具有抗腐蝕性佳的富磷化層，因此能防止鑽石粒表面的金屬層被上砂電鍍液腐蝕，從而可製作出品質佳的切割線。In summary, the present invention uses a phosphating reaction to form a rich phosphating layer with good corrosion resistance on the surface of diamond particles. Therefore, it can prevent the metal layer on the surface of diamond particles from being corroded by the sand electroplating solution, thereby making it possible to produce high-quality products. Best cutting line.
雖然本發明已以實施例揭露如上，然其並非用以限定本發明，任何所屬技術領域中具有通常知識者，在不脫離本發明的精神和範圍內，當可作些許的更動與潤飾，故本發明的保護範圍當視後附的申請專利範圍所界定者為準。Although the present invention has been disclosed above through embodiments, they are not intended to limit the present invention. Anyone with ordinary knowledge in the technical field may make some modifications and modifications without departing from the spirit and scope of the present invention. Therefore, The protection scope of the present invention shall be determined by the appended patent application scope.
100:磨粒
100a、200a:表面
102:含鎳磷的金屬層
102a:第一鎳磷層
102b:第二鎳磷層
104:富磷化層
106:含Ni
2P的鑽石粒
200:切割線
202:電鍍鎳層
100:
圖1是依照本發明的一實施例的一種磷化磨粒的方法示意圖。 圖2是依照本發明的另一實施例的一種切割線的示意圖。 圖3是實驗例1~2與比較例2的X光繞射（XRD）圖。 圖4是實驗例1~2的磷化處理的設備圖。 圖5A是實驗例2的產物的掃描式電子顯微鏡(SEM)影像。 圖5B是實驗例2的產物經過腐蝕試驗的SEM影像。 圖6A是比較例1的產物經腐蝕試驗後的SEM影像。 圖6B是比較例2的產物經腐蝕試驗後的SEM影像。 圖7A是實驗例1的產物經由電鍍形成在不銹鋼線上的SEM影像。 圖7B是實驗例2的產物經由電鍍形成在不銹鋼線上的SEM影像。 Figure 1 is a schematic diagram of a method for phosphating abrasive particles according to an embodiment of the present invention. Figure 2 is a schematic diagram of a cutting line according to another embodiment of the present invention. Figure 3 is an X-ray diffraction (XRD) chart of Experimental Examples 1 to 2 and Comparative Example 2. Figure 4 is an equipment diagram of the phosphating treatment of Experimental Examples 1 to 2. Figure 5A is a scanning electron microscope (SEM) image of the product of Experimental Example 2. Figure 5B is an SEM image of the product of Experimental Example 2 after a corrosion test. Figure 6A is an SEM image of the product of Comparative Example 1 after a corrosion test. Figure 6B is an SEM image of the product of Comparative Example 2 after the corrosion test. Figure 7A is an SEM image of the product of Experimental Example 1 formed on a stainless steel wire through electroplating. Figure 7B is an SEM image of the product of Experimental Example 2 formed on a stainless steel wire through electroplating.
100:磨粒 100:Abrasive grains
100a:表面 100a: Surface
102:金屬層 102:Metal layer
102a:第一鎳磷層 102a: First nickel phosphorus layer
102b:第二鎳磷層 102b: Second nickel-phosphorus layer
104:富磷化層 104: Rich phosphate layer
106:含Ni2P的磨粒 106: Abrasive grains containing Ni 2 P
Claims (15)
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