ALUMINUM PRECURSOR AND PROCESS FOR THE GENERATION OF METAL-CONTAINING FILMS

20210024549 ยท 2021-01-28

    Inventors

    Cpc classification

    International classification

    Abstract

    The present disclosure is in the field of processes for the generation of thin inorganic films on substrates, in particular atomic layer deposition processes. Described herein is a process for preparing metal-containing films including: (a) depositing a metal-containing compound from the gaseous state onto a solid substrate, and (b) bringing the solid substrate with the deposited metal-containing compound in contact with a compound of general formula (I)

    ##STR00001## wherein Z is a C.sub.2-C.sub.4 alkylene group, and R is hydrogen, an alkyl group, an alkenyl group, an aryl group, or a silyl group.

    Claims

    1. Process for preparing metal-containing films, the process comprising: (a) depositing a metal-containing compound from a gaseous state onto a solid substrate, and (b) bringing the solid substrate with the deposited metal-containing compound in contact with a compound of general formula (I) ##STR00005## wherein Z is a C.sub.2-C.sub.4 alkylene group, and R is hydrogen, an alkyl group, an alkenyl group, an aryl group, or a silyl group.

    2. The process according to claim 1, wherein R comprises no hydrogen atom in the 1-position.

    3. The process according to claim 2, wherein R is tert-butyl.

    4. The process according to claim 1, wherein Z is ethylene.

    5. The process according to claim 1, wherein the compound of general formula (I) has a molecular weight of not more than 600 g/mol.

    6. The process according to claim 1, wherein the compound of general formula (I) has a vapor pressure of at least 1 mbar at a temperature of 200 C.

    7. The process according to claim 1, wherein (a) and (b) are successively performed at least twice.

    8. The process according to claim 1, wherein the metal-containing compound contains Ti, Ta, Mn, Mo, W, or Al.

    9. The process according to claim 1, wherein the metal-containing compound is a metal halide.

    10. The process according to claim 1, wherein a temperature does not exceed 350 C.

    11. A compound of general formula (I), ##STR00006## wherein Z is a C.sub.2-C.sub.4 alkylene group, and R is hydrogen, an alkyl group, an alkenyl group, an aryl group, or a silyl group.

    12. The compound according to claim 11, wherein R comprises no hydrogen atom in the 1-position.

    13. The compound according to claim 12, wherein R is tert-butyl.

    14. The compound according to claim 11, wherein Z is ethylene.

    Description

    BRIEF DESCRIPTION OF THE FIGURES

    [0051] FIG. 1 shows the thermogravimetry (TG) and the differential thermogravimetry (DTG) curves of compound I-1.

    [0052] FIG. 2 shows the vapor pressure (P) dependence on the temperature (T) of compound I-1.

    [0053] FIG. 3 shows the crystal structure of compound C-1 as obtained from single crystal X-ray diffraction analysis.

    [0054] FIG. 4 shows the grazing incidence X-ray diffractogram (GIXRD) for examples 2 and 3.

    EXAMPLES

    Example 1: Synthesis of I-1

    [0055] ##STR00004##

    [0056] NN-di-tert-butyl imidazolidene-2-yl was heated with 2 equivalents of AlH.sub.3(NMe.sub.3) in refluxing toluene until evolution of NMe.sub.3 ceased after about 30 min. Evaporation of the solvent allowed isolation of C-1 in 82% yield.

    [0057] The thermogravimetry curve is shown in FIG. 1. The weight loss at 200 C. is 76.6%, at 500 C. it is 95.3%. Vapor pressure measurements are shown in FIG. 2, wherein the triangles, squares and crosses represent results of different measurements and the solid line is a line fit for the results below 150 C.

    [0058] Crystals suitable for X-ray diffraction analysis were grown from a concentrated toluene solution at 20 C. The crystal structure is shown in FIG. 3.

    Example 2: Al Film Deposition on TiN

    [0059] A TiN substrate was kept at 140 C. in an ALD apparatus. A supply of AlCl.sub.3 was kept at 95 C., a separate supply for compound I-1 was kept at 100 C. 300 cycles were performed, wherein one cycle was: 2 s AlCl.sub.3, 20 s nitrogen purge, 3 s compound I-1, 10 s nitrogen purge.

    Example 3: Al Film Deposition on Cu

    [0060] Example 2 was repeated, but instead of TiN, a Cu substrate was used.

    [0061] FIG. 4 shows the grazing incidence X-ray diffractogram (GIXRD) measured under an angle of 1 for both samples obtained in examples 2 and 3. Reflections matching Al metal are indicated in the diffractogram.